CN114965866B - System for measuring physical properties of a material - Google Patents
System for measuring physical properties of a material Download PDFInfo
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- CN114965866B CN114965866B CN202110208277.3A CN202110208277A CN114965866B CN 114965866 B CN114965866 B CN 114965866B CN 202110208277 A CN202110208277 A CN 202110208277A CN 114965866 B CN114965866 B CN 114965866B
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 31
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- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 10
- 238000004070 electrodeposition Methods 0.000 claims description 8
- 230000003287 optical effect Effects 0.000 claims description 7
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 6
- 238000003466 welding Methods 0.000 claims description 6
- 238000012423 maintenance Methods 0.000 abstract 1
- 230000001681 protective effect Effects 0.000 description 25
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 4
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01D—MEASURING NOT SPECIALLY ADAPTED FOR A SPECIFIC VARIABLE; ARRANGEMENTS FOR MEASURING TWO OR MORE VARIABLES NOT COVERED IN A SINGLE OTHER SUBCLASS; TARIFF METERING APPARATUS; MEASURING OR TESTING NOT OTHERWISE PROVIDED FOR
- G01D21/00—Measuring or testing not otherwise provided for
- G01D21/02—Measuring two or more variables by means not covered by a single other subclass
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- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Medicinal Chemistry (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Materials Using Thermal Means (AREA)
Abstract
The present invention provides a system for measuring a physical property of a material, comprising: the device comprises a deposition unit, a wire bonding unit, a variable-temperature electrotransport measurement unit and a gas purification unit; the deposition unit, the wire bonding unit and the variable-temperature electric transport measurement unit are communicated through a sample transfer channel; the gas purifying unit is in airtight communication with the deposition unit, the wire bonding unit and the variable temperature electric transportation measuring unit through a gas circulation channel, so that the system forms a gas circulation loop; the deposition unit comprises an electrode deposition preparation unit and an electrode deposition unit which are communicated in a sealing way through a vacuum gate valve; the system further comprises a sample inlet and outlet conduit for sample to enter and leave the system. The measuring system has the characteristics of cost saving, easy maintenance and simple operation, and is particularly suitable for measuring the physical properties of materials sensitive to oxygen and water vapor.
Description
Technical Field
The present invention relates to the field of physical property measurement. In particular, the present invention relates to a system for measuring physical properties of a material.
Background
The measurement of physical properties such as electrical properties, magnetic properties, optical properties, thermal properties and the like is an experimental basis of subjects such as material science, condensed state physics and the like. The corresponding experimental device is usually placed under the ordinary atmospheric environment to perform experimental operation.
However, recent advances in materials research have presented unprecedented challenges to these conventional physical property measurement systems that currently exist. Specific reasons are explained below, some novel quantum functional materials, such as topological insulator materials (Science 318,766 (2007)), iron-based superconductor materials (Journal of the American Chemical Society 130,3296 (2008)), zinc-arsenic-based diluted magnetic semiconductor materials (Nature Communications, 422 (2011)), quantum anomalous hall effect materials (Science 340,167 (2013)), and the like, are sensitive to air, and easily react with oxygen and water vapor in the air to deteriorate and degrade (Reviews of Modern Physics 83,1589 (2011)). The new materials have very important scientific significance for material science, physical research and technical application, and the acquisition of intrinsic physical properties of the materials under the precondition that the materials do not deteriorate and degenerate is of great importance for developing physical research and technical application.
At present, when the conventional physical property measuring system is used for carrying out experimental study on oxygen and water vapor sensitive materials, the materials are inevitably exposed in the air in the specific operation processes of sample preparation, sample transfer, and the like, and then react with oxygen and water vapor to cause deterioration and degradation.
There is an urgent need for a system for measuring physical properties of materials that is cost effective, easy to maintain and simple to operate, and is suitable for use in materials that are sensitive to oxygen and moisture.
Disclosure of Invention
It is an object of the present invention to provide a system for measuring physical properties of a material. The measuring system can solve the problems that the prior measuring system for physical properties inevitably reacts with oxygen and water vapor to cause material deterioration and degradation in the process of measuring the physical properties of oxygen and water vapor sensitive functional materials.
The above object of the present invention is achieved by the following technical solutions.
