CN106814125B - Online testing device and testing method for material radiation-induced outgassing - Google Patents
Online testing device and testing method for material radiation-induced outgassing Download PDFInfo
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- 230000005855 radiation Effects 0.000 title claims abstract description 115
- 238000010943 off-gassing Methods 0.000 title claims abstract description 72
- 238000012360 testing method Methods 0.000 title claims abstract description 69
- 239000000463 material Substances 0.000 title claims abstract description 36
- 238000005086 pumping Methods 0.000 claims abstract description 86
- 238000001514 detection method Methods 0.000 claims abstract description 20
- 239000007789 gas Substances 0.000 claims description 105
- 239000000725 suspension Substances 0.000 claims description 15
- 239000004642 Polyimide Substances 0.000 claims description 13
- 238000000605 extraction Methods 0.000 claims description 13
- 230000036961 partial effect Effects 0.000 claims description 13
- 229920001721 polyimide Polymers 0.000 claims description 13
- 230000000670 limiting effect Effects 0.000 claims description 11
- 238000010894 electron beam technology Methods 0.000 claims description 6
- 230000001681 protective effect Effects 0.000 claims description 4
- 230000001678 irradiating effect Effects 0.000 claims description 3
- 230000002285 radioactive effect Effects 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 22
- 238000004949 mass spectrometry Methods 0.000 abstract description 12
- 239000000523 sample Substances 0.000 description 52
- 238000004364 calculation method Methods 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 229910052741 iridium Inorganic materials 0.000 description 2
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical group [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 230000002829 reductive effect Effects 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- 238000009529 body temperature measurement Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000012956 testing procedure Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating 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
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Abstract
The invention discloses an online testing device for material radiation induced outgassing, which comprises a vacuum chamber system, a radiation chamber system, an air pumping system, an air supply system, a detection assembly and a numerical control acquisition unit. The invention also provides two methods for testing the amount of the material emitted by radiation: and the dynamic method and the mass spectrometry can be used for testing the total amount of the radiation induced outgassing of the same sample in real time on line, and the mass spectrometry can also accurately measure the outgassing component of each component of the radiation induced outgassing. The device simple structure, convenient operation, and can calibrate mass spectrometer and effective pumping speed, and the test result is more true accurate.
Description
Technical Field
The invention relates to the technical field of measurement, in particular to an online testing device and a testing method for material radiation-induced outgassing under a vacuum condition.
Background
Any solid material can be desorbed and outgassed when placed in a vacuum environment, in the fields of satellites, spaceships, spaces, some semiconductors and the like, the vacuum material is subjected to radiation of light, heat, electron beams and the like to generate an accelerated outgassing process, and the released gas can deteriorate the original vacuum environment, so that some optical components can fail. The accurate analysis of the outgassing behavior of the material under the vacuum radiation condition is an important basis for evaluating the vacuum performance of the material, and comprises the accurate acquisition of the radiation-induced outgassing amount, the outgassing component and the radiation-induced outgassing component.
The Chinese granted patent 'a device and method for measuring material outgassing rate with double test chambers', the publication number of which is CN101696923, as shown in figure 1, comprises a high vacuum chamber (112), an ultrahigh vacuum chamber (102), a separating gauge (107), an ultrahigh vacuum angle valve A (105), an ultrahigh vacuum angle valve B (106), a straight-through valve A (110) and a straight-through valve B (111), and a double molecular pump air-extracting system (101); further comprising: symmetric test chamber a (108) and test chamber B (109). The bi-molecular pump air pumping system (101) is connected with the ultrahigh vacuum chamber (102); the ultrahigh vacuum chamber (102) is respectively communicated with two symmetrical test chambers A (108) and B (109) through small holes, and the diameter range of the small holes is 5.7 mm-14 mm; the separating gauge (107) is bridged above the ultrahigh vacuum chamber (102) and the testing chamber A (108), and the ultrahigh vacuum angle valve A (105) and the ultrahigh vacuum angle valve (106) are respectively arranged at the connecting part of the separating gauge (107) and the ultrahigh vacuum chamber (102) and the testing chamber A (108); the test chamber A (108) and the test chamber B (109) are connected to a high vacuum chamber (112) through a through valve A (110) and a through valve B (111), respectively, and a heating plate is built in the high vacuum chamber (112). The device has the advantages of complex structure, inconvenient operation, more influencing factors due to the adoption of heating and air release of materials, relatively low measurement precision and high manufacturing cost.
