技术领域technical field
本发明涉及材料科学领域中热电材料性能测试技术，特别涉及一种薄膜热电材料热导率测试系统及方法。The invention relates to a thermoelectric material performance testing technology in the field of material science, in particular to a thermal conductivity testing system and method of a thin-film thermoelectric material.
背景技术Background technique
随着微纳米技术、微机电系统(MEMS)、超大规模集成电路技术的快速发展，对微纳米尺寸材料的研究及其应用日益受到重视。热电材料是一种能实现热能与电能之间相互转换的功能材料，在温差发电、温差电制冷以及传感器等方面有着广泛应用。热电材料的热电转换效应(亦称赛贝克效应)可用下式表示：With the rapid development of micro-nano technology, micro-electromechanical systems (MEMS), and ultra-large-scale integrated circuit technology, the research and application of micro-nano-sized materials have been paid more and more attention. Thermoelectric materials are functional materials that can realize mutual conversion between thermal energy and electrical energy, and are widely used in thermoelectric power generation, thermoelectric refrigeration, and sensors. The thermoelectric conversion effect (also known as the Seebeck effect) of thermoelectric materials can be expressed by the following formula:
E＝α(T1-T2)E=α(T1 -T2 )
式中T1和T2是热电材料两端的温度，且T1＞T2，α为赛贝克系数，E为热电材料在温差为(T1-T2)条件下产生的赛贝克电动势。热电材料两端的温差(T1-T2)越大，产生的赛贝克电动势也越大。为了获得高的赛贝克电动势，要求热电材料具有低的热导率。因此，热导率是热电材料的一项重要性能指标。热导率的定义如下：当温度垂直梯度为1℃/m时，单位时间内通过单位水平截面积所传递的热量。在一般情况下，则有：where T1 and T2 are the temperatures at both ends of the thermoelectric material, and T1 > T2 , α is the Seebeck coefficient, and E is the Seebeck electromotive force generated by the thermoelectric material under the condition of a temperature difference of (T1 -T2 ). The greater the temperature difference (T1 -T2 ) between the two ends of the thermoelectric material, the greater the Seebeck electromotive force generated. In order to obtain a high Seebeck electromotive force, thermoelectric materials are required to have low thermal conductivity. Therefore, thermal conductivity is an important performance index of thermoelectric materials. The definition of thermal conductivity is as follows: when the vertical temperature gradient is 1°C/m, the heat transferred through the unit horizontal cross-sectional area per unit time. In general, there are:
dE/dt＝-κ·A·dT/dl (1)dE/dt＝-κ·A·dT/dl (1)
(1)式中E是在时间t内所传递的热量，A为材料的截面积，l为长度，T为温度，κ为热导率。传统的热电材料通常采用冶金的方法或者粉末烧结的方法制造。这类方法制造的块体热电材料，采用激光热导率测试仪可以方便地测出热电材料的热导率。但对于厚度在微米甚至纳米尺度的热电材料，激光热导率测试仪已经不能用于测试其热导率。目前，国内外尚无商品化的用于薄膜热电材料热导率测试的仪器。本发明的薄膜热电材料热导率测试系统及方法，可以快速准确地测量薄膜热电材料的热导率，解决了目前薄膜热电材料热导率无法测量的问题。(1) In the formula, E is the heat transferred in time t, A is the cross-sectional area of the material, l is the length, T is the temperature, and κ is the thermal conductivity. Traditional thermoelectric materials are usually manufactured by metallurgical methods or powder sintering methods. For bulk thermoelectric materials produced by this method, the thermal conductivity of the thermoelectric materials can be easily measured by using a laser thermal conductivity tester. But for thermoelectric materials whose thickness is in the micron or even nanometer scale, the laser thermal conductivity tester can no longer be used to test the thermal conductivity. At present, there is no commercialized instrument for testing the thermal conductivity of thin-film thermoelectric materials at home and abroad. The thermal conductivity testing system and method of the thin-film thermoelectric material of the present invention can quickly and accurately measure the thermal conductivity of the thin-film thermoelectric material, and solve the problem that the thermal conductivity of the thin-film thermoelectric material cannot be measured at present.
发明内容Contents of the invention
本发明的目的在于克服现有技术的不足，提供一种用于测试薄膜热电材料热导率的测试系统及方法，能够实现对薄膜热电材料热导率(厚度在微米甚至纳米尺度的热电材料)的精确测定。The purpose of the present invention is to overcome the deficiencies of the prior art, to provide a test system and method for testing the thermal conductivity of thin-film thermoelectric materials, which can realize the thermal conductivity of thin-film thermoelectric materials (thermoelectric materials with a thickness of micron or even nanoscale) precise measurement.
