CN102556950A - Tunable artificial electromagnetic material based on three-layer structure and manufacturing method thereof - Google Patents

Abstract

Translated fromChinese

本发明涉及一种基于三层结构的可调谐人工电磁材料及其制作方法，该人工电磁材料是由金属-掺杂介质-金属三层结构组成的微纳米图形结构，可用于红外、太赫兹波段。其制作方法包括：选择绝缘硅，利用沉积、粘结、干法刻蚀、湿法腐蚀、再沉积的技术，在基片上获得金属-掺杂介质-金属的三层结构；在三层结构之上进行光刻，获得光刻胶图形；利用离子束刻蚀将光刻胶图形转移到金属膜层上，即可获得基于金属-掺杂介质-金属三层结构的人工电磁材料。本发明的制作方法避免了常规方法如溅射、离子注入、键合等方法制备掺杂硅带来的掺杂难、掺杂不均、掺杂层厚度难控制等缺点，工艺简单，易于控制，是人工电磁材料的一种高效可靠的制作方法。

The invention relates to a tunable artificial electromagnetic material based on a three-layer structure and a manufacturing method thereof. The artificial electromagnetic material is a micro-nano pattern structure composed of a metal-doped medium-metal three-layer structure, and can be used in infrared and terahertz bands. . The production method includes: selecting insulating silicon, and using deposition, bonding, dry etching, wet etching, and redeposition techniques to obtain a three-layer structure of metal-doped medium-metal on the substrate; Photolithography is carried out on the surface to obtain a photoresist pattern; the photoresist pattern is transferred to the metal film layer by ion beam etching, and an artificial electromagnetic material based on a metal-doped medium-metal three-layer structure can be obtained. The production method of the present invention avoids the disadvantages of difficult doping, uneven doping, and difficulty in controlling the thickness of the doped layer caused by conventional methods such as sputtering, ion implantation, and bonding to prepare doped silicon, and the process is simple and easy to control. , is an efficient and reliable manufacturing method of artificial electromagnetic materials.

Description

Translated fromChinese

一种基于三层结构的可调谐人工电磁材料及其制作方法A tunable artificial electromagnetic material based on a three-layer structure and its manufacturing method

技术领域technical field

本发明属于微纳光学元件制作及微纳加工技术领域，特别涉及一种基于三层结构的可调谐人工电磁材料及其制作方法，用于红外、太赫兹波段的人工电磁材料及其制备。The invention belongs to the technical field of micro-nano optical element production and micro-nano processing, and in particular relates to a tunable artificial electromagnetic material based on a three-layer structure and a production method thereof, which are used in infrared and terahertz bands and its preparation.

背景技术Background technique

人工电磁材料是指在自然界中本身并不存在或者没有被发现，而是由电磁学理论的推导计算设计并制作出来的，具有非常规的电磁属性的人造媒质或材料。人工电磁材料通常是由有共振响应的亚波长结构单元周期性排列(或者非周期)而成。由于其结构单元一般比对应的波长小一个数量级以上，应此整体结构对于外界电磁场的响应可以看成是一个平均的效果，所以其整体的电磁特性可以通过等效介电常数和磁导率来描述。这些材料的等效介电常数和磁导率可以接近零甚至为负值，表现出奇异的电磁特性。利用这些奇异的特性，可以实现平板聚焦、完美透镜、超薄谐振腔等功能，在微波和光学领域有着广泛的应用价值，在军事和日常生活中能够发挥重要的作用。因此，近年来人工电磁材料已经成为国际上一个重要的研究热点。Artificial electromagnetic materials refer to artificial media or materials with unconventional electromagnetic properties that do not exist or have not been discovered in nature, but are designed and produced by derivation and calculation of electromagnetic theory. Artificial electromagnetic materials are usually made of periodic (or non-periodic) arrangements of subwavelength structural units with resonance responses. Since its structural unit is generally smaller than the corresponding wavelength by more than an order of magnitude, the response of the overall structure to the external electromagnetic field can be regarded as an average effect, so its overall electromagnetic characteristics can be calculated by the equivalent dielectric constant and magnetic permeability. describe. The equivalent permittivity and permeability of these materials can be close to zero or even negative, showing strange electromagnetic properties. Using these singular characteristics, functions such as flat-plate focusing, perfect lens, and ultra-thin resonant cavity can be realized. It has a wide range of application values in the microwave and optical fields, and can play an important role in military affairs and daily life. Therefore, artificial electromagnetic materials have become an important research hotspot in the world in recent years.

人工电磁材料的结构有多种，但多数结构较为复杂。当人工电磁材料的适用波段为微波时，加工较为容易，而当适用波段为红外甚至可见光时，材料的加工就十分困难。金属线对是目前设计人工电磁材料的一种基础单元结构，金属线对的设计有狭缝结构，该狭缝不会破坏原有金属线对结构的磁响应特性，而且能够在原有磁谐振的基础上引入额外的电谐振，使电谐振和磁谐振在同一单元结构中得到共同调制。其结构较为简单，易于加工制作，受到了广泛的关注。There are many structures of artificial electromagnetic materials, but most of them are complex. When the applicable waveband of artificial electromagnetic materials is microwave, the processing is relatively easy, but when the applicable waveband is infrared or even visible light, the processing of materials is very difficult. The metal wire pair is a basic unit structure for designing artificial electromagnetic materials at present. The metal wire pair is designed with a slit structure. The slit will not destroy the magnetic response characteristics of the original metal wire pair structure, and can Based on the introduction of additional electric resonance, the electric resonance and magnetic resonance are co-modulated in the same unit structure. Its structure is relatively simple, easy to process and manufacture, and has received extensive attention.

