CN105136389A - 10-9Pa magnitude vacuum partial pressure calibration device and calibration coefficient acquisition method - Google Patents
10-9Pa magnitude vacuum partial pressure calibration device and calibration coefficient acquisition method Download PDFInfo
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- CN105136389A CN105136389A CN201510428627.1A CN201510428627A CN105136389A CN 105136389 A CN105136389 A CN 105136389A CN 201510428627 A CN201510428627 A CN 201510428627A CN 105136389 A CN105136389 A CN 105136389A
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Abstract
The invention provides a 0-9Pa magnitude vacuum partial pressure calibration device comprising a fine-adjusting valve, an air source, a sample matching room, eight valves, a sampling room, an auxiliary expansion room, a composite vacuum gauge, a separating vacuum gauge, a small hole, a calibration room, a piston pressure gauge, a sample introducing room and a calibrated partial pressure mass spectrometer. Peripheral equipment is an air exhaust system. An air expansion method is utilized, and higher fore pressure is introduced to the calibration room through air expansion and small hole attenuation so that the lower limit of calibration of the partial pressure mass spectrometer is extended, and calibration of the 10-9Pa magnitude partial pressure mass spectrometer is solved. Besides, the high-precision piston pressure gauge acts as a fore pressure reference standard, and a magnetic suspended rotor vacuum gauge in the prior art is substituted so that uncertainty of measurement is reduced and thus calibration precision is enhanced.
Description
Technical field
The invention belongs to vacuumatic measuring technical guarantee field, particularly relate to a kind of 10
-9the vacuum partial pressure calibrating installation of Pa magnitude and calibration factor acquisition methods.
Background technology
Mass spectrometers for partial pressure is widely used in commercial production every field, and its partial pressure measurement lower limit is mostly 10
-9pa.The calibration of mass spectrometers for partial pressure is an important research direction in vacuumatic measuring field.Document " Li get Tian, Li Zhenghai, Feng Yan, Zhang Dixin, Zhang Jianjun, Xu Hang, Gong Yueli, Li Li. the development of Partial Pressure Mass Spectrometry Calibration System. vacuum science and technology, 2001. " describe current China uniquely with Calibration System of Mass Spectrometers for Partial Pressure.
This calibrating installation adopts two kinds of methods to realize the calibration of mass spectrometers for partial pressure.One is: the forepressure utilizing magnetic suspension spinning rotor vacuum gauge Measurement and calibration indoor standard partial pressure, directly compares with by school mass spectrometers for partial pressure, namely utilizes direct comparison method to realize mass spectrometers for partial pressure 10
-4pa ~ 10
-1calibration in Pa pressure limit, as shown in Figure 1.Another kind is the pressure utilizing magnetic suspension spinning rotor vacuum gauge to measure upstream chamber, calibration chamber is introduced by after the decline of pressure of upstream chamber by aperture, as long as know the decline of pressure ratio of aperture, the standard scores pressure of calibration chamber can be obtained, thus realize mass spectrometers for partial pressure 10
-6pa ~ 10
-4calibration in Pa pressure limit, as shown in Figure 2.
The weak point of this system limits by calibration steps, and calibration range is confined to 10
-6pa ~ 10
-1pa, the measurement lower limit of the mass spectrometers for partial pressure of current space application reaches 10
-9pa magnitude, this system cannot realize 10
-9the accurate alignment of the mass spectrometers for partial pressure of Pa magnitude; Also the system or the method that not yet find that there is other at present can reach 10
-9the accurate alignment of Pa magnitude.In addition, this system uses magnetic suspension spinning rotor vacuum gauge as reference standard, and for measuring forepressure, uncertainty is greater than 1%, and uncertainty is larger.
Summary of the invention
For solving the problem, the invention provides a kind of 10
-9the vacuum partial pressure calibrating installation of Pa magnitude and calibration factor acquisition methods, can realize 10
-9the calibration of the mass spectrometers for partial pressure of Pa magnitude.
Of the present invention 10
-9the vacuum partial pressure calibrating installation of Pa magnitude, it comprises: micrometering valve, source of the gas, sample room, eight valves, sampling hut, secondary expansion room, compound vacuum gauge, aperture, calibration chamber, piston manometer, Sample Room and by school mass spectrometers for partial pressure, separate vacuum meter; Peripherals is extract system.