The first paper "outgassing testing technology research of material under vacuum environment" in volume 20 of vacuum and low temperature "in 2014 introduces that it adopts static pressure-increasing method, fixed flow guiding method and two-channel gas path conversion method to test outgassing rate of infrared radiation heating material at different temperatures, and indicates that outgassing rate increases with the increase of material temperature. But it did not test the outgassing rate due to radiation alone. If the device is used for testing the outgassing caused only by radiation, the outgassing rate of the sample without radiation and the outgassing rate of the sample under radiation are always needed to be tested respectively aiming at the sample with the same material under the same working condition, and the outgassing rate are obtained by subtracting the outgassing rate and the outgassing rate. Because the air release rate of the sample is closely related to air extraction time, temperature, surface condition, surrounding environment and the like, the complete consistency of the two testing conditions is difficult to ensure, and the difficulty is brought to accurate testing of the radiation-induced air release.
At present, a mass spectrometer is mostly adopted for testing the partial pressure of each gas component of the material, gas molecules in the surrounding environment are ionized into ions by heating filaments, the size of ion flow is directly tested, and the partial pressure is indirectly obtained by adopting an internal calculation method.
China has granted a patent of 'composite material outgassing rate testing system and method with self-calibration function', publication number is CN201210431477, the device has many vacuum chambers, extremely complex structure and very high system cost. Although the method of calibrating the sensitivity of the mass spectrometer is pointed out to increase the testing precision, the actual mass spectrometer partial pressure calculation is not only related to the sensitivity, but also related to ionization probability, figure coefficients, conversion factors, detection factors and the like, and is very complex; and the calculation rules of most mass spectrometers on the market at present are slightly different. Therefore, accurate measurement of the outgassing components of the components under irradiation conditions must first suggest a suitable method of mass spectrometer calibration. Secondly, since the vacuum pump set pumping rate and orifice conductance are selective for gas components, accurate measurement of the outgassing component of each component under irradiation conditions must also accurately calibrate the effective pumping rate of the system.
Disclosure of Invention
The purpose of the invention is realized by the following technical scheme.
The invention discloses an online testing device for material radiation induced outgassing, which comprises: a vacuum chamber system, a radiation chamber system, an air pumping system, an air supply system, a detection assembly and a numerical control acquisition unit, wherein,
the vacuum chamber system comprises a vacuum chamber (1), wherein a sample (3) to be detected is placed in the vacuum chamber (1);
the radiation chamber system is connected with the vacuum chamber system through a flange window (4);
the air pumping system is connected with the vacuum chamber system;
the gas supply system is connected with the vacuum chamber system and is used for introducing various gases into the vacuum chamber (1);
the detection assembly comprises a vacuum gauge (19) and a mass spectrometer (20);
the numerical control acquisition unit is used for controlling the vacuum pump set, the radiation source (1) and the detection assembly to be switched on and off, acquiring vacuum data on line in real time, and storing and calculating the acquired data.
Preferably, the vacuum chamber system comprises: the vacuum cavity vacuum pump comprises a vacuum cavity (1), a sample table (2), a sample (3) and a flange window (4), wherein the sample table (2) is fixed on one side of the vacuum cavity (1) instead of above an air suction opening, the sample (3) is placed on the sample table (2), and the flange window (4) is arranged on the vacuum cavity (1).
Preferably, the radiation chamber system comprises: the device comprises a radiation chamber (5), a radiation source (6) and a radiation flow (7), wherein the radiation source (6) is arranged in the radiation chamber (5) and is used for irradiating light, heat or electron beams, and the radiation flow (7) is irradiated to a sample (3) through a flange window (4).
Preferably, the air extraction system comprises: the vacuum pump comprises a dry mechanical pump (8), a magnetic suspension molecular pump (9), a flow limiting small hole (10), a first angle valve (11), a gate valve (12) and a second angle valve (13), wherein the dry mechanical pump (8) and the second angle valve (13) form a first air extraction channel for rough extraction of a vacuum chamber (1); the dry mechanical pump (8), the magnetic suspension molecular pump (9) and the gate valve (12) form a second pumping channel for fine pumping of the vacuum chamber (1); and a third air pumping channel is formed by the dry mechanical pump (8), the magnetic suspension molecular pump (9), the flow limiting small hole (10) and the first angle valve (11) and is used for the sample radiation induced deflation test.
Preferably, the gas supply system comprises: the device comprises an air source (14), a first stop valve (15), a fine adjustment valve (16), a second stop valve (17) and a gas flow controller (18), wherein the air source (14), the first stop valve (15) and the fine adjustment valve (16) form a first gas supply channel, so that the vacuum chamber (1) forms dynamic stable gas flow; the gas source (14), the first stop valve (15) and the second stop valve (17) form a second gas supply channel for filling the vacuum chamber (1) with protective gas; the gas source (14), the first stop valve (15) and the gas flow controller (18) form a third gas supply channel which is used for charging the gas flow with known and controllable flow into the vacuum chamber (1); the gas flow controller (18) is precisely calibrated.
