WO2020073442A1 - 一种石墨烯材料热导率及界面热阻的测量装置和方法 - Google Patents
一种石墨烯材料热导率及界面热阻的测量装置和方法 Download PDFInfo
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- WO2020073442A1 WO2020073442A1 PCT/CN2018/117001 CN2018117001W WO2020073442A1 WO 2020073442 A1 WO2020073442 A1 WO 2020073442A1 CN 2018117001 W CN2018117001 W CN 2018117001W WO 2020073442 A1 WO2020073442 A1 WO 2020073442A1
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- thermal resistance
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/20—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity
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- the invention relates to the technical field of heat transfer, in particular to a device and method for measuring the thermal conductivity and interface thermal resistance of graphene materials.
- Thermal conductivity is a physical quantity that reflects the thermal conductivity of a material. Interfacial thermal resistance is an obstacle to heat transfer due to the presence of interfaces between different materials. Thermal conductivity and interface thermal resistance have a wide range of application backgrounds in engineering fields involving heat transfer. For example, in engineering applications, in order to meet the requirements of the production process, sometimes by increasing the material thermal conductivity and reducing the interface thermal resistance To enhance heat transfer.
- Compressible materials refer to materials whose total volume changes when a certain degree of pressure is applied, such as powder materials or porous materials, of which graphene material is an important compressible material. Compared to incompressible materials, the different compression ratios of compressible materials have important effects on their thermal conductivity and contact thermal resistance. In recent years, as compressible materials have important applications in the electronics industry and the construction industry, it is of great significance to study the thermal conductivity and interface thermal resistance of compressible materials at different compression rates.
- the object of the present invention is to provide a device for measuring the thermal conductivity and interface thermal resistance of graphene materials, which can realize the simultaneous measurement of the thermal conductivity and interface thermal resistance of materials at different compression rates.
- a device for measuring the thermal conductivity and interface thermal resistance of graphene materials including an upper cylinder, a lower cylinder, an upper cap, a press, a water circulation cooling unit, and displacement detection Unit, heating unit, temperature detection unit and data processing unit; the bottom end of the upper cylinder and the top of the lower cylinder are both open and interconnected; the interior of the upper cylinder is a hollow structure to form an upper test cavity,
- the upper test chamber is provided with an upper top cover, a first metal block and a test sample, the top and bottom of the first metal block are in contact with the upper top cover and the test sample, respectively;
- the interior of the lower cylinder body is a hollow structure A lower test cavity is formed.
- the lower test cavity is provided with a support portion and a second metal block, the second metal block is fixed on the support portion, the top of the second metal block is in contact with the test sample, and the bottom is provided It is a fin structure and suspended in the lower test cavity;
- the water circulation cooling unit is connected to the lower test cavity;
- the press is connected to the upper top cover;
- the displacement detection unit includes a displacement sensor and displacement electrically connected to each other Collector card, the displacement sensor is connected to the upper top cover;
- the heating unit includes a power supply and an electric heating component electrically connected to each other, the electric heating component is embedded in the first metal block;
- the temperature detection unit includes a mutual electric A connected thermocouple array and a temperature acquisition card, the thermocouple array is provided in the upper test chamber and the lower test chamber;
- the data processing unit is electrically connected to the press, the displacement acquisition card and the temperature acquisition card, respectively.
- the invention uses a press to apply pressure to the top cover, the top cover transmits the pressure to the test sample, the test sample is compressed by force, and the displacement detection unit is used to monitor and collect the displacement value of the test sample under different forces in real time to obtain the test sample
- the compression ratio Compared with the prior art, the present invention can change the compressibility of compressible materials on the same set of devices for compressible materials, and realize the simultaneous measurement of the thermal conductivity and interface thermal resistance of compressible materials at different compression rates, and The invention can also be used to measure the thermal conductivity and interface thermal resistance of incompressible materials.
- the device of the present invention has the advantages of simple equipment, high measurement accuracy, good reliability, and wide measurement range.
- the inner wall of the upper cylinder is provided with a sliding groove
- the upper top cover is installed in the sliding groove and can slide up and down in the upper test chamber along the sliding groove.
- the side wall of the first metal block is provided with a protrusion corresponding to the sliding groove.
- the depth of the chute is 0.1-2 mm.
- the top of the first metal block is provided with a groove, and the electric heating component is provided in the groove.
- the water circulation cooling unit includes a water cooling chamber, two sections of cooling water pipes and a circulating water pump; the water cooling chamber is respectively connected to the lower test chamber through two sections of cooling water pipes, and a water inlet and a water outlet are formed at the connection parts;
- the circulating water pump is installed in one of the cooling water pipes.
- the rib structure includes several strip-shaped pieces, and two ends of the strip-shaped piece are respectively close to the water inlet and the water outlet.
- outer wall and the inner wall of the upper and lower cylinders are filled with a layer of thermal insulation material.
- thermocouple array is provided in the plurality of through holes.