本发明的目的通过下述技术方案予以实现：The purpose of the present invention is achieved through the following technical solutions:
一种用于测试薄膜热电材料热导率的测试系统，由真空体系、测试卡具和控制及测试电路体系三部分构成。待测薄膜热电材料试样放置在测试卡具内，测试过程中测试卡具内部处于密闭的真空环境中。控制及测试电路体系用于调控流经加热块上的电流，实现薄膜热电材料测试过程热流量的控制以及测试数据的采集，并将测试数据传输至微型计算机，通过微型计算机实现对整个测试系统测试过程的控制、测试数据的处理以及测试数据和计算结果在计算机显示器上的实时显示。该系统可以实现对薄膜热电材料热导率的精确测定。具体结构描述如下：A test system for testing the thermal conductivity of thin-film thermoelectric materials consists of three parts: a vacuum system, a test fixture, and a control and test circuit system. The sample of the thin film thermoelectric material to be tested is placed in the test fixture, and the inside of the test fixture is in a closed vacuum environment during the test. The control and test circuit system is used to regulate the current flowing through the heating block, realize the control of heat flow and the collection of test data during the test process of thin-film thermoelectric materials, and transmit the test data to the microcomputer, and realize the test of the whole test system through the microcomputer Process control, test data processing and real-time display of test data and calculation results on the computer monitor. The system can realize accurate measurement of thermal conductivity of thin film thermoelectric materials. The specific structure is described as follows:
真空体系(如附图5、附图6所示)由压力表20、接压力表三通21、热偶真空计22、接热偶真空计三通23、真空泵三通24、放气阀25、接放气阀三通26、手动真空阀27、真空泵接口28、真空泵29、三通密封盖30、密封卡箍8和密封胶圈9组成。其特征是，启动真空泵29，打开手动真空阀27后，测试系统的测试卡具内逐渐形成真空环境，测试卡具内的真空环境可以最大限度地减少因待测试样4的测试表面以及加热块7表面的热辐射造成的热量损失。The vacuum system (as shown in accompanying drawing 5 and accompanying drawing 6) consists of a pressure gauge 20, a pressure gauge tee 21, a thermocouple vacuum gauge 22, a thermocouple vacuum gauge tee 23, a vacuum pump tee 24, and an air release valve 25 , connect air release valve tee 26, manual vacuum valve 27, vacuum pump interface 28, vacuum pump 29, tee sealing cover 30, sealing clamp 8 and sealing rubber ring 9 and form. It is characterized in that, after starting the vacuum pump 29 and opening the manual vacuum valve 27, a vacuum environment is gradually formed in the test fixture of the test system, and the vacuum environment in the test fixture can minimize the impact caused by the test surface of the sample 4 to be tested and heating. Heat loss due to heat radiation from the surface of block 7.
测试卡具(如附图1、附图2所示)由试样支撑架外罩1、试样支撑架2、试样支撑架连接端口3、第一测温热电偶5、第二测温热电偶6、加热块7、密封卡箍8、密封胶圈9、连接管10、接外引线三通11、外引线接口12组成。其特征是，试样支撑架1的内部形成放置待测试样的样品室；待测试样4放置在位于试样支撑架2上的试样底座32之上，试样底座32通过试样底座固定螺钉34固定在试样支撑架2之上。加热块7放置于加热块底座31上，可通过加热块底座固定螺钉33固定加热块底座31的位置，以保证加热块7与待测试样4的传热端面紧密接触。调整热电偶底座35的位置，旋紧热电偶底座固定螺钉36以保证第一测温热电偶5和第二测温热电偶6与待测试样4的测试面紧密接触。第一测温热电偶5测得待测试样4测试面上该热电偶所处位置处(测温点)的温度，第二测温热电偶6测得得待测试样4测试面上该热电偶所处位置处(测温点)的温度。当通过控制及测试电路体系调节流经加热块7上的电流使其释放热量，在高真空环境中，短时间内电流流经加热块7产生的热量几乎全部通过待测试样4的传热端面沿薄膜热电材料的长度方向传导并在长度方向上建立起温度梯度，通过位于热电偶底座35两端的第一测温热电偶5和第二测温热电偶6，分别测得待测试样4测试面上这二个热电偶所处位置处(测温点)的温度。The test fixture (as shown in accompanying drawing 1 and accompanying drawing 2) consists of a sample support frame outer cover 1, a sample support frame 2, a sample support frame connection port 3, a first temperature measuring thermocouple 5, a second temperature measuring thermocouple Couple 6, heating block 7, sealing clamp 8, sealing rubber ring 9, connecting pipe 10, connecting outer lead wire tee 11, outer lead wire interface 12 composition. It is characterized in that the inside of the sample support frame 1 forms a sample chamber for placing the sample to be tested; the sample to be tested 4 is placed on the sample base 32 on the sample support frame 2, and the sample base 32 passes through the sample chamber. Base fixing screws 34 are fixed on the sample support frame 2 . The heating block 7 is placed on the heating block base 31, and the position of the heating block base 31 can be fixed by the heating block base fixing screw 33 to ensure that the heating block 7 is in close contact with the heat transfer end surface of the test sample 4. Adjust the position of the thermocouple base 35, and tighten the thermocouple base fixing screw 36 to ensure that the first temperature measuring thermocouple 5 and the second temperature measuring thermocouple 6 are in close contact with the test surface of the sample 4 to be tested. The first temperature-measuring thermocouple 5 records the temperature at the position (temperature measuring point) of the thermocouple on the test surface of the test sample 4, and the second temperature-measuring thermocouple 6 records the temperature on the test surface of the test sample 4. The temperature at the position (temperature measurement point) of the thermocouple. When the current flowing through the heating block 7 is adjusted through the control and testing circuit system to release heat, in a high vacuum environment, the heat generated by the current flowing through the heating block 7 in a short period of time is almost completely passed through the heat transfer of the sample 4 to be tested. The end face conducts along the length direction of the thin-film thermoelectric material and establishes a temperature gradient in the length direction. The first temperature measuring thermocouple 5 and the second temperature measuring thermocouple 6 located at both ends of the thermocouple base 35 respectively measure the temperature of the sample to be tested. 4 The temperature at the position (temperature measuring point) of the two thermocouples on the test surface.
