CN110865002A - High-precision material outgassing rate testing system and testing method thereof - Google Patents
High-precision material outgassing rate testing system and testing method thereof Download PDFInfo
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N7/00—Analysing materials by measuring the pressure or volume of a gas or vapour
- G01N7/14—Analysing materials by measuring the pressure or volume of a gas or vapour by allowing the material to emit a gas or vapour, e.g. water vapour, and measuring a pressure or volume difference
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N7/00—Analysing materials by measuring the pressure or volume of a gas or vapour
- G01N7/14—Analysing materials by measuring the pressure or volume of a gas or vapour by allowing the material to emit a gas or vapour, e.g. water vapour, and measuring a pressure or volume difference
- G01N7/16—Analysing materials by measuring the pressure or volume of a gas or vapour by allowing the material to emit a gas or vapour, e.g. water vapour, and measuring a pressure or volume difference by heating the material
Abstract
The invention discloses a high-precision material outgassing rate testing system and a testing method thereof, belonging to the field of high-precision material outgassing rate testing, comprising a first vacuum chamber, a second vacuum chamber, a third vacuum chamber, a first small hole element, a second small hole element, a first vacuum gauge, a second vacuum gauge, a third vacuum gauge, a mechanical pump, a first molecular pump, a second molecular pump, a first vacuum valve, a second vacuum valve, a third vacuum valve, a fourth vacuum valve, a fifth vacuum valve, a sixth vacuum valve, a seventh vacuum valve, an eighth vacuum valve and a ninth vacuum valve, wherein the system comprises a symmetrical structure material outgassing testing device and a temperature control unit, two measuring chambers with the same structure and size are adopted, the symmetrical structure material outgassing testing system realizes the simultaneous measurement of background outgassing of a sample and the testing system, not only improves the measuring precision, and the original measuring process is shortened by a half, and the measuring efficiency is improved.
Description
Technical Field
The invention belongs to the field of high-precision material outgassing rate testing, and particularly relates to a high-precision material outgassing rate testing system and a high-precision material outgassing rate testing method.
Background
Under vacuum conditions, gases adsorbed on the surface of the material or gases inside the material can be released, which is called material outgassing. In space, the deflation of surrounding structural materials can cause pollution to key components such as a lens of a meteorological observation satellite, and the like, so that the service life and the performance of the meteorological observation satellite are greatly reduced; in other ultra-high vacuum applications, material outgassing can also be an obstacle to achieving and maintaining a limited vacuum. In order to ensure that components applied under vacuum conditions in industries such as aerospace equipment, basic electronics industry, nuclear industry, high-energy physics, advanced medical devices, and the like can be used normally, accurate measurement of the outgassing rate of materials applied in vacuum is required. In addition, the temperature is one of the main factors influencing the material outgassing, and the establishment of a wide temperature range material testing system from a liquid nitrogen temperature region to a high temperature region has important significance in the measurement and evaluation of the material outgassing. In the aspect of material outgassing measurement, methods commonly used internationally currently include an accumulation method and a dynamic flow method, and a conductance modulation method, a switching gas path method and the like extended from the dynamic flow method. In the literature, "Measurement system for low-out materials by switching between two pumping paths," Vacuum "1996, 6 th to 8 th pages 749 to 752, a test apparatus based on a gas path switching method is proposed; the document "research on measuring the outgassing rate of a material by a small-hole flow guide method", vacuum, 2010, No. 3, pages 55-58, proposes a testing device for the outgassing rate of a material based on a dynamic flow method. However, the main problem of the existing material outgassing test is that the background outgassing of the test chamber, the influence factors such as the vacuum gauge, the leak hole, the temperature and the like bring great uncertainty (over 50%) to the material outgassing rate test device, and even if the key measurement components such as the vacuum gauge, the leak hole and the like are calibrated, the overall measurement accuracy of the device is difficult to improve. In addition, the two devices adopt a method of firstly testing the sample and then testing the background, and the method has the defects that the consistency of two times of respective tests is poor, the influence of the background is very large, great deviation is caused, the maximum influence can reach 2 orders of magnitude, the requirements of testing a small-volume sample or a sample with a small air release rate cannot be met, and the screening and the service life evaluation of the vacuum device material are seriously influenced. In addition, materials applied in the fields of aerospace, high energy physics and the like generally face harsh environmental conditions, such as extremely high and low temperature conditions, so that the outgassing rate of the materials under the high and low temperature conditions can be measured.