- thermocouple array is composed of several thermocouples arranged at equal intervals.
- the pitch of the thermocouple is 3-15 mm.
- the invention also provides a method for measuring the thermal conductivity of graphene materials.
- the measurement device according to the invention includes the following steps:
- S1 Place the test sample between the upper and lower metal blocks, use a press to apply a pressure to the upper top cover, and the upper top cover transmits the pressure to the test sample through the upper metal block, so that the test sample is compressed by force and moves through the displacement
- the detection unit measures the displacement change of the test sample to obtain its compression rate
- the invention also provides a method for measuring the thermal resistance of the graphene material interface.
- the measurement device based on the invention includes the following steps:
- S1 Place the test sample between the upper and lower metal blocks, use a press to apply a pressure to the upper top cover, and the upper top cover transmits the pressure to the test sample through the upper metal block, so that the test sample is compressed by force and moves through the displacement
- the detection unit measures the displacement change of the test sample to obtain its compression rate
- S3 Draw a temperature distribution curve based on the measured temperature data corresponding to different positions of the upper metal block, the test sample and the lower metal block along the axis of the cylinder, and fit the upper metal block, the test sample and the lower metal respectively The functional relationship between the temperature of the block and the test position points f1, f2 and f3. Using linear interpolation, the position value of the contact interface between the test sample and the upper metal block is substituted into f1 and f2 to obtain the corresponding temperatures T S1 and T S2 .
- FIG. 1 is a schematic structural diagram of a graphene material thermal conductivity and interface thermal resistance measurement device of an embodiment.
- FIG. 2 is a schematic diagram of a partial structure of a graphene material thermal conductivity and interface thermal resistance measuring device of an embodiment.
- FIG. 3 is a test temperature distribution curve and a fitting curve of a functional relationship between temperature and position in an embodiment.
- the graphene material thermal conductivity and interface thermal resistance measurement device of this embodiment includes an upper cylinder 10, a lower cylinder 20, an upper cap 30, a press 40, and a water circulation cooling unit 50 , Displacement detection unit 60, heating unit 70, temperature detection unit 80 and data processing unit 90.
- the bottom end of the upper cylinder 10 and the top end of the lower cylinder 20 are both open and connected to each other.
- the inner and outer diameters of the upper cylinder 10 and the lower cylinder 20 are the same, and the upper cylinder The body 10 and the outer wall of the lower cylinder 20 are connected by a fastening buckle 101, so that the insides of the two cylinders are tightly connected.
- the upper cylinder 10 and the lower cylinder 20 may also be integrally formed. Both the outer wall and the inner wall of the upper cylinder body 10 and the lower cylinder body 20 have a hollow structure, and are filled with a thermal insulation material 102 with low thermal conductivity.
- the inside of the upper cylinder 10 is a hollow structure to form an upper test cavity.
- the inner wall of the upper cylinder 10 is provided with a sliding groove 11.
- the upper top cover 30 is installed in the sliding groove 11 and can be along the sliding groove 11 Slide up and down in the upper test chamber.
- the chute 11 is an elongated chute along the axial direction of the upper cylinder 10, and its depth does not exceed 2 mm, preferably 0.1 to 2 mm.
- a first metal block 12 and a test sample 13 are provided in the upper test cavity.
- the top and bottom of the first metal block 12 are in contact with the upper top cover 30 and the test sample 13, respectively.
- the first metal block 12 is a standard brass material, which has a constant thermal conductivity value during the temperature rising process.
- the first metal block 12 is a cylindrical structure, and its side wall is provided with a protrusion corresponding to the sliding groove 11 for fixing, and its diameter matches the inner diameter of the upper cylinder 10, which can be Slip into the upper cylinder 10 along the chute 11.
- the interior of the lower cylinder 20 is a hollow structure to form a lower test cavity.
- the lower test cavity is provided with a support portion 21 and a second metal block 22, and the second metal block 22 is fixed on the support portion 21.
- the top of the second metal block 22 is in contact with the test sample 13, and the bottom is set as a rib structure and suspended in the lower test cavity.
- the test sample 13 is clamped between the first metal block 12 and the second metal block 22.
- the second metal block 22 is also a standard brass material, which has a constant thermal conductivity value during the temperature rising process.
- the upper half of the second metal block 22 has a cylindrical structure, and its diameter matches the inner diameter of the upper cylinder 10 and can be sleeved into the lower cylinder 10.
- the water circulation cooling unit 50 includes a water cooling chamber 51, two sections of cooling water pipes 52 and a circulating water pump 53; the water cooling chamber 51 communicates with the lower test chamber through two sections of cooling water pipes 52, respectively forming a water inlet and a water outlet at the connected parts ;
- the circulating water pump 53 is provided in one of the cooling water pipes.
- the water cooling chamber 51 is used to provide a stable cooling source, and the circulating water pump 53 is used to ensure the circulating flow of cooling water.
