CN114354678B - Device, method and system for testing performance parameters of thin film thermoelectric material - Google Patents
Device, method and system for testing performance parameters of thin film thermoelectric material Download PDFInfo
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Abstract
The invention relates to a device, a method and a system for testing performance parameters of a thin film thermoelectric material, which are used for solving the problems that the traditional method for testing the performance parameters of the thin film thermoelectric material is complex in operation, low in testing speed, low in testing accuracy and difficult to meet the requirements of rapid and simple testing of a large number of performance parameters of the thin film thermoelectric material. The testing device of the invention comprises: a basic temperature control unit and a temperature difference control unit which are arranged from bottom to top; the basic temperature control unit is used for controlling the basic temperature of the sample to be tested; the temperature difference control unit is used for controlling the temperature difference of two ends of the sample to be detected; the temperature difference control unit comprises a sample bearing part to be detected, and the sample bearing part to be detected is used for bearing a sample to be detected. The technical scheme provided by the invention can simply, conveniently, rapidly and accurately test the thermoelectric performance parameters of the thin film thermoelectric material and can automatically process the thermoelectric performance parameters of the thin film thermoelectric material.
Description
Technical Field
The invention belongs to the technical field of thermoelectric testing, and particularly relates to a device, a method and a system for testing performance parameters of a thin film thermoelectric material.
Background
The thermoelectric material is a special functional material capable of realizing the direct conversion between heat energy and electric energy, and provides a simple and effective utilization mode for waste heat and natural heat. As an energy conversion material, the thermoelectric material has the advantages of compact structure, small volume, no moving parts, no noise, no excrement (no pollution), high reliability and the like, and is widely researched and applied in the aspects of solar energy, geothermal energy, industrial waste heat and waste heat utilization, organism micro-temperature difference power generation, self-powered sensor and the like. In the prior art, the device for testing the performance parameters of the thermoelectric material is mainly designed for the inorganic thermoelectric material, most of samples to be tested are hard blocks or thick plates, the samples can be directly tested without a supporting substrate, and the inorganic thermoelectric material cannot be damaged due to the hard contact between the test part and the materials to be tested. Most of organic thermoelectric materials are thin films or soft structures with the thickness of nanometer to micrometer, and special testing equipment is still fresh at present. The inorganic thermoelectric test equipment for the traditional block or thick sheet test is difficult to directly apply to the performance parameter test of the thin film thermoelectric material with the thickness of nanometer to micrometer which cannot be self-supported.
In terms of thermoelectric material performance parameter testing, accurate characterization of seebeck coefficient and conductivity is one of the most important. The seebeck coefficient S of a material can be expressed as: s=Δv/Δt, where Δt is a temperature difference across the material, and Δv is a seebeck voltage generated across the material at the temperature difference. When the Seebeck coefficient of a material is tested, a temperature difference needs to be created at two ends of a sample, and the voltage generated at the two ends of the sample under the temperature difference is measured to be Seebeck voltage. The traditional testing method generally adopts a temperature thermocouple and a voltage probe to simultaneously measure the temperature difference and the Seebeck voltage at two ends of a sample, has complex operation and low testing precision, and is difficult to be directly applied to Seebeck coefficient testing of a thin film thermoelectric material supported by a substrate.
The conductivity sigma of the material can be calculated by testing its resistance R and the dimensional information of the sample. In the conductivity test, a current I is applied to a sample of a specific size (length L, width W, thickness H), the voltage of which is measured as V, the resistance r=v/I, the conductivity σ=il/(VWH).
The power factor PF of a material is one of the important evaluation parameters of thermoelectric performance, and is determined by the seebeck coefficient and the conductivity together: pf=s 2 Sigma. To obtain accurate power factors, it is often required to test the seebeck coefficient and conductivity sequentially on the same test system and on the same sample.
The thin film thermoelectric material represented by the organic material has the characteristics of good flexibility, low intrinsic heat conductivity, excellent performance in a room temperature region and the like, has advantages in low-temperature micro-temperature difference power generation and the like, is hopeful to be complementary with the traditional inorganic thermoelectric material, and becomes one of important energy devices of a new generation of flexible electronic devices. In recent years, research on thin film thermoelectric materials has undergone rapid development, however, testing of main parameters of thin film thermoelectric materials is currently lacking in efficient and rapid equipment. In view of this, designing a testing device suitable for testing thin film thermoelectric materials is a current urgent need.
Disclosure of Invention
Based on the above analysis, the present invention aims to provide a device, a method and a system for testing performance parameters of a thin film thermoelectric material, so as to solve one of the following technical problems: the traditional thermoelectric performance parameter testing method is complex to operate; (2) The traditional thermoelectric performance parameter testing method has low testing speed and low testing accuracy; (3) The traditional thermoelectric performance parameter testing method is difficult to meet the actual requirements of rapid and simple testing of a large number of thermoelectric material performance parameters of thin films. The device, the method and the system for testing the performance parameters of the thin film thermoelectric material have the characteristics of simplicity, convenience, rapidness and accuracy.
The aim of the invention is mainly realized by the following technical scheme:
in a first aspect, an embodiment of the present invention provides a device for testing performance parameters of a thin film thermoelectric material, including: a basic temperature control unit and a temperature difference control unit which are arranged from bottom to top;
the basic temperature control unit is used for controlling the basic temperature of the sample to be tested;
the temperature difference control unit is used for controlling the temperature difference of two ends of the sample to be detected;
the temperature difference control unit comprises a sample bearing part to be detected, and the sample bearing part to be detected is used for bearing the sample to be detected.
Further, the apparatus further comprises: a buffer layer;
the buffer layer is disposed between the temperature difference control unit and the base temperature control unit.
Further, the base temperature control unit includes: an electric heating block and a liquid nitrogen pipeline;
the electric heating block is used for heating the sample to be tested;
the liquid nitrogen pipeline is used for providing a basic test temperature ranging from room temperature to liquid nitrogen temperature or rapidly cooling and heating a sample to be tested;
the liquid nitrogen pipeline is arranged below the electric heating block.
Further, the electric heating block is provided with a detection hole, and the detection hole is used for installing an electric heating source and a temperature measuring element.
Further, the temperature difference control unit further includes: a heating section;
the heating part is used for controlling the temperature difference between two ends of the sample to be measured.
