CN207488217U - The apparent thermal conductivity of multilayer insulant and outgassing rate test device - Google Patents

The apparent thermal conductivity of multilayer insulant and outgassing rate test device Download PDF

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Publication number
CN207488217U
CN207488217U CN201721560845.1U CN201721560845U CN207488217U CN 207488217 U CN207488217 U CN 207488217U CN 201721560845 U CN201721560845 U CN 201721560845U CN 207488217 U CN207488217 U CN 207488217U
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China
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vacuum
test device
thermal conductivity
chamber
rate test
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CN201721560845.1U
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刘霄
徐旭
罗若尹
甘智华
胡潇
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China Jiliang University
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China Jiliang University
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Abstract

The utility model discloses a kind of apparent thermal conductivity of multilayer insulant and outgassing rate test device, mainly including apparent testing device for measuring thermal conductivity, static deflation rate test device, the first vacuum unit.The utility model proposes the schemes that a kind of calorimeter and high vacuum chamber share a set of first vacuum unit, avoid the first vacuum unit and are only used for the wasting of resources caused by the pre- pumping process of high vacuum chamber, save a set of pumped vacuum systems;The heating unit for being used for sample in outgassing rate test device is evenly heated sample using annular-heating silk, and uses PID temperature controller accurate temperature controllings;Flanged joint normal mixture body gas cylinder is reserved by outgassing rate test device supervacuum chamber to realize to the calibration of mass spectrometric original position, avoids frequently vacuum breaking caused by dismounting.

Description

The apparent thermal conductivity of multilayer insulant and outgassing rate test device
Technical field
The utility model belongs to heat-insulating material performance detection field, is specifically related to a kind of apparent thermal conductivity of multilayer insulant Rate and static outgassing rate test device.
Background technology
With the development of China's low temperature industry, the demand to cryogenic liquid is increasing.The storage and transportation of cryogenic liquid is be unable to do without Efficient adiabatic method generally using high vacuum multiple layer heat insulation, mainly utilizes and multilayer parallel is disposed in adiabatic space in cold The metallic reflection screen of wall and the spacer of lower thermal conductivity under high vacuum environment, reach exhausted by reducing all heat transfer paths The purpose of heat.The heat-insulating property of multilayer insulant is generally weighed with apparent thermal conductivity, the quality of heat-insulating property is true by interlayer The influence of reciprocal of duty cycle, when vacuum degree is better than 10-3During Pa, multilayer insulant could keep its good heat-insulating property, work as vacuum degree It is inferior to 10-3During Pa, heat-insulating property can drastically be deteriorated.In addition, multilayer insulant can be released when dissolving, desorb under vacuum conditions Amplification quantity gas causes interlayer vacuum degree to be deteriorated, and then influences insulation effect.
Apparent thermal conductivity and static deflation rate study multilayer heat insulation as the important indicator for weighing multilayer insulant performance The thermal conductivity of material and the relationship of vacuum degree, influence of the material outgassing to vacuum degree have weight to the application of multilayer insulant Want meaning.It invents a kind of apparent thermal conductivity of multilayer insulant and outgassing rate test system surveys above-mentioned performance indicator Amount, the application for heat-insulating material provide reference.
Invention content
The utility model provides a kind of apparent thermal conductivity of multilayer insulant and outgassing rate test device, can be same The measurement of apparent thermal conductivity and static outgassing rate is completed in set system simultaneously, reduces equipment investment.
