CN107727697B - Four-probe in-situ resistance measurement equipment for high-flux material chip - Google Patents
Four-probe in-situ resistance measurement equipment for high-flux material chip Download PDFInfo
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Abstract
Description
技术领域Technical field
本发明涉及材料测试技术领域,特别是指一种高通量材料芯片四探针原位电阻测量设备。The invention relates to the technical field of material testing, and in particular to a high-throughput material chip four-probe in-situ resistance measurement equipment.
背景技术Background technique
材料基因组计划中的材料高通量实验方法,是一种高效的新材料研发方法。其核心思想是在短时间内完成大量材料样品的制备和表征,并从中筛选出满足性能要求的样品对应相应工艺。相比传统的“试错法”,高通量试验方法具有研发周期短、开发费用低、人员劳动强度低等优点,是当前材料科研和应用领域发展的前沿技术。The high-throughput materials experimental method in the Materials Genome Project is an efficient method for the development of new materials. The core idea is to complete the preparation and characterization of a large number of material samples in a short time, and select the corresponding processes for samples that meet performance requirements. Compared with the traditional "trial and error method", the high-throughput test method has the advantages of short research and development cycle, low development cost, and low personnel labor intensity. It is the cutting-edge technology in the current development of materials research and application fields.
材料组合芯片技术是一种高通量制备大量材料样品的方法,其一般思路是使用PVD设备,采用分立掩模板法或者共溅射法将大量具有不同成分的二元、三元或者多远材料制备到一块小的基片上,该方法可极高的提升样品制备的通量。而对这些样品进行高通量的表征和测试,则对高通量的材料测量技术提出了需求。Material combination chip technology is a high-throughput method for preparing a large number of material samples. The general idea is to use PVD equipment and separate mask methods or co-sputtering methods to combine a large number of binary, ternary or multi-distance materials with different compositions. Prepared on a small substrate, this method can greatly increase the throughput of sample preparation. The high-throughput characterization and testing of these samples puts forward the need for high-throughput material measurement technology.
电阻作为材料的基本物理属性,在新型半导体材料、介电材料、电池材料、磁性材料等的研发中占有重要地位。另外,在一些气敏传感器材料的研究中,也需要测量电阻随气体浓度和温度的变化关系,这就对电阻的原位测量和记录技术提出了要求。将高通量电阻测量技术与材料的组合芯片制备技术结合,就能达到高通量材料制备和检测的目的。传统的电阻测量装置为达到这一目的,通常使用步进电机控制的探头,依次测量各个区域的电阻值,但这样难以满足原位测量和记录的要求,特别是高温高压的严苛环境中,另外当需要连续记录样品的电阻变化时,对每个样品的测量间隔过长,难以应对电阻快速变化的情况。另外,目前国内商用的四探针测试仪表均多为单通道,单台仪表价格通常在5000元以上,若用于高通量电阻测量,不仅成本高昂,也存在连线复杂的问题。本发明使用一体化的设计,针对材料高通量电阻原位测量的应用难题,提供一套专为材料高通量研发中电阻在高温高压环境原位测量和记录的装置,具有操作简单方便、成本相对低廉、运行稳定可靠、测量精度高、数据记录量大的优点,弥补了国内该领域应用技术的空白。As a basic physical property of materials, resistance plays an important role in the research and development of new semiconductor materials, dielectric materials, battery materials, magnetic materials, etc. In addition, in the research of some gas-sensitive sensor materials, it is also necessary to measure the relationship between resistance and gas concentration and temperature, which puts forward requirements for in-situ measurement and recording technology of resistance. Combining high-throughput resistance measurement technology with material combination chip preparation technology can achieve the purpose of high-throughput material preparation and detection. In order to achieve this purpose, traditional resistance measurement devices usually use probes controlled by stepper motors to measure the resistance values of various areas in sequence. However, this is difficult to meet the requirements of in-situ measurement and recording, especially in harsh environments with high temperature and high pressure. In addition, when it is necessary to continuously record the resistance changes of samples, the measurement interval for each sample is too long, making it difficult to cope with rapid changes in resistance. In addition, most of the four-probe test instruments currently commercially available in China are single-channel, and the price of a single instrument is usually more than 5,000 yuan. If it is used for high-throughput resistance measurement, it is not only expensive, but also has complicated wiring problems. This invention uses an integrated design to address the application problem of in-situ measurement of high-flux resistance of materials. It provides a set of devices specifically designed for in-situ measurement and recording of resistance in high-temperature and high-pressure environments during high-throughput research and development of materials. It is simple and convenient to operate. The advantages of relatively low cost, stable and reliable operation, high measurement accuracy and large data recording volume have filled the gaps in domestic application technology in this field.
发明内容Contents of the invention
本发明针对高通量材料研发,提供一种高通量材料芯片四探针原位电阻测量设备,不仅适用于材料组合芯片方法制备的高通量材料样品在高温高压严苛环境中的原位电阻测量记录,也可同时满足少量电阻精确测量的需求。Aiming at the research and development of high-throughput materials, the present invention provides a high-throughput material chip four-probe in-situ resistance measurement equipment, which is not only suitable for in-situ measurement of high-throughput material samples prepared by the material combination chip method in high-temperature and high-pressure harsh environments. Resistance measurement recording can also meet the needs of accurate measurement of a small amount of resistance at the same time.