Further, the heating part includes: a first heating block and a second heating block;
a gap is formed between the first heating block and the second heating block, one end of a sample to be measured is arranged above the first heating block, and the other end of the sample to be measured is arranged above the second heating block.
Further, the sample carrier to be tested includes: a first sample cell and a second sample cell arranged in parallel;
the two ends of the first sample groove are respectively arranged on the first heating block and the second heating block; two ends of the second sample groove are respectively arranged on the first heating block and the second heating block;
the first sample groove is used for bearing a sample to be detected and a substrate, and the second sample groove is used for bearing a blank substrate.
Further, a separation groove is formed in one side, close to the temperature difference control unit, of the buffer layer, and two ends of the sample to be tested are located on two sides of the separation groove.
In a second aspect, an embodiment of the present invention provides a method for testing performance parameters of a thin film thermoelectric material, based on the device in the first aspect, including:
Placing a substrate containing a sample to be tested in a first sample groove, and arranging a blank substrate in a second sample groove;
raising the temperature of the first sample tank and the second sample tank to a set temperature by using a base temperature control unit;
collecting resistance test data corresponding to the first sample groove and first calibration data corresponding to the second sample groove at the set temperature;
according to the set temperature, adjusting the temperature difference of the first sample tank and the second sample tank to a set temperature difference by using a temperature difference control unit;
and acquiring Seebeck voltage corresponding to the first sample tank and second calibration data corresponding to the second sample tank under the set temperature difference.
In a third aspect, an embodiment of the present invention provides a system for testing performance parameters of a thin film thermoelectric material, which is characterized by comprising: a computer device, a control unit and the thermoelectric material performance parameter testing apparatus of any of the first aspects.
The invention can realize one of the following beneficial effects:
1. the basic temperature control unit provides basic temperature and experimental conditions for obtaining the corresponding relation between the temperature and the conductivity. The temperature difference control unit is based on the basic temperature provided by the basic temperature control unit, provides stable temperature difference for the sample to be tested, and provides experimental conditions for obtaining the corresponding relation between the temperature difference and the Seebeck voltage. Therefore, the corresponding relation between the temperature and the conductivity can be completed in one system at the same time, so that the testing process is simplified, and the testing speed is improved. Because the temperature difference is based on the basic temperature and is completed in the same device, the system errors among different systems can be eliminated, and the test accuracy is improved.
2. The thin film thermoelectric material is characterized in that the thin film thermoelectric material is easy to deform when being subjected to external force, so that compared with a bulk material, most of the thin film thermoelectric material can be damaged or uneven in heat distribution due to deformation when being wound by a heating wire or under other test conditions requiring external force, and finally the precision of an experimental result is influenced, or no valuable data is obtained. The temperature difference control unit only controls the temperature difference of two ends of the sample to be tested, so that the thin film thermoelectric material cannot bear too much external force in the testing process, and damage to the thin film thermoelectric material or uneven heat distribution are avoided. Meanwhile, only the temperature difference at two ends of the sample to be detected is controlled, and other operations are not introduced. Therefore, the structure solves the problem that the performance parameters of the thin film thermoelectric material are difficult to quickly and simply measure.
3. By arranging the first sample groove to adapt to the mechanical properties of the thin film thermoelectric material, for example, the thin film thermoelectric material is made into a relatively common chip, the thin film thermoelectric material can be placed into the first sample groove without preprocessing the shape of the thin film thermoelectric material, so that the complexity of a testing method is further simplified.
4. Through the mode of equivalent sample temperature monitoring of the second sample tank, the surface temperature of the sample to be detected is monitored in real time, so that the accuracy and reliability of the temperature and the temperature difference of the sample to be detected can be ensured, and the detection precision and efficiency are improved.
5. The device provided by the embodiment of the invention has a relatively high test range, the internal resistance of the sample to be tested can be higher than 50 megaohms, and the Seebeck coefficient of the sample to be tested can be measured with the internal resistance higher than 50 megaohms.
6. The test system provided by the embodiment of the invention has a simple and compact structure, and can be widely applied to the field of thermoelectric performance test of the thin film thermoelectric material.
7. An automatic detection system is formed by a computer, a control unit and detection equipment, the system can efficiently complete the test, and thermoelectric performance parameters of the thin film thermoelectric material can be automatically processed by a program preset in the computer.
Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention. The objectives and other advantages of the invention may be realized and attained by the structure particularly pointed out in the written description and drawings.
Drawings
The drawings are only for purposes of illustrating particular embodiments and are not to be construed as limiting the invention, like reference numerals being used to refer to like parts throughout the several views.
Fig. 1 is a schematic structural diagram of a thermoelectric performance parameter testing device for thin film thermoelectric materials according to an embodiment of the present invention.
Fig. 2 is a schematic diagram of a temperature control module according to an embodiment of the present invention.
Fig. 3 is a three-dimensional structure diagram of a temperature control module according to an embodiment of the present invention.
Fig. 4 is a schematic structural diagram of a basic temperature control module according to an embodiment of the present invention.
Fig. 5 is a schematic structural view of a stylus fixing apparatus according to an embodiment of the present invention.
Fig. 6 is a schematic structural diagram of a thermoelectric performance parameter testing system for thin film thermoelectric materials according to an embodiment of the present invention.
Fig. 7 is a schematic diagram of a four-electrode structure of a thin film thermoelectric material according to an embodiment of the present invention.
FIG. 8 is a flow chart of a method for testing performance parameters of a thin film thermoelectric material according to an embodiment of the present invention.
Reference numerals illustrate: 101 testing the cavity; 102 a sealing gasket; 103 liquid nitrogen pipeline connection ports; 104, testing a cable connection port; 105 air valve connectors; 106 testing the cavity cover; 107 a glass window on the test chamber lid; 2 a basic temperature control unit; 201 an electrical heating block; 202 a liquid nitrogen pipeline; 203 through holes; 204 a first mounting hole; 3, a buffer layer; 301 a buffer layer fixing block; 302 a first buffer layer; 303 a second buffer layer; 304 a second mounting hole; 305 a third mounting hole; 4 a temperature difference control unit; 401 a first heating block; 402 a second heating block; 403 a first sample cell; 404 a second sample well; 406 a fourth mounting hole; 5 stylus securing means; 501 a stylus fixture mounting block; 502 stylus operating flip cover mounting block; a 503 stylus operates the flip rotation shaft; 504 stylus operated flip; 505 test stylus; 506 are located at the opening of the stylus operated flip; 507 mounting holes 5;601 a substrate; 602 a metal electrode set; 603 the thermoelectric film to be tested.
