CN2608984Y - Nano carbon material field emission property tester - Google Patents
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- CN2608984Y CN2608984Y CN 03213122 CN03213122U CN2608984Y CN 2608984 Y CN2608984 Y CN 2608984Y CN 03213122 CN03213122 CN 03213122 CN 03213122 U CN03213122 U CN 03213122U CN 2608984 Y CN2608984 Y CN 2608984Y
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- 238000005516 engineering process Methods 0.000 abstract description 2
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
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Abstract
本实用新型涉及场致发射性能测试技术，特别是一种纳米炭材料场致发射性能的测试装置，包括真空室、真空获得系统、样品传递系统、样品定位系统、I－V测试系统，其真空室为球形，通过闸板阀与真空获得系统中溅射离子泵相连，测试阳极通过引芯电极B导出真空室外至灵敏电流计，测试样品作为阴极通过引芯电极A与直流高压电源低电位端相连；样品传递系统由真空预抽室、磁性传递杆和样品台组件组成，磁性传递杆一端安装在真空预抽室里，真空预抽室与真空获得系统相连，并与真空室通过隔离闸板阀相通；负载样品的样品台组件设置于真空室内，与安装在真空室正上方的样品定位系统相连。它能在更换样品过程中不直接暴露于大气环境，适用范围广，操作方便。
The utility model relates to field emission performance test technology, in particular to a test device for field emission performance of nano-carbon materials, including a vacuum chamber, a vacuum acquisition system, a sample transfer system, a sample positioning system, and an I-V test system. The chamber is spherical, connected with the sputtering ion pump in the vacuum obtaining system through the gate valve, the test anode is led out of the vacuum chamber to the sensitive ammeter through the lead electrode B, and the test sample is used as the cathode through the lead electrode A and the low potential end of the DC high voltage power supply Connected; the sample transfer system is composed of a vacuum pre-pumping chamber, a magnetic transfer rod and a sample stage assembly. One end of the magnetic transfer rod is installed in the vacuum pre-pumping chamber. The valves are communicated; the sample stage assembly loaded with samples is arranged in the vacuum chamber and connected with the sample positioning system installed directly above the vacuum chamber. It can not be directly exposed to the atmospheric environment during the sample replacement process, has a wide range of applications, and is easy to operate.
Description
技术领域technical field
本实用新型涉及场致发射性能测试技术，特别是提供了一种纳米炭材料场致发射性能的测试装置。The utility model relates to field emission performance test technology, in particular provides a test device for field emission performance of nano-carbon materials.
背景技术Background technique
纳米材料，尤其是纳米炭材料(如纳米碳管)，以其独特的介观结构特征、优异的理化性能在场致发射领域显示出极高的研究价值和巨大的应用潜力。从宏观形态上区分，场发射纳米炭材料可呈纤维状、薄膜状、块状等多种形式，而其场致发射性能的测试一般在超高真空条件下(真空度10-5Pa以上)进行。现有的场致发射性能测试装置或者在更换样品真空系统暴露大气，导致系统真空度上升缓慢、极限真空度低；或者更换样品需要繁复的操作过程，造成样品方位难以调控。Nano-materials, especially nano-carbon materials (such as carbon nanotubes), have shown extremely high research value and great application potential in the field of field emission due to their unique mesoscopic structural characteristics and excellent physical and chemical properties. From the perspective of macroscopic morphology, field emission nano-carbon materials can be in various forms such as fibrous, thin film, block, etc., and its field emission performance is generally tested under ultra-high vacuum conditions (vacuum degree above 10 -5 Pa) conduct. The existing field emission performance testing device is either exposed to the atmosphere when the vacuum system of the sample is replaced, resulting in a slow increase in the vacuum degree of the system and a low ultimate vacuum degree; or the complicated operation process is required to replace the sample, making it difficult to control the sample orientation.
实用新型内容Utility model content
本实用新型的目的是提供一种能在更换样品过程中不直接暴露于大气环境、可以在较短时间内获得超高真空的纳米材料场致发射性能测试装置。The purpose of the utility model is to provide a nano-material field emission performance testing device which can obtain ultra-high vacuum in a relatively short period of time without being directly exposed to the atmospheric environment during the sample replacement process.
