CN102928172B - Gas micro calibration lower limit is extended to 10 by one -14pam 3the system and method of/s - Google Patents
Gas micro calibration lower limit is extended to 10 by one -14pam 3the system and method of/s Download PDFInfo
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- CN102928172B CN102928172B CN201210382529.5A CN201210382529A CN102928172B CN 102928172 B CN102928172 B CN 102928172B CN 201210382529 A CN201210382529 A CN 201210382529A CN 102928172 B CN102928172 B CN 102928172B
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- 238000000034 method Methods 0.000 title claims abstract description 24
- 239000007789 gas Substances 0.000 claims abstract description 83
- 238000004949 mass spectrometry Methods 0.000 claims abstract description 54
- 230000000087 stabilizing effect Effects 0.000 claims abstract description 31
- 239000000725 suspension Substances 0.000 claims abstract description 16
- 239000011261 inert gas Substances 0.000 claims abstract description 11
- 150000002500 ions Chemical class 0.000 claims description 38
- 239000000523 sample Substances 0.000 claims description 24
- 238000005259 measurement Methods 0.000 claims description 18
- 238000005070 sampling Methods 0.000 claims description 6
- 238000001514 detection method Methods 0.000 claims description 5
- 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
- 238000012360 testing method Methods 0.000 abstract description 3
- 238000009825 accumulation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009530 blood pressure measurement Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000013461 design 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
- 238000012544 monitoring process Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 230000033772 system development Effects 0.000 description 1
- 238000013022 venting Methods 0.000 description 1
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Abstract
The present invention relates to one and gas micro calibration lower limit is extended to 10
-14pam
3the system and method of/s, for calibration and the test of vacuum leak, leak locator and gas micro-flowmeter.This system comprises: mechanical pump, two solenoid valves, six vacuum valves, two molecular pumps, mass spectrometric analysis chamber, aperture, two getter pumps, pressure stabilizing chamber, three vacuum gauges, gas bomb, micrometering valve, quadrupole mass spectrometers; Getter pump is adopted to bleed to pressure stabilizing chamber, eliminate non-inert gas that pressure stabilizing chamber wall discharges to tonometric impact, magnetic suspension rotor gauge is adopted accurately to measure gaseous tension P in pressure stabilizing chamber, gas in pressure stabilizing chamber is introduced in mass spectrometric analysis chamber by known conductance aperture expand continuously, calibration adopts accumulative to realize, and solves 10
-11~ 10
-14pam
3the testing and calibration technology of minimum gas micro within the scope of/s.
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, 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, proposes eager demand to minimum gas flow.Document " TT&C system development " aerospace measurement technology " the 24th volume of Constant Pressure Flowmeter, the 6th phase in 2004,14th ~ 16 pages ", introduce the method proposing and adopt constant-voltage method measurement gas micrometeor, its measurement range is 3.9 × 10
-4~ 3.6 × 10
-8pa m
3/ s; Document " design of portable gas micro-flowmeter, " vacuum " the 47th volume, the 2nd phase in 2010,60th ~ 63 pages ", introduce the method proposing and adopt constant volume method and flow conductance method measurement gas micrometeor, its measurement range is 5 × 10
-2~ 5 × 10
-11pam
3/ s; Document " A PRECISION GAS FLOWMETER FOR VACUUM METROLOGY "
vACUUM44 (2): (1993) .135-141. proposes constant conductance method flowmeter can extend to 5 × 10 by gas flow lower limit
-12pam
3/ s, the reason that this flowmeter lower limit can not continue to extend mainly contains two, and one is that firm discharge method adopts magnetic suspension rotor gauge to measure aperture entrance pressure, because mass spectrometric analysis chamber and pipeline venting impact make the aperture entrance low pressure limit that can accurately measure be 10
-3pa; Even if two is obtain to be less than 10
-12pam
3/ s gas flow, what set up at mass spectrometric analysis chamber owing to adopting expand continuously method is the partial pressure of probe gas dynamic stability, and this partial pressure is beyond the Monitoring lower-cut of mass spectrograph.And the minimum detectable leak rate of current commercial leak locator reaches 10
-16pam
3/ s, for this is less than 10 to gas flow
-12pam
3the calibration of/s is a current still unsolved difficult problem.
Summary of the invention
The object of the invention is for being less than 10
-12pam
3the calibration requirements of/s gas micro, proposes one and gas micro-flow measurement lower limit is extended to 10
-14pa m
3the system and method of/s.
The object of the invention is to be achieved through the following technical solutions.
