CN114487607A - Testing device and testing method for contact resistivity of variable-temperature heterogeneous interface - Google Patents
Testing device and testing method for contact resistivity of variable-temperature heterogeneous interface Download PDFInfo
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Abstract
The invention discloses a device and a method for testing contact resistivity of a variable-temperature heterogeneous interface, wherein the testing device comprises a probe testing platform, a micro probe and a temperature sensor, wherein the probe testing platform is used for controlling the scanning of the micro probe on the surface of a sample to be tested; the method comprises the following steps: the micrometer probe seat is used for clamping a micrometer probe; the temperature-changing clamping rack is used for clamping and heating a sample to be tested; the image acquisition module is used for acquiring surface image information of a sample to be detected; the displacement control unit is used for controlling the movement of the micrometer probe on the surface of the sample to be detected; comprises an X displacement module, a Y displacement module and a Z displacement module; wherein the X displacement module and the Z displacement module are connected with the micrometer probe seat, and the Y displacement module is connected with the variable-temperature clamping rack; and the resistance measuring unit is connected with the variable-temperature clamping rack and the micrometer probe. The invention adopts a three-probe method, a heating temperature control technology and machine vision to accurately correct the probe positioning, and can accurately measure the interface contact resistivity between the electrode material and the thermoelectric material under different temperature field working conditions.
Description
Technical Field
The invention relates to the technical field of electrical performance measurement, in particular to a device and a method for testing contact resistivity of a variable-temperature heterogeneous interface.
Background
The semiconductor device always has interface contact between heterogeneous materials such as semiconductor materials, metal alloy electrodes and the like, and different from physical effects in a semiconductor body, the surface and interface physical effects have great influence on characteristic parameters, stability and reliability of the device. Particularly, the manufacture of the similar ohmic contact is always in the packaging process at the later stage of the device manufacture, and the device failure caused by the interface resistance greatly increases the production cost and the loss, so that the method has great technical significance and economic value for representing the contact resistivity of heterogeneous interfaces such as metal/semiconductors.
For example, the thermoelectric refrigeration technology is a technology capable of realizing directional heat transport and active refrigeration based on the Peltier effect, and has the characteristics of high temperature control precision, full static state, high reliability, easiness in integration and the like because the technology takes electrons in materials as heat carriers. Compared with the traditional passive heat dissipation modes such as air cooling, water cooling, heat pipes and the like, the thermoelectric refrigeration technology has ultrahigh refrigeration density and refrigeration rate, and does not need complex auxiliary mechanisms and external field conditions. Therefore, thermoelectric refrigeration technology becomes one of the most potential optoelectronic chips and other high-power chip hot spot active cooling technologies, and has important significance for the development of the semiconductor chip industry in the future.
The heterogeneous interface of the thermoelectric device is generally a sandwich structure formed by compounding a plurality of layers of thermoelectric materials, barrier layers, transition layers, solders, electrodes and the like, and the thickness of each layer reaches the micron level. The barrier layer is used for blocking interdiffusion and chemical reaction between the thermoelectric material and the electrode layer to form a stable interface layer; the transition layer plays a role of an activation layer, promotes the combination of the thermoelectric material and the electrode, and improves the combination strength; the solder is a welding filler, and the thermoelectric material is firmly connected with the electrode to realize the conduction of current and heat flow. However, due to the limitation of mechanical processing precision, the mutual contact of the heterogeneous interfaces of the thermoelectric devices is often only generatedThe actual contact area is far smaller than the theoretical area generated in a plurality of discrete local areas, so that the electric transmission between the interfaces is influenced, and the interface resistance is formed. The interface resistance severely restricts the refrigeration performance of the thermoelectric device, for example, the maximum temperature difference delta T between two ends of the device can be reduced in a steady-state operation mode of the thermoelectric devicesteady,maxRefrigerating capacity QCAnd coefficient of refrigeration efficiency COP; in the transient operation mode, the supercooling temperature difference Delta T can be reducedtransient,maxAnd aggravate temperature overshoot Δ Tovershoot. Therefore, the heterogeneous interface contact resistance of the thermoelectric device must be represented, the result is used as a reference basis for interface resistance regulation, the manufacturing process of the thermoelectric device is optimized, a simulation theoretical model is perfected, an interface resistance optimization standard is established, and low-resistance high-reliability heterogeneous interface connection of thermoelectric particles and electrodes is realized.
