CN204924843U - Material partial pressure gassing rate tester - Google Patents
Material partial pressure gassing rate tester Download PDFInfo
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- CN204924843U CN204924843U CN201520527517.6U CN201520527517U CN204924843U CN 204924843 U CN204924843 U CN 204924843U CN 201520527517 U CN201520527517 U CN 201520527517U CN 204924843 U CN204924843 U CN 204924843U
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- potential drop
- dividing potential
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- 239000000463 material Substances 0.000 title claims abstract description 44
- 238000013022 venting Methods 0.000 claims description 50
- 238000005086 pumping Methods 0.000 claims description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 56
- 239000007789 gas Substances 0.000 abstract description 46
- 238000000034 method Methods 0.000 abstract description 16
- 238000005259 measurement Methods 0.000 abstract description 11
- 230000008569 process Effects 0.000 abstract description 9
- 238000001179 sorption measurement Methods 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 229910001873 dinitrogen Inorganic materials 0.000 abstract 2
- 229910052757 nitrogen Inorganic materials 0.000 description 27
- 238000012360 testing method Methods 0.000 description 22
- 230000035945 sensitivity Effects 0.000 description 7
- 238000011144 upstream manufacturing Methods 0.000 description 4
- 238000010943 off-gassing Methods 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229930195733 hydrocarbon Natural products 0.000 description 2
- 150000002430 hydrocarbons Chemical class 0.000 description 2
- 238000009434 installation Methods 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000010606 normalization Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 1
- 238000009530 blood pressure measurement Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000012938 design process Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000002310 reflectometry Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000007480 spreading Effects 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000001771 vacuum deposition Methods 0.000 description 1
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- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The utility model discloses a material partial pressure gassing rate tester, including a measuring chamber, a vacuum pump package and a current -limiting aperture, the vacuum pump package passes through the push -pull valve to be connected with the measuring chamber, and the front end of current -limiting aperture passes through the angle valve to be connected with the measuring chamber, the direct and vacuum pump group link in rear end, through quadrupole mass spectrometer and extractor gauge, measure the measuring chamber respectively for the background partial pressure and the background nitrogen gas equivalent total pressure of empty not gas of the same race when containing the sample, and then obtain the partial pressure gassing rate of sample nitrogen gas equivalent. The utility model discloses only need a quadrupole mass spectrometer just can accomplish material partial pressure gassing rate real -time, measure in succession, reduce in the measurement process because along with the gaseous secondary adsorption apparatus meeting that the voltage rise brought of vacuum material gassing production in the measuring chamber to can make things convenient for the gaseous horizontal contrast of variance component.
Description
Technical field
The utility model belongs to vacuum measurement technical field, particularly relates to a kind of material dividing potential drop venting rate tester.
Background technology
The material be positioned in vacuum environment can produce the phenomenon of deflation of following three kinds of forms:
1) in atmospheric environment, be adsorbed on the desorption of material surface gas;
2) gas being dissolved in material internal is released by spreading;
3) evaporation of material self, decomposition.
More and more vacuum environment is used, such as spacecraft ground test, vacuum coating, semiconductor machining etc. in modern scientific research and commercial production.Therefore, to carry out vacuum material both at home and abroad always and go out the relevant research work of venting.Along with the progressively raising of experiment, production environment demand, venting rate stagnation pressure is not only paid close attention in the test of vacuum material venting rate, and focuses on the test of material outgassing component and dividing potential drop venting rate thereof.Such as in extreme ultraviolet photolithographic, for preventing hydrocarbon deposit in exposure process in vacuum chamber in optical system surface, reduce optical system surface reflectivity, require exposure system to be placed in the microenvironment of ultra-clean, the hydrocarbon partial pressures power controlled in microenvironment is less than 1 × 10 simultaneously
-8pa; Steam partial pressure simultaneously in microenvironment should be less than 1 × 10
-7pa prevents its oxidation optical system surface.Therefore, before system design process, need to carry out venting component to the material sample that may use in system and dividing potential drop venting rate is tested, as the foundation of the material type selecting in vacuum system.
Nineteen ninety-five, the people such as YYang adopt orifice conductance method to test material outgassing dividing potential drop, proposition utilizes pipeline and two valves to build a road and bridge structure between aperture upstream chamber and aperture downstream chamber, pipeline two ends are connected with upstream chamber, downstream chamber respectively by valve, install quadrupole mass spectrometer in the middle of pipeline; By the switching connecting valve, the gas of upstream and downstream room is incorporated in the pipeline of installation quadrupole mass spectrometer, completes the measurement of the indoor partial pressure of upstream and downstream; The difference of twice partial pressure is multiplied by orifice conductance and obtains dividing potential drop discharge quantity.
