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CN111781148B - Method, device, terminal and system for detecting longitudinal non-uniformity of film - Google Patents

Method, device, terminal and system for detecting longitudinal non-uniformity of film
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CN111781148B
CN111781148BCN201910273286.3ACN201910273286ACN111781148BCN 111781148 BCN111781148 BCN 111781148BCN 201910273286 ACN201910273286 ACN 201910273286ACN 111781148 BCN111781148 BCN 111781148B
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CN111781148A (en
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孙瑶
钟大龙
王新宇
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Shanghai Zhuyang New Energy Technology Co ltd
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Shenhua Beijing Photovoltaic Technology Research And Development Co ltd
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Abstract

The invention discloses a method, a device, a system and a terminal for detecting longitudinal non-uniformity of a film, which relate to the technical field of film detection and aim to improve the application range of a method for nondestructive detection of the longitudinal non-uniformity of the film. The method for detecting the longitudinal non-uniformity of the film comprises the following steps: receiving ellipsometry curve information of a sample to be detected, wherein the sample to be detected at least comprises a film to be detected; establishing an isotropic physical model according to the characteristics of the measured sample, wherein the physical model at least comprises a film model; converting at least one variable parameter contained in the film model into a graded variable parameter; taking ellipsometry curve information of a measured sample as a curve fitting target, and performing curve fitting on the graded variable parameters by using a film model to obtain variation curve information of the photoelectric parameters of the measured sample in the longitudinal direction of the measured sample; and determining the longitudinal non-uniformity of the tested sample according to the change curve information. The invention is used for detecting the longitudinal non-uniformity of the film.

Description

Translated fromChinese
一种薄膜纵向不均匀性检测方法、装置及终端和检测系统A film longitudinal non-uniformity detection method, device, terminal and detection system

技术领域Technical field

本发明涉及薄膜检测技术领域,尤其涉及一种薄膜纵向不均匀性检测方法、装置及终端和检测系统。The invention relates to the technical field of film detection, and in particular to a method, device, terminal and detection system for detecting longitudinal non-uniformity of a film.

背景技术Background technique

透明导电氧化物(Transparent Conductive Oxide,简称TCO)薄膜是一种重要的光学材料,以禁带宽、电阻率低、可见光范围光透射率高和红外光谱区光反射率高等光电特性在透明导电薄膜中占主导地位,广泛应用于太阳能电池、液晶显示器、气体传感器、飞机和汽车用导热玻璃(防雾和防结冰)等光电领域。Transparent Conductive Oxide (TCO) film is an important optical material. It is widely used in transparent conductive films for its optoelectronic properties such as forbidden bandwidth, low resistivity, high light transmittance in the visible range and high light reflectivity in the infrared spectrum. Dominant, widely used in photovoltaic fields such as solar cells, liquid crystal displays, gas sensors, thermal conductive glass for aircraft and automobiles (anti-fog and anti-icing).

TCO薄膜中的氧含量对光电性能有重要影响,若氧含量低,则TCO薄膜呈现类金属的颜色而失去透明性;若氧含量高,则氧空位数量减少,使得外来施主杂质失去掺杂的效果,导致TCO薄膜的化学成分接近于绝缘体直至变为绝缘体;当氧含量适当时,TCO薄膜中氧空位数量适当,替位杂质发挥了施主的作用,TCO薄膜光电性能俱佳。在镀膜过程中,由于工艺缘故,不可避免地存在氧含量沿TCO薄膜表面纵向分布的不均匀性,这是由于TCO薄膜表面弛豫与表面能作用,使得其表面与内部所含有的成分过渡,以实现能量与物质之间的平衡。TCO薄膜表面的纵向不均匀性对薄膜的光电性能有重要影响,因此,需要检测薄膜材料的纵向不均匀。The oxygen content in the TCO film has an important impact on the photoelectric performance. If the oxygen content is low, the TCO film will have a metal-like color and lose transparency; if the oxygen content is high, the number of oxygen vacancies will decrease, causing the foreign donor impurities to lose the ability to be doped. The effect causes the chemical composition of the TCO film to be close to that of an insulator until it becomes an insulator; when the oxygen content is appropriate, the number of oxygen vacancies in the TCO film is appropriate, and the substitutional impurities play the role of donors, and the TCO film has excellent photoelectric properties. During the coating process, due to process reasons, there is inevitably uneven distribution of oxygen content along the longitudinal direction of the TCO film surface. This is due to the interaction of surface relaxation and surface energy of the TCO film, which causes the transition between the components contained on the surface and inside. To achieve a balance between energy and matter. The longitudinal unevenness of the TCO film surface has an important impact on the optical and electrical properties of the film. Therefore, it is necessary to detect the longitudinal unevenness of the film material.

现有技术中,采用深度剖析法测试TCO薄膜中元素成分随深度的变化,根据TCO薄膜中元素成分随深度的变化确定薄膜纵向不均匀性。深度剖析法所使用的测试仪器一般为X射线光电子能谱仪(XPS)、俄歇电子能谱仪(AES)、二次离子质谱仪(SIMS)或辉光放电光谱仪(GDOES),但是这些测试仪器在检测过程中,不可避免地会损伤被测样品。目前,已经出现了一些无损测试薄膜纵向不均匀性的技术,但是其应用范围比较窄。In the existing technology, the depth profiling method is used to test the changes in elemental components in the TCO film with depth, and the longitudinal unevenness of the film is determined based on the changes in the elemental components in the TCO film with depth. The test instruments used in the depth profiling method are generally X-ray photoelectron spectrometer (XPS), Auger electron spectrometer (AES), secondary ion mass spectrometer (SIMS) or glow discharge spectrometer (GDOES). However, these tests During the testing process, the instrument will inevitably damage the sample being tested. At present, some technologies for non-destructively testing the longitudinal non-uniformity of films have emerged, but their application scope is relatively narrow.

发明内容Contents of the invention

本发明的实施例提供一种薄膜纵向不均匀性检测方法、装置及终端和检测系统,以提高无损薄膜纵向不均匀性检测方法的适用范围。Embodiments of the present invention provide a method, device, terminal and detection system for detecting longitudinal non-uniformity of a film, so as to improve the applicable scope of the method for detecting longitudinal non-uniformity of a non-destructive film.

为达到上述目的,本发明的实施例采用如下技术方案:In order to achieve the above objects, embodiments of the present invention adopt the following technical solutions:

第一方面,本发明提供了一种薄膜纵向不均匀性检测方法,包括:In a first aspect, the present invention provides a method for detecting longitudinal non-uniformity of a film, including:

获取被测样品的椭偏光谱曲线信息,所述被测样品至少包括被测薄膜;Obtain ellipsometric spectral curve information of the sample being tested, which sample at least includes the film being tested;

根据所述被测样品的特性建立各向同性的物理模型,所述物理模型至少包括薄膜模型;Establish an isotropic physical model according to the characteristics of the measured sample, and the physical model at least includes a thin film model;

将所述薄膜模型所含有的至少一个变量参数转换为至少一组梯度化变量参数;Convert at least one variable parameter contained in the film model into at least one set of gradient variable parameters;

以所述被测样品的椭偏光谱曲线信息为曲线拟合目标,利用所述薄膜模型对至少一组梯度化变量参数进行曲线拟合,获得被测样品的光电参数在被测样品纵向方向上的变化曲线信息;Using the ellipsometric spectral curve information of the tested sample as a curve fitting target, the film model is used to perform curve fitting on at least one set of gradient variable parameters to obtain the photoelectric parameters of the tested sample in the longitudinal direction of the tested sample. change curve information;

根据所述被测样品的光电参数在被测样品纵向方向上的变化曲线信息确定被测样品的纵向不均匀性。The longitudinal non-uniformity of the tested sample is determined based on the change curve information of the photoelectric parameters of the tested sample in the longitudinal direction of the tested sample.

在一些实施例中,所述进行曲线拟合的收敛条件为均方误差值小于80。In some embodiments, the convergence condition for curve fitting is that the mean square error value is less than 80.

在一些实施例中,所述进行曲线拟合的收敛条件为均方误差值小于20。In some embodiments, the convergence condition for curve fitting is that the mean square error value is less than 20.

在一些实施例中,所述被测样品的光电参数包括满足克莱默-克朗尼格关系的光学常数和/或满足克莱默-克朗尼格关系的介电常数。In some embodiments, the photoelectric parameters of the measured sample include optical constants that satisfy the Kramer-Kronig relationship and/or dielectric constants that satisfy the Kramer-Kronig relationship.

在一些实施例中,所述物理模型还包括基体模型和表面模型,所述薄膜模型位于所述基体模型和所述表面模型之间,所述基体模型为柯西模型,所述薄膜模型为洛伦兹模型或高斯模型,所述表面模型为有效介质模型。In some embodiments, the physical model further includes a matrix model and a surface model, the film model is located between the matrix model and the surface model, the matrix model is a Cauchy model, and the film model is a Lowe model. Lentz model or Gaussian model, the surface model is an effective medium model.

在一些实施例中,所述将所述薄膜模型所含有的至少一个变量参数转换为至少一组梯度化变量参数包括:In some embodiments, converting at least one variable parameter contained in the film model into at least one set of gradient variable parameters includes:

按照对拟合结果影响权重由高到低的顺序,选择薄膜模型中的一个或两个变量参数进行梯度化转换;Select one or two variable parameters in the film model for gradient conversion in order of their impact on the fitting results from high to low;

和/或,and / or,

所述梯度化变量参数包括线性梯度变化的变量参数或非线性梯度变化的变量参数。The gradient variable parameters include variable parameters with linear gradient changes or variable parameters with nonlinear gradient changes.

第二方面,本发明还提供了一种薄膜纵向不均匀性检测装置,包括:In a second aspect, the present invention also provides a film longitudinal non-uniformity detection device, including:

接收单元,用于获取被测样品的椭偏光谱曲线信息,所述被测样品至少包括被测薄膜;A receiving unit, configured to obtain ellipsometric spectral curve information of the sample being tested, where the sample being tested at least includes the film being tested;

模型化单元,用于根据所述被测样品的特性建立各向同性的物理模型,所述物理模型包括至少包括薄膜模型;将所述薄膜模型所含有的至少一个变量参数转换为至少一组梯度化变量参数;A modeling unit, configured to establish an isotropic physical model according to the characteristics of the measured sample, the physical model including at least a film model; convert at least one variable parameter contained in the film model into at least a set of gradients variable parameters;

曲线拟合单元,用于以所述被测样品的椭偏光谱曲线信息为曲线拟合目标,利用所述薄膜模型对至少一组梯度化变量参数进行曲线拟合,获得被测样品的光电参数在被测样品纵向方向上的变化曲线信息;A curve fitting unit, configured to use the ellipsometric spectrum curve information of the tested sample as a curve fitting target, use the film model to perform curve fitting on at least one set of gradient variable parameters, and obtain the photoelectric parameters of the tested sample. Change curve information in the longitudinal direction of the tested sample;

分析单元,用于根据所述被测样品的光电参数在被测样品纵向方向上的变化曲线信息评价被测样品的纵向不均匀性。An analysis unit is used to evaluate the longitudinal non-uniformity of the tested sample based on the change curve information of the photoelectric parameters of the tested sample in the longitudinal direction of the tested sample.

在一些实施例中,所述进行曲线拟合的收敛条件为均方根误差值小于80;In some embodiments, the convergence condition for curve fitting is that the root mean square error value is less than 80;

和/或,and / or,

所述被测样品的光电参数包括满足克莱默-克朗尼格关系的光学常数和/或满足克莱默-克朗尼格关系的介电常数;The photoelectric parameters of the measured sample include optical constants that satisfy the Kramer-Kronig relationship and/or dielectric constants that satisfy the Kramer-Kronig relationship;

和/或,and / or,

所述物理模型还包括基体模型和表面模型,所述薄膜模型位于所述基体模型和所述表面模型之间,所述基体模型为柯西模型,所述薄膜模型为洛伦兹模型或高斯模型,所述表面模型为有效介质模型;The physical model also includes a matrix model and a surface model. The film model is located between the matrix model and the surface model. The matrix model is a Cauchy model, and the film model is a Lorentz model or a Gaussian model. , the surface model is an effective medium model;

和/或,and / or,

所述将所述薄膜模型所含有的至少一个变量参数转换为至少一组梯度化变量参数包括:Converting at least one variable parameter contained in the film model into at least one set of gradient variable parameters includes:

按照对拟合结果影响权重由高到低的顺序,选择薄膜模型中的一个或两个变量参数进行梯度化转换;Select one or two variable parameters in the film model for gradient conversion in order of their impact on the fitting results from high to low;

和/或,and / or,

所述梯度化变量参数包括线性梯度变化的变量参数或非线性梯度变化的变量参数。The gradient variable parameters include variable parameters with linear gradient changes or variable parameters with nonlinear gradient changes.

在一些实施例中,所述进行曲线拟合的收敛条件为均方根误差值小于20。In some embodiments, the convergence condition for curve fitting is that the root mean square error value is less than 20.

第三方面,本发明还提供了一种薄膜纵向不均匀性检测方法,包括:In a third aspect, the present invention also provides a method for detecting longitudinal unevenness of a film, including:

测量被测样品的椭偏光谱曲线;Measure the ellipsometric spectral curve of the sample being tested;

将被测样品的椭偏光谱曲线信息发送给如上述方案中所述的薄膜纵向不均匀性检测装置;所述被测样品的椭偏光谱曲线信息表征所述被测样品的椭偏光谱曲线;The ellipsometric spectral curve information of the tested sample is sent to the film longitudinal non-uniformity detection device as described in the above solution; the ellipsometric spectral curve information of the tested sample represents the ellipsometric spectral curve of the tested sample;

利用所述薄膜纵向不均匀性检测装置确定被测样品的纵向不均匀性。The longitudinal non-uniformity of the measured sample is determined using the film longitudinal non-uniformity detection device.

在一些实施例中,所述测量被测样品的椭偏光谱曲线包括:In some embodiments, measuring the ellipsometric spectral curve of the tested sample includes:

入射线偏振光到被测样品表面,检测到所述被测样品的椭圆偏振p光与s光的振幅比光谱曲线和相位差光谱曲线。Incident polarized light onto the surface of the sample to be measured, and the amplitude ratio spectrum curve and phase difference spectrum curve of the elliptically polarized p-light and s-light of the sample to be measured are detected.

