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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- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
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Abstract
The invention provides high-flux material chip four-probe in-situ resistance measurement equipment, and belongs to the technical field of material testing. The device comprises a high-flux four-probe, a high-temperature and high-pressure resistant airtight tank body, a sample stand, a multi-channel four-probe resistance tester, a transmission cable and data recording software; the sample stand is positioned in the high-temperature and high-pressure resistant airtight tank body, the high-flux four-probe is arranged on the sample stand and connected with the multi-channel four-probe resistance tester through a transmission cable, and the data recording software is arranged on the upper computer and receives data measured by the multi-channel four-probe resistance tester. The invention can simultaneously measure and record the change of four probe resistances of up to 64 samples along with time, air pressure, temperature and other parameters under the high-temperature and high-pressure air environment, has enough precision and reliability, extremely high data acquisition frequency, low hardware cost and simple operation method, and can also meet the requirement of accurately measuring the resistance of a small number of samples.
Description
Technical Field
The invention relates to the technical field of material testing, in particular to high-flux material chip four-probe in-situ resistance measuring equipment.
Background
The material high-throughput experimental method in the material genome project is a high-efficiency new material research and development method. The core idea is to complete preparation and characterization of a large number of material samples in a short time, and screen out samples meeting the performance requirements from the samples corresponding to the corresponding processes. Compared with the traditional trial-and-error method, the high-throughput test method has the advantages of short research and development period, low development cost, low labor intensity of personnel and the like, and is a leading edge technology for the development of the current material scientific research and application fields.
The material combined chip technology is a method for preparing a large number of material samples with high flux, the general idea is to use PVD equipment, adopt a discrete mask plate method or a co-sputtering method to prepare a large number of binary, ternary or multi-far materials with different components on a small substrate, and the method can extremely improve the flux of sample preparation. While high throughput characterization and testing of these samples has created a need for high throughput material measurement techniques.
Resistance, as a fundamental physical property of a material, plays an important role in the development of novel semiconductor materials, dielectric materials, battery materials, magnetic materials, and the like. In addition, in some researches on gas sensor materials, the change relation of resistance with the concentration of gas and the temperature needs to be measured, which makes demands on in-situ measurement and recording technology of the resistance. The high-flux resistance measurement technology is combined with the combined chip preparation technology of the materials, so that the purposes of preparing and detecting the high-flux materials can be achieved. In order to achieve the purpose, a conventional resistance measurement device generally uses a probe controlled by a stepping motor to sequentially measure the resistance values of each area, but it is difficult to meet the requirements of in-situ measurement and recording, especially in a severe environment with high temperature and high pressure, and in addition, when the resistance change of a sample needs to be continuously recorded, the measurement interval of each sample is too long, so that the rapid resistance change situation is difficult to deal with. In addition, the four-probe test meters commercially used in China are all single channels at present, the price of a single meter is usually more than 5000 yuan, and if the four-probe test meter is used for high-flux resistance measurement, the cost is high, and the problem of complex connection exists. The invention uses an integrated design, provides a set of device special for in-situ measurement and recording of the resistor in the high-temperature and high-pressure environment in the high-flux research and development of materials aiming at the application problem of in-situ measurement of the high-flux resistor of the materials, has the advantages of simple and convenient operation, relatively low cost, stable and reliable operation, high measurement precision and large data recording quantity, and makes up the blank of the application technology in the domestic field.
Disclosure of Invention
Aiming at the research and development of high-flux materials, the invention provides high-flux material chip four-probe in-situ resistance measurement equipment which is not only suitable for in-situ resistance measurement record of high-flux material samples prepared by a material combination chip method in a high-temperature high-pressure severe environment, but also can meet the requirement of accurate measurement of a small amount of resistance.
The device comprises a high-flux four-probe, a high-temperature and high-pressure resistant airtight tank body, a sample stand, a multi-channel four-probe resistance tester, a transmission cable and data recording software; the sample stand is positioned in the high-temperature and high-pressure resistant airtight tank body, the high-flux four-probe is arranged on the sample stand and connected with the multi-channel four-probe resistance tester through a transmission cable, the data recording software is arranged on the upper computer, and the data recording software receives data measured by the multi-channel four-probe resistance tester and displays and records the data in real time.
