CN101949873A - Device for measuring solid material heat conductivity - Google Patents
Device for measuring solid material heat conductivity Download PDFInfo
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- CN101949873A CN101949873A CN 201010502257 CN201010502257A CN101949873A CN 101949873 A CN101949873 A CN 101949873A CN 201010502257 CN201010502257 CN 201010502257 CN 201010502257 A CN201010502257 A CN 201010502257A CN 101949873 A CN101949873 A CN 101949873A
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Abstract
一种固体材料导热系数的测量装置，其中包括密闭的真空腔，真空腔通过抽气管与外部抽真空装置相连；设置在真空腔内的加热源；分别紧贴所述加热源两侧的第一金属块和第二金属块；第三金属块和第四金属块，所述第一金属块与第三金属块之间形成一置物空间，所述第二金属块与第四金属块之间形成另一置物空间，置物空间用来放置待测量固体材料；设置在第三块金属块和第四块金属块外侧的冷却装置；温度测量器，所述温度测量器设置在各金属块上，用来测量金属块的温度。本发明的装置能更精确地获得测量值，可提高最终测量精度。A device for measuring the thermal conductivity of solid materials, which includes a closed vacuum chamber connected to an external vacuum device through an exhaust pipe; a heating source arranged in the vacuum chamber; A metal block and a second metal block; a third metal block and a fourth metal block, a storage space is formed between the first metal block and the third metal block, and a storage space is formed between the second metal block and the fourth metal block Another storage space, the storage space is used to place the solid material to be measured; the cooling device arranged on the outside of the third metal block and the fourth metal block; the temperature measuring device, the temperature measuring device is arranged on each metal block, with to measure the temperature of the metal block. The device of the invention can obtain measurement values more accurately and can improve the final measurement precision.
Description
Technical field
The present invention relates to a kind of measurement mechanism of coefficient of heat conductivity, particularly measures the measurement mechanism of the coefficient of heat conductivity of the solid material with bad coefficient of heat conductivity.
Background technology
The coefficient of heat conductivity of material is an important parameter index of research material physical property, in scientific research, and teaching, departments such as production all require the coefficient of heat conductivity of material is predicted or surveyed.Coefficient of heat conductivity is the physical quantity of reflection material thermal conductivity energy, it is not only the foundation of the calorifics of evaluating material, and be the design considerations of material when using, so in scientific experiment and engineering, the thermal Conductivity Determination of material is become the key of exploitation new material.
The coefficient of heat conductivity of measuring material at present mainly contains following three kinds of methods:
One, the laser method that shines.What this method adopted is the transient state method, principle is that beam of laser is beaten at the sample upper surface, temperature variation with infrared detector test lower surface, the actual data that record are thermal diffusivities of sample, by with the density that obtains sample more simultaneously and the specific heat of standard model, can calculate the coefficient of heat conductivity of sample by formula.This method advantage is to measure fast, adopts the noncontact method, is fit to high temperature, the sample of high heat conduction, but be not suitable for sandwich construction, coating, foam, liquid, anisotropic material etc.Reason be laser method test be thermal diffusivity, mathematic(al) mode is based upon on the basis of isotropic material.In addition, also need to record density, could convert and be coefficient of heat conductivity, increased the source of error with additive method.About relevant patent of the method or document is to introduce like this, as: " measuring the coefficient of heat conductivity of graphite material with laser pulse method ", (Yang Hongli, Gansu metallurgy, 1998 1 phase 39-44 pages or leaves), discussed and passed through to survey the graphite material coefficient of heat conductivity, and laser pulse method has been surveyed graphite material coefficient of heat conductivity instrument and equipment carried out debugging and measured data analysis with laser pulse method.
