WO2012162929A1 - 透射电镜用双轴倾转的原位力、电性能综合测试样品杆 - Google Patents

透射电镜用双轴倾转的原位力、电性能综合测试样品杆 Download PDF

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WO2012162929A1
WO2012162929A1 PCT/CN2011/077033 CN2011077033W WO2012162929A1 WO 2012162929 A1 WO2012162929 A1 WO 2012162929A1 CN 2011077033 W CN2011077033 W CN 2011077033W WO 2012162929 A1 WO2012162929 A1 WO 2012162929A1
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Prior art keywords
sensor
sample
electrode
stress
queue
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PCT/CN2011/077033
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English (en)
French (fr)
Inventor
韩晓东
岳永海
张跃飞
刘攀
郑坤
张泽
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北京工业大学
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Priority to US13/519,291 priority Critical patent/US8569714B2/en
Priority to JP2013516990A priority patent/JP5394596B2/ja
Publication of WO2012162929A1 publication Critical patent/WO2012162929A1/zh

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Classifications

    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/02—Details
    • H01J37/20—Means for supporting or positioning the objects or the material; Means for adjusting diaphragms or lenses associated with the support
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/02—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material
    • G01N23/04—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material and forming images of the material
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
    • G01N3/08—Investigating strength properties of solid materials by application of mechanical stress by applying steady tensile or compressive forces
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/26—Electron or ion microscopes; Electron or ion diffraction tubes
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
    • G01N2203/02—Details not specific for a particular testing method
    • G01N2203/026—Specifications of the specimen
    • G01N2203/0286—Miniature specimen; Testing on microregions of a specimen
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00—Investigating materials by wave or particle radiation
    • G01N2223/30—Accessories, mechanical or electrical features
    • G01N2223/307—Accessories, mechanical or electrical features cuvettes-sample holders
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
    • H01J2237/20—Positioning, supporting, modifying or maintaining the physical state of objects being observed or treated
    • H01J2237/202—Movement
    • H01J2237/20207—Tilt
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
    • H01J2237/20—Positioning, supporting, modifying or maintaining the physical state of objects being observed or treated
    • H01J2237/206—Modifying objects while observing
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
    • H01J2237/20—Positioning, supporting, modifying or maintaining the physical state of objects being observed or treated
    • H01J2237/206—Modifying objects while observing
    • H01J2237/2062—Mechanical constraints

Definitions

  • the invention relates to a comprehensive performance test sample rod for a transmission electron microscope, which realizes the comprehensive performance of the material while loading the stress in the plane of the sample while achieving a large angle tilting along a pair of orthogonal axes.
  • the test from the atomic scale to the micro-domain deformation in-situ dynamic real-time study.
  • the invention belongs to the field of transmission electron microscope accessories and nanometer material in situ measurement research.
  • transmission electron microscopy Since the invention of transmission electron microscopy in the 1930s (1932), especially in the past two decades, transmission electron microscopy has been distinguished by spatial resolution and monochromatic light source represented by spherical aberration correction technology. Great progress has been made in the fields of time and resolution represented by high-speed CCD cameras, and has made great contributions to the advancement of science and technology in the fields of physics, chemistry, biology, materials science, and electronic information technology. At the same time, in-situ field technology, as one of the important development directions of transmission electron microscopy in recent years, has attracted more and more research fields.
  • the 654 and 671 TEM sample rods produced by Gatan Company of the United States can realize the in-situ stretching of samples under uniaxial (X-axis) tilting conditions in TEM. Based on this technology, the transmission of single-dip stretching table is utilized. The recoverable properties of the deformed twins in pure aluminum were observed in real time by electron microscopy. In Nanofa, Sweden, the company developed the in-situ deformation technique in TEM for the study of tensile, compressive and bending deformation nanowires under uniaxial (X-axis) tilting conditions, and studied the plastic deformation behavior.
  • the PI 95 transmission electron microscopy picometer indenter from Hysi trcm can also be used to study the plastic deformation behavior of various nanomaterials in situ under uniaxial (X-axis) tilting conditions in transmission electron microscopy.
  • X-axis uniaxial
  • the above-mentioned commercial TEM deformation device provides favorable conditions for in-situ study of changes in microstructure during deformation of nanomaterials. Tools, but there is a technical bottleneck obstacle: Commercial TEM in situ mechanical behavior sample stretching table is basically uniaxial tilting, and it is impossible to achieve tilting along the Y axis.
  • the above methods are required to load the sample stress by installing a complex mechanical transmission on the TEM sample rod. Since these devices are mounted on the TEM sample rod, the sample rod is loaded into the transmission.
  • the stress loading of the sample can only be achieved under uniaxial tilting (X-axis).