The high-temperature and high-pressure resistant airtight tank body is used for providing pressure and atmosphere required by the reaction, and the high-temperature and high-pressure resistant airtight tank body is sealed by an upper sealing cover; the high-temperature and high-pressure resistant airtight tank body is made of high-grade stainless steel, is used under the conditions that the temperature is not higher than 500 ℃ and the pressure is 6MPa, and non-corrosive gases such as hydrogen, oxygen, carbon monoxide, methane and the like react with a sample to be tested in the high-temperature and high-pressure resistant airtight tank body.
The high-temperature and high-pressure resistant airtight tank body is provided with an electrical connecting device, and the electrical connecting device is used for connecting a cable of the high-flux four-probe in the high-temperature and high-pressure resistant airtight tank body with a cable of an external multi-channel four-probe resistance tester, so that the tank body can be ensured not to leak air while the task of electric signal transmission is completed; the upper sealing cover is provided with an air pressure and temperature detecting instrument, an overpressure overtemperature alarming assembly and a pressure relief valve, and an emergency exhaust channel which can empty the gas in the high-temperature and high-pressure resistant airtight tank body within 1-3 seconds, so that the use safety is ensured to the greatest extent.
The high-flux four-probe comprises a shell, a fixed knob, a cable connecting joint and probes, wherein the high-flux four-probe is used for installing probes which are in direct contact with samples, a buffer device is arranged in the probes, the probes are in telescopic mode and can be in non-rigid contact with the surfaces of the samples, the distance between the probes is fixed, the probes are in contact with each sample based on the principle of Van der burg method, and the probes are mainly used for measuring film samples (also called as material chips) with gradient component distribution; the cable connecting joint is positioned in the shell, and the fixing knob is used for fixing the high-flux four-probe with the sample stand.
The internal wires of the transmission cable are made of high-temperature resistant materials, and all the internal wires are shielded by twisted pair wires.
The sample stand adopts an integral structure, the position of the sample can be adjusted and fixed after the sample is loaded, so that the probe on the probe is aligned with each sample strictly, the probe and the sample stand are fixed by bolts, and the relative distance can be adjusted so as to change the contact force between the probe and the surface of the sample. A resistance heating device and a temperature control device are arranged in the sample stand, and are powered by a switching power supply outside the high-temperature-resistant high-pressure airtight tank body; the sample stand comprises an interface, a knob, a base and a clamp, wherein the interface, the knob and the clamp are positioned on the base, the interface is used for being connected with the high-flux four-probe, the knob is used for adjusting the position of a sample, and the clamp is used for adjusting and fixing the position of the sample.
The multi-channel four-probe resistance tester adopts an integrated structure, and a high-precision voltage-controlled constant-current power supply module, a microprocessor control module, a 64-channel voltage sampling circuit, a high-precision ADC module, a temperature detection module, a communication module, a peripheral interface circuit and a switching power supply module which comprise 64 channels and can be independently set with constant current are integrated in one shell structure; the multichannel four-probe resistance tester is externally provided with a connector, four-pin data interfaces, an LCD display screen, a measurement mode selection switch, an LCD brightness adjusting knob and a main power switch, wherein the connector is used for completing data input and output with a transmission cable, the four-pin data interfaces are wiring terminals of 1-8 channels, the sampling frequency of each channel is set in data recording software, and the highest sampling frequency exceeds 50 times/second. In the aspect of peripheral interfaces, two special interfaces are reserved for the instrument, the instrument is respectively used for providing constant-current power supply output for resistance measurement and collecting voltage signal input of a plurality of channels for the high-flux four-probe, and when the instrument is used, only a plug of a special cable is connected into the two interfaces respectively, so that the influence of wiring errors and poor line contact on experiments is effectively avoided, and meanwhile, the labor intensity is greatly reduced. Besides the application of high-flux resistance test, the instrument also reserves wiring terminals of 1-8 channels, and can meet the requirement of four-probe resistance test of a small amount of samples. The instrument reserves RS485 and TCP/IP interfaces for communication with the host computer. In addition, the device can automatically switch the measuring range according to the measured resistance range, the size of the constant current source output value is selected independently, and the work among all channels is independent.
The data recording software displays the current resistance value and the curve of the resistance value changing along with time, air pressure and temperature in real time, and outputs the data in the form of Excel or txt text document files.
