CN106706701A - Device for measuring powder heat conductivity coefficient based on transient plane heat source method - Google Patents
Device for measuring powder heat conductivity coefficient based on transient plane heat source method Download PDFInfo
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- CN106706701A CN106706701A CN201611226319.1A CN201611226319A CN106706701A CN 106706701 A CN106706701 A CN 106706701A CN 201611226319 A CN201611226319 A CN 201611226319A CN 106706701 A CN106706701 A CN 106706701A
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- 239000000843 powder Substances 0.000 title claims abstract description 52
- 238000000034 method Methods 0.000 title claims abstract description 42
- 230000001052 transient effect Effects 0.000 title claims abstract description 22
- 239000000523 sample Substances 0.000 claims abstract description 247
- 238000012360 testing method Methods 0.000 claims abstract description 117
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 74
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 37
- 239000007787 solid Substances 0.000 claims description 134
- 239000000463 material Substances 0.000 claims description 25
- 239000003463 adsorbent Substances 0.000 claims description 13
- 238000005086 pumping Methods 0.000 claims description 13
- 229910000831 Steel Inorganic materials 0.000 claims description 7
- 239000010959 steel Substances 0.000 claims description 7
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 3
- 229910052802 copper Inorganic materials 0.000 claims description 3
- 239000010949 copper Substances 0.000 claims description 3
- 239000011810 insulating material Substances 0.000 abstract description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 24
- 238000005259 measurement Methods 0.000 description 20
- 229910052757 nitrogen Inorganic materials 0.000 description 12
- 238000012546 transfer Methods 0.000 description 12
- 239000010410 layer Substances 0.000 description 10
- 238000012544 monitoring process Methods 0.000 description 10
- 238000004458 analytical method Methods 0.000 description 9
- 238000010438 heat treatment Methods 0.000 description 9
- 238000010276 construction Methods 0.000 description 8
- 238000009434 installation Methods 0.000 description 8
- 238000002955 isolation Methods 0.000 description 8
- 239000007788 liquid Substances 0.000 description 8
- 238000012827 research and development Methods 0.000 description 8
- 239000004519 grease Substances 0.000 description 7
- 229920001296 polysiloxane Polymers 0.000 description 7
- 229910052738 indium Inorganic materials 0.000 description 6
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 6
- 230000005540 biological transmission Effects 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 239000003921 oil Substances 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 239000010963 304 stainless steel Substances 0.000 description 2
- 229910000589 SAE 304 stainless steel Inorganic materials 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 1
- 239000008358 core component Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 235000019362 perlite Nutrition 0.000 description 1
- 239000010451 perlite Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920003223 poly(pyromellitimide-1,4-diphenyl ether) Polymers 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 238000012552 review Methods 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- 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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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Materials Using Thermal Means (AREA)
Abstract
The invention discloses a device for measuring powder heat conductivity coefficient based on a transient plane heat source method, which comprises: a vacuum vessel and a constant temperature system; a vacuum container is arranged in the constant temperature system; the vacuum container comprises a vacuum container cylinder, a vacuum container upper flange and a vacuumizing pipe; the vacuum container barrel comprises a powder sample rack, a test probe, a PT100 platinum resistance thermometer and a fixing ring; compared with the traditional method for measuring the powder heat conductivity coefficient, the device for measuring the powder heat conductivity coefficient based on the transient plane heat source method can quickly obtain the heat conductivity coefficient of the powder heat-insulating material; the device can measure the heat conductivity coefficient of the powder heat-insulating material at a certain temperature and a certain vacuum degree, the test temperature range is 30K-473K, and the vacuum degree range is 10‑3Pa‑1atm。
Description
Technical field
The invention belongs to the hot physical property measurement technical field of solid powder, and in particular to a kind of to be surveyed based on Adsorbent By Using Transient Plane Source Technique
Measure the device of powder thermal conductivity factor.
Background technology
Powder isolation material mainly including expanded perlite, aeroge and hollow glass micropearl etc., with density is small, heat conduction
Coefficient is low, chemical stability is high, good flame resistance the advantages of, be the important heat-insulating material of a class.If powder isolation material is placed in
Under vacuum environment, its heat-insulating property can lift ten times, with very big application value.Thermal conductivity factor is the important heat of heat-insulating material
Physical parameter, therefore, thermal conductivity factor of the measurement powder isolation material under uniform temperature, certain vacuum degree is exhausted for exploring powder
Thermal gauge rule tool is of great significance.