The utility model specific technical solution is as follows:
A kind of apparent thermal conductivity of multilayer insulant and outgassing rate test device, including apparent testing device for measuring thermal conductivity, Static deflation rate test device and the first vacuum unit;
The apparent testing device for measuring thermal conductivity includes calorimeter, flowmeter, bubbler, Keithly2700 types number ten thousand With table and patch type platinum resistance thermometer;
Calorimeter includes inner cylinder and outer barrel, and two setting-out mouths by top include upper protection by flanged joint, inner cylinder Courage, lower protection courage and the measurement courage between upper and lower protection courage, upper protection courage are connected with lower protection Hymecromone piping, on Protection courage and measurement courage are connected separately with the first bubbler and the second bubbler, and measurement Hymecromone crosses the second bubbler and connects use respectively In measure the flowmeter of nitrogen flow that liquid nitrogen vaporization goes out, for the pressure-detecting device that detects nitrogen pressure and for detecting nitrogen The temperature-detecting device of temperature degree;The patch type platinum resistance thermometer is set in calorimeter, for measuring heat-insulating material The temperature of cold wall and hot wall, patch type platinum resistance thermometer are connected with Keithly2700 type digital multimeter;Platinum resistance thermometer Precision for 0.1K, during test, heat-insulating material is wound in inner cylinder, and it is cold wall that heat-insulating material, which contacts side with inner cylinder, and opposite side is Hot wall, platinum resistance thermometer test heat-insulating material cold wall and the temperature of hot wall respectively;Flowmeter is preferably Alicat flow measurements Amount;Second bubbler makes the low temperature nitrogen evaporated as saturated vapor at room temperature;First bubbler ensures protection courage water column It is higher than measuring courage water column, gas is prevented through being condensed during overprotection courage.
The static deflation rate test device vacuumizes list including high vacuum chamber, supervacuum chamber, gripper, second Member, annular-heating unit, PID temperature controllers, level four bars mass spectrograph, mass spectrograph calibration gas circuit and pressure-detecting device;
High vacuum chamber is connected with supervacuum chamber, and gate valve is provided between high vacuum chamber and supervacuum chamber, and superelevation is true Empty room is connect with the second vacuum unit, and gate valve is provided between supervacuum chamber and the second vacuum unit, and gripper is used In crawl heat-insulating material and high vacuum chamber and supervacuum chamber can be freed in and out;Pressure-detecting device is set to supervacuum chamber It is interior, for detecting ultrahigh vacuum intraventricular pressure force value;Annular-heating unit is set in ultrahigh vacuum room, annular-heating unit with PID temperature controllers are connected;Level four bars mass spectrograph and mass spectrograph calibration gas circuit are connect respectively with supervacuum chamber, mass spectrograph calibration gas circuit For calibrating level four bars mass spectrograph;Using annular-heating silk so as to homogeneous heating, PID temperature controller controls heater strip unit, It is automatically adjusted according to set temperature and the temperature difference, keeps constant temperature, temperature-controlled precision 0.5K.Supervacuum chamber passes through flanged joint Level four bars mass spectrograph, level four bars mass spectrograph are used to detect sample deflation component.
First vacuum unit is connected by triple valve respectively in high vacuum chamber and calorimeter outer barrel and calorimeter The calorimeter enclosure space that cylinder is formed, the triple valve valve are gate valve;Triple valve is with calorimeter enclosure space by setting Put the CF100 flanged joints on calorimeter outer barrel.
Preferably, first vacuum unit is made of molecular pump and mechanical pump, and mechanical pump is connect with molecular pump, molecule Pump is connect with triple valve, and the second vacuum unit is pumped by first order molecular, secondary molecules pump and mechanical pump form, first order molecular pump, Secondary molecules pump and mechanical pump composition is sequentially connected, and first order molecular pump is connect with supervacuum chamber.First vacuum unit can make The vacuum degree of calorimeter enclosure space that high vacuum chamber and calorimeter outer barrel are formed with calorimeter inner cylinder reaches 1 × 10-6Pa.Second Vacuum unit can enable supervacuum chamber vacuum degree up to 1 × 10-7Pa。
Preferably, mass spectrograph calibration gas circuit includes three normal mixture body bottles, and three normal mixture body bottles pass through one A total air valve is connect with supervacuum chamber, and vent valve is respectively arranged between three normal mixture body bottles and total air valve.Mass spectrum Instrument calibration gas circuit is used to verify level four bars mass spectrograph.In normal mixture body bottle for known concentration than H2/N2、H2O/N2、CO2/ N2
Preferably, calorimeter outer barrel wall surface is provided with 6 vacuum interfaces, and vacuum between inner cylinder and outer barrel is measured for connecting The vacuum meter of degree.
Preferably, supervacuum chamber is directly docked with the first order molecular pump of the second vacuum unit, is not connected by bellows It connects.