At present, experimental measurement data of the interface resistivity of a heterogeneous interface of a semiconductor device is single, and the experimental measurement data is a fixed measurement value at room temperature generally. However, the interface resistivity changes along with the change of the temperature under the actual working condition, the refrigeration performance of the thermoelectric device is greatly influenced by the small change, the representation of the interface resistivity by the fixed measurement value at room temperature is insufficient, and the optimal regulation and control method of the interface resistance cannot be established more comprehensively and accurately. Meanwhile, the thickness of the heterogeneous interface of the thermoelectric device reaches the micron level, a motor is driven by a conventional control means to drive a probe to carry out precise stepping scanning, but because the probe arm and the probe swing, the actually realized probe positioning precision is low, the scanning path interval is too large or inaccurate, and the interface resistivity error extracted from the relation curve diagram of the scanning path and the resistance value is large. For example, chinese patent CN 108508273 a discloses a device and method for directly measuring interface contact resistivity, which is characterized in that a sample to be measured is mounted on a sample test fixture to provide fixed current for two ends of the sample, a conventional control means is adopted to drive a motor to drive a probe to perform precise step scanning and obtain voltage, and finally a relation curve graph between a scanning path and a resistance value at room temperature is obtained through conversion. However, the method can only obtain the fixed interface resistivity at room temperature, and cannot directly measure and obtain the interface resistivity corresponding to different temperatures under actual working conditions. Because the interface resistivity can change along with the change of the temperature under the actual working condition, the refrigeration performance of the thermoelectric device can be greatly influenced by small changes, the representation of the interface resistivity by a fixed measurement value at room temperature is insufficient, and the optimal regulation and control method of the interface resistance can not be established more comprehensively and accurately. Meanwhile, the thickness of the heterogeneous interface of the thermoelectric device reaches the micron level, and due to the fact that the probe arm and the probe swing, the actually-realized probe positioning precision is low, the scanning path interval is too large or inaccurate, and the interface resistivity error extracted from the relation curve graph of the scanning path and the resistance value is large. Therefore, a testing device and a method for accurately measuring the interface contact resistivity between the electrode material and the thermoelectric material under different temperature field working conditions are still needed.
Disclosure of Invention
Aiming at the defects of the heterogeneous interface contact resistivity testing technology of the thermoelectric device, the invention provides a temperature-variable heterogeneous interface contact resistivity testing device and a testing method, a three-probe method and a heating temperature control technology are adopted to simulate the actual temperature field working condition of the thermoelectric device, the contact resistivity of heterogeneous interfaces such as metal/semiconductor under different temperature field working conditions is accurately measured, and the device has reference significance for optimizing the manufacturing process of the thermoelectric device and perfecting a simulation theoretical model; the method has potential application value for the representation of the interface electrical properties of electronic components such as thermoelectric devices, semiconductor packaging and interconnection and the like.
In order to achieve the purpose, the invention adopts the technical scheme that:
in one aspect, the present invention provides a device for testing contact resistivity of a temperature-variable heterogeneous interface, including:
the probe test platform is used for controlling the scanning of the micrometer probe on the surface of the sample to be tested; the method comprises the following steps: the micrometer probe seat is used for clamping the micrometer probe; the temperature-changing clamping rack is used for clamping and heating a sample to be tested; the image acquisition module is used for acquiring surface image information of the sample to be detected;
the displacement control unit is used for controlling the movement of the micrometer probe on the surface of the sample to be detected; comprises an X displacement module, a Y displacement module and a Z displacement module; the X displacement module and the Z displacement module are connected with the micrometer probe seat, and the Y displacement module is connected with the variable-temperature clamping rack;
and the resistance measuring unit is connected with the variable-temperature clamping rack and the micrometer probe.
Preferably, the temperature-changing clamping rack comprises a first power supply interface, a second power supply interface, a heater for clamping and heating a sample to be detected, and a temperature-measuring thermocouple; the temperature thermocouple is arranged at one end of the heater, which is contacted with the sample to be detected; the first power supply interface is electrically connected with the resistance testing unit and the sample to be tested to form a closed loop; the sample to be tested is arranged between the first power interface and the second power interface.