此类人工电磁材料的制备常涉及到金属/介质/金属三层结构的膜层制备，其中介质通常为非晶硅，二氧化硅，氮化硅，氟化镁，三氧化二铝等。如制备可见光波段的人工电磁材料的结构膜层通常为Ag/Al₂O₃/Ag；制备近红外波段的人工电磁材料的结构膜层通常为Au/MgF₂/Au。利用真空蒸镀或磁控溅射的方法能够实现这些膜层的制备。而根据人工电磁材料的设计要求，可能要满足一些特殊三层结构的介质层制备，如类似金属/高浓度均匀掺杂硅/金属的结构，此时便无法通过蒸镀或溅射的方法来制作高浓度均匀掺杂硅。因为该介质层的掺杂浓度和均匀性都无法在镀膜过程中控制。其他的方法如离子注入法是硅掺杂的常用方法，但是该方法也不能控制纵向的掺杂均匀性；若采用分子束外延法和键合法又受限于该介质层下的金属层。因此需要提出一种用于制作金属/高浓度均匀掺杂硅/金属三层结构的新方法。The preparation of such artificial electromagnetic materials often involves the preparation of a metal/dielectric/metal three-layer structure, in which the dielectric is usually amorphous silicon, silicon dioxide, silicon nitride, magnesium fluoride, aluminum oxide, etc. For example, the structural film layer for preparing artificial electromagnetic materials in the visible light band is usually Ag/Al₂ O₃ /Ag; the structural film layer for preparing artificial electromagnetic materials in the near-infrared band is usually Au/MgF₂ /Au. These films can be prepared by vacuum evaporation or magnetron sputtering. According to the design requirements of artificial electromagnetic materials, it may be necessary to meet the preparation of some special three-layer dielectric layers, such as metal-like/high-concentration uniformly doped silicon/metal structures. At this time, evaporation or sputtering cannot be used. Fabrication of high-concentration uniformly doped silicon. Because the doping concentration and uniformity of the dielectric layer cannot be controlled during the coating process. Other methods such as ion implantation are common methods for silicon doping, but this method cannot control the vertical doping uniformity; if molecular beam epitaxy and bonding are used, they are limited to the metal layer under the dielectric layer. Therefore, it is necessary to propose a new method for fabricating a metal/high-concentration uniformly doped silicon/metal three-layer structure.

发明内容Contents of the invention

本发明要解决的技术问题是：针对现有人工电磁材料的复杂结构设计，提出一种基于金属-掺杂介质-金属的开口金属线对的阵列结构，实现介电常数和磁导率同时调制的作用；并对于现有高浓度均匀掺杂介质制备技术的局限性，提出一种制备金属-掺杂介质-金属的三层结构的方法，并基于该三层结构制备红外、太赫兹波段的人工电磁材料。The technical problem to be solved by the present invention is: aiming at the complex structure design of existing artificial electromagnetic materials, an array structure of open metal wire pairs based on metal-doped medium-metal is proposed to realize simultaneous modulation of permittivity and permeability and for the limitations of the existing high-concentration uniformly doped medium preparation technology, a method for preparing a three-layer structure of metal-doped medium-metal is proposed, and based on the three-layer structure to prepare infrared and terahertz bands Artificial electromagnetic materials.

本发明解决其技术问题所采用的技术方案是：The technical solution adopted by the present invention to solve its technical problems is:

一种基于三层结构的可调谐人工电磁材料制作方法，步骤如下：A method for manufacturing a tunable artificial electromagnetic material based on a three-layer structure, the steps are as follows:

步骤(1)选取合适的双面抛光的SOI片，清洗干净，并在SOI片顶层的掺杂硅表面沉积一层金属膜；Step (1) select a suitable double-sided polished SOI sheet, clean it, and deposit a layer of metal film on the doped silicon surface of the top layer of the SOI sheet;

步骤(2)另取单面抛光的硅片，在抛光表面涂覆一层粘结剂；Step (2) take another silicon wafer polished on one side, and coat a layer of adhesive on the polished surface;

步骤(3)利用粘连剂将沉积有金属膜的SOI片与硅片粘结，并将粘结好的硅片-SOI片进行烘烤固化；Step (3) bonding the SOI sheet deposited with the metal film to the silicon sheet with an adhesive, and baking and curing the bonded silicon sheet-SOI sheet;

步骤(4)利用干法刻蚀将硅片-SOI片结构中SOI片的底层单晶硅进行刻蚀减薄；Step (4) using dry etching to etch and thin the bottom single crystal silicon of the SOI sheet in the silicon wafer-SOI sheet structure;

步骤(5)采用氢氧化钾湿法腐蚀，将硅片-SOI片结构中SOI片上剩余的底层单晶硅腐蚀完毕，使SOI片的二氧化硅中间层露出；Step (5) using potassium hydroxide wet etching to etch the remaining bottom single crystal silicon on the SOI sheet in the silicon wafer-SOI sheet structure, so that the silicon dioxide intermediate layer of the SOI sheet is exposed;

步骤(6)采用氢氟酸湿法腐蚀，将硅片-SOI片结构中SOI片的二氧化硅中间层腐蚀完毕，露出掺杂硅表面；Step (6) using hydrofluoric acid wet etching to etch the silicon dioxide intermediate layer of the SOI sheet in the silicon wafer-SOI sheet structure to expose the doped silicon surface;

步骤(7)在步骤(6)中的掺杂硅表面沉积一层金属膜，从而在硅片上形成金属-掺杂介质-金属的三层结构；Step (7) depositing a layer of metal film on the doped silicon surface in step (6), thereby forming a three-layer structure of metal-doped medium-metal on the silicon wafer;

步骤(8)在所得金属-掺杂介质-金属三层结构上涂覆光刻胶，并在烘箱或热板中进行前烘；Step (8) Coating a photoresist on the obtained metal-doped medium-metal three-layer structure, and pre-baking in an oven or a hot plate;

步骤(9)利用光刻设备对基片进行曝光，在光刻胶上获得所设计的二维周期性阵列微纳结构图形，并置于烘箱或热板中进行坚膜；Step (9) Exposing the substrate with photolithography equipment, obtaining the designed two-dimensional periodic array micro-nano structure pattern on the photoresist, and placing it in an oven or a hot plate to harden the film;

步骤(10)采用干法刻蚀将步骤(9)中的光刻胶图形转移至金属-掺杂介质-金属三层结构中的上层金属；Step (10) using dry etching to transfer the photoresist pattern in step (9) to the upper metal in the metal-doped medium-metal three-layer structure;

步骤(11)用有机溶剂浸泡刻蚀后的样品，将刻蚀后剩余的光刻胶去除，即可获得基于金属-掺杂介质-金属三层结构的可调谐人工电磁材料。Step (11) Soak the etched sample with an organic solvent, remove the remaining photoresist after etching, and obtain a tunable artificial electromagnetic material based on a metal-doped medium-metal three-layer structure.