The utility model passes through valve control using a set of while connect the first vacuum unit of calorimeter and high vacuum chamber System, can realize the vacuumize process to the two respectively.This structure can cause the first vacuum unit to be effectively used. Meanwhile arrange annular-heating silk in supervacuum chamber, supervacuum chamber is made to obtain uniform temperature by PID temperature controllers to survey Measure influence of the different temperatures to material outgassing.In addition, using calibrating gas mixing method to mass spectrograph before carrying out outgassing rate test Original position calibration is carried out, is avoided vacuum breaking caused by mass spectrograph dismounting calibration.
Description of the drawings
Fig. 1 is the connection block diagram of the apparent thermal conductivity of the utility model heat-insulating material and outgassing rate test device;
Fig. 2 is the front view of the apparent thermal conductivity of the utility model heat-insulating material and outgassing rate test device;
Fig. 3 is that the side of the apparent thermal conductivity of the utility model heat-insulating material and outgassing rate test device attempts;
Fig. 4 is the vertical view of the apparent thermal conductivity of the utility model heat-insulating material and outgassing rate test device;
Fig. 5 is the oblique view of the apparent thermal conductivity of the utility model heat-insulating material and outgassing rate test device.
Specific embodiment
The utility model provides a kind of apparent thermal conductivity of multilayer insulant and outgassing rate test device, can be to multilayer Heat-insulating material carries out the measurement of apparent thermal conductivity and static outgassing rate.Have both the mass spectrometric calibration work(of supervacuum chamber simultaneously Energy.Concrete principle is as follows:
Apparent thermal conductivity measuring principle:Calorimetry is evaporated, i.e., after system reaches stable state, is measured from being wound with high vacuum The temperature T of the nitrogen flow V evaporated in the measurement container of multilayer insulant and the hot and cold wall of high vacuum multiple layer heat insulation materialC With TH, heat-insulating material is wound in inner cylinder, and heat-insulating material contacts side with inner cylinder as cold wall, and opposite side is hot wall, with reference to surveying Winding thickness δ, the gas flowmeter exit nitrogen temperature T arrived1, pressure P1, acquired using formula (1) (2) calculating high under the system The apparent thermal conductivity λ of vacuum multi-layer insulation material:
In formula:
Q is leaking heat, unit W;
LvFor the latent heat of vaporization of liquid nitrogen, unit J/kg;
After V stablizes for system, from measuring the flow of nitrogen that evaporates in courage, unit m3/ s is converted to obtain by measured value;
ρ0For the density of nitrogen under standard state (273.15K, 1013kPa), units/kg/m3
P1、T1Flow down the pressure and temperature of gauge exit nitrogen for experimental condition, and unit is respectively kPa, K;
P0、T0For the pressure and temperature under standard state (273.15K, 1013kPa), unit is respectively kPa, K;
λ be apparent thermal conductivity, unit W/ (mK);
TH、TCThe respectively temperature of room temperature and liquid nitrogen, unit K;
R be measure courage outer radius, unit m;
Average winding thickness of the δ for multilayer insulant, unit m;
L be measure courage length, unit m.
Static outgassing rate test philosophy is static pressurizing method:Sample after pumping, closes superelevation in supervacuum chamber Vacuum chamber valve stands one hour, the outgassing rate of supervacuum chamber calculation of pressure sample before and after record is stood.
In formula:
q:It is detected the outgassing rate of heat-insulating material, unit Pam3/s;
p0:Supervacuum chamber pressure value before standing, unit Pa;
p1:Supervacuum chamber pressure value after standing one hour, unit Pa;
Δt:The time range of recorded vacuum cavity vacuum degree variation, unit s;
V:The volume of vacuum cavity, unit m residing for tested heat-insulating material3
Mass spectrograph calibrating principle:Normal mixture body calibration method, i.e., by the normal mixture body of known concentration (generally CO2/N2、H2O/N2、H2/N2) bottle is connected to supervacuum chamber by four-way valve and reserves on CF16 flanges, gas enters ultrahigh vacuum Behind room, gas concentration ratio is recalculated, the ratio of peak that mass spectrograph measures mixed gas spectral peak is opened, by concentration ratio divided by ratio of peak Obtain calibration factor.
The test system structure block diagram of the utility model is shown in Fig. 1, and a kind of three-dimensional structure diagram sees reference Fig. 2, Fig. 3, Fig. 4 and figure 5, including apparent thermal conductivity measuring device, static deflation rate measuring device, the first vacuum unit.