本发明的薄膜热电材料热导率测试系统在真空条件下进行测试，按照附图5和6所示，将测试卡具与真空体系相连接。即接外接引线三通11通过密封卡箍8与接压力表三通21相连接，接压力表三通上的压力表20用于显示测试体系内部的压力。接热偶真空计三通23通过密封卡箍8与接压力表三通21相连接，其上安装的热偶真空计22用于显示带真空体系测试卡具内部的真空度。接真空泵三通24通过密封卡箍8与接热偶真空计三通23相连接，其上安装的手动真空阀27用于调节测试体系内部的真空度，通过密封卡箍8将手动真空阀27与真空泵接口28相连，真空泵接口28通过外接管线与真空泵29连接。接放气阀三通26通过密封卡箍8与接真空泵三通24相连接，其上安装的放气阀25用于调节测试系统内部的压力。The thermal conductivity test system of the thin film thermoelectric material of the present invention is tested under vacuum conditions, and the test fixture is connected with the vacuum system as shown in Figures 5 and 6 . That is, the external lead wire tee 11 is connected to the pressure gauge tee 21 through the sealing clamp 8, and the pressure gauge 20 on the pressure gauge tee is used to display the internal pressure of the test system. The tee 23 connected to the thermocouple vacuum gauge is connected to the tee 21 connected to the pressure gauge through the sealing clamp 8, and the thermocouple vacuum gauge 22 installed on it is used to display the vacuum degree inside the test fixture with a vacuum system. The tee 24 connected to the vacuum pump is connected to the tee 23 connected to the thermocouple vacuum gauge through the sealing clamp 8, and the manual vacuum valve 27 installed on it is used to adjust the vacuum degree inside the test system. It is connected with the vacuum pump interface 28, and the vacuum pump interface 28 is connected with the vacuum pump 29 through an external pipeline. The tee 26 connected to the air release valve is connected to the tee 24 connected to the vacuum pump through the sealing clamp 8, and the air release valve 25 installed on it is used to adjust the internal pressure of the test system.
控制及测试电路体系(如附图3所示)由加热块导线13、第一测温热电偶导线14、第二测温热电偶导线15、控制及数据采集装置16、数据传输线17、微型计算机18、冰水混合浴19组成。其特征是，样品室内的加热块7、第一测温热电偶5和第二测温热电偶6均通过安装在接外引线三通11上的外引线接口12延伸出测试卡具。控制及数据采集装置16通过加热块导线13实现对流经测试卡具内的加热块7上的加热电流大小的控制，从而控制流入待测薄膜温差电材料的热量；控制及数据采集装置16通过第一测温热电偶导线14与第一测温热电偶5相连、第二测温热电偶导线15与第二测温热电偶6相连，实现对待测试样4测试面上二个热电偶所处位置处(测温点)温度的采集；控制及数据采集装置16由A/D转换器、单片机、串口转换器、电源、进行电流控制和信号传输及信号处理的电子电路等组成；控制及数据采集装置16通过数据传输线17连接到微型计算机18上，由微型计算机18对控制及数据采集装置16采集到并上传的数据进行处理，并在微型计算机18的显示器上实时显示采集到的数据以及数据处理结果。The control and test circuit system (as shown in accompanying drawing 3) is made up of heating block wire 13, first temperature measuring thermocouple wire 14, second temperature measuring thermocouple wire 15, control and data acquisition device 16, data transmission line 17, microcomputer 18, ice water mixed bath 19 composition. It is characterized in that the heating block 7 in the sample chamber, the first temperature measuring thermocouple 5 and the second temperature measuring thermocouple 6 all extend out of the test fixture through the outer lead interface 12 installed on the outer lead tee 11 . The control and data acquisition device 16 realizes the control of the magnitude of the heating current flowing through the heating block 7 in the test fixture through the heating block wire 13, thereby controlling the heat flowing into the thin film thermoelectric material to be tested; the control and data acquisition device 16 passes through the first A temperature-measuring thermocouple wire 14 is connected to the first temperature-measuring thermocouple 5, and a second temperature-measuring thermocouple wire 15 is connected to the second temperature-measuring thermocouple 6 to realize the position of the two thermocouples on the test surface of the test sample 4. Acquisition of temperature at (temperature measuring point); control and data acquisition device 16 is made up of A/D converter, single-chip microcomputer, serial port converter, power supply, electronic circuit for current control, signal transmission and signal processing; control and data acquisition The device 16 is connected to the microcomputer 18 through the data transmission line 17, and the data collected and uploaded by the control and data acquisition device 16 is processed by the microcomputer 18, and the collected data and data processing are displayed in real time on the display of the microcomputer 18. result.