1999, for accurately measuring each gas composition dividing potential drop, the people such as ShuWatanabe utilized calibrating gas and magnetic suspension rotor gauge first to measure the response sensitivity of quadrupole mass spectrometer to gas with various, and recycling quadrupole mass spectrometer is analyzed chamber venting partial component pressure.
2013, publication number is CN103267705A, the Chinese utility model patent application that patent name is " material dividing potential drop venting rate measuring system and measuring method thereof " proposes device as shown in Figure 1, at supervacuum chamber and test cabinet, a four-electrode spectrum is respectively installed and takes into account an angle valve, utilize two quadrupole mass spectrometers to measure gas composition dividing potential drop when chamber background and load when zero load have a sample respectively by controlling two angle valves, thus obtain sample dividing potential drop discharge quantity.
Quadrupole mass spectrometer is the effective tool measuring vacuum material venting rate.At present, there is the problem of the following aspects in the vacuum material venting partial pressure measurement utilizing quadrupole mass spectrometer to carry out:
When 1, adopting voltage rise method to carry out the measurement of vacuum material venting rate dividing potential drop, along with the test duration increases, vacuum cavity pressure raises and easily causes gas second adsorption, affects measurement result accuracy;
2, the ionization vacuum ga(u)ge measured of high vacuum and the sensitivity of quadrupole mass spectrometer all closely related with gas ionization probability, but at present, the modifying factor of ionization vacuum ga(u)ge, quadrupole mass spectrometer sensitivity are actually measuring equipment to the modifying factor of nitrogen or argon gas or sensitivity, the ionization probability of gas with various is not identical, ignoring measuring equipment will inevitably cause measurement result inaccurate to the difference of gas with various sensitivity, and the dividing potential drop venting rate of different venting components does not have comparability;
3, the testing process of existing vacuum material dividing potential drop venting rate proving installation is comparatively complicated, needs repeatedly switch valve or adopts two quadrupole mass spectrometers to complete measurement, be unfavorable for the industrial demand completing the test of dividing potential drop venting rate fast, in real time.
Utility model content
(1) technical matters that will solve
The purpose of this utility model is to provide a kind of material dividing potential drop venting rate tester, only need a quadrupole mass spectrometer just can complete real-time, the continuous coverage of material dividing potential drop venting rate, reduce owing to measuring with the gas second adsorption chance that the voltage rise of vacuum material venting generation brings in chamber in measuring process, and the across comparison of heterogeneity gas can be facilitated.
(2) technical scheme
For solving the problems of the technologies described above, the utility model provides a kind of material dividing potential drop venting rate tester, comprises extractor gauge, measuring chamber, angle valve, current limliting aperture, molecular pump, vacuum pump group, push-pull valve, quadrupole mass spectrometer, wherein: measuring chamber is for placing sample; Vacuum pump group is connected with measuring chamber by push-pull valve, and it is for vacuumizing measuring chamber; The front end of current limliting aperture is connected with measuring chamber by angle valve, and rear end is directly connected with vacuum pump group; Quadrupole mass spectroscope and extractor gauge are directly connected with described measuring chamber respectively.
According to a kind of embodiment of the present utility model, the aperture of current limliting aperture is 4mm ~ 200mm.
According to a kind of embodiment of the present utility model, vacuum pump group comprises molecular pump and dry-type mechanical pump, and the front end of molecular pump is connected with measuring chamber by push-pull valve, and rear end is connected with dry-type mechanical pump.
The utility model also provides a kind of material dividing potential drop venting rate measuring method, and be applied to material dividing potential drop venting rate measuring appliance, method comprises the steps:
S1, open vacuum pump group to bleed to measuring chamber, after elapsed time T, close vacuum pump group, open the angle valve of current limliting aperture front end, the push-pull valve of closure molecule pump front end, after current limliting aperture two ends gaseous tension is stable, by the background partial pressure of the indoor gas not of the same race of quadrupole mass spectrometer read test, read background nitrogen equivalent total pressure by extractor gauge;
S2, measures the length of sample, calculates the surface area of described sample;
S3, sample is sent in test cabinet, open vacuum pump group to bleed to measuring chamber, after elapsed time T, open the angle valve of current limliting aperture front end, the push-pull valve of closure molecule pump front end, after current limliting aperture two ends gaseous tension is stable, by the partial pressure of the indoor gas not of the same race of quadrupole mass spectrometer read test, read background nitrogen equivalent total pressure by extractor gauge;
S4, completes the normalization of gas not of the same race to nitrogen equivalent by following formula, finally obtains the dividing potential drop venting rate of sample nitrogen equivalent:
Wherein, C is the conductance of current limliting aperture,
be the nitrogen equivalent dividing potential drop venting rate of i-th kind of gas componant, i is natural number, P
tt () is for comprising nitrogen equivalent total pressure time sample (3) in measuring chamber; P
ithe partial pressure of the i-th gas componant t () is for comprising sample in measuring chamber time; P
t0t background nitrogen equivalent total pressure that () is empty measuring chamber; P
i0(t) for the background partial pressure of i-th kind of gas componant in empty measuring chamber, t be the time, S is the surface area of sample.
