CN1963985A - A grid of transmission electronic microscope driven by thermal dual metal sheets - Google Patents
A grid of transmission electronic microscope driven by thermal dual metal sheetsDownload PDFInfo
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Abstract
Translated fromChinese
Description
Translated fromChinese技术领域：Technical field:
本发明涉及一种透射电子显微镜样品载网，利用透射电子显微镜样品加热台，使载网中的双金属片发生热膨胀应力诱导的弯曲变形，驱动分布在其上的样品发生拉伸或弯曲变形，提供了一种方便的样品原位实时动态观察方法，属于纳米材料微区变形原位表征方法。The invention relates to a transmission electron microscope sample carrier grid, which uses a transmission electron microscope sample heating platform to cause the bimetal sheet in the carrier grid to undergo thermal expansion stress-induced bending deformation, and to drive the samples distributed on it to undergo stretching or bending deformation. A convenient in-situ real-time dynamic observation method of a sample is provided, which belongs to the in-situ characterization method of micro-region deformation of nanomaterials.
背景技术：Background technique:
透射电子显微镜(以下称透射电镜或电镜)是现代化的大型仪器，是研究物质微观结构的有力工具，它在物理，化学，材料科学，生命科学等领域有着广泛的应用，特别是目前发展迅速的纳米科学和技术领域，是最为有力的研究工具之一，目前透射电子显微镜的分辨能力已达0.2nm，接近固态物质原子间距。透射电子显微镜载网是用来支撑被检测的样品，目前常用的一般为铜网，非晶碳支持膜或微栅，这些载网只能承载被检测的样品，透射电子显微镜只能观测分布在这些载网上的样品的静态组织结构，不能利用这些载网对样品进行操纵，实行动态原位检测。随着微机电系统(MEMS，microelectromechanical system)和纳机电系统(NEMS，nano electromechanicalsysterm)的发展，对于单根纳米线或薄膜在外力作用下力学性能研究显的尤为迫切，但是由于单根纳米线或薄膜结构细小，难于操纵，在透射电子显微镜中如何对单根纳米线或纳米薄膜样品进行固定和原位变形，从纳米尺度和原子层次揭示纳米材料在外力作用下变形机制，和尺寸效应成为摆在研究人员面前的难题。目前在透射电子显微镜中由于受到样品台与极靴极为有限的空间，一般是1-3mm，在原子尺度分辨率下对于单根纳米线或纳米薄膜的操纵和力学性能的直接测量非常困难，文献中已经报道的主要有两种方法。Transmission electron microscope (hereinafter referred to as transmission electron microscope or electron microscope) is a modern large-scale instrument and a powerful tool for studying the microstructure of matter. It has a wide range of applications in physics, chemistry, material science, life science and other fields, especially the rapidly developing In the field of nano science and technology, it is one of the most powerful research tools. At present, the resolution of the transmission electron microscope has reached 0.2nm, which is close to the atomic distance of solid matter. The transmission electron microscope grid is used to support the sample to be tested. At present, copper grid, amorphous carbon support film or micro-grid are commonly used. These grids can only carry the sample to be tested, and the transmission electron microscope can only observe the samples distributed in The static organizational structure of the samples on these grids cannot be used to manipulate the samples and implement dynamic in-situ detection. With the development of microelectromechanical systems (MEMS, microelectromechanical system) and nanoelectromechanical systems (NEMS, nanoelectromechanicalsystem), it is particularly urgent to study the mechanical properties of a single nanowire or film under external force. The film structure is small and difficult to manipulate. How to fix and in-situ deform a single nanowire or nanofilm sample in a transmission electron microscope reveals the deformation mechanism of nanomaterials under external force at the nanoscale and atomic level, and the size effect becomes a pendulum Conundrums before researchers. At present, due to the extremely limited space between the sample stage and the pole piece in the transmission electron microscope, generally 1-3mm, it is very difficult to directly measure the mechanical properties of a single nanowire or nanofilm at atomic scale resolution. There are mainly two approaches that have been reported.