本发明提出的测试系统的测试原理是基于一维傅里叶传热方程(Fourier thermalconductivity equation)求解热导率的稳态方法，即：The test principle of the test system proposed by the present invention is based on the one-dimensional Fourier heat transfer equation (Fourier thermalconductivity equation) to solve the steady-state method of thermal conductivity, namely:
q是热流密度矢量，它表示在单位等温面面积上，沿温度降低的方向，单位时间内传导的热量。热导率κ反映物质的导热能力，其单位是W/(m·K)，其中，W为功率单位(瓦特)，m为长度单位(米)，K为温度单位(开尔文)。ΔT为两测温点之间的温差。Δx为两测温点之间的距离。在微尺度传热学理论中，当材料的传热尺度L及传热时间t可以和声子的平均自由程1(10-7～10-8m数量级)及平均自由时间τ(10-12s数量级)相比拟时，将不满足傅立叶传热定律。因此用这种方法测量薄膜热导率，要求被测薄膜的厚度大于声子的平均自由程，即要求被测薄膜的厚度在微米数量级或纳米数量级。本测试系统由第一测温热电偶5和第二测温热电偶6分别测得待测试样4测试面上这二个热电偶所处位置处(测温点)的温度T1和T2，则(2)式中的温差ΔT＝T1-T2；待测试样4测试面上这二个热电偶之间的距离为Δx；控制流经加热块7上的电流强度为I，加热块的电阻值为R，待测试样4沿温度降低方向的横截面积为S，则(2)式中的热流密度矢量q＝I2R/S。将q、Δx和ΔT带入公式(2)，即可得到热导率κ。q is the heat flux density vector, which represents the heat conduction per unit time along the direction of temperature decrease on the unit isothermal surface area. Thermal conductivity κ reflects the thermal conductivity of a substance, and its unit is W/(m K), where W is the unit of power (watt), m is the unit of length (meter), and K is the unit of temperature (Kelvin). ΔT is the temperature difference between the two temperature measuring points. Δx is the distance between two temperature measuring points. In the theory of microscale heat transfer, when the heat transfer scale L and the heat transfer time t of the material can be compared with the mean free path 1 of the phonon (on the order of 10-7 ~ 10-8 m) and the mean free time τ (10-12 s order of magnitude) compared, will not satisfy Fourier's law of heat transfer. Therefore, to measure the thermal conductivity of a thin film by this method, the thickness of the measured thin film is required to be greater than the mean free path of phonons, that is, the thickness of the measured thin film is required to be on the order of microns or nanometers. This test system measures the temperatures T1 and T1 of the two thermocouples at the positions (temperature measuring points) on the test surface of the sample 4 to be tested by the first temperature measuring thermocouple 5 and the second temperature measuring thermocouple6 respectively.2 , then the temperature difference ΔT=T1 -T2 in (2) formula; The distance between these two thermocouples on the testing surface of sample 4 to be tested is Δx; , the resistance value of the heating block is R, and the cross-sectional area of the sample 4 to be tested along the direction of temperature drop is S, then the heat flux vector q in formula (2)=I2 R/S. Bringing q, Δx and ΔT into formula (2), the thermal conductivity κ can be obtained.
在利用本发明的测试系统对薄膜热电材料进行热导率测试时，可按照下述步骤进行：When utilizing the test system of the present invention to carry out the thermal conductivity test to the thin-film thermoelectric material, it can be carried out according to the following steps:
首先，将待测试样4放置并固定在位于试样支撑架2上的试样底座32之上，通过试样底座固定螺钉34固定试样底座32的位置。调节加热块底座31的位置，并通过加热块底座固定螺钉33固定加热块底座31的位置，以保证加热块7与待测试样4的传热端面紧密接触。调整热电偶底座35的位置，以保证第一测温热电偶5和第二测温热电偶6与待测试样4的测试面紧密接触，旋紧热电偶底座固定螺钉36使其定位。将试样支撑架外罩1用密封卡箍8及密封胶圈9固定到连接管10上，保证测试卡具内部处于封闭状态；First, the sample 4 to be tested is placed and fixed on the sample base 32 on the sample support frame 2 , and the position of the sample base 32 is fixed by the sample base fixing screws 34 . Adjust the position of the heating block base 31, and fix the position of the heating block base 31 by the heating block base fixing screw 33, so as to ensure that the heating block 7 is in close contact with the heat transfer end surface of the sample 4 to be tested. Adjust the position of the thermocouple base 35 to ensure that the first temperature-measuring thermocouple 5 and the second temperature-measuring thermocouple 6 are in close contact with the test surface of the sample 4 to be tested, and tighten the thermocouple base fixing screw 36 to make it positioned. Fix the outer cover 1 of the sample support frame to the connecting pipe 10 with the sealing clamp 8 and the sealing rubber ring 9 to ensure that the inside of the test fixture is in a closed state;
之后，启动真空泵29，打开手动真空阀27，并通过压力表20和热偶真空计22检测测试系统内部的压力，至测试系统内部压力达到测试所需真空度时，关闭手动真空阀27以及真空泵29；Afterwards, start the vacuum pump 29, open the manual vacuum valve 27, and detect the pressure inside the test system by the pressure gauge 20 and the thermocouple vacuum gauge 22, and when the internal pressure of the test system reaches the required vacuum degree for the test, close the manual vacuum valve 27 and the vacuum pump 29;
第三，加热块导线13、第一测温热电偶导线14、第二测温热电偶导线15分别与控制及数据采集装置16相连，实现对流经测试卡具内的加热块7上的加热电流大小的控制和对待测试样4测试面上二个热电偶所处位置处(测温点)温度的采集；The 3rd, the heating block wire 13, the first temperature-measuring thermocouple wire 14, the second temperature-measuring thermocouple wire 15 are connected with the control and data acquisition device 16 respectively, realize the heating current flowing through the heating block 7 in the test fixture The control of the size and the acquisition of the temperature at the positions (temperature measuring points) of the two thermocouples on the test surface of the test sample 4;
第四，启动微型计算机18和控制及数据采集装置16，并对控制及数据采集装置16进行校正；The 4th, start microcomputer 18 and control and data acquisition device 16, and control and data acquisition device 16 are calibrated;
第五，选择与实际电路相应的通讯端口、冷热端测温通道，输入控制电路的相应电阻值、第一测温热电偶5和第二测温热电偶6与待测试样4测试面相接触点(测温点)之间的间距、待测试样的传热横截面积、加热块的加热功率，利用微型计算机18和控制及数据采集装置16进行数据采集并进行运算，以得到最终测试结果。Fifth, select the communication port corresponding to the actual circuit, the hot and cold end temperature measurement channel, input the corresponding resistance value of the control circuit, the first temperature measurement thermocouple 5 and the second temperature measurement thermocouple 6 and the test surface of the sample 4 to be tested. The distance between contact points (temperature measuring points), the heat transfer cross-sectional area of the sample to be tested, and the heating power of the heating block are collected and calculated by using the microcomputer 18 and the control and data acquisition device 16 to obtain the final Test Results.