Disclosure of Invention
The invention aims to solve the technical problem that aiming at the requirements of wide temperature range and high precision test on the material outgassing rate of a sample with a small outgassing rate, the invention provides a high precision material outgassing rate test system with a temperature range of-175-1000 ℃ and a test method thereof, which realize the simultaneous measurement of the background outgassing of the sample and the test system, not only improve the measurement precision, but also shorten the original measurement process by half and improve the measurement efficiency.
The invention adopts the following technical scheme to solve the technical problems
A high-precision material outgassing rate testing system comprises a first vacuum chamber, a second vacuum chamber, a third vacuum chamber, a first small hole element, a second small hole element, a first vacuum gauge, a second vacuum gauge, a third vacuum gauge, a mechanical pump, a first molecular pump, a second molecular pump, a first vacuum valve, a second vacuum valve, a third vacuum valve, a fourth vacuum valve, a fifth vacuum valve, a sixth vacuum valve, a seventh vacuum valve, an eighth vacuum valve and a ninth vacuum valve;
wherein, the mechanical pump is respectively connected with one end of a first vacuum valve and one end of a second vacuum valve, the other end of the first vacuum valve is connected with the air exhaust outlet of a first molecular pump, the air exhaust inlet of the first molecular pump is connected with the air exhaust outlet of the second molecular pump, the air exhaust inlet of the second molecular pump is connected with a fourth vacuum valve, the other end of the fourth vacuum valve is connected with one end of a third vacuum chamber, the other end of the vacuum valve is respectively connected with one end of a first vacuum gauge, one end of a third vacuum valve and one end of the first vacuum chamber, the other end of the third vacuum valve is respectively connected with one end of a sixth vacuum valve, one end of a first small hole element and the other end of the first vacuum chamber, the other end of the first small hole element is connected with the other end of the third vacuum chamber through a fifth vacuum valve, the other end of the sixth vacuum valve is respectively connected with one end of the second vacuum gauge, one end of a seventh vacuum valve is connected, the other end of the seventh vacuum valve is respectively connected with one end of the second small-hole element and one end of the second vacuum chamber, the other end of the second small-hole element is connected with the third vacuum chamber through an eighth vacuum valve, one ends of a third vacuum gauge and a ninth vacuum valve are respectively connected with one end of the third vacuum chamber, and the other end of the vacuum valve is connected with the first ion pump;
and temperature control units are arranged around the first vacuum chamber and the second vacuum chamber and comprise a tubular furnace heating device and a two-way liquid nitrogen refrigerating device.
As a further preferable scheme of the high-precision material outgassing rate testing system, the first vacuum chamber and the second vacuum chamber are both made of high-purity quartz, and the outgassing rate is less than 1 x 10-16Pam3/(scm2)。
As a further preferable scheme of the high-precision material outgassing rate testing system, the first vacuum chamber, the second vacuum chamber and a flange joint connected with the first vacuum chamber and the second vacuum chamber are machined by a high-precision machine tool, the high-precision machine tool is guaranteed to have the same structure and size, the machining process adopts ultrahigh vacuum treatment including cleaning, high-temperature annealing and film coating, the whole baking and degassing treatment is carried out periodically during the use period, and the baking temperature is set to be 150 ℃.
As a further preferable scheme of the high-precision material outgassing rate testing system, the second vacuum gauge is respectively connected with the first vacuum chamber and the second vacuum chamber through a sixth vacuum valve and a seventh vacuum valve; the first vacuum gauge is a full-scale vacuum gauge whose full-scale is 1000Torr as a monitoring vacuum gauge, and the second vacuum gauge and the third vacuum gauge are ultra-high vacuum separation gauges as a sub-reference standard.