在一些实施例中,所述测量被测样品的椭偏光谱曲线包括:In some embodiments, measuring the ellipsometric spectral curve of the tested sample includes:

设定线偏振光的入射角度,使得所述线偏振光的入射角度包括至少一个第一入射角度和至少一个第二入射角度,每个所述第一入射角度大于被测样品材料的布儒斯特角,每个所述第二入射角度小于被测样品材料的布儒斯特角;The incident angle of the linearly polarized light is set so that the incident angle of the linearly polarized light includes at least one first incident angle and at least one second incident angle, and each of the first incident angles is greater than the Brucella of the tested sample material. special angle, each of the second incident angles is smaller than the Brewster angle of the sample material being tested;

分别在至少一个第一入射角度和至少一个第二入射角度下,向被测样品入射线偏振光,检测被测样品的椭圆偏振p光与s光的振幅比和被测样品的椭圆偏振p光与s光的相位差;Under at least one first incident angle and at least one second incident angle, linearly polarized light is incident on the sample to be measured, and the amplitude ratio of the elliptically polarized p-light and s-light of the sample to be measured and the elliptically polarized p-light of the sample to be measured are detected Phase difference with s light;

根据所述被测样品的椭圆偏振p光与s光的振幅比和线偏振光的波长范围,获得被测样品的椭偏振幅比光谱曲线;According to the amplitude ratio of the elliptically polarized p-light and s-light of the tested sample and the wavelength range of the linearly polarized light, the elliptical polarization amplitude ratio spectral curve of the tested sample is obtained;

根据所述被测样品的椭圆偏振p光与s光的相位差和线偏振光的波长范围,获得被测样品的椭偏相位差光谱曲线。According to the phase difference between the elliptically polarized p-light and the s-light of the tested sample and the wavelength range of the linearly polarized light, the elliptical phase difference spectrum curve of the tested sample is obtained.

在一些实施例中,所述线偏振光的波长范围为300nm-2400nm。In some embodiments, the wavelength range of the linearly polarized light is 300nm-2400nm.

第四方面,本发明实施例也提供了一种检测系统,包括:In a fourth aspect, embodiments of the present invention also provide a detection system, including:

椭偏光谱仪;spectroscopic ellipsometry;

如上述方案中所述的薄膜纵向不均匀性检测装置,所述薄膜纵向不均匀性检测装置所包括的接收器与所述椭偏光谱仪连接。As for the film longitudinal non-uniformity detection device described in the above solution, the receiver included in the film longitudinal non-uniformity detection device is connected to the ellipsometer.

第五方面,本发明提供了一种终端,包括:In a fifth aspect, the present invention provides a terminal, including:

存储器,用于储存一个或多个计算机软件指令,其包含用于执行上述方案中所述的薄膜纵向不均匀性检测方法所涉及的程序;A memory used to store one or more computer software instructions, which include programs involved in executing the film longitudinal non-uniformity detection method described in the above solution;

处理器,用于执行一个或多个计算机软件指令,以实现上述方案中所述的薄膜纵向不均匀性检测方法所涉及的程序。A processor, configured to execute one or more computer software instructions to implement the programs involved in the film longitudinal non-uniformity detection method described in the above solution.

本发明提供的一种薄膜纵向不均匀性检测方法,根据被测样品的特性建立各向同性的物理模型,使得该物理模型至少包括薄膜模型;然后将薄膜模型所含有的至少一个变量参数转换为至少一组梯度化变量参数,接着以被测样品的椭偏光谱曲线信息为曲线拟合目标,利用薄膜模型对至少一组梯度化变量参数进行曲线拟合,获得被测样品的光电参数在被测样品纵向方向上的变化曲线信息;此时,被测样品的光电参数在被测薄膜纵向方向上的变化曲线信息与被测样品的椭偏光谱曲线信息相适应,说明所建立的物理模型与实际被测样品相匹配,且被测薄膜的光电参数在被测薄膜纵向方向上的变化曲线信息可以反映被测薄膜的纵向不均匀性,因此,当所建立的物理模型与实际被测样品相匹配时,可以根据被测样品的光电参数在被测样品纵向方向上的变化曲线信息确定被测样品的纵向不均匀性;由此可见,本发明提供的薄膜纵向不均匀性检测方法,可针对任何薄膜样品进行无损检测,以确定其纵向不均匀性,不受薄膜组成的限制;同时,还可以在确定被测样品的纵向不均匀性时,通过调节工艺参数和/或薄膜组成,判断工艺参数和/或薄膜组成对拟合过程中所使用的梯度化变量参数的影响,如果发现工艺参数和/或薄膜组成对拟合过程中所使用的梯度化变量参数有影响,则说明是工艺参数和/或薄膜组成导致了薄膜的纵向不均匀性。也就是说,本发明提供的薄膜纵向不均匀性检测方法,还可以利用拟合所使用的梯度化变量参数分析产生薄膜纵向不均匀性的原因,用以指导成膜工艺或者薄膜组成的选择。The invention provides a method for detecting longitudinal non-uniformity of a film. It establishes an isotropic physical model according to the characteristics of the sample to be measured, so that the physical model at least includes a film model; and then converts at least one variable parameter contained in the film model into At least one set of gradient variable parameters is used, and then the ellipsometry spectrum curve information of the tested sample is used as the curve fitting target, and the thin film model is used to perform curve fitting on at least one set of gradient variable parameters to obtain the photoelectric parameters of the tested sample in the measured sample. The change curve information in the longitudinal direction of the measured sample; at this time, the change curve information of the photoelectric parameters of the measured sample in the longitudinal direction of the measured film is consistent with the ellipsometric spectral curve information of the measured sample, indicating that the established physical model is consistent with The actual measured sample matches, and the change curve information of the photoelectric parameters of the measured film in the longitudinal direction of the measured film can reflect the longitudinal non-uniformity of the measured film. Therefore, when the established physical model matches the actual measured sample At this time, the longitudinal non-uniformity of the tested sample can be determined based on the change curve information of the photoelectric parameters of the tested sample in the longitudinal direction of the tested sample; it can be seen that the longitudinal non-uniformity detection method of the film provided by the present invention can be used for any The film sample is subjected to non-destructive testing to determine its longitudinal unevenness, which is not limited by the film composition; at the same time, the process parameters can also be judged by adjusting the process parameters and/or film composition when determining the longitudinal unevenness of the tested sample. and/or the influence of film composition on the gradient variable parameters used in the fitting process. If it is found that the process parameters and/or the film composition have an impact on the gradient variable parameters used in the fitting process, it means that the process parameters and /or the film composition results in longitudinal non-uniformity of the film. That is to say, the method for detecting longitudinal non-uniformity of a film provided by the present invention can also use the gradient variable parameters used in fitting to analyze the causes of longitudinal non-uniformity of the film to guide the film formation process or the selection of film composition.

附图说明Description of the drawings

为了更清楚地说明本发明实施例或现有技术中的技术方案,下面将对实施例或现有技术描述中所需要使用的附图作简单地介绍,显而易见地,下面描述中的附图仅仅是本发明的一些实施例,对于本领域普通技术人员来讲,在不付出创造性劳动的前提下,还可以根据这些附图获得其他的附图。In order to explain the embodiments of the present invention or the technical solutions in the prior art more clearly, the drawings needed to be used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings in the following description are only These are some embodiments of the present invention. For those of ordinary skill in the art, other drawings can be obtained based on these drawings without exerting creative efforts.

图1为本发明实施例提供的一种检测系统的结构框图;Figure 1 is a structural block diagram of a detection system provided by an embodiment of the present invention;

图2为本发明实施例一提供的一种薄膜纵向不均匀性检测方法的流程图;Figure 2 is a flow chart of a method for detecting longitudinal non-uniformity of a film provided in Embodiment 1 of the present invention;

图3为本发明实施例一提供的另一种薄膜纵向不均匀性检测方法的流程图;Figure 3 is a flow chart of another method for detecting longitudinal non-uniformity of a film provided in Embodiment 1 of the present invention;

图4为本发明实施例一的被测样品的结构示意图;Figure 4 is a schematic structural diagram of the tested sample according to Embodiment 1 of the present invention;

图5为本发明实施例提供的薄膜纵向不均匀性检测终端的框架图;Figure 5 is a frame diagram of a film longitudinal non-uniformity detection terminal provided by an embodiment of the present invention;

图6为本发明实施例中测量被测样品的椭偏光谱曲线的具体流程图;Figure 6 is a specific flow chart for measuring the ellipsometric spectral curve of the tested sample in the embodiment of the present invention;

图7为实施例二中ITO薄膜的椭偏Δ光谱曲线图;Figure 7 is the ellipsometry Δ spectrum curve of the ITO film in Example 2;

图8为实施例二中ITO薄膜的椭偏Ψ光谱曲线图;Figure 8 is the ellipsometry Ψ spectrum curve of the ITO film in Example 2;

图9为实施例二中线性梯度变化的中心峰位分布示意图;Figure 9 is a schematic diagram of the center peak position distribution of linear gradient changes in Example 2;

图10为实施例二中ITO薄膜的折射率和消光系数在被测样品纵向方向上的变化曲线图;Figure 10 is a graph showing the changes in the refractive index and extinction coefficient of the ITO film in the longitudinal direction of the tested sample in Example 2;

图11为实施例二中ITO薄膜顶部与底部的介电常数随光子能量的变化曲线图;Figure 11 is a graph showing changes in dielectric constant at the top and bottom of the ITO film in Example 2 as a function of photon energy;

图12为实施例三中AZO薄膜的椭偏Δ光谱曲线图;Figure 12 is the ellipsometry Δ spectrum curve of the AZO film in Example 3;

图13为实施例三中AZO薄膜的椭偏Ψ光谱曲线图;Figure 13 is the ellipsometry Ψ spectrum curve of the AZO film in Example 3;

图14为实施例三中非线性梯度变化的中心峰位分布示意图;Figure 14 is a schematic diagram of the center peak position distribution of nonlinear gradient changes in Example 3;

图15为实施例三中AZO薄膜的折射率和消光系数在被测样品纵向方向上的变化曲线图;Figure 15 is a graph showing the changes in the refractive index and extinction coefficient of the AZO film in Example 3 in the longitudinal direction of the tested sample;

图16为实施例三中AZO薄膜顶部与底部的介电常数随光子能量的变化曲线图。Figure 16 is a graph showing changes in dielectric constant at the top and bottom of the AZO film in Example 3 as a function of photon energy.

具体实施方式Detailed ways

下面将结合本发明实施例中的附图,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only some of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts fall within the scope of protection of the present invention.

实施例一Embodiment 1

透明导电薄膜是一种重要的光电材料,既有高导电性,又在可见光范围内有很高的透光性,且在远红外范围有很高的反射性,在太阳能电池、液晶显示器、气体传感器、飞机和汽车用导热玻璃(防雾和防结冰)等光电领域得到了广泛应用。Transparent conductive film is an important optoelectronic material. It has high conductivity, high transmittance in the visible light range, and high reflectivity in the far infrared range. It is widely used in solar cells, liquid crystal displays, gas It has been widely used in optoelectronic fields such as sensors, thermally conductive glass for aircraft and automobiles (anti-fog and anti-icing).

上述透明导电薄膜中的氧含量对光电性能有重要影响,若氧含量低,则氧空位使得透明导电薄膜呈现类金属的颜色而失去透明性;若氧含量高,则透明导电薄膜中的氧空位数量减少,或者使外来施主杂质(施主杂质是指为了控制半导体的性质可以人为地掺入某种化学元素的原子,掺入杂质元素与半导体材料价电子的不同而产生的多余价电子会挣脱束缚,成为导电的自由电子,杂质电离后形成正电中心)失去掺杂的效果,导致透明导电薄膜的化学成分接近于100%,甚至使得透明导电薄膜失去导电性而变为绝缘体;当氧含量适当时,透明导电薄膜中氧空位数量适当,替位杂质(以半导体材料硅为例,杂质原子进入半导体硅后,只可能以两种方式存在:一种方式是杂质原子位于晶格原子间的间隙位置,常称为间隙式杂质;另一种方式是杂质原子去掉晶格原子而位于晶格格点处,常称为替位式杂质)发挥了施主的作用,使得透明导电薄膜的光电性能俱佳。The oxygen content in the above-mentioned transparent conductive film has an important impact on the photoelectric performance. If the oxygen content is low, the oxygen vacancies will cause the transparent conductive film to show a metal-like color and lose transparency; if the oxygen content is high, the oxygen vacancies in the transparent conductive film will The quantity is reduced, or foreign donor impurities (donor impurities refer to atoms that can be artificially doped with certain chemical elements in order to control the properties of semiconductors. The excess valence electrons generated by the difference between the doped impurity elements and the valence electrons of the semiconductor material will break free. , become conductive free electrons, and form positive centers after ionization of impurities) lose the doping effect, causing the chemical composition of the transparent conductive film to be close to 100%, and even cause the transparent conductive film to lose conductivity and become an insulator; when the oxygen content is appropriate When the number of oxygen vacancies in the transparent conductive film is appropriate, replacement impurities (taking the semiconductor material silicon as an example), after impurity atoms enter the semiconductor silicon, can only exist in two ways: one way is that the impurity atoms are located in the gaps between the crystal lattice atoms position, often called interstitial impurities; another way is that the impurity atoms remove the lattice atoms and are located at the lattice points, often called substitutional impurities) play the role of donors, making the transparent conductive film have excellent photoelectric properties .

由于表面弛豫与表面能的作用使得薄膜表面与内部存在成分或结构的过渡,以实现能量与物质的平衡,使得采用镀膜工艺所形成的透明导电薄膜不可避免的存在氧含量沿透明导电薄膜的纵向(透明导电薄膜的厚度方向)分布不均,因此需要检测薄膜材料的纵向不均匀。针对于此,现有技术中,通常需要通过给被测样品入射能量并检测出射粒子或发射的荧光光谱,如采用X射线辐照或轰击刻蚀,最终获得被测样品的纵向不均匀性,但是也对被测样品造成了破坏,均为有损检测。虽然也有人提供了一种无损检测薄膜纵向不均匀的方法,但是其所检测的薄膜属于双组分体系,需要使用有效介质模型建立薄膜模型,其不具有普适性。Due to the effects of surface relaxation and surface energy, there is a transition of components or structures between the surface and the interior of the film to achieve a balance between energy and matter. Therefore, the transparent conductive film formed by the coating process inevitably contains oxygen content along the surface of the transparent conductive film. The distribution in the longitudinal direction (the thickness direction of the transparent conductive film) is uneven, so it is necessary to detect the longitudinal unevenness of the film material. To this end, in the existing technology, it is usually necessary to inject energy into the sample to be measured and detect the emitted particles or the emitted fluorescence spectrum, such as using X-ray irradiation or bombardment etching, to finally obtain the longitudinal non-uniformity of the sample to be measured. However, it also caused damage to the samples being tested, all of which are destructive tests. Although some people have provided a method for non-destructively detecting longitudinal non-uniformity of films, the film they detect belongs to a two-component system, and an effective medium model needs to be used to establish a film model, which is not universal.