其中，所述测试卡具内的真空度可以选择为10-5～10-6Pa，为避免热量的散失，可进一步提高真空度值，但需要注意整个测试系统的密封程度。Wherein, the vacuum degree in the test fixture can be selected as 10-5 ~ 10-6 Pa, in order to avoid heat loss, the vacuum degree value can be further increased, but attention should be paid to the sealing degree of the entire test system.
在进行测试时，可采用实时测试和实时显示方式，绘制待测试样4测试面上两温度测试点的温度-时间曲线、待测试样4的热导率-温差曲线。During the test, real-time testing and real-time display methods can be used to draw the temperature-time curves of the two temperature test points on the test surface of the test sample 4 and the thermal conductivity-temperature difference curve of the test sample 4 .
采用本发明的本发明的薄膜热电材料热导率测试系统及方法，可以快速准确地测量薄膜热电材料的热导率，解决了目前薄膜热电材料热导率无法测量的问题。The thermal conductivity testing system and method of the thin-film thermoelectric material of the present invention can quickly and accurately measure the thermal conductivity of the thin-film thermoelectric material, and solve the problem that the thermal conductivity of the thin-film thermoelectric material cannot be measured at present.
附图说明Description of drawings
图1测试卡具结构示意图Figure 1 Schematic diagram of test fixture structure
图2测试卡具结构局部剖视示意图Figure 2 Schematic diagram of partial cross-section of the structure of the test fixture
图3薄膜热电材料热导率测试系统各部分之间的电路连接示意图Figure 3 Schematic diagram of the circuit connection between the various parts of the thermal conductivity test system for thin-film thermoelectric materials
图4安装在微型计算机上的数据处理软件程序框图Figure 4 is a block diagram of the data processing software installed on the microcomputer
图5带真空体系测试卡具结构示意图Figure 5 Schematic diagram of the test fixture with vacuum system
图6带真空体系测试卡具结构局部剖视示意图Figure 6 Schematic diagram of a partial cross-sectional view of the structure of a test fixture with a vacuum system
附图中，1、试样支撑架外罩；2、试样支撑架；3、试样支撑架连接端口；4、待测试样；5、第一测温热电偶；6、第二测温热电偶；7、加热块；8、密封卡箍；9、密封胶圈；10、连接管；11、接外引线三通；12、外引线接口；13、接加热块导线；14、第一测温热电偶导线；15、第二测温热电偶导线；16、控制及数据采集装置；17、数据传输线；18、微型计算机；19、冰水混合浴；20、压力表；21、接压力表三通；22、热偶真空计；23、接热偶真空计三通；24、接真空泵三通；25、放气阀；26、接放气阀三通；27、手动真空阀；28、真空泵接口；29、真空泵；30、三通密封盖；31、加热块底座；32、试样底座；33、加热块底座固定螺钉；34、试样底座固定螺钉；35、热电偶底座；36、热电偶底座固定螺钉。In the attached drawings, 1. The outer cover of the sample support frame; 2. The sample support frame; 3. The connection port of the sample support frame; 4. The sample to be tested; 5. The first temperature measurement thermocouple; 6. The second temperature measurement Thermocouple; 7. Heating block; 8. Sealing clamp; 9. Sealing rubber ring; 10. Connecting pipe; 11. Tee connection to the outer lead wire; 12. Outer lead wire interface; 13. Connecting to the heating block wire; 14. The first Temperature measuring thermocouple wire; 15. Second temperature measuring thermocouple wire; 16. Control and data acquisition device; 17. Data transmission line; 18. Microcomputer; 19. Ice-water mixed bath; 20. Pressure gauge; 21. Connection pressure Table tee; 22, thermocouple vacuum gauge; 23, thermocouple vacuum gauge tee; 24, vacuum pump tee; 25, air release valve; 26, air release valve tee; 27, manual vacuum valve; 28 , vacuum pump interface; 29, vacuum pump; 30, tee sealing cover; 31, heating block base; 32, sample base; 33, heating block base fixing screw; 34, sample base fixing screw; 35, thermocouple base; 36 , Thermocouple base fixing screws.