所述步骤(1)的SOI片是由底层单晶硅、中间层二氧化硅、顶层掺杂硅组成，底层厚度为300～450μm，中间层厚度为100～300nm，顶层是厚度为0.5～1.5μm的高浓度均匀掺杂的N型硅或P型硅，掺杂浓度为10¹⁸～10²⁰cm^-1；The SOI sheet in the step (1) is composed of bottom single crystal silicon, middle layer silicon dioxide and top layer doped silicon, the bottom layer has a thickness of 300-450 μm, the middle layer has a thickness of 100-300 nm, and the top layer has a thickness of 0.5-1.5 nm. N-type silicon or P-type silicon uniformly doped with a high concentration of μm, the doping concentration is 10¹⁸ ~ 10²⁰ cm^-1 ;

所述步骤(1)的沉积方法可以为磁控溅射法、蒸镀法；The deposition method of described step (1) can be magnetron sputtering method, evaporation method;

所述步骤(1)中的金属膜可以为金、铜、银，金属膜厚度为100～200nm；The metal film in the step (1) can be gold, copper, silver, and the thickness of the metal film is 100-200nm;

所述步骤(2)中的粘结剂是一种耐高温、耐强酸强碱及有机溶剂的胶；The binding agent in the described step (2) is a kind of glue resistant to high temperature, strong acid and strong alkali and organic solvent;

所述步骤(3)中的粘结方式是将SOI的金属膜层与旋涂有粘结剂的硅片相粘连；The bonding method in the step (3) is to bond the metal film layer of SOI with the silicon chip that is spin-coated with adhesive;

所述步骤(3)中的烘烤设备可以为烘箱和热板，温度范围为100～120℃，烘烤时间为5～10min；The baking equipment in the step (3) can be an oven and a hot plate, the temperature range is 100-120° C., and the baking time is 5-10 minutes;

所述步骤(4)中的干法刻蚀可以为电感耦合等离子刻蚀、等离子刻蚀、离子束刻蚀；The dry etching in the step (4) can be inductively coupled plasma etching, plasma etching, ion beam etching;

所述步骤(4)中的SOI片的底层单晶硅减薄后的厚度为20～50μm；The thinned bottom single crystal silicon of the SOI sheet in the step (4) has a thickness of 20-50 μm;

所述步骤(7)中沉积方法可以为磁控溅射法、蒸镀法；Deposition method in described step (7) can be magnetron sputtering method, evaporation method;

所述步骤(7)中沉积金属膜可以为金、铜、银，金属膜厚度为40～60nm；The metal film deposited in the step (7) can be gold, copper, silver, and the thickness of the metal film is 40-60nm;

所述步骤(8)中光刻胶的厚度为100～200nm，前烘温度范围为100～120℃，烘烤时间为20～30min；In the step (8), the thickness of the photoresist is 100-200nm, the pre-baking temperature range is 100-120°C, and the baking time is 20-30min;

所述步骤(9)中的光刻设备可以为接近接触式光刻机、投影式光刻机、电子束直写曝光机；The lithography equipment in the step (9) can be a near-contact lithography machine, a projection lithography machine, an electron beam direct writing exposure machine;

所述步骤(9)中的二维周期性阵列微纳结构图形的线宽可以为0.3～60μm，周期可以为12～160μm；The line width of the two-dimensional periodic array micro-nano structure pattern in the step (9) may be 0.3-60 μm, and the period may be 12-160 μm;

所述步骤(9)中的坚膜温度为：100～120℃，坚膜时间为：20～30min；The hardening temperature in the step (9) is: 100-120°C, and the hardening time is: 20-30min;

所述步骤(10)中的干法刻蚀可以为等离子刻蚀、离子束刻蚀、电感耦合等离子刻蚀；The dry etching in the step (10) can be plasma etching, ion beam etching, inductively coupled plasma etching;

所述步骤(10)中的刻蚀深度应该等于金属-掺杂介质-金属三层结构中上层金属层厚度，误差不超过5％；The etching depth in the step (10) should be equal to the thickness of the upper metal layer in the metal-doped medium-metal three-layer structure, and the error should not exceed 5%;

所述步骤(11)中的有机溶剂为可以溶解光刻胶的溶剂。The organic solvent in the step (11) is a solvent that can dissolve the photoresist.

一种基于三层结构的可调谐人工电磁材料，该可调谐人工电磁材料由上述的加工方法制成。A tunable artificial electromagnetic material based on a three-layer structure, which is made by the above-mentioned processing method.

本发明与现有技术相比具有以下优点：Compared with the prior art, the present invention has the following advantages:

本发明基于金属-掺杂介质-金属的三层结构，设计了开口金属线对，将电谐振和磁谐振统一在同一个单元结构中，在实现介电常数调制的同时，将磁导率同时进行调制。并且本发明基于SOI片，利用粘结-干法刻蚀-湿法腐蚀的组合技术获得SOI片中的高浓度均匀掺杂硅，结合镀膜技术实现了基于金属/高浓度均匀掺杂硅/金属三层结构人工电磁材料的制备。避免了采用常规方法如溅射、离子注入、键合等方法制备掺杂硅带来的掺杂难、掺杂不均、掺杂层厚度难控制等缺点。同时该方法的工艺简单，易于控制，是人工电磁材料的一种高效可靠的制作方法。Based on the three-layer structure of metal-doped medium-metal, the invention designs open metal wire pairs, unifies the electric resonance and magnetic resonance in the same unit structure, realizes the modulation of the permittivity, and simultaneously adjusts the magnetic permeability to modulate. And the present invention is based on the SOI sheet, and utilizes the combination technology of bonding-dry etching-wet etching to obtain high-concentration uniformly doped silicon in the SOI sheet, and combines the coating technology to realize the method based on metal/high-concentration uniformly doped silicon/metal Preparation of artificial electromagnetic materials with three-layer structure. It avoids the disadvantages of difficult doping, uneven doping, and difficulty in controlling the thickness of the doped layer caused by the preparation of doped silicon by conventional methods such as sputtering, ion implantation, and bonding. At the same time, the process of the method is simple and easy to control, and is an efficient and reliable manufacturing method of artificial electromagnetic materials.