As a further preferable scheme of the high-precision material outgassing rate testing system, the tubular furnace heating device adopts two tubular furnaces for respectively heating the sample chamber and the reference chamber, and the heating temperature can reach 1000 ℃; the double-path liquid nitrogen refrigerating device adopts a double-path liquid nitrogen refrigerating system and is used for refrigerating the measuring chamber and the reference chamber simultaneously, and the refrigerating temperature can reach-175 ℃.
As a further preferred scheme of the high-precision material outgassing rate testing system, the two-way liquid nitrogen refrigerating device consists of 2 vacuum constant-temperature cavities, a two-way temperature control device, a self-pressurization liquid nitrogen tank, a low-temperature control valve, a mechanical pump and a two-channel temperature measuring instrument and is used for synchronously refrigerating the measuring chamber and the sample chamber.
As a further preferable scheme of the high-precision material outgassing rate testing system, the tubular furnace heating device and the two-way liquid nitrogen refrigerating device are both in modular design, and the bottom of the tubular furnace heating device and the two-way liquid nitrogen refrigerating device are provided with guide rail structures, so that the tubular furnace heating device and the two-way liquid nitrogen refrigerating device are convenient to move, disassemble and assemble, and the time interval for switching high and low temperature testing conditions is shortened.
A testing method based on a high-precision material outgassing rate testing system specifically comprises the following steps:
step 2, opening and monitoring a first vacuum gauge, a first mechanical pump, a first vacuum valve, a second vacuum valve, a third vacuum valve, a fourth vacuum valve, a fifth vacuum valve, a sixth vacuum valve, a seventh vacuum valve, an eighth vacuum valve and a ninth vacuum valve in sequence to vacuumize the system; when the indication number of the first vacuum gauge is monitored to be less than 10Pa, closing the second vacuum valve and the third vacuum valve, and sequentially starting the first molecular pump and the second molecular pump to vacuumize the first vacuum chamber, the second vacuum chamber and the third vacuum chamber; when the first vacuum gauge is detected to be less than 1 × 10-3When Pa, the first ion pump, the second vacuum gauge and the third vacuum gauge are opened;
step 3, a heating device or a refrigerating device is arranged at the first vacuum chamber and the second vacuum chamber by utilizing a guide rail mechanism, the temperature is set according to requirements, and heating or refrigerating is started;
step 4, after the temperature reaches the set temperature and is stabilized for 1 hour, using the second stepTwo vacuum gauges measure the vacuum degree of the first vacuum chamber and the second vacuum chamber respectively, and the vacuum degree is pa、pb(ii) a Then repeating the above process every 1h, recording a group of pa0、pb0Testing for 24h, and reading 25 groups of data;
step 5, after the test is finished, stopping the heating device or the refrigerating device, stopping air extraction after the room temperature is recovered, filling high-purity nitrogen into the sample chamber, and removing the heating device or the refrigerating device;
step 6, according to a formula Qoutgasing＝C·[(pa-pa0)-(pb-pb0)]Calculating to obtain the gas flow released by the material at each moment;
wherein Q isoutgasingFor the gas flow released by the material at each moment, C is a constant;
if the geometric surface area a of the sample to be measured is known, the gas flow rate released by the material at each time point is calculated in the detecting step S4, and can be represented by the formula q QoutgasingThe corresponding air release rate q is obtained by the calculation of/A, and the test result can be represented by an air release rate-time relation curve or a table.
Compared with the prior art, the invention adopting the technical scheme has the following technical effects:
1. the invention adopts a system comprising a symmetrical structure material deflation testing device and a temperature control unit, and adopts two measuring chambers with the same structure and size, wherein one measuring chamber is used as a sample chamber for measuring the deflation of a sample, and the other measuring chamber is used as a reference chamber for measuring the background deflation of the testing device. The material deflation test system with the symmetrical structure realizes the simultaneous measurement of background deflation of the sample and the test system, not only improves the measurement precision, but also shortens the original measurement process by half and improves the measurement efficiency;
2. the system also comprises a heating and refrigerating device with special design, and the temperature of the material outgassing sample is expanded to-175-1000 ℃. The heating device adopts two tubular furnaces to respectively heat the sample chamber and the reference chamber, and the heating temperature can reach 1000 ℃; the refrigerating device adopts a specially designed two-way liquid nitrogen refrigerating system, and can simultaneously refrigerate the measuring chamber and the reference chamber, and the refrigerating temperature can reach-175 ℃;
3. the heating and refrigerating devices are in modular design, the guide rails are arranged at the bottoms of the heating and refrigerating devices, the heating and refrigerating devices are convenient to move, disassemble and assemble, and the time interval for switching the high-temperature and low-temperature test conditions is shortened.
