CN106441731A - High-low-temperature vacuum leak hole calibration device and method - Google Patents
High-low-temperature vacuum leak hole calibration device and method Download PDFInfo
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- CN106441731A CN106441731A CN201610796942.4A CN201610796942A CN106441731A CN 106441731 A CN106441731 A CN 106441731A CN 201610796942 A CN201610796942 A CN 201610796942A CN 106441731 A CN106441731 A CN 106441731A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01M—TESTING STATIC OR DYNAMIC BALANCE OF MACHINES OR STRUCTURES; TESTING OF STRUCTURES OR APPARATUS, NOT OTHERWISE PROVIDED FOR
- G01M3/00—Investigating fluid-tightness of structures
- G01M3/02—Investigating fluid-tightness of structures by using fluid or vacuum
- G01M3/26—Investigating fluid-tightness of structures by using fluid or vacuum by measuring rate of loss or gain of fluid, e.g. by pressure-responsive devices, by flow detectors
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Abstract
The invention relates to a high-low-temperature vacuum leak hole calibration device and method, and belongs to the field of measurement. In the device, a standard vacuum leak hole is connected with a calibration room through a first valve; an air exhauster set is connected with the calibration room through a third valve; a calibrated vacuum leak hole is connected with the calibration room through a second valve, and is disposed in a high-low-temperature room; a mass spectrometer is connected with the calibration room; a vacuum gauge is connected with the calibration room; a temperature control board is disposed in the high-low-temperature room, and is connected with a temperature control system outside the high-low-temperature room. The method is implemented through the device, and obtains the leak rate of the calibrated vacuum leak hole. The method and device can achieve the accurate calibration of the leak rate of the vacuum leak hole under different temperature conditions, avoids a problem of bigger measurement uncertainty caused by that a vacuum leak rate is calibrated under a lab temperature condition and a standard flow is provided in different application environments in the prior art, and achieves the calibration of the vacuum leak rate under the actual application temperature of the vacuum leak rate.
Description
Technical field
The present invention relates to a kind of high/low temperature vacuum leak calibration device and method, especially, is related to a kind of realization at -50 DEG C
In～+50 DEG C, the device and method of vacuum leak rate accurate calibration, belongs to fields of measurement.
Background technology
In Measurement Laboratory, the calibration of vacuum leak is provided using referance leak and high-precision gas micro-flowmeter mostly
Known gas flow, is compared by measuring probe gas ion stream.Using relative method, constant conductance method, shunting and
During the calibration of static buildup method, the calibration to vacuum leak leak rate is all carried out under the conditions of laboratory temperature (23 DEG C ± 3 DEG C).
Document " Li get Tian, Li Zhenghai, Guo Meiru, etc. the development of superelevation/XHV calibrating installation. vacuum science and skill
Art journal 26 (2), 2007. " describe a kind of new method-shunting that current calibration extreme high vacuum gauge is adopted.Shunting be by
High-precision gas micro-flowmeter provides known gas flow and is injected into diffluence room, then by diffluence room, gas flow is diverted to pole
Fine vacuum calibration chamber and ultrahigh vacuum calibration chamber, it is achieved that calibration lower limit is extended to 1 × 10-10Pa·m3/ s, shunting is right
The development of dynamic flow method.
Static buildup method is measured using ion stream climbing, it is to avoid in the case of minimum vacuum leak rate is minimum, quadrupole
Mass spectrograph cannot be distinguished by being calibrated ion stream and background ions stream, and calibration lower limit is extended to 1 × 10-12Pa·m3/s.
The weak point of above method is to lay particular emphasis on calibration lower limit extension and the reduction of uncertainty of measurement, to vacuum leak
The calibration of leak rate is all carried out under the conditions of laboratory temperature (23 DEG C ± 3 DEG C).
Vacuum leak is calibrated under ambient laboratory conditions, provides normal flow during use at different ambient temperatures, by
Under different temperatures, small opening working condition, gaseous state occurs all change, and causes the leak rate value under relevant temperature point inclined
Leak rate value at a temperature of using room temperature as calibration, so as to introduce larger uncertainty of measurement.