What two, coefficient of heat conductivity method (Hot Disk(TPS technology)) this method adopted is the transient state method equally, and principle is to utilize the thermal resistance material---nickel is made the probe on a plane, simultaneously as thermal source and temperature sensor.The relation of the thermal resistivity of nickel and temperature and resistance is linear, promptly can know the loss of heat by understanding changes in resistance, thus the heat conductivility of reflection sample.By the response time of record temperature and probe, these characteristics of material can be calculated.Can directly obtain coefficient of heat conductivity and thermal diffusion coefficient by mathematical model, both ratio obtains volume specific heat.Advantage is quick, convenient, specimen preparation especially, can be used for original position/single face test, be applicable to polytype samples such as solid, powder, liquid, coating, cellular material, but be subjected to the restriction of detecting head surface coating, temperature range can only arrive 700 ° of C, and the probe cost is higher, and design is complicated, can not effectively promote.About relevant patent of the method or document is to introduce like this: No. the 87213622nd, the Chinese patent of announcing " intellectual hot line thermal conductivity coefficient measurement instrument " on July 27th, 1988, method according to the Hot Wire Technique for Measuring material thermal conductivity is the thermal resistance wire that is made of nickel chromium triangle, be arranged in the tested material, energising heating then, take out the temperature signal of tested material by being welded in thermopair on the thermal resistance wire in the tested material, input to signal Processing then, finally record the coefficient of heat conductivity of material.
Three, temperature gradient method.This method is that testing sample is placed between a thermal source and the cryogenic refrigerating unit, measures the thermograde that forms therebetween, thereby calculates the coefficient of heat conductivity of material.
Under the perfect condition, all heats of thermal source are passed to the cryogenic refrigeration end by testing sample, but in fact inevitably some heat sheds from other direction, thereby cause measuring error, reduce the accuracy of measuring.Therefore, the measuring accuracy of this kind method depends primarily on and how to reduce heat and shed from other direction in transmittance process, generally can use thermal insulation material as heat insulation layer in order to thermal source is hedged off from the outer world, reduce the loss of heat as far as possible, but still have the part heat and outwards conduct.About relevant patent of the method or document is to introduce like this: " heat conducting coefficient measuring device ", the Chinese patent application of on August 24th, 2005 bulletin numbers 200410015458.0, according to the thermograde principle, utilize pumped vacuum systems that internal gas is discharged, utilize the radially athermanous characteristic of carbon nano-tube again, make that heat can only be to the predetermined direction transmission.The China Patent No. 200720063809.4 of " a kind of good conductor thermal conductivity coefficient measurement instrument " on June 11st, 2008 bulletin and for example, its device is that well heater is equipped with in the hot junction of detected materials, cold junction is close to cooling device, and available setting adjusting knob is in order to control thermal source or cold junction temperature.
Given this, the present invention is directed to the deficiencies in the prior art, design a kind of new solid material heat conductivity measuring device, overcome in the said method that error is big, complicated operation, accuracy is low and shortcoming such as cost height.
Summary of the invention
The purpose of this invention is to provide a kind of easy to operate, low-cost, good stability, thermal insulation is good, can accurately measure the solid material heat conductivity measuring device of solid or gluey sample, is used for the coefficient of heat conductivity of solid material is accurately measured.
The invention provides a kind of measurement mechanism of solid material coefficient of heat conductivity, comprising the enclosed vacuum chamber, vacuum chamber links to each other with outside vacuum extractor by exhaust tube; Be arranged on the heating source in the vacuum chamber; First derby and second derby of being close to described heating source both sides respectively; The 3rd derby and the 4th derby form a material-putting space between described first derby and the 3rd derby, form another material-putting space between described second derby and the 4th derby, and material-putting space is used for placing solid material to be measured; Be arranged on the cooling device in the 3rd block of derby and the 4th derby outside; Temperature meter, described temperature meter is arranged on each derby, is used for measuring the temperature of derby.
The invention provides a kind of measurement mechanism of solid material coefficient of heat conductivity, the vacuum chamber side is provided with opening, and solid material to be measured is placed in the material-putting space by opening, and opening is sealed by side cover.