Preferably, the detection assembly comprises: a vacuum gauge (19), a mass spectrometer (20), a third angle valve (21) and a fourth angle valve (22). The vacuum gauge (19) is precisely calibrated and connected to the vacuum chamber (1) through a third angle valve (21); the mass spectrometer (20) is connected to the vacuum chamber (1) via a fourth angle valve (22).
An on-line testing method for the radiation-induced outgassing of materials, which adopts an on-line testing device for the radiation-induced outgassing of materials, and comprises the following steps:
s1: for the vacuum chamber (1) reaching the ultimate vacuum, all the air exhaust channels are closed, the second air supply channel is started, and the vacuum chamber (1) is filled with dry N of 1.2atm2Placing a sample to be detected into the vacuum chamber (1), and closing the second gas supply channel;
s2: starting the first pumping channel to perform rough pumping on the vacuum chamber (1), and then switching to a second pumping channel for fine pumping;
s3: opening the vacuum gauge (19), detecting the pressure P of the vacuum chamber (1), pumping the vacuum chamber (1) to the limit vacuum again, and switching to a third pumping channel;
s4: turning on the radiation source (6), the radiation time being t in units of s, the pressure rise Δ P of the vacuum gauge (19) in units of Pa;
s5: the radiation source (6) and the third pumping channel are closed, and the vacuum chamber (1) is filled with dry N of 1.2atm2And taking out the measured sample, and calculating the radiation induced outgassing amount of the sample in unit time.
A method for the in-line testing of radiation-induced outgassing of a material using an apparatus for the in-line testing of radiation-induced outgassing of the material, the method comprising:
s1: for the vacuum chamber (1) reaching the ultimate vacuum, all the air exhaust channels are closed, the second air supply channel is started, and the vacuum chamber (1) is filled with dry N of 1.2atm2Placing a sample to be detected into the vacuum chamber (1), and closing the second gas supply channel;
s2: starting the first pumping channel to perform rough pumping on the vacuum chamber (1), and then switching to a second pumping channel for fine pumping;
s3: opening the mass spectrometer (20), detecting the outgassing component of the vacuum chamber (1) and the partial pressure Pi of each component i, wherein the unit is Pa, pumping the vacuum chamber (1) to the limit vacuum again, and switching to a third pumping channel;
s4: turning on the radiation source (6) for a radiation time t in units of s, the mass spectrometer (20) measuring an increase in the partial pressure of the gas component i in units of Δ Pi in units of Pa;
s5: the radiation source (6) and the third pumping channel are closed, and the vacuum chamber (1) is filled with dry N of 1.2atm2And taking out the measured sample, and calculating the amount of the sample radiation-induced outgassing component in unit time and the total amount of the sample radiation-induced outgassing in unit time.
Preferably, the mass spectrometer (20) and vacuum gauge (19) are calibrated in comparison prior to performing the in-line test.
Preferably, after calibration of the mass spectrometer (20), the effective pumping speed S is measuredeAnd (6) carrying out calibration.
Compared with the prior art, the invention provides a set of on-line testing device for material radiation-induced deflation under the vacuum condition, the device has a simple structure, only has one vacuum chamber, overcomes the problem of multiple vacuum chambers in the prior art, and is convenient to operate; the radiation influence of a vacuum gauge and a mass spectrometer hot filament is effectively avoided, and the influence of a test sample on the effective pumping speed is reduced; and the mass spectrometer and the effective pumping speed can be calibrated, the problem of difficulty in accurate radiation testing caused by deflation in the prior art is solved, and the test result is more real and accurate. The invention also provides two methods for testing the material radiation induced outgassing: the dynamic method and the mass spectrometry can be used for online real-time testing, and the two testing methods are compared and calibrated through the mass spectrometry and the vacuum gauge; wherein the mass spectrometry can accurately measure the outgassing components of the radiation induced outgassing. No matter the total amount of the outgas or the component of the outgas, the device can specifically calculate the number of molecules outgas caused by the radiation of the material in unit time, and the characterization of the result is more intuitive and easy to understand.
Drawings
Various other advantages and benefits will become apparent to those of ordinary skill in the art upon reading the following detailed description of the preferred embodiments. The drawings are only for purposes of illustrating the preferred embodiments and are not to be construed as limiting the invention. Also, like reference numerals are used to refer to like parts throughout the drawings. In the drawings:
FIG. 1 is a diagram illustrating a conventional apparatus for measuring outgassing rate of a material in a dual test chamber;
FIG. 2 is a test apparatus for radiation-induced outgassing of materials under vacuum conditions in accordance with the present invention;
FIG. 3 is a graph of a laser emission gas component spectrum of a polyimide sample according to the present invention;
FIG. 4 is a graph showing the total outgassing amount and outgassing component of the outgassing caused by laser irradiation of polyimide samples of the present invention.