Content of the invention
For the weak point of existing calibration steps, an object of the present invention is to provide a kind of high/low temperature vacuum leak
Calibrating installation, the second object of the present invention is to provide a kind of high/low temperature vacuum leak calibration method；Described device and method can
To realize under condition of different temperatures, the accurate alignment of vacuum leak leak rate, it is to avoid in prior art, vacuum leak leak rate is in reality
Calibrate under the conditions of testing room temperature (23 DEG C ± 3 DEG C), but under different use environments, normal flow is provided, so as to introduce larger measurement
The problem of uncertainty, it is achieved that the calibration to vacuum leak rate at the actually used temperature of vacuum leak rate.
For the purpose of the present invention is realized, technical scheme below is provided.
A kind of high/low temperature vacuum leak calibration device, the main building block of described device include standard vacuum small opening,
One valve, mass spectrograph, calibration chamber, vacuometer, the second valve, high and low temperature room, the 3rd valve, pumping unit, temperature control plate and temperature
Degree control system.
Wherein, standard vacuum small opening is connected with calibration chamber by the first valve, for for calibrating indoor offer calibrating gas
Flow；Pumping unit is connected with calibration chamber by the 3rd valve, for gas bleeding, realizes vacuum；Passed through by school vacuum leak
Second valve is connected with calibration chamber, is placed in high and low temperature room；Mass spectrograph is connected with calibration chamber, for measuring ion stream；Vacuum
Meter is connected with calibration chamber, for monitoring vacuum；Temperature control plate is placed in high and low temperature room, with the temperature control outside high and low temperature room
System connects, and realizes to calibration chamber and the temperature control by school vacuum leak.
First valve, the second valve and the 3rd valve are all-metal ultrahigh vacuum valve.
Mass spectrograph is preferably four-stage mass spectrometer.
Standard vacuum small opening and by school vacuum leak can be connected with having air source or with source of the gas acquisition source of the gas.
Pumping unit is the device for reaching vacuum described in state of the art for pumping, can be mechanical pump, molecule
Pump, bimolecular pump or mechanical pump are combined with molecular pump.
A kind of high/low temperature vacuum leak calibration method, methods described adopts a kind of high/low temperature vacuum leak of the present invention
Calibrating installation is carried out, and in described device, all building blocks are using being front in closed mode, the leak rate of standard vacuum small opening
Known；Methods described step is as follows：
(1) the 3rd valve is opened, is started pumping unit, gas bleeding from calibration chamber, and continue in following steps
Gas bleeding, to reach required vacuum, until all steps are completed；
(2) bakeout degassing is integrally carried out to described device, baking temperature is risen to after 200 DEG C～250 DEG C with the uniform velocity speed,
60h～80h is kept, then again room temperature is gradually decreased down with the uniform velocity speed, the at the uniform velocity speed of raising and lowering is identical, is 20 DEG C/h
～40 DEG C/h；
(3) with vacuometer, vacuum measurement is carried out to calibration chamber, when the pressure of calibration chamber meets the operating pressure of mass spectrograph
During requirement, open mass spectrograph and adjust its parameter and be at stable working condition；
(4) start-up temperature control system and temperature control plate, the calibration temperature needed for making high and low temperature indoor temperature balance and reaching
Degree, is represented with t, keeps the temperature fluctuation in high and low temperature room to be less than or equal to 3 DEG C/min；
(5) the corresponding ion stream of described device background being obtained with mass spectrograph measurement, uses I0Represent；
(6) the second valve is opened, the gas for being flowed out by school vacuum leak is introduced in calibration chamber；
(7) after indoor gas to be calibrated reach dynamic equilibrium, with mass spectrograph measurement obtain when school vacuum leak is opened from
Subflow, uses ILRepresent；
(8) the first valve is opened, the gas that standard vacuum small opening is flowed out is introduced in calibration chamber, flows into the standard of calibration chamber
Gas flow is the leak rate of standard vacuum small opening, uses QSRepresent；
(9), after indoor gas to be calibrated reach dynamic equilibrium, obtained when standard vacuum small opening is opened with mass spectrograph measurement
Ion stream, uses ISRepresent；
(10) leak rate by school vacuum leak at a temperature of calibration, uses QL, (t)Represent, calculated by equation below (1)
Arrive：
In formula：
QL, (t)By leak rate of the school vacuum leak at a temperature of calibration, unit is：Pa·m3/s；
QSThe calibrating gas flow of calibration chamber is flowed into, unit is：Pa·m3/s；
I0The corresponding ion stream of described device background, unit is：A；
ILIon stream when being opened by school vacuum leak, unit is：A；
ISIon stream when standard vacuum small opening is opened, unit is：A；
By the leak rate of school vacuum leak at a temperature of new calibration after obtaining if desired changing in -50 DEG C～50 DEG C, can
Realized by following steps：
The first valve is closed, high and low temperature indoor temperature balance is made by regulating and controlling temperature control system and temperature control plate and is reached
New calibration temperature, keeps the temperature fluctuation in high and low temperature room to be less than or equal to 3 DEG C/min；
Repeat step (5) and (7)～(10) are obtained the leak rate by school vacuum leak at a temperature of new calibration.