  • X-axis uniaxial tilting
  • the tilting of the Y-axis cannot be achieved.
  • the object of the present invention is to provide a sample rod for in-situ force and electrical performance comprehensive testing of biaxial tilting for transmission electron microscopy, which mainly includes a self-designed transmission electron microscope hollow sample rod (hereinafter referred to as a sample rod).
  • a sample rod for in-situ force and electrical performance comprehensive testing of biaxial tilting for transmission electron microscopy, which mainly includes a self-designed transmission electron microscope hollow sample rod (hereinafter referred to as a sample rod).
  • the power performance sensor the tablet, the front end of the sample head, the sensor stage; wherein, the force performance sensor is fixed on the sensor stage on the front end of the sample rod by a tablet, and the sensor stage passes the shaft and the sample rod on both sides
  • the front end is connected and can be rotated around the two axes in a plane perpendicular to the front end of the sample stalk (ie, about the x-axis, ⁇ 30 °); the electrode on the force sensor is connected to the front end of the sample rod by a tablet.
  • the wire in the hollow sample is connected to an external test device to realize in-plane loading of the force electrical signal (in the sensor plane) and real-time monitoring of the feedback. Therefore, it is possible to obtain the force and electrical comprehensive performance parameters by diverting the sample under study to the low-index positive band axis to realize the in-situ atomic scale observation.
  • a double-axis tilting in-situ force and electrical performance comprehensive test sample rod for transmission electron microscopy mainly includes a handle 1, a sample rod 2, a sample head
  • the front end 3, the sensor stage 4 is fixed on the front end 3 of the sample head by two support shafts 5 located inside the front end 3 of the sample head, and is tilted about the support shaft 5 in a plane perpendicular to the sample head (ie, rotating about the x-axis, ⁇ 30 ° , as shown in Figure 5
  • a wire I 6 introduced from the outside of the electron microscope through the sample rod 2 is symmetrically distributed, and is connected to the array electrode 17 which is distributed on both side walls of the front end 3 of the sample head.
  • the other end of the wire 16 is connected to the electrode interface 8 on the handle, and is connected to the external device of the electron mirror through the electrode interface 8.
  • the position of the queue electrode I 7 is symmetrically distributed on the both side walls of the front end 3 of the sample head with the support axis 5 as a center line.
  • the rotation of the sensor stage 4 is driven by a Y-axis tilt drive 9 at its tail.
  • a groove 10 is formed on the sensor stage 4 with the support shaft 5 as a center line.
  • the groove 10 is a through hole, and the lower portion has a supporting edge to support the sensor 11.
  • the thickness of the sensor 11 is designed such that it is placed in the groove.
  • the plane of the rear upper surface lies in the same plane as the center of focus of the TEM electron beam, so that the xenon electron beam passes through the slit and the groove 10 on the sensor 11 and is focused on the sample 12 located on the upper surface of the sensor 11.
  • a through hole I is formed at a position of the sensor stage 4 away from the support shaft 5 near the Y-axis tilting drive 9.
  • the through hole I 13 causes the sensor stage 4 to tilt around the Y axis and the sample stalk is entirely around the X.
  • the sensor stage 4 does not come into contact with the pole piece of the electron microscope when the shaft is tilted.
  • Two rows of queue electrodes II are prepared symmetrically on the side of the support shaft 5, and two rows of queue electrodes III are also prepared on the tablet 15, and each queue electrode III 16 is distributed in two upper and lower faces of the tablet.
  • the two electrodes are connected by wires; after the sensor 11 is placed in the recess 10 of the sensor stage 4, the pressing piece 15 is pressed against the sensor 11, and the precise design ensures that the array electrode III 16 is distributed on the sheet.
  • the electrodes on the lower surface of the 15 are connected to the array electrode II 14 on the sensor 11 in a one-to-one correspondence, the pressing piece 15 is fixed on the sensor stage 4, and the electrode and distribution of the array electrode III 16 on the upper surface of the pressing sheet 15 are arranged by wires.
  • the queue electrodes I 7 - one corresponding to each other on both sides of the front end 3 of the sample head are connected.
  • the pressing piece 15 is provided with a through hole II 17, so that the electron beam is condensed on the sample 12 of the sensor 11 through the pressing sheet.
  • the sensor 1 1 includes a queue electrode II 14, a stress applying portion # 18, a stress testing member 19, a test electrode 20, and a sample 12 to be studied.
  • the stress applying member 18 and the stress testing member 19 are arranged in parallel on the sensor 11, parallel to the queue.
  • the electrode II 14 is placed between the two rows of the queue electrodes 1114, a slit for the passage of the electron beam between the stress applying member 18 and the stress test member 19, and two tests are performed on the stress applying member 18 and the stress test member 19.