本发明实施例提供了一种检测系统,如图1所示,该检测系统包括椭偏光谱仪100和薄膜纵向不均匀性检测装置200,椭偏光谱仪100与薄膜纵向不均匀性检测装置200连接。下面结合图1和图2对本发明实施例提供的检测系统的检测方法进行说明,以下说明仅用于解释,不作为限定。An embodiment of the present invention provides a detection system, as shown in Figure 1. The detection system includes an ellipsometer 100 and a film longitudinal non-uniformity detection device 200. The ellipsometer 100 is connected to the film longitudinal non-uniformity detection device 200. The detection method of the detection system provided by the embodiment of the present invention will be described below with reference to Figures 1 and 2. The following description is for explanation only and is not intended to be limiting.

第一步:椭偏光谱仪100测量被测样品的椭偏光谱曲线;该椭偏光谱仪又称为椭圆偏振光谱仪,可检测被测样品的椭偏光谱曲线,椭偏光谱曲线可以为椭偏相位差光谱曲线(又称椭偏Δ光谱曲线)和/或椭偏振幅比Ψ光谱曲线(又称椭偏Ψ光谱曲线)。The first step: the ellipsometry spectrometer 100 measures the ellipsometry spectrum curve of the sample being tested; the spectrometer ellipsometry, also known as the ellipsometry spectrometer, can detect the ellipsometry spectrum curve of the sample being tested, and the ellipsometry spectrum curve can be the ellipsometry phase difference. Spectral curve (also known as ellipsometry Δ spectrum curve) and/or ellipsometry amplitude ratio Ψ spectrum curve (also known as ellipsometry Ψ spectrum curve).

第二步:将被测样品的椭偏光谱曲线信息发送给薄膜纵向不均匀性检测装置200。Step 2: Send the ellipsometric spectral curve information of the tested sample to the film longitudinal non-uniformity detection device 200.

第三步:利用薄膜纵向不均匀性检测装置200确定被测样品的纵向不均匀性。Step 3: Use the film longitudinal unevenness detection device 200 to determine the longitudinal unevenness of the sample being tested.

在第一种实现方式中,请参阅图3,本发明实施例提供了一种薄膜纵向不均匀性检测方法,纵向不均匀性指由于在薄膜纵向方向上成分或结构不均匀导致的光学常数或介电常数不均匀。该薄膜纵向不均匀性检测方法包括:In a first implementation, please refer to Figure 3. An embodiment of the present invention provides a method for detecting longitudinal non-uniformity of a film. Longitudinal non-uniformity refers to optical constants or optical constants caused by uneven composition or structure in the longitudinal direction of the film. The dielectric constant is not uniform. The film longitudinal non-uniformity detection method includes:

步骤S110:获取被测样品的椭偏光谱曲线信息,该椭偏光谱曲线信息表征的椭偏光谱曲线(椭圆偏振光谱)为上述椭偏光谱曲线。被测样品至少包括被测薄膜402,被测薄膜的层数可以为一层,也可以为多层;例如,被测薄膜为透明导电氧化物膜,其所使用的材料可以为In2O3、SnO2、ZnO、In2O3:Sn(ITO)、In2O3:Mo(IMO)、SnO2:Sb(ATO)、SnO2:F(FTO)、ZnO:Al(AZO)等中的一种或多种,当然不仅限于此。Step S110: Obtain the ellipsometry spectrum curve information of the sample under test, and the ellipsometry spectrum curve (ellipsometry spectrum) represented by the ellipsometry spectrum curve information is the above-mentioned ellipsometry spectrum curve. The sample to be tested at least includes the thin film to be tested 402. The number of layers of the thin film to be tested may be one layer or multiple layers; for example, the thin film to be tested may be a transparent conductive oxide film, and the material used may be In2 O3 , SnO2 , ZnO, In2 O3 :Sn(ITO), In2 O3 :Mo(IMO), SnO2 :Sb(ATO), SnO2 :F(FTO), ZnO:Al(AZO), etc. One or more, of course not limited to these.

如图4所示,在符合实际情况的基础上,考虑到被测样品/空气界面并不是理想的光滑平面,被测样品还包括粗糙层401和基体层403,被测薄膜402位于基体层403与粗糙层401之间,被测薄膜402采用成膜设备在基体表面制作而成。成膜工艺选用电子束蒸发法、磁控溅射法、化学气相沉积法中的任意一种,当然不仅限于此。As shown in Figure 4, based on the actual situation, considering that the tested sample/air interface is not an ideal smooth plane, the tested sample also includes a rough layer 401 and a base layer 403, and the tested thin film 402 is located in the base layer 403 Between the film and the rough layer 401, the thin film 402 to be measured is made on the surface of the substrate using film forming equipment. The film formation process may be any one of electron beam evaporation, magnetron sputtering, and chemical vapor deposition, but of course it is not limited to these.

上述基体层403为各种种类的透明玻璃,透明塑料等,上述粗糙层401是指被测薄膜接触大气的表面,其不质密,较疏松,其采用有效介质理论设计而成,有效介质理论是指纳米金属颗粒弥散于陶瓷(电介质)基体所构成的复合纳米金属陶瓷薄膜微结构的模型理论,所设计的粗糙层包括50%孔隙率的表面疏松层,即该表面疏松层包括体积百分比为50%的孔隙和体积百分比为50%的被测薄膜材料,其光学常数为被测薄膜的光学常数的二分之一。The above-mentioned base layer 403 is made of various types of transparent glass, transparent plastic, etc. The above-mentioned rough layer 401 refers to the surface of the film under test that contacts the atmosphere. It is not dense and relatively loose. It is designed using the effective medium theory. The effective medium theory It refers to the model theory of the microstructure of a composite nano-cermet film composed of nano-metal particles dispersed in a ceramic (dielectric) matrix. The designed rough layer includes a surface loose layer with a porosity of 50%, that is, the surface loose layer includes a volume percentage of The optical constant of a film material under test with 50% pores and 50% volume percentage is one-half that of the film under test.

步骤S120:根据被测样品的特性建立各向同性的物理模型,物理模型至少包括薄膜模型。当被测样品还包括基体层和粗糙层时,建模时,设置该物理模型还包括基体模型和表面模型。Step S120: Establish an isotropic physical model based on the characteristics of the sample being tested, and the physical model at least includes a thin film model. When the sample under test also includes a matrix layer and a rough layer, when modeling, set the physical model to also include a matrix model and a surface model.

具体而言,根据基体层的特性建立基体模型,根据被测薄膜的特性建立薄膜模型,根据粗糙层的特性建立表面模型。Specifically, the matrix model is established based on the characteristics of the matrix layer, the film model is established based on the characteristics of the measured film, and the surface model is established based on the characteristics of the rough layer.

上述各向同性的物理模型所包括的薄膜模型、基体模型和表面模型均被为认为是各向同性的模型,其对应的实体膜层所含有的物质也具有各向同性。其中,各向同性(又称均质性)是指物体的物理、化学等方面的性质不会因方向的不同而有所变化的特性。The film model, matrix model and surface model included in the above-mentioned isotropic physical model are all considered to be isotropic models, and the substances contained in the corresponding solid film layers are also isotropic. Among them, isotropy (also called homogeneity) refers to the characteristic that the physical, chemical and other properties of an object do not change due to different directions.

上述被测样品的特性既可以包括被测样品的物质组成,也可以包括被测样品的光电参数。由于建立物理模型的特性为被测样品的物质组成,椭偏光谱仪测量被测样品的椭偏光谱曲线,所以,被测样品的物理模型选择对于后期拟合非常重要,此处的物理模型包括柯西模型(即Cauchy Model)、洛伦兹模型(即Lorentz Model)、高斯模型(即GaussianModel)、杜鲁德模型(即Drude Model),但不仅限于此。上述被测样品所包括的各个膜层的物理模型选择根据被测样品的特性选择即可;其中,柯西模型适用于透明或弱吸收材料,洛伦兹模型和高斯模型均适用于半导体材料,而杜鲁德模型适用于金属材料。例如:当上述基体层203为透明玻璃,则选择柯西模型作为基体层的物理模型;当上述被测薄膜402为透明导电薄膜时,则选择洛伦兹模型和高斯模型作为透明导电薄膜的物理模型。当上述表面模型对应的膜层具有一定的粗糙度,则采用有效介质方法构建表面模型,该表面模型的类型为有效介质模型。The above-mentioned characteristics of the sample to be measured may include the material composition of the sample to be measured, or the photoelectric parameters of the sample to be measured. Since the characteristics of establishing a physical model are the material composition of the measured sample, and the ellipsometry spectrometer measures the ellipsometric spectral curve of the measured sample, the selection of the physical model of the measured sample is very important for later fitting. The physical model here includes Ke Cauchy Model, Lorentz Model, Gaussian Model, Drude Model, but not limited to these. The physical model of each film layer included in the above-mentioned tested sample can be selected according to the characteristics of the tested sample; among them, the Cauchy model is suitable for transparent or weakly absorbing materials, and the Lorentz model and Gaussian model are both suitable for semiconductor materials. The Durude model is suitable for metallic materials. For example: when the base layer 203 is transparent glass, the Cauchy model is selected as the physical model of the base layer; when the measured film 402 is a transparent conductive film, the Lorentz model and the Gaussian model are selected as the physical model of the transparent conductive film. Model. When the film layer corresponding to the above surface model has a certain roughness, the effective medium method is used to construct the surface model, and the type of the surface model is an effective medium model.

步骤S130:将薄膜模型所含有的至少一个变量参数转换为至少一组梯度化变量参数。即一个变量参数可转换为一组梯度化变量参数。Step S130: Convert at least one variable parameter contained in the film model into at least one set of gradient variable parameters. That is, a variable parameter can be converted into a set of gradient variable parameters.

例如:上述被测薄膜容易出现纵向不均匀性,因此,此处选择薄膜模型中的至少一个变量参数,将至少一个变量参数梯度化变量参数。考虑到薄膜模型中有若干个变量参数,为了降低拟合难度,选取至少一个变量参数并将其转换为梯度化变量参数。优选地,通过表达该变量参数沿膜层深度变化的梯度函数的方式将变量参数转换为梯度化变量参数。For example: the above-mentioned measured film is prone to longitudinal non-uniformity. Therefore, at least one variable parameter in the film model is selected here, and at least one variable parameter is gradient variable parameter. Considering that there are several variable parameters in the film model, in order to reduce the difficulty of fitting, at least one variable parameter is selected and converted into a gradient variable parameter. Preferably, the variable parameters are converted into gradient variable parameters by expressing a gradient function in which the variable parameters change along the depth of the film layer.

可以理解的是,上述薄膜模型所含有的变量参数在数值上沿膜层深度方向(纵向)梯度变化多是由于膜层生产工艺导致的纵向不均匀,如氧气量的供给,纵向自由能的变化,电负性的变化等各种原因的驱动力导致。基于此,上述将薄膜模型所含有的至少一个变量参数转换为至少一组梯度化变量参数包括:It can be understood that the numerical gradient changes in the variable parameters contained in the above-mentioned thin film model along the film layer depth direction (longitudinal direction) are mostly due to the longitudinal unevenness caused by the film layer production process, such as the supply of oxygen amount and changes in longitudinal free energy. , changes in electronegativity and other driving forces caused by various reasons. Based on this, the above-mentioned conversion of at least one variable parameter contained in the film model into at least one set of gradient variable parameters includes:

按照对拟合结果影响权重由高到低的顺序,选择薄膜模型中的一个或两个变量参数进行梯度化转换。According to the order of influence weight on the fitting results from high to low, select one or two variable parameters in the film model for gradient transformation.

例如:当选择薄膜模型中的一个变量参数进行梯度化转换,从薄膜模型中选取对拟合结果影响权重最大的一个变量参数进行梯度化转换。For example: when selecting a variable parameter in the membrane model for gradient transformation, select a variable parameter from the membrane model that has the greatest influence on the fitting result for gradient transformation.

又例如:当选择薄膜模型中的两个变量参数进行梯度化转换,按照对拟合结果影响权重由高到低的顺序,从薄膜模型中选取排序在前两位的变量参数进行梯度化转换。Another example: when selecting two variable parameters in the film model for gradient transformation, select the top two variable parameters from the film model in order of their impact on the fitting results from high to low for gradient transformation.

上述梯度化变量参数包括线性梯度变化的变量参数或非线性梯度变化的变量参数。若选用两个变量参数进行梯度化变换,可以根据需要选择其中一个变量参数做线性梯度化变换,另一个变量参数做非线性梯度化变化。将变量参数转换成线性梯度变化的变量参数还是非线性梯度变化的变量参数采用试错确定。试错优先级按照先线性梯度变化的变量参数拟合曲线,拟合不出较好地结果,再转换为非线性梯度变化的变量参数拟合曲线;如果拟合不出来,再选取另一个变量参数重新进行试错。如果仍然无法拟合成功,则需要考虑所建立的物理模型是否恰当。例如:本来为金属模型却建立为适合透明材料的柯西模型;或者,输入的初始值是否与实际情况偏差太多,例如:膜厚为350nm的薄膜的膜厚初始值输入为1000nm,所拟合的结果就会与实际情况产生较大的偏差。The above-mentioned gradient variable parameters include variable parameters with linear gradient changes or variable parameters with nonlinear gradient changes. If two variable parameters are used for gradient transformation, one variable parameter can be selected for linear gradient transformation and the other variable parameter can be selected for nonlinear gradient transformation according to needs. Whether to convert the variable parameters into linear gradient changing variable parameters or nonlinear gradient changing variable parameters is determined by trial and error. The priority of trial and error is to first fit the curve with variable parameters with linear gradient changes. If the fitting cannot produce a better result, then convert it to a curve fitting curve with variable parameters with non-linear gradient changes; if the fitting cannot be achieved, select another variable. Trial and error the parameters again. If the fitting still cannot be successful, you need to consider whether the physical model established is appropriate. For example: It was originally a metal model but it was established as a Cauchy model suitable for transparent materials; or, whether the input initial value deviates too much from the actual situation. For example: the initial value of the film thickness of a film with a film thickness of 350nm is entered as 1000nm. The combined results will deviate greatly from the actual situation.

步骤S140:以被测样品的椭偏光谱曲线信息为曲线拟合目标,利用薄膜模型对至少一组梯度化变量参数进行曲线拟合,若拟合成功,获得被测样品的光电参数在被测样品纵向方向上的变化曲线信息。此处的光电参数包括折射率n、消光系数k、介电常数中的一种或多种,具体根据实际需要选择不同种类的光电参数。Step S140: Using the ellipsometric spectral curve information of the measured sample as the curve fitting target, use the thin film model to perform curve fitting on at least one set of gradient variable parameters. If the fitting is successful, obtain the photoelectric parameters of the measured sample. Change curve information in the longitudinal direction of the sample. The photoelectric parameters here include one or more of refractive index n, extinction coefficient k, and dielectric constant. Different types of photoelectric parameters can be selected according to actual needs.