附图说明Description of drawings

图1是本发明方法的流程图；Fig. 1 is a flow chart of the inventive method;

图2是本发明步骤1中在SOI片的掺杂硅表面沉积金属膜层的结构示意图；Fig. 2 is the schematic structural view of depositing a metal film layer on the doped silicon surface of the SOI sheet instep 1 of the present invention;

图3是本发明步骤3中SOI片与普通硅片粘贴示意图；Fig. 3 is the sticking schematic diagram of SOI chip and common silicon chip instep 3 of the present invention;

图4是本发明步骤6中干法刻蚀硅和湿法腐蚀硅及二氧化硅后的结构示意图；Fig. 4 is the structure diagram after dry etching silicon and wet etching silicon and silicon dioxide instep 6 of the present invention;

图5是本发明步骤7完成后得到的金属/高浓度均匀掺杂硅/金属三层结构示意图；Fig. 5 is a schematic diagram of the metal/high-concentration uniformly doped silicon/metal three-layer structure obtained afterstep 7 of the present invention is completed;

图6是本发明步骤9光刻、显影完毕后的结构示意图；Fig. 6 is a schematic structural view after photolithography and development in Step 9 of the present invention;

图7是本发明步骤11完成后得到的成品结构示意图；Fig. 7 is a schematic diagram of the structure of the finished product obtained after step 11 of the present invention is completed;

图面说明如下：1为SOI片的底层单晶硅；2为SOI片的中间层二氧化硅；3为SOI片的顶层掺杂硅；4为金属膜层；5为粘结剂；6为普通硅片；7为金属膜；8为抗蚀剂。The drawings are described as follows: 1 is the bottom monocrystalline silicon of the SOI sheet; 2 is the middle layer of silicon dioxide of the SOI sheet; 3 is the top layer of the SOI sheet doped with silicon; 4 is the metal film layer; 5 is the adhesive; 6 is Ordinary silicon wafer; 7 is the metal film; 8 is the resist.

具体实施方式：Detailed ways:

下面将参照附图详述金属/高浓度均匀掺杂硅/金属三层结构的制备，附图中给出了本发明方法的示例性实施例，在不同的图中相同的标号表示相同的部分，附图不一定是按比例的，其重点在解释本发明的方法上。但以下的实施例仅限于解释本发明，本发明的保护范围应包括权利要求的全部内容，而且通过以下实施例对本领域的技术人员即可以实现本发明权利要求的全部内容。The preparation of the metal/highly concentrated uniformly doped silicon/metal triple-layer structure will be described in detail below with reference to the accompanying drawings. In the accompanying drawings, an exemplary embodiment of the method of the present invention is provided, and the same reference numerals represent the same parts in different figures. , the drawings are not necessarily to scale, and emphasis is placed on explaining the method of the present invention. But following embodiment only limits to explain the present invention, and protection scope of the present invention should include the whole content of claim, and promptly can realize the whole content of claim of the present invention to those skilled in the art through following embodiment.

实施例1Example 1

本发明的一个典型实施例，是制作铜/高浓度均匀掺杂硅/铜的三层结构，适用的波段为太赫兹波段。其中铜的厚度分别为100nm和50nm，掺杂层的厚度为1μm，掺杂元素是磷，掺杂浓度为10¹⁸cm^-1。A typical embodiment of the present invention is to make a three-layer structure of copper/high-concentration uniformly doped silicon/copper, and the applicable wave band is the terahertz wave band. The thickness of the copper is 100nm and 50nm respectively, the thickness of the doped layer is 1 μm, the doping element is phosphorus, and the doping concentration is 10¹⁸ cm⁻¹ .

该图形的制作流程如图1所示，具体实现步骤如下：The graphic production process is shown in Figure 1, and the specific implementation steps are as follows:

(1)选择尺寸为15mm×15mm的双面抛光SOI片，并用丙酮溶液清洗干净，放置于干净容器里，于烘箱160℃烘烤15min，待其自然冷却。其中底层单晶硅1的厚度为450μm，中间层二氧化硅2的厚度为300nm，顶层高浓度均匀掺杂的N型硅3的厚度为1μm，厚度精度±0.05μm，掺杂磷的浓度为10¹⁸cm^-1。(1) Choose a double-sided polished SOI chip with a size of 15mm×15mm, clean it with acetone solution, place it in a clean container, bake it in an oven at 160°C for 15min, and wait for it to cool naturally. The thickness of the bottomsingle crystal silicon 1 is 450 μm, the thickness of the middle layer ofsilicon dioxide 2 is 300 nm, the thickness of the top layer of high-concentration and uniformly doped N-type silicon 3 is 1 μm, the thickness accuracy is ±0.05 μm, and the concentration of doped phosphorus is 10¹⁸ cm^-1 .

(2)利用磁控溅射镀膜设备，在SOI片的顶层掺杂硅3表面沉积一层厚度为100nm的金属铜4，完成后结构如图2所示。(2) A layer ofmetal copper 4 with a thickness of 100 nm is deposited on the surface of the dopedsilicon 3 on the top layer of the SOI sheet by using magnetron sputtering coating equipment, and the completed structure is shown in FIG. 2 .

(3)选择尺寸为20mm×20mm的单面抛光普通硅片6，用丙酮溶液清洗干净，并采用旋涂的方式在抛光表面涂一层TH04095-2胶5，用于粘结SOI片与普通硅片。(3) Choose a single-sided polishedordinary silicon wafer 6 with a size of 20mm×20mm, clean it with acetone solution, and apply a layer of TH04095-2 adhesive 5 on the polished surface by spin coating, which is used to bond the SOI wafer with the ordinary silicon wafer. silicon wafer.

(4)将沉积有金属铜的SOI片与普通硅片粘结，金属铜表面与粘结剂相贴。然后再放置于热板上，从室温逐步升温至120℃，加热10min，完成普通硅片与SOI片的粘结。粘结完成后结构如图3所示。(4) bonding the SOI sheet deposited with metal copper to the ordinary silicon wafer, and the surface of the metal copper is attached to the adhesive. Then place it on a hot plate, gradually raise the temperature from room temperature to 120°C, and heat for 10 minutes to complete the bonding of ordinary silicon wafers and SOI wafers. The structure after bonding is shown in Figure 3.