Detailed Description
It should be noted that, in the present invention, the description of the directions or positional relationships such as "upper, lower, left, right, front, rear, inner, outer, vertical, horizontal, top, bottom, middle" or the like is used merely for convenience of description and understanding of the present invention, and does not indicate or imply that the devices or elements must have a specific orientation, be configured or operated in a specific orientation, especially when a certain component or device is described as being "fixed" or "connected" to another device or element, the device or element may be directly fixed or connected to another element, or may be indirectly fixed or connected to another element, and thus, the present invention is not to be construed as being limited.
Also, the terms "first," "second," and the like are used merely to distinguish between similar elements that have the same arrangement and function, and are not to be construed as indicating or implying a relative importance.
With the advent of electronics, organic thermoelectricity has emerged. The related data indicate that the number of articles and quotation in the field of organic thermoelectric research has increased dramatically since 2015. The method is used as a new technical field while being studied deeply, and the detection means is imperfect, so that how to rapidly and accurately complete the thermoelectric performance test of the organic thin film thermoelectric material becomes a bottleneck for restricting the rapid development of the field.
The invention provides a performance parameter testing device for a thin film thermoelectric material, which comprises a basic temperature control unit and a temperature difference control unit, wherein the basic temperature control unit is used for controlling the thermoelectric material to be at a preset testing temperature, and the temperature difference control unit creates temperature differences for two ends of a sample to be tested.
The temperature and the temperature difference of the sample to be detected can be ensured to be accurate and reliable through the basic temperature control unit and the temperature difference control unit, so that the detection precision and the detection efficiency are improved.
The thin film thermoelectric material performance parameter testing device of the invention further comprises: a cavity, a detection device and a stylus holder that enable a high vacuum.
The detection device includes: metal contact pin, current source, temperature thermocouple, voltmeter and test circuit. The test circuit connects the metal contact pins, the current source, the voltmeter and the electrodes of the thin film material together. And the basic temperature and the temperature difference are tested by a temperature thermocouple or a thermal resistor.
After changing the basic temperature of the film, testing the resistance at the basic temperature; and at the set specific basic temperature, regulating and controlling the temperature difference at the two ends of the film, measuring the electromotive force (namely the Seebeck voltage) generated by the temperature difference at the two ends of the film at the specific basic temperature and the temperature difference, and automatically calculating and outputting the Seebeck coefficient by a computer program. For resistance test, the current source is used for providing current flowing through the film when the resistance is tested by the four-probe method, and the voltmeter is used for testing voltage; for the seebeck voltage test, a voltmeter is used to measure the seebeck voltage between the hot and cold ends of the thin film hot material.
The base temperature control unit includes: an electric heating block and a liquid nitrogen pipeline; the electric heating block is used for heating the sample to be tested; the liquid nitrogen pipeline is used for providing a basic test temperature ranging from room temperature to liquid nitrogen temperature or rapidly cooling and heating a sample to be tested; the liquid nitrogen pipeline is arranged below the electric heating block.
The temperature difference control unit includes: a heating part and a sample bearing part to be tested; the heating part is used for controlling the temperature difference of two ends of the sample to be detected; the sample to be measured bearing part is used for bearing the sample to be measured.
The heating part includes: a first heating block and a second heating block. The sample to be measured is rectangular, and first heating piece heats the one end of sample to be measured, and the other end of sample to be measured is heated to the second heating piece. At the time of the seebeck voltage test, the temperature of the first heating block is different from that of the second heating block. The temperature of the first heating block is the same as the second heating block during resistance or conductivity testing.
The first heating block, the second heating block and the base temperature control unit are all made of materials with high heat conductivity.
The first heating block and the second heating block are internally provided with blind holes for installing an electric heater and a temperature measuring probe, and the temperature measuring probe is an armored thermocouple or a thermal resistor and is used for detecting the temperature at two ends of the first sample tank and the temperature at two ends of the second sample tank.
The surfaces of the first heating block and the second heating block are subjected to polishing treatment so as to enhance the heat conduction capability from the surfaces of the heating blocks to the sample to be tested.
A temperature control buffer layer is added between the first and second heating blocks and the base temperature control unit to enhance a temperature difference creation capability between the first and second heating blocks.
The thin film thermoelectric material performance parameter testing device further comprises: a buffer layer; the buffer layer is disposed between the temperature difference control unit and the base temperature control unit. The surface of the buffer layer is polished to enhance the heat conduction capability between the buffer layer and the heating block and between the buffer layer and the basic temperature control unit.
A sample carrier to be tested, comprising: a first sample well and a second sample well. The first heating block and the second heating block of the temperature control unit are arranged in parallel, two ends of the first sample groove are respectively arranged on the upper surfaces of the first heating block and the second heating block, and the two ends of the first sample groove are respectively contacted with the cold end and the hot end of the thermoelectric film to be tested; the second sample groove is parallel to the first sample groove, is positioned on the upper surfaces of the first heating block and the second heating block, and is respectively contacted with the cold end and the hot end of the base standard sample for temperature calibration.
The first sample groove is used for placing a sample to be tested. The second sample groove is used for placing the same substrate material (called a substrate standard sample) adopted by the sample to be detected, and is used for calibrating and monitoring the temperature and the temperature difference of the two ends of the sample to be detected in real time. And a thermometer is arranged on the surface of the base standard sample and respectively positioned at the appointed positions of the first heating block and the second heating block (for example, the positions of the thermometer are the same as the positions of the middle two electrodes of the four electrodes of the sample to be tested of the first sample tank), and the thermometer is used for equivalently measuring the temperature and the temperature difference of the specific position of the surface of the sample in real time. In the invention, the real-time temperature and the temperature difference monitored at the two ends of the surface of the base standard sample on the second sample tank are equivalent to the real-time temperature and the temperature difference at the two ends of the sample to be measured in the first sample tank. During testing, the pre-established thin film thermoelectric device (comprising a substrate) is arranged in the first sample groove, and heat conducting glue is smeared on the surface of the first sample groove and the back surface of the substrate of the thin film thermoelectric device, so that two ends of the substrate of the thermoelectric device are respectively in close contact with the two heating blocks, and good heat conduction is realized.