例如:选取一到两个变量参数,同时将其转换为梯度化变量参数,获得一组到两组梯度化变量参数,然后将这一组到两组梯度化变量参数代入至薄膜模型中通过反演计算进行拟合。若拟合失败,则重新选取其他变量参数进行梯度化处理,然后进行拟合。若仍然拟合失败,则说明建立的各向同性物理模型有可能不合适,需要返回步骤S120改变所建立的各向同性物理模型的种类,然后按照执行步骤S130和步骤S140,直到拟合成功为止。For example: select one or two variable parameters, convert them into gradient variable parameters at the same time, obtain one to two sets of gradient variable parameters, and then substitute this set to two sets of gradient variable parameters into the film model through inversion Perform calculations to fit. If the fitting fails, reselect other variable parameters for gradient processing, and then perform fitting. If the fitting still fails, it means that the established isotropic physical model may not be appropriate. You need to return to step S120 to change the type of the established isotropic physical model, and then perform steps S130 and S140 until the fitting is successful. .

S150:根据被测样品的光电参数在被测样品纵向方向上的变化曲线信息确定被测样品的纵向不均匀性。由于光电参数在一定程度上反映了膜层的均匀性,因此,可通过被测样品的光电参数在被测样品纵向方向上的变化曲线确定被测样品的纵向不均匀性,进而确认被测样品的性质,从而将其应用到合适的领域中。S150: Determine the longitudinal non-uniformity of the sample under test based on the change curve information of the photoelectric parameters of the sample under test in the longitudinal direction of the sample under test. Since the photoelectric parameters reflect the uniformity of the film layer to a certain extent, the longitudinal non-uniformity of the tested sample can be determined through the change curve of the photoelectric parameters of the tested sample in the longitudinal direction of the tested sample, and then the tested sample can be confirmed properties so that it can be applied to appropriate fields.

由上可以看出:根据被测样品的特性建立各向同性的物理模型,使得该物理模型至少包括薄膜模型;然后将薄膜模型所含有的至少一个变量参数转换为至少一组梯度化变量参数,接着以被测样品的椭偏光谱曲线信息为曲线拟合目标,利用薄膜模型对至少一组梯度化变量参数进行曲线拟合,获得被测样品的光电参数在被测样品纵向方向上的变化曲线信息;此时,被测样品的光电参数在被测薄膜纵向方向上的变化曲线信息与被测样品的椭偏光谱曲线信息相适应,说明所建立的物理模型与实际被测样品相匹配,且被测薄膜的光电参数在被测薄膜纵向方向上的变化曲线信息可以反映被测薄膜的纵向不均匀性,因此,当所建立的物理模型与实际被测样品相匹配时,可以根据被测样品的光电参数在被测样品纵向方向上的变化曲线信息确定被测样品的纵向不均匀性;由此可见,本发明实施例提供的薄膜纵向不均匀性检测方法,可针对任何薄膜样品进行无损检测,以确定其纵向不均匀性,不受薄膜组成的限制;同时,还可以在确定被测样品的纵向不均匀性时,通过调节工艺参数和/或薄膜组成,判断工艺参数和/或薄膜组成对拟合过程中所使用的梯度化变量参数的影响,如果发现工艺参数和/或薄膜组成对拟合过程中所使用的梯度化变量参数有影响,则说明是工艺参数和/或薄膜组成导致了薄膜的纵向不均匀性。也就是说,本发明提供的薄膜纵向不均匀性检测方法,还可以利用拟合所使用的梯度化变量参数分析产生薄膜纵向不均匀性的原因,用以指导成膜工艺或者薄膜组成的选择。因此,相较于现有技术,本发明实施例提供的一种薄膜纵向不均匀性检测方法不需要检测入射粒子或射线束与被测样品碰撞产生出射粒子或起辉发射荧光,为非接触式无损检测,不损伤被测样品的物质组成,也不影响被测样品的使用性能,非常适用于生产线上对产品或实验室对样品的无损检测。It can be seen from the above that: an isotropic physical model is established based on the characteristics of the sample being measured, so that the physical model at least includes a film model; then at least one variable parameter contained in the film model is converted into at least one set of gradient variable parameters, Then, the ellipsometric spectral curve information of the tested sample is used as the curve fitting target, and the thin film model is used to perform curve fitting on at least one set of gradient variable parameters to obtain the change curve of the photoelectric parameters of the tested sample in the longitudinal direction of the tested sample. information; at this time, the change curve information of the photoelectric parameters of the measured sample in the longitudinal direction of the measured film is consistent with the ellipsometric spectral curve information of the measured sample, indicating that the established physical model matches the actual measured sample, and The change curve information of the photoelectric parameters of the measured film in the longitudinal direction of the measured film can reflect the longitudinal non-uniformity of the measured film. Therefore, when the established physical model matches the actual measured sample, it can be based on the measured sample. The change curve information of the photoelectric parameters in the longitudinal direction of the tested sample determines the longitudinal non-uniformity of the tested sample; it can be seen that the longitudinal non-uniformity detection method of the film provided by the embodiment of the present invention can perform non-destructive testing on any film sample. In order to determine the longitudinal unevenness, it is not limited by the film composition; at the same time, when determining the longitudinal unevenness of the tested sample, the process parameters and/or film composition can be adjusted to determine the pairing of the process parameters and/or film composition. The influence of the gradient variable parameters used in the fitting process. If it is found that the process parameters and/or film composition have an impact on the gradient variable parameters used in the fitting process, it means that the process parameters and/or film composition cause the problem. Longitudinal unevenness of the film. That is to say, the method for detecting longitudinal non-uniformity of a film provided by the present invention can also use the gradient variable parameters used in fitting to analyze the causes of longitudinal non-uniformity of the film to guide the film formation process or the selection of film composition. Therefore, compared with the existing technology, the method for detecting longitudinal non-uniformity of a film provided by embodiments of the present invention does not require the detection of incident particles or ray beams colliding with the sample to be measured to produce outgoing particles or ignition and emission of fluorescence, and is non-contact. Non-destructive testing does not damage the material composition of the sample being tested, nor does it affect the performance of the sample being tested. It is very suitable for non-destructive testing of products on the production line or samples in the laboratory.

在一些实施例中,上述曲线拟合主要依据是均方误差值(Mean Squared Error,缩写为MSE)确定判断曲线拟合是否成功;其中,均方误差值越小意味着拟合出的变化曲线信息与被测样品的椭偏光谱曲线信息越吻合。而上述曲线拟合就是寻找最小均方误差值的过程,将进行曲线拟合的收敛条件设置为均方误差值小于80;进一步,将进行曲线拟合的收敛条件设置为均方误差值小于20,可较快的拟合出符合要求的被测样品的光电参数在被测样品纵向方向上的变化曲线信息。In some embodiments, the above-mentioned curve fitting is mainly based on the mean squared error value (Mean Squared Error, abbreviated as MSE) to determine whether the curve fitting is successful; wherein, the smaller the mean squared error value means that the fitted change curve The information is more consistent with the ellipsometric spectral curve information of the sample being measured. The above curve fitting is the process of finding the minimum mean square error value. The convergence condition for curve fitting is set to a mean square error value less than 80; further, the convergence condition for curve fitting is set to a mean square error value less than 20. , can quickly fit the change curve information of the photoelectric parameters of the tested sample in the longitudinal direction of the tested sample that meets the requirements.

可以理解的是,由于镀膜法或化学沉积法等成膜工艺的原因,使得所制作的薄膜的成品规格不可避免的存在一定的误差,即成品规格与所要求的规格之间有一定的差距,这导致向基础模型输入薄膜的已知值时,所拟合出的结果与设定规格有所出入。例如:当透明导电薄膜的初始膜厚为350nm,将350nm作为基础模型的初始值输入基础模型,所获得的拟合结果在350nm左右,而不会与初始膜厚保持一致,这种误差是允许的。为了提高拟合的准确性,可在进行曲线拟合前将已知的初始值输入基础模型进行拟合后,根据拟合结果重新设定膜厚初始值为100nm-700nm,此时同样可以拟合出的结果,只是MSE值结果会不同,但如果膜厚初始值的偏差太多,比如设定膜厚初始值为1000nm,则拟合出的结果就相差甚远了。由此可见,在拟合过程中,将所需拟合的参数设定为一组梯度化变量参数,可有效缩短拟合时间,从而提高拟合准确率。It is understandable that due to film-forming processes such as coating or chemical deposition, there is inevitably a certain error in the finished specifications of the films produced, that is, there is a certain gap between the finished specifications and the required specifications. This causes the fitting results to differ from the set specifications when the known values of the film are input into the basic model. For example: when the initial film thickness of the transparent conductive film is 350nm, and 350nm is input into the basic model as the initial value of the basic model, the obtained fitting result will be around 350nm, which will not be consistent with the initial film thickness. This error is allowed of. In order to improve the accuracy of fitting, you can input the known initial value into the basic model before performing curve fitting. After fitting, the initial value of the film thickness can be reset to 100nm-700nm based on the fitting results. At this time, you can also simulate The combined results will be different only in the MSE value. However, if the initial value of the film thickness deviates too much, for example, if the initial value of the film thickness is set to 1000nm, the fitting results will be very different. It can be seen that during the fitting process, setting the required fitting parameters as a set of gradient variable parameters can effectively shorten the fitting time and thereby improve the fitting accuracy.

为了使获得的被测样品的光电参数在被测样品纵向方向上的变化曲线信息更为精确,可以要求被测样品的光电参数满足克莱默-克朗尼格关系(Kramers-Kronig关系,简称K-K关系),光电参数可以为光学常数、介电常数中的一种或两种。In order to obtain more accurate information about the change curve of the photoelectric parameters of the tested sample in the longitudinal direction of the tested sample, the photoelectric parameters of the tested sample can be required to satisfy the Kramer-Kronig relationship (Kramers-Kronig relationship, referred to as K-K relationship), the photoelectric parameters can be one or both of optical constants and dielectric constants.

例如:光学常数包括折射率n与消光系数k,当光学常数满足K-K关系时,折射率n和消光系数k满足K-K关系。另外,由于光的本质是电磁波,根据麦克斯韦方程可推导出光学常数与介电常数之间的关系式:n2-k2=εr,2nk=σ/(ωe0)(εr为相对介电常数,为复数;σ为电导率,ω为平面波的角频率,e0为真空介电常数)。而根据光学常数与介电常数之间的关系式,可以确定光学常数与介电常数之间存在的数学关系,因此,进行曲线拟合时,可以根据实际需要选择拟合结果为光学常数还是介电常数,或者是光学常数和介电常数。For example: optical constants include refractive index n and extinction coefficient k. When the optical constants satisfy the KK relationship, the refractive index n and extinction coefficient k satisfy the KK relationship. In addition, since the nature of light is electromagnetic waves, the relationship between optical constants and dielectric constants can be derived according to Maxwell's equations: n2 -k2r , 2nk =σ/(ωe0 ) (εr is the relative medium The electrical constant is a complex number; σ is the conductivity, ω is the angular frequency of the plane wave, and e0 is the vacuum dielectric constant). According to the relationship between optical constants and dielectric constants, the mathematical relationship between optical constants and dielectric constants can be determined. Therefore, when performing curve fitting, you can choose whether the fitting result is an optical constant or a dielectric constant according to actual needs. Electrical constant, or optical constant and dielectric constant.

可以理解的是,上述薄膜纵向不均匀性检测方法可依靠处理器执行,该处理器可以是一个处理器,也可以是多个处理元件的统称。例如,该处理器可以是中央处理器(Central Processing Unit,简称CPU),也可以是特定集成电路(Application SpecificIntegrated Circuit,简称ASIC),或者是被配置成实施本发明实施例的一个或多个集成电路,例如:一个或多个微处理器(digital signal processor,简称DSP),或,一个或者多个现场可编程门阵列(Field Programmable Gate Array,简称FPGA)。It can be understood that the above-mentioned method for detecting longitudinal non-uniformity of a film can be executed by relying on a processor, and the processor can be a processor or a collective name for multiple processing elements. For example, the processor may be a Central Processing Unit (CPU), an Application Specific Integrated Circuit (ASIC), or one or more integrated circuits configured to implement embodiments of the present invention. Circuits, for example: one or more microprocessors (digital signal processor, DSP for short), or one or more field programmable gate arrays (Field Programmable Gate Array, FPGA for short).

在实际应用中,可以将上述处理器设在椭偏光谱仪中,使得其作为椭偏光谱仪的一部分,从而实现对椭偏光谱仪的升级改造;同时,该处理器可以与椭偏光谱仪内的处理器以芯片的形式集成在一起。当然,也可以将上述处理器设在其他终端设备中,并保持该终端设备与椭偏光谱仪通信。In practical applications, the above-mentioned processor can be set up in the ellipsometer, so that it can be used as a part of the ellipsometer, thereby upgrading the ellipsometer; at the same time, the processor can be combined with the processor in the ellipsometer. Integrated together in the form of chips. Of course, the above processor can also be installed in other terminal equipment and maintain communication between the terminal equipment and the ellipsometer.

本发明实施例还提供了一种薄膜纵向不均匀性检测终端300,如图5所示,包括:存储器301和处理器302;其中,存储器301用于储存一个或多个计算机软件指令,其包含用于执行上述第一种实现方式的薄膜纵向不均匀性检测方法所涉及的程序;处理器302用于执行一个或多个计算机软件指令,以实现上述方案中薄膜纵向不均匀性检测方法。The embodiment of the present invention also provides a film longitudinal non-uniformity detection terminal 300, as shown in Figure 5, including: a memory 301 and a processor 302; wherein the memory 301 is used to store one or more computer software instructions, which includes The processor 302 is used to execute the program involved in the film longitudinal non-uniformity detection method in the first implementation mode; the processor 302 is used to execute one or more computer software instructions to implement the film longitudinal non-uniformity detection method in the above solution.

该薄膜纵向不均匀性检测终端还包括收发器303以及总线304,存储器301、处理器302和收发器303通过总线304互相通信;收发器303可支持处理器与椭偏光谱仪100和显示模组500通信。The film longitudinal non-uniformity detection terminal also includes a transceiver 303 and a bus 304. The memory 301, the processor 302 and the transceiver 303 communicate with each other through the bus 304; the transceiver 303 can support the processor, the ellipsometer 100 and the display module 500. communication.