The measuring method of thermal conductivity factor is generally divided into steady state method and Transient Method, and steady state method is with Fourier one dimensional heat transfer law
Theoretical foundation, it is desirable to which the heat transfer inside testing sample reaches the state of stabilization, even if setting up one inside testing sample surely
Fixed Temperature Distribution, by determining heating power, heat transfer sectional area and thermograde come calculation of thermal conductivity.This method tool
Have clear principle, can Accurate Determining testing sample thermal conductivity factor, it is adaptable to the advantages of warm area wide is measured, but steady state method, test
Time it is long (difference of thermal conductivity factor and test environment according to testing sample, the testing time typically a few houres, ten a few houres,
Tens hours), and to measuring environment (temperature control, the shape of sample such as in the adiabatic condition of measuring system, measurement process
Shape size etc.) requirement it is more harsh.Transient Method, is divided into heat-pole method, Hot-strip Method and hot plate method (i.e. Adsorbent By Using Transient Plane Source Technique) again,
The Temperature Distribution time to time change of sample in this kind of method measurement process, according to the Unsteady Heat Transfer differential equation, by measurement
Temperature changes with time relation on sample, just can calculate the thermal conductivity factor of testing sample.Transient Method takes short, and response is fast,
It is widely used.
Gustafsson in 1991 invented Adsorbent By Using Transient Plane Source Technique (Transient Plane Source Method,
TPS) the thermal conductivity factor of test material, its method of testing is published in《Scientific instrument are summarized》The 797-804 pages of 3 phases of volume 62 in 1991
(Gustafsson S E.Transient plane source techniques for thermal conductivity
and thermal diffusivity measurements of solid materials[J].Review of
scientific instruments,1991,62(3):797-804.).The core component of Adsorbent By Using Transient Plane Source Technique be it is a kind of both
Can be used as thermal source, again can be used as the probe of temperature sensor, one 10 μ m-thick of the probe are with continuous double-stranded
Metallic nickel thin slice is made, and nickel thin slice is protected by very thin (every the is 0.25 μ m-thick) insulating protective layer (Kapton) of two panels
Shield, similar to sandwich structure.During test, first, probe is clamped in the middle of two pieces of testing samples of identical material.Then,
According to the general heat transfer property of testing sample, to the power that probe input is constant within the regular hour, with probe temperature
Increase, heat is transmitted to testing sample, while resistance of popping one's head in accordingly increases, the increased speed of probe temperature depends on testing sample
Rate of heat transfer.During this period of time, the voltage at probe two ends is recorded.Due to power invariability, by two ends of popping one's head in
Voltage change can just extrapolate the change of probe resistance.Finally, it is known that voltage changes with time, temperature changes with time and
Heat flow, can just calculate the thermal conductivity factor and volumetric heat capacity of detected materials.Powder sample is measured with Adsorbent By Using Transient Plane Source Technique
Time used by thermal conductivity factor is general in the range of tens seconds to hundreds of seconds, can quickly obtain the thermal conductivity factor of sample, and measurement is convenient
Fast.If measuring the thermal conductivity factor of powder isolation material with steady state method, the thermal conductivity factor and test environment according to testing sample
Difference, the testing time is typically in a few houres, ten a few houres even tens hours.
The content of the invention
In order to solve the problems, such as that steady state method measures the thermal conductivity factor overlong time of powder isolation material, the present invention provides a kind of
Powder heat conductivity measuring device based on Adsorbent By Using Transient Plane Source Technique, the device can quickly measure powder isolation material in a constant temperature
Thermal conductivity factor under degree, certain vacuum degree.
To reach above-mentioned purpose, the present invention uses following technical proposals：
A kind of device that powder thermal conductivity factor is measured based on Adsorbent By Using Transient Plane Source Technique, the device is included：Vacuum tank and perseverance
Warm system；Vacuum tank is set in the constant temperature system；
The constant temperature system is baking oven (RT-200 DEG C), water-bath system (0 DEG C -100 DEG C), (100 DEG C -200 of oil bath system
DEG C) or other cryogenic systems are (such as：Liquid nitrogen (77K), liquid nitrogen deep case (77K-RT) etc.) etc.；Constant temperature system can be according to measurement need
Will, for testing sample provides certain environment temperature；2 PT100 platinum resistance thermometers, monitoring constant temperature system are set in constant temperature system
System internal temperature is constant.
Described vacuum tank is cylindrical structure, for powder sample to be measured provides certain vacuum environment.