(5)将粘结好的SOI片-普通硅片置于ICP刻蚀腔体内，如图3所示的底层单晶硅1的表面朝上，普通硅片6的表面朝下，利用ICP干法刻蚀的方法对SOI片底层单晶硅1进行深刻蚀，刻蚀深度为400μm。(5) Place the bonded SOI sheet-ordinary silicon wafer in the ICP etching chamber, the surface of the bottomsingle crystal silicon 1 shown in Figure 3 is facing upwards, and the surface of theordinary silicon wafer 6 is facing downwards. Themonocrystalline silicon 1 at the bottom of the SOI sheet is deeply etched by the etching method, and the etching depth is 400 μm.

(6)利用氢氧化钾湿法腐蚀的方法对SOI片剩余的底层单晶硅1进行腐蚀，腐蚀厚度为50μm，直至将单晶硅完全去除。(6) Etch the remaining underlyingmonocrystalline silicon 1 of the SOI sheet by using a potassium hydroxide wet etching method, with an etching thickness of 50 μm, until the monocrystalline silicon is completely removed.

(7)利用氢氟酸湿法腐蚀的方法对SOI片中间层二氧化硅2进行腐蚀，腐蚀厚度为300nm，露出高浓度均匀掺杂的N型硅表面3，完成后结构如图4所示。(7) Thesilicon dioxide 2 in the middle layer of the SOI sheet is etched by hydrofluoric acid wet etching with a thickness of 300 nm, exposing the N-type silicon surface 3 uniformly doped with a high concentration. The completed structure is shown in Figure 4 .

(8)利用磁控溅射镀膜设备，在露出的高浓度均匀掺杂的N型硅表面3沉积一层厚度为50nm的金属铜7，完成铜/高浓度均匀掺杂的N型硅/铜三层结构的制作，结构如图5所示。(8) Using magnetron sputtering coating equipment, deposit a layer ofmetal copper 7 with a thickness of 50nm on the exposed high-concentration uniformly doped N-type silicon surface 3 to complete copper/high-concentration uniformly doped N-type silicon/copper The fabrication of the three-layer structure, the structure is shown in Figure 5.

(9)在基片的铜表面上采用旋涂的方式涂覆抗蚀剂AR3120，旋涂的转速为5000rpm；涂覆完成后以温度100℃烘烤10min。(9) Coating the resist AR3120 on the copper surface of the substrate by spin coating, the rotation speed of the spin coating is 5000 rpm; after coating, bake at 100° C. for 10 min.

(10)采用接近式光刻对基片进行曝光，将所设计的金属线阵列微结构图形转移到抗蚀剂上。使用掩膜的线条宽度W＝30μm，长度L＝80μm，开口间距S＝3μm；周期Px＝40μm，Py＝150μm。将曝光后的基片进行显影及定影，得到阵列结构的抗蚀剂图形，完成后结构如图6所示。(10) Expose the substrate by using proximity lithography, and transfer the designed metal line array microstructure pattern to the resist. The line width W=30 μm, the length L=80 μm, the opening pitch S=3 μm, the period Px=40 μm, and the Py=150 μm of the mask used. The exposed substrate is developed and fixed to obtain a resist pattern with an array structure, and the completed structure is shown in FIG. 6 .

(11)将具有抗蚀剂图形的基片放入IBE刻蚀设备中，以抗蚀剂图形为掩膜，对基片表面的金属层进行刻蚀；其中采用的离子束流为30mA、电子束流为40mA、屏极电压为400V、加速板电压为200V，样品台温度20℃，溅射角度60°、刻蚀时间180s，使基片表面的上层金属层完全刻蚀。(11) The substrate with the resist pattern is put into the IBE etching equipment, and the metal layer on the substrate surface is etched with the resist pattern as a mask; the ion beam current adopted is 30mA, electron The beam current is 40mA, the screen electrode voltage is 400V, the accelerator plate voltage is 200V, the sample stage temperature is 20°C, the sputtering angle is 60°, and the etching time is 180s, so that the upper metal layer on the substrate surface is completely etched.

(12)用丙酮浸泡刻蚀好的样品，将刻蚀剩余的抗蚀剂去除，获得铜/高浓度均匀掺杂的N型硅/铜三层结构的可调谐人工电磁材料，结构如图7所示。(12) Soak the etched sample in acetone, remove the remaining etching resist, and obtain a tunable artificial electromagnetic material with a three-layer structure of copper/high concentration uniform doping N-type silicon/copper, as shown in Figure 7 shown.

实施例2Example 2

本发明的一个典型实施例，是制作金/高浓度均匀掺杂硅/金的三层结构，适用波段为中红外。其中金的厚度分别为200nm和40nm，掺杂层的厚度为1.05μm，掺杂元素是磷，掺杂浓度为10¹⁹cm^-1。A typical embodiment of the present invention is to make a three-layer structure of gold/high-concentration uniformly doped silicon/gold, and the applicable waveband is mid-infrared. The thicknesses of gold are 200nm and 40nm respectively, the thickness of the doped layer is 1.05μm, the doping element is phosphorus, and the doping concentration is 10¹⁹ cm^-1 .

(1)选择尺寸为15mm×15mm的双面抛光SOI片，置于浓硝酸∶水＝3∶1的混合溶液里浸泡1.5h，再放置在去离子水里超声三次，每次超声时间为5min，最后用丙酮擦洗，于烘箱160℃烘30min，待其自然冷却。该SOI片底层单晶硅1的厚度为450μm，中间层二氧化硅2的厚度为300nm，顶层高浓度均匀掺杂的N型硅3的厚度为1.05μm，厚度精度±0.05μm，掺杂磷的浓度为10¹⁹cm^-1。(1) Choose a double-sided polished SOI chip with a size of 15mm×15mm, soak it in a mixed solution of concentrated nitric acid: water = 3:1 for 1.5h, and then place it in deionized water for three times for ultrasonication, each time for 5min , and finally scrub with acetone, bake in an oven at 160°C for 30 minutes, and let it cool naturally. The bottomsingle crystal silicon 1 of the SOI sheet has a thickness of 450 μm, the middle layer ofsilicon dioxide 2 has a thickness of 300 nm, and the top layer of high-concentration and uniformly doped N-type silicon 3 has a thickness of 1.05 μm, with a thickness accuracy of ±0.05 μm, doped with phosphorus The concentration is 10¹⁹ cm^-1 .