The present invention provides a system for measuring a physical property of a material, comprising:
the device comprises a deposition unit, a wire bonding unit, a variable-temperature electrotransport measurement unit and a gas purification unit; wherein,,
the deposition unit, the wire bonding unit and the variable-temperature electrotransport measurement unit are communicated through a sample transfer channel; the gas purifying unit is in airtight communication with the deposition unit, the wire bonding unit and the variable temperature electric transportation measuring unit through a gas circulation channel, so that the system forms a gas circulation loop; the deposition unit comprises an electrode deposition preparation unit and an electrode deposition unit which are communicated in a sealing way through a vacuum gate valve;
the system further comprises a sample inlet and outlet conduit for sample to enter and leave the system.
Preferably, in the measurement system according to the present invention, the sample inlet and outlet pipe is provided on at least one of the deposition unit, the wire bonding unit, and the temperature-changing electrotransport measurement unit. When the sample inlet and outlet pipe is provided on the deposition unit, the sample inlet and outlet pipe is provided on the electrode deposition preparation unit of the deposition unit. On the one hand, the electrode deposition preparation unit is connected with other functional units of the measuring system to form a gas circulation loop. On the other hand, the electrode deposition preparation unit provides a buffer and stable ambient atmosphere for the electrode deposition unit, so that an operator can put in a sample to be processed, can take out the processed sample, and can perform the operation of installing a metal mask plate and the like serving the electrode deposition unit.
Preferably, in the system for measuring physical properties of materials according to the present invention, sealing valves are provided at both sides of the sample inlet and outlet pipe.
Preferably, in the system for measuring physical properties of a material according to the present invention, a sample carrier is provided in the sample transfer channel, so that the sample is free to move in the sample transfer channel.
Preferably, in the system for measuring physical properties of a material according to the present invention, both ends of the sample transfer channel are provided with sealing valves.
Preferably, in the system for measuring physical properties of materials according to the present invention, the gas circulation channel is provided with an oxygen content probe, a water vapor content probe and a gas pressure probe, and is connected to a gas source and a mechanical pump through electromagnetic valves, respectively.
Preferably, in the system for measuring physical properties of a material according to the present invention, the electrodeposition preparing unit includes an electrodeposition preparing enclosure; the electrode deposition preparation airtight box body is provided with a first airtight box body observation window and a first rubber glove interface.
Preferably, in the system for measuring physical properties of a material according to the present invention, the electrode deposition unit includes an electrode deposition vacuum chamber, a magnetron sputtering target, and a sample transfer bar; and a deposition sample stage is arranged in the electrode deposition vacuum chamber.
In a specific embodiment of the invention, the electrode deposition unit further comprises a vacuum pump matched with the electrode deposition unit to vacuumize the electrode deposition vacuum chamber; preferably, the vacuum pump may be a two-stage pump set consisting of a molecular pump and a mechanical pump. The air inlet of the molecular pump is connected with the electrode deposition vacuum chamber through a vacuum gate valve, the air outlet of the molecular pump is connected with the air inlet of the mechanical pump, and the air outlet of the mechanical pump is connected with a tail gas recovery pipeline.
Preferably, in the system for measuring physical properties of a material according to the present invention, the vacuum chamber for electrode deposition is provided with a vacuum chamber observation window.
Preferably, in the system for measuring physical properties of a material according to the present invention, the wire bonding unit includes a wire bonding enclosure and an ultrasonic bonding Device, a bonding sample stage, a temperature change measurement sample carrier, an optical microscope, a CCD (Charge-coupled Device) camera, and a display disposed therein.
Preferably, in the system for measuring physical properties of a material according to the present invention, the wire bonding enclosure is provided with a second enclosure viewing window and a second rubber glove port.
Preferably, in the system for measuring physical properties of a material according to the present invention, the temperature change measurement sample carrier comprises a heat sink, a thermally conductive insulating plate on the heat sink, and a bonding metal post on the thermally conductive insulating plate.
Preferably, in the system for measuring physical properties of materials according to the present invention, the temperature-varying electrotransport measurement unit includes a temperature-varying electrotransport measurement enclosure and a measurement cable, a microwave waveguide cable and antenna, a cold head and a temperature-varying electrotransport measurement vacuum chamber disposed therein, and a helium compressor, a compressed helium pipeline, a refrigerator, a measurement instrument, and a vacuum aviation connector disposed outside thereof.