本实用新型的技术方案为：测试装置包括真空室、真空获得系统、样品传递系统、样品定位系统、I-V测试系统，真空室通过闸板阀与真空获得系统中溅射离子泵管路相连；真空室为球形，测试阳极通过引芯电极B导出真空室外、至I-V测试系统中灵敏电流计，测试样品作为阴极通过引芯电极A与直流高压电源低电位端相连；所述样品传递系统由真空预抽室、磁性传递杆和样品台组件组成，所述磁性传递杆用于在真空预抽室与真空室之间进行样品的交递，真空预抽室与真空获得系统中涡轮分子泵和机械泵所组成真空机组相连，并与真空室通过隔离闸板阀相通；负载样品的样品台组件设置于真空室内，通过刚性支杆与安装在真空室正上方的样品定位系统相连。The technical scheme of the utility model is: the test device includes a vacuum chamber, a vacuum acquisition system, a sample transfer system, a sample positioning system, and an I-V test system, and the vacuum chamber is connected to the sputtering ion pump pipeline in the vacuum acquisition system through a gate valve; The chamber is spherical, and the test anode is led out of the vacuum chamber through the core electrode B to the sensitive ammeter in the I-V test system. The test sample is used as the cathode and connected to the low potential end of the DC high-voltage power supply through the core electrode A; the sample delivery system is pre-vacuum. Composed of a pumping chamber, a magnetic transfer rod and a sample stage assembly, the magnetic transfer rod is used to transfer samples between the vacuum pre-pumping chamber and the vacuum chamber, the turbomolecular pump and the mechanical pump in the vacuum pre-pumping chamber and the vacuum obtaining system The formed vacuum unit is connected and communicated with the vacuum chamber through an isolation gate valve; the sample stage assembly for loading samples is arranged in the vacuum chamber, and connected with the sample positioning system installed directly above the vacuum chamber through rigid struts.
另外，本实用新型所述测试用纳米炭材料的样品台组件为棱柱形，在磁性传递杆端部支座上设有凹槽与之配合；所述测试阳极为ITO导电玻璃平面阳极和/或探针式金属阳极；所述磁性传递杆与真空预抽室相通，其轴线与真空预抽室、隔离闸板阀、真空室的中心点以及样品定位系统支杆的尖端在同一水平面内。In addition, the sample stage assembly of the nano-carbon material for testing described in the utility model is prismatic, and a groove is provided on the support at the end of the magnetic transmission rod to cooperate with it; the test anode is an ITO conductive glass plane anode and/or Probe type metal anode; the magnetic transmission rod communicates with the vacuum pre-pumping chamber, and its axis is in the same horizontal plane as the vacuum pre-pumping chamber, the isolation gate valve, the central point of the vacuum chamber and the tip of the sample positioning system pole.
本实用新型具有如下有益效果：The utility model has the following beneficial effects:
1.能在更换样品过程中不直接暴露于大气环境。本实用新型用于测试纳米炭材料场致发射性能，测试系统在更换样品过程中不会直接暴露于大气环境，样品交递过程在不低于1×10-4Pa的高真空条件下进行。1. Can not be directly exposed to the atmospheric environment during the sample replacement process. The utility model is used to test the field emission performance of nano-carbon materials. The test system will not be directly exposed to the atmospheric environment during the sample replacement process, and the sample delivery process is carried out under high vacuum conditions not lower than 1×10 -4 Pa.
2.能在较短时间内获得超高真空。采用本实用新型可以在较短时间内(＜12小时)获得5.0×10-7Pa以上的超高真空；系统真空度还可以在大范围内(1.3×10-3～2.0×10-7Pa)实现有效控制。2. Ultra-high vacuum can be obtained in a short period of time. Adopting the utility model can obtain an ultra-high vacuum of 5.0×10 -7 Pa or more in a relatively short period of time (<12 hours) ; ) to achieve effective control.
