CN106841297A - A kind of hot physical property testing device of multifunctional solid material and method - Google Patents
A kind of hot physical property testing device of multifunctional solid material and method Download PDFInfo
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- CN106841297A CN106841297A CN201710056171.XA CN201710056171A CN106841297A CN 106841297 A CN106841297 A CN 106841297A CN 201710056171 A CN201710056171 A CN 201710056171A CN 106841297 A CN106841297 A CN 106841297A
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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
- G01N25/48—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 on solution, sorption, or a chemical reaction not involving combustion or catalytic oxidation
- G01N25/4846—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 on solution, sorption, or a chemical reaction not involving combustion or catalytic oxidation for a motionless, e.g. solid sample
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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
- G01N25/005—Investigating or analyzing materials by the use of thermal means by investigating specific heat
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Abstract
The invention discloses a kind of hot physical property testing device of multifunctional solid material and method, including the hot junction pressure strip and cold end pressure strip that are connected by hold-down gear, the hot junction pressure strip of hot junction pressure strip is contacted with hot end seal plate, hot end seal plate is connected by elastic module with fever tablet, and fever tablet is fixed on the pedestal of hot junction；Seal pipe is provided between hot end seal plate and cold end pedestal, hold-down gear produces thrust, the corresponding sealing ring of crush seal pipe, the pressure bearing and seal cavity that formation is made up of hot end seal plate, seal pipe and cold end pedestal by hot junction pressure strip and cold end pressure strip；Temperature measuring equipment and pressure tester be respectively used to measure in pressure bearing and seal cavity hot physical property measurement sample to be tested be filled with or gas bleeding after temperature and pressure before and after gas, then realize the test to thermal physical property of solid material.Test device of the present invention and method of testing can eliminate thermal contact resistance, radiation and test error caused by heat convection, effectively improve thermal physical property parameter measuring accuracy.
Description
Technical field
The present invention relates to technical field of measurement and test, more particularly to a kind of hot physical property testing device of multifunctional solid material and side
Method.
Background technology
At present, the present situation of solid material class product is：As material science develops, to all kinds of novel solid materials heat conduction systems
The testing requirement of the thermal physical property parameters such as number, specific heat capacity is increasing.The thermal transient physical property up to a million compared to initial cost tens is surveyed
Trial assembly is put, and the general initial cost of stable state subtraction unit is can be controlled within ten thousand yuan.
There is certain deficiency in it, test material heat conduction system is adapted to steady state method more in the test processes of thermal physical property parameter
Number, is not easy to test material specific heat capacity.Additionally, plant bulk requirement is all larger needed for steady state method, for many new materials,
Set-up procedure too complex.
《GB/T 5598-1985 beryllia ceramics Measured Results of Thermal Conductivity methods》Document discloses a kind of small-size flaky structure heat conduction
Coefficient testing device and method of testing, but it there is also certain deficiency, and the device needs a huge seal cavity, passes through
Vacuum mode overcomes heat convection to measuring accuracy influence, and has Multi-layer thermal radome and many set water cooling plants reduction radiation heat transfers
Measuring accuracy is influenceed, causes test device integrally excessive, housing not easy to operate, the thermostatted water system complex of heaviness is difficult to control.
On the other hand, the disciplinary study such as chemical gas-solid reaction and absorption is progressively deep, at present to solid adsorption material
Study on thermal property is no longer limited in its intrinsic thermal physical property parameter test, in order to disclose its reaction or the change of adsorption process heat-transfer character
Change, the influence test of conversion ratio or adsorbance to hot physical property then seems particularly necessary, does not utilize steady state method suitably at present
Or the special hot physical property testing device of Transient Method is tested for this aspect.
In sum, in the prior art for thermal physical property parameters such as all kinds of novel solid materials thermal conductivity factors, specific heat capacities
Test problem, still lacks effective solution.
The content of the invention
In order to solve the deficiencies in the prior art, the invention provides a kind of hot physical property testing device of multifunctional solid material,
Including the hot junction pressure strip and cold end pressure strip that are connected by hold-down gear, the hot junction pressure strip of the hot junction pressure strip and hot junction
Sealing plate is contacted, and the hot end seal plate is connected by elastic module with fever tablet, and the fever tablet is fixed on the pedestal of hot junction；
The cold end pressure strip is contacted with cold end muff, and the cold end muff is embedded in cold drawing, the cold drawing and cold end
Base into contact, is used to place hot physical property measurement sample to be tested between the cold end pedestal and hot junction pedestal；
Be provided with seal pipe between the hot end seal plate and cold end pedestal, the hold-down gear by hot junction pressure strip and
Cold end pressure strip produces thrust, and the corresponding sealing ring of crush seal pipe is formed by hot end seal plate, seal pipe and cold end pedestal
The pressure bearing and seal cavity of composition；
Temperature measuring equipment and pressure tester are respectively used to hot physical property measurement sample to be tested in measurement pressure bearing and seal cavity and exist
Be filled with or gas bleeding after temperature and pressure before and after gas, then realize the test to thermal physical property of solid material.
It has the effect that：The above-mentioned test device of the application can not only be used for testing the intrinsic thermal conductivity factor of solid material
And specific heat capacity, it may also be used for thermal physical property parameter Changing Pattern of the test solid material in gas-solid reaction or adsorption process.
Further, the present invention also uses following technical scheme：
The hot junction pressure strip lower plane and plane contact on hot end seal plate, under seal pipe upper end insertion hot end seal plate
Flat seal groove, sealing ring is filled between seal groove top and seal pipe upper end；
In the equal temperature section of cold end of seal pipe lower end insertion cold end pedestal in the seal groove of plane, sealing trench bottom with it is close
Sealing ring is filled between tube sealing lower end.