Samples to be tested (typically on the order of nanometers to micrometers in thickness) are typically pre-deposited (grown) on insulating substrates such as glass, which are prepared with a set of four electrodes. Wherein the space between the two middle electrodes is the same as the space between the hollow positions of the first sample groove (the space between the first heating block and the second heating block), and the two middle electrodes are positioned above the first heating block and the second heating block and aligned with the inner side edges of the first heating block and the second heating block respectively during sample testing and are used for monitoring the temperature difference electromotive force (Seebeck voltage); the four electrodes can be used for testing resistance by a four-probe method at the same time, and the resistivity and the conductivity can be automatically calculated according to the length, the width and the thickness of the film sample.
Alternatively, the sample material to be measured may be deposited (grown) directly on the blank substrate, and the four electrodes are redeposited (grown) on the surface of the sample to be measured.
The metal contact pin for sample test is fixed on the operation turnover cover of the contact pin fixing device, when the turnover cover device is covered by the contact pin, the test contact pin is in quick electric contact with four electrodes prepared in advance on the surface of the film sample, and when the turnover cover is opened, the test contact pin is separated from the sample electrodes.
The test cavity is also provided with an air valve and a test line external interface. The air valve and the test line external interface are arranged on the side wall of the test cavity. The air valve is used for vacuumizing or replacing the air in the cavity so as to enable the inside of the test cavity to be vacuum or preset test atmosphere. The position of the air valve deviates from the position of the thermoelectric material to be detected so as to avoid the damage of air flow to the sample to be detected. Optionally, a transparent glass window is further arranged on the top of the testing cavity, opposite to the position of the sample to be tested, and the transparent glass window can be used for observing the sample to be tested in real time in the testing process and can also be used for an excitation light source irradiation window for thermoelectric performance testing under the light excitation response.
The invention also provides a method for testing the performance parameters of the thin film thermoelectric material, which is applied to the thermoelectric material performance parameter testing system and comprises the following steps:
placing a substrate containing a sample to be tested in a first sample groove, and arranging a blank substrate in a second sample groove;
raising the temperature of the first sample tank and the second sample tank to a set temperature by utilizing a basic temperature control unit;
collecting resistance test data corresponding to a first sample tank and first calibration data corresponding to a second sample tank at a set temperature;
according to the set temperature, the temperature difference of the first sample tank and the second sample tank is adjusted to the set temperature difference by utilizing a temperature difference control unit;
and acquiring Seebeck voltage corresponding to the first sample tank and second calibration data corresponding to the second sample tank under the set temperature difference.
Specifically, the basic temperature control unit, the first heating block and the second heating block are respectively set and controlled at the same temperature, the temperature monitored in real time by the thermometers at the two ends of the standard substrate surface of the second sample tank is fed back and controlled, the thin film thermoelectric material to be tested is heated to the preset temperature and stabilized, and then the sample current I and the voltage V at the preset basic temperature are measured and recorded by a four-probe method.
Specifically, at a preset basic temperature, the first heating block and the second heating block are respectively subjected to (different) temperature control, and the temperature monitored in real time by the thermometers at the two ends of the standard substrate surface of the second sample tank is subjected to feedback and control, so that the two ends of the sample to be detected are in a preset temperature difference delta T at the preset basic temperature. The seebeck voltage Δv of the sample at this temperature difference was measured and recorded.
The computer equipment receives the performance parameters and calculates the Seebeck coefficient of the thin film thermoelectric material to be tested according to the performance parameters. Specifically, the value of the seebeck coefficient is found according to the formula s=Δv/Δt.
Optionally, the computer device is according to the formula pf=s 2 Sigma calculating the power factor of the sample to be measured.
Optionally, temperature control is performed on the first heating block and the second heating block respectively, preset temperature difference values at two ends of the sample to be measured are changed, and seebeck voltages generated under different temperature difference values are measured. And performing linear fitting on the plurality of temperature differences and the corresponding seebeck voltages at the same preset basic temperature, wherein the slope of the obtained linear function curve is the seebeck coefficient with reduced error.
The invention also provides a system for testing the performance parameters of the thin film thermoelectric material, which comprises computer equipment, a control unit and a thermoelectric material performance parameter testing device in the first aspect.
The control unit includes: and a temperature controller. The temperature controller is connected with the electric heater and the temperature measuring probe of the basic temperature control unit and is used for realizing the real-time control and monitoring of the temperature of the basic temperature control unit (thereby controlling the basic temperature of the thin film thermoelectric material to be tested); the temperature controller is also connected with an electric heater and a temperature measuring probe of the temperature difference control unit (a first heating block and a second heating block) and is used for realizing the real-time control and monitoring of the temperatures of the basic temperature control unit and the temperature difference control unit (thereby controlling the temperature and the temperature difference of the thin film thermoelectric material to be tested); the temperature controller is also connected with a thermometer on the surface of the base standard sample, so that the surface of the base standard sample and the equivalent surface of the sample to be detected are monitored in real time.
The computer equipment is connected with the control unit, the current source and the voltmeter and is used for receiving, storing and automatically processing the performance parameters acquired by the electricity source table and calculating the Seebeck coefficient and the conductivity of the thin film thermoelectric material to be tested according to the performance parameters. The test record performance parameters comprise the temperature of a basic temperature control unit, the temperature and the temperature difference of a first heating block and a second heating block, the real-time temperature and the temperature difference (equivalent to the temperature and the temperature difference of two ends of the surface of a sample to be tested in a first sample tank) of two ends of the surface of a base standard sample in a second sample tank, the Seebeck voltage of the thin film thermoelectric material to be tested, and the sample current value and the voltage value recorded by a four-probe resistance measurement method.
The computer device receives the parameters current I and voltage V. Effective size information of a sample to be measured, such as length L, width W and height H, is recorded in computer equipment, resistance R is calculated according to formula r=v/I, resistivity ρ is calculated according to formula ρ=rwh/l=vwh/(IL), and conductivity σ is calculated according to formula σ=1/ρ=l/rwh=il/(VWH).