3.适用范围广。本实用新型适用于绳束状、薄膜状、块状样品，完成对不同类型纳米炭材料场致发射性能的测试工作。3. Wide application range. The utility model is suitable for rope-like, film-like and block-like samples, and completes the test work on the field emission performance of different types of nano-carbon materials.
4.操作方便。更换样品时避免了现有技术中所需的繁复操作过程，而且对测试参数(系统真空度、样品方位等)的控制调整简单、方便。4. Easy to operate. The complex operation process required in the prior art is avoided when replacing the sample, and the control and adjustment of the test parameters (system vacuum degree, sample orientation, etc.) are simple and convenient.
附图说明Description of drawings
附图1为本实用新型纳米炭材料场致发射性能测试装置结构示意图。Accompanying drawing 1 is the structural schematic diagram of the field emission performance testing device of the nano-carbon material of the present invention.
具体实施方式Detailed ways
如附图1所示，本实用新型所提供纳米炭材料场致发射性能测试装置由真空室、真空获得系统、样品传递系统、样品定位系统、I-V测试系统所组成，真空室3采用球形，与溅射离子泵8管路相连，以闸板阀6控制管道的连通，安装电离真空计测试端于真空室3与溅射离子泵8之间；闸板阀6的存在可以起到节控溅射离子泵8工作效率、调整系统真空度(2.0×10-7Pa～1.3×10-3Pa范围)的作用。负载样品的组件4设置于真空室3内，通过刚性支杆与真空室3外部正上方的样品定位系统1相连；样品定位系统1购置于美国Huntington公司，其功能是除起到固定样品的作用外，还可以在较大范围内对样品的方位进行调控，包括三维方向上的线性移动、水平面内的任意转动以及一定范围内的倾斜等等，可满足不同形貌、尺寸样品的测试需求。测试阳极9除可采用ITO导电玻璃平面阳极外，还配备有一套探针式金属阳极(本实施例测试阳极9为由ITO导电玻璃装配成的平面阳极)；测试阳极9通过引芯电极B17导出真空室3外至灵敏电流计18，测试样品作为阴极通过引芯电极A2与直流高压电源20低电位端相连。真空室3还配置有多个不同尺寸(φ35mm、φ150mm)的观察窗16。真空室3采用球形目的是提高内部空间利用率，便于样品和电极组件的工艺布置，同时可配置更多大尺寸法兰接口以满足测试和观察要求。As shown in accompanying drawing 1, nano-carbon material field emission performance test device provided by the utility model is made up of vacuum chamber, vacuum acquisition system, sample delivery system, sample positioning system, IV test system, and vacuum chamber 3 adopts spherical shape, and The sputtering ion pump 8 is connected to the pipeline, and the connection of the pipeline is controlled by the gate valve 6, and the test port of the ionization vacuum gauge is installed between the vacuum chamber 3 and the sputtering ion pump 8; the existence of the gate valve 6 can play a role in controlling the sputtering The working efficiency of the ion pump 8 and the adjustment of the vacuum degree of the system (2.0×10 -7 Pa～1.3×10 -3 Pa range). The component 4 that loads the sample is arranged in the vacuum chamber 3, and is connected with the sample positioning system 1 directly above the outside of the vacuum chamber 3 through rigid struts; the sample positioning system 1 was purchased from Huntington Company in the United States, and its function is to fix the sample In addition, the orientation of the sample can be regulated in a wide range, including linear movement in the three-dimensional direction, arbitrary rotation in the horizontal plane, and inclination within a certain range, etc., which can meet the testing requirements of samples with different shapes and sizes. In addition to the use of ITO conductive glass plane anodes, the test anode 9 is also equipped with a set of probe-type metal anodes (the test anode 9 in this embodiment is a plane anode assembled from ITO conductive glass); the test anode 9 is derived through the lead electrode B17 The outside of the vacuum chamber 3 is connected to the sensitive ammeter 18, and the test sample is connected to the low potential end of the DC high voltage power supply 20 as a cathode through the core electrode A2. The vacuum chamber 3 is also equipped with a plurality of observation windows 16 of different sizes (φ35mm, φ150mm). The purpose of adopting the spherical shape of the vacuum chamber 3 is to improve the utilization rate of the internal space, facilitate the process arrangement of samples and electrode assemblies, and at the same time, more large-size flange interfaces can be configured to meet the requirements of testing and observation.
