CN117969596A - Material thermophysical property measuring device based on thermal equilibrium method under ultralow temperature condition - Google Patents
Material thermophysical property measuring device based on thermal equilibrium method under ultralow temperature condition Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 156
- 238000000034 method Methods 0.000 title claims abstract description 20
- 239000001307 helium Substances 0.000 claims abstract description 37
- 229910052734 helium Inorganic materials 0.000 claims abstract description 37
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims abstract description 37
- 239000007788 liquid Substances 0.000 claims abstract description 30
- 238000012360 testing method Methods 0.000 claims abstract description 25
- 230000001105 regulatory effect Effects 0.000 claims abstract description 16
- 239000007789 gas Substances 0.000 claims abstract description 12
- 230000000704 physical effect Effects 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims description 127
- 238000010438 heat treatment Methods 0.000 claims description 76
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 47
- 229910052802 copper Inorganic materials 0.000 claims description 39
- 239000010949 copper Substances 0.000 claims description 39
- 230000001276 controlling effect Effects 0.000 claims description 20
- 238000007789 sealing Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 claims description 6
- 238000005057 refrigeration Methods 0.000 claims description 6
- 238000012544 monitoring process Methods 0.000 claims description 3
- 239000001257 hydrogen Substances 0.000 abstract description 12
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 12
- 239000012774 insulation material Substances 0.000 abstract description 12
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 11
- 238000009413 insulation Methods 0.000 description 9
- 239000010410 layer Substances 0.000 description 8
- 238000012546 transfer Methods 0.000 description 5
- 238000013461 design Methods 0.000 description 3
- 238000004088 simulation Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- ZZUFCTLCJUWOSV-UHFFFAOYSA-N furosemide Chemical compound C1=C(Cl)C(S(=O)(=O)N)=CC(C(O)=O)=C1NCC1=CC=CO1 ZZUFCTLCJUWOSV-UHFFFAOYSA-N 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
Abstract
The invention belongs to the technical field of low-temperature physical property testing, and discloses a material thermal physical property measuring device under an ultralow temperature condition based on a thermal equilibrium method. According to the device for measuring the thermal physical properties of the material under the ultralow temperature condition, the vacuum degree of the multilayer heat insulation material can be regulated and controlled through vacuumizing and a corresponding gas filling method, helium which is suitable for a liquid hydrogen or liquid helium storage tank to use a temperature region is used as filling gas, and other low-temperature liquid storage tanks can be filled with gas in a corresponding temperature region. The material cavity with variable capacity of the material thermophysical property measuring device under the ultralow temperature condition has the advantages that the thickness of the measured material is controllable within a certain range, the range of a test sample is enlarged to a certain extent, and the limitation on the material specification in the low temperature conductivity test of the existing material is broken.
Description
Technical Field
The invention belongs to the technical field of low-temperature physical property testing, and relates to a material thermal physical property measuring device under an ultralow-temperature condition based on a thermal equilibrium method.
Background
The hydrogen energy is used as a clean energy source with no toxicity and harm, good combustion performance, high heat value and zero carbon emission, and is an important object for future research. For large-scale and long-distance hydrogen energy storage and transportation, a low-temperature liquid state mode is generally adopted, and as the boiling point temperature of liquid hydrogen is far lower than that of conventional low-temperature liquid energy sources such as LNG, liquid nitrogen and the like, correspondingly, higher requirements for cold insulation of a storage tank are also provided, so that the development of hydrogen energy is limited to a certain extent.
At present, a vacuum multilayer heat insulation technology is mostly adopted at home and abroad to store liquid Hydrogen, and a vehicle-mounted liquid Hydrogen storage tank of a BMW hydro 7 model adopts 70 layers of glass fiber heat insulation materials (national energy information platform, the first liquid Hydrogen heavy truck of the Ministry of North automobile and Futian of the disclosure); the 125m3 low-temperature liquid hydrogen ball tank of NASA adopts 80 layers of multi-layer heat insulation materials with the thickness of 21mm as heat insulation layers, and the heat conductivity coefficient reaches 10 -4 W/m.K (ALGHAFRIS Z S, et al energy.) so that the multi-layer heat insulation mode can well control the heat entering the storage tank from the outside, and is an ideal heat insulation mode. When the storage and transportation equipment is designed, the heat leakage quantity of the vacuum multilayer heat insulation material is generally analyzed and estimated by adopting a numerical simulation means, and the structural parameters of the storage and transportation equipment are determined based on thermal coupling. Wu Xiaofang et al, in the design and analysis of tank body of low-temperature liquid transport vehicle, analyze the stress distribution rule of the low-temperature tank body under the condition of thermal shock by adopting a numerical simulation method; ma Xiaoyong et al in the development of heat insulation performance research of multilayer heat insulation materials for low temperature containers, predict the heat insulation performance of multilayer heat insulation materials with different boundary temperatures and different layers by using a Lockheed analysis model to obtain an optimized heat insulation scheme. In practice, the heat conduction process of the vacuum multilayer heat insulation structure comprises various forms such as radiation, heat conduction, convection and the like, and different heat conduction forms change along with the changes of the vacuum degree of the vacuum interlayer, the types of heat insulation materials and the number of layers, so that accurate universal model unified description is difficult, and particularly certain calculation errors can exist for an ultra-large liquid hydrogen storage and transportation device. Therefore, the device for accurately measuring the heat transfer performance of the vacuum multilayer material under the ultralow temperature working condition can be designed, is a key for advancing the hydrogen energy storage and transportation technology, has very important significance, and has become an important subject in the field of hydrogen energy application.