In the present invention, the gas reaches dynamic equilibrium and refers under evacuation state, and calibration gas pressure inside is not sent out
Changing.
Beneficial effect
1. the invention provides a kind of high/low temperature vacuum leak calibration device and method, adopts by calibration chamber, by school vacuum
Small opening is placed in high and low temperature room, it is achieved that vacuum leak use when different temperature points environmental simulation so that vacuum leak
Working condition be consistent with use environment；
2. the invention provides a kind of high/low temperature vacuum leak calibration device and method, using high and low temperature indoor and outdoor temperature control
Plate and temperature control system, make to obtain arbitrary temp point in the range of uniform, stable -50 DEG C～+50 DEG C in high/low temperature room, adopt
Mass spectrograph measurement standard vacuum leak ion stream and it is compared by school vacuum leak probe gas ion stream, it is to avoid vacuum leakage
Hole calibration and the uncertainty of measurement for being introduced using two kinds of different conditions, it is achieved that vacuum leak leak rate at actually used temperature
Accurate calibration.
Description of the drawings
Fig. 1 is a kind of structural representation of high/low temperature vacuum leak calibration device in embodiment.
In figure：1- standard vacuum small opening, the first valve of 2-, 3- mass spectrograph, 4- calibration chamber, 5- vacuometer, 6-
Two valves, 7- is by school vacuum leak, 8- high and low temperature room, the 3rd valve of 9-, and 10- is evacuated unit, 11- temperature control plate, 12-
Temperature control system.
Specific embodiment
Embodiment 1
As shown in figure 1, for a kind of high/low temperature vacuum leak calibration device in the present embodiment, the main composition of described device
Part includes standard vacuum small opening 1, the first valve 2, mass spectrograph 3, calibration chamber 4, vacuometer 5, the second valve 6, high and low temperature room
8th, the 3rd valve 9, pumping unit 10, temperature control plate 11 and temperature control system 12.
Wherein, standard vacuum small opening 1 is connected with calibration chamber 4 by the first valve 2, for for offer standard in calibration chamber 4
Gas flow；Pumping unit 10 is connected with calibration chamber 4 by the 3rd valve 9, for gas bleeding, realizes vacuum；By school vacuum
Small opening 7 is connected with calibration chamber 4 by the second valve 6, is placed in high and low temperature room 8；Mass spectrograph 3 is connected with calibration chamber 4, for surveying
Amount ion stream；Vacuometer 5 is connected with calibration chamber 4, for monitoring vacuum；Temperature control plate 11 is placed in high and low temperature room 8, with height
Temperature control system 12 outside temperature chamber 8 connects, and realizes to calibration chamber 4 and the temperature control by school vacuum leak 7.
Wherein, the first valve 2, the second valve 6 and the 3rd valve 9 are all-metal ultrahigh vacuum valve；Mass spectrograph 3 is level Four
Mass spectrograph；Standard vacuum small opening 1 and helium source of the gas is carried respectively by school vacuum leak 7；Pumping unit 10 is mechanical pump and molecule
Pump.