Description of the reference numerals
1 vacuum chamber 2 sample stage
3 sample 4 flanged Window
5 radiation Chamber 6 radiation Source
7 radiation flow 8 dry type mechanical pump
9 magnetic suspension molecular pump 10 current-limiting small hole
11 first angle valve 12 gate valve
13 second angle valve 14 air source
15 first stop valve 16 trim valve
17 second stop valve 18 gas flow controller
19 vacuum gauge 20 mass spectrometer
21 third angle valve 22 fourth angle valve
23 numerical control acquisition unit
101 double molecular pump pumping system 102 ultrahigh vacuum chamber
103 aperture A104 aperture B
105 super high vacuum angle valve A106 super high vacuum angle valve B
107 separation gauge 108 test chamber A
109 test chamber B110 straight-through valve a
111 straight-through valve B112 high vacuum chamber
113 sample Material
Detailed Description
Exemplary embodiments of the present disclosure will be described in more detail below with reference to the accompanying drawings. While exemplary embodiments of the present disclosure are shown in the drawings, it should be understood that the present disclosure may be embodied in various forms and should not be limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the disclosure to those skilled in the art.
Embodiments of the present invention will be described in detail below with reference to the accompanying drawings.
As shown in FIG. 2, the embodiment of the invention discloses an online testing device for material radiation-induced outgassing under vacuum condition, which comprises a vacuum chamber system, a radiation chamber system, an air pumping system, an air supply system, a detection assembly and a numerical control acquisition unit.
The vacuum chamber system is only provided with one vacuum chamber, a sample to be detected is placed in the vacuum chamber system, and the sample is prevented from being directly placed on the air suction port;
the radiation chamber system is connected with the vacuum chamber system through a flange window and is used for radiating a sample, the radiation chamber can be vacuum or non-vacuum, and a radiation source can be light, heat or electron beams and the like;
the air pumping system is connected with the vacuum chamber system and is used for vacuumizing the vacuum chamber system;
the gas supply system is connected with the vacuum chamber system, and various gases are introduced into the vacuum chamber, so that the mass spectrometer can be calibrated and the effective pumping speed can be reduced;
the detection assembly comprises a vacuum gauge and a mass spectrometer, the position of the detection assembly is optimized, and a filament of the detection assembly is prevented from directly thermally radiating a sample;
the numerical control acquisition unit can conveniently control the switches of the vacuum pump set, the radiation source and the detection assembly, can acquire vacuum data on line in real time and brings convenience to operation.
Specifically, the vacuum chamber system comprises: vacuum chamber 1, sample stage 2, sample 3 and flange window 4. The vacuum chamber 1 is cylindrical, and has typical dimensions of phi 200mm × 250mm, and the ultimate vacuum degree of 1 × 10-7Pa. The sample table 2 is fixed on one side of the vacuum chamber 1, so that the influence on the effective pumping speed of the vacuum pump caused by directly arranging the sample table on the pumping hole is avoided, and a temperature measurement platinum resistor is arranged on the sample table and used for testing the temperature of a sample. Sample 3 was placed on the sample stage, and was typically in the form of a square plate of 100mm by 100mm in size. The flange window 4 is arranged on the vacuum chamber 1 and can pass through radiation flow, and a water cooling device is distributed on the flange window to prevent the flange window from being deformed and cracked by heat.
The radiation chamber system comprises: a radiation chamber 5, a radiation source 6 and a radiation flow 7. The radiation chamber 5 may be a vacuum or non-vacuum chamber. A radiation source 6, which may be optical, thermal or electron beam radiation, is disposed in the radiation chamber 5 and a stream of radiation 7 is radiated through the flange window 4 onto the sample 3.
The air extraction system comprises: the device comprises a dry mechanical pump 8, a magnetic suspension molecular pump 9, a small flow limiting hole 10, a first angle valve 11, a gate valve 12 and a second angle valve 13. Wherein the pumping speed of the magnetic suspension molecular pump 9 is about 300L/s. The dry mechanical pump 8 and the second angle valve 13 form a first pumping channel for rough pumping of the vacuum chamber 1; the dry mechanical pump 8, the magnetic suspension molecular pump 9 and the gate valve 12 form a second pumping channel for fine pumping of the vacuum chamber 1; the dry type mechanical pump 8, the magnetic suspension molecular pump 9, the small flow limiting hole 10 and the first angle valve 11 form a third air exhaust channel for sample air exhaust test, wherein the diameter of the small flow limiting hole 10 is 20-100 mm, and the diameter of the small flow limiting hole 10 can be selected according to the effective pumping speed required by application.