上述存储器301可以是一个存储装置,也可以是多个存储元件的统称,且用于存储执行本发明方案的程序代码,并由处理器302来控制执行。存储器301可以是只读存储器(read-only memory,ROM)或可存储静态信息和指令的其他类型的静态存储设备,随机存取存储器(random access memory,RAM)或者可存储信息和指令的其他类型的动态存储设备,也可以是电可擦可编程只读存储器(Electrically Erasable Programmable Read-OnlyMemory,EEPROM)、只读光盘(Compact Disc Read-Only Memory,CD-ROM)或其他光盘存储、光碟存储(包括压缩光碟、激光碟、光碟、数字通用光碟、蓝光光碟等)、磁盘存储介质或者其他磁存储设备、或者能够用于携带或存储具有指令或数据结构形式的期望的程序代码并能够由计算机存取的任何其他介质,但不限于此。The above-mentioned memory 301 can be a storage device, or can be a collective name for multiple storage elements, and is used to store program codes for executing the solution of the present invention, and is controlled by the processor 302 for execution. The memory 301 may be a read-only memory (ROM) or other type of static storage device that can store static information and instructions, a random access memory (random access memory (RAM)) or other type that can store information and instructions. The dynamic storage device can also be Electrically Erasable Programmable Read-Only Memory (EEPROM), Compact Disc Read-Only Memory (CD-ROM) or other optical disk storage, optical disk storage ( Including compressed optical discs, laser discs, optical discs, digital versatile discs, Blu-ray discs, etc.), magnetic disk storage media or other magnetic storage devices, or can be used to carry or store desired program code in the form of instructions or data structures and can be stored by a computer. any other medium, but not limited to this.

上述处理器302可以是一个处理器,也可以是多个处理元件的统称。例如,该处理器302可以是中央处理器(Central Processing Unit,简称CPU),也可以是特定集成电路(Application Specific Integrated Circuit,简称ASIC),或者是被配置成实施本发明实施例的一个或多个集成电路,例如:一个或多个微处理器(digital signal processor,简称DSP),或,一个或者多个现场可编程门阵列(Field Programmable Gate Array,简称FPGA)。The above-mentioned processor 302 may be one processor, or may be a collective name for multiple processing elements. For example, the processor 302 may be a Central Processing Unit (CPU), an Application Specific Integrated Circuit (ASIC), or one or more processors configured to implement embodiments of the present invention. An integrated circuit, such as one or more microprocessors (digital signal processor, DSP for short), or one or more field programmable gate arrays (Field Programmable Gate Array, FPGA for short).

上述收发器303则用于与其他设备或通信网络通信,如以太网,无线接入网(RAN),无线局域网(Wireless Local Area Networks,WLAN)等。The above-mentioned transceiver 303 is used to communicate with other devices or communication networks, such as Ethernet, Radio Access Network (RAN), Wireless Local Area Networks (WLAN), etc.

上述总线304可以是工业标准体系结构(Industry Standard Architecture,ISA)总线、外部设备互连(Peripheral Component,PCI)总线或扩展工业标准体系结构(Extended Industry Standard Architecture,EISA)总线等。该总线304可以分为地址总线、数据总线、控制总线等。为便于表示,图5中仅用一条粗线表示,但并不表示仅有一根总线或一种类型的总线。The above-mentioned bus 304 may be an Industry Standard Architecture (ISA) bus, a Peripheral Component Interconnect (PCI) bus or an Extended Industry Standard Architecture (EISA) bus, etc. The bus 304 can be divided into an address bus, a data bus, a control bus, etc. For ease of presentation, only one thick line is used in Figure 5, but it does not mean that there is only one bus or one type of bus.

请参阅图1和图3,本发明实施例提供了一种薄膜纵向不均匀性检测装置,该薄膜纵向不均匀性检测装置可执行上述第一种实现方式中的薄膜纵向不均匀性检测方法,该薄膜纵向不均匀性检测装置包括:Referring to Figures 1 and 3, an embodiment of the present invention provides a film longitudinal non-uniformity detection device. The film longitudinal non-uniformity detection device can perform the film longitudinal non-uniformity detection method in the above first implementation manner, The film longitudinal unevenness detection device includes:

接收单元201,用于获取被测样品的椭偏光谱曲线信息,如图4所示,被测样品至少包括被测薄膜402。The receiving unit 201 is used to obtain the ellipsometric spectral curve information of the sample to be tested. As shown in FIG. 4 , the sample to be tested at least includes the film to be tested 402 .

模型化单元202,用于根据被测样品的物质组成建立各向同性的物理模型,该物理模型包括至少包括薄膜模型;将薄膜模型所含有的至少一个变量参数转换为至少一组梯度化变量参数。Modeling unit 202 is used to establish an isotropic physical model according to the material composition of the sample to be measured. The physical model includes at least a film model; convert at least one variable parameter contained in the film model into at least one set of gradient variable parameters. .

曲线拟合单元203,用于以被测样品的椭偏光谱曲线信息为曲线拟合目标,利用至少一组薄膜模型对梯度化变量参数进行曲线拟合,获得被测样品的光电参数在被测样品纵向方向上的变化曲线信息。The curve fitting unit 203 is used to use the ellipsometric spectrum curve information of the measured sample as a curve fitting target, use at least one set of film models to perform curve fitting on the gradient variable parameters, and obtain the photoelectric parameters of the measured sample in the measured Change curve information in the longitudinal direction of the sample.

分析单元204,用于根据被测样品的光电参数在被测样品纵向方向上的变化曲线信息评价被测样品的纵向不均匀性。The analysis unit 204 is used to evaluate the longitudinal non-uniformity of the tested sample based on the change curve information of the photoelectric parameters of the tested sample in the longitudinal direction of the tested sample.

具体实施时,接收单元201接收被测样品的椭偏光谱曲线信息;如图4所示,考虑到被测样品/空气界面并不是理想的光滑平面,被测样品包括粗糙层401、被测薄膜402和基体层403;粗糙层401由体积百分比为50%的被测薄膜和体积百分比为50%的孔隙组成,且被测薄膜402可以为不止一层。During specific implementation, the receiving unit 201 receives the ellipsometric spectral curve information of the tested sample; as shown in Figure 4, considering that the tested sample/air interface is not an ideal smooth plane, the tested sample includes a rough layer 401, a tested thin film 402 and base layer 403; the rough layer 401 is composed of 50% volume percentage of the film to be measured and 50% volume percentage of pores, and the film 402 to be measured can be more than one layer.

模型化单元202对被测样品建立各向同性的物理模型,以模拟出符合被测样品特性的物理模型,并且考虑到对被测样品光电常数起决定性作用的为薄膜层,故所建立的物理模型至少包括薄膜模型;并且薄膜模型包括若干个变量参数,同时,由于被测薄膜容易出现纵向不均匀的问题,将至少一个变量参数转换为至少一组梯度化变量参数。The modeling unit 202 establishes an isotropic physical model for the sample to be measured to simulate a physical model that conforms to the characteristics of the sample to be measured, and considering that the thin film layer plays a decisive role in the photoelectric constant of the sample to be measured, the physical model established The model at least includes a film model; and the film model includes several variable parameters. At the same time, since the measured film is prone to longitudinal non-uniformity, at least one variable parameter is converted into at least one set of gradient variable parameters.

曲线拟合单元203以椭偏光谱曲线信息为拟合目标,利用薄膜模型对至少一组梯度化变量参数进行曲线拟合,获得被测样品的光电参数在被测样品纵向方向上的变化曲线信息。The curve fitting unit 203 takes the ellipsometric spectrum curve information as the fitting target, uses the film model to perform curve fitting on at least one set of gradient variable parameters, and obtains the change curve information of the photoelectric parameters of the tested sample in the longitudinal direction of the tested sample. .

分析单元204根据被测样品的光电参数在被测样品纵向方向上的变化曲线信息来确定被测样品的纵向不均匀性。The analysis unit 204 determines the longitudinal non-uniformity of the tested sample based on the change curve information of the photoelectric parameters of the tested sample in the longitudinal direction of the tested sample.

可以理解的是,上述物理模型包括透明材料物理模型和/或折射色散振子模型;而梯度化变量参数包括线性梯度变化的变量参数或非线性梯度变化的变量参数,具体效果分析参见前文,此处不再赘述。It can be understood that the above physical model includes a transparent material physical model and/or a refractive dispersion oscillator model; and the gradient variable parameters include linear gradient variable parameters or nonlinear gradient variable parameters. For specific effect analysis, please refer to the previous article, here No longer.

上述曲线拟合的过程实质是寻找最小均方误差值的过程,为了较快得到被测样品的光电参数在被测样品纵向方向上的变化曲线信息,将进行曲线拟合的收敛条件设置为均方误差值小于80;进一步,将进行曲线拟合的收敛条件设置为均方误差值小于20。The essence of the above curve fitting process is to find the minimum mean square error value. In order to quickly obtain the change curve information of the photoelectric parameters of the tested sample in the longitudinal direction of the tested sample, the convergence condition for curve fitting is set to uniform. The square error value is less than 80; further, the convergence condition for curve fitting is set to a mean square error value less than 20.

为了使获得的被测样品的光电参数在被测样品纵向方向上的变化曲线信息更为精确,可以要求被测样品的光学常数和/或介电常数满足K-K关系。In order to obtain more accurate information about the change curve of the photoelectric parameters of the tested sample in the longitudinal direction of the tested sample, the optical constant and/or dielectric constant of the tested sample can be required to satisfy the K-K relationship.

在第二种可实现方式中,如图2所示,提供一种薄膜纵向不均匀性检测方法,包括:In the second possible way, as shown in Figure 2, a method for detecting longitudinal non-uniformity of a film is provided, including:

步骤S210:测量被测样品的椭偏光谱曲线,可采用椭偏法测量椭偏光谱曲线,椭偏法不但高灵敏度、高精度,并且还为无损非接触的检测方式,不会对被测样品造成损害。Step S210: Measure the ellipsometry spectrum curve of the sample to be tested. The ellipsometry method can be used to measure the ellipsometry spectrum curve. The ellipsometry method is not only highly sensitive and precise, but also a non-destructive and non-contact detection method, which will not affect the sample being tested. cause damage.

步骤S220:将被测样品的椭偏光谱曲线信息发送给上述薄膜纵向不均匀性检测装置。其中,被测样品的椭偏光谱曲线信息表征被测样品的椭偏光谱曲线。Step S220: Send the ellipsometric spectral curve information of the tested sample to the above-mentioned film longitudinal non-uniformity detection device. Among them, the ellipsometric spectral curve information of the tested sample represents the ellipsometric spectral curve of the tested sample.

步骤S230:利用薄膜纵向不均匀性检测装置确定被测样品的纵向不均匀性。Step S230: Determine the longitudinal unevenness of the tested sample using a film longitudinal unevenness detection device.

与现有技术相比,本发明实施例提供的薄膜纵向不均匀性检测方法可参见前文描述,此处不做详述。Compared with the prior art, the method for detecting longitudinal non-uniformity of the film provided by the embodiment of the present invention can be referred to the previous description and will not be described in detail here.

在一些实施例中,如图6所示,上述测量被测样品的椭偏光谱曲线具体包括:In some embodiments, as shown in Figure 6, the above-mentioned measurement of the ellipsometric spectral curve of the tested sample specifically includes:

步骤S211:设定线偏振光的入射角度,使得线偏振光的入射角度包括至少一个第一入射角度和至少一个第二入射角度,第一入射角度大于被测样品材料的布儒斯特角,第二入射角度小于被测样品材料的布儒斯特角。Step S211: Set the incident angle of linearly polarized light so that the incident angle of linearly polarized light includes at least one first incident angle and at least one second incident angle, and the first incident angle is greater than the Brewster angle of the sample material to be tested, The second incident angle is smaller than the Brewster angle of the sample material being tested.

步骤S212:向被测样品入射线偏振光,检测被测样品的椭圆偏振p光与s光的振幅比和被测样品的椭圆偏振p光与s光的相位差。考虑到透明导电薄膜或者其他薄膜的的光学常数梯度变化存在于可见光及近红外波段,因此,设定线偏振光的波长范围为300nm-2400nm。Step S212: Inject linearly polarized light into the sample to be tested, and detect the amplitude ratio of the elliptically polarized p-light and s-light of the sample to be tested and the phase difference between the elliptically-polarized p-light and s-light of the sample to be tested. Considering that the optical constant gradient changes of transparent conductive films or other films exist in the visible light and near-infrared bands, the wavelength range of linearly polarized light is set to 300nm-2400nm.

步骤S213:根据被测样品的椭圆偏振p光与s光的振幅比和线偏振光的波长范围,获得被测样品的椭偏Ψ光谱曲线;根据被测样品的椭圆偏振p光与s光的相位差和线偏振光的波长范围,获得被测样品的椭偏Δ光谱曲线。Step S213: According to the amplitude ratio of the elliptically polarized p light and s light of the tested sample and the wavelength range of the linearly polarized light, obtain the elliptical polarization Ψ spectrum curve of the tested sample; according to the amplitude ratio of the elliptically polarized p light and s light of the tested sample The phase difference and the wavelength range of linearly polarized light are used to obtain the ellipsometric Δ spectral curve of the sample under test.

当第一入射角度大于被测样品材料的布儒斯特角,第二入射角度小于被测样品材料的布儒斯特角时,使得所测量的被测样品的椭圆偏振p光与s光的相位差具有突变,可利用该突变确定后期曲线拟合结果是否准确,因此,当第一入射角度大于被测样品材料的布儒斯特角,第二入射角度小于被测样品材料的布儒斯特角时,所测得的被测样品的椭偏光谱曲线比较利于后期曲线拟合;如果第一入射角度和第二入射角度均大于被测样品材料的布儒斯特角,或者第一入射角度和第二入射角度均小于被测样品材料的布儒斯特角,则所测量的被测样品的椭偏光谱曲线没有太大的差别,不利于后期曲线拟合,容易造成曲线拟合不准确的问题。例如:如玻璃的布儒斯特角为56.7°,那么测试角度需要至少有分别小于56.7°和大于56.7°的两个入射角度。When the first incident angle is greater than the Brewster angle of the sample material to be measured, and the second incident angle is smaller than the Brewster angle of the sample material to be measured, the measured elliptically polarized p-light and s-light of the sample to be measured are The phase difference has a sudden change, which can be used to determine whether the later curve fitting results are accurate. Therefore, when the first incident angle is greater than the Brewster's angle of the sample material being tested, the second incident angle is smaller than the Brewster's angle of the sample material being tested. When the angle is special, the measured ellipsometric spectral curve of the tested sample is more conducive to later curve fitting; if the first incident angle and the second incident angle are both greater than the Brewster angle of the tested sample material, or the first incident angle If both the angle and the second incident angle are smaller than the Brewster angle of the material being tested, then the measured ellipsometric spectral curves of the sample being tested are not very different, which is not conducive to later curve fitting and can easily lead to inaccuracies in curve fitting. Exact question. For example: If the Brewster angle of glass is 56.7°, then the test angle needs to have at least two incident angles less than 56.7° and greater than 56.7°.

至于上述第一入射角度的数量和上述第二入射角度的数量可以根据实际情况决定;当上述第一入射角度的数量至少为两个时,各个第一入射角度不同,当上述第二入射角度的数量至少为两个时,各个第二入射角度不同。The number of the above-mentioned first incident angles and the above-mentioned second incident angles can be determined according to the actual situation; when the number of the above-mentioned first incident angles is at least two, each first incident angle is different, and when the above-mentioned second incident angles are When the number is at least two, each second incident angle is different.