Its technique effect having is：Sealing ring can be o types circle, X-type sealing ring, I-shaped sealing ring, U-shaped sealing
Ring, pad or fluid sealant etc., material are generally rubber, silica gel or polytetrafluoroethylene (PTFE) etc., can be according to being passed through gas compatible Sexual behavior mode.
The application realizes that sealing ring deformation reaches sealing function by the extruding force of hold-down gear.
Further, the present invention also uses following technical scheme：
The hot end seal plate side-wall hole, connects the hot end seal plate side wall and lower wall surface, the hot end seal plate
Side-wall hole, module, thermometric line extraction module, pressure tester, vacuum valve and intake valve are drawn for connecting power line.
Its technique effect having is：The application is realized to pressure bearing and seal by way of hot end seal plate side-wall hole
The measurement of the input and output of gas, gas pressure and temperature in cavity.
Further, the present invention also uses following technical scheme：
The hot end seal plate side-wall hole, opens a hole by threeway expansion interface or continuously opens multiple holes, mutually solely
It is vertical.
Its technique effect having is：The need for above-mentioned perforate mode of the invention is used to meet reality, according to measurement
How much comprehensive decisions of physical quantity and measurement point.
Further, the present invention also uses following technical scheme：
The hot end seal plate lower plane center is contacted over elastic module, elastic module lower plane and fever tablet
Upper plane contact, fever tablet power line is drawn module and exports to the external world by the power line of hot end seal plate side wall.
Elastic module can be metal spring, gas spring, have resilient organic material etc. in the application.Elastic module
Stiffness factor fixed value or to possess regularity, when needing different clamping forces for sample, suitable stiffness factor can be selected
Elastic module, according to thickness of sample, select the spring of the certain stiffness factor of certain length, you can produce the clamping force for needing,
Reduce the thermal contact resistance of test sample and temperature measuring area, it might even be possible to for studying thermal contact resistance change during different clamping forces.
Said power is drawn module and can be bonded by insulate colloid and conducting terminal and formed, it is considered to during high pressure, typically
Should realize that wire is passed from high-pressure chamber using glass frit seal terminal.
Further, the present invention also uses following technical scheme：
The hot junction pedestal is upper coarse and lower fine T-type structure body, and top is the equal temperature section in hot junction, and bottom is hot junction thermometric section.
Be to ensure axiality and machining accuracy in view of actual conditions, the equal temperature section in hot junction and end thermometric section for cylinder more
It is easy to process.
Further, the present invention also uses following technical scheme：
The fever tablet lower plane is fixed on plane in the equal temperature section in hot junction, and the hot junction muff is wrapped in the equal temperature section in hot junction
With fever tablet outside, axial arranged at least 2 temperature sensors of the hot junction thermometric section；
The hot junction muff side wall matches with seal pipe internal face, hot junction muff, hot junction pedestal and seal pipe
The central shaft of three overlaps with cold end thermometric section and hot junction thermometric section central shaft, and the hot junction insulation is cased with above-below direction
Through hole.
Above-mentioned hot junction muff side wall matches for shapes and sizes match with seal pipe internal face, hot junction insulation
Set side wall is in close contact with seal pipe internal face.
In above-mentioned hot junction muff, hot junction pedestal and seal pipe, due to shape and it is uncertain be circular, but for samming
Property, such as the shape such as square, circular, the central shaft of three should be overlapped.But three's size is simultaneously unequal, because hot junction
Muff is wrapped in hot junction pedestal outside, and side wall is close to hot junction pedestal.
Above-mentioned hot junction muff is mainly prevents equal temperature section heat radiation from spreading out of, and influences Determination of conductive coefficients precision, to protect
Card hot junction pedestal and the alignment of seal pipe, should typically use hard insulating material.Hot junction insulation is cased with the through hole of above-below direction
For the wire through temperature measuring equipment.
Further, the present invention also uses following technical scheme：
The cold end pedestal is up-thin-low-thick inverted T-type structure body, and Upper cylindrical is cold end thermometric section, and lower cylindrical is cold
Hold equal temperature section, axial arranged at least 2 temperature sensors of cold end thermometric section；Temperature sensor wires beam is small from hot junction muff
Hole passes through, and drawing module through thermometric line exports to the external world.
Said temperature sensor can be thermal resistance or thermocouple, but be easily caused test mistake because thermocouple is blocked
Difference, using glass capsulation terminal, binding post needs identical with thermocouple material.Temperature sensor fixation will axially, as far as possible
One temperature of point in test axial direction.
Further, the present invention also uses following technical scheme：
Hot junction thermometric section, cold end thermometric section is coaxial with hot physical property measurement sample and external diameter is equal, hot physical property measurement sample
Product are clamped between hot junction pedestal thermometric section lower plane and the upper plane of cold end pedestal thermometric section, and folder is provided by elastic module deformation
Hold pressure.
Further, the present invention also uses following technical scheme：
Plane is contacted with cold end pedestal lower plane on the cold drawing, and cold drawing side wall is provided with the import and export of constant temperature cooling fluid；
Cold end base side wall, cold drawing side wall and lower wall surface insertion cold end muff；Put down on cold end muff lower plane and cold end pressure strip
Face contacts.
Above-mentioned cold end base side wall, cold drawing side wall and lower wall surface insertion cold end muff, wherein, above cold end pedestal,
Namely with the face of cold end thermometric section connection, inside seal cavity, it is not necessary to insulation set parcel, it is not easy to realize.Insulation
The only part of each part of cold end on the outside of annular seal space of set parcel.
Hold-down gear produces thrust by cold and hot end pressure strip in the present invention, and crush seal ring forms hot end seal plate
Lower plane, sealing inside pipe wall and the pressure bearing and seal cavity that plane is constituted in the equal temperature section of cold end pedestal.Hold-down gear can for bolt,
The devices such as hydraulic press, there is provided the thrust of stabilization.