According to a kind of embodiment of the present utility model, before described step S2, also comprise: the surface of cleaning sample.
(3) beneficial effect
Compared with prior art, the measuring appliance that the utility model proposes and method, have the following advantages:
1, the mode control survey vacuum cavity pressure utilizing current limliting aperture dynamically to bleed, reduces owing to measuring with the gas second adsorption chance that the voltage rise of vacuum material venting generation brings in chamber in measuring process, raising measurement accuracy.
2, achieved the test of dividing potential drop venting rate that is real-time, continuous print material and discharge quantity by the combination of extractor gauge and quadrupole mass spectrometer, achieve the measurement of the function of time of material dividing potential drop venting rate, stagnation pressure venting rate.
3, normalize on nitrogen equivalent by the pressure of gas with various, unified gaseous tension contrast initial point, under same experimental conditions, makes different types of gasmetry pressure have comparability.
4, comparing the device the utility model adopting multiple quadrupole mass spectrometer to carry out the test of material dividing potential drop venting rate only needs a quadrupole mass spectrometer to complete DATA REASONING, and measurement mechanism structure is simple, and laboratory operating procedures is succinct, is convenient to real-time, continuous coverage.Further, owing to only adopting same quadrupole mass spectrometer in measuring process, the different quadrupole mass spectrometer in use experimental error brought of sensitivity difference is each other avoided.
Accompanying drawing explanation
Fig. 1 is the structural representation of material dividing potential drop venting rate measurement mechanism in prior art.
The structural representation of the material dividing potential drop venting rate measuring appliance that Fig. 2 provides for the utility model.
Embodiment
The utility model provides a kind of material dividing potential drop venting rate tester, and this device comprises a measuring chamber, a vacuum pump group and a current limliting aperture.Vacuum pump group is connected with measuring chamber by push-pull valve, and the front end of current limliting aperture is connected with measuring chamber by angle valve, and rear end is directly connected with vacuum pump group.
Surveying instrument of the present utility model is quadrupole mass spectroscope and extractor gauge, and to measure measuring chamber be respectively empty and the background partial pressure of gas not of the same race when comprising sample and background nitrogen equivalent total pressure, and then obtain the dividing potential drop venting rate of sample nitrogen equivalent.
For making the purpose of this utility model, technical scheme and advantage clearly understand, below in conjunction with specific embodiment, and with reference to accompanying drawing, the utility model is further described.
The structural representation of the material dividing potential drop venting rate measuring appliance that Fig. 2 provides for the utility model.As shown in Figure 2, material dividing potential drop venting rate measuring appliance comprises extractor gauge 1, measuring chamber 2, angle valve 4, current limliting aperture 5, molecular pump 6, dry-type mechanical pump 7, push-pull valve 8 and quadrupole mass spectrometer 9.Wherein, measuring chamber 2 is for placing sample 3, the front end of molecular pump 6 is connected with measuring chamber 2 by push-pull valve 8, rear end is connected with dry-type mechanical pump 7, the front end of current limliting aperture 5 is connected with measuring chamber 2 by angle valve 4, rear end is directly connected with molecular pump 6, and quadrupole mass spectroscope 9 and extractor gauge 1 are directly connected with described measuring chamber 2 respectively.
The aperture of current limliting aperture 5 is determined by required gas conduction, and in a kind of embodiment, it can get the scope of 4mm ~ 200mm, such as, can be 50mm.
Molecular pump 6 and dry-type mechanical pump 7 vacuumize measuring chamber 2 in combination.
Quadrupole mass spectroscope 9 is for measuring the partial pressure of the gas not of the same race in this measuring chamber 2.
Extractor gauge 1 is for measuring the nitrogen equivalent total pressure in this measuring chamber 2.