Sample room is connected with source of the gas by micrometering valve, is connected with sampling hut by the first valve; Sampling hut is connected with Sample Room by the second valve, is connected with piston manometer by the 7th valve; Sample Room is connected with secondary expansion room by the 3rd valve, is connected with compound vacuum gauge by the 4th valve, and is connected with calibration chamber by the 5th valve after connecting aperture; Calibration chamber is connected with by school mass spectrometers for partial pressure by the 8th valve, is connected with separate vacuum meter by the 6th valve; And the pipeline of vacuum partial pressure calibrating installation is connected with extract system.
Further, described micrometering valve is ultrahigh vacuum all-metal micrometering valve.
Further, described source of the gas is the mixed gas of multiple pure gas source of the gas or known component.
Further, described sample room is stainless steel spherical structure, and volume is 10L.
Further, described eight valves are ultrahigh vacuum all-metal ball valve.
Further, described sampling hut, secondary expansion room, Sample Room are stainless steel spherical structure.
Further, described Sample Room and secondary expansion room volumetric ratio are 10.
Further, the decline of pressure ratio of described aperture is 1/1000.
Further, sample room, Sample Room, calibration chamber are vacuumized by the different extract system of three covers.
The present invention also provides a kind of 10
-9the calibration factor acquisition methods of the vacuum partial pressure calibrating installation of Pa magnitude, it comprises the following steps:
Step 1, measures the volumetric ratio of sampling hut and Sample Room
Step 2, extracts the gas in vacuum partial pressure calibrating installation and in pipeline, and closes micrometering valve, the first valve, the second valve, the 3rd valve, the 4th valve, the 5th valve, the 6th valve, the 7th valve and the 8th valve;
Step 3, opens micrometering valve and the first valve, is incorporated in sampling hut by the gas in source of the gas by sample room, and closedown first valve after pressure stabilisation, then opens the 7th valve, is measured the pressure p of insufflation gas in sampling hut by piston manometer;
Step 4, opens the second valve, and by gas expansion in sampling hut in Sample Room, closedown second valve after pressure stabilisation, because of V
sample introduction>>V
sampling, then Sample Room gaseous tension is
Step 5, open the 3rd valve, by gas expansion in secondary expansion room, after pressure stabilisation, open the 4th valve, read the gaseous tension of compound vacuum gauge, whether calibration requirements is met according to the gaseous tension that this gaseous tension judges in Sample Room, if do not meet, continue by gas expansion to secondary expansion room, until meet calibration requirements; If the gaseous tension in Sample Room meets calibration requirements, then close the 3rd valve, now Sample Room gaseous tension is
Step 6, open the 5th valve, gas is incorporated in calibration chamber by aperture, after pressure stabilisation, open the gaseous tension that the 6th valve reads separate vacuum meter, and whether meet calibration requirements, if do not meet according to the gaseous tension that this gaseous tension judges in calibration chamber, continue gas to be incorporated into calibration chamber by aperture, until meet calibration requirements; If the gaseous tension in calibration chamber meets calibration requirements, then close the 5th valve, now the standard scores pressure of calibration chamber is
Step 8, opens the 8th valve, after pressure stabilisation, reads by the pressure reading of school mass spectrometers for partial pressure, closes the 8th valve;
Step 9, by described standard scores pressure with compared by the pressure reading of school mass spectrometers for partial pressure, obtain by the calibration factor of school mass spectrometers for partial pressure.
Beneficial effect:
Present invention utilizes gas expansion method, by higher forepressure by being incorporated into again in calibration chamber after gas expansion and aperture decay, extending the calibration lower limit of mass spectrometers for partial pressure, solving 10
-9the calibration of the mass spectrometers for partial pressure of Pa magnitude.In addition, with high-precision piston manometer as standard vacuum gauge, substituted for magnetic suspension spinning rotor vacuum gauge of the prior art, reduce uncertainty of measurement, thus improve calibration accuracy.
Accompanying drawing explanation
Fig. 1 is direct comparison method device schematic diagram of the prior art;
Fig. 2 is decline of pressure subtraction unit schematic diagram of the prior art;
Fig. 3 is of the present invention 10
-9the structure design principle schematic diagram of the vacuum partial pressure calibrating installation of Pa magnitude.
In figure:
1-micrometering valve, 2-source of the gas, 3-sample room, 4-first valve, 6-second valve, 7-the 3rd valve, 10-the 4th valve, 12-the 5th valve, 14-the 6th valve, 15-the 7th valve, 19-the 8th valve, 5-sampling hut, 8-secondary expansion room, 9-compound vacuum gauge, 11-aperture, 13-calibration chamber, 16-piston manometer, 17-Sample Room, 18-are by school mass spectrometers for partial pressure, 20-separate vacuum meter, 21-valve; 22-magnetic suspension spinning rotor vacuum gauge, 23-upstream chamber.