Disclosure of Invention
The invention aims to provide a thermal conductivity testing device for a material under an ultralow temperature condition based on a thermal balance method, which can realize the testing of thermal conductivities under different vacuum conditions.
The technical scheme of the invention is as follows:
The device for measuring the thermal physical properties of the material under the ultralow temperature condition based on the thermal equilibrium method comprises a cold source module 1, a vacuum cavity pressure control module 2, a vacuum cavity 3, a bracket component 4, a primary cold table component 5, a secondary cold table component 6, a measured material cavity 7, a cold screen 8 and a measuring and controlling module 9;
The cold source module 1 comprises a compressor 1-1, a water chilling unit 1-2 and a cold head 1-3, wherein the water chilling unit 1-2, the compressor 1-1 and the cold head 1-3 are sequentially connected through pipelines; the cold head 1-3 is fixedly suspended by a cold head supporting plate 4-1 and a first-stage cold table oxygen-free copper 5-1; the cold source module 1 is matched with equipment of corresponding specifications according to the test temperature requirement of the tested materials, and necessary ultralow temperature environment temperature is provided for the test.
The vacuum cavity pressure control module 2 comprises a molecular pump group 2-1, a helium leak detector 2-2, a vacuumizing control valve 2-3, an inflation control valve 2-4, a liquid helium storage tank 2-5 and a vacuum gauge 2-6; the molecular pump set 2-1 is used for vacuumizing, and an outlet pipeline connected with the molecular pump set 2-1 is provided with a vacuumizing control valve 2-3; the liquid helium storage tank 2-5 is used for providing low-temperature gas, and an outlet pipeline connected with the liquid helium storage tank 2-5 is provided with an inflation control valve 2-4 for controlling the vacuum degree; the outlet pipeline connected with the molecular pump group 2-1 and the outlet pipeline connected with the liquid helium storage tank 2-5 are combined into one pipeline, and a vacuum gauge 2-6 and a connection helium leak detector 2-2 are arranged on the pipeline; when vacuumizing, opening the vacuumizing control valve 2-3, closing the inflation control valve 2-4, opening the molecular pump group 2-1, vacuumizing to a high vacuum state of 10 -4 Pa, and closing the vacuumizing control valve 2-3 and the molecular pump group 2-1; when gas is filled, the vacuumizing control valve 2-3 is closed, the inflating control valve 2-4 is opened, helium in the liquid helium storage tank 2-5 is filled in through a pipeline under the action of pressure difference, the numerical value of the vacuum gauge 2-6 is observed, and when the pressure reaches the test requirement, the inflating control valve 2-4 is closed; the vacuum gauge 2-6 is used for monitoring the vacuum degree, and the helium leak detector 2-2 is used for detecting the leakage condition of the system at the pipeline joint;
The vacuum cavity 3 is a space surrounded by an upper shell 3-1 and a lower shell 3-2 and comprises an upper shell 3-1, a lower shell 3-2, a sealing ring 3-3 between the upper shell and the lower shell, a fixing bolt 3-4, a vacuum cavity evacuation joint 3-5 and a tested material cavity evacuation joint 3-6; the upper shell 3-1 and the lower shell 3-2 are connected through flanges and are provided with a sealing ring 3-3, and are fixed by fixing bolts 3-4; the side wall of the upper shell is provided with a vacuum cavity evacuating connector 3-5 and a material cavity 7 evacuating connector 3-6, which are both connected with a combined pipeline of the vacuum cavity pressure control module 2 and are respectively used for controlling the vacuum degree in the vacuum cavity 3 and the vacuum degree of the material cavity 7 to be tested;
The bracket assembly 4 comprises a cold head supporting plate 4-1, an equipment bracket 4-2 and a lead port 4-3; the cold head supporting plate 4-1 is fixed at the upper end of the equipment bracket 4-2 to form an external frame, and a lead port 4-3 is arranged on the cold head supporting plate 4-1; the cold head 1-3 is inversely arranged on the upper surface of the cold head supporting plate 4-1, and the upper end surface of the upper shell 3-1 is connected with the lower surface of the cold head supporting plate 4-1 through a flange; the vacuum cavity 3 is arranged in the outer frame in a suspending way, so that the distance between the bottom of the vacuum cavity 3 and the bottom of the equipment bracket 4-2 is ensured, and the equipment is convenient to assemble and disassemble, and the materials are convenient to place and replace; the temperature sensor, the heating film, the power line of the cooling film and the lead wire of the data acquisition inside the vacuum cavity 3 are led out to the measuring and controlling module 9 through the lead wire port 4-3;
