CN102928172A - System and method capable of extending lower limit of gas micro-flow calibration to 10<-14> Pam<3>/s - Google Patents
System and method capable of extending lower limit of gas micro-flow calibration to 10<-14> Pam<3>/s Download PDFInfo
- Publication number
- CN102928172A CN102928172A CN2012103825295A CN201210382529A CN102928172A CN 102928172 A CN102928172 A CN 102928172A CN 2012103825295 A CN2012103825295 A CN 2012103825295A CN 201210382529 A CN201210382529 A CN 201210382529A CN 102928172 A CN102928172 A CN 102928172A
- Authority
- CN
- China
- Prior art keywords
- vacuum
- valve
- gas
- vacuum valve
- gauge
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 238000000034 method Methods 0.000 title claims abstract description 25
- 239000007789 gas Substances 0.000 claims abstract description 85
- 230000000087 stabilizing effect Effects 0.000 claims abstract description 31
- 238000005259 measurement Methods 0.000 claims abstract description 17
- 239000011261 inert gas Substances 0.000 claims abstract description 10
- 238000004949 mass spectrometry Methods 0.000 claims description 52
- 150000002500 ions Chemical class 0.000 claims description 40
- 239000000523 sample Substances 0.000 claims description 24
- 239000000725 suspension Substances 0.000 claims description 12
- 238000001514 detection method Methods 0.000 claims description 6
- 238000005070 sampling Methods 0.000 claims description 6
- 230000000740 bleeding effect Effects 0.000 claims description 4
- 238000005086 pumping Methods 0.000 claims description 4
- 238000007789 sealing Methods 0.000 claims description 4
- 238000005516 engineering process Methods 0.000 abstract description 6
- 238000009825 accumulation Methods 0.000 abstract description 2
- 238000012360 testing method Methods 0.000 abstract description 2
- 238000001819 mass spectrum Methods 0.000 abstract 2
- 238000009530 blood pressure measurement Methods 0.000 abstract 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 238000013022 venting Methods 0.000 description 1
Images
Landscapes
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention relates to a system and a method capable of extending the lower limit of gas micro-flow calibration to 10<-14> Pam<3>/s, which are used for the calibration and the test on vacuum holes, a leak detector and a gas micro-flowmeter. The system comprises a mechanical pump, two solenoid valves, six vacuum valves, two molecular pumps, a mass spectrum analysis chamber, a small hole, two degasifier pumps, a pressure stabilizing chamber, three vacuum gauges, a gas bomb, a micrometering valve and a quadrupole mass spectrometer, wherein the degasifier pumps are adopted to pump the pressure stabilizing chamber so as to eliminate the influence on the pressure measurement caused by non-inert gas released by the wall of the pressure stabilizing chamber, a magnetic floating rotor gauge is adopted to accurately measure the gas pressure P in the pressure stabilizing chamber, the gas in the pressure stabilizing chamber is input into the mass spectrum analysis chamber through the continuous expansion of the existing flow guiding hole, the calibration is realized by adopting an accumulation method, and the measurement and calibration technologies of the micro-flow of minimum gas within the scope being 10<-11>-10<-14> Pam<3>/s can be realized.
Description
Technical field
The invention belongs to field of measuring technique, be specifically related to a kind of minimum gas flow calibration system and method, be used for calibration and the measurement of vacuum leak, leak locator and gas micro-flowmeter.
Background technology
Leak Detection is the gordian technique in the applications such as aerospace engineering, semi-conductor industry, solar industry, especially in aerospace engineering minimum gas flow has been proposed eager demand.Document " TT﹠C system of Constant Pressure Flowmeter development " aerospace instrumentation technology " the 24th volume, the 6th phase in 2004, the 14th～16 page " is introduced the method that has proposed to adopt constant-voltage method measurement gas micrometeor, and its measurement range is 3.9 * 10
-4～3.6 * 10
-8Pam
3/ s; Document " design of portable gas micro-flowmeter, " vacuum " the 47th volume, the 2nd phase in 2010, the 60th～63 page " is introduced the method that has proposed to adopt constant volume method and flow conductance method measurement gas micrometeor, and its measurement range is 5 * 10
-2～5 * 10
-11Pam
3/ s; Document ＂ APRECISION GAS FLOWMETER FOR VACUUM METROLOGY ＂
VACUUM44 (2): (1993) .135-141. has proposed the constant conductance method flowmeter can extend to 5 * 10 with the gas flow lower limit
-12Pam
3/ s, the reason that this flowmeter lower limit can not continue to extend mainly contains two, and the one, the firm discharge method adopts magnetic suspension rotor gauge to measure the aperture inlet pressure, is limited to 10 because mass spectrometric analysis chamber and pipeline venting impact make under the aperture inlet pressure that can accurately measure
-3Pa; The 2nd, even obtained less than 10
-12Pam
3/ s gas flow, because what adopt that the expand continuously method sets up at mass spectrometric analysis chamber is the partial pressure of probe gas dynamic stability, this partial pressure has exceeded the detection lower limit of mass spectrograph.And the minimum detectable leak rate of present commercial leak locator reaches 10
-16Pam
3/ s, for this to gas flow less than 10
-12Pam
3The calibration of/s is a present unsolved difficult problem still.
Summary of the invention
The objective of the invention is for less than 10
-12Pam
3The calibration requirements of/s gas micro has proposed a kind of the gas micro-flow measurement lower limit to be extended to 10
-14Pam
3The system and method of/s.