Preferably, in the system for measuring physical properties of materials according to the present invention, the temperature-changing electrotransport measurement enclosure is provided with a third enclosure observation window and a third rubber glove port.
Preferably, in the system for measuring physical properties of a material according to the present invention, the gas purifying unit includes a gas purifying tank and a blower, an organic gas purifying column, and an oxygen water purifying column disposed therein.
In the specific embodiment of the invention, an electrode deposition preparation closed box, a wire bonding closed box, a temperature-changing electrotransport measurement closed box and a gas purifying box are connected through a sample transfer channel or a gas circulation channel, and the inside is filled with protective atmosphere gas with atmospheric pressure to form a closed loop of the gas environment.
In a specific embodiment of the invention, the temperature change measurement sample carrier is composed of a heat sink, a heat conducting insulating plate and a bonding metal column. The heat sink is preferably made of oxygen-free copper, the heat conducting insulating plate is preferably made of sapphire, and the bonding metal column is preferably made of a stainless steel column with an electro-gold plating coating on the surface.
In the specific embodiment of the invention, the sample transfer channel not only can meet the air tightness, but also can transfer samples between the electrode deposition preparation sealed box, the lead bonding sealed box and the temperature-changing electrotransport measurement sealed box under the environment of one atmosphere.
In particular embodiments of the present invention, a sample carrier may be provided within the sample transfer channel to transfer the sample. Specifically, fixed pulleys can be placed at two ends of the sample transfer channel to move the sample carrier, so that the sample transfer is realized.
In a specific embodiment of the invention, the gas pressure in the measurement system is regulated by a gas purification unit. A gas pressure probe may be provided on the gas circulation channel to detect the pressure within the measurement system. The mechanical pump and the gas source can be connected with the gas circulation channel through electromagnetic valves respectively. In order to maintain the balance between the air pressure in the air circulation channel and the air pressure in the surrounding environment of the system, in a set error range, when the value detected by the air pressure probe is smaller than the air pressure value in the surrounding environment of the system, the first electromagnetic valve is opened, and the air source supplements air into the air circulation channel; and when the value detected by the gas pressure probe is larger than the gas pressure value of the surrounding environment of the system, the second electromagnetic valve is opened, and the mechanical pump extracts gas from the gas circulation channel.
In a specific embodiment of the present invention, the protective atmosphere gas is typically nitrogen or argon. In the measuring system of the invention, the total air pressure in the control system is about 1 standard atmosphere, and the residual oxygen and water vapor content in the air in the control system is maintained at a low level. The relative content of residual oxygen and water vapor is generally less than 1×10 -7 I.e. 0.1ppm.
In a specific embodiment of the invention, one end of the sample inlet and outlet pipe can be connected with an electrode deposition preparation closed box, a wire bonding closed box or a temperature-changing electrotransport measurement closed box. The other end of the sample inlet and outlet pipeline can be connected with a closed box body under other protective atmosphere environments, and can also be connected with an air environment according to actual working requirements.
In particular embodiments of the invention, the gaseous environment of the sample inlet and outlet conduit can be switched between a vacuum environment and a protective atmosphere environment at one atmosphere, depending on the operational requirements.
In the specific embodiment of the invention, the inside of the organic gas purifying column is filled with a material such as activated carbon for adsorbing organic molecules, and the inside of the oxygen water purifying column is filled with a material such as copper catalyst, molecular sieve for adsorbing oxygen and water vapor.
In the specific embodiment of the invention, the materials of the vacuum chamber observation window and the closed box observation window can be glass, organic glass, quartz and the like.
In the specific embodiment of the invention, the magnetron sputtering target material is made of common electrode metals such as gold, silver, platinum and the like, and common transition layer metals such as titanium, nickel and the like.
The invention has the following beneficial effects:
the measuring system can finish the physical property measurement of the sample in the protective atmosphere environment, thereby obtaining more essential physical properties of oxygen and water vapor sensitive materials.
The measurement system of the present invention places a portion of the functional units for physical property measurement in an oxygen-free, water-free protective atmosphere. Compared with the technical scheme that the physical property measurement platform is integrally placed in an oxygen-free and water-free protective atmosphere environment, the system cost and the measurement operation cost of the scheme are low. In addition, it is contemplated that if the physical property measurement system is placed entirely within a closed environment and the atmosphere within the closed environment is converted to an oxygen-free, water-free, protective atmosphere environment, it is apparent that the equipment manufacturing and operating costs of such a solution would be very expensive, and, more importantly, the operator would need to wear costly protective clothing to complete the experimental measurement operation, which is very detrimental to practical use.