一种是方法报道于《Applied physics letters》2002年80卷第21期，其主要原理是利用特殊沉积的压电陶瓷薄膜(PZT)做为载网，将研究的薄膜沉积在压电陶瓷表面，用可以通电的透射电镜样品杆将载网和样品放入透射电子显微镜中，在电场的作用下压电陶瓷的变形实现对薄膜的拉伸和压缩操作，同时利用透射电镜成像系统记录薄膜的疲劳断裂变化过程。该方法样品制作过程较复杂，由于样品杆倾转角度的限制(一般只能单轴倾转或双轴倾转±5°)，不能在最佳分辨率情况下(高分辨原子尺度)进行原位观察，不能从根本上了解其变形机制。One is the method reported in "Applied physics letters" 2002, volume 80, No. 21. The main principle is to use a specially deposited piezoelectric ceramic film (PZT) as a grid, and deposit the researched film on the surface of the piezoelectric ceramic. Use the TEM sample rod that can be energized to put the grid and the sample into the TEM. Under the action of the electric field, the deformation of the piezoelectric ceramic realizes the stretching and compression of the film, and at the same time, the TEM imaging system is used to record the fatigue of the film. Fracture change process. The sample preparation process of this method is more complicated. Due to the limitation of the tilting angle of the sample rod (generally only single-axis tilting or biaxial tilting ±5°), the original sample cannot be performed at the best resolution (high-resolution atomic scale). It is impossible to understand its deformation mechanism fundamentally.
另一种方法分别报道于《Physics Review Letters》2005年第94卷236802页和《Nature》2006年439卷281页，其主要原理是将扫描隧道显微镜探针放入透射电子显微镜种，利用外接控制系统控制探针运动来操纵单根碳纳米管，实现对碳纳米管的拉伸变形，利用导电的探针实现了在通电的同时对碳纳米管的拉伸，发现了碳纳米管在电流作用下高温超塑性变形行为和断裂机制。这种方法虽然对精心设计的样品可以实现原子分辨，并同时进行拉伸和通电测量，但由于较为复杂的机械结构放入透射电镜样品室中，样品台只能小角度倾转(±5°)或只能单轴倾转(不超过±20°)，仍然限制了其应用范围，不利于普及推广。Another method was reported in "Physics Review Letters" 2005, Volume 94, page 236802 and "Nature" 2006, Volume 439, page 281. The main principle is to put the scanning tunneling microscope probe into the transmission electron microscope, and use external The system controls the movement of the probe to manipulate a single carbon nanotube to achieve stretching and deformation of the carbon nanotube. The conductive probe is used to stretch the carbon nanotube while electrifying. Deformation behavior and fracture mechanism of superplasticity at high temperature. Although this method can achieve atomic resolution for well-designed samples and simultaneously perform tensile and energized measurements, due to the relatively complicated mechanical structure placed in the sample chamber of the transmission electron microscope, the sample stage can only be tilted at a small angle (±5° ) or can only be tilted on a single axis (no more than ±20°), which still limits its application range and is not conducive to popularization.
上述所有透射电子显微镜原位纳米材料力学性能测试中，样品操纵台或载网均不能实现大角度倾转，对于大部分需要在正带轴下实时观察在外力作用下结构变化的纳米材料，其应用受到限制。In all the above-mentioned in-situ nanomaterial mechanical property tests by transmission electron microscopy, the sample manipulation table or the grid cannot be tilted at a large angle. Application is limited.