Preferably, the temperature-changing clamping rack further comprises a base, a bracket for fixing the heater and a hand-operated clamping mechanism for adjusting the clamping tightness of the sample to be measured; the bracket comprises a fixed bracket and a sliding bracket; the hand-operated clamping mechanism is arranged on the base and connected with the sliding support.
Preferably, the hand-operated clamping mechanism comprises a hand-operated wheel and a sliding block; the sliding block is arranged on the base and is fixedly connected with the sliding support; the hand-operated wheel is in transmission connection with the sliding block.
Preferably, the heater is selected from any one of alumina ceramic, aluminum nitride ceramic and silicon nitride ceramic with a built-in heating wire; a copper heat transfer block is wrapped outside the heater, and the sample to be tested forms a closed loop with the first power interface and the second power interface through the copper heat transfer block; the temperature thermocouple is arranged at one end of the copper heat transfer block, which is contacted with the sample to be detected;
preferably, the micrometer probe seat is made of low-thermal-conductivity insulating heat-resistant materials, such as zirconia ceramics, glass fiber composites, polytetrafluoroethylene and the like;
preferably, the microprobe is made of tungsten.
Preferably, the temperature control system further comprises a PID controller, wherein the PID controller realizes accurate temperature control of the heater according to the temperature information collected by the temperature thermocouple; the temperature control range of the heater is between room temperature and 800 ℃, and the temperature control precision is preferably within +/-1 ℃.
Preferably, the image acquisition module comprises an optical imaging system for acquiring surface image information of the sample to be detected; the light source of the optical imaging system is directed to the sample to be measured, and in some embodiments, the optical imaging system is an industrial camera;
preferably, the image acquisition module further comprises an XYZ imaging fine adjustment module for fine adjustment focusing of the optical imaging system.
Preferably, the resistance measuring unit comprises a voltage-stabilizing and current-stabilizing power supply and a data acquisition module; the voltage-stabilizing and current-stabilizing power supply is electrically connected with the first power interface and supplies power to a sample to be detected; and the data acquisition module is connected with the second power interface and the micrometer probe and is used for measuring the contact voltage of the sample to be measured and the micrometer probe.
Preferably, the device further comprises a computer unit, which is used for reading the surface image information of the sample to be measured, which is acquired by the image acquisition module, reading the information of the data acquisition module, setting the movement parameters of the displacement control unit, and controlling the focusing of the XYZ imaging fine adjustment module; the optical imaging system collects surface image information of a sample to be measured, inputs the surface image information into a computer and positions the micrometer probe as closed loop correction information of the displacement control unit;
in the technical scheme of the invention, the movement of the displacement control unit is controlled by the computer unit, and the precision of the displacement control unit can reach below 1 mu m.
Preferably, the pixels of the industrial camera are not less than 2000 ten thousand pixels, and in the technical scheme of the invention, after the displacement control unit is subjected to closed-loop correction by using the industrial camera with more than 2000 ten thousand pixels, the positioning accuracy of the micrometer probe can reach below 0.5 μm.
Preferably, the testing process of the testing device is completed under a vacuum condition; in some specific embodiments, the testing device further comprises a vacuum cover body, and during testing, the vacuum cover body is vacuumized by using a vacuum pump, and the vacuum degree of the vacuum is less than or equal to 10 Pa.