The invention provides a kind of measurement mechanism of solid material coefficient of heat conductivity, temperature meter is by output lead, and the data acquisition system (DAS) outer with vacuum chamber is connected.
The invention provides a kind of measurement mechanism of solid material coefficient of heat conductivity, heating source is an electrical-heating source, further comprises: micarex or mica sheet and twine thereon resistive heater, and as the sheet metal of support protecting sheathing; Heating source is skeleton and insulation course with micarex or mica sheet, and sheet metal is galvanized sheet or corrosion resistant plate, and described sheet metal is tabular, sheet, cylindric, coniform, tubular, circle shape.
The invention provides a kind of measurement mechanism of solid material coefficient of heat conductivity, wherein derby is surperficial polished.
The invention provides a kind of measurement mechanism of solid material coefficient of heat conductivity, wherein the surface-coated of derby has antiradiation coating.
The invention provides a kind of measurement mechanism of solid material coefficient of heat conductivity, the stationary installation with thermal insulation material is made is fastened on thermal source, copper billet, cooling device in the vacuum chamber, and thermal insulation material is complex magnesium aluminum silicate compound, pottery or aerogel material.
The invention provides a kind of measurement mechanism of solid material coefficient of heat conductivity, cooling device is one or more in semiconductor cooling device, fan or the cooling water circulation unit.
The invention provides a kind of measurement mechanism of solid material coefficient of heat conductivity, each derby has identical cross-sectional area.
The invention provides a kind of measurement mechanism of solid material coefficient of heat conductivity, temperature meter is thermoelectric corner or digital temperature sensor.
Device of the present invention is the center with the thermal source, is up and down symmetric form design fully, make that heat can be balanced to the two ends vertical diffusion that has cooling device.Thereby can avoid, and more accurate acquisition measured value from monolateral or diffusion all around.Because of this device is placed in the vacuum system, utilize pumped vacuum systems that internal gas is discharged again, can get rid of the harmful effect of gas, can improve final measuring accuracy.
The present invention compared with prior art, have easy to operate, the advantage that cost is low, good stability, thermal insulation is good, test speed is fast, the coefficient of heat conductivity scope of measurement is wide, applicable to the accurate measurement of the coefficient of heat conductivity of solid or gluey sample.
Description of drawings
Fig. 1 is the schematic perspective view of solid material heat conductivity measuring device in the example of the present invention.
Fig. 2 is the inner structure synoptic diagram of solid material heat conductivity measuring device in the example of the present invention.
Fig. 3 is the derby schematic perspective view of solid material heat conductivity measuring device in the example of the present invention.
Fig. 4 is the cooling device schematic perspective view of solid material heat conductivity measuring device in the example of the present invention.
Fig. 5 is the structural representation of the heating plate of solid material heat conductivity measuring device in the example of the present invention.
Fig. 6 is the measuring system synoptic diagram of solid material heat conductivity measuring device in the example of the present invention.
Fig. 7 is the sample testing data and curves figure of solid material coefficient of heat conductivity tester in the example.
Embodiment
Below in conjunction with Figure of description and embodiment the present invention is described in further detail:
See also Fig. 1, the schematic perspective view of the measurement mechanism of solid material coefficient of heat conductivity in the example promptly of the present invention.This device comprises, vacuum chamber 1, vacuum chamber 1 are a cylindrical seal container, but it has a closed vacuum cavity 1 upper shed A(and consults Fig. 2) side cover 2, this side cover 2 can be opened or be closed, so that testing sample is put into vacuum chamber 1 by opening A or take out from vacuum chamber 1.In addition, an end of an exhaust tube 3 extends to the inner space of vacuum chamber 1, and the other end links to each other with vacuum extractor (figure does not show).Can will be evacuated in the vacuum chamber 1, get rid of the harmful effect of gas, make that heat can only be to the predetermined direction transmission.And utilize ZJ-32 type ultrahigh vacuum to regulate (B-A) nude gauge and survey vacuum tightness in the vacuum chamber 1.