The objective of the invention is to be achieved through the following technical solutions
A kind of the gas micro calibration lower limit is extended to 10
-14Pam
3The system of/s comprises:
The first mechanical pump, the second mechanical pump, the first solenoid valve, the second solenoid valve, the first vacuum valve, the second vacuum valve, the 3rd vacuum valve, the 4th vacuum valve, the 5th vacuum valve, the 6th vacuum valve, the first molecular pump, the second molecular pump, mass spectrometric analysis chamber, aperture, the first getter pump, the second getter pump, pressure stabilizing chamber, the first vacuum gauge, the second vacuum gauge, the 3rd vacuum gauge, gas bomb, micrometering valve, quadrupole mass spectrometer and vacuum are blank;
In this system, the first mechanical pump is connected with the first solenoid valve, and the first molecular pump one end is connected with the first solenoid valve, and the other end is connected with the first vacuum valve; The second vacuum gauge, quadrupole mass spectrometer are installed on the mass spectrometric analysis chamber, the second getter pump is connected with mass spectrometric analysis chamber by the 6th vacuum valve, the lower end bleeding point of mass spectrometric analysis chamber is connected with the first vacuum valve, and the upper end of mass spectrometric analysis chamber is connected with aperture, the 4th vacuum valve respectively; The other end of the 4th vacuum valve is connected with vacuum leak; One end of the second vacuum valve is connected with aperture, and the other end is connected with micrometering valve, pressure stabilizing chamber and the 3rd vacuum gauge, and gas bomb is connected with micrometering valve; Six interfaces are arranged on the pressure stabilizing chamber, be connected with the first vacuum gauge, micrometering valve, the 5th vacuum valve, the 3rd vacuum gauge, the 3rd vacuum valve and the second vacuum valve respectively, the first getter pump is connected with the 5th vacuum valve; The second molecular pump two ends are connected with the 3rd vacuum valve, the second solenoid valve respectively, and the other end of the second solenoid valve and second connects mechanical pump and is connected.
Preferably, calibration range is 10
-11～10
-14Pam
3/ s.
Preferably, described the first vacuum gauge adopts magnetic suspension rotor gauge (SRG), and hole diameter is less than 2u, and SRG stablized more than 3 hours before measuring.
Preferably, described first cool down pump, second cool down pump to inert gas without pumping speed.
Preferably, the probe gas of described vacuum leak and gas bomb is inert gas.
Preferably, work was more than 3 hours before described quadrupole mass spectrometer was measured.
The present invention also provides a kind of the gas micro calibration lower limit is extended to 10
-14Pam
3The method of the system of/s comprises step:
S1, will be calibrated vacuum leak and be connected with the 4th vacuum valve, and check sealing, then close the 4th vacuum valve;
S2, open the first mechanical pump, the second mechanical pump is bled, then opening the first solenoid valve, the first vacuum valve, the second vacuum valve, the 3rd vacuum valve, the second solenoid valve bleeds to mass spectrometric analysis chamber and valve pipe, open the second vacuum gauge, the 3rd vacuum gauge, when the second vacuum gauge, the 3rd vacuum gauge measured value during less than 10Pa, open the first molecular pump, the second molecular pump vacuumizes, keeping environment temperature on every side is 23 ± 3 ℃;
S3, open the first vacuum gauge when gaseous tension is less than 1Pa in the pressure stabilizing chamber 10, vacuum tightness is less than 1 * 10 in mass spectrometric analysis chamber
-3Open quadrupole mass spectrometer during Pa, vacuum tightness is less than 1 * 10 in pressure stabilizing chamber and mass spectrometric analysis chamber
-4Open true the 5th vacuum valve, the 6th vacuum valve during Pa, in the indicated value of the 3rd vacuum gauge less than 5 * 10
-6Pa, and in the first vacuum gauge work after 3 hours, set the background of magnetic suspension rotor gauge;
S4, in quadrupole mass spectrometer work more than 3 hours, and the indicated value of the second vacuum gauge is less than 1 * 10
-6During Pa, close behind the first vacuum valve and measure probe gas background ions stream I along with the variation of time t by quadrupole mass spectrometer, behind Δ t after a while, the slope that increases along with the time according to ion current
S5, open the first vacuum valve mass spectrometric analysis chamber is bled, when the probe gas ion current drops to initial background ions stream, slowly opening the 4th vacuum valve will be calibrated in the vacuum leak probe gas introducing mass spectrometric analysis chamber, after quadrupole mass spectrometer detection ion current is stable, close behind the first vacuum valve and writing time, behind Δ t after a while, the slope that increases along with the time of small opening ion current
S6, opening the first vacuum valve bleeds to mass spectrometric analysis chamber, close the second vacuum valve, the 3rd vacuum valve, the 4th vacuum valve, introduce the gas of certain pressure in the pressure stabilizing chamber by fine tuning valve, in the time of after the ion current of probe gas in mass spectrometric analysis chamber is reduced to background ions stream and the first vacuum gauge pressure stability, opening the second vacuum valve introduces gas in the mass spectrometric analysis chamber by aperture, after the probe gas ion current is stable, close writing time the first vacuum valve while, record the indicated value P of the first vacuum gauge, behind Δ t after a while, according to the slope of the growth of ion current
S7, close all vacuum valves, close quadrupole mass spectrometer, vacuum gauge, molecular pump, mechanical pump all working instrument, then be calibrated leak hole leak rate and be
The small opening 18 that is calibrated in described step S1 is placed in the constant temperature system, and its temperature variation is no more than 0.5 degree in the experimentation.