(2)利用磁控溅射镀膜设备，在SOI片的顶层掺杂硅3表面沉积一层厚度为200nm的金膜4，完成后结构如图2所示。(2) Agold film 4 with a thickness of 200nm is deposited on the surface of the topdoped silicon 3 of the SOI sheet by magnetron sputtering coating equipment, and the completed structure is shown in FIG. 2 .

(3)选择尺寸为20mm×20mm的单面抛光的普通硅片6，用丙酮溶液清洗干净，并采用旋涂的方式在抛光表面涂一层TH04095-2胶5，用于粘结SOI片与普通硅片。(3) Select a single-sided polishedordinary silicon wafer 6 with a size of 20mm×20mm, clean it with acetone solution, and apply a layer of TH04095-2glue 5 on the polished surface by spin coating, which is used to bond the SOI wafer and Ordinary silicon wafers.

(4)将沉积有金膜的SOI片与普通硅片粘结，金膜表面与粘结剂相贴，如图3所示。然后再放置于热板上，从室温逐步升温至120℃，加热10min，完成普通硅片与SOI片的粘结。粘结完成后结构如图3所示。(4) Bond the SOI wafer deposited with the gold film to the ordinary silicon wafer, and the surface of the gold film is attached to the adhesive, as shown in FIG. 3 . Then place it on a hot plate, gradually raise the temperature from room temperature to 120°C, and heat for 10 minutes to complete the bonding of ordinary silicon wafers and SOI wafers. The structure after bonding is shown in Figure 3.

(5)将粘结好的SOI片-普通硅片置于ICP刻蚀腔体内，底层单晶硅1的表面朝上，普通硅片6的表面朝下，如图3所示。利用ICP干法刻蚀的方法对SOI片底层单晶硅1深刻蚀，刻蚀深度为420μm。(5) Put the bonded SOI sheet-ordinary silicon wafer in the ICP etching chamber, with the surface of the bottomsingle crystal silicon 1 facing upwards and the surface of theordinary silicon wafer 6 facing downwards, as shown in FIG. 3 . Themonocrystalline silicon 1 at the bottom of the SOI sheet was deeply etched by the ICP dry etching method, and the etching depth was 420 μm.

(6)利用氢氧化钾湿法腐蚀的方法对SOI片剩余的底层单晶硅1进行腐蚀，腐蚀厚度为30μm，直至将单晶硅完全去除。(6) Etch the remaining underlyingmonocrystalline silicon 1 of the SOI sheet by using a potassium hydroxide wet etching method, with an etching thickness of 30 μm, until the monocrystalline silicon is completely removed.

(7)利用氢氟酸湿法腐蚀的方法对SOI片中间层二氧化硅层2进行腐蚀，腐蚀厚度为300nm，露出高浓度均匀掺杂的N型硅表面3，完成后结构如图4所示。(7) Thesilicon dioxide layer 2, the middle layer of the SOI sheet, is etched by hydrofluoric acid wet etching with a thickness of 300 nm, exposing the N-type silicon surface 3 uniformly doped with a high concentration. The structure after completion is shown in Figure 4 Show.

(8)利用磁控溅射镀膜设备，在露出的高浓度均匀掺杂的N型硅表面3沉积一层厚度为40nm的金膜，如图5所示，完成金/高浓度均匀掺杂的N型硅/金三层结构的制作，结构如图5所示。(8) Utilize the magnetron sputtering film coating equipment, on the N-type silicon surface 3 that exposes high-concentration uniform doping, deposit one layer of thickness to be the gold film of 40nm, as shown in Figure 5, complete the gold/high-concentration uniform doping Fabrication of N-type silicon/gold three-layer structure, the structure is shown in Figure 5.

(9)在基片的金表面上采用旋涂的方式涂覆ZEP 520A电子抗蚀剂，旋涂的转速为6000rpm；涂覆完成后以温度100℃烘烤10min。(9) Coating ZEP 520A electronic resist on the gold surface of the substrate by spin coating, the spin coating speed is 6000rpm; after coating, bake at 100°C for 10min.

(10)采用电子束直写进行曝光，将所设计的金属线阵列微纳结构图形转移到抗蚀剂上。电子束直写的线条宽度W＝300nm，长度L＝800nm，开口间距S＝100nm；周期Px＝1.2μm，Py＝1.5μm。将曝光后的基片进行显影及定影，得到阵列结构的抗蚀剂图形，完成后结构如图6所示。(10) Electron beam direct writing is used for exposure, and the designed micro-nano structure pattern of the metal wire array is transferred to the resist. The line width of the electron beam direct writing is W=300nm, the length L=800nm, the opening spacing S=100nm; the period Px=1.2μm, Py=1.5μm. The exposed substrate is developed and fixed to obtain a resist pattern with an array structure, and the completed structure is shown in FIG. 6 .

(11)具有抗蚀剂图形的基片放入IBE刻蚀设备中，以抗蚀剂图形为掩膜，对基片表面的金属层进行刻蚀；其中采用的离子束流为30mA、电子束流为40mA、屏极电压为400V、加速板电压为200V，样品台温度20℃，溅射角度60°、刻蚀时间120s，将基片表面的金膜完全刻蚀。(11) The substrate with the resist pattern is put into the IBE etching equipment, and the metal layer on the substrate surface is etched with the resist pattern as a mask; the ion beam current adopted is 30mA, electron beam The current is 40mA, the plate voltage is 400V, the accelerator plate voltage is 200V, the temperature of the sample stage is 20°C, the sputtering angle is 60°, and the etching time is 120s to completely etch the gold film on the surface of the substrate.