The measuring system has expandability, and can enable operations such as sample manufacture, crystal structure characterization, micro-nano processing, physical property measurement and the like to be carried out in a protective atmosphere environment through design and integration.
Drawings
Embodiments of the present invention are described in detail below with reference to the attached drawing figures, wherein:
FIG. 1 is a schematic diagram of a system for measuring physical properties of a material according to one embodiment of the present invention;
FIG. 2 is a schematic diagram of a temperature change measurement sample carrier according to one embodiment of the present invention;
wherein, the reference numerals:
1-an electrode deposition vacuum chamber; 2-magnetron sputtering target; 3-sample transfer bar; 4-electrode deposition sample stage; 5-a vacuum chamber viewing window; 6-a vacuum gate valve; 7-preparing a closed box body by electrode deposition; 8-a first closed box observation window; 9-a first rubber glove port; 10-a first sample transfer channel; 11-sample carrier; 12-sample inlet and outlet pipes; 13-closed box under other protective atmosphere environment; 14-wire bonding the closed box body; 15-a second closed box observation window; 16-a second rubber glove port; 17-an ultrasonic pressure welding device; 18-bonding the sample stage; 19-a temperature change measurement sample carrier; 20-optical microscope; a 21-CCD camera; 22-a display; 23-a second sample transfer channel; 24-measuring the closed box body by variable-temperature electric transportation; 25-a third closed box observation window; 26-a third rubber glove port; 27-changing temperature electrotransport measurement vacuum chamber; 28-cold head; 29-measuring cable; 30-microwave waveguide cable and antenna; 31-a refrigerator; 32-vacuum air connectors; 33-compressed helium piping; a 34-helium compressor; 35-measuring instrument; 36-a first gas circulation channel; 37-a gas purifying box; 38-a fan; 39-an oxygen water purifying column; 40-an organic gas purifying column; 41-a second gas circulation channel; 42-a first solenoid valve; 43-gas source; 44-a second solenoid valve; 45-mechanical pump; 46-gas pressure probe; 47-oxygen content probe; 48-a water vapor content probe; 49-a heat sink; a 50-bond metal column; 51-a heat conducting insulating plate.
Detailed Description
Referring now to the drawings, illustrative versions of the disclosed architecture are described in detail. Although the drawings are provided to present embodiments of the invention, the drawings are not necessarily to scale and certain features may be exaggerated, removed, or partially sectioned to better illustrate and explain the present disclosure. Certain directional terms used hereinafter to describe the drawings will be understood to have their ordinary meaning and refer to those directions as they would normally be in reference to the drawings.
In the measurement of physical properties of materials, measurement of electrotransport measurement is generally indispensable. Referring to fig. 1, fig. 1 shows a schematic diagram of a measurement system according to one embodiment of the present invention. The system for measuring physical properties of a material of the present invention comprises: the device comprises a deposition unit, a wire bonding unit, a variable-temperature electrotransport measurement unit and a gas purification unit; the deposition unit, the wire bonding unit and the variable-temperature electric transport measurement unit are communicated through a sample transfer channel; the gas purifying unit is in airtight communication with the deposition unit, the wire bonding unit and the variable temperature electric transportation measuring unit through a gas circulation channel, so that the system forms a gas circulation loop; the deposition unit comprises an electrode deposition preparation unit and an electrode deposition unit which are communicated in a sealing way through a vacuum gate valve 6; the system further includes a sample access conduit 12 to enable sample access to the system.
In the specific embodiment of the present invention, sealing valves are provided on both sides of the sample inlet and outlet pipe 12. A sample carrier 11 is provided in the first sample transfer channel 10 so that the sample is free to move within the sample transfer channel. The second sample transfer channel 23 may not be provided with a sample carrier, but the transfer of the sample may be performed manually.
In the embodiment of the present invention, the second gas circulation path 41 is provided with a gas pressure probe 46, an oxygen content probe 47, and a moisture content probe 48.
In a specific embodiment of the present invention, the electrodeposition preparing unit includes an electrodeposition preparing enclosure 7; the first airtight box observation window 8 and the first rubber glove port 9 are arranged on the electrode deposition preparation airtight box 7.