Drawings
FIG. 1 is a schematic structural diagram of a high-precision material outgassing rate testing system according to the present invention.
Detailed Description
The technical solution of the present invention is further described in detail below with reference to the accompanying drawings.
A high-precision material outgassing rate testing system, as shown in FIG. 1, comprises a first vacuum chamber VC1, a second vacuum chamber VC2, a third vacuum chamber VC3, a first small-hole element C1, a second small-hole element C2, a first vacuum gauge G1, a second vacuum gauge G2, a third vacuum gauge G3, a mechanical pump RP1, a first molecular pump TMP1, a second molecular pump TMP2, a first vacuum valve V1, a second vacuum valve V2, a third vacuum valve V3, a fourth vacuum valve V4, a fifth vacuum valve V5, a sixth vacuum valve V6, a seventh vacuum valve V7, an eighth vacuum valve V8 and a ninth vacuum valve V9.
Wherein, the mechanical pump RP1 is respectively connected with one end of a first vacuum valve V1 and one end of a second vacuum valve V2, the other end of the first vacuum valve V1 is connected with the pumping outlet of a first molecular pump TMP1, the pumping inlet of the first molecular pump TMP1 is connected with the pumping outlet of a second molecular pump TMP2, the pumping inlet of the second molecular pump TMP2 is connected with a fourth vacuum valve V4, the other end of the fourth vacuum valve V4 is connected with one end of a third vacuum chamber VC3, the other end of the vacuum valve V2 is respectively connected with one end of a first vacuum gauge G1, one end of a third vacuum valve V3 and one end of a first vacuum chamber VC1, the other end of the third vacuum valve V3 is respectively connected with one end of a sixth vacuum valve V6, one end of a first small-hole element C1 and the other end of the first vacuum chamber VC1, the other end of the first small-hole element C5 is connected with the other end of the third vacuum chamber VC3 through a fifth vacuum valve V5, the other end of the sixth vacuum valve V6 is respectively connected with one end of a second vacuum gauge G2 and one end of a seventh vacuum valve V7, the other end of the seventh vacuum valve V7 is respectively connected with one end of a second small hole element C2 and one end of a second vacuum chamber VC2, the other end of the second small hole element C2 is connected with a third vacuum chamber VC3 through an eighth vacuum valve V8, one ends of the third vacuum gauge G3 and the ninth vacuum valve V9 are respectively connected with one end of a third vacuum chamber VC3, and the other end of the vacuum valve V9 is connected with a first ion pump SIP 1.
Temperature control units are arranged around the first vacuum chamber VC1 and the second vacuum chamber VC2, and each temperature control unit comprises a tube furnace heating device and a two-way liquid nitrogen refrigerating device.
The first vacuum chamber VC1 and the second vacuum chamber VC2 are both made of high-purity quartz, and the body gas release rate is less than 1 x 10-16Pam3/(scm 2).
The first vacuum chamber VC1, the second vacuum chamber VC2 and a flange joint connected with the first vacuum chamber VC1 and the second vacuum chamber VC2 are all machined by a high-precision machine tool, the guarantee, the structure and the size are all the same, the machining process adopts ultrahigh vacuum treatment, including cleaning, high-temperature annealing and film coating, integral baking and degassing treatment are carried out periodically during use, and the baking temperature is set to be 150 ℃.
The second vacuum gauge G2 is respectively connected with the first vacuum chamber VC1 and the second vacuum chamber VC2 through a sixth vacuum valve V6 and a seventh vacuum valve V7; the first gauge G1 is a full-scale gauge for monitoring full-scale of the gauge at 1000Torr, and the second gauge G2 and the third gauge G3 are ultra-high vacuum separation gauges as sub-reference standards.