该设备包括高通量四探针探头、耐高温高压气密罐体、样品架台、多通道四探针电阻测试仪、传输线缆和数据记录软件;样品架台位于耐高温高压气密罐体内,高通量四探针探头安装在样品架台上,高通量四探针探头通过传输线缆连接多通道四探针电阻测试仪,数据记录软件安装于上位机,数据记录软件接收来自多通道四探针电阻测试仪测量的数据,并进行实时显示和记录。The equipment includes a high-throughput four-probe probe, a high-temperature and high-pressure resistant airtight tank, a sample holder, a multi-channel four-probe resistance tester, a transmission cable and data recording software; the sample holder is located in a high-temperature and high-pressure resistant airtight tank. The high-throughput four-probe probe is installed on the sample holder. The high-throughput four-probe probe is connected to the multi-channel four-probe resistance tester through a transmission cable. The data recording software is installed on the host computer. The data recording software receives data from the multi-channel four-probe resistance tester. The data measured by the probe resistance tester are displayed and recorded in real time.
其中,耐高温高压气密罐体用于提供反应所需的压力和气氛,通过上密封盖对耐高温高压气密罐体进行密封;耐高温高压气密罐体采用高级不锈钢材质,在内部不超过500℃和6MPa压力的条件下使用,非腐蚀性气体如氢气、氧气、一氧化碳、甲烷等在耐高温高压气密罐体内与被测样品反应。Among them, the high temperature and high pressure resistant airtight tank is used to provide the pressure and atmosphere required for the reaction. The high temperature and high pressure resistant airtight tank is sealed by the upper sealing cover; the high temperature and high pressure resistant airtight tank is made of high-grade stainless steel and has no internal components. Used under conditions exceeding 500℃ and 6MPa pressure, non-corrosive gases such as hydrogen, oxygen, carbon monoxide, methane, etc. react with the sample under test in a high-temperature and high-pressure airtight tank.
耐高温高压气密罐体上设有电器连接器件,用于耐高温高压气密罐体内的高通量四探针探头的线缆与外部多通道四探针电阻测试仪的线缆进行连接,可在完成电信号传输任务的同时保证罐体不漏气;上密封盖上设有气压和温度检测仪表,并设有超压超温报警组件和泄压阀,另设有紧急排气通道,紧急排气管道能够在1~3s之内排空耐高温高压气密罐体内的气体,最大限度地保证使用安全性。The high-temperature and high-pressure-resistant airtight tank is equipped with electrical connecting devices, which are used to connect the cables of the high-throughput four-probe probe in the high-temperature and high-pressure-resistant airtight tank with the cables of the external multi-channel four-probe resistance tester. It can complete the electrical signal transmission task while ensuring that the tank does not leak; the upper sealing cover is equipped with air pressure and temperature detection instruments, and is equipped with overpressure and overtemperature alarm components and pressure relief valves, and is also equipped with an emergency exhaust channel. The emergency exhaust pipe can evacuate the gas in the high-temperature and high-pressure-resistant airtight tank within 1 to 3 seconds, ensuring maximum safety in use.
高通量四探针探头包括外壳、固定旋钮、线缆连接接头和探针,高通量四探针探头用于安装与样品直接接触的探针,探针内置缓冲装置,为可伸缩模式,能够与样品表面非硬性接触,探针间距固定,基于范德堡法原理与各样品接触,主要用于测量具有梯度成分分布的薄膜样品(也被成为材料芯片);线缆连接接头位于外壳内,固定旋钮用于高通量四探针探头与样品架台固定。The high-throughput four-probe probe includes a housing, a fixed knob, a cable connection connector and a probe. The high-throughput four-probe probe is used to install probes that are in direct contact with the sample. The probe has a built-in buffer device and is in retractable mode. It can have non-hard contact with the sample surface, and the probe spacing is fixed. It is in contact with each sample based on the principle of the Van der Pauw method. It is mainly used to measure thin film samples with gradient component distribution (also called material chips); the cable connection joint is located inside the casing. , the fixing knob is used to fix the high-throughput four-probe probe and the sample holder.
传输线缆内部导线为耐高温材质,且全部使用双绞线屏蔽处理。The internal conductors of the transmission cable are made of high-temperature resistant material, and all are shielded using twisted pairs.
样品架台使用整体式结构,装载样品后可调整和固定样品位置,以利于探头上的探针与每个样品严格对准,探头与样品架之间使用螺栓固定,可调节相对距离从而改变探针与样品表面的接触力大小。样品架台内部设置了电阻加热设备和温度控制设备,由耐高温高压气密罐体外部的开关电源供电;样品架台包括接口、旋钮、基座和夹具,接口、旋钮和夹具位于基座上,接口用于与高通量四探针探头连接,旋钮用于调节样品位置,夹具用于调节和固定样品位置。The sample holder uses an integral structure. After loading the sample, the sample position can be adjusted and fixed to facilitate the strict alignment of the probe on the probe with each sample. The probe and the sample holder are fixed with bolts, and the relative distance can be adjusted to change the probe. The amount of contact force with the sample surface. The sample holder is equipped with resistance heating equipment and temperature control equipment inside, and is powered by a switching power supply outside the high-temperature and high-pressure resistant airtight tank; the sample holder includes an interface, a knob, a base and a clamp. The interface, knob and clamp are located on the base, and the interface Used to connect to the high-throughput four-probe probe, the knob is used to adjust the sample position, and the clamp is used to adjust and fix the sample position.