In a specific embodiment of the present invention, the electrode deposition unit comprises an electrode deposition vacuum chamber 1, a magnetron sputtering target 2 and a sample transfer rod 3; an electrode deposition sample stage 4 is arranged in the electrode deposition vacuum chamber 1; preferably, the vacuum chamber 1 is provided with a vacuum chamber observation window 5.
In the specific embodiment of the invention, the wire bonding unit comprises a wire bonding closed box 14, an ultrasonic pressure welding device 17, a bonding sample stage 18, a temperature change measurement sample carrier 19, an optical microscope 20, a CCD camera 21 and a display 22, wherein the ultrasonic pressure welding device 17, the bonding sample stage 18, the temperature change measurement sample carrier and the display 22 are arranged in the wire bonding closed box; preferably, the wire bonding airtight box 14 is provided with a second airtight box observation window 15 and a second rubber glove port 16.
Referring to fig. 2, in a specific embodiment of the present invention, temperature change measurement sample carrier 19 includes a heat sink 49, a thermally conductive insulating plate 51 positioned on heat sink 49, and a bonding metal post 50 positioned on thermally conductive insulating plate 51.
In the specific embodiment of the invention, the temperature-varying electrotransport measurement unit comprises a temperature-varying electrotransport measurement closed box body 24, a measurement cable 29, a microwave waveguide cable and antenna 30, a cold head 28 and a temperature-varying electrotransport measurement vacuum chamber 27 which are arranged in the temperature-varying electrotransport measurement closed box body, and a helium gas compressor 34, a compressed helium gas pipeline 33, a refrigerator 31, a measurement instrument 35 and a vacuum aviation connector 32 which are arranged outside the temperature-varying electrotransport measurement closed box body; preferably, a third sealed box observation window 25 and a third rubber glove port 26 are arranged on the temperature-changing electrotransport measurement sealed box 24.
In the specific embodiment of the present invention, the gas cleaning unit includes a gas cleaning tank 37 and a blower 38, an organic gas cleaning column 40 and an oxygen water cleaning column 39 disposed therein.
In a specific embodiment of the invention, the gas pressure in the measurement system is regulated by a gas purification unit. A gas pressure probe 46 may be provided on the second gas circulation channel 41 to detect the gas pressure within the measurement system. The mechanical pump 45 and the protective gas source 43 may be connected to the second gas circulation passage 41 through solenoid valves, respectively. In order to maintain the balance between the air pressure in the second air circulation channel 41 and the air pressure in the system surrounding environment, in a set error range, when the value detected by the air pressure probe 46 is smaller than the air pressure value in the system surrounding environment, the first electromagnetic valve 42 is opened, and the protective air source 43 supplements air into the second air circulation channel 41; and when the value detected by the gas pressure probe 44 is greater than the air pressure value of the surrounding environment of the system, the second electromagnetic valve 44 is opened, and the mechanical pump 45 pumps the gas from the second gas circulation channel 41.
The sample electrotransport measurement generally consists of an early preparation and actual measurement. The pre-preparation generally comprises three steps of sample transfer, electrode deposition, wire bonding and the like. In a specific embodiment of the invention, the sample transfer is performed in a sample transfer channel. The transfer of the sample is performed in a controlled protective atmosphere. When the distance between the two closed boxes involved in sample transfer is relatively short, the sample can be directly transferred manually through the sample transfer channel. When the distance between the two closed boxes is far, the sample can be transferred by means of the sample carrier. In the specific embodiment of the invention, a fixed pulley is arranged at two ends of a longer sample transfer channel, and the sample carrier can move back and forth in the sample transfer channel by means of the fixed pulley and a rope, so that the transfer of samples is realized. The disclosure of the present invention is further illustrated below by specific operational steps.