The vacuum tank includes vacuum tank cylinder, vacuum tank upper flange and vacuum-pumping tube；
The vacuum tank cylinder and the matching of vacuum tank upper flange are fixed；Vacuum tank cylinder and vacuum tank upper flange
Between using indium seal, it is ensured that the air-tightness of device；
The vacuum-pumping tube is connected through vacuum tank upper flange with vacuum tank cylinder；
Include solid sample holder, test probe, PT100 platinum resistance thermometers and retainer ring in the vacuum tank cylinder；
3 PT100 platinum resistance thermometers are set in the vacuum tank cylinder, and monitoring vacuum tank inner barrel temperature is permanent
It is fixed；
The retainer ring is hollow ring structure, and retainer ring includes that left half of retainer ring and retainer ring are right half, and this is fixed
Right half of ring and left half of retainer ring are connected；
The upper surface of the retainer ring sets 1 PT100 platinum resistance thermometer.
The retainer ring is connected with the bottom surface of vacuum tank cylinder；Solid sample holder lower half is set in retainer ring only；
The solid sample holder lower half only only matches fixation with solid sample holder upper half；The solid sample holder upper half only with solid sample holder on
Lid matching is fixed；
The solid sample holder is the cylindrical structure with hollow cylinder chamber；Solid sample holder is included on solid sample holder
Lid, solid sample holder upper half only and solid sample holder lower half only；
The solid sample holder lower half only, solid sample holder upper half only, solid sample holder upper lid surface be respectively provided with 1
PT100 platinum resistance thermometers.
The solid sample holder lower half only, solid sample holder upper half only, the solid sample holder top cap place of connecing smear thin layer
Silicone grease, beneficial to the heat transfer between the part of solid sample holder three.
Thermometer hole and air-vent are covered with the solid sample holder；
One end of the test probe is arranged between solid sample holder lower half and solid sample holder upper half, the other end
It is connected with wire；
Described PT100 platinum resistance thermometers one end is connected through the thermometer hole of lid on solid sample holder with test probe,
The other end is connected with wire；
The wire is arranged in vacuum-pumping tube.
Further, the air-vent is provided with stainless (steel) wire.So that when vacuumizing, powder sample to be measured will not be extracted,
The quantity of air-vent and depending on neglecting the size of solid sample holder greatly；
Further, the material of the solid sample holder and retainer ring is to use red copper material.
Further, the material of the vacuum tank is using 304 stainless steel materials.
Further, the PT100 platinum resistance thermometers can be increased or decreased according to measurement demand and actual conditions.
Thermal conductivity factor of the measurement powder sample under uniform temperature, certain vacuum degree, method of testing is as follows：
1) Hot Disk thermal constant analysis softwares are installed in computer.
2) installation of testing sample：Testing sample area first by solid sample holder lower half only fills powder sample, places
Test probe, by solid sample holder, upper and lower half is connected (with the upper and lower half clamping test probe of solid sample holder)；Will
Fill powder sample in solid sample holder upper half testing sample area only；The inner surface covered on solid sample holder is stained with 600-1000
Purpose stainless (steel) wire, only fixation is connect by solid sample holder upper half with top cap；One end of PT100 platinum resistance thermometers is passed through into powder
The thermometer hole covered on last specimen holder is connected with test probe；Solid sample holder lower half only, solid sample holder upper half only, powder-like
Smear thin layer silicone grease in the product frame top cap place of connecing.
3) installation of retainer ring
The solid sample holder that testing sample and test probe will be installed is arranged on left half of retainer ring and retainer ring right half
Centre only, left half of retainer ring and right half of retainer ring are connected；3 are set in the outer surface of solid sample holder
PT100 platinum resistance thermometers (solid sample holder lower half only, solid sample holder upper half only, on solid sample holder cover each 1)；Solid
The upper surface for determining ring sets 1 PT100 platinum resistance thermometer；The bottom surface of the lower surface of retainer ring and vacuum tank cylinder is smeared
Thin layer silicone grease, and be connected.
4) construction of vacuum environment
The base plate of vacuum tank cylinder is set into 1 PT100 platinum resistance thermometer, inwall sets 2 PT100 RTD temperature
Degree meter, monitors the temperature of vacuum tank cylinder；Vacuum tank cylinder and vacuum tank upper flange are sealed with indium, is connected；
Mechanical pump is opened, by vacuum-pumping tube for test device is vacuumized, treats that vacuum reaches 10-1Pa magnitudes, open molecular pump and continue
It is evacuated to 10-3Pa, closes vacuum tank valve, molecular pump and mechanical pump；A small amount of nitrogen is filled with vacuum tank, in treating vacuum tank
Vacuum reach test needed for vacuum when, close charging valve；If after being filled with nitrogen, higher than required vacuum, also needing out
Open mechanical pump and vacuum is evacuated to required vacuum.