多通道四探针电阻测试仪采用一体化结构,在一个壳体结构内部集成了包括64通道的可独立设置恒定电流大小的高精度压控恒流电源模块、微处理器控制模块、64通道电压采样电路和高精度型ADC模块、温度检测模块、通信模块、外围接口电路和开关电源模块;多通道四探针电阻测试仪外部设置接头、四针数据接口、LCD显示屏、测量模式选择开关、LCD亮度调节旋钮和总电源开关,接头用于与传输线缆完成数据输入输出,四针数据接口为1~8个通道的接线端子,每个通道的采样频率在数据记录软件中设置,最高采样频率超过50次/秒。外围接口方面,仪器预留了两个专用接口,分别用于为高通量四探针探头提供电阻测量用的恒流电源输出和采集多个通道的电压信号输入,使用时只需将专用线缆的插头分别接入两个接口即可,有效避免了接线失误和线路接触不良对实验的影响,同时极大地降低了劳动强度。除高通量电阻测试的应用之外,该仪器也预留了1~8个通道的接线端子,可满足对少量样品四探针电阻测试的需求。该仪器预留了RS485和TCP/IP接口用于与上位机通信。另外,该设备可根据被测电阻范围自动切换量程,自主选择恒流源输出值得大小,且各通道之间的工作相互独立。The multi-channel four-probe resistance tester adopts an integrated structure, which integrates a 64-channel high-precision voltage-controlled constant current power supply module that can independently set the constant current size, a microprocessor control module, and a 64-channel voltage Sampling circuit and high-precision ADC module, temperature detection module, communication module, peripheral interface circuit and switching power supply module; multi-channel four-probe resistance tester external connector, four-pin data interface, LCD display, measurement mode selection switch, LCD brightness adjustment knob and main power switch. The connector is used to complete data input and output with the transmission cable. The four-pin data interface is a terminal block for 1 to 8 channels. The sampling frequency of each channel is set in the data recording software. The highest sampling rate is Frequency exceeds 50 times/second. In terms of peripheral interfaces, the instrument has reserved two special interfaces, which are used to provide constant current power output for resistance measurement for high-throughput four-probe probes and to collect voltage signal inputs of multiple channels. When using, you only need to connect the dedicated wires. The cable plugs can be connected to the two interfaces respectively, which effectively avoids the impact of wiring errors and poor line contact on the experiment, and greatly reduces labor intensity. In addition to the application of high-throughput resistance testing, the instrument also reserves terminal blocks for 1 to 8 channels, which can meet the needs of four-probe resistance testing of a small amount of samples. The instrument has reserved RS485 and TCP/IP interfaces for communication with the host computer. In addition, the device can automatically switch the range according to the resistance range being measured, independently select the output value of the constant current source, and the work of each channel is independent of each other.
数据记录软件实时显示测得的当前电阻值和电阻值随时间、气压、温度变化的曲线,将数据以Excel或者txt文本文档文件的形式输出。The data recording software displays the measured current resistance value and the curve of resistance value changing with time, air pressure, and temperature in real time, and outputs the data in the form of Excel or txt text document file.
本发明的上述技术方案的有益效果如下:The beneficial effects of the above technical solutions of the present invention are as follows:
本发明设计的成套设备,样品放置在带有温度功能和探头固定功能的样品台上,能够保证探针的精确对准和精确的样品温度控制,高温高压密封罐为样品提供了安全的测试环境,特制的信号传输线缆使实验组装和连接过程简单方便,自主设计的高通量电阻测试仪能配合探头实现多达64个样品四探针电阻测量和记录的目的,数据记录软件界面友好,更能强大,使用方便。该设备针对高通量实验应用设计,同时也能满足日常少量样品的电阻测试需求,同时成本相对低廉,可靠性好,在材料的高通量研究领域具有广阔的应用范围。In the complete set of equipment designed by the present invention, the sample is placed on a sample stage with a temperature function and a probe fixing function, which can ensure precise alignment of the probe and precise sample temperature control. The high-temperature and high-pressure sealed tank provides a safe testing environment for the sample. , the special signal transmission cable makes the experimental assembly and connection process simple and convenient. The self-designed high-throughput resistance tester can cooperate with the probe to achieve the purpose of measuring and recording the four-probe resistance of up to 64 samples. The data recording software has a friendly interface. More powerful and easy to use. This equipment is designed for high-throughput experimental applications, and can also meet the daily resistance testing needs of a small number of samples. At the same time, the cost is relatively low, the reliability is good, and it has a broad range of applications in the field of high-throughput research on materials.