Magnetic suspension rotor gauge measures 10 in described step S3
-1～10
-3During Pa pressure, the sampling time is set as 10 seconds, when measuring 10
-4During Pa pressure, the sampling time is set as 30 seconds.
In described step S6, get
The mean value of measuring more than at least six times is as measurement result.
In described step S6, get
The mean value of measuring more than at least six times is as measurement result.
C is known in described step S7, and its combined standard uncertainty is less than 2%.
Beneficial effect
The gas micro calibration system that the present invention sets up is compared with above technology has following characteristics: the one, and adopt getter pump that pressure stabilizing chamber and vacuum chamber mass spectrometric analysis chamber are bled, the characteristics of bleeding of getter pump are without pumping speed to inert gas, being calibrated object generally adopts helium as probe gas, therefore adopt and avoided behind this pump non-indifferent gas that aperture entrance pressure stabilizing chamber and pipeline material emit on the impact of measurement result, the accurate measurement lower limit of aperture inlet pressure can be extended to 10
-4Pa; After closing the first vacuum valve, the second getter pump is bled to the non-inert gas in the mass spectrometric analysis chamber simultaneously, not only makes mass spectrometric analysis chamber keep good high vacuum state, and has avoided non-inert gas on the impact of probe gas measurement result; The 2nd, adopt the method for accumulation to improve the quadrupole mass spectrometer measurement less than 10
-12Pam
3The sensitivity of/s gas; The 3rd, adopt the aperture of diameter 2u as leakage component, can obtain 10
-14Pam
3The calibrating gas flow of/s, and the combined standard uncertainty of system is less than 10%.
Adopt magnetic suspension rotor gauge accurately to measure gaseous tension P in the pressure stabilizing chamber, gas in the pressure stabilizing chamber is introduced in the mass spectrometric analysis chamber by known conductance aperture (conductance is C) expand continuously, calibration adopts accumulative to realize, at first measures the probe gas background signal with quadrupole mass spectrometer
Then measure and be calibrated the signal that minimum gas flow causes
Measure at last the signal that the known gas micrometeor causes
Measured minimum gas micro then
Solved 10
-11～10
-14Pam
3The testing and calibration technology of minimum gas micro in the/s scope.
Description of drawings
Fig. 1 is structural principle synoptic diagram of the present invention;
Wherein, 1-the first mechanical pump, 2-the first solenoid valve, 3-the first molecular pump, 4-the first vacuum valve, the 5-mass spectrometric analysis chamber, the 6-aperture, 7-the second vacuum valve, 8-the first getter pump, 9-the first vacuum gauge, the 10-pressure stabilizing chamber, 11-the 3rd vacuum valve, 12-the second molecular pump, 13-the second solenoid valve, 14-the second mechanical pump, 15-the second vacuum gauge, the 16-quadrupole mass spectrometer, 17-the 4th vacuum valve, the 18-vacuum leak, the 19-gas bomb, the 20-micrometering valve, 21-the 5th vacuum valve, 22-the 3rd vacuum gauge, 23-the second getter pump, 24-the 6th vacuum valve.
Embodiment
Below in conjunction with drawings and Examples, the specific embodiment of the present invention is described in further detail.Following examples are used for explanation the present invention, but do not limit the scope of the invention.
As shown in Figure 1, a kind of the gas micro calibration lower limit is extended to 10
-14Pam
3The system of/s comprises: the first mechanical pump 1, the second mechanical pump 14, the first solenoid valve 2, the second solenoid valve 13, the first vacuum valve 4, the second vacuum valve 7, the 3rd vacuum valve 11, the 4th vacuum valve 17, the 5th vacuum valve 21, the 6th vacuum valve 24, the first molecular pump 3, the second molecular pump 12, mass spectrometric analysis chamber 5, aperture 6, the first getter pump 8, the second getter pump 23, pressure stabilizing chamber 10, the first vacuum gauge 9, the second vacuum gauge 15, the 3rd vacuum gauge 22, gas bomb 19, micrometering valve 20, quadrupole mass spectrometer 16 and vacuum blank 18;
In this system, the first mechanical pump 1 is connected with the first solenoid valve 2, and the first molecular pump 3 one ends are connected with the first solenoid valve 2, and the other end is connected with the first vacuum valve 4; The second vacuum gauge 15, quadrupole mass spectrometer 16 are installed on the mass spectrometric analysis chamber 5, the second getter pump 23 is connected with mass spectrometric analysis chamber 5 by the 6th vacuum valve 24, the lower end bleeding point of mass spectrometric analysis chamber 5 is connected with the first vacuum valve 4, and the upper end of mass spectrometric analysis chamber 5 is connected with aperture 6, the 4th vacuum valve 17 respectively; The other end of the 4th vacuum valve 17 is connected with vacuum leak 18; One end of the second vacuum valve 7 is connected with aperture 6, and the other end is connected with micrometering valve 20, pressure stabilizing chamber 10 and the 3rd vacuum gauge 22, and gas bomb 19 is connected with micrometering valve 20; Six interfaces are arranged on the pressure stabilizing chamber 10, be connected with the first vacuum gauge 9, micrometering valve 20, the 5th vacuum valve 21, the 3rd vacuum gauge 22, the 3rd vacuum valve 11 and the second vacuum valve 7 respectively, the first getter pump 8 is connected with the 5th vacuum valve 21; The second molecular pump 12 two ends are connected with the 3rd vacuum valve 11, the second solenoid valve 13 respectively, and the other end of the second solenoid valve 13 and second connects mechanical pump 14 and is connected.
