CN-116773639-B - Dewar internal atmosphere test analysis device and test analysis method thereof

CN116773639BCN 116773639 BCN116773639 BCN 116773639BCN-116773639-B

Abstract

The invention discloses a Dewar internal atmosphere test analysis device and a test analysis method, wherein the device comprises a first valve, a first molecular pump, a first isolation valve, a first dry pump, a quadrupole mass spectrometer, a second valve, a high vacuum gauge, a heating cover, a Dewar component to be tested, a heating cover bracket, a composite vacuum gauge, a third valve, a second molecular pump, a second isolation valve and a second dry pump; the quadrupole mass spectrometer and the high vacuum gauge form a test analysis system, the heating cover, the Dewar component to be tested and the composite vacuum gauge form a gas accumulation heating system, the first dry pump, the first isolation valve, the first molecular pump and the first valve form a main air exhaust system, the second dry pump, the second isolation valve, the second molecular pump and the third valve form an auxiliary air exhaust system, and the test analysis system is connected with the gas accumulation heating system through the second valve. The invention adopts a static accumulation method to improve the sensitivity, and adopts independent air extraction to avoid equipment from polluting a gas accumulation heating system.

Inventors

ZHANG YAPING
LI JIE
WANG YAN
CHEN ZHENGCHAO
GAO LING
HE JING
YANG MANYUN

Assignees

昆明物理研究所

Dates

Publication Date: 20260512
Application Date: 20230526

Claims (9)

1. The method for testing and analyzing the internal atmosphere of the Dewar comprises the steps of utilizing a Dewar internal atmosphere testing and analyzing device, wherein the device comprises a first valve (1), a first molecular pump (2), a first isolating valve (3), a first dry pump (4), a quadrupole mass spectrometer (5), a second valve (6), a high vacuum gauge (7), a heating cover (8), a Dewar component (9) to be tested, a heating cover bracket (10), a composite vacuum gauge (11), a third valve (12), a second molecular pump (13), a second isolating valve (14) and a second dry pump (15); The quadrupole mass spectrometer (5) is connected with the high vacuum gauge (7) through a pipeline to form a test analysis system; The heating cover (8), the dewar assembly to be detected (9), the heating cover bracket (10) and the composite vacuum gauge (11) form a gas accumulation heating system, the heating cover (8) covers the dewar assembly to be detected (9), the heating cover bracket (10) is used for supporting the heating cover (8), and the dewar assembly to be detected (9) is connected with the composite vacuum gauge (11) through a pipeline; The first dry pump (4), the first isolating valve (3), the first molecular pump (2) and the first valve (1) are sequentially connected to form a main air extraction system, and are connected to the test analysis system through the first valve (1); the second dry pump (15), the second block valve (14), the second molecular pump (13) and the third valve (12) are sequentially connected to form an auxiliary air extraction system, and are switched to the gas accumulation heating system through the third valve (12); the test analysis system is connected with the gas accumulation heating system through a second valve (6); the method is characterized by comprising the following steps of: s1, enabling a second valve (6) to be in a closed state; S2, sequentially opening a first dry pump (4), a first isolating valve (3), a first molecular pump (2) and a first valve (1), heating and baking a test analysis system, and continuously vacuumizing until the vacuum degree of a high vacuum gauge (7) is better than 1 multiplied by 10 -9 mabr; s3, sequentially opening a second dry pump (15), a second isolating valve (14), a second molecular pump (13) and a third valve (12), heating and baking the gas accumulation heating system, and continuously vacuumizing until the vacuum degree of the composite vacuum gauge (11) is better than 1 multiplied by 10 -9 mabr; s4, continuously baking and exhausting the Dewar assembly (9) to be tested through a heating cover (8), wherein the temperature is controlled to be 60-100 ℃; S5, closing a third valve (12) to accumulate gas, adjusting the accumulated time, and monitoring the accumulated gas quantity through a composite vacuum gauge (11); s6, after gas accumulation is finished, closing the first valve (1), and opening the quadrupole mass spectrometer (5) to perform equipment background atmosphere test, wherein the scanning time is 30-300 seconds; S7, opening a second valve (6), and scanning the mass spectrum change condition, wherein the scanning time is 30-300 seconds; s8, accessing standard gas, and repeating the process; And S9, after the test is finished, opening a third valve (12) and opening a first isolating valve (3) to continuously vacuumize, so as to obtain lower equipment background.
2. The method of claim 1, wherein the measuring and analyzing the gas content of CO 2 and the measuring the CO 2 gas content of the workpiece require measuring three signal parameters with a mass number of 44, wherein the three signal parameters are a background signal rising rate, a signal rising rate with the workpiece, and a standard gas signal rising rate, wherein each signal measurement requires closing a main valve, and the standard leak valve is opened when the standard leak signal is measured, and the method comprises: (1) Background Signal Rate of rise I Background of the invention , In the formula, The initial state is the ion current value of CO 2 ; A CO 2 ion current value at the end of the accumulation time; To correspond to Is set to be a constant value; To correspond to Corresponding time of (2); (2) With rate of rise of the workpiece signal I Workpiece , In the formula, The current value of CO 2 ions at the initial pressure of the workpiece is set; A CO 2 ion current value at the end of the accumulation time; To correspond to Is set to be a constant value; To correspond to Corresponding time of (2); (3) Signal net increment I Increase the number of ; (4) Rate of rise of standard gas signal I Label (C) , In the formula, The current value of CO 2 ions at the initial pressure of the workpiece is set; A CO 2 ion current value at the end of the accumulation time; To correspond to Is set to be a constant value; To correspond to Corresponding time of (2); (5) The standard gas is calibrated to flow ; (6) CO 2 gas flow Q of test piece co2 。
3. The test analysis method of claim 1, wherein: the test analysis monitored water vapor by mass number 18, hydrogen by mass number 2, methane by mass number 16, oxygen by mass number 32, and argon by mass number 40.
4. The method for testing and analyzing the internal atmosphere of the dewar according to claim 1, wherein: The dewar assembly (9) to be tested is mutually connected with the second valve (6), the composite vacuum gauge (11) and the third valve (12) through exhaust pipes.
5. The method for testing and analyzing the internal atmosphere of the dewar according to claim 1, wherein: the first valve (1), the second valve (6) and the third valve (12) are all-metal sealing gate valves or all-metal sealing angle valves.
6. The method for testing and analyzing the internal atmosphere of the dewar according to claim 1, wherein: The mass number of the quadrupole mass spectrometer (5) is in the range of 1-200Amu, and the electron multiplier is arranged.
7. The method for testing and analyzing the internal atmosphere of the dewar according to claim 1, wherein: the high vacuum gauge (7) adopts A B-A type vacuum gauge, and the measurement lower limit is better than 1X 10 -9 mabr; the measuring range of the composite vacuum gauge (11) is 1atm-1×10 -9 mabr.
8. The method for testing and analyzing the internal atmosphere of the dewar according to claim 4, wherein: and an exhaust pipe connected with the to-be-detected Dewar assembly (9) and the gas accumulation heating system is in transition formation of reliable sealing connection by adopting a soft metal pipe.
9. The method for testing and analyzing the internal atmosphere of the dewar according to claim 5, wherein: the all-metal sealing gate valve or all-metal sealing angle valve interface adopts a knife edge sealing mode, and the adopted specifications comprise CF16, CF35, CF63 or CF100.