附图说明Description of drawings
图1为本发明的高通量材料芯片四探针原位电阻测量设备结构示意图;Figure 1 is a schematic structural diagram of the high-throughput material chip four-probe in-situ resistance measurement equipment of the present invention;
图2为本发明的自主研发的多通道四探针电阻测试仪结构示意图;Figure 2 is a schematic structural diagram of the independently developed multi-channel four-probe resistance tester of the present invention;
图3为本发明的带有温度控制功能的样品架台结构示意图;Figure 3 is a schematic structural diagram of the sample rack with temperature control function of the present invention;
图4为本发明的高通量四探针探头结构示意图。Figure 4 is a schematic structural diagram of the high-throughput four-probe probe of the present invention.
其中:1-包括高通量四探针探头;2-耐高温高压气密罐体;3-样品架台;4-上密封盖;5-传输线缆;6-多通道四探针电阻测试仪;7-数据记录软件;11-外壳;12-固定旋钮;13-线缆连接接头;14-探针;31-接口;32-旋钮;33-基座;34-夹具;61-接头;62-四针数据接口;63-LCD显示屏;64-测量模式选择开关;65-LCD亮度调节旋钮;66-总电源开关。Among them: 1-Including high-throughput four-probe probe; 2-High temperature and high pressure resistant airtight tank; 3-Sample stand; 4-Upper sealing cover; 5-Transmission cable; 6-Multi-channel four-probe resistance tester ; 7-data recording software; 11-casing; 12-fixing knob; 13-cable connection connector; 14-probe; 31-interface; 32-knob; 33-base; 34-clamp; 61-connector; 62 -Four-pin data interface; 63-LCD display; 64-Measurement mode selection switch; 65-LCD brightness adjustment knob; 66-Master power switch.
具体实施方式Detailed ways
为使本发明要解决的技术问题、技术方案和优点更加清楚,下面将结合附图及具体实施例进行详细描述。In order to make the technical problems, technical solutions and advantages to be solved by the present invention clearer, a detailed description will be given below with reference to the accompanying drawings and specific embodiments.
本发明提供一种高通量材料芯片四探针原位电阻测量设备。The invention provides a high-throughput material chip four-probe in-situ resistance measurement equipment.
如图1所示,为该设备结构示意图,该设备中,样品架台3位于耐高温高压气密罐体2内,高通量四探针探头1安装在样品架台3上,高通量四探针探头1通过传输线缆5连接多通道四探针电阻测试仪6,数据记录软件7安装于上位机,数据记录软件7接收来自多通道四探针电阻测试仪6测量的数据,并进行实时显示和记录。As shown in Figure 1, it is a schematic structural diagram of the equipment. In this equipment, the sample rack 3 is located in the high-temperature and high-pressure resistant airtight tank 2, and the high-flux four-probe probe 1 is installed on the sample rack 3. The high-flux four-probe probe The needle probe 1 is connected to the multi-channel four-probe resistance tester 6 through the transmission cable 5. The data recording software 7 is installed on the host computer. The data recording software 7 receives the measured data from the multi-channel four-probe resistance tester 6 and performs real-time Display and record.
如图2所示,多通道四探针电阻测试仪6采用一体化结构,在一个壳体结构内部集成了包括64通道的可独立设置恒定电流大小的高精度压控恒流电源模块、微处理器控制模块、64通道电压采样电路和高精度型ADC模块、温度检测模块、通信模块、外围接口电路和开关电源模块;多通道四探针电阻测试仪6外部设置接头61、四针数据接口62、LCD显示屏63、测量模式选择开关64、LCD亮度调节旋钮65和总电源开关66,接头61用于与传输线缆完成数据输入输出,四针数据接口62为1~8个通道的接线端子,每个通道的采样频率在数据记录软件7中设置,最高采样频率超过50次/秒。As shown in Figure 2, the multi-channel four-probe resistance tester 6 adopts an integrated structure and integrates a 64-channel high-precision voltage-controlled constant current power supply module and a microprocessor that can independently set the constant current size within a shell structure. Control module, 64-channel voltage sampling circuit and high-precision ADC module, temperature detection module, communication module, peripheral interface circuit and switching power supply module; multi-channel four-probe resistance tester 6 external setting connector 61, four-pin data interface 62 , LCD display 63, measurement mode selection switch 64, LCD brightness adjustment knob 65 and main power switch 66. The connector 61 is used to complete data input and output with the transmission cable, and the four-pin data interface 62 is a terminal block for 1 to 8 channels. , the sampling frequency of each channel is set in the data recording software 7, and the maximum sampling frequency exceeds 50 times/second.
如图3所示,样品架台3使用整体式结构,样品架台3内部设置了电阻加热设备和温度控制设备,由耐高温高压气密罐体2外部的开关电源供电;样品架台3包括接口31、旋钮32、基座33和夹具34,接口31、旋钮32和夹具34位于基座33上,接口31用于与高通量四探针探头1连接,旋钮32用于调节样品位置,夹具34用于调节和固定样品位置。As shown in Figure 3, the sample rack 3 uses an integral structure. The sample rack 3 is equipped with resistance heating equipment and temperature control equipment, and is powered by a switching power supply outside the high temperature and high pressure resistant airtight tank 2; the sample rack 3 includes an interface 31, The knob 32, the base 33 and the clamp 34. The interface 31, the knob 32 and the clamp 34 are located on the base 33. The interface 31 is used to connect to the high-throughput four-probe probe 1, the knob 32 is used to adjust the sample position, and the clamp 34 is used to for adjusting and fixing the sample position.