In another aspect, the invention provides a testing method using the temperature-variable hetero-interface contact resistivity testing apparatus, comprising the following steps:
(1) installing a sample to be detected in a variable-temperature clamping rack, and heating the sample to be detected;
(2) collecting a surface image of the sample to be detected, setting a scanning path and a scanning step length, and generating a micrometer probe target position;
(3) scanning measurement, wherein the micrometer probe performs resistance measurement once every step, a relation curve graph of a scanning path and a voltage value is drawn, and the contact resistance R of the heterogeneous interface at the heating temperature is obtained through calculationcAccording to the geometric parameters of the sample to be measured and the contact resistance RcAnd calculating to obtain the contact resistivity rho of the heterogeneous interface at the heating temperaturec。
Further, the testing method of the contact resistivity testing device of the variable temperature heterogeneous interface specifically comprises the following steps:
clamping a sample to be detected in a variable-temperature clamping rack, and shaking a hand-operated wheel to clamp the sample to be detected;
connecting a first power supply interface with a voltage and current stabilizing power supply to provide a fixed current for the sample to be detected;
setting heating temperature for a heater, collecting the temperature of the heater by a temperature thermocouple and feeding the temperature back to a PID controller, and controlling the accurate temperature control of the heater by the PID controller;
fourthly, connecting the data acquisition module with the micrometer probe and a second power interface, and setting the scanning interval of the micrometer probe on the surface of the sample to be detected through a computer unit;
scanning measurement, wherein along with the movement of the micrometer probe, the optical imaging system collects surface image information of the sample to be measured and inputs the surface image information into a computer, the surface image information is used as closed-loop correction information of a displacement control unit to position the micrometer probe, and a relation curve graph of a scanning path and a voltage value is generated in the computer according to corresponding voltage of each scanning measurement;
step (ii)Calculating to obtain the contact resistance R of the heterogeneous interface at the temperature according to the relation curve chart of the scanning path and the voltage value and the fixed current value of the sample to be measuredc；
Seventhly, adjusting the heating temperature of the heater, and repeating the step III to obtain the contact resistance of the heterogeneous interface under different temperature field working conditions; and calculating the contact resistivity of the variable temperature heterogeneous interface by combining the sectional area size S of the sample to be detected.
In the technical scheme of the invention, the calculation formula for calculating the contact resistivity of the temperature-changing interface is rhoc＝Rc×S。
The technical scheme has the following advantages or beneficial effects:
aiming at the defects of the thermoelectric device heterogeneous interface contact resistivity testing technology in the prior art, the invention provides a testing device and a testing method for the temperature-variable heterogeneous interface contact resistivity.
The method adopts a three-probe method and a heating temperature control technology, can simulate the actual temperature field working condition of the thermoelectric device, measures and obtains the corresponding contact resistivity, and has great reference value for optimizing the manufacturing process of the thermoelectric device and perfecting a simulation theoretical model; by adopting the technology of matching machine vision with the positioning probe, the industrial camera can shoot images and identify the position of the probe to be used as high-precision closed-loop correction information of the positioning probe, the positioning precision of the probe can reach below 0.5 mu m, and the testing precision of the contact resistivity is greatly improved.
Drawings
Fig. 1 is a schematic structural diagram of a temperature-variable hetero-interface contact resistivity testing apparatus provided in embodiment 1 of the present invention.
Fig. 2 is a schematic structural diagram of a temperature-variable clamping rack of the temperature-variable hetero-interface contact resistivity testing apparatus according to embodiment 1 of the present invention.
Fig. 3 is an enlarged view of a part (a) of a temperature-variable holding stage of the temperature-variable hetero-interface contact resistivity test apparatus according to embodiment 1 of the present invention.
Fig. 4 is a graph showing the relationship between the scan path and the resistance in embodiment 2 of the present invention.
FIG. 5 is a graph showing the relationship between the scan path and the resistance in embodiment 3 of the present invention.
Detailed Description
In the following, the technical solutions in the embodiments of the present invention are clearly and completely described with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. Thus, the following detailed description of the embodiments of the present invention, presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments of the invention without making creative efforts, belong to the protection scope of the invention.
In the description of the present invention, it should be noted that, as the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc. appear, their indicated orientations or positional relationships are based on those shown in the drawings, and are only for convenience of description and simplicity of description, but do not indicate or imply that the referred device or element must have a specific orientation, be constructed in a specific orientation, and be operated, and thus, should not be construed as limiting the present invention.