As shown in Figs. 1-5, apparent thermal conductivity device is mainly by calorimeter 26, bubbler, flowmeter 33, patch type platinum resistance Thermometer, Keithly2700 types digital multimeter 36 form.Calorimeter internal measurement courage 28, upper protection courage 30, lower protection courage 27 It fills liquid nitrogen, is sealed after wrapped multiple heat-insulating material 29 by metal flange 37 on the outside of liner, pass through the first vacuum unit and take out Vacuum.External world's leakage thermal conductivity causes to measure courage liquid nitrogen vaporization, and the liquid nitrogen of evaporation is measured by flowing through flowmeter 33 after the second bubbler 32 Liquid nitrogen vaporization amount measures leaking heat and apparent thermal conductivity so as to calculate.
Apparent thermal conductivity device further includes level four bars mass spectrograph and mass spectrograph calibration gas circuit.Mass spectrograph calibration gas circuit includes three A normal mixture body bottle, three normal mixture body bottles are connect by a total air valve 17 with supervacuum chamber, three standards Vent valve 16, vent valve 15 and vent valve 14 are respectively arranged between mixed gas bottle and total air valve.Mass spectrograph calibration gas circuit is used In verification level four bars mass spectrograph.
Mainly by gripper 19, high vacuum chamber 20, supervacuum chamber 5 form static outgassing rate test device.It is ready to Sample place and high vacuum chamber and seal, after the pre- pumping process of the first vacuum unit, gripper 19 passes through telescopic rod 38 Sample is sent into 5 backed off after random of supervacuum chamber, starts the second vacuum unit and sample is evacuated, one is stood after being evacuated several hours Hour measures pressure variety by vacuum meter 8, vacuum meter 6, and then calculates material outgassing rate.
First vacuum unit is made of molecular pump 24 and mechanical pump 25, and mechanical pump 25 is connect with molecular pump 24, molecular pump 24 connect with triple valve, and the second vacuum unit is made of first order molecular pump 3, secondary molecules pump 2 and mechanical pump 1, first order molecular Pump 3, secondary molecules pump 1 and the composition of mechanical pump 1 are sequentially connected, and first order molecular pump 3 is connect with supervacuum chamber 5.
First vacuum unit realizes the vacuumize process to high vacuum chamber and calorimeter interlayer.Carry out outgassing rate experiment When, gate valve 21, gate valve 23 are opened, closes gate valve 22, first starts mechanical pump 25 and treats that high vacuum chamber vacuum degree is less than 10Pa When restart molecular pump 24.When carrying out apparent thermal conductivity experiment, gate valve 22,23 is opened, closes gate valve 21, first starts machinery Pump 25 restarts molecular pump 24 when calorimeter layer vacuum is less than 10Pa.
Before carrying out static outgassing rate test, need to calibrate mass spectrograph 9.Heat-insulating material deflation component is mainly H2、N2、H2O、CO2, prepare known concentration than H2/N2、H2O/N2、CO2/N2Normal mixture body bottle 11, normal mixture body Bottle 12, normal mixture body bottle 13 introduce gas into supervacuum chamber 5 by vent valve, open mass spectrograph 9 and record different component The peak height of spectral peak obtains calibration factor according to concentration ratio and ratio of peak.
When testing the outgassing rate under different temperatures, by 10 set temperature of PID temperature controllers, make annular-heating silk 7 in phase Steady operation at a temperature of answering, loop configuration are conducive to entire supervacuum chamber and are heated evenly.
Measurement process:
1. apparent thermal conductivity test
A) courage 30, measurement courage 28, lower protect is protected to arrange cold wall temperature measuring point on courage 27, and record temperature measuring point on calorimeter Position and number;
B) sample is equably wrapped on calorimeter inner cylinder, and records the winding number of plies, by stylus with a scale six A uniform position measurement thickness of sample, is averaged.