Embodiment
As shown in Figure 3, of the present invention 10
-9the vacuum partial pressure calibrating installation of Pa magnitude and calibration factor acquisition methods, wherein device comprises: micrometering valve 1, source of the gas 2,3, eight, sample room valve, sampling hut 5, secondary expansion room 8, compound vacuum gauge 9, aperture 11, calibration chamber 13, piston manometer 16, Sample Room 17, by school mass spectrometers for partial pressure 18, separate vacuum meter 20.
Wherein, eight valves are respectively the first valve 4, second valve 6, the 3rd valve 7, the 4th valve 10, the 5th valve 12, the 6th valve 14, the 7th valve 15 and the 8th valve 19.
Micrometering valve 1 is ultrahigh vacuum all-metal micrometering valve, and leak rate is less than 10
-9pam
3/ s magnitude.
Source of the gas 2 is the mixed gas of multiple single high-purity gas combination or known component.
Sample room 3 is 316L stainless steel spherical structure, and volume is 10L, fully mixes for the gas provided by source of the gas 2, the calibration gas needed for formation.
Sampling hut 5, obtains the calibration gas of required pressure from sample room 3; Wherein calibration gas forepressure is recorded by piston manometer 16.
Eight valves are ultrahigh vacuum all-metal ball valve.
Described sampling hut 5, secondary expansion room 8, Sample Room 17 are 316L stainless steel spherical structure; Sample Room and secondary expansion room volumetric ratio are 10; CV is much smaller than Sample Room volume, and volumetric ratio is selected according to by the calibration range of school mass spectrometers for partial pressure.Above-mentioned 316L is a kind of stainless steel material trade mark.
Sample Room 17 completes the once expansion of calibration gas, and gaseous tension is once reduced.
Secondary expansion room 8 completes the reexpansion of calibration gas, and gaseous tension secondary is reduced.
The attenuation ratio of aperture 11 is 1/1000, and gaseous tension is reduced for three times.
Calibration chamber 13 obtains the standard scores pressure of calibration gas, compares with by the partial pressure shown in school mass spectrometers for partial pressure 18, obtains calibration factor.
Compound vacuum gauge 9 is for monitoring the gaseous tension in Sample Room 17; Separate vacuum meter 20 is for monitoring the gaseous tension in calibration chamber 13.
Source of the gas 2 is connected with sample room 3 by micrometering valve 1; Sampling hut 5 is connected with sample room 3 by the first valve 4, is connected with Sample Room 17 by the second valve 6; Piston manometer 16 is connected with sampling hut 5 by the 7th valve 15, for measuring the gaseous tension in sampling hut 5; Secondary expansion room 8 is connected with Sample Room 17 by the 3rd valve 7; Compound vacuum gauge 9 is connected with Sample Room 17 by the 4th valve 10, for measuring the gaseous tension in Sample Room 17; Aperture 11 and the 5th valve 12 are connected between Sample Room 17 and calibration chamber 13; Be connected with calibration chamber 13 by the 8th valve 19 by school mass spectrometers for partial pressure 18; Separate vacuum meter 20 is connected with calibration chamber 13, for the gaseous tension in Measurement and calibration room 13 by the 8th valve 19; Sample room 3 and sampling hut 5 are vacuumized by the first extract system, and secondary expansion room 8 and Sample Room 17 are vacuumized by the second extract system, and calibration chamber 13 is vacuumized by the 3rd extract system.