  • the electrode 20, the two ends of the sample 12 are respectively mounted on the test electrode 20 on the stress applying member 18 and the stress test member 19 and span a slit through which the electron beam is passed; the stress applying member 18 and the stress test portion
  • the circuit of the test electrode 20 is connected to the queue electrode III 14 formed on the sensor 11 through a wire.
  • the stress applying member 18 is made of a material such as a hot bimetal, a piezoelectric ceramic, a memory alloy, or the like which is deformed by an external heating field or an electric field, so as to be away from or approach the stress testing member 19, thereby fixing the both ends to the stress applying member.
  • the sample 12 on the 18 and the stress test component 19 exerts a tensile or compressive force to effect loading of the in-plane stress of the sample 12.
  • the stress testing component 19 utilizes the currently commercially available cantilever beam technology to accurately design the cantilever beam structure and to fabricate structures and devices on the cantilever beam that accurately measure the stress signal when the stress applying component 18 applies stress to the sample 12.
  • Real-time monitoring of the stress signal is achieved by converting the signal of the stress change caused by the shape change of the cantilever beam into an electrical signal output to an external test device through a test device located outside the electron microscope.
  • the sensor stage 4 and the sample rod 2 are tilted about the Y axis and the X axis, so that the in-situ atomic scale observation is performed while the sample is located.
  • the loading of the sample stress is realized in the plane, and the changes of the signals such as the force and power are monitored in real time through external signal input and output devices.
  • the electrode leads 4 are all electrically conductive materials with an insulating layer attached thereto.
  • the sample head front end 3, the sensor stage 4, and the surface of the pressing piece 15 are distributed with an insulating dielectric layer, and the insulating dielectric layer material may be silicon dioxide, silicon carbide, silicon nitride, and oxidation. Insulating materials such as enamel.
  • the queue electrode 177, the argon electrode ⁇ 14, and the queue electrode ⁇ 16 are all made of a material having good electrical conductivity, and may be Rh, Pd, Rti/Aii, Ti/Au, W/Pt, Cr/Pt. , Ni /Pt, Ag or Cu.
  • the invention produces a sample cup for in-situ mechanical and electrical performance test of biaxial tilting in transmission electron microscope through precise mechanical processing and semiconductor processing technology, and realizes in-situ mechanics of materials in transmission electron microscopy. Electrical comprehensive performance test.
  • the invention utilizes precise structural design, the sample rod can realize high angle tilting in two directions of X and Y, realize high resolution imaging from the optimal ribbon axis, and directly reveal the nano material in the in-plane stress from the atomic scale.
  • the invention is applicable not only to one-dimensional nanostructures such as nanowires, nanobelts, nanotubes, but also to two-dimensional film materials, as well as TEM samples prepared from bulk materials. A powerful in situ research tool can be provided for the deformation mechanism of the material.
  • the invention utilizes the precise structural design to solve the defects caused by directly introducing the electrode lead into the sample in the prior art, and the length of the wire connecting the sample and the external device is greatly shortened by the transfer of the tablet. This makes it possible to limit the tilting of the Y-axis in the case of a multi-electrode lead.
  • the invention can design the sensor according to the need to achieve the performance test purpose, that is, the sensor can be various, and the design can be used to test the corresponding performance under the original scale resolution.
  • Figure 5 Stereo view of the front end of the sample head about the Y axis
  • the test sample rod mainly comprises a handle 1, a sample rod 2, a sample head front end 3, and a sensor stage 4 fixed on the front end 3 of the sample head through two support shafts 5 located inside the front end 3 of the sample head, around the support shaft 5 Tilting in a plane perpendicular to the sample head (ie, rotating about the Y axis, ⁇ 30°), on the walls on both sides of the front end 3 of the sample head, symmetrically distributed with wires I6 introduced from the outside of the electron microscope through the sample rod 2 and
  • the queuing electrode I 7 is distributed on the two side walls of the front end 3 of the sample head, and the other end of the wire I 6 is connected to the electrode interface 8 on the handle, and is connected to the external device of the electron microscope through the electrode interface 8.
  • the position of the queue electrode I 7 is symmetrically distributed on the front wall 3 of the sample head with the support shaft 5 as a center line.
  • the rotation of the sensor stage 4 is driven by a Y-axis tilt drive 9 at its tail.
  • a groove 10 is formed on the sensor stage 4 with the support shaft 5 as a center line, the groove 10 is a through, the lower portion has a supporting edge to support the sensor 11, and the sensor stage 4 is away from the support shaft 5 near the Y axis.
  • the position of the tilting drive 9 is made with a through hole I13.