Step 1: electrode deposition
Firstly, samples processed (such as micro-nano processing) in other protective atmosphere closed boxes are transferred into a wire bonding closed box through a sample inlet and outlet pipeline, and then further transferred into an electrode deposition preparation closed box through a first sample transfer channel by a sample carrier. Then, the sample is placed on a special carrier for electrode deposition, and a metal mask plate with an artificial designed pattern is fixed on the surface of the sample. Then, the protective atmosphere with 1 atmosphere is filled in the vacuum chamber for the electrodeposition, the vacuum gate valve is opened, and then the special carrier for the electrodeposition is placed on the electrodeposition sample stage by using the sample conveying rod. Next, the electrode deposition vacuum vessel is evacuated to about 2X 10 -6 Pa, and heating the heating table to a suitable temperature. And finally, closing the vacuum system, filling high-purity argon with the pressure of about 10Pa into the electrode deposition vacuum chamber, and then applying proper voltage to the magnetron sputtering target. At this time, under the combined action of the electric field and the magnetic field, plasma glow of argon and metal to be deposited is formed in the electrode deposition vacuum chamber. When the plasma reaches the sample stage, it will grow into a thin film electrode according to the design pattern of the metal mask. The metal to be deposited is typically gold, silver, platinum, etc.
Step 2: wire bonding
First, the sample obtained in step 1 is transferred into a wire-bonded hermetic container. Subsequently, the temperature change measurement sample carrier is placed onto the bonding sample stage and the sample is glued to the heat sink of the carrier using a low temperature heat conductive glue. The temperature change measurement sample carrier with the adhered sample is then moved to the focal point of the optical microscope to determine the position of the electrode. Since wire bonding is accomplished in a closed enclosure, the eyepiece of the optical microscope is inconvenient to observe, and a CCD camera and display are provided to position the electrodes to aid in wire bonding of the electrodes. Finally, working parameters of the ultrasonic pressure welding device are adjusted, and electrodes deposited on the sample and bonding metal columns on the temperature change measuring sample carrier are bonded together by using metal wires. The bond metal posts are partially embedded on the heat conducting insulating plate to ensure insulation between the bond metal posts and the heat sink without large temperature difference.
Step 3: temperature-changing electrotransport property measurement
Firstly, transferring the temperature change measurement sample carrier with the sample obtained in the step 2 to a temperature change electric transportation measurement closed box body. Then, the temperature-variable electrotransport measurement vacuum chamber is opened. And fixing the temperature-changing measurement sample carrier on the cold head, and connecting the measurement cable, the microwave waveguide cable and the antenna. The measuring cable and the microwave waveguide cable are connected with a measuring instrument outside the closed box body through a vacuum aviation connector. Thus, it has been possible to measure electric transport properties such as resistivity, electrical impedance, current-voltage curve, electric transport properties under microwave irradiation, and the like at ordinary temperature (about 300K). Finally, the temperature-varying electrotransport measurement vacuum chamber is closed and evacuated, followed by the refrigerator or heater being turned on. As the temperature of the sample decreases or increases, the electric transport property of the sample under the temperature change condition can be obtained. The cryocooler used in the embodiments of the present invention is a McMahon-Gifford refrigerator (see for specific principles: in Advances in Cryogenic Engineering, page 354.Springer (1960)), equipped with a helium compressor and compressed helium piping, among other components. The cryocooler used in the embodiments of the present invention is a dry-refrigeration refrigerator, i.e., it does not require frequent replenishment of liquid helium. The cryogenic refrigerator used in embodiments of the present invention may reach a minimum temperature of 2.5K.
The embodiment of the invention can obtain the intrinsic electric transport property of the sample under different temperature conditions. All of the above operations are performed in a closed enclosure or vacuum chamber, i.e., the sample is protected from a controlled protective atmosphere throughout. In the actual use process, air can be inevitably leaked into the sealed box body, so that the contents of oxygen and water vapor of protective atmosphere gas are continuously increased. Meanwhile, in the operations of applying low-temperature glue and the like, organic gas molecules may enter the gas environment of the closed box body in the invention. In order to keep the residual oxygen and water vapor content in the protective atmosphere at a low level and remove a small amount of organic gas molecules in the gas, a gas purifying unit is required. The gas purifying unit mainly comprises a gas purifying box body, a fan, an oxygen water purifying column and an organic molecule purifying column. The gas purifying unit is connected with the closed box body through a gas circulating channel to form a closed loop. Under the action of the fan, the protective gas circulates in a closed loop. When the gas circulates to the oxygen water purifying column, residual oxygen and water vapor in the protective atmosphere gas can be adsorbed respectively through the copper catalyst and the molecular sieve in the oxygen water purifying column, so that the oxygen and water vapor content can be ensured to meet the standard of less than 0.1ppm. The oxygen and water vapor contents are read by an oxygen content probe and a water vapor content probe. When the gas is circulated to the organic molecule purification column, it adsorbs organic gas molecules in the protective atmosphere gas through the activated carbon inside.