The tubular furnace heating device adopts two tubular furnaces for respectively heating the sample chamber and the reference chamber, and the heating temperature can reach 1000 ℃; the double-path liquid nitrogen refrigerating device adopts a double-path liquid nitrogen refrigerating system and is used for refrigerating the measuring chamber and the reference chamber simultaneously, and the refrigerating temperature can reach-175 ℃.
The double-path liquid nitrogen refrigerating device consists of 2 vacuum constant temperature cavities, a double-path temperature control device, a self-pressurization liquid nitrogen tank, a low-temperature control valve, a mechanical pump and a double-path temperature measuring instrument and is used for synchronously refrigerating the measuring chamber and the sample chamber.
The tube furnace heating device and the double-path liquid nitrogen refrigerating device are in modular design, the guide rail structure is arranged at the bottom of the tube furnace heating device and the double-path liquid nitrogen refrigerating device, the tube furnace heating device and the double-path liquid nitrogen refrigerating device are convenient to move, disassemble and assemble, and the time interval for switching high and low temperature test conditions is shortened.
A testing method based on a high-precision material outgassing rate testing system specifically comprises the following steps:
step 2, opening and monitoring a first vacuum gauge G1, a first mechanical pump RP1, a first vacuum valve V1, a second vacuum valve V2, a third vacuum valve V3, a fourth vacuum valve V4, a fifth vacuum valve V5, a sixth vacuum valve V6, a seventh vacuum valve V7, an eighth vacuum valve V8 and a ninth vacuum valve V9 in sequence to vacuumize the system; when the indication number of the first vacuum gauge G1 is monitored to be less than 10Pa, the second vacuum valve V2 and the third vacuum valve V3 are closed, and the first molecular pump TMP1 and the second molecular pump TMP2 are sequentially started to vacuumize the first vacuum chamber VC1, the second vacuum chamber VC2 and the third vacuum chamber VC 3; when the indication number of the first vacuum gauge G1 is monitored to be less than 1 x 10 < -3 > Pa, the first ion pump SIP1, the second vacuum gauge G2 and the third vacuum gauge G3 are turned on;
step 3, a heating device or a refrigerating device is arranged at the first vacuum chamber VC1 and the second vacuum chamber VC2 by utilizing a guide rail mechanism, and the heating or the refrigerating is started according to the set temperature required;
step 4, after the temperature reaches the set temperature and is stabilized for 1 hour, respectively measuring the vacuum degrees of the first vacuum chamber VC1 and the second vacuum chamber VC2 by using a second vacuum meter G2, wherein the vacuum degrees are respectively measured as pa、pb(ii) a Then repeating the above process every 1h, recording a group of pa0、pb0Testing for 24h, and reading 25 groups of data;
step 5, after the test is finished, stopping the heating device or the refrigerating device, stopping air extraction after the room temperature is recovered, filling high-purity nitrogen into the sample chamber, and removing the heating device or the refrigerating device;
step 6, according to a formula Qoutgasing＝C·[(pa-pa0)-(pb-pb0)]Calculating to obtain the gas flow released by the material at each moment;
wherein Q isoutgasingFor each time materialThe gas flow released by the material, C is a constant;
if the geometric surface area a of the sample to be measured is known, the gas flow rate released by the material at each time point is calculated in the detection step S4, and can be represented by the formula Q-QoutgasingThe corresponding air release rate q is obtained by the calculation of/A, and the test result can be represented by an air release rate-time relation curve or a table.
The invention adopts a system comprising a symmetrical structure material deflation testing device and a temperature control unit, and adopts two measuring chambers with the same structure and size, wherein one measuring chamber is used as a sample chamber for measuring the deflation of a sample, and the other measuring chamber is used as a reference chamber for measuring the background deflation of the testing device. The material deflation test system with the symmetrical structure realizes the simultaneous measurement of background deflation of the sample and the test system, not only improves the measurement precision, but also shortens the original measurement process by half and improves the measurement efficiency. In addition, the system also comprises a heating and refrigerating device which is specially designed, and the measured temperature of the material outgassing sample is expanded to-175-1000 ℃. The heating device adopts two tubular furnaces to respectively heat the sample chamber and the reference chamber, and the heating temperature can reach 1000 ℃; the refrigerating device adopts a specially designed double-path liquid nitrogen refrigerating system, can simultaneously refrigerate the measuring chamber and the reference chamber, and the refrigerating temperature can reach-175 ℃. The heating and refrigerating devices are in modular design, the guide rails are arranged at the bottoms of the heating and refrigerating devices, the heating and refrigerating devices are convenient to move, disassemble and assemble, and the time interval for switching the high-temperature and low-temperature test conditions is shortened.