Calibration range is 10
-11～10
-14Pam
3/ s, the first vacuum gauge 9 adopts magnetic suspension rotor gauge (SRG), the diameter 2u of aperture 6, and SRG stablized more than 3 hours before measuring; Described the first getter pump 8,23 pairs of inert gases of the second getter pump are without pumping speed; Source of the gas in the gas bomb 19 is inert gas; Work was more than 3 hours before quadrupole mass spectrometer 16 was measured.
A kind of the gas micro calibration lower limit is extended to 10
-14Pam
3The method of the system of/s comprises step:
S1, will be calibrated vacuum leak 18 and be connected with the 4th vacuum valve 17, and check sealing, then close the 4th vacuum valve 17;
S2, open the first mechanical pump 1, the second mechanical pump 14 is bled, then opening the first solenoid valve 2, the first vacuum valve 4, the second vacuum valve 7, the 3rd vacuum valve 11,13 pairs of mass spectrometric analysis chambers 5 of the second solenoid valve and valve pipe bleeds, open the second vacuum gauge 15, the 3rd vacuum gauge 22, when the second vacuum gauge 15, the 3rd vacuum gauge 22 measured values during less than 10Pa, open the first molecular pump 3, the second molecular pump 12 vacuumizes, keeping environment temperature on every side is 23 ± 3 ℃;
S3, open the first vacuum gauge 9 when gaseous tension is less than 1Pa in the pressure stabilizing chamber 10, vacuum tightness is less than 1 * 10 in mass spectrometric analysis chamber 5
-3Open quadrupole mass spectrometer 16 during Pa, vacuum tightness is less than 1 * 10 in pressure stabilizing chamber 10 and mass spectrometric analysis chamber 5
-4Open true the 5th vacuum valve 21, the 6th vacuum valve 24 during Pa, in the indicated value of the 3rd vacuum gauge 22 less than 5 * 10
-6Pa, and after the first vacuum gauge 9 was worked 3 hours, set the background of magnetic suspension rotor gauge;
S4, in quadrupole mass spectrometer 16 work more than 3 hours, and the indicated value of the second vacuum gauge 15 is less than 1 * 10
-6During Pa, measure probe gas background ions stream I along with the variation of time t by quadrupole mass spectrometer after closing the first vacuum valve 4, behind Δ t after a while, the slope that increases along with the time according to ion current
S5, open 4 pairs of mass spectrometric analysis chambers 5 of the first vacuum valve and bleed, when the probe gas ion current drops to initial background ions stream, slowly opening the 4th vacuum valve 17 will be calibrated in the vacuum leak probe gas introducing mass spectrometric analysis chamber 5, after quadrupole mass spectrometer 16 detection ion currents are stable, close behind the first vacuum valve 4 and writing time, behind Δ t after a while, the slope that increases along with the time of small opening ion current
S6, opening 4 pairs of mass spectrometric analysis chambers 5 of the first vacuum valve bleeds, close the second vacuum valve 7, the 3rd vacuum valve 11, the 4th vacuum valve 17, introduce the gas of certain pressure in the pressure stabilizing chamber 10 by fine tuning valve 20, in the time of after the ion current of probe gas in mass spectrometric analysis chamber 5 is reduced to background ions stream and the first vacuum gauge 9 pressure stabilitys, opening the second vacuum valve 7 introduces gas in the mass spectrometric analysis chamber 5 by aperture 6, after the probe gas ion current is stable, close the first vacuum valve 4 writing times simultaneously, record the indicated value P of the first vacuum gauge 9, behind Δ t after a while, according to the slope of the growth of ion current
S7, close all vacuum valves, close quadrupole mass spectrometer, vacuum gauge, molecular pump, mechanical pump all working instrument, then be calibrated leak hole leak rate and be
The small opening 18 that is calibrated among the step S1 is placed in the constant temperature system, and its temperature variation is no more than 0.5 degree in the experimentation.
Magnetic suspension rotor gauge measures 10 among the step S3
-1～10
-3During Pa pressure, the sampling time is set as 10 seconds, when measuring 10
-4During Pa pressure, the sampling time is set as 30 seconds.
Get among the step S5
The mean value of measuring more than at least six times is as measurement result.
Get among the step S6
The mean value of measuring more than at least six times is as measurement result.
C is known among the step S7, and its combined standard uncertainty is less than 2%.