Gas micro calibration lower limit is extended to 10 by one
-14pam
3the system of/s, comprising:
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;
Within the system, the first mechanical pump is connected with the first solenoid valve, and first molecular pump one end is connected with the first solenoid valve, and the other end is connected with the first vacuum valve; Mass spectrometric analysis chamber is provided with the second vacuum gauge, quadrupole mass spectrometer, 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 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; Pressure stabilizing chamber has six interfaces, 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; Second molecular pump two ends are connected with the 3rd vacuum valve, the second solenoid valve respectively, and the other end and second of the second solenoid valve connects mechanical pump and is connected.
Preferably, calibration range is 10
-11~ 10
-14pa m
3/ s.
Preferably, described first vacuum gauge adopts magnetic suspension rotor gauge (SRG), and hole diameter is less than 2um, and before measuring, magnetic suspension rotor gauge (SRG) stablizes more than 3 hours.
Preferably, the described first pump, second of cooling down cools down pump to inert gas without pumping speed.
Preferably, the probe gas of described vacuum leak and gas bomb is inert gas.
Preferably, described quadrupole mass spectrometer works more than 3 hours before measuring.
The present invention also provides a kind of and gas micro calibration lower limit is extended to 10
-14pam
3the method of the system of/s, comprises step:
S1, vacuum leak will be calibrated 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 open the first solenoid valve, the first vacuum valve, the second vacuum valve, the 3rd vacuum valve, the second solenoid valve bleed 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 are less than 10Pa, open the first molecular pump, the second molecular pump vacuumizes, keep environment temperature to be 23 ± 3 DEG C around;
S3, open the first vacuum gauge when gaseous tension is less than 1Pa in pressure stabilizing chamber 10, when in mass spectrometric analysis chamber, vacuum tightness is less than 1 × 10
-3open quadrupole mass spectrometer during Pa, in pressure stabilizing chamber and mass spectrometric analysis chamber, vacuum tightness is less than 1 × 10
-4open true 5th vacuum valve, the 6th vacuum valve during Pa, be less than 5 × 10 in the indicated value of the 3rd vacuum gauge
-6pa, and in the first vacuum gauge work after 3 hours, the background of setting magnetic suspension rotor gauge;
S4, quadrupole mass spectrometer work more than 3 hours, and the indicated value of the second vacuum gauge was less than 1 × 10
-6during Pa, close after the first vacuum valve and measure the change of probe gas background ions stream I along with time t by quadrupole mass spectrometer, after Δ t after a while, according to the slope that ion current increased along with the time
S5, open the first vacuum valve mass spectrometric analysis chamber is bled, when probe gas ion current drops to initial background ions stream, slowly opening the 4th vacuum valve will be calibrated in vacuum leak probe gas introducing mass spectrometric analysis chamber, after quadrupole mass spectrometer detection ion current is stable, to close after the first vacuum valve and writing time, after Δ t after a while, the slope increased along with the time of small opening ion current
S6, open the first vacuum valve to bleed to mass spectrometric analysis chamber, close the second vacuum valve, 3rd vacuum valve, 4th vacuum valve, in pressure stabilizing chamber, the gas of certain pressure is introduced by fine tuning valve, when the ion current of probe gas in mass spectrometric analysis chamber be reduced to background ions stream and after the first vacuum gauge pressure stability time, opening the second vacuum valve introduces in mass spectrometric analysis chamber by gas by aperture, after probe gas ion current is stable, close the first vacuum valve simultaneously writing time, record the indicated value P of the first vacuum gauge, after 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, being then calibrated leak hole leak rate is
Be placed in constant temperature system by vacuum leak 18 in described step S1, in experimentation, its temperature variation is no more than 0.5 degree.
In described step S3, magnetic suspension rotor gauge measures 10
-1~ 10
-3during Pa pressure, the sampling time is set as 10 seconds, when measurement 10
-4during Pa pressure, the sampling time is set as 30 seconds.
Get in described step S6
the mean value measured for more than at least six times is as measurement result.
In described step S7, C is known, and its combined standard uncertainty is less than 2%.
Beneficial effect
The gas micro calibration system that the present invention sets up has following characteristics compared with above technology: one is adopt getter pump to bleed to pressure stabilizing chamber and vacuum chamber mass spectrometric analysis chamber, the feature of bleeding of getter pump is without pumping speed to inert gas, being calibrated object generally adopts helium as probe gas, accurate for aperture entrance pressure measurement lower limit, on the impact of measurement result, can be extended to 10 by the non-inert gas avoiding aperture entrance pressure stabilizing chamber and pipeline material releasing after therefore adopting this pump
-4pa; Simultaneously after closedown first vacuum valve, the second getter pump is bled to the non-inert gas in mass spectrometric analysis chamber, not only makes the high vacuum state that mass spectrometric analysis chamber keeps good, and avoids the impact of non-inert gas on probe gas measurement result; Two is adopt the method for accumulation to improve quadrupole mass spectrometer measurement to be less than 10
-12pam
3the sensitivity of/s gas; Three be adopt diameter be less than 2um aperture as leakage component, can 10 be obtained
-14pa m
3the calibrating gas flow of/s, and the combined standard uncertainty of system is less than 10%.