(12)用丙酮浸泡刻蚀好的样品，将刻蚀剩余的抗蚀剂去除，获得金/高浓度均匀掺杂的N型硅/金三层结构的可调谐人工电磁材料，结构如图7所示。(12) Soak the etched sample in acetone, remove the remaining resist from etching, and obtain a tunable artificial electromagnetic material with a three-layer structure of gold/highly uniformly doped N-type silicon/gold, as shown in Figure 7. shown.

本发明未详细阐述的部分属于本领域公知技术。The parts not described in detail in the present invention belong to the well-known technology in the art.

Claims (19)

Translated fromChinese

1.一种基于三层结构的可调谐人工电磁材料的制作方法，其特征在于该方法包括如下步骤：1. A method for making a tunable artificial electromagnetic material based on a three-layer structure, characterized in that the method may further comprise the steps:步骤(1)选取合适的双面抛光的SOI片，清洗干净，并在SOI片顶层的掺杂硅表面沉积一层金属膜；Step (1) select a suitable double-sided polished SOI sheet, clean it, and deposit a layer of metal film on the doped silicon surface of the top layer of the SOI sheet;步骤(2)另取单面抛光的硅片，在抛光表面涂覆一层粘结剂；Step (2) take another silicon wafer polished on one side, and coat a layer of adhesive on the polished surface;步骤(3)利用粘连剂将沉积有金属膜的SOI片与硅片粘结，并将粘结好的硅片-SOI片进行烘烤固化；Step (3) bonding the SOI sheet deposited with the metal film to the silicon sheet with an adhesive, and baking and curing the bonded silicon sheet-SOI sheet;步骤(4)利用干法刻蚀将硅片-SOI片结构中SOI片的底层单晶硅进行刻蚀减薄；Step (4) using dry etching to etch and thin the bottom single crystal silicon of the SOI sheet in the silicon wafer-SOI sheet structure;步骤(5)采用氢氧化钾湿法腐蚀，将硅片-SOI片结构中SOI片上剩余的底层单晶硅腐蚀完毕，使SOI片的二氧化硅中间层露出；Step (5) using potassium hydroxide wet etching to etch the remaining bottom single crystal silicon on the SOI sheet in the silicon wafer-SOI sheet structure, so that the silicon dioxide intermediate layer of the SOI sheet is exposed;步骤(6)采用氢氟酸湿法腐蚀，将硅片-SOI片结构中SOI片的二氧化硅中间层腐蚀完毕，露出掺杂硅表面；Step (6) using hydrofluoric acid wet etching to etch the silicon dioxide intermediate layer of the SOI sheet in the silicon wafer-SOI sheet structure to expose the doped silicon surface;步骤(7)在步骤(6)中的掺杂硅表面沉积一层金属膜，从而在硅片上形成金属-掺杂介质-金属的三层结构；Step (7) depositing a layer of metal film on the doped silicon surface in step (6), thereby forming a three-layer structure of metal-doped medium-metal on the silicon wafer;步骤(8)在所得金属-掺杂介质-金属三层结构上涂覆光刻胶，并在烘箱或热板中进行前烘；Step (8) Coating a photoresist on the obtained metal-doped medium-metal three-layer structure, and pre-baking in an oven or a hot plate;步骤(9)利用光刻设备对基片进行曝光，在光刻胶上获得所设计的二维周期性阵列微纳结构图形，并置于烘箱或热板中进行坚膜；Step (9) Exposing the substrate with photolithography equipment, obtaining the designed two-dimensional periodic array micro-nano structure pattern on the photoresist, and placing it in an oven or a hot plate to harden the film;步骤(10)采用干法刻蚀将步骤(9)中的光刻胶图形转移至金属-掺杂介质-金属三层结构中的上层金属；Step (10) using dry etching to transfer the photoresist pattern in step (9) to the upper metal in the metal-doped medium-metal three-layer structure;步骤(11)用有机溶剂浸泡刻蚀后的样品，将刻蚀后剩余的光刻胶去除，即可获得基于金属-掺杂介质-金属三层结构的可调谐人工电磁材料。Step (11) Soak the etched sample with an organic solvent, remove the remaining photoresist after etching, and obtain a tunable artificial electromagnetic material based on a metal-doped medium-metal three-layer structure.2.根据权利要求1所述的一种基于三层结构的可调谐人工电磁材料的制作方法，其特征在于，所述步骤(1)的SOI片是由底层单晶硅、中间层二氧化硅、顶层掺杂硅组成，底层厚度为300～450μm，中间层厚度为100～300nm，顶层是厚度为0.5～1.5μm的高浓度均匀掺杂的N型硅或P型硅，掺杂浓度为10¹⁸～10²⁰cm^-1。2. the manufacture method of a kind of tunable artificial electromagnetic material based on three-layer structure according to claim 1, is characterized in that, the SOI sheet of described step (1) is made of bottom monocrystalline silicon, middle layer silicon dioxide The top layer is composed of doped silicon, the thickness of the bottom layer is 300-450 μm, the thickness of the middle layer is 100-300 nm, and the top layer is N-type silicon or P-type silicon with a thickness of 0.5-1.5 μm uniformly doped at a high concentration, and the doping concentration is 10^18-1020 cm^-1 .3.根据权利要求1所述的一种基于三层结构的可调谐人工电磁材料的制作方法，其特征在于，所述步骤(1)的沉积方法可以为磁控溅射法或者蒸镀法。3. A method for manufacturing a tunable artificial electromagnetic material based on a three-layer structure according to claim 1, wherein the deposition method in step (1) can be magnetron sputtering or evaporation.4.根据权利要求1所述的一种基于三层结构的可调谐人工电磁材料的制作方法，其特征在于，所述步骤(1)中的金属膜可以为金、铜或者银，金属膜厚度为100～200nm。4. the manufacture method of a kind of tunable artificial electromagnetic material based on three-layer structure according to claim 1, is characterized in that, the metal film in described step (1) can be gold, copper or silver, metal film thickness 100-200nm.5.根据权利要求1所述的一种基于三层结构的可调谐人工电磁材料的制作方法，其特征在于，所述步骤(2)中的粘结剂是一种耐高温、耐强酸强碱及有机溶剂的胶。5. A kind of manufacture method based on the tunable artificial electromagnetic material of three-layer structure according to claim 1, it is characterized in that, the binding agent in the described step (2) is a kind of high temperature resistant, strong acid strong alkali resistant and organic solvent glue.6.根据权利要求1所述的一种基于三层结构的可调谐人工电磁材料的制作方法，其特征在于，所述步骤(3)中的粘结方式是将SOI的金属膜层与旋涂有粘结剂的硅片相粘连。