The primary cooling table assembly 5 comprises primary cooling table oxygen-free copper 5-1, primary cooling table connecting rods 5-2 and primary cooling table connecting stranded wires 5-3, wherein the upper surface of the primary cooling table oxygen-free copper 5-1 is connected with the cooling head 1-3 through the primary cooling table connecting stranded wires 5-3, so that the surface of the primary cooling table is cooled; the upper surface of the oxygen-free copper 5-1 of the primary cooling table is connected with the lower surface of the end plate of the upper shell 3-1 through three primary cooling table connecting rods 5-2, so that the primary cooling table is supported and positioned;
The secondary cooling table assembly 6 comprises a secondary cooling table oxygen-free copper 6-1, a secondary cooling table connecting rod 6-2, a secondary cooling table connecting stranded wire 6-3 and a cold end heating film 6-4, wherein the upper surface of the secondary cooling table oxygen-free copper 6-1 is connected with the cold head 1-3 through the secondary cooling table connecting stranded wire 6-3, so that the cooling of the secondary cooling table is realized; the upper surface of the secondary cooling table oxygen-free copper 6-1 is connected with the lower surface of the primary cooling table oxygen-free copper 5-1 through a secondary cooling table connecting rod 6-2, so that the support and the positioning of the secondary cooling table are realized; the lower surface of the oxygen-free copper 6-1 of the secondary cooling table is covered with a cold end heating film 6-4, the cold end heating film 6-4 is connected with a heating wire, and the heating quantity is regulated according to the cold end temperature requirement;
The measured material cavity 7 is a space surrounded by a material cavity shell 7-1 and a material cavity lower cover 7-2 and comprises a material cavity shell 7-1, a movable material shelf 7-2, an adjusting screw rod 7-3, a hot end heating film 7-4, a hot end cooling film 7-5 and a material cavity lower cover 7-6, wherein the material cavity shell 7-1, the movable material shelf 7-2 and the material cavity lower cover 7-6 are surrounded into a material cavity, the adjusting screw rod 7-3 is propped against the movable material shelf 7-2 through the material cavity lower cover 7-6, and the position of the movable material shelf 7-2 is adjusted by screwing a screw on the adjusting screw rod 7-3, so that the volume of the material cavity is changed according to the specification and the size requirements of a measured material; the upper part of the material cavity shell 7-1 is connected with the lower surface of the oxygen-free copper 6-1 of the secondary cooling table through a flange; the lower surface of the material cavity lower cover 7-6 is covered with a hot end heating film 7-4 and a hot end cooling film 7-5, and the heating and cooling quantity is regulated according to the hot end temperature requirement; the hot end heating film 7-4 is connected with a heating wire, the hot end cooling film 7-5 is connected with a refrigeration power supply wire, and the heating wire and the refrigeration power supply wire are led out to the outer side of the device through a lead port 4-3;
The cold screen 8 is arranged on the outer side of the tested material cavity 7, an air cavity is arranged between the cold screen 8 and the tested material cavity 7, and different vacuum degrees are controlled by vacuumizing or filling helium according to test requirements in the test process;
The measuring and controlling module 9 comprises a power regulator 9-1 of the cold end heating film 6-4, a power regulator 9-2 of the hot end heating film 7-4, a power regulator 9-3 of the hot end cooling film 7-5, a cold end temperature sensor 9-4 of the measured material, a hot end temperature sensor 9-5 of the measured material and a data acquisition system 9-6; the power regulator 9-1 of the cold end heating film 6-4 is used for regulating the heating capacity of the cold end heating film 6-4, controlling the temperature of the cold end of the measured material together with the refrigerating capacity provided by the cold head 1-3, wherein the temperature is monitored by the cold end temperature sensor 9-4 of the measured material, and the cold end temperature sensor 9-4 of the measured material is arranged on the lower surface of the oxygen-free copper 6-1 of the secondary cold table; the power regulator 9-2 of the hot end heating film 7-4 is used for regulating the heating amount of the hot end heating film 7-4, the power regulator 9-3 of the hot end cooling film 7-5 is used for regulating the cooling amount of the hot end cooling film 7-5, the heating amount and the cooling amount jointly control the hot end temperature of the measured material, the temperature is monitored by the hot end temperature sensor 9-5 of the measured material, and the hot end temperature sensor 9-5 of the measured material is arranged on the lower surface of the movable material shelf 7-2.