5) construction of temperature environment
2 PT100 platinum resistance thermometers will be set in constant temperature system, and monitoring constant temperature system internal temperature is constant；Will assembling
Good vacuum tank is placed in constant temperature system, constant temperature system can be baking oven (RT-200 DEG C), water-bath system (0 DEG C -100 DEG C),
Oil bath system (100 DEG C -200 DEG C) or other cryogenic systems are (such as：Liquid helium (4.2K), liquid nitrogen (77K), liquid nitrogen deep case (77K-
RT) etc.) etc., needed according to measurement and selected；Temperature needed for the internal temperature of constant temperature system is set in into measurement.
6) test is started：Treat the PT100 RTDs at vacuum tank cylinder, solid sample holder, retainer ring and test probe
When the reading of thermometer reaches temperature needed for measurement, start test；Hot Disk thermal constants analysis software is by computer to survey
Probe header applies certain power within a period of time, and (time for being applied and power can be by the thermal conductivity factors of testing sample
Sets itself), then test probe surface temperature is raised, to powder internal transmission heat while test probe heats up；Test is visited
The head increased speed of temperature depends on the rate of heat transfer of testing sample, and the material resistance change based on test probe is right with temperature rise
Should be related to, the temperature data points of test probe in record heating process, untill the set heat time, computer will
Automatically then data are returned, are calculated by 200 data points of record by Hot Disk thermal constant analysis softwares, so that
To the thermal conductivity factor of powder.
Further, present invention uses the collection and treatment that Hot Disk thermal constants analysis softwares carry out data, selection point
Double-surfaces Method and isotropism module in analysis software, set specific heating power and heat time.
Further, the test probe selected by the present invention is 4922 types.
Beneficial effects of the present invention are as follows：
1st, compared with the method for traditional measurement powder thermal conductivity factor, the present invention is led based on Adsorbent By Using Transient Plane Source Technique measurement powder
The device of hot coefficient, can quickly obtain the thermal conductivity factor of powder isolation material.
2nd, device of the invention can measure thermal conductivity factor of the powder isolation material under uniform temperature, certain vacuum degree,
, in 30K-473K, vacuum ranges are 10 for Range of measuring temp-3Pa-1atm。
Brief description of the drawings
Specific embodiment of the invention is described in further detail below in conjunction with the accompanying drawings.
Fig. 1 is apparatus structure schematic diagram of the invention.
Fig. 2 is the profile of solid sample holder of the present invention.
Fig. 3 is the structural representation of retainer ring of the present invention.
In figure：1. test probe, 2.PT100 platinum resistance thermometers, 3. wire, 4. testing sample area, 5. solid sample holder,
6. retainer ring, 7. vacuum tank, 8. vacuum tank cylinder, 9. vacuum tank upper flange, 10. vacuum-pumping tube, 11. constant temperature systems,
Covered on 12. solid sample holders, 13. solid sample holder upper half, 14. solid sample holder lower half, 15. thermometer holes, 16. breathe freely
Hole, half, a 17. retainer rings left side, half, the 18. retainer rings right side, 19. retainer rings and vacuum tank base plate connecting hole, 20. retainer rings are left
Right half connecting hole.
Specific embodiment
In order to illustrate more clearly of the present invention, the present invention is done further with reference to preferred embodiments and drawings
It is bright.Similar part is indicated with identical reference in accompanying drawing.It will be appreciated by those skilled in the art that institute is specific below
The content of description is illustrative and be not restrictive, and should not be limited the scope of the invention with this.
