CN116773639A - Dewar internal atmosphere test analysis device and test analysis method thereof - Google Patents

Dewar internal atmosphere test analysis device and test analysis method thereof Download PDF

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Publication number
CN116773639A
CN116773639A CN202310603153.4A CN202310603153A CN116773639A CN 116773639 A CN116773639 A CN 116773639A CN 202310603153 A CN202310603153 A CN 202310603153A CN 116773639 A CN116773639 A CN 116773639A
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China
Prior art keywords
valve
test analysis
dewar
vacuum gauge
gas
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CN202310603153.4A
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张亚平
李�杰
王艳
陈正超
高玲
何晶
杨曼云
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Kunming Institute of Physics
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Kunming Institute of Physics
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Priority to CN202310603153.4A priority Critical patent/CN116773639A/en
Publication of CN116773639A publication Critical patent/CN116773639A/en
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/62Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/44Sample treatment involving radiation, e.g. heat

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  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Electrochemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)

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 block valve, the first molecular pump and the first valve form a main air extraction system; the second dry pump, the second block valve, the second molecular pump and the third valve form an auxiliary air extraction system; the test analysis system is connected with the gas accumulation heating system through a 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.

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 releasing 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; the vacuum system achieves good vacuum and background.
Currently, ge Shuping and the like of Kunming institute of physics report in the literature "infrared focal plane Dewar exhaust residual gas analysis experiment research", and in the 28 th year of the "infrared technology" 2006 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 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 is connected with the high vacuum gauge through a pipeline to form a test analysis system; the heating cover, the dewar component to be tested, the heating cover bracket and the composite vacuum gauge form a gas accumulation heating system, the heating cover is covered on the dewar component to be tested, the heating cover bracket is used for supporting the heating cover, and the dewar component to be tested is connected with the composite vacuum gauge through a pipeline; the first dry pump, the first block valve, the first molecular pump and the first valve are sequentially connected to form a main air extraction system, and are connected to the test analysis system through the first valve; the second dry pump, the second block valve, the second molecular pump and the third valve are sequentially connected to form an auxiliary air extraction system, and are connected to the gas accumulation heating system through the third valve; the test analysis system is connected with the gas accumulation heating system through a second 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 ase:Sub>A B-A type vacuum gauge, and the lower measurement limit is better than 1X 10 -9 A mabr; the measuring range of the composite vacuum gauge is 1atm-1×10 -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: the dewar assembly to be tested is reliably and hermetically connected with the second valve, the composite vacuum gauge and the third valve through the soft metal pipe; and the second valve is brought to a closed state.
S2: sequentially opening a first dry pump, a first isolating valve, a first molecular pump and a first valve, heating and baking a test analysis system, and continuously vacuumizing until a high vacuum gauge is better than 1 multiplied by 10 -9 mabr。
S3: sequentially opening a second dry pump, a second block valve, a second molecular pump and a second valve, heating and baking the gas accumulation heating system, and continuously vacuumizing until the composite vacuum gauge is better than 1×10 -9 mabr。
S4: continuously baking and exhausting the dewar assembly to be tested through the heating cover, the heating cover bracket and the temperature control device thereof, wherein the temperature is controlled to be 60-100 ℃.
S5: and closing a third valve to accumulate gas, wherein the accumulated time is adjustable, and monitoring the accumulated gas quantity through a compound vacuum gauge.
S6: and after the gas accumulation is finished, closing the first valve, opening the quadrupole mass spectrometer to perform equipment background atmosphere test, and scanning for 30-300 seconds.
S7: and opening a second valve, and scanning the mass spectrum change condition, wherein the scanning time is 30 seconds to 300 seconds.
S8: and (5) accessing standard gas, and repeating the process.
S9: and after the test is finished, opening a third valve, opening a first isolating valve, and continuously vacuumizing to obtain lower equipment background.
Compared with the prior art, the invention has the beneficial effects that:
(1) According to the invention, atmosphere analysis is performed in a static accumulation state (namely, an all-metal valve between a molecular pump and a gas accumulation heating system is in a closed state, and an all-metal valve between the molecular pump and a test analysis system is in a closed state), so that the detection sensitivity can be remarkably enhanced, and meanwhile, the baking temperature and time of a sample can be flexibly adjusted according to different application requirements, so that different application requirements are met;
(2) The gas accumulation heating system and the test analysis system adopted by the invention are arranged separately by adopting all-metal valves, and are communicated through the test valves, and the gas accumulation heating system and the test analysis system respectively adopt independent air extraction systems, so that the pollution of equipment is avoided, and the detection efficiency is obviously improved;
(3) According to the Dewar internal atmosphere test analysis device, the sample accumulation time is convenient to adjust, and the gas quantity can be flexibly adjusted according to different application requirements;