发明内容：Invention content:
针对现有技术存在的问题，本发明的目的是提供一种利用热双金属片驱动的智能透射电子显微镜样品载网，此载网和目前常用的透射电镜微栅尺寸相当，固定在现有技术产品双倾透射电镜加热台上，不受样品驱动元件尺寸的限制，放入透射电子显微镜中可以实现大角度倾转(目前商业化双倾加热台可以达到±30°/±60°)，使样品能在正带轴下实现原子层次分辨的同时实现纳米材料的原位变形操作，通过图像记录系统实时记录变形过程。载网的基本结构是在普通用的透射电镜铜环上面固定一条或两条热敏形变的双金属片，利用商业化的双倾透射电子显微镜加热台加热，使载网中的双金属片发生弯曲变形，分布在载网上的纳米线或纳米薄膜会被拉伸或压缩，同时原位实时记录纳米线或薄膜在外力作用的结构信息和变形过程，将微区力学性能与微观结构直接对应起来，从原子层次上揭示一维纳米线或薄膜的力学性能和变形机制。In view of the problems existing in the prior art, the purpose of the present invention is to provide an intelligent transmission electron microscope sample carrier grid driven by a thermal bimetallic sheet. The product is on the double-tilt transmission electron microscope heating stage, which is not limited by the size of the sample driving element. It can be tilted at a large angle when placed in the transmission electron microscope (the current commercial double-tilt heating stage can reach ±30°/±60°), making The sample can achieve atomic-level resolution under the positive band axis and at the same time realize the in-situ deformation operation of nanomaterials, and record the deformation process in real time through the image recording system. The basic structure of the grid is to fix one or two thermally deformed bimetallic strips on the copper ring of the transmission electron microscope commonly used, and use a commercial double-tilt transmission electron microscope heating table to heat the bimetallic strips in the grid. Bending deformation, the nanowires or nanofilms distributed on the grid will be stretched or compressed, and at the same time, the structural information and deformation process of the nanowires or films under the action of external force will be recorded in situ in real time, and the mechanical properties of the micro-area will directly correspond to the microstructure , to reveal the mechanical properties and deformation mechanisms of one-dimensional nanowires or films from the atomic level.
为了实现上面的目的，本发明是通过如下的技术方案来实现的：In order to achieve the above purpose, the present invention is achieved through the following technical solutions:
方案一，载网包括支撑部分和驱动部分，所述的支撑部分是金属环(1)，所述的驱动部分是两个对称排列的不同线膨胀系数组成的热双金属片(2)且线膨胀系数大的金属片在内侧，线膨胀系数小的金属片在外侧，热双金属片一端用压片(3)固定在金属环上面，另一端自由搭到金属环上；所述的热双金属片对称分布在金属环的中心。Option 1, the grid includes a supporting part and a driving part, the supporting part is a metal ring (1), and the driving part is a thermal bimetal sheet (2) composed of two symmetrically arranged different linear expansion coefficients and the wire The metal sheet with a large expansion coefficient is on the inside, and the metal sheet with a small linear expansion coefficient is on the outside. One end of the thermal bimetallic sheet is fixed on the metal ring with a pressing piece (3), and the other end is freely attached to the metal ring; The metal pieces are symmetrically distributed in the center of the metal ring.
当载网固定在现有技术的透射电镜加热台上时，随着热台温度的升高，双金属片由于热膨胀系数不同向两侧横向自由弯曲，固定在双金属片上的纳米线或薄膜则被双向拉伸变形，根据升温速率可以控制纳米线或薄膜的应变速率，当温度恢复在室温时，双金属片回弹到原位。通过透射电镜成像系统原位记录纳米线或薄膜的变形过程，从微观结构变化揭示纳米材料的变形机制。When the carrier grid is fixed on the prior art TEM heating stage, as the temperature of the heating stage increases, the bimetal sheet will bend freely laterally to both sides due to the difference in thermal expansion coefficient, and the nanowires or films fixed on the bimetal sheet will Being biaxially stretched and deformed, the strain rate of the nanowire or film can be controlled according to the heating rate, and when the temperature returns to room temperature, the bimetallic sheet springs back to its original position. The deformation process of nanowires or thin films is recorded in situ by the transmission electron microscope imaging system, and the deformation mechanism of nanomaterials is revealed from the microstructure changes.