具体实施方式Detailed ways
下面结合附图对本发明做进一步的详细说明：Below in conjunction with accompanying drawing, the present invention is described in further detail:
图1和图2为测试卡具外观结构示意图和部分内部结构剖视示意图。测试卡具由试样支撑架外罩1、试样支撑架2、试样支撑架连接端口3、第一测温热电偶5、第二测温热电偶6、加热块7、密封卡箍8、密封胶圈9、连接管10、接外引线三通11、外引线接口12组成。其特征是，试样支撑架1的内部形成放置待测试样的样品室；待测试样4放置在位于试样支撑架2上的试样底座32之上，可通过试样底座固定螺钉34固定试样底座32的位置。加热块7放置于加热块底座31上，可通过加热块底座固定螺钉33固定加热块底座31的位置，并保证加热块7与待测试样4的传热端面紧密接触。调整热电偶底座35的位置，旋紧热电偶底座固定螺钉36以保证第一测温热电偶5和第二测温热电偶6与待测试样4的测试面紧密接触。当通过控制及测试电路体系调节流经加热块7的电流使其释放热量，该热量传入测试样4并建立起温差，通过位于热电偶底座35两端的第一测温热电偶5和第二测温热电偶6，分别测得待测试样4测试面上这二个热电偶所处位置处(测温点)的温度T1和T2Figure 1 and Figure 2 are a schematic diagram of the external structure of the test fixture and a schematic cross-sectional view of part of the internal structure. The test fixture consists of a sample support frame cover 1, a sample support frame 2, a sample support frame connection port 3, a first temperature measuring thermocouple 5, a second temperature measuring thermocouple 6, a heating block 7, a sealing clamp 8, The sealing rubber ring 9, the connecting pipe 10, the outer lead wire tee 11, and the outer lead wire interface 12 are formed. It is characterized in that the inside of the sample support frame 1 forms a sample chamber for placing the sample to be tested; the sample to be tested 4 is placed on the sample base 32 on the sample support frame 2, and the screw can be fixed by the sample base. 34 fixes the position of the sample base 32. The heating block 7 is placed on the heating block base 31, the position of the heating block base 31 can be fixed by the heating block base fixing screw 33, and the heating block 7 is in close contact with the heat transfer end surface of the sample 4 to be tested. Adjust the position of the thermocouple base 35, and tighten the thermocouple base fixing screw 36 to ensure that the first temperature measuring thermocouple 5 and the second temperature measuring thermocouple 6 are in close contact with the test surface of the sample 4 to be tested. When the current flowing through the heating block 7 is adjusted by the control and test circuit system to release heat, the heat is transferred to the test sample 4 and a temperature difference is established, and the first temperature-measuring thermocouple 5 and the second thermocouple located at the two ends of the thermocouple base 35 are passed through the heat. The temperature measuring thermocouple 6 measures the temperaturesT1 andT2 at the positions (temperature measuring points) of the two thermocouples on the test surface of the sample 4 to be tested respectively.
图3为薄膜热电材料热导率测试系统各部分之间的电路连接示意图。样品室内的加热块7、第一测温热电偶5和第二测温热电偶6均通过安装在接外引线三通11上的外引线接口12延伸出测试卡具。控制及数据采集装置16通过接加热块导线13实现对流经测试卡具内的加热块7上的电流大小的控制，从而控制传入待测试样4内的热量；控制及数据采集装置16通过第一测温热电偶导线14与第一测温热电偶5相连、第二测温热电偶导线15与第二测温热电偶6相连，由此实现对待测试样4测试面上的二个热电偶所处位置处(测温点)温度的采集；控制及数据采集装置16由A/D转换器、单片机、串口转换器、电源、进行电流控制和信号传输及信号处理的电子电路等组成；控制及数据采集装置16通过数据传输线17连接到微型计算机18上；由微型计算机18对控制及数据采集装置16采集到并上传的数据进行处理，并在微型计算机18的显示器上实时显示采集到的数据以及数据处理结果。Fig. 3 is a schematic diagram of circuit connections among various parts of the thermal conductivity test system for thin film thermoelectric materials. The heating block 7, the first temperature measuring thermocouple 5 and the second temperature measuring thermocouple 6 in the sample chamber all extend out of the test fixture through the outer lead interface 12 installed on the outer lead tee 11. The control and data acquisition device 16 realizes the control of the magnitude of the current flowing through the heating block 7 in the test fixture by connecting the heating block wire 13, thereby controlling the heat introduced into the sample 4 to be tested; the control and data acquisition device 16 passes through The first temperature-measuring thermocouple wire 14 is connected with the first temperature-measuring thermocouple 5, and the second temperature-measuring thermocouple wire 15 is connected with the second temperature-measuring thermocouple 6, thereby realizing the two thermocouples on the test surface of the test sample 4. Acquisition of the temperature at the position (temperature measuring point) of the couple; the control and data acquisition device 16 is composed of an A/D converter, a single-chip microcomputer, a serial port converter, a power supply, an electronic circuit for current control, signal transmission and signal processing, etc.; Control and data acquisition device 16 is connected on the microcomputer 18 by data transmission line 17; The data collected and uploaded by the control and data acquisition device 16 is processed by microcomputer 18, and on the display of microcomputer 18, display the collected data in real time. data and data processing results.