  • the through hole I13 ensures that the sensor stage 4 does not contact the pole piece of the electron microscope when rotating around the Y axis and when the sample rod is rotated around the X axis, so as not to cause Damage to the electron microscope.
  • the sensor 11 is a commercially available sensor.
  • the stress applying member 18 is based on a hot bimetal.
  • the thermal resistance and the thermocouple element are prepared on the bimetal.
  • the stress test component 19 is based on a Si cantilever beam. To measure the fine deflection displacement and convert the stress signal into a Wheatstone bridge system by an external test device, the sample 12 is fixed on the test electrode 20 on the sensor 11, and the specific assembly drawing is as shown in FIG.
  • the sensor 11 is fixed on the sensor stage 4 by the pressing piece 15, and the electrode of the queue electrode III16 on the pressing piece 15 under the pressing piece is connected with the array electrode II 14 - which is formed on the sensor 11, and the sensor is connected.
  • the thickness of the 11 is in the same plane as the depth of the groove 10 and the center of focus of the TEM electron beam, so that the TEM electron beam passes through the slit in the sensor 11 and the through hole of the groove 10 and is focused on the sample 12 fixed on the sensor 11.
  • the electrode of the queue electrode III16 on the upper surface of the pressing piece 15 is connected to the column electrode T7 distributed on both sides of the front end 3 of the sample head in a one-to-one correspondence by a wire, and the electron beam is condensed through the through hole II 17 formed on the pressing piece 15 On sample 12.
  • the sample cup assembled as shown in FIG. 4 is placed in a transmission electron microscope, and the electrode interface 8 on the sample rod is connected to the external test device by a wire. Open the electron beam of the TEM, find the sample to be studied in the finder window, if it is a single crystal sample, tilt the sample to the low-index positive belt axis you want to observe, and use the external test equipment to stress the sensor 11.
  • the application member 18 applies a drive signal to apply a force to the sample 12,