实施例二Embodiment 2

本发明实施例提供了一种薄膜纵向不均匀性检测方法,包括:The embodiment of the present invention provides a method for detecting longitudinal non-uniformity of a film, which includes:

第一步,采用椭圆偏振光谱仪测试膜厚为350nm的In2O3:Sn(又称为ITO)薄膜,椭圆偏振光谱仪为美国J.A.Woollam公司生产的V型自动变角光谱型椭圆偏振光谱仪。采用椭圆偏振光谱仪测试膜厚为350nm的In2O3:Sn(又称为ITO)薄膜包括:在V型自动变角光谱型椭圆偏振光谱仪处在高精度模式时,设定线偏振光的入射角度为52.5°~75°,线偏振光的波长范围为300nm-900nm;在线偏振光的入射角度为52.5°~75°下,分别利用线偏振光照射ITO薄膜,获得如图7中粗虚线所示的ITO薄膜的椭偏Δ光谱实测曲线和如图8中粗虚线所示的ITO薄膜的椭偏Ψ光谱实测曲线。In the first step, an In2 O3 :Sn (also known as ITO) film with a film thickness of 350 nm was tested using an ellipsometer. The ellipsometer was a V-type automatic variable angle spectrum ellipsometer produced by the American JAWoollam Company. Using an ellipsometry spectrometer to test an In2 O3 :Sn (also known as ITO) film with a film thickness of 350 nm includes: setting the incidence of linearly polarized light when the V-type automatic angle-changing spectrum ellipsometry spectrometer is in the high-precision mode The angle is 52.5°~75°, and the wavelength range of linearly polarized light is 300nm-900nm; when the incident angle of linearly polarized light is 52.5°~75°, linearly polarized light is used to irradiate the ITO film, and the thick dotted line in Figure 7 is obtained. The measured ellipsometric Δ spectrum curve of the ITO film is shown in Figure 8 and the measured ellipsometric Ψ spectrum curve of the ITO film is shown as the thick dotted line in Figure 8.

第二步,上述ITO薄膜形成在基体层之上,同时还包括形成在ITO薄膜远离基体层之上的粗糙层;基体层为6mm厚普通浮法玻璃,粗糙层是采用有效介质理论设定的体积百分比为50%的ITO膜和体积百分比为50%的孔隙的表面疏松层,其光学常数为ITO膜光学常数的一半。基于此,根据基体层、ITO薄膜和粗糙层的特性建立各向同性的物理模型,该物理模型包括表面模型、ITO模型和基体模型,在建模过程中,按照建模空间次序依次建立表面模型、ITO模型和基体模型,使得表面模型、ITO模型和基体模型在建模空间上呈现由上至下的顺序。In the second step, the above-mentioned ITO film is formed on the base layer, and also includes a rough layer formed on the ITO film away from the base layer; the base layer is 6mm thick ordinary float glass, and the rough layer is set using the effective medium theory The optical constant of the surface loose layer of the ITO film with a volume percentage of 50% and the pores with a volume percentage of 50% is half of the optical constant of the ITO film. Based on this, an isotropic physical model is established based on the characteristics of the matrix layer, ITO film and rough layer. The physical model includes a surface model, an ITO model and a matrix model. During the modeling process, the surface model is established sequentially according to the order of the modeling space. , ITO model and matrix model, so that the surface model, ITO model and matrix model present a top-to-bottom order in the modeling space.

上述表面模型是根据粗糙层的特性建立的有效介质模型,ITO模型是根据ITO薄膜的特性建立,基体模型是根据浮法玻璃的特性建立对于浮法玻璃来说,浮法玻璃所使用的材料透明材料,所建立的基体模型的种类为柯西模型。对于ITO薄膜来说,ITO薄膜所使用的材料为半导体材料,所建立的薄膜模型为洛伦兹模型或高斯模型。基于此,根据ITO薄膜的透明导电特性,建立为作为ITO模型的高斯模型,高斯模型是用高斯概率密度函数(对应的曲线为正态分布曲线)精确地量化事物,将一个事物分解成若干的基于高斯概率密度函数形成的模型。The above surface model is an effective medium model established based on the characteristics of the rough layer, the ITO model is established based on the characteristics of the ITO film, and the matrix model is established based on the characteristics of float glass. For float glass, the material used in float glass is transparent Material, the type of matrix model established is Cauchy model. For ITO films, the materials used in ITO films are semiconductor materials, and the film model established is a Lorentz model or a Gaussian model. Based on this, based on the transparent conductive characteristics of the ITO film, a Gaussian model was established as an ITO model. The Gaussian model uses a Gaussian probability density function (the corresponding curve is a normal distribution curve) to accurately quantify things and decompose one thing into several A model formed based on Gaussian probability density function.

第三步,高斯模型中的变量参数有中心峰位En、振幅(即峰高Amp)、半高宽Br等。从高斯模型所含有的选择中心峰位En作为变量参数,将中心峰位En转换为线性梯度变化的变量参数,即将中心峰位En在纵向的最大值与最小值之间分成若干个台阶,且台阶数目越多,拟合时间较长但是拟合效果较好;台阶数目越少,拟合时间较短但拟合效果不佳。In the third step, the variable parameters in the Gaussian model include the central peak position En, amplitude (ie, peak height Amp), half-maximum width Br, etc. Select the center peak position En as a variable parameter from the Gaussian model, and convert the center peak position En into a linear gradient variable parameter, that is, divide the center peak position En into several steps between the maximum and minimum values in the longitudinal direction, and The greater the number of steps, the longer the fitting time but the better the fitting effect; the smaller the number of steps, the shorter the fitting time but the poorer the fitting effect.

例如:图9示出了线性梯度变化的中心峰位分布示意图,其纵坐标为中心峰位En,横坐标为高斯模型对应的实体膜层的深度(也可以为纵向长度)。如图9所示,采用线性梯度模型将中心峰位En设置为沿纵向方向(高斯模型对应的实体膜层的纵向方向或者厚度方向)变化的10个高度相等的台阶,获得线性梯度变化的中心峰位。For example: Figure 9 shows a schematic diagram of the central peak position distribution of a linear gradient change. The ordinate is the central peak position En, and the abscissa is the depth of the solid film layer corresponding to the Gaussian model (it can also be the longitudinal length). As shown in Figure 9, the linear gradient model is used to set the central peak position En to 10 steps of equal height that change along the longitudinal direction (the longitudinal direction or thickness direction of the physical film layer corresponding to the Gaussian model) to obtain the center of the linear gradient change. peak position.

第四步,利用高斯模型采用反演计算的方式对线性梯度化中心峰位进行曲线拟合,拟合的MSE值为9;其中,在进行曲线拟合的过程中,所拟合出的曲线为如图7中细实线所示的ITO薄膜的椭偏Δ光谱拟合曲线和如图8中细实线所示的ITO薄膜的椭偏Ψ光谱拟合曲线。在拟合成功时,将所获得的ITO薄膜的椭偏Δ光谱拟合曲线和ITO薄膜的椭偏Δ光谱拟合曲线进行变换,获得如图10所示的ITO薄膜的折射率和消光系数在被测样品纵向方向上的变化曲线的相关信息,当然也可以获得如图11所示的ITO薄膜顶部与底部的介电常数随光子能量的变化曲线的相关信息。The fourth step is to use the Gaussian model to perform curve fitting on the linear gradient center peak position using inversion calculation. The fitted MSE value is 9; among them, during the curve fitting process, the fitted curve The ellipsometric Δ spectrum fitting curve of the ITO film shown in the thin solid line in Figure 7 and the ellipsometric Ψ spectrum fitting curve of the ITO film shown in the thin solid line in Figure 8 are fitted. When the fitting is successful, the obtained ellipsometry Δ spectrum fitting curve of the ITO film and the ellipsometry Δ spectrum fitting curve of the ITO film are transformed to obtain the refractive index and extinction coefficient of the ITO film as shown in Figure 10. Information about the change curve in the longitudinal direction of the tested sample can also be obtained. Information about the change curve of the dielectric constant with photon energy at the top and bottom of the ITO film as shown in Figure 11 can also be obtained.

图7和图8中a~j代表线偏振光的入射角度,a=52.5°,b=57.5°,c=62.5°,d=55°,e=65°,f=60°,g=70°,h=67.5°,i=72.5°,j=75°;将图7中粗虚线所示的ITO薄膜的椭偏Δ光谱实测曲线和细实线所示的ITO薄膜的椭偏Δ光谱拟合曲线进行对比可以发现:根据所建立的高斯模型以及设置的线性梯度变化的变量参数,得到ITO薄膜的椭偏Δ光谱拟合曲线与ITO薄膜的椭偏Δ光谱实测曲线相吻合,且ITO薄膜的椭偏Δ光谱实测曲线满足K-K关系,说明采用高斯模型对线性梯度变化的中心峰位进行拟合的拟合结果很好。将图8中粗虚线所示的ITO薄膜的椭偏Ψ光谱实测曲线和细实线所示的ITO薄膜的椭偏Ψ光谱拟合曲线进行对比可以发现:根据所建立的高斯模型以及设置的线性梯度变化的变量参数,得到ITO薄膜的椭偏Ψ光谱拟合曲线与ITO薄膜的椭偏Ψ光谱实测曲线相吻合,且ITO薄膜的椭偏Ψ光谱实测曲线满足K-K关系,说明采用高斯模型对线性梯度变化的中心峰位进行拟合的拟合结果很好。此时,可将如图10所示的ITO薄膜的折射率和消光系数在被测样品纵向方向上的变化曲线信息输出,当然也可以选择如图11所示的ITO薄膜顶部与底部的介电常数随光子能量的变化曲线输出,所输出的图10和图11可通过显示模组显示,以方便数据分析。In Figures 7 and 8, a~j represent the incident angles of linearly polarized light, a=52.5°, b=57.5°, c=62.5°, d=55°, e=65°, f=60°, g=70 °, h = 67.5°, i = 72.5°, j = 75°; the measured curve of the ellipsometric Δ spectrum of the ITO film shown in the thick dotted line in Figure 7 and the simulated ellipsometric Δ spectrum of the ITO film shown in the thin solid line By comparing the combined curves, it can be found that according to the established Gaussian model and the set linear gradient variable parameters, the ellipsometry Δ spectrum fitting curve of the ITO film is consistent with the measured ellipsometry Δ spectrum curve of the ITO film, and the ITO film The measured curve of the ellipsometric Δ spectrum satisfies the K-K relationship, indicating that the fitting result of using the Gaussian model to fit the central peak position of the linear gradient change is very good. Comparing the measured ellipsometric Ψ spectrum curve of the ITO film shown in the thick dashed line in Figure 8 with the ellipsometric Ψ spectrum fitting curve of the ITO film shown in the thin solid line, it can be found that: according to the established Gaussian model and the set linear By using gradient variable parameters, the fitting curve of the ellipsometry Ψ spectrum of the ITO film is consistent with the measured ellipsometry Ψ spectrum curve of the ITO film, and the measured ellipsometry Ψ spectrum curve of the ITO film satisfies the K-K relationship, indicating that the Gaussian model is used for linear The fitting result of fitting the central peak position of the gradient change is very good. At this time, the change curve information of the refractive index and extinction coefficient of the ITO film in the longitudinal direction of the tested sample can be output as shown in Figure 10. Of course, you can also choose the dielectric at the top and bottom of the ITO film as shown in Figure 11. The constant changes with photon energy are output as a curve. The output Figures 10 and 11 can be displayed through the display module to facilitate data analysis.

第五步,图10中示出的上折射率是指ITO薄膜相对粗糙层的表面(下文简称ITO薄膜的顶部)的折射率,下折射率是指ITO薄膜相对基体层的表面(下文简称ITO薄膜的底部)的折射率,可利用下折射率代表ITO薄膜的内部折射率;上消光系数是指ITO薄膜顶部的消光系数,下消光系数是指ITO薄膜底部的消光系数,可利用下消光系数代表ITO薄膜的内部消光系数。由图10可以看出:对于折射率来说,ITO薄膜的顶部折射率大于ITO薄膜的底部(内部)折射率,且差别随波长无变化。对于消光系数来说,在短波长的范围内,ITO薄膜的顶部消光系数与ITO薄膜的底部(内部)消光系数相同;在长波长的范围内,ITO薄膜的顶部消光系数大于ITO薄膜的底部(内部)的消光系数,因此,可以根据图10可以确定ITO薄膜的折射率与消光系数同时沿ITO薄膜纵向方向的变化,而ITO薄膜的折射率与消光系数同时随纵向方向的变化时,确定ITO薄膜的氧含量随ITO薄膜纵向方向不均匀。In the fifth step, the upper refractive index shown in Figure 10 refers to the refractive index of the surface of the ITO film relative to the rough layer (hereinafter referred to as the top of the ITO film), and the lower refractive index refers to the surface of the ITO film relative to the base layer (hereinafter referred to as ITO). The refractive index of the bottom of the ITO film), the lower refractive index can be used to represent the internal refractive index of the ITO film; the upper extinction coefficient refers to the extinction coefficient at the top of the ITO film, and the lower extinction coefficient refers to the extinction coefficient at the bottom of the ITO film, the lower extinction coefficient can be used Represents the internal extinction coefficient of the ITO film. It can be seen from Figure 10 that for the refractive index, the refractive index of the top of the ITO film is greater than the bottom (internal) refractive index of the ITO film, and the difference does not change with wavelength. For the extinction coefficient, in the short wavelength range, the top extinction coefficient of the ITO film is the same as the bottom (internal) extinction coefficient of the ITO film; in the long wavelength range, the top extinction coefficient of the ITO film is greater than the bottom of the ITO film ( Therefore, according to Figure 10, it can be determined that the refractive index and extinction coefficient of the ITO film change along the longitudinal direction of the ITO film at the same time, and when the refractive index and extinction coefficient of the ITO film change along the longitudinal direction at the same time, the ITO can be determined The oxygen content of the film is not uniform along the longitudinal direction of the ITO film.