In the description of the present invention, it should be noted that, unless otherwise explicitly stated or limited, the terms "mounted," "connected," and "connected" should be interpreted broadly, e.g., as being fixed or detachable or integrally connected; they may be mechanically coupled, directly coupled, indirectly coupled through intervening media, or may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
Example 1:
aiming at the defects of the contact resistivity testing technology of the heterogeneous interface of the thermoelectric device in the prior art, the invention provides a contact resistivity testing device of a variable-temperature heterogeneous interface, which is shown in the figures 1-3: the method comprises the following steps:
the probe test platform is used for controlling the scanning of the micrometer probe 51 on the surface of a sample 53 to be tested; the method comprises the following steps: a micrometer probe seat 4 for holding a micrometer probe 51; a variable temperature holding stage 5 for holding and heating a sample 53 to be measured; the image acquisition module 6 is used for acquiring surface image information of the sample 53 to be detected;
the displacement control unit is used for controlling the movement of the micrometer probe 51 on the surface of the sample 53 to be measured; comprises an X displacement module 2, a Y displacement module 3 and a Z displacement module 1; wherein the X displacement module 2 and the Z displacement module 1 are connected with the micrometer probe seat 4, and the Y displacement module 3 is connected with the variable temperature clamping rack 5;
and the resistance measuring unit is connected with the temperature-changing clamping rack 5 and the micrometer probe 51.
In the using process of the device provided by the invention, a sample 53 to be detected is arranged in the temperature-changing clamping rack 5, and the X displacement module 2 and the Y displacement module 3 realize the movement of the micrometer probe 51 on the horizontal plane by controlling the movement of the micrometer probe seat 4; the Y displacement module 3 adjusts the height of the sample 53 to be measured by controlling the temperature-variable holding stage 5.
Further, the temperature-changing clamping rack 5 comprises a first power interface 52-1, a second power interface 52-2, a heater 54 for clamping and heating the sample 53 to be measured, and a temperature thermocouple 55; the temperature thermocouple 55 is arranged at one end of the heater 54 contacting the sample 53 to be measured; the first power interface 52-1 is electrically connected with the resistance testing unit and the sample 53 to be tested to form a closed loop; the sample 53 to be tested is disposed between the first power interface 52-1 and the second power interface 52-2.
In the device provided by the invention, the heater 54 is used for heating the sample 53 to be measured so as to measure the contact resistivity at different temperatures, and the temperature of the sample 53 to be measured can be monitored by arranging the temperature thermocouple 54.
Further, the temperature-changing clamping rack 5 further comprises a base 59, a bracket 56 for fixing the heater 54 and a hand-operated clamping mechanism for adjusting the clamping tightness of the sample 53 to be measured; the bracket 56 includes a fixed bracket 56-1 and a sliding bracket 56-2; the hand-operated clamping mechanism is disposed on the base 59 and is connected to the sliding bracket 56-2.
In the device provided by the invention, in the use process, the distance between the sliding support 56-1 and the sliding support 56-2 can be adjusted through the hand-operated clamping mechanism, so that samples with different specifications can be measured on one hand, and the clamping tightness of the sample 53 to be measured can be adjusted on the other hand.
Preferably, the hand-operated clamping mechanism comprises a hand-operated wheel 57 and a slider 58; the sliding block 58 is arranged on the base 59 and is fixedly connected with the sliding bracket 56-2; the hand-operated wheel 57 is in transmission connection with the slide block 58.
According to the device provided by the invention, the hand-operated wheel 57 is matched with the sliding block 58, and in the using process, the sliding block 58 moves towards or away from the fixed support 56-1 by shaking the hand-operated wheel 57, so that the distance between the sliding support 56-2 and the fixed heater and the fixed support 56-1 and the fixed heater is shortened or increased, and the measurement of samples with different specifications and the clamping degree of the sample to be measured 53 are adjusted.
Further, the heater 54 is selected from any one of alumina ceramics, aluminum nitride ceramics, and silicon nitride ceramics with a built-in heater wire; a copper heat transfer block is wrapped outside the heater 54, and the sample 53 to be tested forms a closed loop with the first power interface 52-1 and the second power interface 52-2 through the copper heat transfer block; the temperature thermocouple 55 is arranged at one end of the copper heat transfer block contacting the sample 53 to be measured;
further, the micrometer probe holder 4 is made of a heat-resistant insulating material with low thermal conductivity, such as zirconia ceramics, glass fiber composites, polytetrafluoroethylene, and the like;
further, the microprobe 51 is made of tungsten.
According to the testing device provided by the invention, the sample 53 to be tested is heated through the alumina ceramic, the aluminum nitride ceramic or the silicon nitride ceramic with the built-in heating wires, the outer surface of the heater 54 is wrapped by the copper heat transfer block, so that the sample 53 to be tested, the first power interface 52-1 and the second power interface 52-2 form a closed loop, and the heater 54 is powered by an external power supply.