如图4所示,高通量四探针探头1包括外壳11、固定旋钮12、线缆连接接头13和探针14,高通量四探针探头1用于安装与样品直接接触的探针14,探针14内置缓冲装置,能够与样品表面非硬性接触,探针14间距固定;线缆连接接头13位于外壳11内,固定旋钮12用于高通量四探针探头1与样品架台3固定。As shown in Figure 4, the high-throughput four-probe probe 1 includes a housing 11, a fixing knob 12, a cable connection joint 13 and a probe 14. The high-throughput four-probe probe 1 is used to install probes that are in direct contact with the sample. 14. The probe 14 has a built-in buffer device, which can make non-hard contact with the sample surface. The distance between the probes 14 is fixed; the cable connection joint 13 is located in the housing 11, and the fixing knob 12 is used for the high-throughput four-probe probe 1 and the sample holder 3 fixed.
在实际使用过程中,首先将材料组合芯片技术制备的含有64种不同成分,沉积在同一不导电基片上的薄膜样品,放入如图2所示的样品架台样品室内,调整好位置并夹持好。In the actual use process, first put the thin film sample containing 64 different components prepared by material combination chip technology and deposited on the same non-conductive substrate into the sample chamber of the sample rack as shown in Figure 2, adjust the position and clamp it good.
将图3所示的高通量四探针探头的探针端对准样品一侧,用螺栓将探头和样品架台连接好,由于样品是采用配套掩模板制备的,且样品已经调整好位置并夹紧,因此探头上的每个探针恰好能与样品接触,并满足范德堡法测量电阻原理对探针正好与样品边缘接触的要求。Align the probe end of the high-throughput four-probe probe shown in Figure 3 to the side of the sample, and use bolts to connect the probe and the sample holder. Since the sample is prepared using a matching mask, the position of the sample has been adjusted and Clamping, so that each tip on the probe can just be in contact with the sample, and meet the requirement of the Vanderbilt method to measure resistance that the probe is in perfect contact with the edge of the sample.
高通量四探针探头的另一侧为由专用传输线缆引出,并配备一个插头,将该插头与气密罐体的电器连接件内部相连。然后盖上气密罐体的上密封盖,使用配套螺栓拧紧,并进行气体检漏操作。The other side of the high-throughput four-probe probe is led out by a special transmission cable and is equipped with a plug, which is connected to the internal electrical connector of the airtight tank. Then cover the upper sealing cover of the airtight tank, tighten it with the matching bolts, and perform gas leak detection.
将外部专用传输线缆的两个插头分别与气密罐体的电器连接件外部和如图2所示的多通道四探针电阻测量仪的输入输出专用接口连接。Connect the two plugs of the external dedicated transmission cable to the outside of the electrical connector of the airtight tank and the dedicated input and output interface of the multi-channel four-probe resistance measuring instrument as shown in Figure 2.
使用标准的RS485通信线将多通道四探针电阻测量仪与上位机连接,开启多通道四探针电阻测量仪的电源开关,预热20min。然后打开上位机中安装的自主开发的数据记录软件,对所需测量的样品各通道进行配置。配置内容包括:可根据各个样品的大致电阻范围手动设置仪器的测量区间,此时仪器会根据被测电阻值的范围配置恒流源输出的电流大小和电压采集电路运算放大器的放大倍数,也可选择不进行配置,系统会在测试中根据初次测得的电阻值动态调整相关参数。选择各通道数据记录的时间间隔,即采样频率。软件的测试模式共分为三类:“时间-电阻”、“温度-电阻”、“气压-电阻”,除非另行设置,系统将默认为“时间-电阻”模式,以电阻为纵坐标,时间为横坐标进行持续的数据记录,直到按下停止记录按钮。如果配置成其它两种模式,则分别以温度或气压为横坐标,电阻未纵坐标进行记录,而软件也提供了选项:“记录时间为第二横坐标”,若需要同时记录时间,则在该项复选框下打钩即可,此时软件会在测量过程中以时间为第二横坐标进行记录,否则软件再测量过程中将不记录时间。配置完毕后,即可启动整个设备的电阻测量和数据记录功能。Use a standard RS485 communication line to connect the multi-channel four-probe resistance measuring instrument to the host computer, turn on the power switch of the multi-channel four-probe resistance measuring instrument, and preheat for 20 minutes. Then open the self-developed data recording software installed in the host computer and configure each channel of the sample to be measured. The configuration content includes: you can manually set the measurement interval of the instrument according to the approximate resistance range of each sample. At this time, the instrument will configure the current output of the constant current source and the amplification factor of the voltage acquisition circuit operational amplifier according to the range of the measured resistance value. You can also If you choose not to configure, the system will dynamically adjust relevant parameters during the test based on the resistance value measured for the first time. Select the time interval for data recording of each channel, that is, the sampling frequency. The test modes of the software are divided into three categories: "time-resistance", "temperature-resistance", and "air pressure-resistance". Unless otherwise set, the system will default to the "time-resistance" mode, with resistance as the ordinate and time. Continuous data logging is performed for the abscissa until the Stop Logging button is pressed. If configured in the other two modes, the temperature or air pressure will be used as the abscissa, and the resistance will be recorded without the ordinate. The software also provides an option: "Record time as the second abscissa". If you need to record time at the same time, then record the time on the ordinate. Just tick this check box. At this time, the software will record with time as the second abscissa during the measurement process. Otherwise, the software will not record the time during the measurement process. After the configuration is completed, the resistance measurement and data logging functions of the entire device can be started.