The technical scheme of the invention has the following beneficial effects:
the complete equipment designed by the invention has the advantages that the samples are placed on the sample table with the temperature function and the probe fixing function, the accurate alignment of probes and the accurate sample temperature control can be ensured, the high-temperature high-pressure sealing tank provides a safe testing environment for the samples, the special signal transmission cable enables the experimental assembly and connection process to be simple and convenient, the autonomous designed high-flux resistance tester can be matched with the probes to realize the aim of four-probe resistance measurement and recording of up to 64 samples, and the data recording software is friendly in interface, more powerful and convenient to use. The device is designed aiming at high-flux experiment application, can meet the requirement of daily resistance test of a small amount of samples, is relatively low in cost and good in reliability, and has a wide application range in the field of high-flux research of materials.
Drawings
FIG. 1 is a schematic diagram of a high throughput material chip four-probe in-situ resistance measuring apparatus;
FIG. 2 is a schematic diagram of an autonomous development multi-channel four-probe resistance tester according to the present invention;
FIG. 3 is a schematic view of a sample stage with temperature control according to the present invention;
FIG. 4 is a schematic view of a high throughput four-probe head of the present invention.
Wherein: 1-including a high throughput four-probe; 2-a high-temperature and high-pressure resistant airtight tank body; 3-sample stand; 4-an upper sealing cover; 5-a transmission cable; 6-multichannel four-probe resistance tester; 7-data recording software; 11-a housing; 12-fixing a knob; 13-a cable connection joint; 14-probe; 31-interface; 32-a knob; 33-a base; 34-a clamp; 61-linker; 62-four pin data interface; 63-LCD display screen; 64-a measurement mode selection switch; 65-LCD brightness adjusting knob; 66-mains power switch.
Detailed Description
In order to make the technical problems, technical solutions and advantages to be solved more apparent, the following detailed description will be given with reference to the accompanying drawings and specific embodiments.
The invention provides high-flux material chip four-probe in-situ resistance measuring equipment.
As shown in fig. 1, in the apparatus, a sample stand 3 is located in a high temperature and high pressure resistant airtight tank 2, a high flux four-probe 1 is mounted on the sample stand 3, the high flux four-probe 1 is connected to a multi-channel four-probe resistance tester 6 through a transmission cable 5, a data recording software 7 is mounted on an upper computer, and the data recording software 7 receives data measured by the multi-channel four-probe resistance tester 6 and displays and records the data in real time.
As shown in fig. 2, the multi-channel four-probe resistance tester 6 adopts an integrated structure, and a high-precision voltage-controlled constant-current power supply module, a microprocessor control module, a 64-channel voltage sampling circuit, a high-precision ADC module, a temperature detection module, a communication module, a peripheral interface circuit and a switching power supply module which comprise 64 channels and can be independently set with constant current are integrated in one shell structure; the multi-channel four-probe resistance tester 6 is externally provided with a connector 61, a four-pin data interface 62, an LCD display screen 63, a measurement mode selection switch 64, an LCD brightness adjusting knob 65 and a main power switch 66, wherein the connector 61 is used for completing data input and output with a transmission cable, the four-pin data interface 62 is a wiring terminal of 1-8 channels, the sampling frequency of each channel is set in the data recording software 7, and the highest sampling frequency exceeds 50 times/second.
As shown in fig. 3, the sample stand 3 is of an integral structure, and a resistance heating device and a temperature control device are arranged inside the sample stand 3 and are powered by a switching power supply outside the high-temperature and high-pressure resistant airtight tank body 2; the sample stand 3 comprises an interface 31, a knob 32, a base 33 and a clamp 34, wherein the interface 31, the knob 32 and the clamp 34 are positioned on the base 33, the interface 31 is used for being connected with the high-flux four-probe head 1, the knob 32 is used for adjusting the position of a sample, and the clamp 34 is used for adjusting and fixing the position of the sample.
As shown in fig. 4, the high-flux four-probe 1 comprises a shell 11, a fixing knob 12, a cable connecting joint 13 and probes 14, wherein the high-flux four-probe 1 is used for installing probes 14 which are in direct contact with a sample, a buffer device is arranged in the probes 14 and can be in non-rigid contact with the surface of the sample, and the distance between the probes 14 is fixed; a cable connection 13 is located within the housing 11, and a fixing knob 12 is used to fix the high-throughput four-probe head 1 with the sample stage 3.
In the practical use process, firstly, film samples which are prepared by a material combination chip technology and contain 64 different components and are deposited on the same non-conductive substrate are placed into a sample chamber of a sample stand shown in fig. 2, and the positions are adjusted and clamped.