Further, the present invention also uses following technical scheme：
The hot junction pedestal and cold end pedestal vary with temperature very little or with clear and definite using thermal conductivity factor and specific heat capacity
Regular material makes, while ensureing possess thermal conductivity factor higher as far as possible, it is ensured that thermometric section radial temperature uniformity；Hot junction
The thermometric section of pedestal and cold end pedestal can increase weakening infra-red radiation radiating coating.
Further, the present invention also uses following technical scheme：
The seal pipe material is at least one of metal, ceramics, bearing composite material and glass；Seal pipe can be used
Vacuum double structure, sealing inside pipe wall can plate infrared reflection film, isolate the outside heat loss through radiation in temperature measuring area, improve test essence
Degree.
Further, the present invention also uses following technical scheme：
Seal pipe is using ceramics or glass material (such as saturating infrared ray trade mark quartz, the fluorination for having high infrared transmittance material
Titanate ceramicses etc.) when, thermometric line draws module can be removed, using infrared non-contact temperature measuring mode, on the outside of pressure bearing and seal cavity,
Thermometric section to hot junction pedestal and cold end pedestal carries out axial thermometric, and temperature data needed for collection, which design structure is simpler
It is single, operate easier.
Further, between the fever tablet lower surface and hot junction pedestal upper surface, hot junction thermometric section lower surface and hot thing
Property test sample upper surface between, hot physical property measurement sample lower surface and cold end thermometric section upper surface between, cold end pedestal following table
Filling heat conduction colloid between face and cold drawing upper surface, such as heat-conducting silicone grease, heat-conducting daub, heat-conducting pad, two-sided heat-conducting glue band etc.,
Reduce thermal contact resistance.
Further, the power line and thermometric line are drawn module and are derived using pressure-bearing cavity lead, ensure insulation with
Sealing simultaneously, realizes that power line and thermometric line are derived from pressure-bearing inside cavity；Power line and thermometric line are drawn module and are directly welded
Or hot end seal plate side wall is bonded in, also detachable pressure bearing and seal connected mode can be formed by screw thread or flange method.
Further, the hot junction pressure strip and hot end seal plate are integral type structure or split-type structural, cold end pedestal
It is integral type structure or split-type structural with cold drawing；Equal temperature section and the thermometric section of cold end pedestal are integral type structure or split type knot
Structure, equal temperature section and the thermometric section of hot junction pedestal are integral type structure or split-type structural；The seal pipe includes some sections of compositions,
Increase sealing ring between section and section and realize sealing.
When such as seal pipe includes two sections, one section of two ends seal pipe is fixed on hot end seal plate and cold with fluid sealant respectively
In the seal groove of end group seat, truncated position uses I-shaped sealing ring, and dismounting every time is only dismantled from truncated position, changes sample, operation
More facilitate.
Further, the thermometric line draws module can two, and one, in hot end seal plate side wall, is drawn hot junction base
Thermometric wire harness on seat temperature sensor, another draws thermometric wire harness on cold end base-plate temp sensor in cold end base side wall,
Dismounting is so easily facilitated, but it is even to be easily caused the equal temperature section temperature distributing disproportionation of cold end pedestal.
Further, the test device is vacuumized by vacuum valve to seal cavity, then the intrinsic heat of test material
Physical property, eliminates the test error that the heat exchange of seal cavity inner air convection causes；
To having vacuumized seal cavity insufflation gas, gas intake is controlled by intake valve, test material and be filled with gas
There is hot physical property when chemical reaction or different degrees of physical absorption in body；Gas participates in reaction or adsorbance by temperature before and after gas
Degree and pressure change are calculated and obtained.
Further, the test device assembling is disposed vertically by finishing, it is also possible to which different angles are placed as needed,
Cause error to suppress heat transfer free convection in principle, hot junction is above, and cold end is optimal in the following method that is disposed vertically, but
It is when not considering free convection effect, to be inverted, level or even inclination certain angle can be tested.
Further, the invention also discloses a kind of hot physical property measurement method of multifunctional solid material, when cold end and hot junction
When temperature measuring area side Wall Radiation and heat convection can be ignored, comprise the following steps：
(1) when whole test device temperature is normal temperature, heating plate firm power heating, cold drawing is passed through constant temperature fluid, together
The instantaneous value of Shi Jilu point for measuring temperature temperature, untill temperature spot no longer changes substantially, all point for measuring temperature collections are with the time
Change the temperature point data of collection for dynamic data is considered as dynamic temperature, the temperature data at finally gather a time point is considered as
Steady temperature；Dynamic data is the matrix of n*m, and n is the number of times of collection, that is, time term, and m is the number of temperature spot.
(2) consider that temperature measuring area radiation and convection losses can be ignored, it is considered to which temperature measuring area radial temperature difference is minimum, temperature measuring area heat conduction
Coefficient is definite value, is transmitted only along axial direction by the heat flow of hot junction temperature measuring area and cold end temperature measuring area, by the heat of sample
Flow is the half of the heat flow sum by hot junction temperature measuring area and cold end temperature measuring area；
Temperature according to the upper and lower surface of sample and pass through the heat flow of sample and calculate sample thermal resistance, finally obtain sample
Thermal conductivity factor；
(3) topmost arrive between the point for measuring temperature of bottom and partly set up one-dimensional dynamic heat transfer model；
It is (4) discrete to the axial location x and time t of Mathematical Modeling based on finite element, limited bulk or finite difference method,
Form one group of algebraic equation, it is known that the dynamic temperature of test point, the density and each several part thermal conductivity factor of hot physical property measurement sample,
Therefore the algebraic equation is positive definite or overdetermination Algebraic Equation set, and hot physical property measurement sample specific heat can be obtained by optimization algorithm
Hold；
(5) when the point for measuring temperature of the temperature measuring area arrangement of hot junction and cold end pedestal is more than two so that thermal conductivity factor and specific heat capacity
Solution Mathematical Modeling be changed into overdetermination Algebraic Equation set, both least square solution is solved by optimization algorithm.