Embodiment 1
A kind of device that powder thermal conductivity factor is measured based on Adsorbent By Using Transient Plane Source Technique, the device is included：Vacuum tank 7 and perseverance
Warm system 11；Vacuum tank 7 is set in the constant temperature system 11；
The constant temperature system 11 is baking oven (RT-200 DEG C), water-bath system (0 DEG C -100 DEG C), (100 DEG C -200 of oil bath system
DEG C) or other cryogenic systems (most as little as 30K) are (such as：Liquid nitrogen (77K), liquid nitrogen deep case (77K-RT) etc.) etc.；This transient state plane
Heat resource method test device of thermal conductivity coefficient observable temperature scope is 30K-473K, the ring certain for testing sample is provided of constant temperature system 11
Border temperature；
2 PT100 platinum resistance thermometers are set in the constant temperature system 11, and the monitoring internal temperature of constant temperature system 11 is constant；
The vacuum tank 7 includes vacuum tank cylinder 8, vacuum tank upper flange 9 and vacuum-pumping tube 10；
The vacuum tank cylinder 8 and the matching of vacuum tank upper flange 9 are fixed；On vacuum tank cylinder 8 and vacuum tank
Sealed using indium between flange 9；
The vacuum-pumping tube 10 is connected through vacuum tank upper flange 9 with vacuum tank cylinder 8；
Include solid sample holder 5, test probe 1, PT100 platinum resistance thermometers 2 in the vacuum tank cylinder 8 and fix
Ring 6；
3 PT100 platinum resistance thermometers 2, the inside temperature of monitoring vacuum tank cylinder 8 are set in the vacuum tank cylinder 8
Degree is constant；
The upper surface of the retainer ring 6 sets 1 PT100 platinum resistance thermometer 2；The bottom surface of retainer ring 6 is provided with retainer ring
With the connecting hole 19 of vacuum tank cylinder bottom surface；Retainer ring 6 is provided with half connecting hole 20 of retainer ring or so；
The retainer ring 6 is hollow ring structure, and retainer ring 6 includes that left half 17 of retainer ring and retainer ring are right half 18,
Right half 18 of the retainer ring and left half 17 of retainer ring are bolted fixation；
The retainer ring 6 is threadedly coupled fixation with the underrun of vacuum tank cylinder 8；Powder-like is set in retainer ring 6
Product frame lower half 14；The solid sample holder lower half only 14 only 13 matches fixation with solid sample holder upper half；On the solid sample holder
Fixation is matched with lid on solid sample holder 12 for half 13；
It is diameter 60mm, the hollow cylinder chamber of 60mm high that the solid sample holder 5 is inner chamber, outer surface be diameter 80mm,
The cylindrical structure of 80mm high；Solid sample holder 5 includes on solid sample holder lid 12, solid sample holder upper half only 13 and powder-like
Product frame lower half 14；
Solid sample holder lower half only 14 only 13 clamps test probe 2 with solid sample holder upper half；
The solid sample holder lower half 14, the upper half 13, surface of lid 12 is respectively provided with 1 PT100 platinum resistance temperature
Meter 2.
The solid sample holder lower half 14, the upper half 13, junction of lid 12 smears thin layer silicone grease, beneficial to powder-like
Heat transfer between the part of product frame 5 three.
Lid 12 is provided with thermometer hole 15 and air-vent 16 on the solid sample holder；
One end of the test probe 2 is arranged between solid sample holder lower half 14 and solid sample holder upper half 13,
The other end is connected with wire 3；
Thermometer hole 15 and test probe 1 of the described one end of PT100 platinum resistance thermometers 2 through lid 12 on solid sample holder
Connection, the other end is connected with wire 3；
The wire 3 is arranged in vacuum-pumping tube 10.
Lid 12 is provided with 12 air-vents of a diameter of 5mm 16 on the solid sample holder, and the air-vent is provided with 1000
Mesh stainless (steel) wire.
The material of the solid sample holder 5 and retainer ring 6 is to use red copper material.
The material of the vacuum tank 7 is using 304 stainless steel materials.
The meter of PT100 platinum resistance temperatures 2 can be increased or decreased according to measurement demand and actual conditions.
Measurement powder is in 293K, 10-3Thermal conductivity factor under Pa, step is as follows：
1) Hot Disk thermal constant analysis softwares are installed in computer；
2) installation of testing sample：The testing sample area 4 of solid sample holder lower half 14 is filled into powder sample first, is put
Test probe 1 is put, solid sample holder upper half 13, solid sample holder lower half 14 is connected and (is used solid sample holder upper half
Only 13, solid sample holder lower half only 14 clamp test probe)；The testing sample area 4 of solid sample holder upper half 13 is filled into powder
Last sample；The inner surface of lid 12 is stained with the stainless (steel) wire of 1000 mesh on solid sample holder, by solid sample holder upper half only 13 with
Upper lid 12 is connected；The thermometer hole 15 through lid 12 on solid sample holder and survey by one end of PT100 platinum resistance thermometers 2
Probe header 1 is connected；The junction of lid 12 applies in solid sample holder lower half 14, solid sample holder upper half 13, solid sample holder
Smear thin layer silicone grease.
3) installation of retainer ring
The solid sample holder 5 that testing sample and test probe 1 will be installed is arranged on a retainer ring left side half 17 and retainer ring
Right half 18 centre, left half 17 of retainer ring and right half 18 of retainer ring are connected；In the outer surface of solid sample holder 5
3 PT100 platinum resistance thermometers 2 of setting are (in solid sample holder lower half 14, solid sample holder upper half 13, solid sample holder
12 each 1, lid)；In the upper surface of retainer ring 6,1 PT100 platinum resistance thermometer 2 is set；By the lower surface and vacuum of retainer ring 6
Thin-layer silicon fat is smeared in the bottom surface of shell 8, and is connected.