The gas supply system includes: a gas source 14, a first stop valve 15, a trim valve 16, a second stop valve 17, and a gas flow controller 18. Wherein the gas source 14 can be various gases, such as He, N2、CO2Etc., the gas flow controller 18 is precisely calibrated. The gas source 14, the first stop valve 15 and the fine adjustment valve 16 form a first gas supply channel, so that the vacuum chamber 1 forms a dynamic stable gas flow, and the pressure adjustable range is 10-7Pa-1 Pa; the gas source 14, the first cutoff valve 15 and the second cutoff valve 17 constitute a second gas supply passage for charging the vacuum chamber 1 with a protective gas (e.g., N)2) (ii) a The gas source 14, the first stop valve 15 and the gas flow controller 18 constitute a third gas supply channel for feeding a gas flow of a known and controllable flow rate in the range of 7 x 10 into the vacuum chamber 1-2～7×10- 5Pa·m3/s。
The detection assembly comprises: a vacuum gauge 19, a mass spectrometer 20, a third angle valve 21 and a fourth angle valve 22. The vacuum gauge 19 is used for measuring the pressure of the vacuum chamber 1, and is precisely calibrated; selecting a cold cathode ionization gauge, wherein a filament is an iridium filament; connected to the vacuum chamber 1 through the third angle valve 21, the filament is not directed to the sample 3 and is slightly higher than the connecting port of the third angle valve 21 and the vacuum chamber 1, thereby reducing the radiation of the hot filament (> 1000 ℃) to the chamber wall and the sample to the utmost extent. The mass spectrometer 20 is used for measuring the gas composition and partial pressure in the vacuum chamber 1; the mass number range is 1-200amu, the model of QMG220 is preferred, and the filament is an iridium filament; the filament is not directly directed to the sample 3, but is slightly higher than the connection port of the fourth angle valve 22 to the vacuum chamber 1 by connecting the fourth angle valve 22 to the vacuum chamber 1, thereby minimizing the heat radiation to the chamber wall and the sample.
The numerical control acquisition unit 23 controls the starting, stopping and signal feedback of the radiation source 6, the dry mechanical pump 8, the magnetic suspension molecular pump 9 and the mass spectrometer 20 on the one hand, and acquires the test data of the vacuum gauge 19 and the mass spectrometer 20 on the other hand through the software of an industrial personal computer, and can store the data and simply calculate the data.
With the inventive apparatus of fig. 2, mass spectrometer 20 can be calibrated. First, mass number position and peak shape need to be calibrated: aiming at the vacuum chamber 1 which achieves ultimate vacuum, starting the first gas supply channel and the third gas extraction channel, and introducing low-quality high-purity He gas (4amu) into the vacuum chamber 1 to keep the dynamic stable gas flow at 5 multiplied by 10-6Pa, adjusting ion source parameters to enable the peak value to be Gaussian-shaped and the center to be positioned at 4 amu; similarly, a high quality amount of high purity Xe gas (132amu) was introduced into the vacuum chamber 1 to maintain a dynamically stable gas flow of 5X 10-6Pa, ion source parameters were adjusted so that the peak shape was gaussian and centered at 132 amu. Secondly, since the vacuum gauge 19 is calibrated, the mass spectrometer 20 and the vacuum gauge 19 are calibrated in comparison, and the consistency and reliability of the test result can be ensured. Aiming at the vacuum chamber 1 which reaches the ultimate vacuum, starting the first gas supply channel and the third gas extraction channel, introducing high-purity gas i into the vacuum chamber 1, keeping the dynamic stable gas flow, and ensuring the vacuum degree to be about 10-6Pa; when more than 95% of gas in the chamber is i, recording the total pressure P measured by the vacuum gauge 19ionAnd the partial pressure P of the gas i measured by the mass spectrometer 20iThe ratio of which is used to obtain a correction factor P for the partial pressure measured by the mass spectrometer 20ion/Pi。
By using the inventive device shown in FIG. 2, the effective pumping speed S can be adjustede(m3/s) for calibration. For the vacuum chamber 1 which has reached the ultimate vacuum, the third gas supply channel and the third gas exhaust channel are activated, and the gas flow controller 18 is adjusted to have a certain flow rate Qi(Pa·m3/s) introducing a gas i into the vacuum chamber 1, and after dynamic equilibrium is reached, testing the partial pressure P of the gas i in the vacuum chamber 1 with the calibrated mass spectrometer 20iThen the effective pumping speed S of the pumping system to the gas iei＝Qi/Pi。
Therefore, the total amount, the components and the components of the outgassing gas of the material under the vacuum condition can be conveniently, quickly, accurately and truly measured on line in real time by accurately calibrating the mass spectrometer and the effective pumping speed of the system.