Further, the temperature control device also comprises a PID controller, wherein the PID controller realizes accurate temperature control of the heater 54 according to temperature information collected by the temperature thermocouple 55; the temperature control range of the heater 54 is between room temperature and 800 ℃, and the temperature control precision is preferably within +/-1 ℃.
In the testing device provided by the invention, the temperature information acquired by the temperature thermocouple 55 is fed back to the PID controller, and the temperature control of the heater 54 is realized through the PID controller.
Further, the image collecting module 6 includes an optical imaging system for collecting surface image information of the sample 53 to be measured; the light source of the optical imaging system is directed towards the sample 53 to be measured.
Further, an XYZ imaging fine adjustment module 7 for fine adjustment focusing of the optical imaging system is also included.
The testing device provided by the invention realizes fine tuning focusing of the optical imaging system through the XYZ imaging fine tuning module 7, collects the surface image of the sample 53 to be tested, processes the image, and effectively realizes machine vision positioning.
Furthermore, the resistance measuring unit comprises a voltage-stabilizing and current-stabilizing power supply and a data acquisition module; the voltage-stabilizing current-stabilizing power supply is electrically connected with the first power interface 52-1 and supplies power to the sample 53 to be detected; the data acquisition module is connected with the second power interface 52-2 and the micrometer probe 51 and is used for measuring the contact voltage of the sample 53 to be measured and the micrometer probe 51.
Further, the device also comprises a computer unit, which is used for reading the surface image information of the sample 53 to be detected, which is acquired by the image acquisition module 6, reading the information of the data acquisition module, setting the movement parameters of the displacement control unit, and controlling the focusing of the XYZ imaging fine adjustment module 7; the optical imaging system collects the surface image information of the sample 53 to be measured and inputs the information into the computer, and the micrometer probe 51 is positioned as the closed loop correction information of the displacement control unit.
The testing device provided by the embodiment, the X displacement module 2, the Y displacement module 3 and the Z displacement module 1 comprise a stepping motor and a sliding table in transmission connection with the stepping motor, and the computer unit can control the displacement of the sliding table by regulating and controlling the parameters of the stepping motor, wherein the control precision is preferably less than 1 μm. In the embodiment, an industrial camera with auto-focusing and more than 2000 ten thousand pixels is used as an optical imaging system, the surface image of the sample 53 to be detected is collected and input into a computer, the probe position information fed back by the displacement control unit is corrected in a closed loop mode, and finally the positioning accuracy of the probe can reach below 0.5 μm.
Furthermore, the testing device provided by the invention also comprises a vacuum cover body 8, and during testing, the vacuum pump is adopted to vacuumize the cover body, and the vacuum degree of the vacuum is less than or equal to 10 Pa.
The testing method applying the temperature-variable heterogeneous interface contact resistivity testing device comprises the following steps of:
firstly, clamping a sample 53 to be detected in a temperature-changing clamping rack 5, and shaking a hand-operated wheel 57 to clamp the sample 53 to be detected;
secondly, connecting the first power interface 52-1 with a voltage-stabilizing and current-stabilizing power supply to provide a fixed current for the sample 53 to be tested;
setting heating temperature for the heater 54, collecting the temperature of the heater 54 by the temperature thermocouple 55 and feeding the temperature back to the PID controller, and controlling the accurate temperature control of the heater 54 by the PID controller;
fourthly, connecting the data acquisition module with the micrometer probe 51 and the second power interface 52-2, and setting the scanning interval of the micrometer probe 51 on the surface of the sample 53 to be detected through a computer unit;
scanning measurement, wherein along with the movement of the micrometer probe 51, the optical imaging system collects surface image information of a sample 53 to be measured and inputs the surface image information into a computer, the surface image information is used as closed-loop correction information of a displacement control unit to position the micrometer probe 51, and a relation curve graph of a scanning path and a voltage value is generated in the computer according to the corresponding voltage of each scanning measurement;
step sixthly, calculating and obtaining the contact resistance R of the heterogeneous interface at the temperature according to the relation curve chart of the scanning path and the voltage value and the fixed current value of the sample 53 to be measuredc；
Seventhly, adjusting the heating temperature of the heater 54, and repeating the step III to obtain the contact resistance of the heterogeneous interface under different temperature field working conditions; and calculating the contact resistivity of the temperature-changing heterogeneous interface by combining the sectional area size S of the sample 53 to be measured.
