CN101995275A - Static expansion method vacuum standard based method for measuring minimum gas flow - Google Patents
Static expansion method vacuum standard based method for measuring minimum gas flow Download PDFInfo
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- CN101995275A CN101995275A CN 201010523159 CN201010523159A CN101995275A CN 101995275 A CN101995275 A CN 101995275A CN 201010523159 CN201010523159 CN 201010523159 CN 201010523159 A CN201010523159 A CN 201010523159A CN 101995275 A CN101995275 A CN 101995275A
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Abstract
The invention relates to a static expansion method vacuum standard based method for measuring minimum gas flow, which comprises the following steps of: 1, exhausting a calibration chamber and a connecting vacuum pipe; 2, roasting the whole device for degassing; 3, controlling the inside of the calibration chamber to reach an ultimate vacuum of 10<-9> Pa in magnitude; 4, slowly raising the pressure inside the calibration chamber; 5, charging a high-purity gas with a certain pressure for the front stage of the static expansion method vacuum standard; 6, introducing the gas inside the calibration chamber into a vacuum system through a small hole; and 7, attenuating the pressure in the system according to the conductance of the small hole and the gas pressure to obtain gas flow. The gas pressure generated by using the static expansion method vacuum standard is used to replace the charged gas pressure of a fixed conductance method gas flow meter, and thus the method avoids using a capacitance film gauge or magnetic suspension rotor gauge to measure the pressure, thereby further improving the measurement accuracy of the gas flow.
Description
Technical field
The present invention relates to a kind of apparatus and method of measuring minimum gas flow, particularly a kind of apparatus and method of the minimum gas flow of measurement based on static expanding method vacuum standard.
Background technology
In Measurement Laboratory, adopt the high-precision gas micro-flowmeter to measure and provide the known gas flow mostly.
Document " Li Detian. German federal physical technique research institute (PTB) gas micro metering review. vacuum science and technology journal 23 (4), 2003. " introduced the gas meter that is in the German PTB of international highest level at present.The gas meter of PTB development is with three kinds of different pattern work: flow is in that (the Pa.m3/s scope of 10-8～10-4) is used constant-voltage method; Flow is used the fixed flow inducing defecation by enema and suppository during less than 10-8Pa.m3/s; Flow is used constant volume method during greater than 10-4Pa.m3/s.When adopting the fixed flow inducing defecation by enema and suppository, the gaseous tension that charges into of gas meter is measured with capacitor thin film rule or magnetic suspension rotor gauge usually.The transfer coefficient of magnetic suspension rotor gauge can change along with time, gaseous species and variation of temperature, there is the thermal transpiration effect in capacitor thin film rule under low-pressure, these effects limit the accurate measurement of pressure, thereby become the uncertainty factor that influences the maximum that flow accurately measures.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art part, a kind of minimum gas flow measurement apparatus and method based on static expanding method vacuum standard are provided, avoid with capacitor thin film rule or magnetic suspension rotor gauge gaging pressure, thereby further improve the measuring accuracy of gas flow, make flow value less than 1 * 10
-8Pa.m
3The gas flow of/s can accurately be measured, and the measurement lower limit of flow has been extended to 10
-16Pa.m
3/ s magnitude.
The invention provides a kind of minimum gas flow measurement device based on static expanding method vacuum standard, comprise the forepressure measuring system, valve one, the gaseous tension attenuation factor, valve two, calibration chamber, valve three, aperture, valve four, valve five, getter pump, valve six, molecular pump, forepump and ionization gauge are formed, the forepressure measuring system is connected with the gaseous tension attenuation factor by valve one, the gaseous tension attenuation factor is connected with calibration chamber by valve two, aperture links to each other with calibration chamber by valve three with valve four backs in parallel one end, one end links to each other with vacuum system, getter pump links to each other with calibration chamber by valve five, forepump is connected with calibration chamber by valve six with molecular pump polyphone back, and ionization gauge directly is connected on the calibration chamber.
Described forepressure measuring system is the standard source of the gas.
Described gaseous tension attenuation factor is made up of one-level sampling hut, secondary sampling hut and big volume vacuum chamber.
Described aperture, its molecular flow conductance is 10
-9m
3/ s magnitude.
Described valve six is the ultrahigh vacuum push-pull valve.
Described getter pump is the nonevaporable getter pump.
The measuring principle of device of the present invention is: after using molecular pump, forepump and getter pump that calibration chamber is evacuated to end vacuum, use getter pump to keep, because getter pump does not have pumping speed to inert gas, can make calibration chamber reach higher final vacuum; Inert gas flows out from the forepressure measuring system, expand into the gaseous tension attenuation factor, can calculate pressure in the gaseous tension attenuation factor according to Boyle's law; Conductance and the intrasystem pressure of gas pressure attenuation by aperture can obtain gas flow.Ionization gauge is used to detect the final vacuum of calibration chamber.