  • the stress and strain are detected by the signal fed back to the external test equipment by the stress test component 19, and at the same time, the test electrode 20 applies an electrical signal to the sample, and the TEM is observed under the TEM image acquisition system.
  • Mechanism and corresponding mechanisms of electricity are described in detail below.
  • Fig. 7a is a transmission electron micrograph of a polycrystalline film sample
  • the inset is a selected area electron diffraction pattern
  • Fig. 7b is a stress-strain curve of the polycrystalline A1 film sample obtained by using the test sample rod during tensile deformation. .
  • the senor 11 can also be used in our previous patent: a thermal bimetal driven transmission electron microscope carrier, patent number: ZL2006I0144031. X; transmission electron microscope ⁇ nano material stress test network, patent number: ZL200810056836. 8; Quantitative test force electrical performance and microstructure of the sensor and its manufacturing method, patent application number: 200920269907. 2 made of the network and sensors, to achieve the measurement of sample performance.

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Abstract

透射电镜用双轴倾转的原位力、电性能综合测试样品杆包括透射电镜样品杆，力电性能传感器，压片，样品头前端，传感器载台；力电性能传感器通过压片固定在样品杆前端上的传感器载台上，传感器载台通过位于两侧的转轴与样品杆前端连接并且可以绕这两个转轴在垂直于样品杆前端的平面内旋转（即绕着Y轴旋转，±30°）；力电性能传感器上的电极通过压片连接到位于样品杆前端两侧的电极上，经样品杆内的导线连接到外部测试设备上实现力电信号的面内加载（传感器平面内）及反馈的实时监测。本发明可将研究样品倾转到低指数正带轴下实现原位原子尺度观察的同时获得力、电综合性能参数。

Description

,
- ½ 透射电镜用双轴倾转的原位力、 电性能综合测试样品秆 技术领域：
本发明涉及一种用于透射电镜的综合性能测试样品杆，该样品杆 在实现沿一对正交轴大角度倾转的同时，实现在样品所在平面内应力 的加载的同时实现材料综合性能的测试，从原子尺度对 ^料微区变形 原位动态实时研究。该发明属于透射电子显微镜配件及纳米^料原位 测量研究领域。
背景技术：
自上世纪三十年代（1932 年)透射电子显微镜发明以来， 特别是 近二十年来，透射电子显微学技术在以球差矫正技术为代表的空间分 辨率、单色光源为代表的能量分辨率、 高速 CCD相机为代表的时间分 辨率等领域都取得了巨大进步， 为物理学、化学、生物学、材料科学、 电子信息技术等领域的科技进步做出了巨大贡献。与此同时， 原位外 场技术作为透射电子显微学近年的重要发展方向之一，已经为越来越 多的研究领域关注。 透射电子显微学原位外场技术为物理学、 化学、 生物学、材料科学、 电子信息技术等领域的深入科学研究提供了崭新 物理图像， 为发展新原理、 新应用提供了重要机遇。直接在原子点阵 尺度研究物质的结构及其演化过程是理解物理、化学和材料科学的重 要基础。但目前由于瓶颈性技术的限制， 研究者多采 ^透射电子显微 镜对材料中的塑性变形行为进行静态的非原位研究，由于缺乏直观的 显微结构演化规律， 对于许多科学问题不能给出确切的结论。