Optionally, a graph of temperature difference versus seebeck voltage and a linear fitting curve are displayed on a computer system in real time, and the slope of the curve, i.e. the seebeck coefficient, is displayed.
Optionally, the basic temperature setting is changed, the above test steps are repeated, the conductivities and seebeck coefficients of the thin film thermoelectric materials at different basic temperatures are measured, and the formula pf=s is used 2 Sigma automatic calculation obtains power factors under different basic temperatures (temperature dependence).
Optionally, the base temperature dependent seebeck coefficient, conductivity, power factor curve is displayed in real time on a computer device.
The various embodiments of the invention and features of the embodiments may be combined without conflict, and the invention is further described in detail in conjunction with the drawings and detailed description.
Example 1
The embodiment of the invention provides a thermoelectric performance parameter testing device of a thin film thermoelectric material, as shown in fig. 1, the thermoelectric performance parameter testing device of the thin film thermoelectric material mainly comprises: the device comprises a cavity (101-107), a basic temperature control unit 2, a buffer layer 3, a temperature difference control unit 4, a contact pin fixing device 5 and detection equipment.
The basic temperature control unit 2, the buffer layer 3, the sample temperature and temperature difference control unit 4 are oppositely arranged inside the test cavity 101.
The basic temperature control unit 2 is carried at the bottom of the test cavity 101 and is used for controlling the basic test temperature of the sample to be tested; after the end of a single test, the base temperature control unit 2 can be used to quickly bring the sample back to room temperature.
The buffer layer 3 is carried on the surface of the basic temperature control unit 2.
The temperature difference control unit 4 is carried on the surface of the buffer layer 3.
The stylus holder 5 is mounted to the test chamber 101 at a position higher than the sample temperature difference control unit 4.
The liquid nitrogen pipeline connector 103, the test cable connector 104 and the air valve connector 105 are respectively positioned on the side wall of the cavity. The liquid nitrogen pipeline connector 103, the test cable connector 104 and the air valve connector 105 are respectively arranged on independent panels, and the independent panels are sealed with the test cavity 101 through sealing gaskets. Alternatively, the connection port may be designed integrally with the test cavity.
The gas valve 105 is used to evacuate the test chamber or replace the gas. In the embodiment of the present invention, when a sample to be tested is tested, the whole environment is required to be a preset test atmosphere (for example, vacuum or a specific air pressure or in a specific air), and the air in the cavity is replaced by setting the air valve 105.
The test cavity cover 106 is located above the test cavity 10101 and is hermetically sealed by a sealing gasket. A glass window 107 is positioned in the middle of the test chamber lid 106 and is aligned with the sample locations (first sample well and second sample well) to be tested.
Referring to fig. 2 and 4, a liquid nitrogen pipeline 202 is integrated with an electric heating block 201 of the basic temperature control unit 2 to form a basic temperature control unit together, so as to realize basic temperature control from the liquid nitrogen temperature to a high temperature region. The basic temperature control unit electric heating block 201 comprises a through hole 203, and an electric heating source and a temperature thermocouple are fixed inside the through hole 203. The base temperature control unit 2 is connected to the buffer layer 3 through the first mounting hole 204 and the second mounting hole 304.
If the first heating block 401 and the second heating block 402 are respectively in direct contact with the electric heating block 201, since the first heating block 401, the second heating block 402, and the base temperature control unit 2 are all made of a material having high thermal conductivity, heat of the first heating block 401 or the second heating block 402 is rapidly diffused to the electric heating block 201 and rapidly diffused to the second heating block 402 or the first heating block 401 through the electric heating block 201, so that a temperature difference that can be created between the two heating blocks 401 and 402 is limited. In order to solve the above-described problem, as shown in fig. 2, a first buffer layer 302 and a second buffer layer 303 are provided, and the first buffer layer 302 and the second buffer layer 303 are fixed to the buffer layer fixing block 301 through a third mounting hole (305). The first heating block 401 is fixed to the first buffer layer 302, and the second heating block 402 is fixed to the second buffer layer 303.
The first heating block 401 and the second heating block 402 are identical in structure and material and are made of high thermal conductive materials, such as copper, so that the heating blocks reach a preset temperature quickly and uniformly. The first buffer layer 302, the second buffer layer 303 and the buffer layer fixing block 301 are made of materials with moderate heat conduction, such as stainless steel. In this way, it is possible to ensure that the temperature controlled by the base temperature control unit 2 can be effectively conducted to the first and second heating blocks 401 and 402, and also to relatively suppress the speed of temperature interdiffusion between the first heating block 401 and the second heating block 402 due to the temperature difference, effectively creating a desired temperature difference.
In the embodiment of the present invention, the structures and materials of the first buffer layer 302 and the second buffer layer 303 are the same, and the space between the first buffer layer 302 and the second buffer layer 303 is the same as the space between the first heating block 401 and the second heating block 402. A partition groove is provided in the middle of the buffer layer fixing block 301, and the groove width is the same as the interval between the first heating block 401 and the second heating block 402. In the above manner, the horizontal heat transfer between the first buffer layer 302 and the second buffer layer 303 and the horizontal heat transfer between the first heating block 401 and the second heating block 402 are suppressed to the maximum extent, so that the temperature difference control is facilitated.
Alternatively, the buffer layer fixing block 301, the first buffer layer 302, and the second buffer layer 303 may be integrally processed. Alternatively, the first buffer layer 302 and the second buffer layer 303 may be directly fixed to the base temperature control unit heating block 201.
In addition, the first heating block 401 and the second heating block 402 have blind holes 405, and an electric heating source and a temperature thermocouple for temperature control and monitoring of the first heating block 401 and the second heating block 402 are fixed inside the blind holes 405. The first heating block 401 and the second heating block 402 are used for carrying and heating the thin film thermoelectric material (including the substrate) to be tested and the substrate standard sample, and creating a temperature difference for the sample to be tested and the substrate standard sample.