The present invention also provides a kind of minimum gas flow measurement method based on static expanding method vacuum standard, may further comprise the steps:
(1) opens valve three, valve four, valve six, start forepump and molecular pump successively, calibration chamber and connection vacuum pipe are bled;
(2) carry out bakeout degassing to installing integral body, after baking temperature rises to peak respectively with the uniform speed, keep 60～80h;
(3) during the baking maximum temperature keeps, open the connection valve of getter pump, getter pump is activated, stop after activating 2～4h, close getter pump and connect valve, and then reduce to room temperature gradually with the uniform speed, after temperature returns to room temperature, open getter pump again and connect valve, continue the 24～48h that bleeds, in calibration chamber, reach 10
-9The end vacuum of the Pa order of magnitude;
(4) valve-off three, valve six, the interior pressure of calibration chamber this moment begins slow rising, and pressure reaches stable after a period of time;
(5) charge into the high-purity gas of certain pressure for the prime of static expanding method vacuum standard, in the gaseous tension attenuation factor, choose corresponding expansion path and expansion progression, gas expand into calibration chamber by valve two;
(6) after the indoor pressure stability to be calibrated, open valve three, valve-off four is incorporated into the indoor gas of calibration in the vacuum system by aperture;
(7) conductance and the intrasystem pressure of gas pressure attenuation according to aperture obtains gas flow.
Be 200～300 ℃ to installing the highest whole baking temperature in the step (2), the uniform speed that baking temperature rises and descends is 20～40 ℃/h.
Activationary temperature to getter pump (10) in the step (3) is 450～500 ℃.
The present invention's beneficial effect compared with prior art is:
The gaseous tension that charges into that replaces fixed flow inducing defecation by enema and suppository gas meter with the gaseous tension of static expanding method vacuum standard generation, the uncertainty of measurement of having introduced when having avoided like this with capacitor thin film rule or magnetic suspension rotor gauge gaging pressure, thus the measuring accuracy of gas flow further improved.
Description of drawings
Fig. 1 is the minimum gas flow measurement structure drawing of device that the present invention is based on static expanding method vacuum standard.
Among the figure: 1-forepressure measuring system, 2,4,6,8,9,11-valve, 3-gaseous tension attenuation factor, 5-calibration chamber, 7-aperture, 10-getter pump, 12-molecular pump, 13-forepump, 14-ionization gauge.
Embodiment
As shown in Figure 1, for the minimum gas flow measurement device based on static expanding method vacuum standard of the present invention, form by forepressure measuring system 1, valve 1, gaseous tension attenuation factor 3, valve 24, calibration chamber 5, valve 36, aperture 7, valve 48, valve 59, getter pump 10, valve 6 11, molecular pump 12, forepump 13 and ionization gauge 14.
Gaseous tension attenuation factor 3 is made up of one-level sampling hut, secondary sampling hut and big volume vacuum chamber.
Valve 6 11 is the ultrahigh vacuum push-pull valve.
Getter pump 10 is the nonevaporable getter pump.
The measuring principle of this device is: after using molecular pump, forepump and getter pump that calibration chamber is evacuated to end vacuum, use getter pump to keep, because getter pump does not have pumping speed to inert gas, can make calibration chamber reach higher final vacuum; Inert gas flows out from the forepressure measuring system, expand into the gaseous tension attenuation factor, can calculate pressure in the gaseous tension attenuation factor according to Boyle's law; Conductance and the intrasystem pressure of gas pressure attenuation by aperture can obtain gas flow.Ionization gauge is used to detect the final vacuum of calibration chamber.
The implementation step of present embodiment is as follows:
(1) opens valve 36, valve 48, valve 6 11, start forepump 13 and molecular pump 12 successively, calibration chamber 5 and connection vacuum pipe are bled;
(2) carry out bakeout degassing to installing integral body, baking temperature keeps 72h, and then reduces to room temperature gradually with the uniform speed of 30 ℃/h after rising to separately peak respectively with the uniform speed of 30 ℃/h;
(3) during the baking maximum temperature keeps, open the connection valve 9 of getter pump 10, getter pump 10 is activated, activationary temperature is 500 ℃, stops behind the activation 2h, closes getter pump and connects valve, after temperature returns to room temperature, open getter pump again and connect valve, continue the 48h that bleeds, this moment, calibration chamber 5 interior final vacuums were 6.7 * 10
-9Pa;
(4) valve-off 36, valve 11, this moment, calibration chamber 5 interior pressure began slow rising, and pressure reaches stationary value behind the 120min, and the reading of ionization gauge 14 is 3.2 * 10
-8Pa;
(5) high-purity He gas of charging into for the prime of static expanding method vacuum standard in gaseous tension attenuation factor 3, is chosen corresponding expansion path and expansion progression, and gas is introduced calibration chamber 5 by valve 24;
(6) after the pressure stability in the chamber 5 to be calibrated, the reading of ionization gauge 14 is 8.1 * 10
-7Pa is by the gaseous tension P of static expanding method vacuum standard generation
0Be 7.644 * 10
-7Pa.Open valve 36, valve-off 48 is incorporated into the gas in the calibration chamber 5 in the vacuum system by aperture 7, reaches mobile equilibrium behind the 10min.