The invention has the beneficial effects that:
(1) The invention provides a material thermophysical property measuring device under an ultralow temperature condition based on a thermal balance method, which breaks through the single-form limitation that a vacuum multilayer heat insulation material obtains heat transfer characteristics through a theoretical calculation or numerical simulation method at present, reproduces the actual operation working condition of an ultralow temperature storage tank through a cold and hot end temperature control and material cavity vacuum degree control mode, directly obtains the heat exchange quantity of the heat insulation material through a hot end heating quantity, and further calculates the heat transfer coefficient of the multilayer heat insulation material.
(2) The invention designs a material thermophysical property measuring device under an ultralow temperature condition based on a thermal equilibrium method, which can realize the regulation and control of the vacuum degree of a multi-layer heat insulation material through vacuumizing and a corresponding gas filling method.
(3) The invention designs the material cavity with variable capacity, the thickness of the tested material is controllable within a certain range, the range of the test sample is enlarged to a certain extent, and the limitation of the low temperature conductivity test of the current material on the specification of the material is broken.
Drawings
FIG. 1 is a schematic diagram of a thermal equilibrium method-based device for measuring thermal properties of a material under ultralow temperature conditions.
In the figure: 1, a cold source module; 2, a vacuum cavity pressure control module; 3, a vacuum cavity; 4 a bracket assembly; a stage 5 cooling table assembly; a secondary cooling table assembly; 7, a tested material cavity assembly; 8, cooling; 9, a measuring and controlling module; 1-1 compressors; 1-2 water chilling units; 1-3 cold heads; 2-1 molecular pump group; a 2-2 helium leak detector; 2-3 vacuumizing control valves; 2-4 an inflation control valve; 2-5 liquid helium storage tanks; 2-6 vacuum gauge; 3-1 upper housing; 3-2 lower housing; 3-3 sealing rings; 3-4 fixing bolts; 3-5 vacuum cavity evacuation joint; 3-6, evacuating the material cavity to be tested; 4-1 cold head support plate; 4-2 equipment rack; 4-3 lead ports; 5-1 stage of cooling table oxygen-free copper; 5-2 primary cold table connecting rods; 5-3 primary cold table connecting stranded wires; 6-1 second-stage cooling table oxygen-free copper; 6-2 second-stage cold table connecting rods; 6-3 second-stage cold table connecting stranded wires; 6-4 cold end heating film; 7-1 material cavity shell; 7-2 a movable material shelf; 7-3, adjusting a screw rod; 7-4 hot end heating film; 7-5 hot end cooling films; 7-6 material cavity lower cover; 9-1 power regulator of the cold end heating film of the second-stage cooling table; 9-2 a power regulator of a heating film at the hot end of the material cavity to be tested; 9-3 a power regulator of the hot end cooling film of the measured material cavity; 9-4 a cold end temperature sensor of the measured material; 9-5 a material hot end temperature sensor; 9-6 data acquisition system.
Detailed Description
The following describes the embodiments of the present invention further with reference to the drawings and technical schemes.
As shown in FIG. 1, the device for measuring the thermal physical properties of the material under the ultralow temperature condition based on the thermal equilibrium method comprises a cold source module 1, a vacuum cavity pressure control module 2, a vacuum cavity 3, a bracket component 4, a primary cooling table component 5, a secondary cooling table component 6, a measured material cavity 7, a cooling screen 8 and a measuring and controlling module 9;
The cold source module 1 comprises a compressor 1-1, a water chilling unit 1-2 and a cold head 1-3, wherein the water chilling unit 1-2, the compressor 1-1 and the cold head 1-3 are sequentially connected through pipelines; the cold head 1-3 is fixedly suspended by a cold head supporting plate 4-1 and a first-stage cold table oxygen-free copper 5-1; the cold source module 1 is matched with equipment of corresponding specifications according to the test temperature requirement of the tested materials, and necessary ultralow temperature environment temperature is provided for the test.