Further, the invention also discloses a kind of hot physical property measurement method of multifunctional solid material, when cold end and hot junction
When temperature measuring area side Wall Radiation and heat convection cannot be ignored, comprise the following steps：
(1) temperature measuring area of hot junction and cold end pedestal is axially respectively arranged point for measuring temperature, while arranging seal cavity internal gas
Temperature point for measuring temperature and environment temperature point for measuring temperature, if seal pipe can not pass through infrared ray, arrangement sealing inside pipe wall point for measuring temperature substitution
Environment temperature point for measuring temperature, when whole test device temperature is normal temperature, heating plate firm power heating, cold drawing is passed through constant temperature stream
Body, at the same record temperature spot instantaneous value, until temperature spot substantially not find change untill, all point for measuring temperature gathered datas with
The corresponding matrix of time is considered as dynamic temperature, and the temperature data at finally gather a time point is considered as steady temperature；
(2) respectively to the top of hot junction and the temperature measuring area of cold end pedestal to partly setting up one-dimensional between the point for measuring temperature of bottom
Steady heat conduction Mathematical Modeling；
(3) system radiation coefficient and convection transfer rate can be obtained by optimization algorithm；
(4) hot junction pedestal most gone up respectively point for measuring temperature to lower plane region and cold end plane to most descending point for measuring temperature region
One-dimensional stable heat conduction equation seeks numerical solution, and the temperature and hot-fluid for obtaining plane on hot junction pedestal lower plane and cold end pedestal are close
Degree, according to the actual (real) thickness of hot physical property measurement sample, you can obtain the thermal conductivity factor of test sample；
(5) topmost arrive between the point for measuring temperature of bottom and partly set up one-dimensional dynamic heat transfer model；
(6) hot physical property measurement sample specific heat capacity can be obtained by optimization algorithm；
(7) during the point for measuring temperature more than three of the temperature measuring area arrangement of hot junction and cold end pedestal so that thermal conductivity factor and specific heat capacity
Solution Mathematical Modeling be changed into overdetermination Algebraic Equation set, both least square solution is solved by optimization algorithm.
Compared with prior art, the beneficial effects of the invention are as follows：
Hot physical property measurement method of the invention, can direct discrete one-dimensional dynamic heat transfer model, set up on heat conduction
The positive definite or overdetermined equation of coefficient and specific heat capacity, by optimal method, while thermal conductivity factor and specific heat capacity are obtained, due to so
Discrete equation group known variables out are excessive, easily dissipated by iterative process, therefore to computing power, derivation
It is higher with iterative algorithm requirement, but this kind of method need not always test temperature data stabilization, and a few minutes dynamic data is
The thermal physical property parameter of test sample can be directly obtained.
Hot physical property measurement method of the invention, when test sample upper and lower surface thermal contact resistance is larger, can test two
The sample entire thermal resistance of different length, entire thermal resistance formula can be represented with following formula：
Therefore, the thermal resistance of different condition difference length is obtained by different length sample entire thermal resistance is subtracted each other, contact heat is eliminated
Resistance causes test error, obtains sample thermal conductivity factor.
Test device of the present invention is compact, convenient disassembly, is easy to operation.Test sample of the present invention is small, is easy to make.
The present invention is tested by steady state data and obtains sample heat conductivility, and then obtains sample specific heat according to its dynamic data
Hold, the drawbacks of overcoming existing steady state method and be unable to test sample specific heat capacity；Test device of the present invention can not only be used for testing
The intrinsic thermal conductivity factor of solid material and specific heat capacity, it may also be used for hot thing of the test solid material in gas-solid reaction or adsorption process
Property Parameter Variation.
Test device of the present invention and method of testing can eliminate thermal contact resistance, radiation and test caused by heat convection
Error, effectively improves thermal physical property parameter measuring accuracy.
Brief description of the drawings
The Figure of description for constituting the part of the application is used for providing further understanding of the present application, and the application's shows
Meaning property embodiment and its illustrated for explaining the application, does not constitute the improper restriction to the application.
Fig. 1 is schematic structural view of the invention；
In figure, 1, hold-down gear, 2, power line draw module, 3, thermometric line draw module, 4, sealing ring, 5, seal pipe,
6th, temperature sensor, 7, cold drawing, 8, hot junction pressure strip, 9, vacuum valve, 10, intake valve, 11, hot end seal plate, 12, springform
Block, 13, fever tablet, 14, hot junction muff, 15, hot junction pedestal, 16, hot physical property measurement sample, 17, cold end pedestal, 18, cold end
Muff, 19, pressure gauge, 20, cold end pressure strip.
Specific embodiment
It is noted that described further below is all exemplary, it is intended to provide further instruction to the application.Unless another
Indicate, all technologies used herein and scientific terminology are with usual with the application person of an ordinary skill in the technical field
The identical meanings of understanding.
It should be noted that term used herein above is merely to describe specific embodiment, and be not intended to restricted root
According to the illustrative embodiments of the application.As used herein, unless the context clearly indicates otherwise, otherwise singulative
Be also intended to include plural form, additionally, it should be understood that, when in this manual use term "comprising" and/or " bag
Include " when, it indicates existing characteristics, step, operation, device, component and/or combinations thereof.
As background technology is introduced, there is the deficiency in thermal physical property of solid material measuring technology in the prior art, be
Technical problem as above is solved, present applicant proposes a kind of hot physical property testing device of multifunctional solid material and method.