图5和图6为带真空体系的测试卡具外观结构示意图和部分内部结构剖视示意图。真空体系接外接引线三通11通过密封卡箍8与接压力表三通21相连接，接压力表三通上的压力表20用于显示测试体系内部的压力。接热偶真空计三通23通过密封卡箍8与接压力表三通21相连接，其上安装的热偶真空计22用于显示带真空体系测试卡具内部的真空度。接真空泵三通24通过密封卡箍8与接热偶真空计三通23相连接，其上安装的手动真空阀27用于调节测试体系内部的真空度，通过密封卡箍8将手动真空阀27与真空泵接口28相连，真空泵接口28通过外接管线与真空泵29连接。接放气阀三通26通过密封卡箍8与接真空泵三通24相连接，其上安装的放气阀25用于调节测试系统内部的气体压力。启动真空泵29，打开手动真空阀27后，测试卡具内逐步形成真空环境，测试卡具内的真空环境可以最大限度地减少因待测试样4的测试表面以及加热块7表面的热辐射造成的热量损失。Fig. 5 and Fig. 6 are schematic diagrams of the external structure and partial internal structure of the test fixture with a vacuum system. The vacuum system connected to the external lead wire tee 11 is connected to the pressure gauge tee 21 through the sealing clamp 8, and the pressure gauge 20 on the pressure gauge tee is used to display the pressure inside the test system. The tee 23 connected to the thermocouple vacuum gauge is connected to the tee 21 connected to the pressure gauge through the sealing clamp 8, and the thermocouple vacuum gauge 22 installed on it is used to display the vacuum degree inside the test fixture with a vacuum system. The tee 24 connected to the vacuum pump is connected to the tee 23 connected to the thermocouple vacuum gauge through the sealing clamp 8, and the manual vacuum valve 27 installed on it is used to adjust the vacuum degree inside the test system. It is connected with the vacuum pump interface 28, and the vacuum pump interface 28 is connected with the vacuum pump 29 through an external pipeline. The tee 26 connected to the air release valve is connected to the tee 24 connected to the vacuum pump through the sealing clamp 8, and the air release valve 25 installed on it is used to adjust the gas pressure inside the test system. Start the vacuum pump 29 and open the manual vacuum valve 27 to gradually form a vacuum environment in the test fixture. The vacuum environment in the test fixture can minimize the heat radiation caused by the test surface of the test sample 4 and the surface of the heating block 7. heat loss.
在利用上述装置进行测试时，首先启动微型计算机18，启动控制及数据采集装置16，将测试转换开关拨到“校正”档，校正控制及数据采集装置16后，将测试转换开关拨到“测试”档；打开微型计算机18上薄膜热电材料热导率测试软件，点击“通讯设置”，选择与实际电路相应的通讯端口、冷热端测温通道，点击“基本设置”，键入控制电路的相应电阻值，键入待测试样4测试面上两温度测试点之间的间距，键入待测试样的传热横截面积，输入加热块的加热功率值。打开控制电路，点击“开始测试”，此时计算机显示器开始实时绘制待测试样4测试面上两温度测试点的温度-时间曲线、待测试样4的热导率-温差曲线。测试完成后，点击“停止测试”以停止数据采集，点击“保存数据”以保存数据。如果需要继续测试，则点击“清空实时数据”以清除上一次的测试结果，在测试卡具中放入新的待测试样，重复上述步骤，以进行下一组测试。若测试结束，则退出测试界面。When utilizing the above-mentioned device to test, first start the microcomputer 18, start the control and data acquisition device 16, turn the test changeover switch to the "correction" file, and after the correction control and data acquisition device 16, turn the test changeover switch to "test". " file; open the thermal conductivity test software of thin film thermoelectric material on the microcomputer 18, click "communication setting", select the communication port corresponding to the actual circuit, the temperature measurement channel of the cold and hot end, click "basic setting", enter the corresponding control circuit For the resistance value, input the distance between two temperature test points on the test surface of the sample to be tested 4, input the heat transfer cross-sectional area of the sample to be tested, and input the heating power value of the heating block. Open the control circuit, click "start test", and now the computer display starts to draw the temperature-time curves of the two temperature test points on the test surface of the test sample 4 and the thermal conductivity-temperature difference curve of the test sample 4 in real time. After the test is complete, click "Stop Test" to stop data collection, and click "Save Data" to save the data. If you need to continue the test, click "Clear Real-time Data" to clear the last test result, put a new sample to be tested in the test fixture, and repeat the above steps for the next set of tests. If the test is over, exit the test interface.