The vacuum cavity pressure control module 2 comprises a molecular pump group 2-1, a helium leak detector 2-2, a vacuumizing control valve 2-3, an inflation control valve 2-4, a liquid helium storage tank 2-5 and a vacuum gauge 2-6; the molecular pump set 2-1 is used for vacuumizing, and an outlet pipeline connected with the molecular pump set 2-1 is provided with a vacuumizing control valve 2-3; the liquid helium storage tank 2-5 is used for providing low-temperature gas, and an outlet pipeline connected with the liquid helium storage tank 2-5 is provided with an inflation control valve 2-4 for controlling the vacuum degree; the outlet pipeline connected with the molecular pump group 2-1 and the outlet pipeline connected with the liquid helium storage tank 2-5 are combined into one pipeline, and a vacuum gauge 2-6 and a connection helium leak detector 2-2 are arranged on the pipeline; when vacuumizing, opening the vacuumizing control valve 2-3, closing the inflation control valve 2-4, opening the molecular pump group 2-1, vacuumizing to a high vacuum state of 10 -4 Pa, and closing the vacuumizing control valve 2-3 and the molecular pump group 2-1; when gas is filled, the vacuumizing control valve 2-3 is closed, the inflating control valve 2-4 is opened, helium in the liquid helium storage tank 2-5 is filled in through a pipeline under the action of pressure difference, the numerical value of the vacuum gauge 2-6 is observed, and when the pressure reaches the test requirement, the inflating control valve 2-4 is closed; the vacuum gauge 2-6 is used for monitoring the vacuum degree, and the helium leak detector 2-2 is used for detecting the leakage condition of the system at the pipeline joint;
The vacuum cavity 3 is a space surrounded by an upper shell 3-1 and a lower shell 3-2 and comprises an upper shell 3-1, a lower shell 3-2, a sealing ring 3-3 between the upper shell and the lower shell, a fixing bolt 3-4, a vacuum cavity evacuation joint 3-5 and a tested material cavity evacuation joint 3-6; the upper shell 3-1 and the lower shell 3-2 are connected through flanges and are provided with a sealing ring 3-3, and are fixed by fixing bolts 3-4; the side wall of the upper shell is provided with a vacuum cavity evacuating connector 3-5 and a material cavity 7 evacuating connector 3-6, which are both connected with a combined pipeline of the vacuum cavity pressure control module 2 and are respectively used for controlling the vacuum degree in the vacuum cavity 3 and the vacuum degree of the material cavity 7 to be tested;
The bracket assembly 4 comprises a cold head supporting plate 4-1, an equipment bracket 4-2 and a lead port 4-3; the cold head supporting plate 4-1 is fixed at the upper end of the equipment bracket 4-2 to form an external frame, and a lead port 4-3 is arranged on the cold head supporting plate 4-1; the cold head 1-3 is inversely arranged on the upper surface of the cold head supporting plate 4-1, and the upper end surface of the upper shell 3-1 is connected with the lower surface of the cold head supporting plate 4-1 through a flange; the vacuum cavity 3 is arranged in the outer frame in a suspending way, so that the distance between the bottom of the vacuum cavity 3 and the bottom of the equipment bracket 4-2 is ensured, and the equipment is convenient to assemble and disassemble, and the materials are convenient to place and replace; the temperature sensor, the heating film, the power line of the cooling film and the lead wire of the data acquisition inside the vacuum cavity 3 are led out to the measuring and controlling module 9 through the lead wire port 4-3;
The primary cooling table assembly 5 comprises primary cooling table oxygen-free copper 5-1, primary cooling table connecting rods 5-2 and primary cooling table connecting stranded wires 5-3, wherein the upper surface of the primary cooling table oxygen-free copper 5-1 is connected with the cooling head 1-3 through the primary cooling table connecting stranded wires 5-3, so that the surface of the primary cooling table is cooled; the upper surface of the oxygen-free copper 5-1 of the primary cooling table is connected with the lower surface of the end plate of the upper shell 3-1 through three primary cooling table connecting rods 5-2, so that the primary cooling table is supported and positioned;
The secondary cooling table assembly 6 comprises a secondary cooling table oxygen-free copper 6-1, a secondary cooling table connecting rod 6-2, a secondary cooling table connecting stranded wire 6-3 and a cold end heating film 6-4, wherein the upper surface of the secondary cooling table oxygen-free copper 6-1 is connected with the cold head 1-3 through the secondary cooling table connecting stranded wire 6-3, so that the cooling of the secondary cooling table is realized; the upper surface of the secondary cooling table oxygen-free copper 6-1 is connected with the lower surface of the primary cooling table oxygen-free copper 5-1 through a secondary cooling table connecting rod 6-2, so that the support and the positioning of the secondary cooling table are realized; the lower surface of the oxygen-free copper 6-1 of the secondary cooling table is covered with a cold end heating film 6-4, the cold end heating film 6-4 is connected with a heating wire, and the heating quantity is regulated according to the cold end temperature requirement;