4) construction of vacuum environment
The base plate of vacuum tank cylinder 8 is set into 1 PT100 platinum resistance thermometer 2, inwall sets 2 PT100 RTDs
Thermometer 2, the temperature of monitoring vacuum tank cylinder 8；Vacuum tank cylinder 8 and vacuum tank upper flange 9 are sealed with indium, connection
It is fixed；Mechanical pump is opened, by vacuum-pumping tube 10 for test device is vacuumized, treats that vacuum reaches 10-1Pa magnitudes, open molecule
Pump continues to be evacuated to 10-3Pa, closes vacuum tank valve, molecular pump and mechanical pump.
5) construction of temperature environment
Because measurement temperature is just in room temperature, thus vacuum tank 7 is disposed within.
6) test is started：Treat the PT100 RTDs at vacuum tank cylinder, solid sample holder, retainer ring and test probe
When the reading of thermometer 2 reaches temperature needed for test, start test；Enter present invention uses Hot Disk thermal constant analysis softwares
The collection and treatment of row data, Double-surfaces Method and isotropism module in selection analysis software, set specific heating power and
Heat time；Hot Disk thermal constants analysis software applies set electric rating by computer to test probe 1, surveys
Sound out head surface temperature to raise, the test probe 1 is 4922 types；To powder internal transmission heat while test probe 1 heats up
Amount, while the temperature of test probe 1 changes, the increased speed of the temperature of test probe 1 depends on the rate of heat transfer of testing sample,
Material resistance change and the corresponding relation of temperature rise based on test probe 1, record the temperature data of test probe 1 in heating process
Point, until the set heat time, computer can automatically record 200 data points, then by Hot Disk thermal constants point
Analysis software is returned to data, calculated, so as to obtain the thermal conductivity factor of powder.
Embodiment 2
A kind of device that powder thermal conductivity factor is measured based on Adsorbent By Using Transient Plane Source Technique, as described in Example 1.
Thermal conductivity factor of the measurement powder under 100 DEG C, 10Pa, step is as follows：
1) Hot Disk thermal constant analysis softwares are installed in computer；
2) installation of testing sample：The testing sample area 4 of solid sample holder lower half 14 is filled into powder sample first, is put
Test probe 1 is put, solid sample holder upper half 13, solid sample holder lower half 14 is connected and (is used solid sample holder upper half
Only 13, lower half only 14 clamp test probe)；The testing sample area 4 of solid sample holder upper half 13 is filled into powder sample；In powder
The inner surface of lid 12 is stained with the stainless (steel) wire of 1000 mesh on last specimen holder, and only 13 solid sample holder upper half is connected into solid with upper lid 12
It is fixed；One end of PT100 platinum resistance thermometers 2 is connected through the thermometer hole 15 of lid 12 on solid sample holder with test probe 1；
Thin layer silicone grease is smeared in the junction of lid 12 in solid sample holder lower half 14, solid sample holder upper half 13, solid sample holder.
3) installation of retainer ring
The solid sample holder 5 that testing sample and test probe 1 will be installed is arranged on a retainer ring left side half 17 and retainer ring
Right half 18 centre, left half 17 of retainer ring and right half 18 of retainer ring are connected；In the outer surface of solid sample holder 5
3 PT100 platinum resistance thermometers 2 of setting are (in solid sample holder lower half 14, solid sample holder upper half 13, solid sample holder
12 each 1, lid)；In the upper surface of retainer ring 6,1 PT100 platinum resistance thermometer 2 is set；By the lower surface and vacuum of retainer ring 6
Thin-layer silicon fat is smeared in the bottom surface of shell 8, and is connected.
4) construction of vacuum environment
The base plate of vacuum tank cylinder 8 is set into 1 PT100 platinum resistance thermometer 2, inwall sets 2 PT100 RTDs
Thermometer 2, the temperature of monitoring vacuum tank cylinder 8；Vacuum tank cylinder 8 and vacuum tank upper flange 9 are sealed with indium, connection
It is fixed；Mechanical pump is opened, by vacuum-pumping tube 10 for test device is vacuumized, treats that vacuum reaches 10-1Pa magnitudes, open molecule
Pump continues to be evacuated to 10-3Pa, closes vacuum tank valve, molecular pump and mechanical pump；A small amount of nitrogen is filled with vacuum tank 7, treats true
When vacuum in empty container 7 reaches 10Pa, charging valve is closed.If after being filled with nitrogen, higher than required vacuum, also needing to open
Vacuum is evacuated to 10Pa by mechanical pump.