(4) According to the Dewar internal atmosphere test analysis device, the gas accumulation heating system and the test analysis system are arranged separately, so that pollution to equipment can be avoided;
(5) Compared with a standard internal atmosphere analyzer, the Dewar internal atmosphere test analysis device adopts an accumulated gas method in the test process, and has test sensitivity which is more than 2 orders of magnitude higher than that of the standard internal atmosphere analyzer.
Drawings
FIG. 1 is a schematic diagram showing the composition of the high sensitivity Dewar internal atmosphere test analysis device of the present invention.
Detailed Description
The invention is further described below with reference to the drawings and detailed description.
As shown in fig. 1, the device for testing and analyzing the atmosphere inside the dewar comprises a first VAT all-metal angle valve 1, a first molecular pump 2, a first block valve 3, a first dry pump 4, a quadrupole mass spectrometer 5, a second VAT all-metal angle 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 VAT all-metal angle valve three 12, a second molecular pump 13, a second block valve 14 and a second dry pump 15.
The quadrupole mass spectrometer 5, the high vacuum gauge 7 and the pipeline thereof form a test analysis system; the dewar assembly 9 to be tested, the composite vacuum gauge 11 and pipelines thereof form a gas accumulation heating system; the first VAT all-metal angle valve 1, the first molecular pump 2, the first block valve 3 and the first dry pump 4 are sequentially connected and are connected to a test analysis system; the VAT all-metal angle valve III 12, the second molecular pump 13, the second block valve 14 and the second dry pump 15 are sequentially connected and are switched to a gas accumulation heating system; the test analysis system is separated from the gas accumulation heating system by a second VAT all-metal angle valve 6; the dewar assembly forms a heating system through a heating mantle 8, a heating mantle bracket 10 and a temperature control device thereof.
The dewar assembly 9 to be tested is connected with the gas accumulation heating system through an exhaust pipe, and is in high-reliability sealing connection through soft metal InSn transition.
The first VAT all-metal angle valve 1, the second VAT all-metal angle valve 6 and the VAT all-metal angle valve three 12 are all-metal seal angle valves DN40, and the interfaces adopt a knife edge sealing mode and adopt CF35 specifications.
The quadrupole mass spectrometer 5 adopts a Pu-generator QMG250, the mass number range is 1-200Amu, and an electron multiplier is arranged.
Wherein, the high vacuum gauge 7 adopts ase:Sub>A B-A type vacuum gauge, and the lower measurement limit is better than 1X 10 -9 A mabr. The measurement range of the composite vacuum gauge 11 is 1atm to 1×10 -9 mabr。
Referring to fig. 1, a method for implementing test analysis by using the Dewar internal atmosphere test analysis device of the present invention is as follows:
s1: the second VAT all-metal angle valve 6 is in a closed state.
S2: sequentially opening a first dry pump 4, a first block valve 3, a first molecular pump 2 and a first VAT all-metal angle valve 1, heating and baking a test analysis system, and continuously vacuumizing until a high vacuum gauge 7 is better than 1 multiplied by 10 -9 mabr。
S3: sequentially opening a second dry pump 15, a second block valve 14, a second molecular pump 13 and a second VAT all-metal angle valve 12, heating and baking the gas accumulation heating system, and continuously vacuumizing until the composite vacuum gauge 11 is better than 1 multiplied by 10 -9 mabr。
S4: the dewar assembly 9 to be tested is continuously baked and exhausted through the heating cover 8, the heating cover bracket 10 and the temperature control device thereof, and the temperature is controlled at 80 ℃.
S5: the third valve 12 is closed to perform gas accumulation, the accumulation time is adjustable, and the accumulated gas amount is monitored by the composite vacuum gauge 11.
S6: after the gas accumulation is finished, the first valve 1 is closed, the quadrupole mass spectrometer 5 is opened for carrying out equipment background atmosphere test, and the scanning time is 100 seconds.
S7: the second valve 6 was opened and the mass spectrum change was scanned for a scan time of 100 seconds.
S8: access to standard gas CO 2 The above process is repeated.
S9: and after the test is finished, opening the third valve 12, and opening the first isolating valve 3 to continuously vacuumize, so as to obtain lower equipment background.
The CO is analyzed by the following test 2 The gas content of (2) is used as an illustration of the calculation method. Testing CO of a workpiece 2 The gas quantity needs to measure three signal parameters with the mass number of 44, namely, the background signal rising rate, the workpiece-carrying signal rising rate and the standard gas signal rising rate. Each signal measurement requires closing of the main valve and opening of the standard leak valve when measuring the standard leak signal.
S1, background signal rising rate:
wherein P is 01 Is in the initial state CO 2 Ion current value; p (P) 11 For CO at the end of the accumulation time 2 Ion current value; t (T) 01 To correspond to P 01 Is set to be a constant value; t (T) 11 To correspond to P 11 Is a function of the time corresponding to the time of the corresponding time.
S2, signal rising rate with workpiece
Wherein P is 02 For CO with initial pressure of the workpiece 2 Ion current value; p (P) 12 For CO at the end of the accumulation time 2 Ion current value; t (T) 02 To correspond to P 02 Is set to be a constant value; t (T) 12 To correspond to P 12 Is a function of the time corresponding to the time of the corresponding time.
S3, signal net increment
I Increase the number of =I Workpiece -I Background of the invention
S4, standard gas signal rising rate
Wherein P is 03 For CO with initial pressure of the workpiece 2 Ion current value; p (P) 13 For CO at the end of the accumulation time 2 Ion current value; t (T) 03 To correspond to P 03 Is set to be a constant value; t (T) 13 To correspond to P 13 Is a function of the time corresponding to the time of the corresponding time.
S5, calibrating the flow of the standard gas to be Q 0
S6, testing CO of the workpiece 2 Flow rate of gas
The analysis of the common gas is performed by monitoring signals of corresponding mass numbers, such as monitoring water vapor through mass number 18, monitoring hydrogen through mass number 2, monitoring methane through mass number 16, monitoring oxygen through mass number 32, monitoring argon through mass number 40, and the like, and the calculation method is similar to that and is not repeated.