The method utilizing material dividing potential drop venting rate measuring appliance of the present utility model to measure material dividing potential drop venting rate comprises the steps:
S1, open vacuum pump group to bleed to measuring chamber 2, after elapsed time T, close vacuum pump group, open the angle valve 4 of current limliting aperture 5 front end, the push-pull valve 8 of closure molecule pump 6 front end, after current limliting aperture 5 two ends gaseous tension is stable, by the background partial pressure of gas not of the same race in quadrupole mass spectrometer 9 read test room 2, read background nitrogen equivalent total pressure by extractor gauge 1.
S2, described sample 3 is sent in test cabinet 2, open vacuum pump group to bleed to measuring chamber 2, after elapsed time T, open the angle valve 4 of current limliting aperture 5 front end, the push-pull valve 8 of closure molecule pump 6 front end, after current limliting aperture 5 two ends gaseous tension is stable, by the partial pressure of gas not of the same race in quadrupole mass spectrometer 9 read test room 2, read nitrogen equivalent total pressure by extractor gauge 1.
Before sample 3 is sent into test cabinet 2, the step on the surface of cleaning sample 3 can be comprised, when needing, also can comprise the step measuring sample 3 surface area, such as, after measuring length, calculate the surface area of described sample 3.S3, completes the normalization of gas not of the same race to nitrogen equivalent by following formula, finally obtains the dividing potential drop venting rate of sample (3) nitrogen equivalent:
In formula:
S is the surface area of sample 3, and unit is cm
2;
C is the conductance of current limliting aperture 5, and unit is L/s;
be the nitrogen equivalent dividing potential drop venting rate of i-th kind of gas componant, unit is PaL/ (scm
2), i is natural number;
P
tt (), for comprising nitrogen equivalent total pressure during sample 3 in measuring chamber 2, unit is Pa;
P
ithe partial pressure of i-th kind of gas t () is for comprising sample 3 in measuring chamber 2 time, unit is Pa;
P
t0t background nitrogen equivalent total pressure that () is empty measuring chamber 2, unit is Pa;
P
i0t () is the background partial pressure of i-th kind of gas componant in empty measuring chamber 2, unit is Pa.
In step S1 and step S3, the combination pumping speed of vacuum pump group 6 should be greater than the current limliting orifice conductance of 50 times, now the gaseous tension of current limliting aperture 5 rear end comparatively current limliting aperture 5 forward end gas pressure can ignore.
In the material dividing potential drop venting rate measuring process of step S3, bled by current limliting aperture 5 pairs of test cabinets 2, in the process, in test cabinet 2, gas is constantly pumped by aperture on the one hand, sample 3 on the other hand in test cabinet 2 constantly releases gas under vacuum, above two processes impel the pressure at current limliting aperture two ends to reach dynamic balance state, reduce the gas second adsorption phenomenon because pressure increase in test cabinet 2 causes.After current limliting aperture 5 pressure at two ends is stable, sample 3 with the discharge quantity summation of measuring chamber 2 is:
Q＝C(p-p')①
Wherein, Q is the discharge quantity summation of sample 3 and measuring chamber 2; C is the conductance of current limliting aperture 5; The gas pressure of p, p ' point current limliting aperture 5 front end and current limliting aperture 5 backend gas pressure; Can ignore relative to p according to design p ' above, formula can be rewritten as:
Q＝C·p②
Q is the discharge quantity summation of sample 3 and measuring chamber 2; C is current limliting orifice conductance; P is the gas stagnation pressure in test cabinet 2.In like manner, the background discharge quantity of measuring chamber 2 is:
Q
0＝C·p
0③
Q
0for background discharge quantity during measuring chamber 2 cavity; p
0for background gas pressure during measuring chamber 2 cavity.Total venting rate of sample 3 is:
Q is total venting rate of sample 3; S is the surface area of sample 3.
Because quadrupole mass spectrometer 9 sensitivity in vacuum material dividing potential drop venting rate measuring appliance, current limliting aperture 5 conductance, extractor gauge 1 modifying factor, molecular pump 6 pumping speed all adopt nitrogen to carry out calibration and obtain, therefore in the venting of material dividing potential drop, following formula is utilized to be normalized to nitrogen equivalent the dividing potential drop of all gas:
In formula:
-the i-th kind of gas normalizing returns the partial pressure of nitrogen equivalent by force, and unit is; PaL/ (scm
2)
P
ithe partial pressure of i-th kind of gas that-quadrupole mass spectrometer 9 records, unit is Pa;
The biggest quality number that m-quadrupole mass spectrometer 9 is tested, unit is Pa;
P
tthe total pressure of standard that what-extractor gauge measured with nitrogen is, unit is Pa.