- the volume of the water cooling chamber 51 cannot be set too small, and it should be ensured that the temperature of the internal water should be close to room temperature during the long-term circulation, and its volume is generally not less than 10cm ⁇ 10cm ⁇ 10cm.
- the fin structure at the bottom of the second metal block 22 is connected to the water circulation cooling circuit, which can ensure rapid heat exchange with the circulating water, and it includes a plurality of strips, and the two ends of the strip are close The water inlet and the water outlet.
- the press 40 is connected to the upper top cover 30 to apply pressure.
- the upper top cover 30 transmits the pressure to the test sample 13 so that the test sample 13 is forced to compress and deform to produce displacement changes.
- the displacement detection unit 60 includes a displacement sensor 61 and a displacement acquisition card 62 that are electrically connected to each other.
- the displacement sensor 61 is connected to the upper top cover 30 to monitor the displacement change of the test sample 13 in real time.
- the heating unit 70 includes a power supply 71 and an electric heating assembly 72 that are electrically connected to each other.
- the electric heating assembly 72 is embedded in the first metal block 12.
- the electric heating component 72 is an electric heating plate, a groove is provided on the top of the first metal block 12, and the electric heating plate is provided in the groove.
- the temperature detection unit 80 includes a thermocouple array 81 and a temperature acquisition card 82 that are electrically connected to each other.
- the thermocouple array 81 is provided in the upper test chamber and the lower test chamber. Specifically, the thermocouple array 81 may be located in the upper cylinder 10 and the lower cylinder
- the side wall of the body 20 is provided with a plurality of through holes arranged at equal intervals in the axial direction.
- the thermocouple array 81 is provided in the through holes and directly communicates with the first metal block 12, the test sample 13, and the second metal block 22 The contact is used to detect the temperature of the first metal block 12, the test sample 13 and the second metal block 22 at different positions along the axial direction of the cylinder.
- the thermocouple array 81 is formed by arranging a plurality of thermocouples at equal intervals, and the interval is generally not less than 3 mm, preferably 3-15 mm.
- the data processing unit 90 may be a computer, which is electrically connected to the press 40, the displacement acquisition card 62, and the temperature acquisition card 82 to collect corresponding data in real time.
- This embodiment also provides a method for measuring the thermal conductivity and interface thermal resistance of graphene materials. Based on the above measurement device, the method includes the following steps:
- test sample which can be a porous material or a powder type material.
- the test sample is a graphene powder material, which is a circular sheet structure, and its cross-sectional size is the same as that of the first metal block and the first The cross-sectional dimensions of the two metal blocks are the same, and the initial thickness L is measured to be 30 mm.
- the pressure applied by the press should not be too large. It is necessary to ensure that the test sample will not be denatured due to structural damage during the process of force application. Its value is related to the material of the test sample. When the force is applied, it will gradually increase from zero to small. Increase to the set value.
- the pressure can be adjusted by a press to obtain test samples at different compression rates. In this embodiment, the displacement value ⁇ L of the test sample is 6.0 mm, and the compression rate ⁇ L / L is 20%.
- the length of time is generally greater than two hours.
- Use a temperature acquisition card to record the temperature values at different positions in the upper test chamber and the lower test chamber , Where the temperature values of the first metal block, the test sample, and the second metal block at different test locations are listed in Table 1, Table 2, and Table 3 respectively, taking the position of the electric heating plate as the heat source as the reference position, and x indicates the edge The distance between the axial downward direction of the cylinder and the reference position.
- the average temperature gradient dT 1 / dx 1 through the first metal block is calculated by the test data in Table 1 to be -30K / m, and the average temperature gradient through the second metal block is calculated through the test data in Table 3.
- dT 2 / dx 2 is -23K / m
- the first and second metal blocks in this embodiment are standard brass materials
- the thermal conductivity k is 102W / (m ⁇ K)
- using the formula Q 2 -k ⁇ dT 2 / dx 2 calculating the heat flux density passing through the second metal block Q 2 is 2346W / m 2
- calculate the heat flux density Q 0 of the tested sample by the formula Q 0 (Q 1 + Q 2 ) / 2 is 2703W / m 2 .
- the upper interface of the test sample is in contact with the bottom interface of the first metal block at a position of 45 mm, and the position value is substituted into f2 and f1 respectively to calculate the temperature corresponding to the position;
- the interface at the top of the block is in contact at a position of 75mm. Substitute this position value into f2 and f3, and calculate the temperature corresponding to the position.
- Table 4 The above calculation data is shown in Table 4.
- the present invention can change the compressibility of compressible materials on the same set of devices for compressible materials, and realize the simultaneous measurement of the thermal conductivity and interface thermal resistance of compressible materials at different compression rates, and The invention can also be used to measure the thermal conductivity and interface thermal resistance of incompressible materials.
- the present invention has the advantages of simple equipment, convenient operation, high measurement accuracy, good reliability, and wide measurement range.