选择样品的测试环境,若需要测量样品电阻随温度的变化关系,可配置密封罐内样品支架温度控制器件对应控制器,设置初始温度,升温步长和最高温度,另外还需要在数据记录软件中选择“温度-电阻”测试模式,此时系统将持续接收罐体内样品支架上的温度温度传感器数据,并以温度为纵坐标,电阻值为横坐标记录数据。若应用于气敏材料的电阻研究,则需要在数据记录软件中选择“气压-电阻”测试功能,此时系统将采集和记录罐体内数字气压表的数据,并以气压为横坐标,电阻为纵坐标进行记录。需额外配给气源给罐内施加压力,从而满足样品电阻测量的环境要求。Select the test environment of the sample. If you need to measure the relationship between the sample resistance and temperature, you can configure the corresponding controller of the temperature control device of the sample holder in the sealed tank, set the initial temperature, heating step length and maximum temperature. In addition, you need to set the temperature in the data recording software. Select the "temperature-resistance" test mode. At this time, the system will continue to receive the temperature sensor data on the sample holder in the tank, and record the data with the temperature as the ordinate and the resistance value as the abscissa. If it is applied to the resistance research of gas-sensitive materials, you need to select the "air pressure-resistance" test function in the data recording software. At this time, the system will collect and record the data of the digital air pressure meter in the tank, and use the air pressure as the abscissa and the resistance as The vertical coordinate is recorded. An additional air source is required to apply pressure inside the tank to meet the environmental requirements for sample resistance measurement.
当使用易燃易爆危险气体时,若出现泄漏,或监测到罐内压力超过警戒水平时,密封盖上安装的自动控压阀将启动抽真空操作,也可手动启动抽真空操作,以避免出现安全问题。When using flammable and explosive dangerous gases, if leakage occurs or the pressure in the tank is detected to exceed the warning level, the automatic pressure control valve installed on the sealing cover will start the vacuuming operation, or the vacuuming operation can be started manually to avoid A security issue has occurred.
电阻测量完成后,首先在上位机的数据记录软件中选择数据结果输出形式,可设置为Excel表格输出,或者Txt文本文档格式输出。After the resistance measurement is completed, first select the data result output format in the data recording software of the host computer, which can be set to Excel table output or Txt text document format output.
关闭多通道电阻测量仪的电源,对密封罐进行抽真空或者降温操作,待温度达到室温或者罐内抽真空结束后,即可打开密封盖,拆除固定的高通量四探针探头,解除样品架固定,取出样品结束测试。Turn off the power of the multi-channel resistance measuring instrument, vacuum or cool down the sealed tank. When the temperature reaches room temperature or the vacuum in the tank is completed, open the sealing cover, remove the fixed high-throughput four-probe probe, and remove the sample. The rack is fixed, and the sample is taken out to end the test.
实施例1Example 1
本实施例以采用高通量方法,从某种三元材料中筛选一种具有最小电阻温度效应的成分为例,来说明高通量原位电阻测试设备的研究应用。本实施例的具体步骤如下:This embodiment uses a high-throughput method to select a component with the smallest resistance temperature effect from a certain ternary material as an example to illustrate the research and application of high-throughput in-situ resistance testing equipment. The specific steps of this embodiment are as follows:
A1,选取采用组合芯片法制备的,以3英寸石英片为基片,表面镀有64个相互独立且成分各不相同的尺寸为A×A(A=1~3mm)的某三元材料薄膜样品。放入样品架台,调整好位置并固定。A1, select a ternary material film prepared by the combined chip method, with a 3-inch quartz sheet as the substrate, and the surface is coated with 64 independent and different compositions of a certain ternary material film with a size of A×A (A=1~3mm) sample. Put it into the sample holder, adjust the position and fix it.
B1,将高通量四探针探头采用螺栓与样品架台固定,由于样品的制备与探头的设计采用了兼容尺寸,此时探头的探针正好能与样品表面合适位置接触良好。B1, use bolts to fix the high-throughput four-probe probe to the sample holder. Since the sample preparation and probe design adopt compatible sizes, at this time, the probe tip can make good contact with the appropriate position on the sample surface.