测试电化学沉积n型薄膜热电材料Bi2Te2.7Se0.3的热导率。热导率的测试按照以下步骤进行：The thermal conductivity of the electrochemically deposited n-type thin film thermoelectric material Bi2 Te2.7 Se0.3 was tested. The thermal conductivity test is carried out according to the following steps:
第一步：将试样支撑架外罩1取下，将待测试样4放置在位于试样支撑架2上的试样底座32之上，通过试样底座固定螺钉34固定试样底座32的位置。调节加热块底座31的位置，并通过加热块底座固定螺钉33固定加热块底座31的位置，以保证加热块7与待测试样4的传热端面紧密接触。调整热电偶底座35的位置，以保证试样第一测温热电偶5和试样第二测温热电偶6与待测试样4的测试面紧密接触，旋紧热电偶底座固定螺钉36使其定位。将试样支撑架外罩1用密封卡箍8及密封胶圈9固定到连接管10上，保证测试卡具内部处于封闭状态；The first step: remove the sample support frame outer cover 1, place the sample 4 to be tested on the sample base 32 on the sample support frame 2, and fix the sample base 32 by the sample base fixing screw 34 Location. Adjust the position of the heating block base 31, and fix the position of the heating block base 31 by the heating block base fixing screw 33, so as to ensure that the heating block 7 is in close contact with the heat transfer end surface of the sample 4 to be tested. Adjust the position of the thermocouple base 35 to ensure that the first temperature-measuring thermocouple 5 of the sample and the second temperature-measuring thermocouple 6 of the sample are in close contact with the test surface of the sample 4 to be tested, and tighten the thermocouple base fixing screw 36 so that its positioning. Fix the outer cover 1 of the sample support frame to the connecting pipe 10 with the sealing clamp 8 and the sealing rubber ring 9 to ensure that the inside of the test fixture is in a closed state;
第二步：启动真空泵29，打开手动真空阀27，并通过压力表20和热偶真空计22检测测试系统内部的压力，至测试系统内部真空度达到10-6pa时，关闭手动真空阀27以及真空泵29；Step 2: start the vacuum pump 29, open the manual vacuum valve 27, and detect the pressure inside the test system through the pressure gauge 20 and thermocouple vacuum gauge 22, and close the manual vacuum valve 27 when the vacuum inside the test system reaches 10−6 pa and a vacuum pump 29;
第三步：启动微型计算机18，启动控制及数据采集装置16，将测试转换开关拨到“校正”档，校正控制及数据采集装置16后，将测试转换开关拨到“测试”档；The third step: start the microcomputer 18, start the control and data acquisition device 16, turn the test changeover switch to the "calibration" file, and after the calibration control and data acquisition device 16, turn the test changeover switch to the "test" file;
第四步：打开微型计算机18上薄膜热电材料热导率测试软件，点击“通讯设置”，选择与实际电路相应的通讯端口、冷热端测温通道；点击“基本设置”，键入控制电路的相应电阻值，键入第一测温热电偶5和第二测温热电偶6与待测试样4测试面相接触点(测温点)之间的间距15mm，键入待测试样的传热横截面积2×10-7m2，输入加热块的加热功率值92.8mW。打开控制电路，点击“开始测试”，此时计算机显示器上开始实时绘制待测试样4测试面上两温度测试点的温度-时间曲线、待测试样4的热导率-温差曲线。Step 4: Open the thin-film thermoelectric material thermal conductivity test software on the microcomputer 18, click "communication settings", select the corresponding communication port and hot and cold end temperature measurement channels corresponding to the actual circuit; click "basic settings", enter the control circuit Corresponding resistance value, key in the distance between the first temperature measuring thermocouple 5 and the second temperature measuring thermocouple 6 and the contact point (temperature measuring point) of the test surface of the sample 4 to be tested 15mm, key in the heat transfer cross section of the sample to be tested The cross-sectional area is 2×10-7 m2 , and the heating power value of the input heating block is 92.8mW. Open the control circuit, click "start test", and start to draw the temperature-time curve of the two temperature test points on the test surface of the test sample 4 and the thermal conductivity-temperature difference curve of the test sample 4 in real time on the computer display.
第五步：测试完成后，点击“停止测试”以停止数据采集，之后点击“保存数据”以保存测试结果，退出测试界面。Step 5: After the test is completed, click "Stop Test" to stop data collection, then click "Save Data" to save the test results and exit the test interface.
计算机显示器显示的测试结果如下：室温条件下，试样的热导率为1.59W/(m·K)。The test results displayed on the computer monitor are as follows: at room temperature, the thermal conductivity of the sample is 1.59W/(m·K).
以上对本发明做了示例性的描述，应该说明的是，在不脱离本发明的核心的情况下，任何简单的变形、修改或者其他本领域技术人员能够不花费创造性劳动的等同替换均落入本发明的保护范围。The present invention has been described as an example above, and it should be noted that, without departing from the core of the present invention, any simple deformation, modification or other equivalent replacements that can be made by those skilled in the art without creative labor all fall within the scope of this invention. protection scope of the invention.
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210039803.9ACN102590274B (en) | 2012-02-21 | 2012-02-21 | System and method used for testing heat conductivity of thin film thermoelectric material |
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210039803.9ACN102590274B (en) | 2012-02-21 | 2012-02-21 | System and method used for testing heat conductivity of thin film thermoelectric material |
| Publication Number | Publication Date |
|---|---|
| CN102590274A CN102590274A (en) | 2012-07-18 |
| CN102590274Btrue CN102590274B (en) | 2014-07-30 |
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210039803.9AExpired - Fee RelatedCN102590274B (en) | 2012-02-21 | 2012-02-21 | System and method used for testing heat conductivity of thin film thermoelectric material |
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| CN (1) | CN102590274B (en) |
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| CN115248228A (en)* | 2021-04-26 | 2022-10-28 | 中国科学院化学研究所 | Thin film thermoelectric parameter tester and testing method |
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| CN102253082A (en)* | 2011-06-29 | 2011-11-23 | 上海大学 | Device and method for dynamically measuring thermal physical parameters of film |
| CN102297877A (en)* | 2011-05-27 | 2011-12-28 | 上海大学 | Device and method for measuring thermoelectric parameters of film |
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102297877A (en)* | 2011-05-27 | 2011-12-28 | 上海大学 | Device and method for measuring thermoelectric parameters of film |
| CN102253082A (en)* | 2011-06-29 | 2011-11-23 | 上海大学 | Device and method for dynamically measuring thermal physical parameters of film |
| Publication number | Publication date |
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| CN102590274A (en) | 2012-07-18 |
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