Abstract
一种石墨烯材料热导率及界面热阻的测量装置和方法。测量装置包括上筒体（10）、下筒体（20）、上顶盖（30）、压力机（40）、水循环冷却单元（50）、位移检测单元（60）、加热单元（70）、温度检测单元（80）和数据处理单元（90），上、下筒体（20，30）内分别设有第一金属块（12）和第二金属块（22），测试样品（13）设于两金属块之间，上顶盖（30）位于第一金属块（12）上方，压力机（40）与上顶盖（30）相连。利用压力机（40）对上顶盖（30）施加压力，上顶盖（30）将压力传递给测试样品（13），测试样品（13）受力压缩，利用位移检测单元（60）实时监控并采集测试样品（13）在不同受力下的位移值，获得测试样品（13）的压缩率，并实现测试样品（13）在不同压缩率下的热导率和界面热阻测量。
Description
本发明涉及传热技术领域，尤其涉及一种石墨烯材料热导率及界面热阻的测量装置和方法。
热导率是反映材料热传导能力的物理量。界面热阻是因不同材料间交界面的存在而产生的对热量传递的阻碍。热导率与界面热阻在涉及到传热的工程领域中有广泛的应用背景，如在工程应用中，为了满足生产工艺的要求，有时通过提升材料热导率和减小界面热阻的方式以强化传热。
可压缩材料是指施加一定程度的压力时，其自身的总体积会发生变化的材料，例如粉末类材料或多孔材料，其中石墨烯材料是一种重要的可压缩材料。相比于不可压缩材料而言，可压缩材料的不同压缩率对自身的热导率与接触热阻均有重要的影响。近年来，随着可压缩材料在电子工业领域以及建筑行业等均有重要的应用，研究可压缩材料在不同压缩率下的热导率以及界面热阻具有重要的意义。
发明内容
基于此，本发明的目的在于，提供一种石墨烯材料热导率及界面热阻的测量装置，可实现材料在不同压缩率下的热导率及界面热阻的同步测量。
本发明的目的是通过以下技术方案实现的：一种石墨烯材料热导率及界面热阻的测量装置，包括上筒体、下筒体、上顶盖、压力机、水循环冷却单元、位移检测单元、加热单元、温度检测单元和数据处理单元；所述上筒体的底端与下筒体的顶端均为开口且相互连接；所述上筒体的内部为空心结构以形成上测试腔，所述上测试腔内设有上顶盖、第一金属块和测试样品，所述第一金属块的顶部和底部分别与上顶盖和测试样品接触；所述下筒体的内部为空心结构以形成下测试腔，所述下测试腔内设有支撑部和第二金属块，所述第二金属块固设于支撑部上，所述第二金属块的顶部与测试样品接触，底部设为肋片结构且悬空于下测试腔内；所述水循环冷却单元与下测试腔相连；所述压力机与上顶盖相连；所述位移检测单元包括相互电连接的位移传感器和位移采集卡，所述位移传感器与上顶盖相连；所述加热单元包括相互电连接的电源和电加热组件，所述电加热组件内嵌于第一金属块内；所述温度检测单元包括相互电连接的热电偶阵列和温度采集卡，所述热电偶阵列设于上测试腔和下测试腔内； 所述数据处理单元分别与压力机、位移采集卡和温度采集卡电连接。
本发明利用压力机对上顶盖施加压力，上顶盖将压力传递给测试样品，测试样品受力压缩，利用位移检测单元实时监控并采集测试样品在不同受力下的位移值，获得测试样品的压缩率。相对于现有技术，本发明可针对可压缩材料，在同一套装置上改变可压缩材料的压缩率，并实现可压缩材料在不同压缩率下的热导率与界面热阻的同步测量，且本发明也可用于测量不可压缩材料的热导率与界面热阻。此外，本发明装置具有设备简单，测量精度高，可靠性好，测量使用范围广的优点。
进一步地，所述上筒体的内壁设有滑槽，所述上顶盖安装于所述滑槽内并可沿着滑槽在上测试腔内上下滑动。
进一步地，所述第一金属块的侧壁设有与所述滑槽相对应的突起部。
进一步地，所述滑槽的深度为0.1～2mm。
进一步地，所述第一金属块的顶端设有凹槽，所述电加热组件设于所述凹槽内。
进一步地，所述水循环冷却单元包括水冷腔、两段冷却水管和循环水泵；所述水冷腔分别通过两段冷却水管与下测试腔连通，在连通部位处分别形成进水口和出水口；所述循环水泵设于其中一段冷却水管中。
进一步地，所述肋片结构包括若干根条形片，所述条形片的两端分别靠近进水口和出水口。
进一步地，所述上、下筒体的外壁和内壁之间均填充有保温材料层。
进一步地，所述上筒体和下筒体的侧壁沿轴向均设有若干个通孔，所述热电偶阵列设于所述若干个通孔内。
进一步地，所述热电偶阵列由若干个热电偶等间距排布而成。
进一步地，所述热电偶的间距为3～15mm。