美国 Gatan公司生产的 654、 671型透射电镜样品杆， 可以实现 透射电镜中单轴 （X轴）倾转条件下样品的原位拉伸， 以此技术为依 托，利用单倾拉伸台的透射电镜实时观测到纯铝中形变孪晶的可恢复 特性。瑞典 Nanofa,ctory公司设 生产了透射电镜中原位变形技术用 于单轴 （X轴） 倾转条件下研究拉伸、 压缩、 弯曲变形纳米线， 并对 其塑性变形行为进行研究。 美国 Hysi trcm公司的 PI 95 透射电镜皮 米压痕仪也可用于单轴 （X轴） 倾转条件下， 在透射电镜中原位压缩 变形各种纳米材料研究其塑性变形行为。虽然上述商业化透射电镜变 形装置为原位研究纳米材料变形过程中显微结构的变化提供了有利 工具， 但存在一个技术性的瓶颈性障碍： 商业化透射电镜原位力学行 为样品拉伸台基本为单轴倾转， 无法实现沿 Y轴的倾转。 此外， 尽管 商用的双轴倾转样品杆技术已经非常成熟，但是这些样品杯只能实现 对样品观察而无法实现双轴倾转条件下在样品平面内对样品的应力 加载， 从而限制了研究者从原子尺度下原位研究材料的变形、 断裂、 相变等机制。
需要特别指出的是，以上这些方法 要是通过在透射电子显微镜 样品杆上安装复杂的机械传动装置来实现对样品应力的加载，由于这 些装置安装在透射电镜样品杆上，致使样品杆在装入透射电镜中只能 在单轴倾转（X轴）下对样品实现应力的加载，对于需要在原子尺度正 带轴下原位研究材料相关性能的情况， 由于无法实现在 Y轴的倾转前 提下实现样品所在平面内应力的加载，很难有机会在高分辨状态或原 子层次进行原位变形动态研究，这样就对人们正确的理解材料的性能 带来了巨大的挑战。
发明内容：
针对现有技术存在的问题，本发明的目的是提供一种透射电镜用 双轴倾转的原位力、 电性能综合测试样品杆， 主要包括自设计透射电 镜中空样品杆 （以下简称样品杆）， 力电性能传感器， 压片， 样品头 前端， 传感器载台； 其中， 力电性能传感器通过压片固定在样品杆前 端上的传感器载台上，传感器载台通过位于两侧的转轴与样品杆前端 连接并 ϋ可以绕这两个转轴在垂直于样品秆前端的平面内旋转（即绕 着 Υ轴旋转， ± 30 ° )； 力电性能传感器上的电极通过压片连接到位 于样品杆前端两侧的电极上，经中空样品杼内的导线连接到外部测试 设备上实现力电信号的面内加载（传感器平面内）及反馈的实时监测。 从而可以将所研究的样品倾转到低指数正带轴下实现原位原子尺度 观察的 ί司时获得力、 电综合性能参数。
为了实现上述目的， 本发明是通过如下的技术方案来实现的： 一种透射电镜用双轴倾转的原位力、电性能综合测试样品杆主要 包括手握柄 1， 样品杆 2， 样品头前端 3， 传感器载台 4通过位于样 品头前端 3两内侧的两个支撑轴 5固定在样品头前端 3上，绕支撑轴 5在垂直于样品头的平面内倾转 （即绕着 Υ轴旋转， ± 30 ° ， 如图 5 所示）， 在样品头前端 3两侧的壁上， 对称分布有从电镜外部通过样 品杆 2引入的导线 I 6,并与分布在样品头前端 3两侧壁上的队列电 极 1 7相连， 导线 1 6的另一端连接在手握柄上的电极接口 8上， 通 过电极接口 8与电镜外部设备相连。 队列电极 I 7的位置为以支撑轴 5为中心线对称分布在样品头前端 3两侧壁上。 传感器载台 4的旋转 是通过位于其尾部的 Y轴倾转驱动器 9驱动。在传感器载台 4上以支 撑轴 5为中心线制作了一个凹槽 10， 凹槽 10为一个通孔， 下部有支 撑沿来支撑传感器 1 1， 传感器 11 的厚度设计成使得其放入凹槽 10 后上表面所在平面与 TEM电子束聚焦中心位于同一平面内，使 ΊΈΜ电 子束通过传感器 11上的缝隙和凹槽 10并聚焦在位于传感器 1 1上表 面的样品 12上。
此外在传感器载台 4的远离支撑轴 5靠近 Y轴倾转驱动器 9的位 置制作了一个通孔 I 13， 通孔 I 13使传感器载台 4在绕 Y轴倾转时 以及样品秆整体绕 X轴倾转时传感器载台 4不会与电镜的极靴接触。 传感器 11靠近两侧支撑轴 5对称制备了两排队列电极 II 14，压片 15 上同样制备了两排队列电极 III 16，每一队队列电极 III 16都为分 布于压片上下两个面内的两个电极， 这两个电极通过导线连接； 传感 器 11放入传感器载台 4的凹槽 10中后，将压片 15压在传感器 11上， 精确的设计确保队列电极 III 16分布于压片 15下表面的电极与传感 器 11上的队列电极 I I 14一一对应相连接， 将压片 15固定在传感器 载台 4上， 用导线将队列电极 III 16分布于压片 15上表面的电极与 分布在样品头前端 3两侧的队列电极 I 7—一对应相连接。
此外， 压片 15上设有一个通孔 II 17， 使电子束透过压片会聚 在传感器 1 1的样品 12上。 传感器 1 1上包括队列电极 I I 14， 应力 施加部 # 18， 应力测试部件 19， 测试电极 20以及待研究的样品 12 , 应力施加部件 18与应力测试部件 19并行排列在传感器 11上， 平行 于队列电极 II 14放置并在两列队列电极 1114之间， 应力施加部件 18与应力测试部件 19中间有供电子束通过的一狹缝， 在应力施加部 件 18和应力测试部件 19上制作了两个测试电极 20， 样品 12两端分 别搭载在应力施加部件 18和应力测试部件 19上的测试电极 20上并 且横跨上述供电子束通过的一狭缝； 应力施加部件 18、 应力测试部 件 19、 测试电极 20的电路都通过导线与传感器 11上制作的队列电 极 III 14对应连接。 应力施加部件 18采用热双金属片， 压电陶瓷， 记忆合金等在外加热场或电场作用下发生变形的材料，使其本身远离 或逼近应力测试部件 19， 从而对两端分别固定在应力施加部件 18和 应力测试部件 19上的样品 12施加拉力或者压缩力的作用，实现对样 品 12面内应力的加载。应力测试部件 19采^目前商业上成熟的悬臂 梁技术， 通过精确设计悬臂梁结构， 并在悬臂梁上制备能精确测量应 力信号的结构和装置，当应力施加部件 18对样品 12施加应力作用时 通过位于电镜外部的测试设备将由于悬臂梁形状改变引起的应力变 化的信号转换成电学信号输出到外部测试设备上，实现应力信号的实 时监测。