(1) measured gas micro (vacuum leak) is connected with the 4th vacuum valve 17, and checks sealing, then close the 4th vacuum valve 17;
(2) open machine the first mechanical pump 1, the second mechanical pump 14, then opening the first electric valve valve 2, the first vacuum valve 4, the second vacuum valve 7, the 3rd vacuum valve 11,13 pairs of mass spectrometric analysis chambers 5 of the second solenoid valve and valve pipe bleeds, open the second vacuum gauge 15, when the second vacuum gauge 15 measured values during less than 10pa (1.2Pa), open the first molecular pump 3 and the second molecular pump 12 vacuumizes, keeping environment temperature is 23 ± 3 ℃ (23 ± 0.5 ℃);
(3) open the first vacuum gauge 9 when gaseous tension in the pressure stabilizing chamber 10 during less than 1Pa (0.1Pa), vacuum tightness is less than 1 * 10 in pressure stabilizing chamber 10
-4Pa (6.2 * 10
-5Pa) open the 5th vacuum valve 21 time, vacuum tightness is less than 1 * 10 in mass spectrometric analysis chamber 5
-3Pa (8.5 * 10
-5Pa) open quadrupole mass spectrometer 16 time, in the indicated value of the 3rd vacuum gauge 22 less than 5 * 10
-6Pa (1.2 * 10
-6Pa), and in 9 work of the first vacuum gauge after 3 hours (3.4 hours), set the background (1.1231 * 10 of magnetic suspension rotor gauge
-5Pa);
(4) in quadrupole mass spectrometer work more than 3 hours (3.8 hours), and the indicated value of the second vacuum gauge 15 is less than 1 * 10
-6During Pa (2.3 * 10
-7Pa), by the variation that quadrupole mass spectrometer is measured probe gas background ions stream, close the first vacuum valve 4 writing times simultaneously, behind Δ t after a while (300 seconds), according to the slope of the growth of ion current
(1.1 * 10
-15A/min).
(5) opening 4 pairs of mass spectrometric analysis chambers 5 of the first vacuum valve bleeds, when the probe gas ion current drops to background ions stream, slowly open the 4th vacuum valve 17, after quadrupole mass spectrometer 16 detection ion currents are stable, close the first vacuum valve 4 writing times simultaneously, behind Δ t after a while (300 seconds), according to the slope of the growth of ion current
(9.3 * 10
-13A/min).
(6) open 4 pairs of mass spectrometric analysis chambers 5 of the first vacuum valve and bleed, close the second vacuum valve 7, the 3rd vacuum valve 11, the 4th vacuum valve 17, open the gas that micrometering valve 20 is introduced certain pressure in the pressure stabilizing chamber 10.In the time of after the ion current of probe gas in mass spectrometric analysis chamber 5 is reduced to background ions stream and the first vacuum gauge 9 pressure stabilitys, opening the second vacuum valve 7 introduces gas in the mass spectrometric analysis chamber 5 by aperture 6, after the probe gas ion current is stable, close the first vacuum valve 4 writing times simultaneously, record the indicated value P (2.3151 * 10 of the first vacuum gauge 9
-4Pa), behind Δ t after a while (300 seconds), according to the slope of the growth of ion current
(4.7 * 10
-13A/min).
(7), close all vacuum valves, close quadrupole mass spectrometer, vacuum gauge, molecular pump, mechanical pump all working instrument, then be calibrated leak hole leak rate and be
(C=9.2 * 10
-10m
3/ s, Q
L=4.2 * 10
-13Pam
3/ s).
The above only is preferred implementation of the present invention; should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the technology of the present invention principle; can also make some improvement and replacement, these improvement and replacement also should be considered as protection scope of the present invention.
Claims (8)
1. one kind extends to 10 with the gas micro calibration lower limit
-14Pam
3The system of/s, it is characterized in that this system comprises: the first mechanical pump (1), the second mechanical pump (14), the first solenoid valve (2), the second solenoid valve (13), the first vacuum valve (4), the second vacuum valve (7), the 3rd vacuum valve (11), the 4th vacuum valve (17), the 5th vacuum valve (21), the 6th vacuum valve (24), the first molecular pump (3), the second molecular pump (12), mass spectrometric analysis chamber (5), aperture (6), the first getter pump (8), the second getter pump (23), pressure stabilizing chamber (10), the first vacuum gauge (9), the second vacuum gauge (15), the 3rd vacuum gauge (22), gas bomb (19), micrometering valve (20), quadrupole mass spectrometer (16) and vacuum blank (18);
In this system, the first mechanical pump (1) is connected with the first solenoid valve (2), and the first molecular pump (3) one ends are connected with the first solenoid valve (2), and the other end is connected with the first vacuum valve (4); The second vacuum gauge (15), quadrupole mass spectrometer (16) are installed on the mass spectrometric analysis chamber (5), the second getter pump (23) is connected with mass spectrometric analysis chamber (5) by the 6th vacuum valve (24), the lower end bleeding point of mass spectrometric analysis chamber (5) is connected with the first vacuum valve (4), and the upper end of mass spectrometric analysis chamber (5) is connected with aperture (6), the 4th vacuum valve (17) respectively; The other end of the 4th vacuum valve (17) is connected with vacuum leak (18); One end of the second vacuum valve (7) is connected with aperture (6), and the other end is connected with micrometering valve (20), pressure stabilizing chamber (10) and the 3rd vacuum gauge (22), and gas bomb (19) is connected with micrometering valve (20); Six interfaces are arranged on the pressure stabilizing chamber (10), be connected with the first vacuum gauge (9), micrometering valve (20), the 5th vacuum valve (21), the 3rd vacuum gauge (22), the 3rd vacuum valve (11) and the second vacuum valve (7) respectively, the first getter pump (8) is connected with the 5th vacuum valve (21); The second molecular pump (12) two ends are connected with the 3rd vacuum valve (11), the second solenoid valve (13) respectively, and the other end of the second solenoid valve (13) and second connects mechanical pump (14) and is connected.