A kind of high/low temperature vacuum leak calibration method, methods described is using a kind of high/low temperature vacuum described in the present embodiment
Leak hole calibration device is carried out, in described device all building blocks using being front in closed mode, standard vacuum small opening 1
Leak rate is 1.54 × 10-8Pa·m3/ s, methods described step is as follows：
(1) the 3rd valve 9 is opened, starts the mechanical pump in pumping unit 10, from gas bleeding calibration chamber 4, until true
The pressure that empty meter 5 is measured in calibration chamber 4 reaches 1 × 10-2Pa, starts the molecular pump in pumping unit 10, and in following steps
In continue evacuation, to reach required vacuum, until all steps complete；
(2) bakeout degassing is integrally carried out to described device, baking temperature is risen to after 220 DEG C with the uniform velocity speed, keeps temperature
Degree 60h, then gradually decreases down room temperature with the uniform velocity speed again；The at the uniform velocity speed of raising and lowering is consistent, is 20 DEG C/h；
(3) with vacuometer 5, vacuum measurement is carried out to calibration chamber 4, when the pressure in calibration chamber 4 is less than 1.0 × 10-8Pa
When, open mass spectrograph 3 and adjust its parameter and be at stable working condition；
(4) start-up temperature control system 12 and temperature control plate 11, the school needed for making hygral equilibrium in high and low temperature room 8 and reaching
Quasi- temperature, is -10 DEG C, is represented with t, keeps the temperature fluctuation in high and low temperature room 8 to be less than or equal to 3 DEG C/min；
(5) the corresponding ion stream of described device background is obtained for 3.35 × 10 with the measurement of mass spectrograph 3-15A, uses I0Represent；
(6) open the second valve 6 gas for being flowed out by school vacuum leak 7 is introduced in calibration chamber 4；
(7) after in room to be calibrated 4, gas reaches dynamic equilibrium, when obtaining being opened by school vacuum leak 7 with the measurement of mass spectrograph 3
Ion stream be 1.08 × 10-11A, uses ILRepresent；
(8) open the first valve 2 gas that standard vacuum small opening 1 flows out is introduced in calibration chamber 4, flow into calibration chamber 4
Calibrating gas flow is the leak rate of standard vacuum small opening 1, uses QSRepresent；
(9) after in room to be calibrated 4, gas reaches dynamic equilibrium, when obtaining the unlatching of standard vacuum small opening 1 with the measurement of mass spectrograph 3
Ion stream be 3.18 × 10-11A, uses ISRepresent；
(10) leak rate by school vacuum leak 7 at a temperature of calibration, uses QL, (t)Represent, calculated by formula as follows (1)
Obtain：
In formula：
QL, (t)By leak rate of the school vacuum leak 7 at a temperature of calibration, unit is：Pa·m3/s；
QSThe calibrating gas flow of calibration chamber 4 is flowed into, unit is：Pa·m3/s；
I0The corresponding ion stream of described device background, unit is：A；
ILBy school vacuum leak 7 unlatching when ion stream, unit is：A；
ISIon stream when standard vacuum small opening 1 is opened, unit is：A；
It is 7.92 × 10 to be calculated the leak rate by school vacuum leak 7 at -10 DEG C of temperature of calibration-9Pa·m3/s；
(11) the first valve 2 is closed, temperature in high and low temperature room 8 is made by regulating and controlling temperature control system 12 and temperature control plate 11
Balance and reach new 40 DEG C of calibration temperature after changing, keep the temperature fluctuation in high and low temperature room 8 to be less than or equal to 3 DEG C/min；
(12) the corresponding ion stream of described device background is obtained for 8.71 × 10 with the measurement of mass spectrograph 3-15A, uses I0Represent；
(13), after in room to be calibrated 4, gas reaches dynamic equilibrium, obtain being opened by school vacuum leak 7 with the measurement of mass spectrograph 3
When ion stream be 8.23 × 10-11A, uses ILRepresent；
(14) open the first valve 2 gas that standard vacuum small opening 1 flows out is introduced in calibration chamber 4；
(15), after gas reaches dynamic equilibrium in room to be calibrated 4, standard vacuum small opening 1 is obtained with the measurement of mass spectrograph 3 and open
When ion stream be 1.68 × 10-10A, uses ISRepresent；
(16) data are substituted into formula (1) and is calculated the leak rate by school vacuum leak 7 at 40 DEG C new of calibration temperature
For 1.48 × 10-8Pa·m3/ s, uses QL, (t)Represent.