Seeing also Fig. 2, is the inner structure synoptic diagram of solid material heat conductivity measuring device in the example of the present invention.In vacuum cavity 1, comprise heating source 4, be close to first copper billet 5 and second copper billet 6 of heating source 4 both sides respectively; Form the material-putting space 9' that places detected sample 9 between the 3rd copper billet 7 and the 4th copper billet 8, the first copper billets 5 and the 3rd copper billet 7, form the material-putting space 10 ' of placing another detected sample 10 between second copper billet 6 and the 4th copper billet 8; Respectively be provided with cooling device 11,12 as cooling device in the 3rd copper billet 7 and the 4th copper billet 8 outside.On first copper billet to the, four copper billets 5,6,7,8, respectively be provided with temperature meter 13, be used for measuring the temperature of derby.
Consult the structural representation of Fig. 5 for the heating plate of solid material heat conductivity measuring device in this example.Heating source 4 in vacuum chamber 1 is to twine insulating property and all good mica sheet 22 of resistance to elevated temperatures by resistive heater 21, and auxilliary diameter is that the circle shape copper billet of 3cm is made supportive protection.As shown in Figure 5, mica sheet 22 is cut into disk, thereon around resistive heater 21, the diameter of electric cloudy heating wire is 0.5mm.After said structure was made into, again with on circle mica sheet 22 folders, mica sheet thickness was 1mm, with on the copper coin folder, seals admittedly with epoxy resin at last more up and down.Heating plate adopts constant voltage or constant power.
Wherein first copper billet to the, four copper billets 5,6,7,8 are 3cm with the floorage diameter all, and height is the cylindrical copper billet of 5mm.Detected sample the 9, the 10th, floorage diameter are 3cm, and height is the cylindrical solid material of 1cm.Wherein as the semiconductor cooling device of cooling device, its used dimensions is the rectangular parallelepiped of long 3 cm * wide 3 cm * high 1 cm.
Consult the copper billet schematic perspective view of Fig. 3 for solid material heat conductivity measuring device in this example.Copper billet among Fig. 3 is in first copper billet to the, four copper billets, is coated with antiradiation coating on its side surface 14, can reduce the thermal loss that causes because of heat radiation.Upper and lower surperficial 15, the 16 process polishing technologies of copper billet are handled, and make that upper and lower surperficial 15,16 of copper billet are Paint Gloss, and are tightr when contacting with other assembly, reduce interface resistance.
Fig. 4 is the schematic perspective view of the cooling device of solid material heat conductivity measuring device in this example.Cooling device 11 can adopt semiconductor cooling device and fan to form easy cooling system, bonds with silica gel between semiconductor and the fan.Two ends temperature in the vacuum cavity is reduced, and reduced volume greatly.
As shown in Figure 2, be closely to paste between each assembly wherein, 11 upper surface 17 is close to the lower surface of upper end in the vacuum cavity.The lower surface of cooling device 12 tight 18 is pasting the upper surface of lower end in the vacuum cavity.
When test, open the side cover 2 of vacuum cavity 1, two identical detected samples 9,10 are placed first copper billet 5 in the vacuum cavity 1 and the material-putting space 10 ' between the material-putting space 9 ' between the 3rd copper billet 7 and second copper billet 6 and the 4th copper billet 8 respectively by opening A.Cover side cover 2, open vacuum extractor, the air in the vacuum chamber 1 is extracted into 1 * 10 by exhaust tube 3
-4～1 * 10
-5The vacuum tightness of pa scope.
In addition, the sample place is pressed close in a side at first copper billet to the, four copper billets 5,6,7,8, the probe of temperature meter 13 is set, when heat transfer reaches steady state (SS), measured temperature is respectively between T1, T2, T3, T4. first copper billet 5 this moment and the 3rd copper billet 7, should be between second copper billet 6 and the 48 equidistantly, and be about the testing sample thickness d.