The two ends of the first sample groove 403 are respectively positioned on one side of the surfaces of the first heating block 401 and the second heating block 402; the two ends of the second sample groove 404 are respectively positioned on the other sides of the surfaces of the first heating block 401 and the second heating block 402. The first sample groove 403 and the second sample groove 404 cross the first heating block 401 and the second heating block 402 and are perpendicular to the length direction of the separation groove in the middle of the buffer layer fixing block 301, the surfaces of the first sample groove 403 and the second sample groove 404 are smooth and flat, the first sample groove 403 is used for bearing a sample to be detected (containing a substrate), the second sample groove 404 is used for bearing a substrate standard sample for real-time monitoring of the surface temperature and the temperature difference of an equivalent sample, and the substrate standard sample is an empty substrate. Alternatively, the number of sample wells may be greater than 2 to facilitate testing multiple sets of materials simultaneously. Specifically, the sample may be one control group or a plurality of experimental groups, or a plurality of control groups or a plurality of experimental groups.
The structure of the temperature control module composed of the basic temperature control unit 2, the buffer layer 3 and the temperature difference control unit 4 is shown in fig. 3.
As shown in fig. 5, the stylus holder mounting block 501 of the stylus holder 5 is fixed to the test cavity 101 through the mounting hole 5 (507), and the height of the stylus holder mounting block 501 is higher than the first heating block 401 and the second heating block 402. The stylus holder mounting block 501 has a stylus-operating flip cover mounting block 502. The stylus operation cover 504 is attached to the stylus operation cover fixing block 502 through a stylus operation cover rotation shaft 503. A set of four test pins 505 are secured to the stylus operating flip 504, the placement locations and spacings of the four test pins corresponding to the four electrode locations and spacings of the sample to be tested in the first sample slot. The position of the stylus-operated flip port 506 aligns the first sample slot 403 with the second sample slot 404 to facilitate viewing of the sample under test from the glass window 107 on the test cavity cover 106. The special flip design of the electric contact pin is monitored and tested in real time through the surface temperature of the equivalent sample, so that the test circuit is quickly and conveniently connected or disconnected, the test process can be ensured to be quick and simple, and the thermoelectric material to be tested is not damaged.
In the embodiment of the invention, the thermoelectric material to be tested can be an organic film thermoelectric material (such as polythiophene, polyaniline, polypyrrole, polycarbazole, pentacene, fullerene and the like) or an inorganic film thermoelectric material (such as constantan film, nichrome and the like). The thin film thermoelectric material with the thickness of nanometer to micrometer is prepared on an insulating substrate (glass, silicon dioxide sheet and the like) for supporting in advance, and a group of four metal electrodes with preset spacing and size can be deposited on the surface of the substrate in advance before the thin film is prepared, or can be deposited on the surface of the thin film after the thin film is prepared. The thin film thermoelectric material is placed in the first sample groove 403 together with the substrate, and the close contact and heat conduction capability between the first and second heating blocks 401 and 402 and the sample to be measured are enhanced by uniformly coating heat conduction glue on the surface of the first sample groove 403 and the back surface of the substrate.
In the embodiment of the invention, the detection device further comprises a thermometer, and the thermometer is fixed at a designated position (corresponding to the position of the voltage test electrode of the sample to be detected) on the upper surface of the base standard sample, so as to monitor and feed back the temperature control of the first heating block 401 and the second heating block 402 in real time.
In an embodiment of the invention, the detection device further comprises a test stylus 505. The test stylus comprises a set of four metallic spring-loaded styli having the same pitch as the electrode pitch on the sample to be tested, and two stylus positions in the middle are aligned with the inner edges of the first sample slot 403 and the second sample slot 404 and correspond to the sample electrode positions. In particular, during testing, when the thermoelectric film is placed in the position of the first sample trench 403, the four electrode positions on the film correspond one-to-one to the four metal elastic test pins 505 fixed to the pin manipulation flip 504. The sample placing operation can be performed by opening the flip 504 by the stylus operation; the contact pins operate the flip cover 504 to cover, and the four contact pins are in quick electrical contact with the four electrodes on the film sample to be tested, so that the electrical test of the resistance and the seebeck voltage of the film to be tested can be performed.
The stylus tail is secured to the stylus operating flip 504 and is connected to a current source and voltmeter external to the test cavity through the wire test cable interface 104.
It should be understood that in the embodiment of the present invention, the obtained performance parameter may be that the temperature difference created by the thermoelectric material to be tested on the first heating block 401 and the second heating block 402 causes the thermometer disposed on the surface of the base standard sample of the second sample tank to obtain the temperature and the temperature difference of the surface of the thermoelectric material of the thin film to be tested, and the seebeck voltage of the thermoelectric material to be tested.
In the embodiment of the invention, the electric heating source can be a single-head heating pipe, and the sample stage (heating block) adopts red copper.
Alternatively, the first heating block 401 and the second heating block 402 may employ peltier temperature control blocks.
As shown in FIG. 6, the embodiment of the invention provides a system for testing thermoelectric performance parameters of a film material. The system for testing the performance parameters of the thermoelectric materials of the thin film comprises a computer, a control unit, a vacuum pump, a liquid nitrogen controller and a thermoelectric material performance parameter testing device in fig. 1-5. Wherein, the control unit includes the accuse temperature appearance.
The computer equipment is connected with the temperature controller, the current source, the voltmeter and the liquid nitrogen controller.
The temperature controller comprises a plurality of temperature control output interfaces, and is respectively electrically connected with the electric heating sources of the basic temperature control unit electric heating block 201, the first heating block 401 and the second heating block 402 and the thermocouples. The temperature controller is used for controlling the temperatures of the electric heating block 201, the first heating block 401 and the second heating block 402 of the basic temperature control unit, and is used for creating basic temperature environments and temperature differences to be tested for the thin film thermoelectric materials to be tested. The temperature controller is also connected with thermometers at two ends of the surface of the base standard sample and is used for monitoring the temperature and the temperature difference of the surface of the base standard sample (equivalent to the surface of the sample to be measured) in real time.
The current source and the voltmeter are respectively and electrically connected with the test contact pins and are used for testing the resistance and the Seebeck voltage of the four probes.
The computer device is used for receiving temperature control and measurement parameters of the electric heating block 201, the first heating block 401 and the second heating block 402 of the basic temperature control unit. The computer device is configured to receive the real-time temperature and temperature differential (equivalent to the real-time temperature and temperature differential of the surface of the sample to be measured) of the surface of the base standard sample located in the second sample well 404. The computer equipment is used for receiving the test data of the electricity source meter and the voltmeter, and calculating the conductivity and the Seebeck coefficient of the thin film thermoelectric material to be tested according to the performance parameters in cooperation with the test options.