In a kind of typical implementation method of the application, as shown in Figure 1, there is provided a kind of hot physical property of multifunctional solid material
Test device, above-mentioned test device include hot junction pressure strip 8, hot end seal plate 11, hold-down gear 1, power line draw module 2,
Pressure gauge 19, fever tablet 13, elastic module 12, hot physical property measurement sample 16, hot junction pedestal 15, hot junction muff 14, seal pipe
5th, sealing ring 4, temperature sensor 6, thermometric line draw module 3, vacuum valve 9, intake valve 10, cold end pedestal 17, cold drawing 7, cold end
Muff 18, cold end pressure strip 20.
In the present embodiment, plane contact on the lower plane of hot junction pressure strip 8 and hot end seal plate 11, the insertion of the upper end of seal pipe 5
The lower plane seal groove of hot end seal plate 11, is filled with sealing ring 4, by extruding force reality between seal groove top and seal pipe upper end
The existing deformation of sealing ring 4 reaches sealing function.
In the present embodiment, the side-wall hole of hot end seal plate 11 connects the side wall of hot end seal plate 11 and lower wall surface, hot end seal
Module 3, pressure gauge 19, vacuum valve 9 and intake valve are drawn with being connected power line and draw module 2, thermometric line at the side-wall hole of plate 11
10 connections, each side-wall hole is independent mutually.
In the present embodiment, the lower plane center of hot end seal plate 11 is contacted over elastic module 12, elastic module 12
Lower plane and plane contact in fever tablet 13, the power line of fever tablet 13 draw module 2 by the power line of hot end seal plate side wall
Export to the external world.Elastic module 12 is the constant metal spring of stiffness factor.Power line is drawn 2 pieces of mould and uses NPT helicitic textures
Glass sintering terminal, realization passed from high-pressure chamber.
In the present embodiment, hot junction pedestal 15 is upper coarse and lower fine T-shaped cylinder, and Upper cylindrical is the equal temperature section in hot junction, bottom
Cylinder is hot junction thermometric section.
In the present embodiment, the lower plane of fever tablet 13 is by being fixed on plane, hot junction muff in the equal temperature section of hot junction pedestal 15
14 are wrapped in the equal temperature section of hot junction pedestal 15 and the outside of fever tablet 13, axial arranged at least 2 temperature of the thermometric of hot junction pedestal 15 section
Sensor 6；The side wall of hot junction muff 14 matches with the internal face of seal pipe 5, hot junction muff 14, hot junction pedestal 15 and sealing
Pipe 5 is coaxial, and hot junction muff 14 has the through hole of above-below direction.Hot junction is incubated 14 sets and uses refractory brick hard insulating material, is divided into
Upper cover plate and lower protective case two parts are processed, and are easily installed.
In the present embodiment, cold end pedestal 17 is up-thin-low-thick inverted T shape cylinder, and Upper cylindrical is cold end thermometric section, under
Portion's cylinder is the equal temperature section of cold end, axial arranged at least 2 temperature sensors 6 of cold end thermometric section；The lead beam of temperature sensor 3 from
The aperture of hot junction muff 14 is passed through, and drawing module 3 through thermometric line exports to the external world.Temperature sensor 6 is thermal resistance PT100.Survey
Warm line draws the glass capsulation terminal that module 3 adds o type circle sealing structures for screw thread, and thermometric line is connected with hermetic terminal using plug-in
Connect, convenient dismounting.Hot junction pedestal 15 and the thermometric of cold end pedestal 17 section mill out radial direction sulculus, and PT100 temperature measuring heads pass through heat conduction
Solidification colloid is inlayed and is solidificated in groove.
In the present embodiment, the thermometric of hot junction pedestal 15 section, the thermometric of cold end pedestal 17 section and hot physical property measurement sample 16 it is coaxial and
External diameter is equal, and hot physical property measurement sample 16 is clamped in the thermometric of hot junction pedestal 15 section lower plane and the upper plane of the thermometric of cold end pedestal 17 section
Between, provide clamp pressure by the deformation of elastic module 12；Plane is close in the equal temperature section of the lower end of seal pipe 5 insertion cold end pedestal 17
In sealing groove, sealing ring 4 is filled between sealing trench bottom and the lower end of seal pipe 5.Sealing ring 4 is perfluoroether material o type circles.
In the present embodiment, plane is contacted with the lower plane of cold end pedestal 17 on cold drawing 7, and the side wall of cold drawing 7 possesses constant temperature cooling stream
Body is imported and exported, and cold drawing constant temperature fluid fluctuating temperature is less than 0.5 DEG C；The side wall of cold end pedestal 17, the side wall of cold drawing 7 and lower wall surface 7 are embedded in
Cold end muff 18；The lower plane of cold end muff 18 and plane contact on cold end pressure strip 20；Hold-down gear 1 is compressed by cold end
Plate 20 and hot junction pressure strip 8 produce thrust, crush seal ring 4, formed the lower plane of hot end seal plate 11, the inwall of seal pipe 5 and
The pressure bearing and seal cavity of plane composition in the equal temperature section of cold end pedestal 17.Hold-down gear 1 is one group of bolt, there is provided the compression of stabilization
Power.
In the present embodiment, hot junction pedestal 15 and cold end pedestal 17 are using the high-purity red copper making of T4, hot junction pedestal 15 and cold end
Pedestal 17 uses fine silver coating, and radiation coefficient is reduced to 0.02 or so.
In the present embodiment, seal pipe 5 has infrared reflection film using double-deck interior vacuum structure quartz ampoule, inwall, further
Reduce radiation loss.
In the present embodiment, between the lower surface of fever tablet 13 and the upper surface of hot junction pedestal 15, the lower surface of cold end pedestal 17 with it is cold
Curing type heat conduction adhesive curing bonding can be filled between the upper surface of plate 7, thermal contact resistance is reduced；The thermometric of hot junction pedestal 15 section lower surface
Between the hot upper surface of physical property measurement sample 16, the hot lower surface of physical property measurement sample 16 and the thermometric of cold end pedestal 17 section upper surface it
Between, heat-conducting daub is added with, reduce both thermal contact resistances.