Claims (8)
1. The utility model provides a high accuracy material gassing rate test system which characterized in that: comprises a first vacuum chamber (VC1), a second vacuum chamber (VC2), a third vacuum chamber (VC3), a first small-hole element (C1), a second small-hole element (C2), a first vacuum gauge (G1), a second vacuum gauge (G2), a third vacuum gauge (G3), a mechanical pump (RP1), a first molecular pump (TMP1), a second molecular pump (TMP2), a first vacuum valve (V1), a second vacuum valve (V2), a third vacuum valve (V3), a fourth vacuum valve (V4), a fifth vacuum valve (V5), a sixth vacuum valve (V6), a seventh vacuum valve (V7), an eighth vacuum valve (V8) and a ninth vacuum valve (V9);
wherein, the mechanical pump (RP1) is respectively connected with one end of a first vacuum valve (V1) and one end of a second vacuum valve (V2), the other end of the first vacuum valve (V1) is connected with the pumping outlet of a first molecular pump (TMP1), the pumping inlet of the first molecular pump (TMP1) is connected with the pumping outlet of a second molecular pump (TMP2), the pumping inlet of the second molecular pump (TMP2) is connected with a fourth vacuum valve (V4), the other end of the fourth vacuum valve (V4) is connected with one end of a third vacuum chamber (VC3), the other end of the vacuum valve (V2) is respectively connected with one end of a first vacuum gauge (G1), one end of a third vacuum valve (V3), one end of a first vacuum chamber (VC1), the other end of the third vacuum valve (V3) is respectively connected with one end of a sixth vacuum valve (V6), one end of a first pinhole element (C1) and one end of the first vacuum chamber (VC1), the other end of the first small hole element (C1) is connected with the other end of a third vacuum chamber (VC3) through a fifth vacuum valve (V5), the other end of a sixth vacuum valve (V6) is respectively connected with one end of a second vacuum gauge (G2) and one end of a seventh vacuum valve (V7), the other end of the seventh vacuum valve (V7) is respectively connected with one end of the second small hole element (C2) and one end of the second vacuum chamber (VC2), the other end of the second small hole element (C2) is connected with the third vacuum chamber (VC3) through an eighth vacuum valve (V8), one ends of the third vacuum gauge (G3) and the ninth vacuum valve (V9) are respectively connected with one end of the third vacuum chamber (VC3), and the other end of the vacuum valve (V9) is connected with a first ion pump (SIP 1);
temperature control units are arranged around the first vacuum chamber (VC1) and the second vacuum chamber (VC2), and each temperature control unit comprises a tube furnace heating device and a two-way liquid nitrogen refrigerating device.
2. A high precision material outgassing rate testing system according to claim 1, wherein the first vacuum chamber (VC1) and the second vacuum chamber (VC2) are made of high purity quartz, and the outgassing rate is less than 1 x 10-16Pam3/(scm2)。
3. A high-precision material outgassing rate testing system according to claim 1, wherein the first vacuum chamber (VC1) and the second vacuum chamber (VC2), and the flange joint connected with the first vacuum chamber and the second vacuum chamber are all processed by a high-precision machine tool, the structure and the size are the same, the processing process adopts ultrahigh vacuum treatment including cleaning, high temperature annealing and coating, the whole baking and degassing treatment is carried out periodically during the use period, and the baking temperature is set at 150 ℃.
4. A high precision material outgassing rate testing system according to claim 1, wherein the second vacuum gauge (G2) is connected to the first vacuum chamber (VC1) and the second vacuum chamber (VC2) through the sixth vacuum valve (V6) and the seventh vacuum valve (V7), respectively; the first gauge (G1) is a full-scale gauge for monitoring full-scale 1000Torr of the gauge, and the second gauge (G2) and the third gauge (G3) are ultra-high vacuum separation gauges as a sub-reference standard.