Performing step is as follows:
(1) according to by the calibration range of school quadrupole mass spectrometer 18, select air inlet path, measure the volumetric ratio of sampling hut 5 and Sample Room 17
(2) start the first extract system, the second extract system, the 3rd extract system, extract the gas in vacuum partial pressure calibrating installation and in pipeline; And close the first valve 4, second valve 6, the 3rd valve 7, the 4th valve 10, the 5th valve 12, the 6th valve 14, the 7th valve 15 and the 8th valve 19;
(3) extract system is closed, open micrometering valve 1 and the first valve 4, gas is incorporated in sampling hut 5 by sample room 3, closedown first valve 4 after pressure stabilisation, then open the 7th valve 15, measured pressure p=1 × 10 of insufflation gas by piston manometer 16
4pa;
(4) open the second valve 6, by gas expansion in Sample Room 17, closedown second valve 6 after pressure stabilisation, then Sample Room 17 gaseous tension is 1 × 10
-5pa;
(5) the 3rd valve 7 is opened, by gas expansion in secondary expansion room 8, after pressure stabilisation, open the 4th valve 10, read the gaseous tension of compound vacuum gauge 9, whether meet calibration requirements, if do not meet according to the gaseous tension that this gaseous tension judges in Sample Room 17, continue by gas expansion to secondary expansion room 8, until meet calibration requirements; If the gaseous tension in Sample Room 17 meets calibration requirements, then close the 3rd valve 7, now Sample Room 17 gaseous tension 9.1 × 10
-6pa;
(6) the 5th valve 12 is opened, gas is incorporated in calibration chamber 13 by aperture 11, after pressure stabilisation, open the gaseous tension that the 6th valve 14 reads separate vacuum meter 20, and whether meet calibration requirements according to the gaseous tension that this gaseous tension judges in calibration chamber 13, if do not meet, continue gas to be incorporated into calibration chamber 13 by aperture 11, until meet calibration requirements; If the gaseous tension in calibration chamber 13 meets calibration requirements, then valve-off 12, now the standard scores pressure of calibration chamber 13 is 9.1 × 10
-9pa;
(7) the 8th valve 19 is opened, after pressure stabilisation, read by the pressure reading of school mass spectrometers for partial pressure 18, close the 8th valve 19;
(8) by standard scores pressure with compared by the partial pressure reading of school mass spectrometers for partial pressure 18, obtain by the calibration factor of school mass spectrometers for partial pressure.
The reason of three kinds of extract systems is adopted to be that the gaseous tension in sample room 3, Sample Room 17 and calibration chamber 13 requires difference, and distant between three, and if use an extract system, then require higher to pipeline, thus cost is higher.
Certainly; the present invention also can have other various embodiments; when not deviating from the present invention's spirit and essence thereof; those of ordinary skill in the art are when making various corresponding change and distortion according to the present invention, but these change accordingly and are out of shape the protection domain that all should belong to the claim appended by the present invention.
Claims (10)
1. one kind 10
-9the vacuum partial pressure calibrating installation of Pa magnitude, it is characterized in that, comprising: micrometering valve (1), source of the gas (2), sample room (3), eight valves (4,6,7,10,12,14,15,19), sampling hut (5), secondary expansion room (8), compound vacuum gauge (9), aperture (11), calibration chamber (13), piston manometer (16), Sample Room (17) and by school mass spectrometers for partial pressure (18), separate vacuum meter (20); Peripherals is extract system;
Sample room (3) is connected with source of the gas (2) by micrometering valve (1), is connected with sampling hut (5) by the first valve (4); Sampling hut (5) is connected with Sample Room (17) by the second valve (6), is connected with piston manometer (16) by the 7th valve (15); Sample Room (17) is connected with secondary expansion room (8) by the 3rd valve (7), is connected with compound vacuum gauge (9) by the 4th valve (10), and connection aperture (11) is connected with calibration chamber (13) by the 5th valve (12) afterwards; Calibration chamber (13) is connected with by school mass spectrometers for partial pressure (18) by the 8th valve (19), is connected with separate vacuum meter (20) by the 6th valve (14); And the pipeline of vacuum partial pressure calibrating installation is connected with extract system.
2. one 10 as claimed in claim 1
-9the vacuum partial pressure calibrating installation of Pa magnitude, is characterized in that, described micrometering valve (1) is ultrahigh vacuum all-metal micrometering valve.
3. one 10 as claimed in claim 1
-9the vacuum partial pressure calibrating installation of Pa magnitude, is characterized in that, the mixed gas that described source of the gas (2) is the combination of multiple pure gas or known component.
4. one 10 as claimed in claim 1
-9the vacuum partial pressure calibrating installation of Pa magnitude, is characterized in that, described sample room (3) is stainless steel spherical structure, and volume is 10L.
5. one 10 as claimed in claim 1
-9the vacuum partial pressure calibrating installation of Pa magnitude, is characterized in that, described eight valves are ultrahigh vacuum all-metal ball valve.
6. one 10 as claimed in claim 1
-9the vacuum partial pressure calibrating installation of Pa magnitude, is characterized in that, described sampling hut (5), secondary expansion room (8), Sample Room (17) are stainless steel spherical structure.
7. one 10 as claimed in claim 1
-9the vacuum partial pressure calibrating installation of Pa magnitude, is characterized in that, described Sample Room (17) and secondary expansion room (8) volumetric ratio are 10.
8. one 10 as claimed in claim 1
-9the vacuum partial pressure calibrating installation of Pa magnitude, is characterized in that, the decline of pressure ratio of described aperture (11) is 1/1000.