Claims (5)
1. a kind of high/low temperature vacuum leak calibration device, it is characterised in that：The main building block of described device includes that standard is true
Empty small opening (1), the first valve (2), mass spectrograph (3), calibration chamber (4), vacuometer (5), the second valve (6), high and low temperature room
(8), the 3rd valve (9), pumping unit (10), temperature control plate (11) and temperature control system (12)；
Standard vacuum small opening (1) is connected with calibration chamber (4) by the first valve (2)；Pumping unit (10) passes through the 3rd valve (9)
It is connected with calibration chamber (4)；It is connected with calibration chamber (4) by the second valve (6) by school vacuum leak (7), is placed in high and low temperature room
(8) in；Mass spectrograph (3) is connected with calibration chamber (4)；Vacuometer (5) is connected with calibration chamber (4)；Temperature control plate (11) is placed in high/low temperature
In degree room (8), it is connected with high and low temperature room (8) temperature control system (12) outward；
First valve (2), the second valve (6) and the 3rd valve (9) are all-metal ultrahigh vacuum valve；
Standard vacuum small opening (1) and it is connected acquisition source of the gas by school vacuum leak (7) having air source or with source of the gas.
2. a kind of high/low temperature vacuum leak calibration device according to claim 1, it is characterised in that：Being evacuated unit (10) is
Mechanical pump, molecular pump, bimolecular pump or mechanical pump are combined with molecular pump.
3. a kind of high/low temperature vacuum leak calibration device according to claim 2, it is characterised in that：Mass spectrograph (3) is four
Level mass spectrograph.
4. a kind of high/low temperature vacuum leak calibration method, it is characterised in that：Methods described is using as any one of claims 1 to 3
A kind of described high/low temperature vacuum leak calibration device is completed, in described device all building blocks using be front in close
State, known to the leak rate of standard vacuum small opening (1)；Methods described step is as follows：
(1) the 3rd valve (9) is opened, starts pumping unit (10), from gas bleeding calibration chamber (4), and in following steps
In continue gas bleeding, to reach required vacuum, until all steps complete；
(2) bakeout degassing is integrally carried out to described device, baking temperature is risen to after 200 DEG C～250 DEG C with the uniform velocity speed, keeps
60h～80h, then gradually decreases down room temperature with the uniform velocity speed again, and the at the uniform velocity speed of raising and lowering is identical, is 20 DEG C/h～40
℃/h；
(3) with vacuometer (5), vacuum measurement is carried out to calibration chamber (4), when the pressure of calibration chamber (4) meets mass spectrograph (3)
When operating pressure is required, open mass spectrograph (3) and adjust its parameter and be at stable working condition；
(4) start-up temperature control system (12) and temperature control plate (11), needed for making the interior hygral equilibrium in high and low temperature room (8) and reaching
Calibration temperature, keeps the temperature fluctuation in high and low temperature room (8) to be less than or equal to 3 DEG C/min；
(5) with mass spectrograph (3) measurement, the corresponding ion stream of described device background is obtained；
(6) the second valve (6) is opened, and the gas that will be flowed out by school vacuum leak (7) is introduced in calibration chamber (4)；
(7), after interior gas to be calibrated to room (4) reaches dynamic equilibrium, obtained when school vacuum leak is opened with mass spectrograph (3) measurement
Ion stream；
(8) the first valve (2) is opened, the gas that standard vacuum small opening (1) is flowed out is introduced in calibration chamber (4), flows into calibration chamber
(4) calibrating gas flow is the leak rate of standard vacuum small opening (1)；
(9), after interior gas to be calibrated to room (4) reaches dynamic equilibrium, with mass spectrograph (3) measurement, standard vacuum small opening (1) unlatching is obtained
When ion stream；
(10) leak rate by school vacuum leak (7) at a temperature of calibration is calculated by equation below (1)：
In formula：
QL, (t)By leak rate of the school vacuum leak (7) at a temperature of calibration,
QSThe calibrating gas flow of calibration chamber (4) is flowed into,
I0The corresponding ion stream of described device background,
ILIon stream when being opened by school vacuum leak (7),
ISIon stream when standard vacuum small opening (1) is opened.