In combination with the online testing device for the vacuum material radiation-induced outgassing shown in fig. 2, the invention also discloses an online testing method for the material radiation-induced outgassing amount, the outgassing component and the material radiation-induced outgassing component, wherein the testing method comprises a dynamic method and a mass spectrometry method, and the testing method is an online real-time test. One set of system respectively adopts two methods to test the radiation induced outgassing amount of the same sample, and is convenient for comparing the advantages and the disadvantages of the test methods. The various gas components and outgassing components of a material's radiation-induced outgassing can also be tested online using mass spectrometry. The laser-induced outgassing of the polyimide is tested as an example.
The dynamic method comprises the following testing steps: s1: for the vacuum chamber 1 reaching the ultimate vacuum, all the pumping channels are closed, the second gas supply channel is started, and the vacuum chamber 1 is charged with dry N of 1.2atm2The polyimide sample to be tested is placed in the vacuum chamber 1, and the second gas supply channel is closed. S2: the first pumping channel is started to perform rough pumping on the vacuum chamber 1, and then the second pumping channel is switched to perform fine pumping. S3: and opening the vacuum gauge 19, detecting the pressure P of the vacuum chamber 1 on line in real time, pumping the vacuum chamber 1 to the limit vacuum again, and switching to a third pumping channel. S4: the radiation source 6 is switched on for a radiation time t(s) and the pressure rise Δ P (Pa) of the vacuum gauge 19. S5: the radiation source 6 and the third pumping channel are turned off and the vacuum chamber 1 is charged with dry N at 1.2atm2And taking out the tested polyimide sample, and finishing the test. The amount of emission Q (molecular. s) of the polyimide sample per unit time-1) See equation 1 for the calculation of (c). Wherein SeN2(m3S) is a third pumping channel pair N2Effective pumping speed of, NA(mol-1) Is the Avgalois constant, T (K) is the temperature at irradiation, R (Pa · m)3·K-1·mol-1) Is the gas constant. The obtained material outgassing amount Q is equivalent to N2The equivalent value of (c).
The mass spectrometry testing procedure was as follows: steps S1-S2 are the same as the dynamic method. S3: the mass spectrometer 20 is opened to detect the outgassing components and the partial pressure P of each component i of the vacuum chamber 1 on-line in real timei(Pa), the vacuum chamber 1 is evacuated to the limit vacuum again, and switched to the third evacuation passage. S4: the radiation source 6 is turned on for a radiation time t(s) and the partial pressure of the gas component i measured by the mass spectrometer 20 rises to Δ Pi(Pa). S5: the radiation source 6 and the third pumping channel are turned off and the vacuum chamber 1 is charged with dry N at 1.2atm2And taking out the tested polyimide sample, and finishing the test. The outgassing component Q of the polyimide sample per unit timei(molecular·s-1) The calculation is shown in formula 2, and the total amount Q (molecular. s) of the outgassed polyimide material in unit time-1) See equation 3 for the calculation of (c). Wherein Sei(m3S) effective pumping speed of the third pumping channel to the gas i, NA(mol-1) Is the Avgalois constant, T (K) is the temperature at irradiation, R (Pa · m)3·K-1·mol-1) And n is the gas constant, the gas fraction of the polyimide sample outgassing measured by the mass spectrometer 20.