方案二，热双金属片驱动的透射电子显微镜载网，其特征在于载网包括支撑部分和驱动部分，所述的驱动部分包括一个热双金属片(2)和一个并行排列的金属丝(4)，热双金属片一端用压片(3)固定在金属环上面，另一端自由搭到金属环上；金属丝两端均用压片(3)固定在金属环上；所述的热双金属片(2)和金属丝(4)对称分布在金属环的中心。Option two, a transmission electron microscope grid driven by a thermal bimetal, is characterized in that the grid includes a supporting part and a driving part, and the driving part includes a thermal bimetal (2) and a metal wire (4) arranged in parallel ), one end of the thermal bimetal sheet is fixed on the metal ring with a pressing piece (3), and the other end is free to ride on the metal ring; both ends of the metal wire are fixed on the metal ring with a pressing piece (3); Metal sheets (2) and metal wires (4) are symmetrically distributed in the center of the metal ring.
当这种载网固定在现有技术的透射电镜加热台上时，随着热台温度的升高，一端自由运动的双金属片由于热膨胀系数不同向外侧横向自由弯曲，金属丝则固定不动，固定在双金属片上的纳米线或薄膜则被单向拉伸变形。When this carrier grid is fixed on the prior art TEM heating stage, as the temperature of the heating stage rises, the free-moving bimetal at one end bends laterally to the outside due to different thermal expansion coefficients, while the metal wire is fixed. , the nanowires or films fixed on the bimetallic sheet are deformed by uniaxial stretching.
进一步地，所述的金属环为导电导热性良好，容易加工的铜环，镍环，金环，为了保证金属环固定在透射电镜样品杆上，金属环的外径与现有技术载网一致为3mm，为了保证电子束透过对样品进行结构分析，中心开孔，金属环的厚度在0.1mm-0.5mm之间。Further, the metal ring is a copper ring, a nickel ring, and a gold ring with good electrical and thermal conductivity and easy processing. In order to ensure that the metal ring is fixed on the sample rod of the transmission electron microscope, the outer diameter of the metal ring is consistent with the prior art grid In order to ensure that the electron beam can pass through the sample for structural analysis, a hole is opened in the center, and the thickness of the metal ring is between 0.1mm-0.5mm.
进一步地，所述的热双金属片为线膨胀系数差异相对很大的金属片叠焊在一起，当温度变化时，因双金属片的两种不同材料线膨胀系数差异相对很大而产生不同的膨胀和收缩，导致双金属片产生弯曲变形。本发明中线膨胀系数大的金属片在内侧，线膨胀系数小的金属片在外侧，对称排列，受热时实现向外侧弯曲运动。根据需要测量的纳米线的材质和直径，热双金属片截面为矩形厚度在0.25mm-0.5mm之间，双金属层宽度在0.25mm-1mm之间，根据金属环内径的大小，热双金属片的长度在1.6mm-2.5mm之间，以一端固定在金属环上，一端自由搭到金属环上为宜。本发明中，为了保证在较低温度下实现较大的的弯曲变形，推荐使用比弯曲大于10/10-6·℃-1的双金属片。Further, the thermal bimetal sheet is welded together with metal sheets with relatively large differences in linear expansion coefficients. When the temperature changes, a difference occurs due to the relatively large difference in the linear expansion coefficients of the two different materials of the bimetal sheet. The expansion and contraction of the bimetal lead to bending deformation. In the present invention, the metal sheet with a large linear expansion coefficient is on the inner side, and the metal sheet with a small linear expansion coefficient is on the outer side, which are symmetrically arranged, and can realize bending movement to the outside when heated. According to the material and diameter of the nanowires to be measured, the cross-section of the thermal bimetal sheet is rectangular, the thickness is between 0.25mm-0.5mm, and the width of the bimetal layer is between 0.25mm-1mm. According to the size of the inner diameter of the metal ring, the thermal bimetal The length of the sheet is between 1.6mm-2.5mm, and it is advisable to fix one end on the metal ring and one end to hang freely on the metal ring. In the present invention, in order to ensure greater bending deformation at a lower temperature, it is recommended to use a bimetal sheet with a ratio bending greater than 10/10-6 ·°C-1 .