9. one 10 as claimed in claim 1
-9the vacuum partial pressure calibrating installation of Pa magnitude, is characterized in that, sample room (3), Sample Room (17), calibration chamber (13) are vacuumized by the different extract system of three covers.
10. one kind 10
-9the calibration factor acquisition methods of the vacuum partial pressure calibrating installation of Pa magnitude, is characterized in that, comprise the following steps:
Step 1, measures the volumetric ratio of sampling hut (5) and Sample Room (17)
Step 2, extract the gas in vacuum partial pressure calibrating installation and in pipeline, and close micrometering valve (1), the first valve (4), the second valve (6), the 3rd valve (7), the 4th valve (10), the 5th valve (12), the 6th valve (14), the 7th valve (15) and the 8th valve (19);
Step 3, open micrometering valve (1) and the first valve (4), gas in source of the gas (2) is incorporated in sampling hut (5) by sample room (3), closedown first valve (4) after pressure stabilisation, then open the 7th valve (15), measured the pressure p of insufflation gas in sampling hut (5) by piston manometer (16);
Step 4, opens the second valve (6), and by gas expansion in sampling hut (5) in Sample Room (17), closedown second valve (6) after pressure stabilisation, because of V
sample introduction>>V
sampling, then Sample Room (17) gaseous tension is
Step 5, open the 3rd valve (7), by gas expansion in secondary expansion room (8), after pressure stabilisation, open the 4th valve (10), read the gaseous tension of compound vacuum gauge (9), judge whether the gaseous tension in Sample Room (17) meets calibration requirements according to this gaseous tension, if do not meet, continue by gas expansion to secondary expansion room (8), until meet calibration requirements; If the gaseous tension in Sample Room (17) meets calibration requirements, then close the 3rd valve (7), now Sample Room (17) gaseous tension is
Step 6, open the 5th valve (12), gas is incorporated in calibration chamber (13) by aperture (11), after pressure stabilisation, open the gaseous tension that the 6th valve (14) reads separate vacuum meter (20), and judge whether the gaseous tension in calibration chamber (13) meets calibration requirements, if do not meet according to this gaseous tension, gas is continued to be incorporated into calibration chamber (13), until meet calibration requirements by aperture (11); If the gaseous tension in calibration chamber (13) meets calibration requirements, then close the 5th valve (12), now the standard scores pressure of calibration chamber (13) is
Step 8, opens the 8th valve (19), after pressure stabilisation, reads by the pressure reading of school mass spectrometers for partial pressure (18), closes the 8th valve (19);
Step 9, by described standard scores pressure with compared by the pressure reading of school mass spectrometers for partial pressure (18), obtain by the calibration factor of school mass spectrometers for partial pressure.
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| CN106289639A (en) * | 2016-08-31 | 2017-01-04 | 兰州空间技术物理研究所 | A kind of measuring method of vacuum partial pressure based on ion gauge |
| CN106441702A (en) * | 2016-08-31 | 2017-02-22 | 兰州空间技术物理研究所 | Dual-hole spectrometer calibration device and method |
| CN107991020A (en) * | 2017-11-29 | 2018-05-04 | 兰州空间技术物理研究所 | A kind of new Calibration System of Mass Spectrometers for Partial Pressure and method |
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| CN106441702A (en) * | 2016-08-31 | 2017-02-22 | 兰州空间技术物理研究所 | Dual-hole spectrometer calibration device and method |
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| CN106289639B (en) * | 2016-08-31 | 2019-04-05 | 兰州空间技术物理研究所 | A kind of measurement method of the vacuum partial pressure based on ion gauge |
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| CN107991020B (en) * | 2017-11-29 | 2020-11-27 | 兰州空间技术物理研究所 | Partial pressure mass spectrometer calibration device and method |
| CN111433571A (en) * | 2017-11-30 | 2020-07-17 | 基斯特勒控股公司 | Method and computer program product for determining a measurement uncertainty of a measurement system |
| CN111433571B (en) * | 2017-11-30 | 2022-06-28 | 基斯特勒控股公司 | Method and computer program product for determining a measurement uncertainty of a measurement system |
| CN108151961B (en) * | 2017-12-08 | 2020-02-07 | 兰州空间技术物理研究所 | Extreme high vacuum calibration device and method |
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| CN112782264B (en) * | 2020-12-14 | 2023-10-24 | 兰州空间技术物理研究所 | Device and method for detecting and calibrating trace harmful gas in closed space |
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