The operation of the gas purifying unit mainly comprises circulation, gas washing, regeneration of oxygen water purifying column materials, replacement of organic molecule purifying column materials and the like. The cyclic operation is as follows: the blower is turned on, and the two purification columns are turned on, so that the protective atmosphere circulates in the purification system and the closed box. The gas washing operation is as follows: the blower is turned off, and the two purifying columns are turned off, and clean protective atmosphere is used for replacing the polluted protective atmosphere in the closed box body. The regeneration operation of the oxygen water purifying column material is as follows: the blower is turned off, and the oxygen water purifying column is turned off, and the reducing gas such as the mixture of hydrogen and argon is used to reduce the purifying material (copper catalyst, molecular sieve) in which enough oxygen and water vapor are adsorbed. The material of the organic molecule purifying column is replaced, and the active carbon in the organic molecule purifying column is replaced periodically.
Finally, it should be noted that the above embodiments are only for illustrating the technical solution of the present invention and are not limiting. Although the present invention has been described in detail with reference to the embodiments, it should be understood by those skilled in the art that modifications and equivalents may be made thereto without departing from the spirit and scope of the present invention, which is intended to be covered by the appended claims.
Claims (4)
1. A system for measuring a physical property of a material, comprising:
a deposition unit composed of an electrode deposition preparation unit and an electrode deposition unit which are in sealed communication through a vacuum gate valve,
a wire bonding unit is provided to bond the wires,
variable temperature electrotransport measurement unit, and
a gas purifying unit; wherein,,
the deposition unit, the wire bonding unit and the variable-temperature electrotransport measurement unit are communicated through a sample transfer channel; the gas purifying unit is in airtight communication with the deposition unit, the wire bonding unit and the variable temperature electric transportation measuring unit through a gas circulation channel, so that the system forms a gas circulation loop;
the electrode deposition preparation unit comprises an electrode deposition preparation closed box body; a first airtight box observation window and a first rubber glove interface are formed in the electrode deposition preparation airtight box;
the electrode deposition unit comprises an electrode deposition vacuum chamber, a magnetron sputtering target and a sample conveying rod; a deposition sample stage is arranged in the electrode deposition vacuum chamber;
the wire bonding unit comprises a wire bonding closed box body, an ultrasonic pressure welding device, a bonding sample table, a temperature change measurement sample carrier, an optical microscope, a CCD camera and a display, wherein the ultrasonic pressure welding device, the bonding sample table, the temperature change measurement sample carrier, the optical microscope, the CCD camera and the display are arranged in the wire bonding closed box body;
the lead bonding airtight box body is provided with a second airtight box body observation window and a second rubber glove interface;
the variable temperature electric transportation measurement unit comprises a variable temperature electric transportation measurement closed box body, a measurement cable, a microwave waveguide cable, an antenna, a cold head, a variable temperature electric transportation measurement vacuum chamber, a helium compressor, a compressed helium pipeline, a refrigerator, a measurement instrument and a vacuum aviation connector, wherein the measurement cable, the microwave waveguide cable, the antenna, the cold head and the variable temperature electric transportation measurement vacuum chamber are arranged in the variable temperature electric transportation measurement closed box body;
a third closed box observation window and a third rubber glove interface are formed in the variable-temperature electric transport measurement closed box;
the system further comprises a sample entry and exit conduit for the sample to enter and leave the system;
sealing valves are arranged on two sides of the sample inlet and outlet pipeline;
sealing valves are arranged at two ends of the sample transfer channel;
the gas circulation channel is provided with an oxygen content probe, a water vapor content probe and a gas pressure probe;
the gas purification unit comprises a gas purification box body, and a fan, an organic gas purification column and an oxygen water purification column which are arranged in the gas purification box body.
2. The system for measuring a physical property of a material of claim 1, wherein a sample carrier is disposed within the sample transfer channel such that the sample is free to move within the sample transfer channel.
3. The system for measuring a physical property of a material of claim 1, wherein the electrodeposition vacuum chamber is provided with a vacuum chamber viewing window.
4. The system for measuring a physical property of a material of claim 1, wherein the temperature change measurement sample carrier comprises a heat sink, a thermally conductive insulating plate on the heat sink, and a bonded metal post on the thermally conductive insulating plate.
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