本发明还提供了一种石墨烯材料热导率的测量方法，基于本发明所述的测量装置，包括以下步骤：
S1：将测试样品置于上、下两金属块之间，使用压力机对上顶盖施加一压力，上顶盖通过上金属块将压力传递给测试样品，使得测试样品受力压缩，通过位移检测单元测量测试样品的位移变化以获得其压缩率；
S2：开启水循环冷却单元和加热单元，对上、下筒体内部进行加热，通过温度检测单元测量得到上金属块、测试样品和下金属块沿筒体轴向的不同位置点所对应的温度数据，并计算上金属块的温度梯度dT
1/dx
1、测试样品的温度梯度dT
0/dx
0和下金属块的温度梯度dT
2/dx
2，利用公式Q
1＝-k
1·dT
1/dx
1计算经过上金属块的热流密度Q
1，利用公式Q
2＝-k
2·dT
2/dx
2计算经过 下金属块的热流密度Q
2，然后通过公式Q
0＝(Q
1+Q
2)/2计算经过测试样品的热流密度Q
0；其中，k
1和k
2分别是上金属块和下金属块的热导率；
S3：利用公式k
0＝-Q
0dx
0/dT
0计算测试样品在所述压缩率下的热导率k
0。
本发明还提供了一种石墨烯材料界面热阻的测量方法，基于本发明所述的测量装置，包括以下步骤：
S1：将测试样品置于上、下两金属块之间，使用压力机对上顶盖施加一压力，上顶盖通过上金属块将压力传递给测试样品，使得测试样品受力压缩，通过位移检测单元测量测试样品的位移变化以获得其压缩率；
S2：开启水循环冷却单元和加热单元，对上、下筒体内部进行加热，通过温度检测单元测量得到上金属块、测试样品和下金属块沿筒体轴向的不同位置点所对应的温度数据，并计算上金属块的温度梯度dT
1/dx
1和下金属块的温度梯度dT
2/dx
2，利用公式Q
1＝-k
1·dT
1/dx
1计算经过上金属块的热流密度Q
1，利用公式Q
2＝-k
2·dT
2/dx
2计算经过下金属块的热流密度Q
2，然后通过公式Q
0＝(Q
1+Q
2)/2计算经过测试样品的热流密度Q
0；其中，k
1和k
2分别是上金属块和下金属块的热导率；
S3：根据测得的上金属块、测试样品和下金属块沿筒体轴向的不同位置点所对应的温度数据画出温度分布曲线，并分别拟合出上金属块、测试样品和下金属块的温度与测试位置点的函数关系f1、f2和f3，利用线性插值，将测试样品与上金属块的接触界面位置值代入f1和f2获得对应的温度T
S1和T
S2，将测试样品与下金属块的接触界面位置值代入f2和f3获得对应的温度T
S2'和T
S3，并计算获得T
S1和T
S2的温差ΔT
上以及T
S2'和T
S3的温差ΔT
下，然后利用公式R
上＝ΔT
上/Q
0计算得到测试样品上界面在所述压缩率下的的界面热阻R
上，利用公式R
下＝ΔT
下/Q
0计算得到测试样品下界面在所述压缩率下的的界面热阻R
下。
为了更好地理解和实施，下面结合附图和实施例说明本发明。
图1为实施例的石墨烯材料热导率及界面热阻的测量装置的结构示意图。
图2为实施例的石墨烯材料热导率及界面热阻的测量装置的部分结构示意图。
图3为实施例的测试温度分布曲线以及温度与位置的函数关系拟合曲线。
请参阅图1和图2，本实施例的石墨烯材料热导率及界面热阻的测量装置，包括上筒体10、下筒体20、上顶盖30、压力机40、水循环冷却单元50、位移检测单元60、加热单元70、 温度检测单元80和数据处理单元90。
所述上筒体10的底端与下筒体20的顶端均为开口且相互连接，本实施例中，所述上筒体10与下筒体20的内外径尺寸均一致，所述上筒体10与下筒体20的外壁通过紧固扣101连接，使得两筒体内部紧密连接。在其它实施例中，所述上筒体10与下筒体20也可一体成型。所述上筒体10和下筒体20的外壁和内壁之间均为空心结构，内填充有低热导率的保温材料102。
所述上筒体10的内部为空心结构以形成上测试腔，所述上筒体10的内壁设有滑槽11，所述上顶盖30安装于滑槽11内并可沿着滑槽11在上测试腔内上下滑动。本实施例中，滑槽11为沿着上筒体10轴向方向的长条形滑槽，其深度不超过2mm，优选0.1～2mm。
所述上测试腔内设有第一金属块12和测试样品13，所述第一金属块12的顶部和底部分别与上顶盖30和测试样品13接触。优选的，所述第一金属块12为标准黄铜材料，其在升温过程拥有恒定的热导率值。进一步地，所述第一金属块12为圆柱体结构，其侧壁设有与滑槽11相对应的突起部，用以起到固定作用，其直径与上筒体10的内径相匹配，可沿着滑槽11套入上筒体10内。