Claims (10)

1. The utility model provides a Dewar inside atmosphere test analytical equipment which characterized in that: the device comprises a first valve (1), a first molecular pump (2), a first isolation 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 isolation 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).
2. The dewar internal atmosphere test analysis device 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.
3. The dewar internal atmosphere test analysis device 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.
4. The dewar internal atmosphere test analysis device 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.
5. The dewar internal atmosphere test analysis device according to claim 1, wherein:
the high vacuum gauge (7) adopts ase:Sub>A B-A type vacuum gauge, and the lower measurement limit is better than 1 multiplied by 10 -9 mabr;
The measuring range of the composite vacuum gauge (11) is 1atm-1×10 -9 mabr。
6. The dewar internal atmosphere test analysis device according to claim 2, 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.
7. A dewar internal atmosphere test analysis device according to claim 3, characterized in that:
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.
8. A test analysis method of the dewar inner atmosphere test analysis device according to any one of claims 1 to 7, comprising the steps of:
s1: so that the second valve (6) is 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 block valve (14), a second molecular pump (13) and a second valve (12), heating and baking a 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), and controlling the temperature to be 60-100 ℃;
s5: the third valve (12) is closed to accumulate gas, the accumulation time is adjustable, and the accumulated gas quantity is monitored through the compound vacuum gauge (11);
s6: after the 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 seconds to 300 seconds;
s8: accessing standard gas, and repeating the above process;
s9: and after the test is finished, opening the third valve (12) and opening the first isolating valve (3) to continuously vacuumize, so as to obtain lower equipment background.
9. The test analysis method of claim 8, wherein the test analysis CO 2 CO of test piece 2 The gas quantity needs to measure three signal parameters with the mass number of 44, namely a background signal rising rate, a workpiece-carrying signal rising rate and a standard gas signal rising rate; each signal measurement needs to close the main valve, and the standard leak valve is opened when the standard leak signal is measured; comprising the following steps:
(1) Background Signal Rate of rise I Background of the invention
Wherein P is 01 Is in the initial state CO 2 Ion current value; p (P) 11 For CO at the end of the accumulation time 2 Ion current value; t (T) 01 To correspond to P 01 Is set to be a constant value; t (T) 11 To correspond to P 11 Corresponding time of (2);
(2) With rate of rise of the workpiece signal I Workpiece
Wherein P is 02 For CO with initial pressure of the workpiece 2 Ion current value; p (P) 12 For CO at the end of the accumulation time 2 Ion current value; t (T) 02 To correspond to P 02 Is set to be a constant value; t (T) 12 To correspond to P 12 Corresponding time of (2);
(3) Signal net increment I Increase the number of
I Increase the number of =I Workpiece -I Background of the invention
(4) Standard gasRate of signal rise I Label (C)
Wherein P is 03 For CO with initial pressure of the workpiece 2 Ion current value; p (P) 13 For CO at the end of the accumulation time 2 Ion current value; t (T) 03 To correspond to P 03 Is set to be a constant value; t (T) 13 To correspond to P 13 Corresponding time of (2);
(5) Standard gas calibrated flow is Q 0
(6) Testing CO of a workpiece 2 Gas flow rate Q co2
10. The test analysis method of claim 8, 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.
CN202310603153.4A 2023-05-26 2023-05-26 Dewar internal atmosphere test analysis device and test analysis method thereof Pending CN116773639A (en)

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Application Number Priority Date Filing Date Title
CN202310603153.4A CN116773639A (en) 2023-05-26 2023-05-26 Dewar internal atmosphere test analysis device and test analysis method thereof

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Application Number Priority Date Filing Date Title
CN202310603153.4A CN116773639A (en) 2023-05-26 2023-05-26 Dewar internal atmosphere test analysis device and test analysis method thereof

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117589847A (en) * 2024-01-04 2024-02-23 中国第一汽车股份有限公司 Oxygen sensor ignition time testing method and testing circuit

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117589847A (en) * 2024-01-04 2024-02-23 中国第一汽车股份有限公司 Oxygen sensor ignition time testing method and testing circuit
CN117589847B (en) * 2024-01-04 2024-04-16 中国第一汽车股份有限公司 Oxygen sensor ignition time testing method and testing circuit

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