Further, the calculation formula for calculating the contact resistivity of the temperature-changing interface is rhoc＝Rc×S。
Example 2:
in this embodiment, the testing apparatus and method in embodiment 1 are used to test the contact resistivity of the interface between the bismuth telluride material and Co in a sample of bismuth telluride/Co/bismuth telluride sandwich structure, the sample has a size of 3mm in height, 3mm in width and 4mm in length, the testing temperature is 27 ℃ at room temperature, the testing current is 100mA dc, and the sample is in a vacuum environment; the test results are shown in FIG. 4, where the interfacial contact resistance value was 0.12 m.OMEGA., and the interfacial contact resistivity was calculated to be 10.8. mu. OMEGA.cm2。
Example 3:
this example used the test apparatus and method of example 1 to test the contact resistivity of a skutterudite material/Mo interface sample, which was Yb0.3Co4Sb12/Mo/Yb0.3Co4Sb12A sandwich structure with a dimension of 2.52mm in height, 2.77mm in width, 4mm in length, a test temperature of 477 ℃, a test current of 100mA direct current and a vacuum environment; the test results are shown in FIG. 5, where the interface contact resistance value is 0.06 m.OMEGA.and the interface contact resistance value is calculated to be 4.2. mu. OMEGA.cm2。
The above description is only for the preferred embodiment of the present invention and is not intended to limit the scope of the present invention, and all equivalent structural changes made by using the contents of the present specification and the drawings, or any other related technical fields, are included in the scope of the present invention.
Claims (10)
1. A temperature-changing heterogeneous interface contact resistivity testing device is characterized by comprising:
the probe test platform is used for controlling the scanning of the micrometer probe on the surface of the sample to be tested; the method comprises the following steps: the micrometer probe seat is used for clamping the micrometer probe; the temperature-changing clamping rack is used for clamping and heating a sample to be tested; the image acquisition module is used for acquiring surface image information of the sample to be detected;
the displacement control unit is used for controlling the movement of the micrometer probe on the surface of the sample to be detected; comprises an X displacement module, a Y displacement module and a Z displacement module; the X displacement module and the Z displacement module are connected with the micrometer probe seat, and the Y displacement module is connected with the variable-temperature clamping rack;
and the resistance measuring unit is connected with the variable-temperature clamping rack and the micrometer probe.
2. The testing device of claim 1, wherein the temperature-changing holding rack comprises a first power interface, a second power interface, a heater for holding and heating a sample to be tested, and a temperature thermocouple; the temperature thermocouple is arranged at one end of the heater, which is contacted with the sample to be detected; the first power supply interface is electrically connected with the resistance testing unit and the sample to be tested to form a closed loop; the sample to be tested is arranged between the first power interface and the second power interface.
3. The testing device of claim 2, wherein the temperature-changing clamping rack further comprises a base, a bracket for fixing the heater and a hand-operated clamping mechanism for adjusting the clamping tightness of the sample to be tested; the bracket comprises a fixed bracket and a sliding bracket; the hand-operated clamping mechanism is arranged on the base and is connected with the sliding support.
4. The testing device of claim 3, wherein the hand-operated clamping mechanism comprises a hand-operated wheel and a slider; the sliding block is arranged on the base and is fixedly connected with the sliding support; the hand-operated wheel is in transmission connection with the sliding block.
5. The test apparatus according to claim 2, wherein the heater is selected from any one of alumina ceramic, aluminum nitride ceramic, and silicon nitride ceramic with a built-in heating wire; a copper heat transfer block is wrapped outside the heater, and the sample to be tested forms a closed loop with the first power interface and the second power interface through the copper heat transfer block; the temperature thermocouple is arranged at one end of the copper heat transfer block, which is contacted with the sample to be detected;
preferably, the micrometer probe seat is made of a low-thermal-conductivity heat-resistant insulating material;
preferably, the microprobe is made of tungsten.
6. The testing device of claim 2, further comprising a PID controller, wherein the PID controller realizes accurate temperature control of the heater according to the temperature information collected by the temperature thermocouple; the temperature control range of the heater is between room temperature and 800 ℃, and the temperature control precision is preferably within +/-1 ℃.