5) construction of temperature environment
2 PT100 platinum resistance thermometers 2 will be set in constant temperature system 11, and the monitoring internal temperature of constant temperature system 11 is constant；Will
The vacuum tank 7 for assembling is placed in constant temperature system 11, and now constant temperature system 11 is baking oven (RT-200 DEG C) or water-bath system
(0 DEG C -100 DEG C)；The internal temperature of constant temperature system 11 is set in 100 DEG C.
6) test is started：Treat the PT100 RTDs at vacuum tank cylinder, solid sample holder, retainer ring and test probe
When the reading of thermometer 2 reaches temperature needed for test, start test；Enter present invention uses Hot Disk thermal constant analysis softwares
The collection and treatment of row data, Double-surfaces Method and isotropism module in selection analysis software, set specific heating power and
Heat time；Hot Disk thermal constants analysis software applies set electric rating by computer to test probe 1, surveys
Sound out head surface temperature to raise, the test probe 1 is 4922 types；To powder internal transmission heat while test probe 1 heats up
Amount, while the temperature of test probe 1 changes, the increased speed of the temperature of test probe 1 depends on the rate of heat transfer of testing sample,
Material resistance change and the corresponding relation of temperature rise based on test probe 1, record the temperature data of test probe 1 in heating process
Point, until the set heat time, computer can automatically record 200 data points, then by Hot Disk thermal constants point
Analysis software is returned to data, calculated, so as to obtain the thermal conductivity factor of powder.
Embodiment 3
A kind of device that powder thermal conductivity factor is measured based on Adsorbent By Using Transient Plane Source Technique, as described in Example 1.
Measurement powder is in 77K, 10-3Thermal conductivity factor under Pa, step is as follows：
1) Hot Disk thermal constant analysis softwares are installed in computer；
2) installation of testing sample：The testing sample area 4 of solid sample holder lower half 14 is filled into powder sample first, is put
Test probe 1 is put, solid sample holder upper half 13, solid sample holder lower half 14 is connected and (is used solid sample holder upper half
Only 13, solid sample holder lower half only 14 clamp test probe)；The testing sample area 4 of solid sample holder upper half 13 is filled into powder
Last sample；The inner surface of lid 12 is stained with the stainless (steel) wire of 1000 mesh on solid sample holder, by solid sample holder upper half only 13 with
Lid 12 is connected on solid sample holder；One end of PT100 platinum resistance thermometers 2 is passed through the temperature of lid 12 on solid sample holder
Meter hole 15 is connected with test probe 1；Lid 12 in solid sample holder lower half 14, solid sample holder upper half 13, solid sample holder
Smear thin layer silicone grease in junction.
3) installation of retainer ring
The solid sample holder 5 that testing sample and test probe 1 will be installed is arranged on a retainer ring left side half 17 and retainer ring
Right half 18 centre, left half 17 of retainer ring and right half 18 of retainer ring are connected；In the outer surface of solid sample holder 5
3 PT100 platinum resistance thermometers 2 of setting are (in solid sample holder lower half 14, solid sample holder upper half 13, solid sample holder
12 each 1, lid)；In the upper surface of retainer ring 6,1 PT100 platinum resistance thermometer 2 is set；By the lower surface and vacuum of retainer ring 6
Thin-layer silicon fat is smeared in the bottom surface of shell 8, and is connected.
4) construction of vacuum environment
The base plate of vacuum tank cylinder 8 is set into 1 PT100 platinum resistance thermometer 2, inwall sets 2 PT100 RTDs
Thermometer 2, the temperature of monitoring vacuum tank cylinder 8；Vacuum tank cylinder 8 and vacuum tank upper flange 9 are sealed with indium, connection
It is fixed；Mechanical pump is opened, by vacuum-pumping tube 10 for test device is vacuumized, treats that vacuum reaches 10-1Pa magnitudes, open molecule
Pump continues to be evacuated to 10-3Pa, closes vacuum tank valve, molecular pump and mechanical pump.
5) construction of temperature environment
2 PT100 platinum resistance thermometers 2 will be set in constant temperature system 11, and the monitoring internal temperature of constant temperature system 11 is constant；Will
The vacuum tank 7 for assembling is placed in constant temperature system 11, and now, constant temperature system 11 is the Dewar container for liquefied nitrogen for filling liquid nitrogen.