In the present embodiment, hot physical property measurement sample 16 has two kinds, and respectively 316L stainless steels and calcium chloride graphite are compound inhales
Attached dose.
In the present embodiment, when hot physical property measurement sample 16 is 316L stainless steels, vavuum pump is by 9 pairs of sealings of vacuum valve first
Cavity is vacuumized, and ignores cold end and hot junction temperature measuring area side Wall Radiation and heat convection influence, and method of testing is as follows：
(1) temperature measuring area of hot junction pedestal 15 and cold end pedestal 17 is axially respectively arranged two points for measuring temperature, treats that whole test is flat
When platform temperature is normal temperature, the constant 200W power heating of heating plate 13, cold drawing 7 is passed through constant temperature fluid, while recording four temperature spots
Instantaneous value, until temperature spot substantially not untill change is found, the corresponding matrix of all point for measuring temperature gathered datas and time
It is considered as dynamic temperature, the temperature data at finally gather a time point is considered as steady temperature.
(2) consider that temperature measuring area radiation and convection losses can be ignored, it is considered to which temperature measuring area radial temperature difference is minimum, temperature measuring area heat conduction
Coefficient is definite value, is transmitted only along axial direction by hot junction pedestal temperature measuring area and cold end pedestal temperature measuring area heat flow, two heat
Flow is respectively：
Heat flow by sample is：
The temperature on the upper and lower surface of sample is respectively：
Therefore, sample thermal resistance is：
If ignoring the thermal contact resistance of sample and temperature measuring area, bringing arrangement into can obtain：
Steady state data and design parameter are brought into above formula, you can 316L thermal conductivity factors are 15.02Wm when obtaining 75 DEG C-1·
K-1, error is less than ± 3%.D in formulasIt is hot physical property measurement thickness of sample, λ12Hot junction pedestal thermal conductivity factor, λ34Cold end pedestal is led
Hot coefficient, d is each thermometric two point for measuring temperature distances of section, T1、T2、T3And T4To be arranged in hot junction and cold end thermometric from top to bottom
The steady temperature of point for measuring temperature, d are arranged in sectionHIt is T2Point for measuring temperature to hot physical property measurement sample upper surface distance, dCIt is T3Point for measuring temperature
To the distance of hot physical property measurement sample lower surface.
(3) topmost arrive between the point for measuring temperature of bottom and partly set up one-dimensional dynamic heat transfer model, such as following formula
It is (4) discrete to the axial location x and time t of Mathematical Modeling based on finite element, limited bulk or finite difference method,
Form one group of algebraic equation, it is known that four the dynamic temperature T of test point, the density p of hot physical property measurement sample and each several parts are led
Hot coefficient lambda, therefore the equation is overdetermination Algebraic Equation set, 316L specific heat capacities c is when can obtain 75 DEG C by optimization algorithm
0.498KJ·kg-1K-1, error is less than ± 4%.
The point for measuring temperature of the temperature measuring area arrangement of hot junction and cold end pedestal can be with more than two so that thermal conductivity factor and specific heat capacity
Solve Mathematical Modeling and be changed into overdetermination Algebraic Equation set, both least square solutions are solved by optimization algorithm.
In the present embodiment, when hot physical property measurement sample 16 is calcium chloride graphite compound adsorbent, vavuum pump is by true first
Empty valve 9 is vacuumized to seal cavity, and ammonia is filled with to having vacuumized seal cavity, and ammonia intake is controlled by intake valve 10,
Gas is participated in reaction or adsorbance and is obtained by temperature and pressure change calculations before and after gas, and method of testing is as follows：
(1) temperature measuring area of hot junction pedestal 15 and cold end pedestal 17 is axially respectively arranged three points for measuring temperature, while arranging sealing
Inside cavity gas temperature point for measuring temperature and sealing inside pipe wall point for measuring temperature, when whole test platform temperature is normal temperature, heating plate is permanent
Determine power heating, cold drawing is passed through constant temperature fluid, while eight instantaneous values of temperature spot are recorded, until temperature spot is not finding substantially
Untill change, all point for measuring temperature gathered datas are considered as dynamic temperature with the corresponding matrix of time, finally gather a time
The temperature data of point is considered as steady temperature；
(2) respectively to the top to part between the point for measuring temperature of bottom of hot junction pedestal 15 and the temperature measuring area of cold end pedestal 17
Set up one-dimensional stable heat transfer model, such as following formula
(3) it is discrete to the axial location x of Mathematical Modeling based on finite element, limited bulk or finite difference method, form two
Group algebraic equation, it is known that six the temperature T of the test point of temperature measuring area, the radius r of temperature measuring area, gas temperature Tf, environment temperature or
Seal pipe temperature TEAnd the thermal conductivity factor λ of temperature measuring area, two equation group simultaneous must be positive definite or overdetermination Algebraic Equation set, pass through
Optimization algorithm can obtain system radiation coefficient CsWith convection transfer rate h；
(4) hot junction pedestal 15 most gone up respectively point for measuring temperature to lower plane region and cold end pedestal 17 plane to most descending thermometric
The one-dimensional stable heat conduction equation in point region seeks numerical solution, obtains the temperature of plane on the lower plane of hot junction pedestal 15 and cold end pedestal 17
And heat flow density, according to the actual (real) thickness of calcium chloride graphite compound adsorbent test sample, you can obtain calcium chloride graphite and answer
The thermal conductivity factor for closing adsorbent absorption 0.6g/g ammonias is 2.58Wm-1·K-1。
(5) topmost arrive between the point for measuring temperature of bottom and partly set up one-dimensional dynamic heat transfer model, such as following formula
It is (6) discrete to the axial location x and time t of Mathematical Modeling based on finite element, limited bulk or finite difference method,
Form one group of algebraic equation, it is known that six the dynamic temperature T of the test point of temperature measuring area, density p, the thermometrics of hot physical property measurement sample
The radius r in area, gas temperature Tf, environment temperature or seal pipe temperature TE, each several part thermal conductivity factor thermal conductivity factor λ, system radiation
Coefficient CsWith convection transfer rate h, therefore the equation be positive definite or overdetermination Algebraic Equation set, by optimization algorithm can obtain
Hot physical property measurement sample specific heat capacity c is 0.8KJkg-1K-1。
The point for measuring temperature of the temperature measuring area arrangement of hot junction and cold end pedestal can be with more than three so that thermal conductivity factor and specific heat capacity
Solve Mathematical Modeling and be changed into overdetermination Algebraic Equation set, both least square solutions are solved by optimization algorithm.