5. a kind of high/low temperature vacuum leak calibration method according to claim 4, it is characterised in that：At -50 DEG C～50 DEG C
At a temperature of new calibration after interior change, realized by following steps by the leak rate of school vacuum leak (7)：
The first valve (2) is closed, the interior temperature in high and low temperature room (8) is made by regulating and controlling temperature control system (12) and temperature control plate (11)
Balance and reach new calibration temperature, keep the temperature fluctuation in high and low temperature room (8) to be less than or equal to 3 DEG C/min；
Repeat step (5) and (7)～(10), obtain the leak rate at a temperature of new calibration by school vacuum leak (7).
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| CN201610796942.4A CN106441731A (en) | 2016-08-31 | 2016-08-31 | High-low-temperature vacuum leak hole calibration device and method |
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| CN201610796942.4A CN106441731A (en) | 2016-08-31 | 2016-08-31 | High-low-temperature vacuum leak hole calibration device and method |
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Cited By (6)
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| CN107843391A (en) * | 2017-09-19 | 2018-03-27 | 兰州空间技术物理研究所 | A kind of small leak rate Pressure Leak Calibration Apparatus and method |
| CN109115425A (en) * | 2018-09-26 | 2019-01-01 | 长春微控机械制造有限公司 | A kind of gas leakage marking apparatus |
| CN109323817A (en) * | 2018-09-13 | 2019-02-12 | 北京东方计量测试研究所 | A kind of lower limit is 10-16Pam3The ultra-sensitivity leakage detection apparatus and method of/s |
| CN112241132A (en) * | 2020-09-20 | 2021-01-19 | 杭州谱育科技发展有限公司 | Control device and method for scanning speed of quadrupole mass spectrometer |
| CN114323421A (en) * | 2021-12-08 | 2022-04-12 | 兰州空间技术物理研究所 | Device and method for protecting IE514 separation rule from humidity |
| CN114526863A (en) * | 2022-01-27 | 2022-05-24 | 中国科学院合肥物质科学研究院 | Ultralow temperature vacuum measurement calibration device and method based on GM refrigerator cooling |
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| CN104280198A (en) * | 2014-09-12 | 2015-01-14 | 兰州空间技术物理研究所 | Minimum leak rate calibrating method based on static ion flow rising rate comparison method |
| CN105092187A (en) * | 2015-07-13 | 2015-11-25 | 兰州空间技术物理研究所 | Measurement apparatus and method for minimum vacuum leak rate |
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| CN104280198A (en) * | 2014-09-12 | 2015-01-14 | 兰州空间技术物理研究所 | Minimum leak rate calibrating method based on static ion flow rising rate comparison method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107843391A (en) * | 2017-09-19 | 2018-03-27 | 兰州空间技术物理研究所 | A kind of small leak rate Pressure Leak Calibration Apparatus and method |
| CN109323817A (en) * | 2018-09-13 | 2019-02-12 | 北京东方计量测试研究所 | A kind of lower limit is 10-16Pam3The ultra-sensitivity leakage detection apparatus and method of/s |
| CN109115425A (en) * | 2018-09-26 | 2019-01-01 | 长春微控机械制造有限公司 | A kind of gas leakage marking apparatus |
| CN112241132A (en) * | 2020-09-20 | 2021-01-19 | 杭州谱育科技发展有限公司 | Control device and method for scanning speed of quadrupole mass spectrometer |
| CN114323421A (en) * | 2021-12-08 | 2022-04-12 | 兰州空间技术物理研究所 | Device and method for protecting IE514 separation rule from humidity |
| CN114323421B (en) * | 2021-12-08 | 2023-07-21 | 兰州空间技术物理研究所 | Device and method for protecting IE514 separating gauge from humidity |
| CN114526863A (en) * | 2022-01-27 | 2022-05-24 | 中国科学院合肥物质科学研究院 | Ultralow temperature vacuum measurement calibration device and method based on GM refrigerator cooling |
| CN114526863B (en) * | 2022-01-27 | 2022-10-14 | 中国科学院合肥物质科学研究院 | Ultralow temperature vacuum measurement calibration device and method based on GM refrigerator cooling |
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Application publication date: 20170222 |