2. as claimed in claim 1ly a kind of the gas micro calibration lower limit is extended to 10
-14Pam
3The system of/s is characterized in that, calibration range is 10
-11～10
-14Pam
3/ s, the first vacuum gauge (9) adopts magnetic suspension rotor gauge (SRG), the diameter 2u of aperture (6), and SRG stablized more than 3 hours before measuring; Described the first getter pump (8), the second getter pump (23) to inert gas without pumping speed; Source of the gas in the gas bomb (19) is inert gas; Work was more than 3 hours before quadrupole mass spectrometer (16) was measured.
3. one kind extends to 10 with the gas micro calibration lower limit
-14Pam
3The method of the system of/s is characterized in that, comprises step:
S1, will be calibrated vacuum leak (18) and be connected with the 4th vacuum valve (17), and check sealing, then close the 4th vacuum valve (17);
S2, open the first mechanical pump (1), the second mechanical pump (14) is bled, then open the first solenoid valve (2), the first vacuum valve (4), the second vacuum valve (7), the 3rd vacuum valve (11), the second solenoid valve (13) is bled to mass spectrometric analysis chamber (5) and valve pipe, open the second vacuum gauge (15), the 3rd vacuum gauge (22), when the second vacuum gauge (15), the 3rd vacuum gauge (22) measured value is during less than 10Pa, open the first molecular pump (3), the second molecular pump (12) vacuumizes, and keeping environment temperature on every side is 23 ± 3 ℃;
S3, open the first vacuum gauge (9) when gaseous tension is less than 1Pa in the pressure stabilizing chamber 10, vacuum tightness is less than 1 * 10 in mass spectrometric analysis chamber (5)
-3Open quadrupole mass spectrometer (16) during Pa, vacuum tightness is less than 1 * 10 in pressure stabilizing chamber (10) and mass spectrometric analysis chamber (5)
-4Open true the 5th vacuum valve (21), the 6th vacuum valve (24) during Pa, in the indicated value of the 3rd vacuum gauge (22) less than 5 * 10
-6Pa, and after the first vacuum gauge (9) was worked 3 hours, set the background of magnetic suspension rotor gauge;
S4, in quadrupole mass spectrometer (16) work more than 3 hours, and the indicated value of the second vacuum gauge (15) is less than 1 * 10
-6During Pa, close behind the first vacuum valve (4) and measure probe gas background ions stream I along with the variation of time t by quadrupole mass spectrometer, behind Δ t after a while, the slope that increases along with the time according to ion current
S5, open the first vacuum valve (4) mass spectrometric analysis chamber (5) is bled, when the probe gas ion current drops to initial background ions stream, slowly opening the 4th vacuum valve (17) will be calibrated in the vacuum leak probe gas introducing mass spectrometric analysis chamber (5), after quadrupole mass spectrometer (16) detection ion current is stable, close behind the first vacuum valve (4) and writing time, behind Δ t after a while, the slope that increases along with the time of small opening ion current
S6, opening the first vacuum valve (4) bleeds to mass spectrometric analysis chamber (5), close the second vacuum valve (7), the 3rd vacuum valve (11), the 4th vacuum valve (17), by the gas of fine tuning valve (20) to the middle introducing of pressure stabilizing chamber (10) certain pressure, in the time of after the ion current of probe gas in mass spectrometric analysis chamber (5) is reduced to background ions stream and the first vacuum gauge (9) pressure stability, opening the second vacuum valve (7) introduces gas in the mass spectrometric analysis chamber (5) by aperture (6), after the probe gas ion current is stable, close writing time the first vacuum valve (4) while, record the indicated value P of the first vacuum gauge (9), behind Δ t after a while, according to the slope of the growth of ion current
S7, close all vacuum valves, close quadrupole mass spectrometer, vacuum gauge, molecular pump, mechanical pump all working instrument, then be calibrated leak hole leak rate and be
Wherein C is conductance.
4. as claimed in claim 3ly a kind of the gas micro calibration lower limit is extended to 10
-14Pam
3The method of the system of/s is characterized in that, the small opening (18) that is calibrated in described step S1 is placed in the constant temperature system, and its temperature variation is no more than 0.5 degree in the experimentation.
5. as claimed in claim 3ly a kind of the gas micro calibration lower limit is extended to 10
-14Pam
3The method of the system of/s is characterized in that, magnetic suspension rotor gauge measures 10 in described step S3
-1～10
-3During Pa pressure, the sampling time is set as 10 seconds, when measuring 10
-4During Pa pressure, the sampling time is set as 30 seconds.
6. as claimed in claim 3ly a kind of the gas micro calibration lower limit is extended to 10
-14Pam
3The method of the system of/s is characterized in that, gets in described step S5
The mean value of measuring more than at least six times is as measurement result.
7. as claimed in claim 3ly a kind of the gas micro calibration lower limit is extended to 10
-14Pam
3The method of the system of/s is characterized in that, gets in described step S6
The mean value of measuring more than at least six times is as measurement result.