In the embodiment of the invention, the performance parameters of the thin film thermoelectric material to be tested can be obtained through the thin film thermoelectric material performance parameter testing system, so that the Seebeck coefficient and the conductivity of the thermoelectric material to be tested are calculated, and finally the power factor is calculated. The Seebeck coefficient, the conductivity and the power factor can be used as important basis for judging the performance of the thermoelectric material to be tested.
As shown in fig. 7, an embodiment of the present invention provides an electrode structure of a thin film thermoelectric material, including: the substrate 601, the thermoelectric film 603 to be tested and the metal electrode group 602 are positioned on the surface of the substrate.
When the cover is covered with the contact pins to operate the flip 504, when the test contact pins 505 are in electrical contact with the metal electrodes 602 of the sample 603 to be tested, the outer two contact pins of the test contact pins 505 are connected with a current source, and the inner two contact pins of the test contact pins 505 are connected with a voltmeter. When the sample to be tested is at the preset basic temperature, the current source and the voltmeter test the resistance value of the thin film thermoelectric material to be tested through the test contact pin, and the computer equipment is used for receiving the current value and the voltage value obtained by the test contact pin, calculating the resistance value and calculating the resistivity and the conductivity of the thin film thermoelectric material to be tested according to the resistance value.
Alternatively, when the resistance (conductivity) is tested by the four-probe method, it is possible to continuously measure at the same excitation current and average the test results.
Further, when the sample to be tested is at the preset basic temperature and the temperature difference, the two contact pins at the inner side of the test contact pin 505 connected with the voltmeter are used for performing the Seebeck voltage test on the thin film thermoelectric material to be tested, and the computer equipment is used for receiving the temperature difference and the Seebeck voltage and calculating the Seebeck coefficient of the thermoelectric material to be tested according to the performance parameters.
In an embodiment of the present invention, alternatively, a plurality of random effective measurements (continuous measurements) may be performed, and the averaging operation is used as the seebeck coefficient; alternatively, multiple groups of different temperature differences can be set at the same basic temperature, the seebeck voltages at the different temperature differences are measured, and linear fitting is performed on a series of seebeck voltages and the temperature differences, and the obtained fitting slope is the seebeck coefficient.
As shown in fig. 8, the method for testing performance parameters of a thin film thermoelectric material provided by the embodiment of the invention comprises the following steps:
step 701, placing a substrate containing a sample to be tested in a first sample tank, and setting a blank substrate in a second sample tank.
Step 702, raising the temperature of the first sample tank and the second sample tank to a set temperature by using a basic temperature control unit.
Step 703, collecting resistance test data corresponding to the first sample tank and first calibration data corresponding to the second sample tank at a set temperature.
In the embodiment of the invention, the second sample cell can be used as a blank control group, and the first calibration data is the temperature. The second sample well may be a standard control group, where the first calibration data includes temperature and/or resistance test data.
Step 704, adjusting the temperature difference between the first sample tank and the second sample tank to the set temperature difference by using the temperature difference control unit according to the set temperature.
Step 705, obtaining the seebeck voltage corresponding to the first sample cell and the second calibration data corresponding to the second sample cell under the set temperature difference.
In the embodiment of the invention, the second sample tank can be used as a blank control group, and the second calibration data is a temperature difference. The second sample cell may be a standard control group, where the first calibration data includes a temperature difference and/or a seebeck voltage.
It will be apparent that the described embodiments are some, but not all, embodiments of the invention. The components of the embodiments generally described and illustrated in the figures herein can be arranged and designed in a wide variety of different configurations.
Thus, the detailed description of the embodiments of the invention provided in the drawings 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 made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In summary, compared with the prior art, the thermoelectric material performance parameter testing device, method and system provided by the invention have at least the following effects:
1. the temperature and temperature difference monitoring mode is optimized:
prior art 1: monitoring the temperature of the heating end or the basic temperature by using a thermometer, testing the Seebeck voltage of a standard sample (such as nichrome) at the temperature, and calculating and calibrating the temperature difference of the sample to be tested according to the known Seebeck coefficient of the standard sample at the basic temperature and the Seebeck voltage obtained by testing.
Prior art 2: the thermometer (Pt thermal resistor) and the testing electrode are directly deposited on a substrate adopted by a sample to be tested, and each time the temperature of the sample is measured, the temperature calibration is needed. After a certain material test is finished, a new material test is carried out, a new substrate with a thermometer and an electrode needs to be replaced, the consumable cost of the substrate is high, and the sample preparation mode is complex.
The method adopts the mode of monitoring the equivalent sample temperature of the second sample tank, the temperature is calibrated once, and the temperature difference of any sample are monitored in real time at the later stage. For different substrates, different temperature calibration substrate standard samples can be replaced conveniently. The sample to be tested and the temperature monitoring are mutually independent, and the sample to be tested only needs to be replaced conveniently and rapidly every time a new sample with the same substrate is tested, and the temperature is not required to be calibrated again.
2. The connection mode of the test circuit and the sample electrode is optimized:
prior art 1: the test circuit is fixed and connected with the sample to be tested through the conductive silver adhesive, the sample to be tested is replaced, and the sample is fixed and connected with the conductive silver adhesive again, so that the operation is complex.
Prior art 2: when the sample to be tested is replaced, the needle seat of the built-in spring probe, which is connected with the sample electrode by the test circuit, needs to be screwed again each time, and the operation is troublesome.
The utility model discloses a flip formula contact pin fixing device is adopted to this application, and simple flip lets contact pin and electrode realize quick contact or break away from promptly, realizes test circuit's quick convenient connection or disconnection.
3. The testable range of the internal resistance of the sample is optimized:
prior art 1: the resistance of the sample was not measured. The error of the Seebeck coefficient result is increased after the internal resistance of the sample to be measured is higher than 100 kiloohms.
Prior art 2: the internal resistance of the sample to be tested is not higher than 1 megaohm, and if the internal resistance of the sample exceeds 1 megaohm, the resistance and the Seebeck coefficient cannot be tested.