所述的传感器 1 安装在传感器载台 4上后随着传感器载台 4以 及样品杆 2绕着 Y轴和 X轴双轴倾转，这样就实现在原位原子尺度观 察的同时， 在样品所在平面内实现对样品应力的加载， 通过外部信号 输入和输出设备实时监测力电等信号的变化。
进一步地， 所述的电极引线 4 都为外部附有绝缘层的导电性材 料。
进一步地， 所述的样品头前端 3， 传感器载台 4， 以及压片 15的 表面都分布有绝缘介电层， 该绝缘介电层材料可以是二氧化硅， 碳化 硅， 氮化硅， 氧化铪等绝缘材料。
进一步地， 所述的队列电极 1 7， 队列电极 Π 14， 队列电极工 Π 16均采用导电性能良好的材料，可以是 Rh， Pd， Rti/Aii, Ti/Au, W/Pt, Cr/Pt, Ni /Pt, Ag或 Cu。
本发明有如下优点：
1.本发明通过精密的机械加工， 半导体加工技术， 制作了一种透 射电子显微镜用双轴倾转原位力学、 电学性能综合测试样品杯， 实现 了在透射电镜中对材料的原位力学、 电学综合性能测试。
2.本发明利用精密的结构设计， 该样品杆可以实现 X, Y两个方 向大角度倾转， 从最佳的晶带轴实现高分辨成像， 从原子尺度直接揭 示纳米材料在受到面内应力作用下的力学相应机制以及电学相应机 制。 3.本发明不仅适用于诸如纳米线、 纳米带、 纳米管等一维纳米 结构，同样适用于二维的薄膜材料，以及体材料制备的透射电镜样品。 可以为材料的变形机制提供强有力的原位研究工具。
4.本发明利用精密的结构设计， 解决了现有技术上将电极引线 直接引入样品所带来的缺陷， 通过压片的转接， 大大缩短了连接样品 和外部设备的导线的长度，丛而使得在多电极引线情况下不限制 Y轴 的倾转。
5.本发明可以根据需要自行设计传感器实现所想要达到性能测 试目的， 即传感器可以是多种多样的， 利用本设计都可以实现原位原 子尺度分辨下相应性能的测试。
險图说明
图 1 透射电镜用双轴倾转原位力、 电性能综合测试样品杆效果 图
图 2 样品头前端放大图
图 3 样品头前端传感器装配立体图
图 4 装配完成的样品头前端俯视图
图 5 样品头前端绕 Y轴倾转立体图
图 6 传感器平面示意图
图 7 多晶 A1薄膜的透射电镜照片及测得的应力应变曲线 附图说明如下
1 手握柄 2样品杆 3样品头前端 4传感器载台
5 支撑轴 6导线 7 队列电极 I 8 电极接口
9 Y轴倾转驱动器 10 凹槽 11传感器 12 样品
13 通孔 I 14 队列电极 II 15压片 16队列电极 III
17 通孔 Π 18 应力施加部件 19 应力测试部件 20测试电 极 具体实施方式：
下面结合附图对本发明做进一步的详细说明。
如图 1， 2 所示， 透射电镜用双轴倾转的原位力、 电性能综合测 试样品杆主要包括手握柄 1 , 样品杆 2 , 样品头前端 3， 传感器载台 4 通过位于样品头前端 3 两内侧的两个支撑轴 5 固定在样品头前端 3 上， 绕支撑轴 5在垂直于样品头的平面内倾转 （即绕着 Y轴旋转， ±30° )， 在样品头前端 3两侧的壁上， 对称分布有从电镜外部通过 样品杆 2引入的导线 I 6，并与分布在样品头前端 3两侧壁上的队列 电极 I 7相连， 导线 I 6的另一端连接在手握柄上的电极接口 8上， 通过电极接口 8与电镜外部设备相连。 队列电极 I 7的位置为以支撑 轴 5为中心线对称分布在样品头前端 3两测壁上。传感器载台 4的旋 转是通过位于其尾部的 Y轴倾转驱动器 9驱动。在传感器载台 4上以 支撑轴 5为中心线制作了一个凹槽 10， 凹槽 10为一个通 ， 下部有 支撑沿来支撑传感器 11，此外在传感器载台 4的远离支撑轴 5靠近 Y 轴倾转驱动器 9的位置制作了一个通孔 I 13， 通孔 I 13确保传感器 载台 4在绕 Y轴旋转的时候以及样品杆整体绕 X轴旋转时不会与电镜 的极靴接触， 以免造成对电镜的损害。 传感器 11采用购买的商业制 作传感器， 应力施加部件 18基于一条热双金属片， 在双金属片上制 备了力 Π热电阻与热电偶原件， 应力测试部件 19基于一条 Si悬臂梁， 其侧面制备了用来测量精细偏转位移并通过外部测试设备转换成应 力信号的惠斯通电桥系统，将样品 12固定在传感器 11上的测试电极 20上， 具体装配图如图 3所示， 将传感器 11放入凹槽 10内， 用压 片 15将传感器 11固定在传感器载台 4上，压片 15上的队列电极 III16 位于压片下方的电极与传感器 11上制作的队列电极 II 14 -一一对应 相连，传感器 11厚度与凹槽 10的深度与 TEM电子束聚焦中心位置在 同一平面内，使 TEM电子束通过传感器 11上的缝隙和凹槽 10的通孔 并聚焦在固定在传感器 11上的样品 12上。 用导线将队列电极 III16 位于压片 15上表面的电极与分布于样品头前端 3上两侧的^列电极 T7一一对应相连接， 电子束通过压片 15上制作的通孔 II 17会聚在 样品 12上。 将如图 4所示装配好的样品杯放入透射电镜中， 用导线 将样品杆上的电极接口 8与外部测试设备对应相连。打开透射电镜的 电子束， 在取景窗中找到所要研究的样品， 如果是单晶样品， 将样品 倾转到所想要观察的低指数正带轴下， 利用外部测试设备对传感器 11上的应力施加部件 18施加驱动信号， 给样品 12施加力的作用， 通过应力测试部件 19反馈到外部测试设备上的信号进行应力应变的 检测， 同时， 利 ^测试电极 20对样品施加电学信号， 在透射电镜图 像采集系统下观测样品 12在收到应力作用下力学相应机制以及电学 相应机制。