FIG. 3 is a graph of outgassing component spectrum of polyimide sample, mainly H, determined by mass spectrometry2(2amu)、H2O(18amu)、N2(CO)(28amu)、O2(32amu), Ar (40amu) and CO2(44 amu). FIG. 4 shows the total outgassing amount and outgassing component of outgassing caused by laser irradiation of a polyimide sample, wherein the total outgassing amount measured by a dynamic method is a nitrogen equivalent value, and the outgassing amount measured by a mass spectrometry method is a real value. The total amount of outgassing for the same sample can be measured using both dynamic and mass spectrometry methods, and the two can be compared. Mass spectrometry can test the outgassing component of a particular outgassing component.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (2)
1. An in-line testing apparatus for radiation-induced outgassing of a material, the apparatus comprising: a vacuum chamber system, a radiation chamber system, an air pumping system, an air supply system, a detection assembly and a numerical control acquisition unit, wherein,
the vacuum chamber system comprises a vacuum chamber (1), wherein a sample (3) to be detected is placed in the vacuum chamber (1);
the radiation chamber system is connected with the vacuum chamber system through a flange window (4);
the air pumping system is connected with the vacuum chamber system;
the gas supply system is connected with the vacuum chamber system and is used for introducing various gases into the vacuum chamber (1);
the detection assembly comprises a vacuum gauge (19) and a mass spectrometer (20);
the numerical control acquisition unit is used for controlling the vacuum pump set, the radiation source (1) and the detection assembly to be switched on and off, acquiring vacuum data on line in real time, and storing and calculating the acquired data; wherein,
the detection assembly comprises: a vacuum gauge (19), a mass spectrometer (20), a third angle valve (21) and a fourth angle valve (22); the vacuum gauge (19) is precisely calibrated and connected to the vacuum chamber (1) through a third angle valve (21); the mass spectrometer (20) is connected to the vacuum chamber (1) through a fourth angle valve (22);
the vacuum chamber system comprises: the vacuum cavity vacuum pump comprises a vacuum cavity (1), a sample table (2), a sample (3) and a flange window (4), wherein the sample table (2) is fixed on one side of the vacuum cavity (1) and is not arranged above an air suction opening, the sample (3) is placed on the sample table (2), and the flange window (4) is arranged on the vacuum cavity (1);
the radiation chamber system comprises: the device comprises a radiation chamber (5), a radiation source (6) and a radiation flow (7), wherein the radiation source (6) is arranged in the radiation chamber (5) and is used for irradiating light, heat or electron beams, and the radiation flow (7) is irradiated onto a sample (3) through a flange window (4);
the air extraction system comprises: the vacuum pump comprises a dry mechanical pump (8), a magnetic suspension molecular pump (9), a flow limiting small hole (10), a first angle valve (11), a gate valve (12) and a second angle valve (13), wherein the dry mechanical pump (8) and the second angle valve (13) form a first air extraction channel for rough extraction of a vacuum chamber (1); the dry mechanical pump (8), the magnetic suspension molecular pump (9) and the gate valve (12) form a second pumping channel for fine pumping of the vacuum chamber (1); a third air pumping channel is formed by the dry mechanical pump (8), the magnetic suspension molecular pump (9), the flow limiting small hole (10) and the first angle valve (11) and is used for the sample radiation induced deflation test;
the gas supply system includes: the device comprises an air source (14), a first stop valve (15), a fine adjustment valve (16), a second stop valve (17) and a gas flow controller (18), wherein the air source (14), the first stop valve (15) and the fine adjustment valve (16) form a first gas supply channel, so that the vacuum chamber (1) forms dynamic stable gas flow; the gas source (14), the first stop valve (15) and the second stop valve (17) form a second gas supply channel for filling the vacuum chamber (1) with protective gas; the gas source (14), the first stop valve (15) and the gas flow controller (18) form a third gas supply channel which is used for charging the gas flow with known and controllable flow into the vacuum chamber (1); the gas flow controller (18) is precisely calibrated;
the online testing method of the device comprises the following steps:
s1: for the vacuum chamber (1) reaching the ultimate vacuum, all the air exhaust channels are closed, the second air supply channel is started, and the vacuum chamber (1) is filled with dry N of 1.2atm2Placing a sample to be detected into the vacuum chamber (1), and closing the second gas supply channel;
s2: starting the first pumping channel to perform rough pumping on the vacuum chamber (1), and then switching to a second pumping channel for fine pumping;
s3: opening the vacuum gauge (19), detecting the pressure P of the vacuum chamber (1), pumping the vacuum chamber (1) to the limit vacuum again, and switching to a third pumping channel;
s4: turning on the radiation source (6), the radiation time being t in units of s, the pressure rise Δ P of the vacuum gauge (19) in units of Pa;
s5: the radiation source (6) and the third pumping channel are closed, and the vacuum chamber (1) is filled with dry N of 1.2atm2Taking out the measured sample, and calculating the amount of radioactive emissions of the sample in unit time; wherein
SeN2Is a third pumping channel pair N2Effective pumping speed of (1) in m3/s；NAIs an Avogastron constant in mol-1(ii) a T is the temperature at the time of irradiation, and the unit is K; r is a gas constant in Pa.m3·K-1·mol-1(ii) a The obtained material outgassing amount Q is equivalent to N2Equivalent value of
Prior to performing the in-line test, the mass spectrometer (20) and the vacuum gauge (19) are comparatively calibrated;
after calibration of the mass spectrometer (20), the effective pumping speed S is measuredeAnd (6) carrying out calibration.