The probe end of the high-flux four-probe shown in fig. 3 is aligned to one side of a sample, the probe and the sample stand are connected by bolts, and as the sample is prepared by adopting a matched mask plate and the sample is well adjusted in position and clamped, each probe on the probe can just contact with the sample, and the requirement of the van der waals method measuring resistance principle on the fact that the probe just contacts with the edge of the sample is met.
The other side of the high-flux four-probe is led out by a special transmission cable and is provided with a plug which is connected with the inside of an electric appliance connecting piece of the airtight tank body. Then the upper sealing cover of the airtight tank body is covered, the matched bolt is used for screwing, and the gas leakage detection operation is carried out.
Two plugs of the external special transmission cable are respectively connected with the outside of an electric appliance connecting piece of the airtight tank body and an input-output special interface of the multi-channel four-probe resistance measuring instrument shown in figure 2.
And connecting the multi-channel four-probe resistance measuring instrument with an upper computer by using a standard RS485 communication line, starting a power switch of the multi-channel four-probe resistance measuring instrument, and preheating for 20min. And then opening independently developed data recording software installed in the upper computer to configure each channel of the sample to be measured. The configuration content comprises: the measuring interval of the instrument can be manually set according to the approximate resistance range of each sample, at the moment, the instrument can configure the current output by the constant current source and the amplification factor of the operational amplifier of the voltage acquisition circuit according to the range of the measured resistance value, or can select to not configure, and the system can dynamically adjust related parameters according to the resistance value measured for the first time in the test. The time interval, i.e. the sampling frequency, of each channel data record is selected. The test modes of software fall into three categories: "time-resistance", "temperature-resistance", "barometric-resistance", unless otherwise set, the system defaults to "time-resistance" mode, with resistance on the ordinate and time on the abscissa, for continuous data recording until the stop record button is pressed. If configured in the other two modes, the resistances are not recorded on the ordinate with temperature or air pressure, respectively, and the software also provides the option: the recording time is the second abscissa, if the time is required to be recorded at the same time, the check box is checked, at the moment, the software can record the time which is the second abscissa in the measuring process, otherwise, the software does not record the time in the measuring process. After the configuration is finished, the resistance measurement and data recording functions of the whole equipment can be started.
Selecting a test environment of a sample, if the change relation of the sample resistance along with the temperature needs to be measured, configuring a corresponding controller of a sample support temperature control device in the sealed tank, setting an initial temperature, a heating step length and a highest temperature, and selecting a temperature-resistance test mode in data recording software, wherein the system continuously receives temperature sensor data on the sample support in the tank, and records the data by taking the temperature as an ordinate and the resistance value as an abscissa. If the system is applied to resistance research of the gas sensitive material, the 'air pressure-resistance' test function is required to be selected in data recording software, at the moment, the system collects and records data of a digital air pressure meter in the tank body, and records by taking air pressure as an abscissa and resistance as an ordinate. Additional dispensing gas sources are needed to apply pressure to the tank to meet the environmental requirements for sample resistance measurement.
When flammable and explosive dangerous gas is used, if leakage occurs or the pressure in the tank is monitored to exceed the warning level, the automatic pressure control valve arranged on the sealing cover starts the vacuumizing operation, and the vacuumizing operation can be started manually, so that the safety problem is avoided.
After the resistance measurement is completed, the data result output form is selected from the data recording software of the upper computer, and can be set to be an Excel form output or a Txt text document format output.
And closing a power supply of the multichannel resistance measuring instrument, vacuumizing or cooling the sealed tank, opening the sealing cover after the temperature reaches the room temperature or the vacuumizing in the tank is finished, dismantling the fixed high-flux four-probe, releasing the fixation of the sample frame, and taking out the sample to finish the test.
Example 1
In this embodiment, a high-flux method is used to screen a component with a minimum resistance temperature effect from a ternary material, so as to illustrate the research application of the high-flux in-situ resistance test device. The specific steps of this embodiment are as follows:
a1, selecting a three-element material film sample which is prepared by adopting a combined chip method and takes a 3-inch quartz plate as a substrate, wherein 64 three-element material film samples which are mutually independent and have different components and have the size of A multiplied by A (A=1-3 mm) are plated on the surface of the three-element material film sample. Placing the sample into a sample stand, adjusting the position and fixing.