C1,将四探针探头的线缆插头与罐体的电器连接件内部连接好,盖好气密封盖并用螺栓固定,完成对罐体的气密性检查并抽真空,为防止升温过程出现样品氧化,通入2MPa氩气作为保护气体。然后用专用线缆将罐体电器连接件外部与多通道四探针电阻测试仪的输入输出端连接好。C1. Connect the cable plug of the four-probe probe to the electrical connector of the tank. Cover the air-tight cover and fix it with bolts. Complete the air tightness check of the tank and evacuate it to prevent sample oxidation during the heating process. , pass in 2MPa argon gas as a protective gas. Then use a special cable to connect the outside of the tank electrical connector to the input and output ends of the multi-channel four-probe resistance tester.
D1,打开上位机的数据记录软件,恒流源和电压采集电路配置设为默认,选择仪器的“温度-电阻”测量模式,不勾选“记录时间为第二横坐标”,设置温度记录步长为1℃,即温度每升高一度,记录一次各个样品的电阻数据。D1, open the data recording software of the host computer, set the constant current source and voltage acquisition circuit configuration to default, select the "temperature-resistance" measurement mode of the instrument, uncheck "recording time as the second abscissa", and set the temperature recording step The length is 1°C, that is, the resistance data of each sample is recorded every time the temperature rises by one degree.
E1,配置控制样品架台内部电阻加热控温原件的设备参数,设置初始温度为25℃,升温模式设置为步进式,即温度每升高1℃则保温3s,然后再继续升温,升温最高温度为200℃。E1, configure the equipment parameters that control the resistance heating temperature control element inside the sample holder, set the initial temperature to 25°C, and set the heating mode to step type, that is, every time the temperature rises by 1°C, it will be kept warm for 3 seconds, and then continue to heat up to the maximum temperature. is 200℃.
F1,点击上位机数据记录软件记录启动按钮,开启升温设备控制电源,系统将自动记录64个样品从25~200℃,以1℃为步长的电阻数据。F1, click the recording start button of the host computer data recording software, turn on the control power of the heating equipment, and the system will automatically record the resistance data of 64 samples from 25 to 200°C in steps of 1°C.
G1,测试结束后,关闭加热控制器,选择数据记录软件中的数据输出形式为Excel输出,选择好数据存盘目录并保存。G1, after the test is completed, turn off the heating controller, select the data output format in the data recording software as Excel output, select the data storage directory and save it.
H1,等样品温度冷却到室温后,手动开启真空泵,将管内气压抽至1bar左右,开启气密封盖,拆卸四探针探头,取出样品保存,关闭与设备相连的电源,整理好线缆即可。H1, after the sample temperature has cooled to room temperature, manually turn on the vacuum pump, pump the air pressure in the tube to about 1 bar, open the air-sealing cover, disassemble the four-probe probe, take out the sample for storage, turn off the power supply connected to the equipment, and organize the cables. .
I1,使用Excel中数据,以温度为横坐标,各个样品的电阻分别为纵坐标,在作图软件中绘制出个样品电阻随温度变化的曲线,从中选出电阻随温度变化斜率最低的样品对应的成分,即为这种三元材料中,电阻温度系数最小的目标成分。I1, using the data in Excel, with temperature as the abscissa and the resistance of each sample as the ordinate, draw a curve of the resistance change of each sample with temperature in the drawing software, and select the sample with the lowest resistance change slope with temperature. The component is the target component with the smallest temperature coefficient of resistance in this ternary material.
实施例2Example 2
本实施例以采用高通量方法,从某种三元氢敏材料中筛选一种具有最快氢敏电阻响应的成分为例,来说明高通量原位电阻测试设备的研究应用。本实施例的具体步骤如下:This embodiment uses a high-throughput method to select a component with the fastest hydrogen-sensitive resistance response from a certain ternary hydrogen-sensitive material as an example to illustrate the research and application of high-throughput in-situ resistance testing equipment. The specific steps of this embodiment are as follows:
A2,选取采用组合芯片法制备的,以3英寸石英片为基片,表面镀有64个相互独立且成分各不相同的尺寸为B×B(A=1~3mm)的某三元材料薄膜样品。放入样品架台,调整好位置并固定。A2, select a ternary material film prepared by the combined chip method, using a 3-inch quartz sheet as the substrate, and the surface is coated with 64 independent and different compositions of a certain ternary material film with a size of B×B (A=1~3mm) sample. Put it into the sample holder, adjust the position and fix it.
B2,将高通量四探针探头采用螺栓与样品架台固定,由于样品的制备与探头的设计采用了兼容尺寸,此时探头的探针正好能与样品表面合适位置接触良好。B2, use bolts to fix the high-throughput four-probe probe to the sample holder. Since the sample preparation and probe design adopt compatible sizes, at this time, the probe tip can make good contact with the appropriate position on the sample surface.
C2,将四探针探头的线缆插头与罐体的电器连接件内部连接好,盖好密封盖并用螺栓固定,完成对罐体的气密性检查并抽真空。然后用专用线缆将罐体电器连接件外部与多通道四探针电阻测试仪的输入输出端连接好。C2, connect the cable plug of the four-probe probe to the electrical connector of the tank, cover the sealing cover and fix it with bolts, complete the air tightness check of the tank and vacuum. Then use a special cable to connect the outside of the tank electrical connector to the input and output ends of the multi-channel four-probe resistance tester.