The preferred embodiment of the application is the foregoing is only, the application is not limited to, for the skill of this area
For art personnel, the application can have various modifications and variations.It is all within spirit herein and principle, made any repair
Change, equivalent, improvement etc., should be included within the protection domain of the application.
Claims (10)
1. a kind of hot physical property testing device of multifunctional solid material, it is characterized in that, including the hot junction being connected by hold-down gear pressed
Tight plate and cold end pressure strip, the hot junction pressure strip of the hot junction pressure strip are contacted with hot end seal plate, and the hot end seal plate leads to
Cross elastic module to be connected with fever tablet, the fever tablet is fixed on the pedestal of hot junction；
The cold end pressure strip is contacted with cold end muff, and the cold end muff is embedded in cold drawing, the cold drawing and cold end pedestal
Contact, is used to place hot physical property measurement sample to be tested between the cold end pedestal and hot junction pedestal；
Seal pipe is provided between the hot end seal plate and cold end pedestal, the hold-down gear passes through hot junction pressure strip and cold end
Pressure strip produces thrust, and the corresponding sealing ring of crush seal pipe, formation is made up of hot end seal plate, seal pipe and cold end pedestal
Pressure bearing and seal cavity；
Temperature measuring equipment and pressure tester are respectively used to hot physical property measurement sample to be tested in measurement pressure bearing and seal cavity and are being filled with
Or temperature and pressure before and after gas after gas bleeding, then realize the test to thermal physical property of solid material.
2. a kind of hot physical property testing device of multifunctional solid material as claimed in claim 1, it is characterized in that,
The hot junction pressure strip lower plane and plane contact on hot end seal plate, seal pipe upper end insertion hot end seal plate lower plane
Seal groove, sealing ring is filled between seal groove top and seal pipe upper end；
In the equal temperature section of cold end of the seal pipe lower end insertion cold end pedestal in the seal groove of plane, trench bottom and seal pipe are sealed
Sealing ring is filled between lower end.
3. a kind of hot physical property testing device of multifunctional solid material as claimed in claim 1, it is characterized in that, the hot end seal
Plate side-wall hole, connects the hot end seal plate side wall and lower wall surface, the hot end seal plate side-wall hole, for connecting power supply
Line is drawn module, thermometric line and draws module, pressure tester, vacuum valve and intake valve；
Or
The hot end seal plate side-wall hole, opens a hole by threeway expansion interface or continuously opens multiple holes, independent mutually.
4. a kind of hot physical property testing device of multifunctional solid material as claimed in claim 3, it is characterized in that,
The hot end seal plate lower plane center is contacted over elastic module, is put down in elastic module lower plane and fever tablet
Face is contacted, and fever tablet power line is drawn module and exports to the external world by the power line of hot end seal plate side wall.
5. a kind of hot physical property testing device of multifunctional solid material as claimed in claim 1, it is characterized in that,
The hot junction pedestal is upper coarse and lower fine T-type structure body, and top is the equal temperature section in hot junction, and bottom is hot junction thermometric section；
Or
The cold end pedestal is up-thin-low-thick inverted T-type structure body, and Upper cylindrical is cold end thermometric section, and lower cylindrical is that cold end is equal
Temperature section, axial arranged at least 2 temperature sensors of cold end thermometric section；Temperature sensor wires beam is worn from hot junction muff aperture
Cross, drawing module through thermometric line exports to the external world；
Or
Hot junction thermometric section, cold end thermometric section is coaxial with hot physical property measurement sample and external diameter is equal, hot physical property measurement specimen holder
Hold between plane on hot junction pedestal thermometric section lower plane and cold end pedestal thermometric section, clamping pressure is provided by elastic module deformation
Power.
6. a kind of hot physical property testing device of multifunctional solid material as claimed in claim 2, it is characterized in that, under the fever tablet
Plane is fixed on plane in the equal temperature section in hot junction, and the hot junction muff is wrapped in the equal temperature section in hot junction and fever tablet outside, the heat
End thermometric axial arranged at least 2 temperature sensors of section；
Or
The hot junction muff side wall matches with seal pipe internal face, hot junction muff, hot junction pedestal and seal pipe three
Central shaft and cold end thermometric section and hot junction thermometric section central shaft overlaps, the hot junction insulation is cased with leading to for above-below direction
Hole；
Or
Plane is contacted with cold end pedestal lower plane on the cold drawing, and cold drawing side wall is provided with the import and export of constant temperature cooling fluid；Cold end
Base side wall, cold drawing side wall and lower wall surface insertion cold end muff；Cold end muff lower plane connects with plane on cold end pressure strip
Touch.