2. An in-line testing apparatus for radiation-induced outgassing of a material, the apparatus comprising: a vacuum chamber system, a radiation chamber system, an air pumping system, an air supply system, a detection assembly and a numerical control acquisition unit, wherein,
the vacuum chamber system comprises a vacuum chamber (1), wherein a sample (3) to be detected is placed in the vacuum chamber (1);
the radiation chamber system is connected with the vacuum chamber system through a flange window (4);
the air pumping system is connected with the vacuum chamber system;
the gas supply system is connected with the vacuum chamber system and is used for introducing various gases into the vacuum chamber (1);
the detection assembly comprises a vacuum gauge (19) and a mass spectrometer (20);
the numerical control acquisition unit is used for controlling the vacuum pump set, the radiation source (1) and the detection assembly to be switched on and off, acquiring vacuum data on line in real time, and storing and calculating the acquired data; wherein,
the detection assembly comprises: a vacuum gauge (19), a mass spectrometer (20), a third angle valve (21) and a fourth angle valve (22); the vacuum gauge (19) is precisely calibrated and connected to the vacuum chamber (1) through a third angle valve (21); the mass spectrometer (20) is connected to the vacuum chamber (1) through a fourth angle valve (22);
the vacuum chamber system comprises: the vacuum cavity vacuum pump comprises a vacuum cavity (1), a sample table (2), a sample (3) and a flange window (4), wherein the sample table (2) is fixed on one side of the vacuum cavity (1) and is not arranged above an air suction opening, the sample (3) is placed on the sample table (2), and the flange window (4) is arranged on the vacuum cavity (1);
the radiation chamber system comprises: the device comprises a radiation chamber (5), a radiation source (6) and a radiation flow (7), wherein the radiation source (6) is arranged in the radiation chamber (5) and is used for irradiating light, heat or electron beams, and the radiation flow (7) is irradiated onto a sample (3) through a flange window (4);
the air extraction system comprises: the vacuum pump comprises a dry mechanical pump (8), a magnetic suspension molecular pump (9), a flow limiting small hole (10), a first angle valve (11), a gate valve (12) and a second angle valve (13), wherein the dry mechanical pump (8) and the second angle valve (13) form a first air extraction channel for rough extraction of a vacuum chamber (1); the dry mechanical pump (8), the magnetic suspension molecular pump (9) and the gate valve (12) form a second pumping channel for fine pumping of the vacuum chamber (1); a third air pumping channel is formed by the dry mechanical pump (8), the magnetic suspension molecular pump (9), the flow limiting small hole (10) and the first angle valve (11) and is used for the sample radiation induced deflation test;
the gas supply system includes: the device comprises an air source (14), a first stop valve (15), a fine adjustment valve (16), a second stop valve (17) and a gas flow controller (18), wherein the air source (14), the first stop valve (15) and the fine adjustment valve (16) form a first gas supply channel, so that the vacuum chamber (1) forms dynamic stable gas flow; the gas source (14), the first stop valve (15) and the second stop valve (17) form a second gas supply channel for filling the vacuum chamber (1) with protective gas; the gas source (14), the first stop valve (15) and the gas flow controller (18) form a third gas supply channel which is used for charging the gas flow with known and controllable flow into the vacuum chamber (1); the gas flow controller (18) is precisely calibrated;
the online testing method of the device comprises the following steps:
s1: for the vacuum chamber (1) reaching the ultimate vacuum, all the air exhaust channels are closed, the second air supply channel is started, and the vacuum chamber (1) is filled with dry N of 1.2atm2Placing a sample to be detected into the vacuum chamber (1), and closing the second gas supply channel;
s2: starting the first pumping channel to perform rough pumping on the vacuum chamber (1), and then switching to a second pumping channel for fine pumping;
s3: opening the mass spectrometer (20), detecting the outgassing component of the vacuum chamber (1) and the partial pressure Pi of each component i, wherein the unit is Pa, pumping the vacuum chamber (1) to the limit vacuum again, and switching to a third pumping channel;
s4: turning on the radiation source (6) for a radiation time t in units of s, the mass spectrometer (20) measuring an increase in the partial pressure of the gas component i in units of Δ Pi in units of Pa;
s5: the radiation source (6) and the third pumping channel are closed, and the vacuum chamber (1) is filled with dry N of 1.2atm2Taking out the measured sample, and calculating the radiation induced air release component Q of the sample in unit timeiTotal amount Q of the sample radiation induced outgassing in unit time;
wherein SeiFor the third pumping channel, the effective pumping speed of the gas i is m3/s；NAIs an Avogastron constant in mol-1(ii) a T is the temperature at the time of irradiation, and the unit is K; r is a gas constant in Pa.m3·K-1·mol-1(ii) a n is the gas component fraction of the polyimide sample outgassing measured by the mass spectrometer (20)
Prior to performing the in-line test, the mass spectrometer (20) and the vacuum gauge (19) are comparatively calibrated;
in calibrating mass spectrometers (20)After calibration, the effective pumping speed S is adjustedeAnd (6) carrying out calibration.
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