Consult the measuring system synoptic diagram of Fig. 6 for solid material heat conductivity measuring device in the example of the present invention.Heating source 4 in vacuum chamber 1, cooling device 11 and temperature meter 13 send controller 22 to by shielded cable bus 21.Controller 22 can according to temperature meter 13 measured datas on its display panel 23, directly show estimate temperature and for and the real power numerical value of cooling device 11, heating source 4.Also can carry out function by the button on the controller 24 this moment and switch, and utilize the constant of button 24 input vacuum system heat-transfer devices, controller will root a tree name input value, calculates and show the coefficient of heat conductivity of tested sample.
Can effectively distinguish the sample of different coefficient of heat conductivity according to our design example device, the data that institute's specimen obtains as shown in Figure 7.Accurate by this device of observation curve data on some levels, but specifically at highly heat-conductive material such as diamond, silver etc., and low thermal conductivity such as vulcanized rubber, crown glass etc., in the actual measurement process, still there is error, the analysis of causes is as follows:
1, when the sample coefficient of heat conductivity is very big, copper billet plays an important role with the thermal potential difference that contacts of detected sample, and we have done contrast with silica gel connection copper billet and sample herein.
2, when the sample coefficient of heat conductivity is very little, thermal source contacts heat leakage with air-flow and plays a major role.
Heat radiation has three kinds of forms:
(1) conduction, contact area is big, and it is just many to pass the heat of walking.
(2) radiation, heat with the form of light (mainly being the far infrared that human eye is not seen) to around transferring heat energy, this part ratio that accounts in heat radiation is little.
(3) heat loss through convection that is produced by circulation of air, this is main in central heat sink.The cross-ventilation heat radiation divides forced draft and natural ventilation again, and the mould heat radiation belongs to natural ventilation.In most cases belong to laminar flow natural ventilation heat radiation again.
U, I are respectively the voltage and current of supplying with thermal source in the above-mentioned formula, and h1, h2 refer to the height of upper and lower sample respectively, and R is the radius of testing sample, and α, β are the error correction coefficient, and λ is a coefficient of heat conductivity.Can make such hypothesis: because heating source 4 power of our usefulness are certain, so only relevant with the degree of roughness on surface, we are decided to be a constant to it for the time being. for different samples, the temperature variation of thermal source is little, therefore also be approximately constant (=8.11993 ,=34.19589).
The measurement mechanism of the solid material coefficient of heat conductivity in example of the present invention also can adopt other modes, detected sample put in the material-putting space, and the side cover 2 that need on vacuum chamber 1, not offer opening A and seal this opening A.
Heating source also can be the electrical-heating source of other structures.The derby that is used for supportive protection in the heating plate 4 in this example can be a galvanized sheet, corrosion resistant plate etc., or copper billet etc., and that its shape can be made is tabular, sheet, cylindric, circle shape etc.
In the foregoing description, be the center successively with the heating source with heating source, first to the 4th derby, cooling device, copper billet, cooling device be symmetry arrangement up and down, and the stationary installation (not shown) made from thermal insulation material is anchored in the vacuum chamber.Insulating material can be as complex magnesium aluminum silicate compound, pottery, aerogel etc.
Cooling device also can adopt one or more in semiconductor cooling device, fan, the cooling water circulation unit etc.
First derby in this example, second derby, the 3rd derby and the 4th derby and detected sample all have identical cross-sectional area, can be that copper billet or other metals are made.
Temperature meter in this example can be thermoelectric corner or digital temperature sensor.