如图 7所示， 图 7a为多晶 薄膜样品的透射电镜照片， 插图为 选区电子衍射图，图 7b为利用该测试样品杆得到的多晶 A1薄膜样品 在拉伸变形过程中的应力应变曲线。
此外， 所述的传感器 11也可采 ^我们以前的专利： 一种热双金 属片驱动的透射电子显微镜载网， 专利号： ZL2006I0144031. X; 透射 电镜 ^纳米材料应力测试载网， 专利号： ZL200810056836. 8 ; 定量测 试力电性能与显微结构的传感器及制作方法， 专利申请号： 200920269907. 2制作的载网及传感器， 实现对样品性能的测量。

Claims

权利要求书
1.一种透射电镜用双轴倾转的原位力、 电性能综合测试样品杆， 其特征在于： 依次包括手握柄 （1)， 样品杆 (2), 样品头前端 (3)， 传感器载台 （4)通过位于样品头前端 （3)两内侧的两个支撑轴 （5) 固定在样品头前端（3)上， 在样品头前端 （3)两侧的壁上， 对称分 布有从电镜外部通过样品杼 (2) 引入的导线 I (6) ，并与分布在样 品头前端 （3)两侧壁上的队列电极 I (7)相连， 导线]: (6) 的另一 端连接在手握柄上的电极接口 （8)上， 通过电极接口 （8)与电镜外 部设备相连； 队列电极 I (7) 的位置为以支撑轴 （5) 为中心线对称 分布在样品头前端（3)两测壁上； 传感器载台 （4)尾部设有用于驱 动传感器载台 （4) Y轴倾转驱动器 9; 在传感器载台 （4) 上以支撑 轴 （5) 为中心线制作了一个凹槽（10)， 凹槽（10) 为一个通孔， 下 部设有用来支撑传感器 (11) 的支撑沿， 传感器 (11)放入凹櫓（10) 后上表面所在平面与 TEM电子束聚焦中心位于同一平面内；此外在传 感器载台 （4) 的远离支撑轴 （5) 靠近 Y轴倾转驱动器 （9) 的位置 设有一个通孔 I (13)， 传感器 （11) 靠近两侧支撑轴 （5) 对称制备 了两排队列电极 Π (14) ,压片（15)上 ί司样制备了两排队列电极 ΙΤΤ (16) ，每一对队列电极 ΠΙ (16) 都为分布于压片上下两个面内的 两个电极， 这两个电极通过导线连接；
传感器 (11) 放入传感器载台 (4) 的凹槽 (10) 中后， 将压片
(15) 压在传感器 （11) 上， 队列电极 III (16) 分布于压片 （15) 下表面的电极与传感器 （11) 上的队列电极 II (14) 一一对应相连 接， 将压片（15) 固定在传感器载台 （4)上， ^导线将队列电极 ΙΠ
(16) 分布于压片 （15) 上表面的电极与分布在样品头前端 （3) 两 侧的队列电极 I (7) -—一对应相连接；
压片 （15) 上设有一个通孔 II (17) ， 使电子束透过压片会聚 在传感器 （11) 的样品 （12)上； 传感器（11)上包括两列队列电极 II (14)， 应力施加部件（18), 应力测试部件（19)， 测试电极（20) 以及样品 （12)， 应力施加部件 （18) 与应力测试部件 （19) 并行排 列在传感器 （11) 上， 平行于队列电极 II (14) 放置并在两列队列 电极 II (14) 之间， 应力施加部件 （18) 与应力测试部件 （19) 中 间有供电子束通过的一狭缝， 在应力施加部件（18)和应力测试部件 权利要求书
(19) 上制作了两个测试电极 （20)， 样品 (12) 两端分别搭载在应 力施加部件（18)和应力测试部件（19)上的测试电极 （20) 上并 _目. 横跨上述供电子束通过的狭缝； 应力施加部件 （18)、 应力测试部件
(19)、 测试电极 (20) 的电路都通过导线与传感器 (11) 上制作的 队列电极 ΠΙ (14)对应连接； 应力施加部件（18)采用热双金属片， 压电陶瓷或记忆合金， 应力测试部件 （19) 用悬臂梁结构。
2.根据权利要求 1所述的样品杆， 其特征在于： 所述的电极引线 ( 4 ) 都为外部 有绝缘层的导电性材料。
3.根据权利要求 1所述的样品杆， 其特征在于： 所述的样品头前 端（3)， 传感器载台 (4), 以及压片 (15) 的表面都分布有绝缘介电 层， 该绝缘介电层材料是二氧化硅， 碳化硅， 氮化硅或氧化铪。
4.根据权利要求 1所述的样品杆， 其特征在于： 所述的队列电极 I (7)， 队列电极 II (14), 队列电极 III (16)采用 Rh, Pd, Rh/Au, Ti/Aii, W/Pt, Cr/Pt, Ni/Pt, Ag或 Cu。
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