5. The high-precision material outgassing rate testing system according to claim 1, wherein the tube furnace heating device employs two tube furnaces, which respectively heat the sample chamber and the reference chamber, and the heating temperature is up to 1000 ℃; the double-path liquid nitrogen refrigerating device adopts a double-path liquid nitrogen refrigerating system, and simultaneously refrigerates the measuring chamber and the reference chamber, wherein the refrigerating temperature reaches-175 ℃.
6. A high accuracy material gassing rate test system of claim 5 wherein, the double-circuit liquid nitrogen refrigerating plant comprises 2 vacuum thermostatic chambers, double-circuit temperature control device, self-pressurizing liquid nitrogen tank, low temperature control valve, mechanical pump, binary channels thermoscope for realize to measuring room and sample room synchronous refrigeration.
7. A high accuracy material gassing rate test system according to claim 6 wherein, said tube furnace heating device and two-way liquid nitrogen refrigerating plant all adopt the modular design and bottom is equipped with the guide rail structure, can remove and dismouting in order to shorten the time interval that high low temperature test condition switches.
8. A testing method based on the high-precision material outgassing rate testing system of any one of claims 1 to 7, which comprises the following steps:
step 1, loading a cleaned and dried sample to be tested into a sample chamber;
step 2, opening and monitoring a first vacuum gauge (G1), a first mechanical pump (RP1), a first vacuum valve (V1), a second vacuum valve (V2), a third vacuum valve (V3), a fourth vacuum valve (V4), a fifth vacuum valve (V5), a sixth vacuum valve (V6), a seventh vacuum valve (V7), an eighth vacuum valve (V8) and a ninth vacuum valve (V9) in sequence to vacuumize the system; when the indication number of the first vacuum gauge (G1) is monitored to be less than 10Pa, the second vacuum valve (V2) and the third vacuum valve (V3) are closed, and the first molecular pump (TMP1) and the second molecular pump (TMP2) are sequentially started to vacuumize the first vacuum chamber (VC1), the second vacuum chamber (VC2) and the third vacuum chamber (VC 3); when the detected indication number of the first vacuum gauge (G1) is less than 1 x 10-3When Pa, the first ion pump (SIP1), the second vacuum gauge (G2) and the third vacuum gauge (G3) are turned on;
step 3, a heating device or a refrigerating device is arranged at the first vacuum chamber (VC1) and the second vacuum chamber (VC2) by utilizing a guide rail mechanism, and the heating or the refrigerating is started according to the set temperature required;
step 4, after the temperature reaches the set temperature and is stabilized for 1 hour, respectively measuring the vacuum degrees of the first vacuum chamber (VC1) and the second vacuum chamber (VC2) by using a second vacuum meter (G2), wherein the vacuum degrees are respectively counted as pa、pb(ii) a Then repeating the above process every 1h, recording a group of pa0、pb0Testing for 24h, and reading 25 groups of data;
step 5, after the test is finished, stopping the heating device or the refrigerating device, stopping air extraction after the room temperature is recovered, filling high-purity nitrogen into the sample chamber, and removing the heating device or the refrigerating device;
step 6, according to a formula Qoutgasing＝C·[(pa-pa0)-(pb-pb0)]Calculating to obtain the gas flow released by the material at each moment;
wherein Q isoutgasingThe flow of gas released for the material at each moment, C beingA constant value; if the geometric surface area a of the sample to be measured is known, the gas flow rate released by the material at each time point is calculated in the detection step S4, and can be represented by the formula Q-QoutgasingThe corresponding air release rate q is obtained by the calculation of/A, and the test result can be represented by an air release rate-time relation curve or a table.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112304804A (en) * | 2020-10-28 | 2021-02-02 | 北京东方计量测试研究所 | Material outgassing rate testing system and testing method thereof |
| CN112683726A (en) * | 2020-12-01 | 2021-04-20 | 中国科学院近代物理研究所 | Device and method for testing air yield of material |
| CN114113285A (en) * | 2021-12-08 | 2022-03-01 | 中国工程物理研究院材料研究所 | Mechanism and method for measuring air release rate of metal material |
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