为避免样品更换过程中球形真空室3暴露于大气环境，本实用新型设计一套样品传递系统，由真空预抽室12、磁性传递杆14和样品台组件4所组成，其中真空预抽室12与机械泵和涡轮分子泵所组成真空机组相连，与真空室3之间则采用隔离闸板阀15；测试用纳米炭材料的样品台组件4外观为三棱柱形，在磁性传递杆14端部支座上加工有相应的凹槽起到安置和传递样品台组件4的作用；磁性传递杆14与真空预抽室12相通，其轴线与真空预抽室12、隔离闸板阀15、真空室3的中心点以及样品定位系统1支杆的尖端基本在同一水平面内，便于进行样品的传递操作；样品传递系统的功能是完成测试样品从大气环境向真空室3内部的传递过程：在大气环境下，纳米炭材料被安置于样品台组件4上，由真空机组的工作使得真空预抽室12内真空气压由大气压力降低到2.0×10-4Pa后，再打开隔离闸板阀15、由磁性传递杆14送入真空室3内，并与样品定位系统1进行交接，磁性传递杆14推出后关闭隔离闸板阀15。在此样品传递过程中，真空室3内真空度不低于1.0×10-4Pa。由于避免了真空室3与大气环境的直接连通，因此系统达到测试真空度所需时间短，极限真空度高：从样品传递过程完毕开始，约8小时后系统真空度达到5.0×10-7Pa以上，24小时超过3.0×10-7Pa。负载样品条件下球形真空室3内的系统真空度最高可达1.3×10-7Pa。In order to prevent the spherical vacuum chamber 3 from being exposed to the atmospheric environment during the sample replacement process, the utility model designs a set of sample transfer system, which is composed of a vacuum pre-pumping chamber 12, a magnetic transfer rod 14 and a sample stage assembly 4, wherein the vacuum pre-pumping chamber 12 It is connected with the vacuum unit composed of a mechanical pump and a turbomolecular pump, and an isolation gate valve 15 is used between the vacuum chamber 3; Corresponding grooves are processed on the support to play the role of placing and transferring the sample stage assembly 4; the magnetic transfer rod 14 communicates with the vacuum pre-pumping chamber 12, and its axis is connected with the vacuum pre-pumping chamber 12, the isolation gate valve 15, and the vacuum chamber. The central point of 3 and the tip of the support rod of sample positioning system 1 are basically in the same horizontal plane, which facilitates the sample transfer operation; the function of the sample transfer system is to complete the transfer process of the test sample from the atmospheric environment to the interior of the vacuum chamber 3: in the atmospheric environment Next, the nano-carbon material is placed on the sample stage assembly 4, and the vacuum pressure in the vacuum pre-evacuation chamber 12 is reduced from atmospheric pressure to 2.0×10 -4 Pa by the work of the vacuum unit, and then the isolation gate valve 15 is opened, and the The magnetic transfer rod 14 is sent into the vacuum chamber 3 and connected with the sample positioning system 1 , and the isolation gate valve 15 is closed after the magnetic transfer rod 14 is pushed out. During this sample transfer process, the vacuum degree in the vacuum chamber 3 is not lower than 1.0×10 -4 Pa. Since the direct communication between the vacuum chamber 3 and the atmospheric environment is avoided, the time required for the system to reach the test vacuum degree is short, and the ultimate vacuum degree is high: from the completion of the sample transfer process, the system vacuum degree reaches 5.0×10 -7 Pa after about 8 hours Above, exceeding 3.0×10 -7 Pa in 24 hours. The system vacuum in the spherical vacuum chamber 3 can reach up to 1.3×10 −7 Pa under the condition of loading the sample.