The measured material cavity 7 is a space surrounded by a material cavity shell 7-1 and a material cavity lower cover 7-2 and comprises a material cavity shell 7-1, a movable material shelf 7-2, an adjusting screw rod 7-3, a hot end heating film 7-4, a hot end cooling film 7-5 and a material cavity lower cover 7-6, wherein the material cavity shell 7-1, the movable material shelf 7-2 and the material cavity lower cover 7-6 are surrounded into a material cavity, the adjusting screw rod 7-3 is propped against the movable material shelf 7-2 through the material cavity lower cover 7-6, and the position of the movable material shelf 7-2 is adjusted by screwing a screw on the adjusting screw rod 7-3, so that the volume of the material cavity is changed according to the specification and the size requirements of a measured material; the upper part of the material cavity shell 7-1 is connected with the lower surface of the oxygen-free copper 6-1 of the secondary cooling table through a flange; the lower surface of the material cavity lower cover 7-6 is covered with a hot end heating film 7-4 and a hot end cooling film 7-5, and the heating and cooling quantity is regulated according to the hot end temperature requirement; the hot end heating film 7-4 is connected with a heating wire, the hot end cooling film 7-5 is connected with a refrigeration power supply wire, and the heating wire and the refrigeration power supply wire are led out to the outer side of the device through a lead port 4-3;
The cold screen 8 is arranged on the outer side of the tested material cavity 7, an air cavity is arranged between the cold screen 8 and the tested material cavity 7, and different vacuum degrees are controlled by vacuumizing or filling helium according to test requirements in the test process;
The measuring and controlling module 9 comprises a power regulator 9-1 of the cold end heating film 6-4, a power regulator 9-2 of the hot end heating film 7-4, a power regulator 9-3 of the hot end cooling film 7-5, a cold end temperature sensor 9-4 of the measured material, a hot end temperature sensor 9-5 of the measured material and a data acquisition system 9-6; the power regulator 9-1 of the cold end heating film 6-4 is used for regulating the heating capacity of the cold end heating film 6-4, controlling the temperature of the cold end of the measured material together with the refrigerating capacity provided by the cold head 1-3, wherein the temperature is monitored by the cold end temperature sensor 9-4 of the measured material, and the cold end temperature sensor 9-4 of the measured material is arranged on the lower surface of the oxygen-free copper 6-1 of the secondary cold table; the power regulator 9-2 of the hot end heating film 7-4 is used for regulating the heating amount of the hot end heating film 7-4, the power regulator 9-3 of the hot end cooling film 7-5 is used for regulating the cooling amount of the hot end cooling film 7-5, the heating amount and the cooling amount jointly control the hot end temperature of the measured material, the temperature is monitored by the hot end temperature sensor 9-5 of the measured material, and the hot end temperature sensor 9-5 of the measured material is arranged on the lower surface of the movable material shelf 7-2.
The working process comprises the following steps:
(1) Placing materials: the lower shell 3-2 of the vacuum cavity 3, the cold screen 8 and the tested material component 7 are dismounted in sequence, the tested material is placed on the movable material shelf 7-2, the screw on the adjusting screw rod 7-3 is rotated, and the movable material shelf 7-2 is adjusted, so that the upper surface of the tested material and the upper edge of the material cavity shell 7-1 are in the same horizontal plane. The tested material assembly 7, the cold screen 8 and the lower shell 3-2 of the vacuum cavity 3 are sequentially installed, and the placement of the tested material is completed.
(2) And (3) vacuumizing a system: the pressure control module 2 is simultaneously connected with the vacuum cavity evacuation joint 3-5 and the material cavity evacuation joint 3-6 to be tested through a tee joint, the evacuation control valve 2-3 is opened, the inflation control valve 2-4 is closed, the molecular pump group 2-1 is opened, the numerical value of the vacuum gauge 2-6 is observed, the vacuum cavity 3 and the material cavity 7 to be tested are evacuated to the required vacuum degree, the evacuation control valve 2-3 is closed, the molecular pump group 2-1 is closed, and the leakage condition of the system is detected at the joint by using the helium leak detector 2-2. When the test is required to be carried out under specific pressure, the vacuum cavity 3 and the tested material cavity 7 are filled with gas, the vacuumizing control valve 2-3 is closed, the inflation control valve 2-4 is opened, helium in the liquid helium storage tank 2-5 enters the vacuum cavity 3 and the tested material cavity 7 through the system pipeline under the action of pressure difference, the numerical value of the vacuum gauge 2-6 is observed, and the inflation control valve 2-4 is closed when the pressure in the vacuum cavity 3 and the tested material cavity 7 meets the test requirement.
(3) And (3) controlling the temperature of the cold end and the hot end: the cold end temperature is controlled by the refrigerating capacity and the heating capacity of the upper surface and the lower surface of the secondary cooling table oxygen-free copper 6-1, and a cold end temperature sensor 9-4 of a measured material is arranged on the lower surface of the secondary cooling table oxygen-free copper 6-1, so that the temperature is monitored in real time. The upper surface of the secondary cooling table oxygen-free copper 6-1 is connected with the cold head 1-3 to realize cooling, the lower surface of the secondary cooling table oxygen-free copper 6-1 is covered with the cold end heating film 6-4, the cold end heating film 6-4 is connected with a heating wire, and the heating quantity is controlled by the power regulator 9-1 of the cold end heating film 6-4. When the heat transfer characteristic of the material under the ultralow temperature condition is tested, the cold end temperature is controlled below 20K. The hot end temperature is controlled by a hot end cooling film 7-5 and a hot end heating film 7-4 on the lower surface of a lower cover 7-6 of the material cavity to be measured, the hot end cooling film 7-5 is arranged on the lower surface of a movable material shelf 7-2, and the temperature is monitored in real time. When the heat transfer characteristic of the material under the ultralow temperature condition is tested, the temperature of the hot end is controlled between 150K and 293K.