所述下筒体20的内部为空心结构以形成下测试腔，所述下测试腔内设有支撑部21和第二金属块22，所述第二金属块22固设于支撑部21上，所述第二金属块22的顶部与测试样品13接触，底部设为肋片结构且悬空于下测试腔内。从而，所述测试样品13被夹紧在第一金属块12和第二金属块22之间。优选的，所述第二金属块22也为标准黄铜材料，其在升温过程拥有恒定的热导率值。进一步地，所述第二金属块22的上半部为圆柱体结构，其直径与上筒体10的内径相匹配，可套入下筒体10内。
所述水循环冷却单元50包括水冷腔51、两段冷却水管52和循环水泵53；所述水冷腔51分别通过两段冷却水管52与下测试腔连通，在连通部位处分别形成进水口和出水口；所述循环水泵53设于其中一段冷却水管中。水冷腔51用于提供一个稳定的冷源，循环水泵53用于保证冷却水的循环流动。优选的，水冷腔51的体积不能设置太小，需保证在长时间循环的过程中，其内部水的温度应接近于室温，其体积一般不小于10cm×10cm×10cm。进一步地，所述第二金属块22底部的肋片结构与水循环冷却回路连接，能够保证与循环水进行快速的热量交换，其包括若干根条形片，所述条形片的两端分别靠近所述进水口和出水口。
所述压力机40与上顶盖30相连，用以施加压力，上顶盖30将压力传递给测试样品13，使得测试样品13受力压缩变形产生位移变化。
所述位移检测单元60包括相互电连接的位移传感器61和位移采集卡62，所述位移传感器61与上顶盖30相连，用以实时监控测试样品13的位移变化。
所述加热单元70包括相互电连接的电源71和电加热组件72，所述电加热组件72内嵌于第一金属块12内。优选的，所述电加热组件72为一电加热片，所述第一金属块12顶端设有凹槽，所述电加热片设于该凹槽中。
所述温度检测单元80包括相互电连接的热电偶阵列81和温度采集卡82，所述热电偶阵列81设于上测试腔和下测试腔内，具体的，可以在上筒体10和下筒体20侧壁沿轴向设置若干个等间距排布的通孔，所述热电偶阵列81设于所述通孔内，并直接与第一金属块12、测试样品13以及第二金属块22接触，用以探测第一金属块12、测试样品13以及第二金属块22沿筒体轴向方向的不同位置的温度。本实施例中，所述热电偶阵列81由若干个热电偶等间距排布而成，其间距一般不小于3mm，优选3～15mm。
所述数据处理单元90可以为一计算机，其与压力机40、位移采集卡62和温度采集卡82分别电连接，以实时采集相应的数据。
本实施例还提供了一种石墨烯材料热导率和界面热阻的测量方法，基于上述测量装置，包括以下步骤：
(1)制备测试样品，测试样品可为多孔材质或粉末类材料，本实施例中，测试样品为石墨烯粉末材料，其为圆形片状结构，其横截面尺寸与第一金属块和第二金属块的横截面尺寸一致，测量其初始厚度L为30mm。
(2)用压力机对测试样品施加一压力F，并记录位移传感器输出的位移值ΔL，通过ΔL/L获得测试样品的体积压缩率。压力机所施加的压力不能过大，需保证测试样品在加力过程中不因结构破坏而发生变性，其值的大小与测试样品的材质有关，施力时由小到大，逐渐地从零升到设定值。压力大小可以通过压力机进行调节，从而获得不同压缩率下的测试样品，本实施例中，测试样品的位移值ΔL为6.0mm，压缩率ΔL/L为20％。
(3)开启循环水泵，使水冷腔充满室温的冷却水，并连通电加热片的电源进行电发热，电加热片的加热功率不能太大，需保证其升温温度不超过筒体的熔化温度，一般不超过180℃。
(4)待上测试腔和下测试腔内的热电偶阵列的输出温度达到稳定后，时间长度一般大于两个小时，利用温度采集卡记录上测试腔和下测试腔内不同位置点的温度值，其中，第一金属块、测试样品、第二金属块的不同测试位置点的温度值分别列于表1、表2和表3，以作为热源的电加热片位置为参考位置，x表示沿着筒体轴向向下的方向与该参考位置的距离。
表1第一金属块的不同测试位置点的温度值
| x 1(mm) | T 1(℃) |
| 10 | 76.7 |
| 20 | 76.6 |
| 30 | 76.3 |
| 40 | 75.8 |
表2测试样品的不同测试位置点的温度值
| x 0(mm) | T 0(℃) |
| 50 | 64.4 |
| 55 | 57.6 |
| 60 | 49.8 |
| 65 | 40.9 |
| 70 | 33.7 |
表3第二金属块的不同测试位置点的温度值
| x 2(mm) | T 2(℃) |
| 80 | 25.8 |