8. as claimed in claim 3ly a kind of the gas micro calibration lower limit is extended to 10
-14Pam
3The method of the system of/s is characterized in that, C is known in described step S7, and its combined standard uncertainty is less than 2%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210382529.5A CN102928172B (en) | 2012-10-11 | 2012-10-11 | Gas micro calibration lower limit is extended to 10 by one -14pam 3the system and method of/s |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210382529.5A CN102928172B (en) | 2012-10-11 | 2012-10-11 | Gas micro calibration lower limit is extended to 10 by one -14pam 3the system and method of/s |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102928172A true CN102928172A (en) | 2013-02-13 |
| CN102928172B CN102928172B (en) | 2015-09-30 |
Family
ID=47643026
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210382529.5A Expired - Fee Related CN102928172B (en) | 2012-10-11 | 2012-10-11 | Gas micro calibration lower limit is extended to 10 by one -14pam 3the system and method of/s |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102928172B (en) |
Cited By (12)
| 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 |
| 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 |
| CN105136389A (en) * | 2015-07-21 | 2015-12-09 | 兰州空间技术物理研究所 | 10-9Pa magnitude vacuum partial pressure calibration device and calibration coefficient acquisition method |
| CN107355681A (en) * | 2017-08-23 | 2017-11-17 | 兰州空间技术物理研究所 | A kind of feeder and air supply method for the calibration of multiple working medium gas micro |
| CN107677329A (en) * | 2017-09-08 | 2018-02-09 | 兰州空间技术物理研究所 | The vacuum leak flow measurement device and method of a kind of more gas componants |
| CN107991949A (en) * | 2018-01-11 | 2018-05-04 | 赵天舒 | A kind of intelligence the Aged Care apartment complexes |
| CN109443653A (en) * | 2018-11-28 | 2019-03-08 | 北京东方计量测试研究所 | A kind of gas sampling system and method for small leak rate PRESSURE LEAK CALIBRATION |
| CN109854494A (en) * | 2018-12-17 | 2019-06-07 | 兰州空间技术物理研究所 | A kind of device and method of constant conductance method flowmeter measurement minipump pumping speed |
| CN110376272A (en) * | 2019-06-12 | 2019-10-25 | 中国科学院微电子研究所 | The on-line measurement device and its On-line Measuring Method of partial pressure |
| CN110927240A (en) * | 2019-11-22 | 2020-03-27 | 南京理工大学 | High-purity NF of ultrahigh vacuum system3Air intake control device and method |
| CN113310626A (en) * | 2021-05-26 | 2021-08-27 | 北京东方计量测试研究所 | Vacuum gauge calibration device and calibration method |
| CN114674501A (en) * | 2021-12-25 | 2022-06-28 | 兰州空间技术物理研究所 | Static leak rate measuring device and method |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7559223B2 (en) * | 2003-08-21 | 2009-07-14 | Appleton Papers Inc. | Real time determination of gas solubility and related parameters in manufacturing processes |
| CN101713696A (en) * | 2009-12-17 | 2010-05-26 | 中国航天科技集团公司第五研究院第五一○研究所 | Device and method for calibrating flow-dividing vacuum leaking hole |
| CN102426079A (en) * | 2011-10-28 | 2012-04-25 | 清华大学 | Simulation system and method for leakage detection of space station by using direction gauge |
| CN102538916A (en) * | 2012-02-06 | 2012-07-04 | 江苏东方航天校准检测有限公司 | Portable gas micro-flow calibration system and method thereof |
| CN202853862U (en) * | 2012-10-11 | 2013-04-03 | 卢耀文 | System for extending lower limit of gas micro-flow calibration to 10<-14>Pam<3>/s |
-
2012
- 2012-10-11 CN CN201210382529.5A patent/CN102928172B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7559223B2 (en) * | 2003-08-21 | 2009-07-14 | Appleton Papers Inc. | Real time determination of gas solubility and related parameters in manufacturing processes |
| CN101713696A (en) * | 2009-12-17 | 2010-05-26 | 中国航天科技集团公司第五研究院第五一○研究所 | Device and method for calibrating flow-dividing vacuum leaking hole |
| CN102426079A (en) * | 2011-10-28 | 2012-04-25 | 清华大学 | Simulation system and method for leakage detection of space station by using direction gauge |
| CN102538916A (en) * | 2012-02-06 | 2012-07-04 | 江苏东方航天校准检测有限公司 | Portable gas micro-flow calibration system and method thereof |
| CN202853862U (en) * | 2012-10-11 | 2013-04-03 | 卢耀文 | System for extending lower limit of gas micro-flow calibration to 10<-14>Pam<3>/s |
Cited By (20)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103759906B (en) * | 2013-12-24 | 2016-09-28 | 兰州空间技术物理研究所 | Device and method based on static expanding method vacuum standard calibration vacuum leak |
| 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 |
| 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 |
| CN105136389B (en) * | 2015-07-21 | 2017-12-12 | 兰州空间技术物理研究所 | 10‑9The vacuum partial pressure calibrating installation and calibration factor acquisition methods of Pa magnitudes |
| CN105136389A (en) * | 2015-07-21 | 2015-12-09 | 兰州空间技术物理研究所 | 10-9Pa magnitude vacuum partial pressure calibration device and calibration coefficient acquisition method |
| CN107355681B (en) * | 2017-08-23 | 2019-09-10 | 兰州空间技术物理研究所 | A kind of feeder and air supply method for the calibration of multiple working medium gas micro |
| CN107355681A (en) * | 2017-08-23 | 2017-11-17 | 兰州空间技术物理研究所 | A kind of feeder and air supply method for the calibration of multiple working medium gas micro |