B1, fixing the high-flux four-probe with a sample stand by adopting bolts, wherein the probe of the probe can just contact with a proper position on the surface of a sample well because the preparation of the sample and the design of the probe adopt compatible sizes.
And C1, connecting the cable plug of the four-probe with the inside of an electric connecting piece of the tank body, covering an airtight cover and fixing the cable plug by bolts, completing the airtight inspection of the tank body and vacuumizing, and introducing 2MPa argon as protective gas to prevent sample oxidation in the heating process. And then the external part of the electric connector of the tank body is connected with the input and output ends of the multi-channel four-probe resistance tester by using a special cable.
And D1, opening data recording software of the upper computer, setting configuration of a constant current source and a voltage acquisition circuit as defaults, selecting a temperature-resistance measuring mode of the instrument, not choosing a second abscissa as the recording time, setting a temperature recording step length to be 1 ℃, namely, recording resistance data of each sample once every time the temperature rises.
E1, configuring equipment parameters for controlling the internal resistance heating temperature control element of the sample stand, setting the initial temperature to 25 ℃, setting the heating mode to be a stepping mode, namely keeping the temperature for 3s when the temperature is increased by 1 ℃, and then continuously heating the sample stand, wherein the heating maximum temperature is 200 ℃.
F1, clicking a data recording software recording start button of the upper computer, starting a control power supply of heating equipment, and automatically recording resistance data of 64 samples from 25-200 ℃ by using the system with the temperature of 1 ℃ as a step length.
And G1, after the test is finished, closing the heating controller, selecting the data output form in the data recording software as Excel output, and selecting and storing the data storage directory.
H1, after the temperature of the sample is cooled to the room temperature, manually starting a vacuum pump, pumping the air pressure in the pipe to about 1bar, starting an air sealing cover, disassembling the four probe probes, taking out the sample for storage, closing a power supply connected with equipment, and finishing the cable.
And I1, using data in Excel, taking temperature as an abscissa, taking the resistance of each sample as an ordinate, drawing a curve of the resistance of each sample along with the temperature change in a drawing software, and selecting a component corresponding to the sample with the lowest gradient of the resistance along with the temperature change, namely the target component with the minimum resistance temperature coefficient in the ternary material.
Example 2
In this embodiment, a high-flux method is used to screen a component with the fastest hydrogen-sensitive resistance response from a certain ternary hydrogen-sensitive material, so as to illustrate the research application of the high-flux in-situ resistance test equipment. The specific steps of this embodiment are as follows:
a2, selecting a three-element material film sample which is prepared by adopting a combined chip method and takes a 3-inch quartz plate as a substrate, wherein 64 three-element material film samples which are mutually independent and have different components and have the size of B multiplied by B (A=1-3 mm) are plated on the surface of the three-element material film sample. Placing the sample into a sample stand, adjusting the position and fixing.
And B2, fixing the high-flux four-probe with the sample stand by adopting bolts, wherein the probe of the probe can just contact with the proper position of the surface of the sample well because the preparation of the sample and the design of the probe adopt compatible sizes.
And C2, connecting the cable plug of the four-probe with the inside of the electric appliance connecting piece of the tank body, covering the sealing cover and fixing the sealing cover by using bolts, and completing the air tightness inspection and vacuumizing of the tank body. And then the external part of the electric connector of the tank body is connected with the input and output ends of the multi-channel four-probe resistance tester by using a special cable.
And D2, opening data recording software of the upper computer, setting configuration of a constant current source and a voltage acquisition circuit as defaults, selecting an air pressure-resistance measuring mode of the instrument, checking the recording time as a second abscissa, setting the time recording step length of the resistance as 0.1s, namely recording a resistance value every 0.1 second for each sample.
E2, configuring equipment parameters for controlling the internal resistance heating temperature control element of the sample stand, setting the initial temperature to 25 ℃, the heating rate to 5 ℃/min, the target temperature to 60 ℃ and the heat preservation time to 100h. And starting a heating power supply to raise the temperature, and waiting for the temperature of the sample to reach 60 ℃ and to be stable.