6. the manufacture method of a kind of tunable artificial electromagnetic material based on three-layer structure according to claim 1, is characterized in that, the bonding mode in the described step (3) is the metal film layer of SOI and spin coating The silicon wafers are bonded with an adhesive.7.根据权利要求1所述的一种基于三层结构的可调谐人工电磁材料的制作方法，其特征在于，所述步骤(3)中的烘烤设备可以为烘箱和热板，温度范围为100～120℃，烘烤时间为5～10min。7. the manufacture method of a kind of tunable artificial electromagnetic material based on three-layer structure according to claim 1, is characterized in that, the baking equipment in described step (3) can be oven and hot plate, and temperature range is 100～120℃, the baking time is 5～10min.8.根据权利要求1所述的一种基于三层结构的可调谐人工电磁材料的制作方法，其特征在于，所述步骤(4)中的干法刻蚀可以为电感耦合等离子刻蚀、等离子刻蚀或者离子束刻蚀。8. A kind of manufacture method based on the tunable artificial electromagnetic material of three-layer structure according to claim 1, is characterized in that, the dry etching in described step (4) can be inductively coupled plasma etching, plasma etching or ion beam etching.9.根据权利要求1所述的一种基于三层结构的可调谐人工电磁材料的制作方法，其特征在于，所述步骤(4)中的SOI片的底层单晶硅减薄后的厚度为20～50μm。9. the manufacture method of a kind of tunable artificial electromagnetic material based on three-layer structure according to claim 1, is characterized in that, the thickness after the thinning of the bottom monocrystalline silicon of the SOI sheet in described step (4) is 20-50μm.10.根据权利要求1所述的一种基于三层结构的可调谐人工电磁材料的制作方法，其特征在于，所述步骤(7)中沉积方法可以为磁控溅射法或者蒸镀法。10. A method for manufacturing a tunable artificial electromagnetic material based on a three-layer structure according to claim 1, characterized in that, the deposition method in the step (7) can be magnetron sputtering or evaporation.11.根据权利要求1所述的一种基于三层结构的可调谐人工电磁材料的制作方法，其特征在于，所述步骤(7)中沉积金属膜可以为金、铜或者银，金属膜厚度为40～60nm。11. a kind of manufacture method based on the tunable artificial electromagnetic material of three-layer structure according to claim 1, is characterized in that, in described step (7), deposited metal film can be gold, copper or silver, metal film thickness It is 40-60nm.12.根据权利要求1所述的一种基于三层结构的可调谐人工电磁材料的制作方法，其特征在于，所述步骤(8)中光刻胶的厚度为100～200nm，前烘温度范围为100～120℃，烘烤时间为20～30min。12. A method for manufacturing a tunable artificial electromagnetic material based on a three-layer structure according to claim 1, wherein the thickness of the photoresist in the step (8) is 100-200 nm, and the pre-baking temperature range is The temperature is 100-120°C, and the baking time is 20-30 minutes.13.根据权利要求1所述的一种基于三层结构的可调谐人工电磁材料的制作方法，其特征在于，所述步骤(9)中的光刻设备可以为接近接触式光刻机、投影式光刻机或者电子束直写曝光机。13. A method for manufacturing a tunable artificial electromagnetic material based on a three-layer structure according to claim 1, wherein the lithography equipment in the step (9) can be a near-contact lithography machine, a projection Type lithography machine or electron beam direct writing exposure machine.14.根据权利要求1所述的一种基于三层结构的可调谐人工电磁材料的制作方法，其特征在于，所述步骤(9)中的二维周期性阵列微纳结构图形的线宽可以为0.3～60μm，周期可以为1.2～160μm。14. the manufacture method of a kind of tunable artificial electromagnetic material based on three-layer structure according to claim 1, is characterized in that, the line width of the two-dimensional periodic array micro-nano structure pattern in the described step (9) can be 0.3-60 μm, and the period may be 1.2-160 μm.15.根据权利要求1所述的一种基于三层结构的可调谐人工电磁材料的制作方法，其特征在于，所述步骤(9)中的坚膜温度为：100～120℃，坚膜时间为：20～30min。15. A method for manufacturing a tunable artificial electromagnetic material based on a three-layer structure according to claim 1, characterized in that the hardening temperature in the step (9) is: 100-120°C, and the hardening time For: 20 to 30 minutes.16.根据权利要求1所述的一种基于三层结构的可调谐人工电磁材料的制作方法，其特征在于，所述步骤(10)中的干法刻蚀可以为等离子刻蚀、离子束刻蚀或者电感耦合等离子刻蚀。16. The manufacturing method of a tunable artificial electromagnetic material based on a three-layer structure according to claim 1, wherein the dry etching in the step (10) can be plasma etching, ion beam etching etching or inductively coupled plasma etching.17.根据权利要求1所述的一种基于三层结构的可调谐人工电磁材料的制作方法，其特征在于，所述步骤(10)中的刻蚀深度应该等于金属-掺杂介质-金属三层结构中上层金属层厚度，误差不超过5％。17. The manufacturing method of a tunable artificial electromagnetic material based on a three-layer structure according to claim 1, wherein the etching depth in the step (10) should be equal to metal-doped medium-metal three The thickness of the upper metal layer in the layer structure, the error is not more than 5%.18.根据权利要求1所述的一种基于三层结构的可调谐人工电磁材料的制作方法，其特征在于，所述步骤(11)中的有机溶剂为可以溶解光刻胶的溶剂。18. A method for manufacturing a tunable artificial electromagnetic material based on a three-layer structure according to claim 1, wherein the organic solvent in the step (11) is a solvent that can dissolve photoresist.19.一种基于三层结构的可调谐人工电磁材料，其特征在于：该可调谐人工电磁材料由权利要求1至18中任一项所述的方法加工制成。19. A tunable artificial electromagnetic material based on a three-layer structure, characterized in that: the tunable artificial electromagnetic material is processed by the method described in any one of claims 1-18.

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