| 90 | 25.3 |
| 100 | 25.1 |
| 110 | 25.1 |
(5)通过表1中的测试数据计算得到经过第一金属块的平均温度梯度dT
1/dx
1为-30K/m，通过表3中的测试数据计算得到经过第二金属块的平均温度梯度dT
2/dx
2为-23K/m，本实施例中的第一、第二金属块均为标准黄铜材料，其热导率k为102W/(m·K)，利用公式Q
1＝-k·dT
1/dx
1计算经过第一金属块的热流密度Q
1为3060W/m
2，利用公式Q
2＝-k·dT
2/dx
2计算经过第二金属块的热流密度Q
2为2346W/m
2，再通过公式Q
0＝(Q
1+Q
2)/2计算经过测试样品的热流密度Q
0为2703W/m
2。
(6)通过表2中的测试数据计算得到经过测试样品的平均温度梯度dT
0/dx
0为-1535K/m，利用公式k
0＝-Q
0dx
0/dT
0计算得到测试样品在该压缩率下的热导率k
0为1.76W/(m·K)。
进一步地，根据表1、表2和表3的测试数据画出温度分布曲线，如图3中虚线所示，拟合出第一金属块、测试样品和第二金属块的温度与测试位置点的函数关系f1、f2和f3，如图3中实线所示，其分别为：f1：T＝-0.3x+77.1；f2：T＝-15.62x+143；f3：T＝-0.23x+27.51。通过线性插值，可获得测试样品与第一金属块、第二金属块的接触界面的温度值。本实施例中，测试样品的上界面与第一金属块底部界面接触，位置为45mm，将该位置值分别代入f2和f1，计算得到该位置对应的温度；测试样品的下界面与第二金属块顶部界面接触，位置为75mm，将该位置值分别代入f2和f3，计算得到该位置对应的温度。上述计算数据如表4所示。
表4界面位置对应的温度值
| x(mm) | T(℃) | |
| 第一金属块底部界面 | 45 | 75.75 |
| 测试样品上界面 | 45 | 72.71 |
| 测试样品下界面 | 75 | 25.85 |
| 第二金属块顶部界面 | 75 | 25.785 |
根据表4数据，计算测试样品上界面与第一金属块底部界面的界面温差ΔT
1为3.04℃，利用公式R
上＝ΔT
1/Q
0计算得到测试样品上界面的界面热阻R
上为1.12×10
-3K·m
2/W；计算测试样品下界面与第二金属块顶部界面的界面温差ΔT
2为0.065℃，利用公式R
下＝ΔT
2/Q
0计算得到测试样品下界面的界面热阻R
下为2.4×10
-6K·m
2/W。
相对于现有技术，本发明可针对可压缩材料，在同一套装置上改变可压缩材料的压缩率，并实现可压缩材料在不同压缩率下的热导率与界面热阻的同步测量，且本发明也可用于测量不可压缩材料的热导率与界面热阻。此外，本发明具有设备简单，操作方便、测量精度高，可靠性好，测量使用范围广的优点。
以上所述实施例仅表达了本发明的几种实施方式，其描述较为具体和详细，但并不能因此而理解为对发明专利范围的限制。应当指出的是，对于本领域的普通技术人员来说，在不脱离本发明构思的前提下，还可以做出若干变形和改进，这些都属于本发明的保护范围。
Claims (13)
- 一种石墨烯材料热导率及界面热阻的测量装置，其特征在于，包括上筒体、下筒体、上顶盖、压力机、水循环冷却单元、位移检测单元、加热单元、温度检测单元和数据处理单元；所述上筒体的底端与下筒体的顶端均为开口且相互连接；所述上筒体的内部为空心结构以形成上测试腔，所述上测试腔内设有上顶盖、第一金属块和测试样品，所述第一金属块的顶部和底部分别与上顶盖和测试样品接触；所述下筒体的内部为空心结构以形成下测试腔，所述下测试腔内设有支撑部和第二金属块，所述第二金属块固设于支撑部上，所述第二金属块的顶部与测试样品接触，底部设为肋片结构且悬空于下测试腔内；所述水循环冷却单元与下测试腔相连；所述压力机与上顶盖相连；所述位移检测单元包括相互电连接的位移传感器和位移采集卡，所述位移传感器与上顶盖相连；所述加热单元包括相互电连接的电源和电加热组件，所述电加热组件内嵌于第一金属块内；所述温度检测单元包括相互电连接的热电偶阵列和温度采集卡，所述热电偶阵列设于上测试腔和下测试腔内；所述数据处理单元分别与压力机、位移采集卡和温度采集卡电连接。
- 根据权利要求1所述的石墨烯材料热导率及界面热阻的测量装置，其特征在于，所述上筒体的内壁设有滑槽，所述上顶盖安装于所述滑槽内并可沿着滑槽在上测试腔内上下滑动。