| CN107677329A (en) * | 2017-09-08 | 2018-02-09 | 兰州空间技术物理研究所 | The vacuum leak flow measurement device and method of a kind of more gas componants |
| CN107677329B (en) * | 2017-09-08 | 2019-09-27 | 兰州空间技术物理研究所 | A kind of the vacuum leak flow measurement device and method of more gas componants |
| CN107991949A (en) * | 2018-01-11 | 2018-05-04 | 赵天舒 | A kind of intelligence the Aged Care apartment complexes |
| CN107991949B (en) * | 2018-01-11 | 2020-10-16 | 盐城颐康智能科技有限公司 | Intelligent old people care apartment system |
| CN109443653B (en) * | 2018-11-28 | 2020-09-22 | 北京东方计量测试研究所 | Gas sampling system and method for micro leak rate positive pressure leak hole calibration |
| CN109443653A (en) * | 2018-11-28 | 2019-03-08 | 北京东方计量测试研究所 | A kind of gas sampling system and method for small leak rate PRESSURE LEAK CALIBRATION |
| CN109854494A (en) * | 2018-12-17 | 2019-06-07 | 兰州空间技术物理研究所 | A kind of device and method of constant conductance method flowmeter measurement minipump pumping speed |
| CN110376272A (en) * | 2019-06-12 | 2019-10-25 | 中国科学院微电子研究所 | The on-line measurement device and its On-line Measuring Method of partial pressure |
| CN110376272B (en) * | 2019-06-12 | 2022-02-08 | 中国科学院微电子研究所 | On-line measuring device and method for gas partial pressure |
| CN110927240A (en) * | 2019-11-22 | 2020-03-27 | 南京理工大学 | High-purity NF of ultrahigh vacuum system3Air intake control device and method |
| CN113310626A (en) * | 2021-05-26 | 2021-08-27 | 北京东方计量测试研究所 | Vacuum gauge calibration device and calibration method |
| CN113310626B (en) * | 2021-05-26 | 2022-08-19 | 北京东方计量测试研究所 | Vacuum gauge calibration device and calibration method |
| CN114674501A (en) * | 2021-12-25 | 2022-06-28 | 兰州空间技术物理研究所 | Static leak rate measuring device and method |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102928172B (en) | 2015-09-30 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102928172A (en) | System and method capable of extending lower limit of gas micro-flow calibration to 10<-14> Pam<3>/s | |
| CN106226000A (en) | A kind of vacuum leakproofness energy measurement apparatus and method | |
| CN111141506B (en) | Device and method for measuring gas pressure and components of cavity of extremely-small sealing device | |
| CN102967527B (en) | There is compound material venting rate test macro and the method for self-calibration function | |
| CN102494741B (en) | Static sampling introduction device and method of calibrating pressure leak hole | |
| CN105004479A (en) | Ionization vacuum gauge and mass spectrometer calibration device and method based on standard pressure measurement | |
| CN103759906B (en) | Device and method based on static expanding method vacuum standard calibration vacuum leak | |
| CN202853862U (en) | System for extending lower limit of gas micro-flow calibration to 10<-14>Pam<3>/s | |
| CN102538916A (en) | Portable gas micro-flow calibration system and method thereof | |
| CN104280198A (en) | Minimum leak rate calibrating method based on static ion flow rising rate comparison method | |
| CN104345087A (en) | Calibration device and calibration method for magnetic deflection mass spectrograph | |
| CN102944356B (en) | Extremely high vacuum gauge calibration device and method | |
| CN106679897A (en) | Leakage hole's leakage rate measuring apparatus | |
| CN105910953A (en) | Device and method for measuring elementary gas outgassing rate of material | |
| CN104006929A (en) | Mass spectrometry single point leak detection system and method based on voltage limiting-shunting method in atmospheric environment | |
| CN106289666B (en) | Calibration device and method for vacuum leak at ambient temperature | |
| EP2924411B1 (en) | Reference leak generating device and ultra-fine leak testing device using same | |
| CN106441702A (en) | Dual-hole spectrometer calibration device and method | |
| CN112781804B (en) | SF6 leak rate calibration stepless adjusting device and method | |
| CN105738037A (en) | Plasma reaction cavity seepage detection method | |
| CN207300820U (en) | It is a kind of to be used to measure under rated differential head film to the system of specific gas leak rate | |
| CN205826251U (en) | A kind of vacuum leakproofness energy measurement apparatus sealing container | |
| CN202885918U (en) | Portable gas micro flow calibrating device | |
| CN109323817A (en) | A kind of lower limit is 10-16Pam3The ultra-sensitivity leakage detection apparatus and method of/s | |
| CN107389498B (en) | Method for measuring methane transmittance |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C41 | Transfer of patent application or patent right or utility model | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20151029 Address after: 100085 No. 1, building 4, building ten, No. 5, 507 street, Beijing, Haidian District Patentee after: Beijing Yongda Hongyu Technology Development Co., Ltd. Address before: 100081 Beijing, Zhongguancun, South Street, No. 5, No. Patentee before: Lu Yaowen |
|
| DD01 | Delivery of document by public notice |
Addressee: Beijing Yongda Hongyu Technology Development Co., Ltd. Document name: Notification of Termination of Patent Right |
|
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20150930 Termination date: 20151011 |