D2,打开上位机的数据记录软件,恒流源和电压采集电路配置设为默认,选择仪器的“气压-电阻”测量模式,勾选“记录时间为第二横坐标”,设置电阻的时间记录步长为0.1s,即每个样品,每间隔0.1秒记录一个电阻值。D2, open the data recording software of the host computer, set the constant current source and voltage acquisition circuit configuration to default, select the "air pressure-resistance" measurement mode of the instrument, check "recording time as the second abscissa", and set the time record of the resistance The step size is 0.1s, that is, for each sample, a resistance value is recorded every 0.1 seconds.
E2,配置控制样品架台内部电阻加热控温原件的设备参数,设置初始温度为25℃,升温速率为5℃/min,目标温度为60℃,保温时间为100h。开启升温加热电源,等待样品温度到达60℃且稳定。E2, configure the equipment parameters that control the resistance heating temperature control element inside the sample holder. Set the initial temperature to 25°C, the heating rate to 5°C/min, the target temperature to 60°C, and the holding time to 100h. Turn on the heating power and wait for the sample temperature to reach 60°C and stabilize.
F2,点击上位机数据记录软件记录启动按钮,设置好氢气瓶减压阀低压侧气压为0.1MPa,打开进气阀,快速地给气密罐内通入0.1MPa H2,此时软件将记录罐内气压变化,以及通入H2后各个样品电阻随时间的变化,即样品的氢敏电阻响应。等待30min。开启真空泵和真空阀,在3s之内抽除罐内的H2,再在极短时间内通入0.1MPa的氩气,此时软件记录的是撤除H2气氛后,各样品电阻的响应特性。等待30min,再次抽除氩气,之后通入0.1MPa的氢气,此时样品记录第二次循环过程中各样品对氢气的电阻响应特性。如此反复10次。F2, click the recording start button of the host computer data recording software, set the low-pressure side pressure of the hydrogen bottle pressure reducing valve to 0.1MPa, open the air inlet valve, and quickly introduce 0.1MPa H2 into the airtight tank. At this time, the software will record the tank The changes in internal air pressure and the changes in the resistance of each sample over time after H2 is introduced are the hydrogen-sensitive resistance response of the sample. Wait 30 minutes. Turn on the vacuum pump and vacuum valve, remove the H2 in the tank within 3 seconds, and then introduce 0.1MPa argon gas in a very short time. At this time, the software records the response characteristics of the resistance of each sample after the H2 atmosphere is removed. Wait for 30 minutes, remove the argon again, and then introduce 0.1MPa hydrogen. At this time, the sample records the resistance response characteristics of each sample to hydrogen during the second cycle. Repeat this 10 times.
G2,测试结束后,首先抽除罐内气氛,然后通入0.1MPa的氩气。关闭加热控制器,选择数据记录软件中的数据输出形式为Excel输出,选择好数据存盘目录并保存。G2, after the test is completed, first remove the atmosphere in the tank, and then introduce 0.1MPa argon gas. Turn off the heating controller, select the data output format in the data recording software as Excel output, select the data save directory and save it.
H2,等样品温度冷却到室温后,手动开启真空泵,将管内气压抽至1bar左右,开启气密封盖,拆卸四探针探头,取出样品保存,关闭与设备相连的电源,整理好线缆即可。H2, wait for the sample temperature to cool to room temperature, manually turn on the vacuum pump, pump the air pressure in the tube to about 1 bar, open the air-sealing cover, disassemble the four-probe probe, take out the sample for storage, turn off the power supply connected to the equipment, and organize the cables. .
I2,使用Excel中数据,以温度为横坐标,各个样品的电阻分别为纵坐标,在作图软件中绘制出个样品电阻随温度变化的曲线,从中可以根据通入氢气和卸除氢气后,各样品电阻随时间的变化速率筛选除这种三元材料中具有最快速氢敏电阻响应特性的成分,另外,根据循环10次后各样品的氢敏电阻响应速率,判断具有在循环过程中最好的性能保持率的材料成分。I2, using the data in Excel, with temperature as the abscissa and the resistance of each sample as the ordinate, draw a curve of the sample resistance changing with temperature in the drawing software, from which you can draw the curve of the resistance of each sample with temperature according to the introduction of hydrogen and the removal of hydrogen. The change rate of the resistance of each sample over time is used to screen out the components with the fastest hydrogen-sensitive resistance response characteristics in this ternary material. In addition, based on the hydrogen-sensitive resistance response rate of each sample after 10 cycles, it is judged to have the fastest response during the cycle. Material composition for good performance retention.
以上所述是本发明的优选实施方式,应当指出,对于本技术领域的普通技术人员来说,在不脱离本发明所述原理的前提下,还可以做出若干改进和润饰,这些改进和润饰也应视为本发明的保护范围。The above is the preferred embodiment of the present invention. It should be pointed out that for those of ordinary skill in the art, several improvements and modifications can be made without departing from the principles of the present invention. These improvements and modifications It should also be regarded as the protection scope of the present invention.
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