所述机械泵10、涡轮分子泵11、溅射离子泵8以及相应的动力控制和真空监测系统构成真空获得系统，机械泵10和涡轮分子泵11主要面对真空预抽室12，溅射离子泵8用于提高和保持真空室3内的真空度条件。The mechanical pump 10, the turbomolecular pump 11, the sputtering ion pump 8 and the corresponding power control and vacuum monitoring system constitute a vacuum acquisition system. The mechanical pump 10 and the turbomolecular pump 11 mainly face the vacuum pre-pumping chamber 12, sputtering ions The pump 8 is used to increase and maintain the vacuum condition in the vacuum chamber 3 .
I-V测试系统包括直流高压电源20和灵敏电流计18以及相关的导线、电极等等，利用直流高压电源所提供的电场条件，纳米材料中发射出的电子由阳极收集后所形成的电流由灵敏电流计进行监测。The I-V test system includes a DC high-voltage power supply 20 and a sensitive ammeter 18 and related wires, electrodes, etc., utilizing the electric field conditions provided by the DC high-voltage power supply, the electrons emitted in the nanomaterials are collected by the anode and the current formed by the sensitive current meter for monitoring.
测试过程中，通过样品定位系统1的作用，测试样品5与阳极9之间的距离可调可控。阳极9采用氧化铟锡(ITO)导电玻璃制成，或者采用导电金属如铜、铝等。为满足薄膜材料的测试需要，真空室3内同时配备有一套探针式阳极，即由铜、铝等金属材料制成直径1mm的光滑平头圆柱用作测试阳极。测试样品5和阳极9分别通过引芯电极A2和B17导出真空室3外，并分别与直流高压电源20低电位端和灵敏电流计18相连。直流高压电源20用于在测试样品5和阳极9之间形成场发射过程所需电场，灵敏电流计18用于记录场发射电流。为避免电压脉冲的破坏作用，测试回路中还引入了一个电阻19。During the test, the distance between the test sample 5 and the anode 9 is adjustable and controllable through the function of the sample positioning system 1 . The anode 9 is made of indium tin oxide (ITO) conductive glass, or conductive metal such as copper, aluminum and the like. In order to meet the test requirements of thin film materials, the vacuum chamber 3 is also equipped with a set of probe-type anodes, that is, smooth flat cylinders with a diameter of 1mm made of metal materials such as copper and aluminum are used as test anodes. The test sample 5 and the anode 9 are led out of the vacuum chamber 3 through the core electrodes A2 and B17 respectively, and connected to the low potential end of the DC high voltage power supply 20 and the sensitive ammeter 18 respectively. The DC high-voltage power supply 20 is used to form the electric field required for the field emission process between the test sample 5 and the anode 9, and the sensitive ammeter 18 is used to record the field emission current. In order to avoid the destructive effect of the voltage pulse, a resistor 19 is also introduced into the test circuit.