7. a kind of hot physical property testing device of multifunctional solid material as claimed in claim 2, it is characterized in that,
The seal pipe material is at least one of metal, ceramics, bearing composite material and glass；Seal pipe can use vacuum
Double-decker, sealing inside pipe wall can plate infrared reflection film；
Or
When seal pipe is using the ceramics or glass material for having high infrared transmittance material, thermometric line draws module can be removed, and be adopted
With infrared non-contact temperature measuring mode, on the outside of pressure bearing and seal cavity, the thermometric section to hot junction pedestal and cold end pedestal carries out axial direction
Thermometric, temperature data needed for collection；
Or
Between the fever tablet lower surface and hot junction pedestal upper surface, hot junction thermometric section lower surface and hot physical property measurement sample upper table
Between face, between hot physical property measurement sample lower surface and cold end thermometric section upper surface, cold end pedestal lower surface and cold drawing upper surface
Between fill heat conduction colloid.
8. a kind of hot physical property testing device of multifunctional solid material as claimed in claim 5, it is characterized in that, the hot junction compresses
Plate and hot end seal plate are integral type structure or split-type structural, and cold end pedestal and cold drawing are integral type structure or split type knot
Structure；Equal temperature section and the thermometric section of cold end pedestal are integral type structure or split-type structural, equal temperature section and the thermometric section of hot junction pedestal
It is integral type structure or split-type structural；The seal pipe includes some sections of compositions, and increase sealing ring is realized close between section and section
Envelope；
Or
The thermometric line draws module can two, and one, in hot end seal plate side wall, is drawn hot junction base-plate temp sensor
Upper thermometric wire harness, another draws thermometric wire harness on cold end base-plate temp sensor, so easily facilitates in cold end base side wall
Dismounting, but it is even to be easily caused the equal temperature section temperature distributing disproportionation of cold end pedestal.
9. the method based on a kind of any described hot physical property testing devices of multifunctional solid material of claim 1-8, works as cold end
When can ignore with hot junction temperature measuring area side Wall Radiation and heat convection, it is characterized in that, comprise the following steps：
(1) when whole test device temperature is normal temperature, heating plate firm power heating, cold drawing is passed through constant temperature fluid, while note
The instantaneous value of point for measuring temperature temperature is recorded, untill temperature spot no longer changes substantially, all point for measuring temperature collections are changed over time
The temperature point data of collection is considered as dynamic temperature for dynamic data, and the temperature data at finally gather a time point is considered as stable state
Temperature；
(2) consider that temperature measuring area radiation and convection losses can be ignored, it is considered to which temperature measuring area radial temperature difference is minimum, temperature measuring area thermal conductivity factor
It is definite value, is transmitted only along axial direction by the heat flow of hot junction temperature measuring area and cold end temperature measuring area, by the heat flow of sample
It is the half of the heat flow sum by hot junction temperature measuring area and cold end temperature measuring area；
Temperature according to the upper and lower surface of sample and pass through the heat flow of sample and calculate sample thermal resistance, it is final to obtain sample heat conduction
Coefficient；
(3) topmost arrive between the point for measuring temperature of bottom and partly set up one-dimensional dynamic heat transfer model；
(4) it is discrete to the axial location x and time t of Mathematical Modeling based on finite element, limited bulk or finite difference method, formed
One group of algebraic equation, it is known that the dynamic temperature of test point, the density and each several part thermal conductivity factor of hot physical property measurement sample, therefore
The algebraic equation is positive definite or overdetermination Algebraic Equation set, and hot physical property measurement sample specific heat capacity can be obtained by optimization algorithm；
(5) when the point for measuring temperature of the temperature measuring area arrangement of hot junction and cold end pedestal is more than two so that thermal conductivity factor and specific heat capacity are asked
Solution Mathematical Modeling is changed into overdetermination Algebraic Equation set, and both least square solutions are solved by optimization algorithm.
10. the method based on a kind of any described hot physical property testing devices of multifunctional solid material of claim 1-8, works as cold end
When cannot ignore with hot junction temperature measuring area side Wall Radiation and heat convection, it is characterized in that, comprise the following steps：
(1) temperature measuring area of hot junction and cold end pedestal is axially respectively arranged point for measuring temperature, while arranging seal cavity internal air temperature
Point for measuring temperature and environment temperature point for measuring temperature, if seal pipe can not pass through infrared ray, arrangement sealing inside pipe wall point for measuring temperature substitution environment
Temperature point for measuring temperature, when whole test device temperature is normal temperature, heating plate firm power heating, cold drawing is passed through constant temperature fluid, together
The instantaneous value of Shi Jilu temperature spots, until temperature spot substantially not untill change is found, all point for measuring temperature collections are changed over time
The temperature point data of collection is considered as dynamic temperature for dynamic data, and the temperature data at finally gather a time point is considered as stable state
Temperature；
(2) one-dimensional stable is partly set up in the top respectively to hot junction and the temperature measuring area of cold end pedestal between the point for measuring temperature of bottom
Heat transfer model；
(3) system radiation coefficient and convection transfer rate can be obtained by optimization algorithm；
(4) hot junction pedestal most gone up respectively point for measuring temperature to lower plane region and cold end plane to most descending the one-dimensional of point for measuring temperature region
Steady heat conduction equation seeks numerical solution, obtains the temperature and heat flow density of plane on hot junction pedestal lower plane and cold end pedestal, root
According to the actual (real) thickness of hot physical property measurement sample, you can obtain the thermal conductivity factor of test sample；
(5) topmost arrive between the point for measuring temperature of bottom and partly set up one-dimensional dynamic heat transfer model；
(6) hot physical property measurement sample specific heat capacity can be obtained by optimization algorithm；
(7) during the point for measuring temperature more than three of the temperature measuring area arrangement of hot junction and cold end pedestal so that thermal conductivity factor and specific heat capacity are asked
Solution Mathematical Modeling is changed into overdetermination Algebraic Equation set, and both least square solutions are solved by optimization algorithm.
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