(7) then the gas flow that provides of this device is calculated by (1) formula
Q＝p
0·C
He..........................................(1)
In the formula: Q-flow, Pa.m
3/ s;
P
0The gaseous tension that-static expanding method vacuum standard produces, Pa;
C
He-under the molecular flow condition, aperture 7 is with respect to the conductance of He, m
3/ s.
Wherein, record C in advance
HeBe 1.26 * 10
-9m
3/ s.
With P
0=7.644 * 10
-7Pa, C=1.26 * 10
-9m
3/ s is substitution formula (1) respectively, and the measured value that calculates flow is 9.631 * 10
-16Pa.m
3/ s.
Claims (3)
1. minimum gas flow measurement method based on static expanding method vacuum standard may further comprise the steps:
(1) opens valve three (6), valve four (8), valve six (11), start forepump (13) and molecular pump (12) successively, calibration chamber (5) and connection vacuum pipe are bled;
(2) carry out bakeout degassing to installing integral body, after baking temperature rises to peak respectively with the uniform speed, keep 60～80h;
(3) during the baking maximum temperature keeps, open the connection valve (9) of getter pump (10), getter pump (10) is activated, stop after activating 2～4h, close getter pump and connect valve, and then reduce to room temperature gradually with the uniform speed, after temperature returns to room temperature, open getter pump again and connect valve, continue the 24～48h that bleeds, in calibration chamber (5), reach 10
-9The end vacuum of the Pa order of magnitude;
(4) valve-off three (6), valve six (11), the pressure in calibration chamber this moment (5) begins slow rising, and pressure reaches stable after a period of time;
(5) charge into the high-purity gas of certain pressure for the prime of static expanding method vacuum standard, in gaseous tension attenuation factor (3), choose corresponding expansion path and expansion progression, gas expand into calibration chamber (5) by valve two (4);
(6) after the pressure stability in chamber to be calibrated (5), open valve three (6), valve-off four (8) is incorporated into the gas in the calibration chamber (5) in the vacuum system by aperture (7);
(7) conductance and the intrasystem pressure of gas pressure attenuation by aperture obtains gas flow.
2. a kind of minimum gas flow measurement method according to claim 1 is characterized in that, is 200～300 ℃ to installing the highest whole baking temperature in the described step (2), and the uniform speed that baking temperature rises and descends is 20～40 ℃/h.
3. a kind of minimum gas flow measurement method according to claim 1 is characterized in that the activationary temperature to getter pump (10) in the described step (3) is 450～500 ℃.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103759906A (en) * | 2013-12-24 | 2014-04-30 | 兰州空间技术物理研究所 | Device and method for correcting vacuum leakage hole based on vacuum standard of static expansion method |
| CN103791985A (en) * | 2014-01-16 | 2014-05-14 | 宁波创盛仪表有限公司 | Static state standard cubic meter calibration device and calibration method of static state standard cubic meter calibration device |
| CN104266820A (en) * | 2014-09-19 | 2015-01-07 | 兰州空间技术物理研究所 | Pressure decay method based small orifice conductance measuring method |
| CN104596747A (en) * | 2014-12-26 | 2015-05-06 | 舟山市恒威船舶配件有限公司 | Vacuum flux test device of air pipe head |
| CN107806565A (en) * | 2017-09-14 | 2018-03-16 | 北京航天控制仪器研究所 | A kind of vacuum gas filling equipment and implementation method |
| CN113447087A (en) * | 2021-06-25 | 2021-09-28 | 北京航空航天大学 | Flow measurement method based on dynamic optimization of three pressure sensors |
| CN113607519A (en) * | 2021-08-02 | 2021-11-05 | 合肥工业大学 | Residual gas analysis device and method based on laser damage sample |
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| CN102589820B (en) * | 2012-02-06 | 2014-10-15 | 江苏东方航天校准检测有限公司 | System and method for calibrating lower limit of positive-pressure leak by extending constant volume method |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103759906A (en) * | 2013-12-24 | 2014-04-30 | 兰州空间技术物理研究所 | Device and method for correcting vacuum leakage hole based on vacuum standard of static expansion method |
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| CN103791985A (en) * | 2014-01-16 | 2014-05-14 | 宁波创盛仪表有限公司 | Static state standard cubic meter calibration device and calibration method of static state standard cubic meter calibration device |
| CN104266820A (en) * | 2014-09-19 | 2015-01-07 | 兰州空间技术物理研究所 | Pressure decay method based small orifice conductance measuring method |
| CN104596747A (en) * | 2014-12-26 | 2015-05-06 | 舟山市恒威船舶配件有限公司 | Vacuum flux test device of air pipe head |
| CN107806565A (en) * | 2017-09-14 | 2018-03-16 | 北京航天控制仪器研究所 | A kind of vacuum gas filling equipment and implementation method |
| CN113447087A (en) * | 2021-06-25 | 2021-09-28 | 北京航空航天大学 | Flow measurement method based on dynamic optimization of three pressure sensors |
| CN113607519A (en) * | 2021-08-02 | 2021-11-05 | 合肥工业大学 | Residual gas analysis device and method based on laser damage sample |
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