C) the location arrangements hot wall temperature measuring point corresponding with cold wall on the outside of the heat-insulating material wound, and record number;
D) calorimeter inner cylinder is put into calorimeter outer barrel, and seal by hanging apparatus;
E) gate valve 22,23 is opened, closes gate valve 21, starts the first vacuum unit mechanical pump 25, makes laminated vacuum Degree reaches below 10Pa;
F) it fills drying nitrogen to vacuum interlayer to restore to atmospheric pressure, as needed repeatedly e, f process;
G) opening molecular pump 24 makes layer vacuum be better than 10-2Pa protects courage, measures courage, lower protection courage note then up Liquid nitrogen, until liquid nitrogen overflows;
H) courage is protected on calorimeter and measures courage outlet and connects the first bubbler 31, the second bubbler 32 respectively, and adjust Bubbler liquid level makes 31 liquid level of the first bubbler avoid the nitrogen of evaporation through being condensed during overprotection courage higher than courage is measured;
I) it measures courage bubbler exit and connects flowmeter 33, temperature-detecting device 34 and pressure-detecting device 35, Mei Geshi Minute recording flowmeter flow, flowmeter outlet pressure and temperature;
J) formula (1) (2) is substituted into according to surveyed parameter and calculates the apparent thermal conductivity of material.
2. outgassing rate is tested
A) test before mass spectrograph 9 is calibrated first, by known concentration than H2/N2、H2O/N2、CO2/N2Standard mix Gas bottle 11,12,13 is closed to be connected on the reserved flange of supervacuum chamber by air valve;
B) start the second vacuum unit and 10 are pumped to supervacuum chamber-2Pa opens mass spectrograph 9, by normal mixture Body is passed through supervacuum chamber, records H2/N2、H2O/N2、CO2/N2Spectral peak;
C) H is recalculated2/N2、H2O/N2、CO2/N2Concentration ratio, adjust mass spectrograph so that the spectral peak of calibrating gas component Than being equal to its concentration ratio, calibration is completed;
D) pass through 105 DEG C before sample test, be dried for 24 hours;
E) high vacuum chamber 20 is put into after the samples weighing handled well, is clamped by gripper 19, and seal;
F) open gate valve 21,23, close gate valve 22, by the first vacuum unit to sample be evacuated one hour, together When open gate valve 4, start the second vacuum unit supervacuum chamber is evacuated;
H) after one hour, gate valve 18 is opened, sample is sent by supervacuum chamber backed off after random by gripper, closes plate Valve 18 is evacuated material one hour in supervacuum chamber;
I) after being evacuated one hour, 8 pressure measurement force value of ionization gauge are recorded, close gate valve 4, sample are made to stand deflation one small When, it opens simultaneously mass spectrograph 9 and records deflation component spectral peak;
J) after standing one hour, 8 pressure measurement force value of ionization gauge are recorded, film is advised 6 pressure measurement force value as reference, protected simultaneously Spectroscopy data is deposited, opens gate valve 4, continues pumping one hour to supervacuum chamber;
K) formula (3) will be substituted into and measures outgassing rate after material is evacuated two hours;
L) i, j are repeated and then can must be evacuated three, four ... the outgassing rates of N hours.
Embodiment described above is a kind of preferable scheme of the utility model, and so it is not to limit this practicality It is novel.Those of ordinary skill in technical field, can be in the case where not departing from the spirit and scope of the utility model It makes a variety of changes and modification.Therefore the technical solution that all modes for taking equivalent substitution or equivalent transformation are obtained, all falls within In the scope of protection of the utility model.