The application comprises the following steps: the system is externally connected with a high-precision electricity source meter, the internal resistance of a sample to be measured can be higher than 50 megaohms, and the Seebeck coefficient of the sample with the internal resistance higher than 50 megaohms can be measured.
4. Simplifying the sample preparation process:
prior art 1: the special test chip board is adopted, and the sample to be tested and the standard sample are simultaneously fixed on two pairs of conductive electrodes on the chip by using conductive adhesive. The blocks were tested mainly. For a non-self-supporting film sample, special treatment is required to be carried out on the electrode chip, and then a film material is deposited on the surface of a sample testing area of the chip; or firstly depositing the sample on the substrate, fixing the sample to be tested and the substrate together to a test chip by referring to a bulk method, and connecting electrodes of the sample to be tested with electrodes of the chip by using gold wires and the like to realize circuit connection. The system is complicated for preparing a non-self-supporting film sample, and the temperature difference inaccuracy of the film sample tested by the testing method is large.
Prior art 2: prefabricating a patterning film on a special test chip as a mask, formulating the film on the basis, and removing the mask to form a patterning sample to be tested with specified specification; the chip is fixed on other substrates in advance to process the sample; the 100nm silicon nitride window film adopted in the middle of the chip is easy to break in the sample preparation process, so that sample preparation failure is caused; the top electrode device cannot be prepared; a single "chip" is expensive; the chip has extremely low recycling rate due to the weakness of the existing silicon nitride window; the base can only employ factory-specified "chips" of silicon-based substrates of multi-layer structure.
Any insulating substrate may be used in the present application; the film patterning mode is simple, the pattern size requirement can be relaxed, and the actual size can be measured after the sample preparation is completed; the glass and other common substrates adopted by the application are cheap, and the new substrate can be directly used without considering the problem of repeated use when testing new materials; even if the problem of substrate reuse needs to be considered, the cleaning is simple and convenient and the substrate is not easy to damage. A top electrode device may be prepared.
5. Optimizing test results:
prior art 1 and prior art 2: only the seebeck coefficient can be tested, and the conductivity needs to be tested independently by other equipment. Since the conductivity and seebeck coefficient are not tested by the same system, the calculation error of the power factor increases.
The Seebeck coefficient and the conductivity are tested in the same system, so that the total error caused by testing multiple parameters in different systems is reduced.
Therefore, the technical scheme provided by the application is simpler and more convenient, the sample preparation requirement is lower, and the consumable cost is low. Meanwhile, the temperature and the temperature difference of the surface of the sample are monitored in real time, a high-precision electrical test source meter is adopted, and the result is better in accuracy and reliability.
The present invention is not limited to the above-mentioned embodiments, and any changes or substitutions that can be easily understood by those skilled in the art within the technical scope of the present invention are intended to be included in the scope of the present invention.
Claims (9)
1. A method for testing performance parameters of a thin film thermoelectric material is completed by a testing device and is characterized by comprising the following steps:
placing a substrate containing a sample to be tested in a first sample groove, and arranging a blank substrate in a second sample groove;
raising the temperature of the first sample tank and the second sample tank to a set temperature by using a base temperature control unit;
collecting resistance test data corresponding to the first sample groove and first calibration data corresponding to the second sample groove at the set temperature;
according to the set temperature, adjusting the temperature difference of the first sample tank and the second sample tank to a set temperature difference by using a temperature difference control unit;
acquiring Seebeck voltage corresponding to the first sample tank and second calibration data corresponding to the second sample tank under the set temperature difference;
when the second sample tank is a blank control group, the first calibration data is temperature; when the second sample cell is a standard sample control group, the first calibration data includes temperature and/or resistance test data;
when the second sample tank is a blank control group, the second calibration data is a temperature difference; when the second sample cell is a standard sample control group, the first calibration data comprises a temperature difference and/or a seebeck voltage;
The test device comprises: a basic temperature control unit and a temperature difference control unit which are arranged from bottom to top;
the basic temperature control unit is used for controlling the basic temperature of the sample to be tested;
the temperature difference control unit is used for controlling the temperature difference of two ends of the sample to be detected;
the temperature difference control unit comprises a sample bearing part to be detected, and the sample bearing part to be detected is used for bearing the sample to be detected.
2. The method of claim 1, wherein the step of determining the position of the substrate comprises,
the test device further includes: a buffer layer;
the buffer layer is disposed between the temperature difference control unit and the base temperature control unit.
3. The method of claim 1, wherein the step of determining the position of the substrate comprises,
the base temperature control unit includes: an electric heating block and a liquid nitrogen pipeline;
the electric heating block is used for heating the sample to be tested;
the liquid nitrogen pipeline is used for providing a basic test temperature ranging from room temperature to liquid nitrogen temperature or rapidly cooling and heating a sample to be tested;
the liquid nitrogen pipeline is arranged below the electric heating block.
4. The method of claim 3, wherein the step of,
the electric heating block is provided with a detection hole, and the detection hole is used for installing an electric heating source and a temperature measuring element.
5. The method according to any one of claim 1 to 4, wherein,
the temperature difference control unit further includes: a heating section;
the heating part is used for controlling the temperature difference between two ends of the sample to be measured.
6. The method of claim 5, wherein the step of determining the position of the probe is performed,
the heating section includes: a first heating block and a second heating block;
a gap is formed between the first heating block and the second heating block, one end of a sample to be measured is arranged above the first heating block, and the other end of the sample to be measured is arranged above the second heating block.
7. The method of claim 6, wherein the step of providing the first layer comprises,
the sample carrier to be tested includes: a first sample cell and a second sample cell arranged in parallel;
the two ends of the first sample groove are respectively arranged on the first heating block and the second heating block; two ends of the second sample groove are respectively arranged on the first heating block and the second heating block;
the first sample groove is used for bearing a sample to be detected and a substrate, and the second sample groove is used for bearing a blank substrate.
8. The method according to claim 2, wherein a separation groove is formed on one side of the buffer layer, which is close to the temperature difference control unit, and two ends of the sample to be measured are located on two sides of the separation groove.
9. A thin film thermoelectric material performance parameter testing system, comprising: computer device, control unit and test apparatus in a method according to any of claims 1-8.
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