进一步地，两个热双金属片或金属片与金属丝可以平行排列或以V字形排列，为了保证较短的纳米线或薄膜能够固定在两个金属片或金属片与金属丝之间，平行排列的间隙要求小于2μm，V字形排列开口角度在5度-45度之间。平行排列的结构对于拉伸较长(≥5μm)的纳米线比较合适，V字行排列的结构可以根据纳米线的长度和变形量的大小，固定在V字口的不同部位进行拉伸。由两个双金属片驱动的载网可以实现双向拉伸变形，由一个双金属片驱动的载网可以实现单向拉伸变形。Further, two thermal bimetallic sheets or metal sheets and metal wires can be arranged in parallel or in a V shape. In order to ensure that shorter nanowires or films can be fixed between the two metal sheets or metal sheets and metal wires, parallel The gap of the arrangement is required to be less than 2 μm, and the opening angle of the V-shaped arrangement is between 5 degrees and 45 degrees. The structure arranged in parallel is more suitable for stretching longer (≥5 μm) nanowires, and the structure arranged in V-shaped rows can be fixed at different parts of the V-shaped mouth for stretching according to the length and deformation of the nanowires. The grid driven by two bimetals can realize bidirectional tensile deformation, and the grid driven by a bimetal can realize unidirectional tensile deformation.
本发明的热双金属片驱动的智能透射电子显微镜载网对纳米材料实行原位动态测试通过如下步骤实施：The smart transmission electron microscope grid driven by the thermal bimetal of the present invention performs in-situ dynamic testing of nanomaterials through the following steps:
1.将纳米线或纳米薄膜固定在金属丝与双金属片之间或双金属片与双金属片之间，将载网固定在带有热台的透射电镜样品杆上，放入透射电镜中。1. Fix the nanowire or nanofilm between the metal wire and the bimetallic sheet or between the bimetallic sheet and the bimetallic sheet, fix the grid on the TEM sample rod with a hot stage, and put it into the TEM.
2.通过双倾透射电镜的热台将样品倾转到最容易观察的正带轴下，对载网进行加热。2. Tilt the sample to the most easily observed positive belt axis through the hot stage of the double-tilt transmission electron microscope, and heat the grid.
3.随着温度的升高热双金属片发生向外侧弯曲变形，拉伸固定在其上的纳米线或薄膜发生变形。3. As the temperature rises, the thermal bimetal sheet bends and deforms outward, and the nanowire or film fixed on it is deformed.
4.通过透射电子显微镜的高分辨原子图像实时原位记录纳米线的变形过程以及晶格结构变化。4. Real-time in-situ recording of the deformation process and lattice structure changes of the nanowires through the high-resolution atomic images of the transmission electron microscope.
5.通过对变形前后纳米材料微结构变化的实时高分辨图像的对比分析，可以在原子层次上揭示纳米材料在弹塑性变形的特点，变形的尺寸效应，变形过程中位错的产生，以及裂纹的扩展变等反映材料力学性能的微观组织结构。5. Through the comparative analysis of the real-time high-resolution images of the microstructure changes of nanomaterials before and after deformation, the characteristics of elastic-plastic deformation of nanomaterials, the size effect of deformation, the generation of dislocations during deformation, and cracks can be revealed at the atomic level The expansion variation of the material reflects the microstructure of the mechanical properties of the material.
本发明有如下优点：The present invention has following advantage:
1.本发明对透射电镜载网进行了新的结构设计，实现在透射电镜中原位操纵纳米材料，提供了一种新的纳米线或薄膜的原位力学测试方法，具有性能可靠，安装方便，结构简单的特点，拓展了透射电镜的功能。1. The present invention has a new structural design for the transmission electron microscope grid, realizes in-situ manipulation of nanomaterials in the transmission electron microscope, and provides a new in-situ mechanical testing method for nanowires or films, which has reliable performance and is easy to install. The simple structure expands the function of the transmission electron microscope.