Claims (5)

1. a kind of apparent thermal conductivity of multilayer insulant and outgassing rate test device, which is characterized in that including apparent thermal conductivity Test device, static deflation rate test device and the first vacuum unit;
The apparent testing device for measuring thermal conductivity includes calorimeter, flowmeter, bubbler, Keithly2700 type digital multimeter With patch type platinum resistance thermometer;
Calorimeter includes inner cylinder and outer barrel, two setting-out mouths by top by flanged joint, inner cylinder include upper protection courage, under Courage and the measurement courage between upper and lower protection courage are protected, upper protection courage is connected with lower protection Hymecromone piping, upper protection courage The first bubbler and the second bubbler are connected separately with courage is measured, measurement Hymecromone crosses the second bubbler and connects to measure respectively The flowmeter for the nitrogen flow that liquid nitrogen vaporization goes out, for the pressure-detecting device that detects nitrogen pressure and for detecting nitrogen temperature Temperature-detecting device;The patch type platinum resistance thermometer is set in calorimeter, for measure heat-insulating material cold wall and The temperature of hot wall, patch type platinum resistance thermometer are connected with Keithly2700 type digital multimeter;
The static deflation rate test device includes high vacuum chamber, supervacuum chamber, gripper, the second vacuum unit, ring Shape heating unit, PID temperature controllers, level four bars mass spectrograph, mass spectrograph calibration gas circuit and pressure-detecting device;
High vacuum chamber is connected with supervacuum chamber, and gate valve, supervacuum chamber are provided between high vacuum chamber and supervacuum chamber It is connect with the second vacuum unit, gate valve is provided between supervacuum chamber and the second vacuum unit, gripper is used to grab It takes heat-insulating material and high vacuum chamber and supervacuum chamber can be freed in and out;Pressure-detecting device is set in ultrahigh vacuum room, is used In detection ultrahigh vacuum intraventricular pressure force value;Annular-heating unit is set in ultrahigh vacuum room, annular-heating unit and PID temperature controls Instrument is connected;Level four bars mass spectrograph and mass spectrograph calibration gas circuit are connect respectively with supervacuum chamber, and mass spectrograph calibration gas circuit is used for school Quasi- level four bars mass spectrograph;
First vacuum unit connects high vacuum chamber and calorimeter outer barrel and calorimeter inner cylindrical by triple valve respectively Into calorimeter enclosure space, the triple valve valve be gate valve;Triple valve is with calorimeter enclosure space by being arranged on CF100 flanged joints on calorimeter outer barrel.
2. a kind of apparent thermal conductivity of multilayer insulant and outgassing rate test device, feature exist as described in claim 1 It is made of in first vacuum unit molecular pump and mechanical pump, mechanical pump is connect with molecular pump, molecular pump and triple valve Connection, the second vacuum unit is pumped by first order molecular, secondary molecules pump and mechanical pump form, first order molecular pump, secondary molecules pump It is sequentially connected with mechanical pump composition, first order molecular pump is connect with supervacuum chamber.
3. a kind of apparent thermal conductivity of multilayer insulant and outgassing rate test device, feature exist as described in claim 1 Include three normal mixture body bottles in the mass spectrograph calibration gas circuit, three normal mixture body bottles pass through a total air valve It is connect with supervacuum chamber, vent valve is respectively arranged between three normal mixture body bottles and total air valve.
4. a kind of apparent thermal conductivity of multilayer insulant and outgassing rate test device, feature exist as described in claim 1 The calorimeter outer barrel wall surface is provided with 6 vacuum interfaces, the true of vacuum degree between inner cylinder and outer barrel is measured for connecting Sky meter.
5. a kind of apparent thermal conductivity of multilayer insulant and outgassing rate test device, feature exist as described in claim 1 It directly docks, is not connected by bellows with the first order molecular pump of the second vacuum unit in the supervacuum chamber.
CN201721560845.1U 2017-11-21 2017-11-21 The apparent thermal conductivity of multilayer insulant and outgassing rate test device Expired - Fee Related CN207488217U (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110907151A (en) * 2019-10-23 2020-03-24 张家港富瑞特种装备股份有限公司 Method for measuring and calculating relationship between vacuum degree of low-temperature gas cylinder and daily evaporation rate and adsorption capacity
CN111505047A (en) * 2020-04-24 2020-08-07 清华大学 Device for measuring heat conductivity of high-temperature high-pressure multi-element gas mixture
CN113390920A (en) * 2021-06-25 2021-09-14 连云港中远海运特种装备制造有限公司 Heat-insulating material performance testing device and testing method

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110907151A (en) * 2019-10-23 2020-03-24 张家港富瑞特种装备股份有限公司 Method for measuring and calculating relationship between vacuum degree of low-temperature gas cylinder and daily evaporation rate and adsorption capacity
CN111505047A (en) * 2020-04-24 2020-08-07 清华大学 Device for measuring heat conductivity of high-temperature high-pressure multi-element gas mixture
CN113390920A (en) * 2021-06-25 2021-09-14 连云港中远海运特种装备制造有限公司 Heat-insulating material performance testing device and testing method

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