7. The testing device of claim 2, wherein the image acquisition module comprises an optical imaging system for acquiring surface image information of the sample to be tested; a light source of the optical imaging system irradiates the sample to be detected;
preferably, the image acquisition module further comprises an XYZ imaging fine adjustment module for fine adjustment focusing of the optical imaging system.
8. The testing device of claim 7, wherein the resistance measuring unit comprises a voltage-stabilizing and current-stabilizing power supply and a data acquisition module; the voltage-stabilizing and current-stabilizing power supply is electrically connected with the first power supply interface; and the data acquisition module is connected with the second power interface and the micrometer probe and is used for measuring the contact voltage of the sample to be measured and the micrometer probe.
9. The testing device of claim 8, further comprising a computer unit for reading the surface image information of the sample to be tested collected by the image collection module, reading the information of the data collection module, setting the movement parameters of the displacement control unit, and controlling the focusing of the XYZ imaging fine adjustment module; the optical imaging system collects surface image information of a sample to be measured, inputs the surface image information into a computer and positions the micrometer probe as closed loop correction information of the displacement control unit;
preferably, the movement accuracy of the displacement control unit is 1 μm or less;
preferably, the micrometer probe has a positioning accuracy of 0.5 μm or less.
10. The testing method of the temperature-changing hetero-interface contact resistivity testing device according to any one of claims 1 to 9, characterized by comprising the steps of:
(1) installing a sample to be detected in a variable-temperature clamping rack, and heating the sample to be detected;
(2) collecting a surface image of the sample to be detected, setting a scanning path and a scanning step length, and generating a micrometer probe target position;
(3) scanning measurement, wherein the micrometer probe performs resistance measurement once every step, a relation curve graph of a scanning path and a voltage value is drawn, and the contact resistance R of the heterogeneous interface at the heating temperature is obtained through calculationcAccording to the geometric parameters of the sample to be measured, and the contact resistance RcAnd calculating to obtain the contact resistivity rho of the heterogeneous interface at the heating temperaturec。
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| WO2023143638A1 (en) * | 2022-01-29 | 2023-08-03 | 深圳先进电子材料国际创新研究院 | Test apparatus and test method for contact resistivity of temperature-variable heterogeneous interface |
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| JP3468300B2 (en) * | 2000-08-18 | 2003-11-17 | インターナショナル・ビジネス・マシーンズ・コーポレーション | Method and apparatus for measuring thermal and electrical properties of thin film thermoelectric materials |
| JP4595073B2 (en) * | 2006-08-28 | 2010-12-08 | 独立行政法人産業技術総合研究所 | Thermoelectric material measuring device |
| CN201716370U (en) * | 2010-03-09 | 2011-01-19 | 北京交通大学 | Vacuum temperature-change thin-film resistance tester |
| CN102539927A (en) * | 2011-12-14 | 2012-07-04 | 东华大学 | Method for measuring temperature-controllable four-probe square resistance and resistivity |
| CN104635058B (en) * | 2015-02-12 | 2017-12-22 | 武汉嘉仪通科技有限公司 | The method of testing and system of automatic measurement semiconductor resistor rate and Seebeck coefficient |
| CN207623414U (en) * | 2017-12-20 | 2018-07-17 | 中国科学院深圳先进技术研究院 | A kind of four-point probe of accurate inserting needle |
| CN108508273B (en) * | 2018-05-15 | 2020-12-11 | 中国科学院上海硅酸盐研究所 | Device and method for directly measuring interface contact resistivity |
| CN111948250B (en) * | 2020-08-13 | 2023-01-13 | 上海大学 | Variable temperature measuring device for high-flux thermoelectric material |
| CN113466557A (en) * | 2021-05-19 | 2021-10-01 | 包头稀土研究院 | Neodymium iron boron resistivity measuring system and measuring method thereof |
| CN113820543A (en) * | 2021-10-29 | 2021-12-21 | 南京工程学院 | Thin film material resistivity and Hall effect measuring device and method |
| CN114487607A (en) * | 2022-01-29 | 2022-05-13 | 深圳先进电子材料国际创新研究院 | Testing device and testing method for contact resistivity of variable-temperature heterogeneous interface |
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