球形真空室3上配备有多个观察窗16，可以观察样品在测试过程中发生的变化。在阳极9ITO玻璃表面涂覆有荧光材料情况下，还可以观察到场发射电子光斑的有关信息。The spherical vacuum chamber 3 is equipped with a plurality of observation windows 16, which can observe the changes of the sample during the test. In the case that the surface of the anode 9ITO glass is coated with fluorescent materials, the relevant information of the field emission electron spot can also be observed.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102809661A (en) * | 2011-05-30 | 2012-12-05 | 中国科学院电子学研究所 | Sample feeding apparatus for ultra-high vacuum test |
| CN104236991A (en) * | 2014-08-19 | 2014-12-24 | 宁波英飞迈材料科技有限公司 | Detachable in-situ heat treatment device and using method thereof |
| CN104865257A (en) * | 2015-04-30 | 2015-08-26 | 中国科学院长春光学精密机械与物理研究所 | Extreme ultraviolet (EUV) multilayer-film carbon pollution experiment device |
| CN105987662A (en) * | 2015-02-02 | 2016-10-05 | 北京大学 | Method and system for measurement of organic semiconductor heterojunction physical properties |
| CN107238726A (en) * | 2017-06-19 | 2017-10-10 | 北京大学 | A kind of multiple degrees of freedom sample transfer device of ultra-high vacuum environment |
| CN108369210A (en) * | 2015-10-26 | 2018-08-03 | 德卡提公司 | Charhing unit and particle monitoring equipment for particle monitoring equipment |
| CN109613064A (en) * | 2018-11-16 | 2019-04-12 | 兰州空间技术物理研究所 | The adjustable field emission test device of electrode spacing and method in a kind of vacuum system |
| CN110014386A (en) * | 2019-04-22 | 2019-07-16 | 哈尔滨工业大学 | An ultra-high temperature sample fixture suitable for thermionic emission performance testing |
| CN110346393A (en) * | 2019-04-22 | 2019-10-18 | 哈尔滨工业大学 | Overlength environment thermionic emission more online testing devices and its test method in situ |
| CN111965110A (en) * | 2020-08-12 | 2020-11-20 | 中国科学院上海高等研究院 | A compact multifunctional vacuum experiment system |
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2003
- 2003-05-15 CN CN 03213122 patent/CN2608984Y/en not_active Expired - Fee Related
Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102809661A (en) * | 2011-05-30 | 2012-12-05 | 中国科学院电子学研究所 | Sample feeding apparatus for ultra-high vacuum test |
| CN102809661B (en) * | 2011-05-30 | 2013-11-06 | 中国科学院电子学研究所 | Sample feeding apparatus for ultra-high vacuum test |
| CN104236991A (en) * | 2014-08-19 | 2014-12-24 | 宁波英飞迈材料科技有限公司 | Detachable in-situ heat treatment device and using method thereof |
| CN105987662A (en) * | 2015-02-02 | 2016-10-05 | 北京大学 | Method and system for measurement of organic semiconductor heterojunction physical properties |
| CN104865257A (en) * | 2015-04-30 | 2015-08-26 | 中国科学院长春光学精密机械与物理研究所 | Extreme ultraviolet (EUV) multilayer-film carbon pollution experiment device |
| CN104865257B (en) * | 2015-04-30 | 2017-07-14 | 中国科学院长春光学精密机械与物理研究所 | EUV multilayer films carbon pollutes experimental provision |
| CN108369210A (en) * | 2015-10-26 | 2018-08-03 | 德卡提公司 | Charhing unit and particle monitoring equipment for particle monitoring equipment |
| CN108369210B (en) * | 2015-10-26 | 2019-12-06 | 德卡提公司 | charging unit for particle monitoring device and particle monitoring device |
| US11101622B2 (en) | 2015-10-26 | 2021-08-24 | Dekati Oy | Charging unit for a particle monitoring apparatus, and a particle monitoring apparatus |
| CN107238726B (en) * | 2017-06-19 | 2018-07-13 | 北京大学 | A kind of multiple degrees of freedom sample transfer device of ultra-high vacuum environment |
| CN107238726A (en) * | 2017-06-19 | 2017-10-10 | 北京大学 | A kind of multiple degrees of freedom sample transfer device of ultra-high vacuum environment |
| CN109613064A (en) * | 2018-11-16 | 2019-04-12 | 兰州空间技术物理研究所 | The adjustable field emission test device of electrode spacing and method in a kind of vacuum system |
| CN110014386A (en) * | 2019-04-22 | 2019-07-16 | 哈尔滨工业大学 | An ultra-high temperature sample fixture suitable for thermionic emission performance testing |
| CN110346393A (en) * | 2019-04-22 | 2019-10-18 | 哈尔滨工业大学 | Overlength environment thermionic emission more online testing devices and its test method in situ |
| CN110346393B (en) * | 2019-04-22 | 2021-10-29 | 哈尔滨工业大学 | A multi-field in-situ device for thermionic emission in extraordinary environment and its on-line testing method |
| CN111965110A (en) * | 2020-08-12 | 2020-11-20 | 中国科学院上海高等研究院 | A compact multifunctional vacuum experiment system |
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