2.本发明中的载网外形尺寸与现有技术载网基本一致，可以方便的装入高分辨透射电镜中，可以实现X，Y两个方向大角度倾转，可以在原位拉伸变形的同时从最佳的晶带轴实现高分辨成像。2. The outer dimensions of the carrier grid in the present invention are basically the same as those of the prior art carrier grid, and can be easily loaded into a high-resolution transmission electron microscope, can realize large-angle tilting in X and Y directions, and can be stretched and deformed in situ Simultaneously achieve high-resolution imaging from the best crystal zone axis.
附图说明Description of drawings
图1两双金属片平行排列双向驱动的载网Figure 1 Two-way driving grid with two bimetallic sheets arranged in parallel
图2两双金属片呈V字形排列的双向驱动的载网Figure 2 Two-way driven grid with two bimetallic sheets arranged in a V shape
图3一便为固定的金属丝另一边为双金属片单向驱动的载网。Fig. 3 just is that the other side of fixed metal wire is the carrying net that bimetal sheet unidirectional drives.
其中，图中虚线示意为受热后变形结构Among them, the dotted line in the figure shows the deformed structure after heating
图面说明如下The drawings are as follows
1金属环 2热双金属片 3压片 4金属丝1 metal ring 2 thermal bimetallic sheet 3 pressing sheet 4 metal wire
具体实施方式：Detailed ways:
按图1利用大的线膨胀系数的Mn72Ni10Cu18合金和较小线膨胀系数的Ni36合金压合的热双金属片，将双金属片加工为厚度0.5mm，宽度0.25mm，长度为2mm，并平行排列，在光学显微镜下利用压片将双金属片一端粘结固定在中间开孔为1.5mm的铜环上面，两双金属片之间的距离保持为2μm，在扫描电子显微镜中利用机械手将一根长为10μm。直径为80nm的SiC纳米线固定在两双金属片上，将做好的载网固定在带有热台的透射电镜样品杆上，放入透射电镜样品室中，通过倾转样品杆使SiC纳米线[011]晶带轴平行于电子束的方向，调整光栅和放大倍数，SiC纳米线呈高分辨原子晶格图像，通过样品杆热台控制载网的温度，从20℃到200℃逐渐升高温度，热双金属片向两侧弯曲，缓慢拉伸SiC纳米线变形，同时通过高分辨原位成像系统记录了变形过程。According to Figure 1, use the thermal bimetal sheet pressed by the Mn72Ni10Cu18 alloy with a large linear expansion coefficient and the Ni36 alloy with a small linear expansion coefficient to process the bimetal sheet into a thickness of 0.5mm, a width of 0.25mm, and a length of 2mm, and arrange them in parallel Under the optical microscope, one end of the bimetallic sheet was bonded and fixed on the copper ring with a hole in the middle of 1.5mm by using a pressure sheet, and the distance between the two bimetallic sheets was kept at 2μm. The length is 10 μm. SiC nanowires with a diameter of 80nm are fixed on two double metal sheets, and the prepared grid is fixed on the sample rod of the transmission electron microscope with a hot stage, and placed in the sample chamber of the transmission electron microscope, and the SiC nanowires are made by tilting the sample rod. [011] The crystal zone axis is parallel to the direction of the electron beam, adjust the grating and magnification, and the SiC nanowire presents a high-resolution atomic lattice image, and the temperature of the grid is controlled by the sample rod hot stage, and gradually increases from 20°C to 200°C temperature, the hot bimetal bends to both sides, slowly stretches the SiC nanowires to deform, and at the same time records the deformation process through a high-resolution in situ imaging system.
通过实施例，发现SiC纳米线在断裂前发生了超过5％的弹性和塑性应变，微观结构变化表明SiC在纳米尺度下表现出与大块体材料不同的变形方式。Through the examples, it is found that SiC nanowires have more than 5% elastic and plastic strain before breaking, and the microstructure changes indicate that SiC exhibits different deformation modes from bulk materials at the nanoscale.
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