F2, clicking a data recording software recording start button of the upper computer, setting the air pressure at the low pressure side of the pressure reducing valve of the hydrogen cylinder to be 0.1MPa, opening an air inlet valve, rapidly introducing 0.1MPa H2 into the air tight tank, at the moment, recording the air pressure change in the tank by the software, and changing the resistance of each sample along with time after introducing H2, namely, responding the hydrogen sensitive resistance of the sample. Wait for 30min. The vacuum pump and the vacuum valve are started, H2 in the tank is pumped out within 3 seconds, and then argon of 0.1MPa is introduced in a very short time, and at the moment, the response characteristics of the resistors of each sample after the H2 atmosphere is removed are recorded by software. After waiting for 30min, argon is pumped out again, and then 0.1MPa of hydrogen is introduced, at this time, the samples record the resistance response characteristics of each sample to hydrogen in the second cycle. This was repeated 10 times.
After the test, the atmosphere in the tank is first pumped out, and then argon of 0.1MPa is introduced. And closing the heating controller, selecting the data output form in the data recording software as Excel output, and selecting and storing the data storage directory.
And H2, after the temperature of the sample is cooled to the room temperature, manually starting a vacuum pump, pumping the air pressure in the pipe to about 1bar, starting an air sealing cover, disassembling the four probe probes, taking out the sample for storage, closing a power supply connected with equipment, and finishing the cable.
And I2, using data in Excel, taking temperature as an abscissa, taking the resistance of each sample as an ordinate, drawing a curve of each sample resistance changing along with the temperature in a drawing software, screening out components with the fastest hydrogen-sensitive resistance response characteristic from the ternary material according to the change rate of each sample resistance along with time after hydrogen is introduced and hydrogen is removed, and judging the material components with the best performance retention rate in the circulation process according to the hydrogen-sensitive resistance response rate of each sample after 10 times of circulation.
While the foregoing is directed to the preferred embodiments of the present invention, it will be appreciated by those skilled in the art that various modifications and adaptations can be made without departing from the principles of the present invention, and such modifications and adaptations are intended to be comprehended within the scope of the present invention.
Claims (4)
1. A high flux material chip four-probe in-situ resistance measuring device is characterized in that: the high-flux four-probe comprises a high-flux four-probe (1), a high-temperature and high-pressure resistant airtight tank body (2), a sample stand (3), a multi-channel four-probe resistance tester (6), a transmission cable (5) and data recording software (7); the high-flux four-probe (1) is arranged on the sample stand (3), the high-flux four-probe (1) is connected with the multi-channel four-probe resistance tester (6) through a transmission cable (5), the data recording software (7) is arranged on an upper computer, and the data recording software (7) receives data measured by the multi-channel four-probe resistance tester (6) and displays and records the data in real time;
the high-temperature and high-pressure resistant airtight tank body (2) is used for providing pressure and atmosphere required by reaction, and the high-temperature and high-pressure resistant airtight tank body (2) is sealed through the upper sealing cover (4); the high-temperature and high-pressure resistant airtight tank body (2) is made of high-grade stainless steel, is used under the conditions that the temperature does not exceed 500 ℃ and the pressure is 6MPa, and non-corrosive gas reacts with a tested sample in the high-temperature and high-pressure resistant airtight tank body (2);
an electrical connection device is arranged on the high-temperature-resistant high-pressure-resistant airtight tank body (2), and a cable of the high-flux four-probe in the high-temperature-resistant high-pressure-resistant airtight tank body (2) is connected with a cable of an external multichannel four-probe resistance tester; the upper sealing cover (4) is provided with an air pressure and temperature detecting instrument, an overpressure overtemperature alarming assembly and a pressure relief valve, and an emergency exhaust channel which can empty the air in the high-temperature and high-pressure resistant airtight tank body (2) within 1-3 seconds;
the high-flux four-probe (1) comprises a shell (11), a fixing knob (12), a cable connecting joint (13) and a probe (14), wherein the high-flux four-probe (1) is used for installing the probe (14) which is in direct contact with a sample, a buffer device is arranged in the probe (14) and can be in non-rigid contact with the surface of the sample, and the distance between the probes (14) is fixed; the cable connecting joint (13) is positioned in the shell (11), and the fixing knob (12) is used for fixing the high-flux four-probe (1) and the sample stand (3);