(4) And (3) measurement and data processing: when the cold end and the hot end are stable in temperature, the heating power of the hot end is recorded, the value is the heat leakage quantity of the measured heat insulation material, and the heat conductivity of the material can be calculated by a formula through the material specification parameters.
Wherein lambda is the thermal conductivity of the insulating material, W/m.K; q is heat leakage quantity, W; delta is the thickness of the sample, m; f is the material sectional area, m 2; delta T is the temperature difference, K.
Claims (1)
1. The device for measuring the thermal physical properties of the material under the ultralow temperature condition based on the thermal equilibrium method is characterized by comprising a cold source module (1), a vacuum cavity pressure control module (2), a vacuum cavity (3), a bracket component (4), a primary cooling table component (5), a secondary cooling table component (6), a measured material cavity (7), a cooling screen (8) and a measuring and controlling module (9);
The cold source module (1) comprises a compressor (1-1), a water chilling unit (1-2) and a cold head (1-3), wherein the water chilling unit (1-2), the compressor (1-1) and the cold head (1-3) are sequentially connected through pipelines; the cold head (1-3) is supercooled with the cold head supporting plate (4-1) and the first-stage cold table oxygen-free copper (5-1), and is fixed and suspended through the cold head supporting plate (4-1); the cold source module (1) is matched with equipment of corresponding specifications according to the test temperature requirement of the tested material, and necessary ultralow temperature environment temperature is provided for the test;
The vacuum cavity pressure control module (2) comprises a molecular pump group (2-1), a helium leak detector (2-2), a vacuumizing control valve (2-3), an inflation control valve (2-4), a liquid helium storage tank (2-5) and a vacuum gauge (2-6); the molecular pump group (2-1) is used for vacuumizing, and an outlet pipeline connected with the molecular pump group (2-1) is provided with a vacuumizing control valve (2-3); the liquid helium storage tank (2-5) is used for providing low-temperature gas, and an outlet pipeline connected with the liquid helium storage tank (2-5) is provided with an inflation control valve (2-4) for controlling the vacuum degree; the outlet pipeline connected with the molecular pump group (2-1) and the outlet pipeline connected with the liquid helium storage tank (2-5) are combined into one pipeline, and a vacuum gauge (2-6) and a connection helium leak detector (2-2) are arranged on the pipeline; when vacuumizing, the vacuumizing control valve (2-3) is opened, the inflation control valve (2-4) is closed, the molecular pump group (2-1) is opened, and after vacuumizing to a high vacuum state of 10 -4 Pa, the vacuumizing control valve (2-3) and the molecular pump group (2-1) are closed; when gas is filled, the vacuumizing control valve (2-3) is closed, the inflating control valve (2-4) is opened, helium in the liquid helium storage tank (2-5) is filled through a pipeline under the action of pressure difference, the numerical value of the vacuum gauge (2-6) is observed, and when the pressure reaches the test requirement, the inflating control valve (2-4) is closed; the vacuum gauge (2-6) is used for monitoring the vacuum degree, and the helium leak detector (2-2) is used for detecting the leakage condition of the system at the pipeline joint;
The vacuum cavity (3) is a space surrounded by an upper shell (3-1) and a lower shell (3-2), and comprises the upper shell (3-1), the lower shell (3-2), a sealing ring (3-3) between the upper shell and the lower shell, a fixing bolt (3-4), a vacuum cavity evacuation joint (3-5) and a tested material cavity evacuation joint (3-6); the upper shell (3-1) and the lower shell (3-2) are connected through a flange and are provided with a sealing ring (3-3) which is fixed by a fixing bolt (3-4); the side wall of the upper shell is provided with a vacuum cavity evacuating connector (3-5) and a material cavity to be tested (7) evacuating connector 3-6, which are both connected with a combined pipeline of the vacuum cavity pressure control module (2) and are respectively used for controlling the vacuum degree in the vacuum cavity (3) and the vacuum degree in the material cavity to be tested (7);
The bracket component (4) comprises a cold head supporting plate (4-1), an equipment bracket (4-2) and a lead port (4-3); the cold head supporting plate (4-1) is fixed at the upper end of the equipment bracket (4-2) to form an external frame, and a lead port (4-3) is arranged on the cold head supporting plate (4-1); the cold head (1-3) is inversely arranged on the upper surface of the cold head supporting plate (4-1), and the upper end surface of the upper shell (3-1) is connected with the lower surface of the cold head supporting plate (4-1) through a flange; the vacuum cavity (3) is arranged in the outer frame in a suspending way, so that the distance between the bottom of the vacuum cavity (3) and the bottom of the equipment bracket (4-2) is ensured, and equipment assembly and disassembly and material placement and replacement are facilitated; the temperature sensor, the heating film, the power line of the cooling film and the lead wire of the data acquisition inside the vacuum cavity (3) are led out to the measuring and controlling module (9) through the lead wire port (4-3);