Therefore, trace to the source the back dividing potential drop venting rate of nitrogen equivalent of any one outgassing constituent in sample is:
In formula:
S is the surface area of sample 3, and unit is cm
2;
C is the conductance of current limliting aperture 5, and unit is L/s;
be the nitrogen equivalent dividing potential drop venting rate of i-th kind of gas componant, unit is PaL/ (scm
2);
P
tt (), for comprising nitrogen equivalent total pressure during sample 3 in measuring chamber 2, unit is Pa;
P
ithe partial pressure of i-th kind of gas t () is for comprising sample 3 in measuring chamber 2 time, unit is Pa;
P
t0t background nitrogen equivalent total pressure that () is empty measuring chamber 2, unit is Pa;
P
i0t () is the background partial pressure of i-th kind of gas componant in empty measuring chamber 2, unit is Pa.
Above-described specific embodiment; the purpose of this utility model, technical scheme and beneficial effect are further described; be understood that; the foregoing is only specific embodiment of the utility model; be not limited to the utility model; all within spirit of the present utility model and principle, any amendment made, equivalent replacement, improvement etc., all should be included within protection domain of the present utility model.
Claims (3)
1. a material dividing potential drop venting rate tester, it is characterized in that, comprise extractor gauge (1), measuring chamber (2), angle valve (4), current limliting aperture (5), vacuum pump group, push-pull valve (8) and quadrupole mass spectrometer (9), wherein:
Described measuring chamber (2) is for placing sample (3);
Described vacuum pump group is connected with described measuring chamber (2) by described push-pull valve (8), and it is for vacuumizing described measuring chamber (2);
The front end of described current limliting aperture (5) is connected with described measuring chamber (2) by angle valve (4), rear end is directly connected with described vacuum pump group, wherein, the pumping speed of described vacuum pump group (6) is greater than the conductance of the described current limliting aperture (5) of 50 times;
Described quadrupole mass spectroscope (9) is directly connected with described measuring chamber (2) respectively with described extractor gauge (1).
2. material dividing potential drop venting rate tester according to claim 1, it is characterized in that, the aperture of described current limliting aperture (5) is 4mm ~ 200mm.
3. material dividing potential drop venting rate tester according to claim 1, it is characterized in that, described vacuum pump group comprises molecular pump (6) and dry-type mechanical pump (7), the front end of described molecular pump (6) is connected with described measuring chamber (2) by described push-pull valve (8), and rear end is connected with dry-type mechanical pump (7).
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| CN201520527517.6U CN204924843U (en) | 2015-07-20 | 2015-07-20 | Material partial pressure gassing rate tester |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105021494A (en) * | 2015-07-20 | 2015-11-04 | 中国科学院光电研究院 | Material partial pressure gas-release rate test device and method |
| CN108318376A (en) * | 2017-12-19 | 2018-07-24 | 兰州空间技术物理研究所 | A method of judging sealing cesium beam tube material out-gassing rate |
-
2015
- 2015-07-20 CN CN201520527517.6U patent/CN204924843U/en active Active
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105021494A (en) * | 2015-07-20 | 2015-11-04 | 中国科学院光电研究院 | Material partial pressure gas-release rate test device and method |
| CN105021494B (en) * | 2015-07-20 | 2017-12-19 | 中国科学院光电研究院 | A kind of material partial pressure deflation rate test system and method |
| CN108318376A (en) * | 2017-12-19 | 2018-07-24 | 兰州空间技术物理研究所 | A method of judging sealing cesium beam tube material out-gassing rate |
| CN108318376B (en) * | 2017-12-19 | 2020-06-23 | 兰州空间技术物理研究所 | Method for judging gas yield of sealed cesium-beam tube material |
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|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20200831 Address after: 100029 Beijing city Chaoyang District Beitucheng West Road No. 3 Patentee after: Institute of Microelectronics of the Chinese Academy of Sciences Address before: 100190, No. 19 West Fourth Ring Road, Beijing, Haidian District Patentee before: Aerospace Information Research Institute,Chinese Academy of Sciences Effective date of registration: 20200831 Address after: 100190, No. 19 West Fourth Ring Road, Beijing, Haidian District Patentee after: Aerospace Information Research Institute,Chinese Academy of Sciences Address before: 9 Dengzhuang South Road, Haidian District, Beijing 100094 Patentee before: Academy of Opto-Electronics, Chinese Academy of Sciences |
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| TR01 | Transfer of patent right |