the multi-channel four-probe resistance tester (6) adopts an integrated structure, and a high-precision voltage-controlled constant-current power supply module, a microprocessor control module, a 64-channel voltage sampling circuit, a high-precision ADC module, a temperature detection module, a communication module, a peripheral interface circuit and a switching power supply module which comprise 64 channels and can be independently set with constant current are integrated in one shell structure; the multi-channel four-probe resistance tester (6) is externally provided with a connector (61), four-pin data interfaces (62), an LCD display screen (63), a measurement mode selection switch (64), an LCD brightness adjusting knob (65) and a main power switch (66), wherein the connector (61) is used for completing data input and output with a transmission cable, the four-pin data interfaces (62) are wiring terminals of 1-8 channels, the sampling frequency of each channel is set in data recording software (7), and the highest sampling frequency exceeds 50 times/second;
wherein,
the using method of the four-probe in-situ resistance measuring device of the high-flux material chip comprises the following steps:
the multi-channel four-probe resistance measuring instrument is connected with an upper computer through an RS485 communication line;
starting a power switch of the multi-channel four-probe resistance measuring instrument, and preheating for 20min;
opening independently developed data recording software installed in an upper computer, and configuring each channel of a sample to be measured, wherein the configuration content comprises:
setting a measuring interval of an instrument manually according to the resistance range of each sample, configuring the current size output by a constant current source and the amplification factor of an operational amplifier of a voltage acquisition circuit by a multi-channel four-probe resistance tester according to the range of the measured resistance value, and dynamically adjusting current parameters and voltage parameters according to the resistance value measured for the first time in the test by the multi-channel four-probe resistance tester if the current size and the amplification factor of the operational amplifier of the voltage acquisition circuit are not configured;
selecting a test environment of a sample, if the change relation of the sample resistance along with the temperature needs to be measured, configuring a corresponding controller of a sample support temperature control device in the sealed tank, and setting an initial temperature, a temperature rising step length and a highest temperature;
selecting a time interval of data recording of each channel in the multi-channel four-probe resistance measuring instrument, namely sampling frequency, and selecting a software testing mode, wherein the software testing mode comprises a time-resistance mode, a temperature-resistance mode and a pressure-resistance mode;
wherein in time-resistance mode: continuously recording data by taking the resistor as an ordinate and the time as an abscissa until a record stopping button is pressed;
in the temperature-resistance mode, continuously recording data by taking the resistance as an ordinate and the temperature as an abscissa until a record stop button is pressed;
in the air pressure-resistance mode, the resistance is taken as an ordinate, and the air pressure is taken as an abscissa to perform continuous data recording until a record stopping button is pressed;
after the resistance measurement is completed, a data result output form is selected in data recording software of the upper computer, and is set to be Excel form output or Txt text document format output.
2. The high throughput material chip four-probe in-situ resistance measuring apparatus of claim 1, wherein: the internal wires of the transmission cable (5) are made of high-temperature resistant materials, and all the internal wires are shielded by twisted pair wires.
3. The high throughput material chip four-probe in-situ resistance measuring apparatus of claim 1, wherein: the sample stand (3) adopts an integral structure, and resistance heating equipment and temperature control equipment are arranged inside the sample stand (3) and are powered by a switching power supply outside the high-temperature-resistant high-pressure airtight tank body (2); the sample stand (3) comprises an interface (31), a knob (32), a base (33) and a clamp (34), wherein the interface (31), the knob (32) and the clamp (34) are positioned on the base (33), the interface (31) is used for being connected with the high-flux four-probe head (1), the knob (32) is used for adjusting the position of a sample, and the clamp (34) is used for adjusting and fixing the position of the sample.
4. The high throughput material chip four-probe in-situ resistance measuring apparatus of claim 1, wherein: the data recording software (7) displays the current resistance value and the curve of the resistance value changing along with time, air pressure and temperature in real time, and outputs the data in the form of Excel or txt text document files.
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| CN110568024A (en) * | 2019-09-02 | 2019-12-13 | 中国工程物理研究院材料研究所 | Gas-sensitive performance testing device based on four-probe method |
| CN110646468B (en) * | 2019-09-29 | 2022-02-11 | 天津职业技术师范大学(中国职业培训指导教师进修中心) | Method for characterizing high-throughput materials |
| CN113504268A (en) * | 2021-06-10 | 2021-10-15 | 上海大学 | System-level electrical performance testing device for perovskite device |
| CN113406392B (en) * | 2021-06-16 | 2022-05-03 | 国网安徽省电力有限公司电力科学研究院 | Resistance measuring device and resistance measuring method in cable buffer layer ablation process |
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