图11中示出的上ε1为ITO薄膜相对粗糙层的表面(下文简称ITO薄膜的顶部)的实部,下ε1为ITO薄膜相对基体层(下文简称ITO薄膜的底面)的表面的实部;上ε2为ITO薄膜相对粗糙层的表面(下文简称ITO薄膜的顶部)的实部,下ε2为ITO薄膜相对基体层的表面(下文简称ITO薄膜的底部部)的实部。由图11可以看出,ITO薄膜的顶部介电常数的实部ε1与虚部ε2均大于ITO薄膜的底部介电常数的实部ε1与虚部ε2,因此,可以根据图11确定ITO薄膜的介电常数沿ITO薄膜的纵向变化;而当ITO薄膜的介电常数沿ITO薄膜的纵向变化时,确定ITO薄膜的氧含量随ITO薄膜纵向方向不均匀。The upper ε1 shown in Figure 11 is the real part of the surface of the ITO film relative to the rough layer (hereinafter referred to as the top of the ITO film), and the lower ε1 is the real part of the surface of the ITO film relative to the base layer (hereinafter referred to as the bottom surface of the ITO film). The upper ε2 is the real part of the surface of the ITO film relative to the rough layer (hereinafter referred to as the top of the ITO film), and the lower ε2 is the real part of the surface of the ITO film relative to the base layer (hereinafter referred to as the bottom of the ITO film). It can be seen from Figure 11 that the real part ε1 and imaginary part ε2 of the dielectric constant at the top of the ITO film are both greater than the real part ε1 and imaginary part ε2 of the dielectric constant at the bottom of the ITO film. Therefore, according to Figure 11 It is determined that the dielectric constant of the ITO film changes along the longitudinal direction of the ITO film; and when the dielectric constant of the ITO film changes along the longitudinal direction of the ITO film, it is determined that the oxygen content of the ITO film is not uniform along the longitudinal direction of the ITO film.

实施例三Embodiment 3

第一步,采用椭圆偏振光谱仪测试膜厚为250nm的ZnO:Al(又称为AZO)薄膜,椭圆偏振光谱仪为美国J.A.Woollam公司生产的V型自动变角光谱型椭圆偏振光谱仪。采用椭圆偏振光谱仪测试膜厚为350nm的In2O3:Sn(又称为ITO)薄膜包括:在V型自动变角光谱型椭圆偏振光谱仪处在高精度模式时,设定线偏振光的入射角度为入射角度为55°与65°,线偏振光的波长范围为300-2500nm;在线偏振光的入射角度为55°与65°,分别利用线偏振光照射ITO薄膜,获得,获得如图12中粗虚线所示的AZO薄膜的椭偏Δ光谱实测曲线和如图13中粗虚线所示的AZO薄膜的椭偏Ψ光谱实测曲线。In the first step, a ZnO:Al (also known as AZO) film with a film thickness of 250 nm was tested using an ellipsometric spectrometer. The ellipsometric spectrometer was a V-type automatic variable-angle spectroscopic ellipsometer produced by the American JAWoollam company. Using an ellipsometry spectrometer to test an In2 O3 :Sn (also known as ITO) film with a film thickness of 350 nm includes: setting the incidence of linearly polarized light when the V-type automatic angle-changing spectrum ellipsometry spectrometer is in the high-precision mode The angle is that the incident angle is 55° and 65°, the wavelength range of linearly polarized light is 300-2500nm; the incident angle of linearly polarized light is 55° and 65°, respectively, the linearly polarized light is used to illuminate the ITO film, and the obtained result is as shown in Figure 12 The measured ellipsometric Δ spectrum curve of the AZO film shown in the middle thick dotted line and the measured ellipsometric Ψ spectrum curve of the AZO film shown in the thick dotted line in Figure 13.

第二步,上述AZO薄膜形成在基体层表面,同时还包括形成在AZO薄膜原理基体层表面的粗糙层,基体层为6mm厚普通浮法玻璃,粗糙层是采用有效介质理论设定的体积百分比为50%的AZO膜和体积百分比为50%的孔隙的表面疏松层,其光学常数为AZO膜光学常数的一半。基于此,根据基体层、AZO薄膜和粗糙层的特性建立各向同性的物理模型,该物理模型包括表面模型、AZO模型和基体模型,在建模过程中,按照建模空间次序依次建立表面模型、ITO模型和基体模型,使得表面模型、ITO模型和基体模型在建模空间上呈现由上至下的顺序。In the second step, the above-mentioned AZO film is formed on the surface of the base layer, and also includes a rough layer formed on the surface of the AZO thin film principle base layer. The base layer is 6mm thick ordinary float glass, and the rough layer is a volume percentage set by the effective medium theory. The optical constant of a surface loose layer of 50% AZO film and 50% pores in volume is half of the optical constant of the AZO film. Based on this, an isotropic physical model is established based on the characteristics of the matrix layer, AZO film and rough layer. The physical model includes a surface model, an AZO model and a matrix model. During the modeling process, the surface model is established sequentially according to the order of the modeling space. , ITO model and matrix model, so that the surface model, ITO model and matrix model present a top-to-bottom order in the modeling space.

上述表面模型是根据粗糙层的特性建立的有效介质模型,AZO模型是根据AZO薄膜的特性建立,基体模型是根据浮法玻璃的特性建立。对于浮法玻璃来说,浮法玻璃所使用的材料透明材料,所建立的基体模型的种类为柯西模型。对于AZO薄膜来说,AZO薄膜所使用的材料为半导体材料,所建立的薄膜模型为洛伦兹模型或高斯模型。基于此,根据AZO薄膜的透明导电特性,建立作为AZO模型的高斯模型,高斯模型是用高斯概率密度函数(对应的曲线为正态分布曲线)精确地量化事物,将一个事物分解成若干的基于高斯概率密度函数形成的模型。The above-mentioned surface model is an effective medium model established based on the characteristics of the rough layer, the AZO model is established based on the characteristics of the AZO thin film, and the matrix model is established based on the characteristics of float glass. For float glass, the material used in float glass is transparent material, and the type of matrix model established is the Cauchy model. For AZO films, the materials used in AZO films are semiconductor materials, and the film model established is a Lorentz model or a Gaussian model. Based on this, based on the transparent conductive characteristics of the AZO film, the Gaussian model as the AZO model is established. The Gaussian model uses the Gaussian probability density function (the corresponding curve is a normal distribution curve) to accurately quantify things and decompose one thing into several based on Model formed by Gaussian probability density function.

第三步,高斯模型中的变量参数有中心峰位En、振幅(即峰高Amp)、半高宽Br等。从高斯模型所含有的选择中心峰位En作为变量参数,将中心峰位En转换为非线性梯度变化的变量参数,即将中心峰位En在纵向的最大值与最小值之间分成若干个台阶,且台阶数目越多,拟合时间较长但是拟合效果较好;台阶数目越少,拟合时间较短但拟合效果不佳。In the third step, the variable parameters in the Gaussian model include the central peak position En, amplitude (ie, peak height Amp), half-maximum width Br, etc. From the Gaussian model, the center peak position En is selected as a variable parameter, and the center peak position En is converted into a variable parameter of nonlinear gradient change, that is, the center peak position En is divided into several steps between the longitudinal maximum value and the minimum value, And the greater the number of steps, the longer the fitting time but the better the fitting effect; the smaller the number of steps, the shorter the fitting time but the poorer the fitting effect.

例如:图14示出了非线性梯度变化的中心峰位分布示意图,其纵坐标为中心峰位En,横坐标为高斯模型对应的实体膜层的深度(也可以纵向长度)。如图14所示,采用非线性梯度模型将中心峰位En设置为沿纵向方向(高斯模型对应的实体膜层的纵向方向或者厚度方向)不均匀变化的20个梯度台阶,台阶走向为先降后升,获得非线性梯度变化的中心峰位。For example: Figure 14 shows a schematic diagram of the center peak position distribution of nonlinear gradient changes. The ordinate is the center peak position En, and the abscissa is the depth of the solid film layer corresponding to the Gaussian model (it can also be the longitudinal length). As shown in Figure 14, the nonlinear gradient model is used to set the central peak position En to 20 gradient steps that vary unevenly along the longitudinal direction (the longitudinal direction or thickness direction of the physical film layer corresponding to the Gaussian model). The direction of the steps is to decrease first. Then rise to obtain the central peak position of the nonlinear gradient change.

第四步,然后利用高斯模型采用反演计算的方式对非线性梯度变化的中心峰位进行曲线拟合,拟合的MSE值为6;其中,在进行曲线拟合的过程中,所拟合出的曲线为如图12中细实线所示的AZO薄膜的椭偏Δ光谱拟合曲线和如图13中细实线所示的AZO薄膜的椭偏Ψ光谱拟合曲线。在拟合成功时,将所获得的AZO薄膜的椭偏Δ光谱拟合曲线和AZO薄膜的椭偏Δ光谱拟合曲线进行变换,获得如图14所示的AZO薄膜的折射率和消光系数在被测样品纵向方向上的变化曲线的相关信息,当然也可以获得如图15所示的AZO薄膜顶部与底部的介电常数随光子能量的变化曲线的相关信息。The fourth step is to use the Gaussian model to perform curve fitting on the central peak position of the nonlinear gradient change using inversion calculation. The fitted MSE value is 6; among them, during the curve fitting process, the fitted The curves shown are the ellipsometry Δ spectrum fitting curve of the AZO film shown in the thin solid line in Figure 12 and the ellipsometry Ψ spectrum fitting curve of the AZO film shown in the thin solid line in Figure 13. When the fitting is successful, the obtained ellipsometry Δ spectrum fitting curve of the AZO film and the ellipsometry Δ spectrum fitting curve of the AZO film are transformed to obtain the refractive index and extinction coefficient of the AZO film as shown in Figure 14. Information related to the change curve in the longitudinal direction of the tested sample can also be obtained, of course, as shown in Figure 15, related information about the change curve of the dielectric constant with photon energy at the top and bottom of the AZO film.

图12和图13中a、b代表线偏振光的入射角度,a=55°,b=65°;将图12中粗虚线所示的AZO薄膜的椭偏Δ光谱实测曲线和细实线所示的AZO薄膜的椭偏Δ光谱拟合曲线进行对比可以发现:根据所建立的高斯模型以及设置的非线性梯度变化的变量参数,得到AZO薄膜的椭偏Δ光谱拟合曲线与AZO薄膜的椭偏Δ光谱实测曲线相吻合,且AZO薄膜的椭偏Δ光谱实测曲线满足K-K关系,说明采用高斯模型对非线性梯度变化的中心峰位进行拟合的拟合结果很好。将图13中粗虚线所示的AZO薄膜的椭偏Ψ光谱实测曲线和细实线所示的AZO薄膜的椭偏Ψ光谱拟合曲线进行对比可以发现:根据所建立的高斯模型以及设置的非线性梯度变化的变量参数,得到AZO薄膜的椭偏Ψ光谱拟合曲线与AZO薄膜的椭偏Ψ光谱实测曲线相吻合,且AZO薄膜的椭偏Ψ光谱实测曲线满足K-K关系,说明采用高斯模型对非线性梯度变化的中心峰位进行拟合的拟合结果很好。此时,可将如图15所示的AZO薄膜的折射率和消光系数在被测样品纵向方向上的变化曲线信息输出,当然也可以选择如图16所示的AZO薄膜顶部与底部的介电常数随光子能量的变化曲线输出,所输出的图15和图16可通过显示模组显示,以方便数据分析。In Figures 12 and 13, a and b represent the incident angles of linearly polarized light, a = 55°, b = 65°; the measured ellipsometric Δ spectrum curve of the AZO film shown in the thick dotted line in Figure 12 and the thin solid line are Comparing the ellipsometry Δ spectrum fitting curve of the AZO film shown below, it can be found that: according to the established Gaussian model and the set nonlinear gradient variable parameters, the ellipse Δ spectrum fitting curve of the AZO film and the ellipsoid ellipse spectrum fitting curve of the AZO film are obtained. The measured curves of the elliptical Δ spectrum are consistent with each other, and the measured curve of the elliptical Δ spectrum of the AZO film satisfies the K-K relationship, indicating that the Gaussian model is used to fit the center peak position of the nonlinear gradient change well. Comparing the measured ellipsometry Ψ spectrum curve of the AZO film shown in the thick dotted line in Figure 13 with the ellipsometry Ψ spectrum fitting curve of the AZO film shown in the thin solid line, it can be found that: according to the established Gaussian model and the set non-linear By using linear gradient variable parameters, the fitting curve of the ellipsometry Ψ spectrum of the AZO film is consistent with the measured ellipsometry Ψ spectrum curve of the AZO film, and the measured ellipsometry Ψ spectrum curve of the AZO film satisfies the K-K relationship, indicating that the Gaussian model is used to The fitting result of fitting the central peak position of the nonlinear gradient change is very good. At this time, the change curve information of the refractive index and extinction coefficient of the AZO film in the longitudinal direction of the tested sample can be output as shown in Figure 15. Of course, you can also choose the dielectric at the top and bottom of the AZO film as shown in Figure 16. The constant changes with photon energy are output as a curve, and the output Figures 15 and 16 can be displayed through the display module to facilitate data analysis.

第五步,图15中示出的上折射率是指AZO薄膜相对粗糙层的表面(下文简称AZO薄膜的顶部)的折射率,下折射率是指AZO薄膜相对基体层的表面(下文简称AZO薄膜的底部)的折射率,可利用下折射率代表AZO薄膜的内部折射率;上消光系数是指AZO薄膜顶部的消光系数,下消光系数是指AZO薄膜底部的消光系数,可利用下消光系数代表AZO薄膜的内部消光系数。由图15可以看出:对于折射率来说,AZO薄膜的顶部折射率大于AZO薄膜的底部(内部)折射率,且差别随波长无变化。对于消光系数来说,在短波长的范围内,AZO薄膜的顶部消光系数与AZO薄膜的底部(内部)消光系数相同;在长波长的范围内,AZO薄膜的顶部消光系数大于AZO薄膜的底部(内部)的消光系数,因此,可以根据图15可以确定AZO薄膜的折射率与消光系数同时沿AZO薄膜纵向方向的变化,而AZO薄膜的折射率与消光系数同时随纵向方向的变化时,确定ITO薄膜的氧含量随AZO薄膜纵向方向不均匀。In the fifth step, the upper refractive index shown in Figure 15 refers to the refractive index of the surface of the AZO film relative to the rough layer (hereinafter referred to as the top of the AZO film), and the lower refractive index refers to the surface of the AZO film relative to the base layer (hereinafter referred to as AZO The refractive index of the bottom of the film), the lower refractive index can be used to represent the internal refractive index of the AZO film; the upper extinction coefficient refers to the extinction coefficient at the top of the AZO film, and the lower extinction coefficient refers to the extinction coefficient at the bottom of the AZO film, the lower extinction coefficient can be used Represents the internal extinction coefficient of AZO film. It can be seen from Figure 15 that for the refractive index, the refractive index of the top of the AZO film is greater than the bottom (inner) refractive index of the AZO film, and the difference does not change with wavelength. Regarding the extinction coefficient, in the short wavelength range, the top extinction coefficient of the AZO film is the same as the bottom (internal) extinction coefficient of the AZO film; in the long wavelength range, the top extinction coefficient of the AZO film is greater than the bottom of the AZO film ( Therefore, according to Figure 15, it can be determined that the refractive index and extinction coefficient of the AZO film change along the longitudinal direction of the AZO film at the same time, and when the refractive index and extinction coefficient of the AZO film change along the longitudinal direction at the same time, ITO can be determined The oxygen content of the film is not uniform along the longitudinal direction of the AZO film.