The primary cooling table assembly (5) comprises primary cooling table oxygen-free copper (5-1), a primary cooling table connecting rod (5-2) and primary cooling table connecting stranded wires (5-3), and the upper surface of the primary cooling table oxygen-free copper (5-1) is connected with the cooling head (1-3) through the primary cooling table connecting stranded wires (5-3) to realize primary cooling table surface cooling; the upper surface of the first-stage cooling table oxygen-free copper (5-1) is connected with the lower surface of the end plate of the upper shell (3-1) through three first-stage cooling table connecting rods (5-2), so that the first-stage cooling table is supported and positioned;
The secondary cooling table assembly (6) comprises secondary cooling table oxygen-free copper (6-1), a secondary cooling table connecting rod (6-2), a secondary cooling table connecting stranded wire (6-3) and a cold end heating film (6-4), and the upper surface of the secondary cooling table oxygen-free copper (6-1) is connected with the cold head (1-3) through the secondary cooling table connecting stranded wire (6-3) to realize cooling of the secondary cooling table; the upper surface of the secondary cooling table oxygen-free copper (6-1) is connected with the lower surface of the primary cooling table oxygen-free copper (5-1) through a secondary cooling table connecting rod (6-2), so that the support and the positioning of the secondary cooling table are realized; the lower surface of the oxygen-free copper (6-1) of the secondary cooling table is covered with a cold end heating film (6-4), the cold end heating film (6-4) is connected with a heating wire, and the heating quantity is regulated according to the cold end temperature;
The measured material cavity (7) is a space surrounded by a material cavity shell (7-1) and a material cavity lower cover (7-6), and comprises the material cavity shell (7-1), a movable material shelf (7-2), an adjusting screw rod (7-3), a hot end heating film (7-4), a hot end cooling film (7-5) and the material cavity lower cover (7-6), wherein the material cavity shell (7-1), the movable material shelf (7-2) and the material cavity lower cover (7-6) enclose a material cavity, the adjusting screw rod (7-3) is propped against the movable material shelf (7-2) through the material cavity lower cover (7-6), and the position of the movable material shelf (7-2) is adjusted by screwing a screw on the adjusting screw rod (7-3), so that the volume of the material cavity is changed according to the specification and the size requirements of the measured material; the upper part of the material cavity shell (7-1) is connected with the lower surface of the oxygen-free copper (6-1) of the secondary cooling table through a flange; the lower surface of the material cavity lower cover (7-6) is covered with a hot end heating film (7-4) and a hot end cooling film (7-5), and the heating and cooling quantity is regulated according to the hot end temperature; the hot end heating film (7-4) is connected with a heating wire, the hot end cooling film (7-5) is connected with a refrigeration power supply wire, and the heating wire and the refrigeration power supply wire are led out to the outer side of the device through a lead port (4-3);
The cold screen (8) is arranged at the outer side of the tested material cavity (7), an air cavity is arranged between the cold screen and the tested material cavity (7), and different vacuum degrees are controlled by vacuumizing or filling helium gas according to the test requirement in the test process;
The measuring and controlling module (9) comprises a power regulator (9-1) of the cold end heating film (6-4), a power regulator (9-2) of the hot end heating film (7-4), a power regulator (9-3) of the hot end cooling film (7-5), a cold end temperature sensor (9-4) of the measured material, a hot end temperature sensor (9-5) of the measured material and a data acquisition system (9-6); the power regulator (9-1) of the cold end heating film (6-4) is used for regulating the heating capacity of the cold end heating film (6-4), controlling the temperature of the cold end of the measured material together with the refrigerating capacity provided by the cold head (1-3), wherein the temperature is monitored by the cold end temperature sensor (9-4) of the measured material, and the cold end temperature sensor (9-4) of the measured material is arranged on the lower surface of the oxygen-free copper (6-1) of the secondary cold table; the power regulator (9-2) of the hot end heating film (7-4) is used for regulating the heating capacity of the hot end heating film (7-4), the power regulator (9-3) of the hot end cooling film (7-5) is used for regulating the cooling capacity of the hot end cooling film (7-5), the heating capacity and the cooling capacity jointly control the hot end temperature of the measured material, the temperature is monitored by the hot end temperature sensor (9-5) of the measured material, and the hot end temperature sensor (9-5) of the measured material is arranged on the lower surface of the movable material shelf (7-2).
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202410293259.3A CN117969596A (en) | 2024-03-14 | 2024-03-14 | Material thermophysical property measuring device based on thermal equilibrium method under ultralow temperature condition |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202410293259.3A CN117969596A (en) | 2024-03-14 | 2024-03-14 | Material thermophysical property measuring device based on thermal equilibrium method under ultralow temperature condition |
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