Description

Dewar internal atmosphere test analysis device and test analysis method thereof Technical Field The invention relates to the field of internal atmosphere analysis of an infrared detector Dewar assembly, in particular to a Dewar internal atmosphere test analysis device and a test analysis method. Background With the continuous development of infrared detectors to large area arrays and high resolution, the requirement on the vacuum life of the Dewar is higher and higher, and especially the application of new materials and new processes brings serious challenges to the vacuum life of the Dewar. In addition, there is an urgent need to perform Dewar internal atmosphere analysis on samples that have early vacuum failure, and related technical means are lacking at present. The internal atmosphere analyzers commonly used at present are developed by the company IPI in germany or the company ORS in the united states, and all use dynamic detection methods. For example, an IVA110-S internal atmosphere analyzer from ORS Inc. of America consists of a sample chamber, an analysis chamber, a vacuum system, etc. The sample chamber releases the gas perforation in the sealing device to the testing system, the analysis chamber comprises a four-stage mass spectrometer for analyzing the components of the gas, and the vacuum system obtains good vacuum degree and background. Currently, ge Shuping and the like in the literature "infrared focal plane Dewar exhaust residual gas analysis experiment research", and "infrared technology" in the 28 th year of 2006 report that a quadrupole mass spectrometer is used for detecting gas components in the Dewar exhaust process, and a dynamic method is adopted in the detection process. The device and the method have the common problems of poor test sensitivity, pollution and the like. Disclosure of Invention The invention aims to solve the technical problems that: (1) Aiming at the problem of poor sensitivity of the traditional internal atmosphere analyzer detection method, the high-sensitivity Dewar internal atmosphere test analysis device and the method are provided, and the structure is also suitable for other vacuum packaging devices needing high-sensitivity internal atmosphere analysis; (2) Aiming at the pollution problem of the test analysis chamber, a simple and reliable isolation measure is provided to avoid a large amount of gas pollution equipment in the initial state of the workpiece. The technical scheme of the invention is as follows: The device comprises a first valve, a first molecular pump, a first isolating valve, a first dry pump, a four-pole mass spectrometer, a second valve, a high vacuum gauge, a heating cover, a to-be-tested Dewar component, a heating cover bracket, a composite vacuum gauge, a third valve, a second molecular pump, a second isolating valve and a second dry pump, wherein the four-pole mass spectrometer and the high vacuum gauge are connected through pipelines to form a test analysis system, the heating cover, the to-be-tested Dewar component, the heating cover bracket and the composite vacuum gauge form a gas accumulation heating system, the heating cover covers the to-be-tested Dewar component, the heating cover bracket is used for supporting the heating cover, the to-be-tested Dewar component and the composite vacuum gauge are connected through pipelines, the first dry pump, the first isolating valve, the first molecular pump and the first valve are sequentially connected to form a main air suction system, the second dry pump, the second isolating valve, the second molecular pump and the third valve are sequentially connected to form an auxiliary air suction system, and are sequentially connected to the gas accumulation heating system through a third valve, and the gas accumulation heating system is connected with the test analysis system through the third valve. Further, the dewar component to be tested is mutually connected with the second valve, the composite vacuum gauge and the third valve through the exhaust pipe. Further, the first valve, the second valve and the third valve are all metal sealing gate valves or all metal sealing angle valves. Further, the mass number of the quadrupole mass spectrometer is in the range of 1-200Amu, and the electron multiplier is arranged. Further, the high vacuum gauge adopts A B-A type vacuum gauge, the lower measurement limit is better than 1X 10 -9 mabr, and the measurement range of the composite vacuum gauge is 1 atm-1X 10 -9 mabr. Further, the exhaust pipe connected with the dewar assembly to be tested and the gas accumulation heating system adopts a soft metal pipe for transition to form reliable sealing connection. Further, all-metal sealing gate valves or all-metal sealing angle valve interfaces adopt a knife edge sealing mode, and the adopted specifications comprise CF16, CF35, CF63 or CF100. The device for testing and analyzing the internal atmosphere of the Dewar comprises the following steps: s1, reliable s