The device of present embodiment is the center with the thermal source, is up and down symmetric form design fully, make that heat can be balanced to the two ends vertical diffusion that has cooling device.Thereby can avoid, and more accurate acquisition measured value from monolateral or diffusion all around.The copper billet side surface is covered with antiradiation coating in this device, can reduce the thermal loss that causes because of heat radiation; Because of this device is placed in the vacuum system, utilize pumped vacuum systems that internal gas is discharged again, can get rid of the harmful effect of gas, make heat can improve final measuring accuracy to the predetermined direction transmission.This device can be measured the coefficient of heat conductivity from the thermal insulation material to the metal material at short notice, and the scope of the coefficient of heat conductivity of its measurement is 0.01～400Wm
-1K
-1, and the uncertainty of measured coefficient of heat conductivity is in 3%.
Being preferred embodiment of the present invention only in sum, is not to be used for limiting practical range of the present invention.Be that all equivalences of doing according to the content of the present patent application claim change and modification, all should belong to technology category of the present invention.
Claims (10)
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| CN104483349A (en) * | 2014-12-19 | 2015-04-01 | 山东大学 | System and method for measuring heat exchange characteristics of tube bundle |
| CN105303936A (en) * | 2014-06-25 | 2016-02-03 | 华北电力大学（保定） | Portable multifunctional heat transfer experiment table |
| CN106153672A (en) * | 2016-06-08 | 2016-11-23 | 东南大学 | Voluminous powder material thermal conductivity measurement apparatus based on one-dimensional heat conduction principle and method |
| CN106682279A (en) * | 2016-12-07 | 2017-05-17 | 中国电子科技集团公司第五十五研究所 | Microelectronic device nanometer interface bonding layer thermal resistance analyzing method |
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| CN111060555A (en) * | 2019-12-30 | 2020-04-24 | 武汉大学 | Method and device for measuring thermal conductivity and thermal diffusivity of thin film material under strain |
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| CN110702731A (en) * | 2019-10-30 | 2020-01-17 | 京正信用评估有限公司 | Method for measuring comprehensive heat transfer coefficient or energy efficiency coefficient of object, system and application thereof |
| CN111060555A (en) * | 2019-12-30 | 2020-04-24 | 武汉大学 | Method and device for measuring thermal conductivity and thermal diffusivity of thin film material under strain |
| WO2021217932A1 (en) * | 2020-04-30 | 2021-11-04 | 国联汽车动力电池研究院有限责任公司 | Method and apparatus for measuring thermal conductivity coefficient of lithium-ion battery cells |
| CN113960105A (en) * | 2020-07-21 | 2022-01-21 | Oppo广东移动通信有限公司 | A detection device, detection method and application of heat capacity |
| CN113960106A (en) * | 2020-07-21 | 2022-01-21 | Oppo广东移动通信有限公司 | A detection device, detection method and application of heat capacity |
| WO2023015410A1 (en) * | 2021-08-09 | 2023-02-16 | Dupont (China) Research & Development And Management Co., Ltd. | Device and method for determining thermal conductivity of insulative cushion under simulated thermal runaway |
| CN114386286A (en) * | 2022-01-18 | 2022-04-22 | 上海交通大学 | Calculation method and system for thermal conductivity of main insulation based on high thermal conductivity mica tape |
| CN114386286B (en) * | 2022-01-18 | 2023-08-08 | 上海交通大学 | Main insulation heat conductivity coefficient calculation method and system based on high heat conductivity mica tape manufacturing |
| CN114894836A (en) * | 2022-04-25 | 2022-08-12 | 武汉钢铁有限公司 | Device and method for detecting heat conductivity coefficient of brittle layer of blast furnace hearth carbon brick |
| CN114910510A (en) * | 2022-06-06 | 2022-08-16 | 重庆川仪调节阀有限公司 | Device and method for measuring heat transfer effect of valve body of liquid hydrogen valve |
| CN117110370A (en) * | 2023-10-20 | 2023-11-24 | 江苏矽时代材料科技有限公司 | Low-error silica gel heat conductivity testing device |
| CN117110370B (en) * | 2023-10-20 | 2023-12-29 | 江苏矽时代材料科技有限公司 | Low-error silica gel heat conductivity testing device |
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