6) test is started：Treat the PT100 RTDs at vacuum tank cylinder, solid sample holder, retainer ring and test probe
When the reading of thermometer 2 reaches temperature needed for test, start test；Enter present invention uses Hot Disk thermal constant analysis softwares
The collection and treatment of row data, Double-surfaces Method and isotropism module in selection analysis software, set specific heating power and
Heat time；Hot Disk thermal constants analysis software applies set electric rating by computer to test probe 1, surveys
Sound out head surface temperature to raise, the test probe 1 is 4922 types；To powder internal transmission heat while test probe 1 heats up
Amount, while the temperature of test probe 1 changes, the increased speed of the temperature of test probe 1 depends on the rate of heat transfer of testing sample,
Material resistance change and the corresponding relation of temperature rise based on test probe 1, record the temperature data of test probe 1 in heating process
Point, until the set heat time, computer can automatically record 200 data points, then by Hot Disk thermal constants point
Analysis software is returned to data, calculated, so as to obtain the thermal conductivity factor of powder.
Description orientation employed in herein word " on ", D score, "left", "right" etc. be for illustrating facilitate base
For orientation in accompanying drawing shown in drawing, these orientation may be due to the disposing way of device in actual device
It is different.
Obviously, the above embodiment of the present invention is only intended to clearly illustrate example of the present invention, and is not right
The restriction of embodiments of the present invention, for those of ordinary skill in the field, may be used also on the basis of the above description
To make other changes in different forms, all of implementation method cannot be exhaustive here, it is every to belong to this hair
Obvious change that bright technical scheme is extended out changes row still in protection scope of the present invention.
Claims (5)
1. it is a kind of based on Adsorbent By Using Transient Plane Source Technique measure powder thermal conductivity factor device, it is characterised in that the device includes：Vacuum
Container (7) and constant temperature system (11)；Vacuum tank (7) is set in the constant temperature system (11)；
The vacuum tank (7) includes vacuum tank cylinder (8) and vacuum tank upper flange (9) and vacuum-pumping tube (10)；
The vacuum tank cylinder (8) and vacuum tank upper flange (9) matching are fixed；
Include in the vacuum tank cylinder (8) solid sample holder (5), test probe (1), PT100 platinum resistance thermometers (2),
Wire (3) and retainer ring (6)；
The solid sample holder (5) is including covering (12), solid sample holder upper half only (13) and solid sample holder on solid sample holder
Lower half is only (14)；
The retainer ring (6) is connected with the bottom surface of vacuum tank cylinder (8)；Set under solid sample holder in retainer ring (6)
Half (14)；Only (14) match fixation to the solid sample holder lower half with solid sample holder upper half (13)；
Only (13) match fixation to the solid sample holder upper half with lid (12) on solid sample holder；
(12) are covered on the solid sample holder and is provided with thermometer hole (15) and air-vent (16)；
One end of the test probe (1) be arranged on solid sample holder lower half only (14) and solid sample holder upper half only (13) it
Between, the other end is connected with wire (3)；
Visited with test through the thermometer hole (15) of lid (12) on solid sample holder described PT100 platinum resistance thermometers (2) one end
Head (1) connection；The other end is connected with wire (3)；
The wire (3) is arranged in vacuum-pumping tube (10).
2. device according to claim 1, it is characterised in that the air-vent (16) is provided with stainless (steel) wire.
3. device according to claim 1, it is characterised in that the material of the solid sample holder (5) and retainer ring (6) is
Using red copper material.
4. the device according to claim 1 or 3, it is characterised in that the solid sample holder (5) is with hollow cylinder chamber
Cylindrical structure.
5. device according to claim 1, it is characterised in that the retainer ring (6) including a retainer ring left side half (17) and
Half (18) in the retainer ring right side, retainer ring right side half (18) and a retainer ring left side half (17) are connected.
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| CN110174431A (en) * | 2019-05-21 | 2019-08-27 | 吉林建筑大学 | A kind of Lignin modification silty clay frost resistance research method |
| CN111537555A (en) * | 2020-05-14 | 2020-08-14 | 合肥工业大学 | Heat conductivity coefficient steady state method testing device and method suitable for vacuum glass beads |
| CN112179943A (en) * | 2019-07-02 | 2021-01-05 | 天津大学 | Probe for measuring heat conductivity coefficient and preparation method thereof |
| CN113295731A (en) * | 2021-05-25 | 2021-08-24 | 中国矿业大学 | Powder sample thermophysical property testing device and method under low-gravity high-vacuum environment |
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