图16中示出的上ε1为AZO薄膜相对粗糙层的表面(下文简称为AZO薄膜的顶部)的实部,下ε1为AZO薄膜相对基体层的表面(下文简称为AZO薄膜的底部的实部;上ε2为ITO薄膜相对基体层的表面(下文简称为AZO薄膜的顶部)的实部,下ε2为AZO薄膜相对基体层的表面(下文简称为AZO薄膜的底部)的实部。由图16可以看出,AZO薄膜的顶部介电常数的实部ε1与虚部ε2均大于AZO薄膜的底部介电常数的实部ε1与虚部ε2,因此,可以根据图16确定AZO薄膜的介电常数沿AZO薄膜的纵向变化;而当AZO薄膜的介电常数沿AZO薄膜的纵向变化时,确定AZO薄膜的氧含量随AZO薄膜纵向方向不均匀。The upper ε1 shown in Figure 16 is the real part of the surface of the AZO film relative to the rough layer (hereinafter referred to as the top of the AZO film), and the lower ε1 is the surface of the AZO film relative to the base layer (hereinafter referred to as the bottom of the AZO film). Real part; the upper ε2 is the real part of the surface of the ITO film relative to the base layer (hereinafter referred to as the top of the AZO film), and the lower ε2 is the real part of the surface of the AZO film relative to the base layer (hereinafter referred to as the bottom of the AZO film) . It can be seen from Figure 16 that the real part ε1 and imaginary part ε2 of the dielectric constant at the top of the AZO film are both larger than the real part ε1 and imaginary part ε2 of the dielectric constant at the bottom of the AZO film. Therefore, according to the figure 16 It is determined that the dielectric constant of the AZO film changes along the longitudinal direction of the AZO film; and when the dielectric constant of the AZO film changes along the longitudinal direction of the AZO film, it is determined that the oxygen content of the AZO film is not uniform along the longitudinal direction of the AZO film.

以上所述,仅为本发明的具体实施方式,但本发明的保护范围并不局限于此,任何熟悉本技术领域的技术人员在本发明揭露的技术范围内,可轻易想到变化或替换,都应涵盖在本发明的保护范围之内。因此,本发明的保护范围应以所述权利要求的保护范围为准。The above are only specific embodiments of the present invention, but the protection scope of the present invention is not limited thereto. Any person familiar with the technical field can easily think of changes or substitutions within the technical scope disclosed by the present invention. should be covered by the protection scope of the present invention. Therefore, the protection scope of the present invention should be subject to the protection scope of the claims.

Claims (14)

Translated fromChinese
1.一种薄膜纵向不均匀性检测方法,其特征在于,包括:1. A method for detecting longitudinal non-uniformity of a film, which is characterized by including:获取被测样品的椭偏光谱曲线信息,所述被测样品至少包括被测薄膜;Obtain ellipsometric spectral curve information of the sample being tested, which sample at least includes the film being tested;根据所述被测样品的特性建立各向同性的物理模型,所述物理模型至少包括薄膜模型;Establish an isotropic physical model according to the characteristics of the measured sample, and the physical model at least includes a thin film model;将所述薄膜模型所含有的至少一个变量参数转换为至少一组梯度化变量参数;Convert at least one variable parameter contained in the film model into at least one set of gradient variable parameters;以所述被测样品的椭偏光谱曲线信息为曲线拟合目标,利用所述薄膜模型对至少一组梯度化变量参数进行曲线拟合,获得被测样品的光电参数在被测样品纵向方向上的变化曲线信息;Using the ellipsometric spectral curve information of the tested sample as a curve fitting target, the film model is used to perform curve fitting on at least one set of gradient variable parameters to obtain the photoelectric parameters of the tested sample in the longitudinal direction of the tested sample. change curve information;根据所述被测样品的光电参数在被测样品纵向方向上的变化曲线信息确定被测样品的纵向不均匀性;Determine the longitudinal non-uniformity of the tested sample based on the change curve information of the photoelectric parameters of the tested sample in the longitudinal direction of the tested sample;其中,通过表达所述至少一个变量参数沿膜层深度变化的梯度函数的方式将所述至少一个变量参数转换为至少一组梯度化变量参数。Wherein, the at least one variable parameter is converted into at least one set of gradient variable parameters by expressing a gradient function in which the at least one variable parameter changes along the depth of the film layer.2.根据权利要求1所述的薄膜纵向不均匀性检测方法,其特征在于,所述进行曲线拟合的收敛条件为均方误差值小于80。2. The film longitudinal non-uniformity detection method according to claim 1, characterized in that the convergence condition for curve fitting is that the mean square error value is less than 80.3.根据权利要求1所述的薄膜纵向不均匀性检测方法,其特征在于,所述进行曲线拟合的收敛条件为均方误差值小于20。3. The film longitudinal non-uniformity detection method according to claim 1, characterized in that the convergence condition for curve fitting is that the mean square error value is less than 20.4.根据权利要求1所述的薄膜纵向不均匀性检测方法,其特征在于,所述被测样品的光电参数包括满足克莱默-克朗尼格关系的光学常数和/或满足克莱默-克朗尼格关系的介电常数。4. The film longitudinal non-uniformity detection method according to claim 1, characterized in that the photoelectric parameters of the measured sample include optical constants that satisfy the Kramer-Kronig relationship and/or satisfy the Kramer-Kronig relationship. Kroniger relation for dielectric constant.5.根据权利要求1所述的薄膜纵向不均匀性检测方法,其特征在于,所述物理模型还包括基体模型和表面模型,所述薄膜模型位于所述基体模型和所述表面模型之间,所述基体模型为柯西模型,所述薄膜模型为洛伦兹模型或高斯模型,所述表面模型为有效介质模型。5. The film longitudinal non-uniformity detection method according to claim 1, characterized in that the physical model further includes a matrix model and a surface model, and the film model is located between the matrix model and the surface model, The matrix model is a Cauchy model, the film model is a Lorentz model or a Gaussian model, and the surface model is an effective medium model.6.根据权利要求1~5任一项所述的薄膜纵向不均匀性检测方法,其特征在于,所述将所述薄膜模型所含有的至少一个变量参数转换为至少一组梯度化变量参数包括:6. The film longitudinal non-uniformity detection method according to any one of claims 1 to 5, characterized in that said converting at least one variable parameter contained in the film model into at least one set of gradient variable parameters includes :按照对拟合结果影响权重由高到低的顺序,选择薄膜模型中的一个或两个变量参数进行梯度化转换;Select one or two variable parameters in the film model for gradient conversion in order of their impact on the fitting results from high to low;和/或,and / or,所述梯度化变量参数包括线性梯度变化的变量参数或非线性梯度变化的变量参数。The gradient variable parameters include variable parameters with linear gradient changes or variable parameters with nonlinear gradient changes.7.一种薄膜纵向不均匀性检测装置,其特征在于,包括:7. A film longitudinal non-uniformity detection device, characterized in that it includes:接收单元,用于获取被测样品的椭偏光谱曲线信息,所述被测样品至少包括被测薄膜;A receiving unit, configured to obtain ellipsometric spectral curve information of the sample being tested, where the sample being tested at least includes the film being tested;模型化单元,用于根据所述被测样品的特性建立各向同性的物理模型,所述物理模型包括至少包括薄膜模型;将所述薄膜模型所含有的至少一个变量参数转换为至少一组梯度化变量参数;其中,通过表达所述至少一个变量参数沿膜层深度变化的梯度函数的方式将所述至少一个变量参数转换为至少一组梯度化变量参数;A modeling unit, configured to establish an isotropic physical model according to the characteristics of the measured sample, the physical model including at least a film model; convert at least one variable parameter contained in the film model into at least a set of gradients variable parameters; wherein, the at least one variable parameter is converted into at least one set of gradient variable parameters by expressing the gradient function of the change of the at least one variable parameter along the depth of the film layer;曲线拟合单元,用于以所述被测样品的椭偏光谱曲线信息为曲线拟合目标,利用所述薄膜模型对至少一组梯度化变量参数进行曲线拟合,获得被测样品的光电参数在被测样品纵向方向上的变化曲线信息;A curve fitting unit, configured to use the ellipsometric spectrum curve information of the tested sample as a curve fitting target, use the film model to perform curve fitting on at least one set of gradient variable parameters, and obtain the photoelectric parameters of the tested sample. Change curve information in the longitudinal direction of the tested sample;分析单元,用于根据所述被测样品的光电参数在被测样品纵向方向上的变化曲线信息评价被测样品的纵向不均匀性。An analysis unit is used to evaluate the longitudinal non-uniformity of the tested sample based on the change curve information of the photoelectric parameters of the tested sample in the longitudinal direction of the tested sample.8.根据权利要求7所述的薄膜纵向不均匀性检测装置,其特征在于,所述进行曲线拟合的收敛条件为均方根误差值小于80;8. The film longitudinal non-uniformity detection device according to claim 7, characterized in that the convergence condition for curve fitting is that the root mean square error value is less than 80;和/或,and / or,所述被测样品的光电参数包括满足克莱默-克朗尼格关系的光学常数和/或满足克莱默-克朗尼格关系的介电常数;The photoelectric parameters of the measured sample include optical constants that satisfy the Kramer-Kronig relationship and/or dielectric constants that satisfy the Kramer-Kronig relationship;和/或,and / or,所述物理模型还包括基体模型和表面模型,所述薄膜模型位于所述基体模型和所述表面模型之间,所述基体模型为柯西模型,所述薄膜模型为洛伦兹模型或高斯模型,所述表面模型为有效介质模型;The physical model also includes a matrix model and a surface model. The film model is located between the matrix model and the surface model. The matrix model is a Cauchy model, and the film model is a Lorentz model or a Gaussian model. , the surface model is an effective medium model;和/或,and / or,所述将所述薄膜模型所含有的至少一个变量参数转换为至少一组梯度化变量参数包括:Converting at least one variable parameter contained in the film model into at least one set of gradient variable parameters includes:按照对拟合结果影响权重由高到低的顺序,选择薄膜模型中的一个或两个变量参数进行梯度化转换;Select one or two variable parameters in the film model for gradient conversion in order of their impact on the fitting results from high to low;和/或,and / or,所述梯度化变量参数包括线性梯度变化的变量参数或非线性梯度变化的变量参数。The gradient variable parameters include variable parameters with linear gradient changes or variable parameters with nonlinear gradient changes.9.根据权利要求7所述的薄膜纵向不均匀性检测装置,其特征在于,所述进行曲线拟合的收敛条件为均方根误差值小于20。9. The film longitudinal non-uniformity detection device according to claim 7, characterized in that the convergence condition for curve fitting is that the root mean square error value is less than 20.10.一种薄膜纵向不均匀性检测方法,其特征在于,包括:10. A method for detecting longitudinal non-uniformity of a film, which is characterized by including:测量被测样品的椭偏光谱曲线;Measure the ellipsometric spectral curve of the sample being tested;将被测样品的椭偏光谱曲线信息发送给如权利要求7~9任一项所述的薄膜纵向不均匀性检测装置;所述被测样品的椭偏光谱曲线信息表征所述被测样品的椭偏光谱曲线;The ellipsometric spectral curve information of the tested sample is sent to the film longitudinal non-uniformity detection device according to any one of claims 7 to 9; the ellipsometric spectral curve information of the tested sample represents the ellipsometric spectral curve information of the tested sample. Ellipsometric spectral curve;利用所述薄膜纵向不均匀性检测装置确定被测样品的纵向不均匀性。The longitudinal unevenness of the measured sample is determined using the film longitudinal unevenness detection device.11.根据权利要求10所述的薄膜纵向不均匀性检测方法,其特征在于,所述测量被测样品的椭偏光谱曲线包括:11. The film longitudinal non-uniformity detection method according to claim 10, characterized in that measuring the ellipsometric spectral curve of the tested sample includes:设定线偏振光的入射角度,使得所述线偏振光的入射角度包括至少一个第一入射角度和至少一个第二入射角度,每个所述第一入射角度大于被测样品材料的布儒斯特角,每个所述第二入射角度小于被测样品材料的布儒斯特角;The incident angle of the linearly polarized light is set so that the incident angle of the linearly polarized light includes at least one first incident angle and at least one second incident angle, and each of the first incident angles is greater than the Brucella of the tested sample material. special angle, each of the second incident angles is smaller than the Brewster angle of the sample material being tested;分别在至少一个第一入射角度和至少一个第二入射角度下,向被测样品入射线偏振光,检测被测样品的椭圆偏振p光与s光的振幅比和被测样品的椭圆偏振p光与s光的相位差;Under at least one first incident angle and at least one second incident angle, linearly polarized light is incident on the sample to be measured, and the amplitude ratio of the elliptically polarized p-light and s-light of the sample to be measured and the elliptically polarized p-light of the sample to be measured are detected Phase difference with s light;根据所述被测样品的椭圆偏振p光与s光的振幅比和线偏振光的波长范围,获得被测样品的椭偏振幅比光谱曲线;According to the amplitude ratio of the elliptically polarized p-light and s-light of the tested sample and the wavelength range of the linearly polarized light, the elliptical polarization amplitude ratio spectral curve of the tested sample is obtained;根据所述被测样品的椭圆偏振p光与s光的相位差和线偏振光的波长范围,获得被测样品的椭偏相位差光谱曲线。According to the phase difference between the elliptically polarized p-light and the s-light of the tested sample and the wavelength range of the linearly polarized light, the elliptical phase difference spectrum curve of the tested sample is obtained.12.根据权利要求11所述的薄膜纵向不均匀性检测方法,其特征在于,所述线偏振光的波长范围为300nm-2400nm。12. The film longitudinal non-uniformity detection method according to claim 11, characterized in that the wavelength range of the linearly polarized light is 300nm-2400nm.13.一种检测系统,其特征在于,包括:13. A detection system, characterized in that it includes:椭偏光谱仪;spectroscopic ellipsometry;如权利要求7~9任一项所述的薄膜纵向不均匀性检测装置,所述薄膜纵向不均匀性检测装置所包括的接收器与所述椭偏光谱仪连接。The film longitudinal unevenness detection device according to any one of claims 7 to 9, wherein the film longitudinal unevenness detection device includes a receiver connected to the ellipsometer.14.一种薄膜纵向不均匀性检测终端,其特征在于,包括:14. A film longitudinal non-uniformity detection terminal, characterized in that it includes:存储器,用于储存一个或多个计算机软件指令,其包含用于执行权利要求1~6任一项所述的薄膜纵向不均匀性检测方法所涉及的程序;A memory used to store one or more computer software instructions, which includes programs for executing the film longitudinal non-uniformity detection method according to any one of claims 1 to 6;处理器,用于执行一个或多个计算机软件指令,以实现权利要求1~6任一项所述的薄膜纵向不均匀性检测方法。A processor, configured to execute one or more computer software instructions to implement the film longitudinal non-uniformity detection method described in any one of claims 1 to 6.
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