- 根据权利要求2所述的石墨烯材料热导率及界面热阻的测量装置，其特征在于，所述第一金属块的侧壁设有与所述滑槽相对应的突起部。
- 根据权利要求2所述的石墨烯材料热导率及界面热阻的测量装置，其特征在于，所述滑槽的深度为0.1～2mm。
- 根据权利要求1所述的石墨烯材料热导率及界面热阻的测量装置，其特征在于，所述第一金属块的顶端设有凹槽，所述电加热组件设于所述凹槽内。
- 根据权利要求1所述的石墨烯材料热导率及界面热阻的测量装置，其特征在于，所述水循环冷却单元包括水冷腔、两段冷却水管和循环水泵；所述水冷腔分别通过两段冷却水管与下测试腔连通，在连通部位处分别形成进水口和出水口；所述循环水泵设于其中一段冷却水管中。
- 根据权利要求6所述的石墨烯材料热导率及界面热阻的测量装置，其特征在于，所述肋片结构包括若干根条形片，所述条形片的两端分别靠近进水口和出水口。
- 根据权利要求1所述的石墨烯材料热导率及界面热阻的测量装置，其特征在于，所述上、下筒体的外壁和内壁之间均填充有保温材料层。
- 根据权利要求1所述的石墨烯材料热导率及界面热阻的测量装置，其特征在于，所述 上筒体和下筒体的侧壁沿轴向均设有若干个通孔，所述热电偶阵列设于所述若干个通孔内。
- 根据权利要求1所述的石墨烯材料热导率及界面热阻的测量装置，其特征在于，所述热电偶阵列由若干个热电偶等间距排布而成。
- 根据权利要求10所述的石墨烯材料热导率及界面热阻的测量装置，其特征在于，所述热电偶的间距为3～15mm。
- 一种石墨烯材料热导率的测量方法，其特征在于，基于权利要求1～11任一所述的测量装置，包括以下步骤：S1：将测试样品置于上、下两金属块之间，使用压力机对上顶盖施加一压力，上顶盖通过上金属块将压力传递给测试样品，使得测试样品受力压缩，通过位移检测单元测量测试样品的位移变化以获得其压缩率；S2：开启水循环冷却单元和加热单元，对上、下筒体内部进行加热，通过温度检测单元测量得到上金属块、测试样品和下金属块沿筒体轴向的不同位置点所对应的温度数据，并计算上金属块的温度梯度dT 1/dx 1、测试样品的温度梯度dT 0/dx 0和下金属块的温度梯度dT 2/dx 2，利用公式Q 1＝-k 1·dT 1/dx 1计算经过上金属块的热流密度Q 1，利用公式Q 2＝-k 2·dT 2/dx 2计算经过下金属块的热流密度Q 2，然后通过公式Q 0＝(Q 1+Q 2)/2计算经过测试样品的热流密度Q 0；其中，k 1和k 2分别是上金属块和下金属块的热导率；S3：利用公式k 0＝-Q 0dx 0/dT 0计算测试样品在所述压缩率下的热导率k 0。
- 一种石墨烯材料界面热阻的测量方法，其特征在于，基于权利要求1～11任一所述的测量装置，包括以下步骤：S1：将测试样品置于上、下两金属块之间，使用压力机对上顶盖施加一压力，上顶盖通过上金属块将压力传递给测试样品，使得测试样品受力压缩，通过位移检测单元测量测试样品的位移变化以获得其压缩率；S2：开启水循环冷却单元和加热单元，对上、下筒体内部进行加热，通过温度检测单元测量得到上金属块、测试样品和下金属块沿筒体轴向的不同位置点所对应的温度数据，并计算上金属块的温度梯度dT 1/dx 1和下金属块的温度梯度dT 2/dx 2，利用公式Q 1＝-k 1·dT 1/dx 1计算经过上金属块的热流密度Q 1，利用公式Q 2＝-k 2·dT 2/dx 2计算经过下金属块的热流密度Q 2，然后通过公式Q 0＝(Q 1+Q 2)/2计算经过测试样品的热流密度Q 0；其中，k 1和k 2分别是上金属块和下金属块的热导率；S3：根据测得的上金属块、测试样品和下金属块沿筒体轴向的不同位置点所对应的温度数据画出温度分布曲线，并分别拟合出上金属块、测试样品和下金属块的温度与测试位置点的函数关系f1、f2和f3，利用线性插值，将测试样品与上金属块的接触界面位置值代入f1和 f2获得对应的温度T S1和T S2，将测试样品与下金属块的接触界面位置值代入f2和f3获得对应的温度T S2'和T S3，并计算获得T S1和T S2的温差ΔT 上以及T S2'和T S3的温差ΔT 下，然后利用公式R 上＝ΔT 上/Q 0计算得到测试样品上界面在所述压缩率下的的界面热阻R 上，利用公式R 下＝ΔT 下/Q 0计算得到测试样品下界面在所述压缩率下的的界面热阻R 下。
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