Magnetic suspension rotor gauge is adopted accurately to measure gaseous tension P in pressure stabilizing chamber, gas in pressure stabilizing chamber is introduced in mass spectrometric analysis chamber by known conductance aperture (conductance is C) expand continuously, calibration adopts accumulative to realize, and first measures probe gas background signal with quadrupole mass spectrometer
then the signal being calibrated minimum gas flow and causing is measured
finally measure the signal that known gas micrometeor causes
then measured minimum gas micro
solve 10
-11~ 10
-14pa m
3the testing and calibration technology of minimum gas micro within the scope of/s.
Accompanying drawing explanation
Fig. 1 is structural principle schematic diagram of the present invention;
Wherein, 1-first mechanical pump, 2-first solenoid valve, 3-first molecular pump, 4-first vacuum valve, 5-mass spectrometric analysis chamber, 6-aperture, 7-second vacuum valve, 8-first getter pump, 9-first vacuum gauge, 10-pressure stabilizing chamber, 11-the 3rd vacuum valve, 12-second molecular pump, 13-second solenoid valve, 14-second mechanical pump, 15-second vacuum gauge, 16-quadrupole mass spectrometer, 17-the 4th vacuum valve, 18-vacuum leak, 19-gas bomb, 20-micrometering valve, 21-the 5th vacuum valve, 22-the 3rd vacuum gauge, 23-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 for illustration of the present invention, but do not limit the scope of the invention.
As shown in Figure 1, gas micro calibration lower limit is extended to 10 by one
-14pam
3the system of/s, comprising: the first mechanical pump 1, second mechanical pump 14, first solenoid valve 2, second solenoid valve 13, first vacuum valve 4, second vacuum valve 7, the 3rd vacuum valve 11, the 4th vacuum valve 17, the 5th vacuum valve 21, the 6th vacuum valve 24, first molecular pump 3, second molecular pump 12, mass spectrometric analysis chamber 5, aperture 6, first getter pump 8, second getter pump 23, pressure stabilizing chamber 10, first vacuum gauge 9, second vacuum gauge 15, the 3rd vacuum gauge 22, gas bomb 19, micrometering valve 20, quadrupole mass spectrometer 16 and vacuum leak 18;
Within the system, the first mechanical pump 1 is connected with the first solenoid valve 2, and first molecular pump 3 one end is connected with the first solenoid valve 2, and the other end is connected with the first vacuum valve 4; Mass spectrometric analysis chamber 5 is provided with the second vacuum gauge 15, quadrupole mass spectrometer 16, 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 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; Pressure stabilizing chamber 10 has six interfaces, 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; Second molecular pump 12 two ends are connected with the 3rd vacuum valve 11, second solenoid valve 13 respectively, and the other end of the second solenoid valve 13 is connected with the second mechanical pump 14.
Calibration range is 10
-11~ 10
-14pam
3/ s, the first vacuum gauge 9 adopts magnetic suspension rotor gauge (SRG), and the diameter of aperture 6 is for being less than 2um, and before measuring, magnetic suspension rotor gauge (SRG) stablizes more than 3 hours; Described first getter pump 8, second getter pump 23 pairs of inert gases are without pumping speed; Source of the gas in gas bomb 19 is inert gas; Quadrupole mass spectrometer 16 works more than 3 hours before measuring.
Gas micro calibration lower limit is extended to 10 by one
-14pam
3the method of the system of/s, comprises step:
S1, vacuum leak 18 will be calibrated 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, second mechanical pump 14 and bleed, then open the first solenoid valve 2, first vacuum valve 4, second vacuum valve 7, the 3rd vacuum valve 11, second solenoid valve 13 pairs of mass spectrometric analysis chambers 5 and valve pipe to bleed, open the second vacuum gauge 15, the 3rd vacuum gauge 22, when the second vacuum gauge 15, the 3rd vacuum gauge 22 measured value are less than 10Pa, open the first molecular pump 3, second molecular pump 12 to vacuumize, keep environment temperature to be 23 ± 3 DEG C around;
S3, open the first vacuum gauge 9 when gaseous tension is less than 1Pa in pressure stabilizing chamber 10, when in mass spectrometric analysis chamber 5, vacuum tightness is less than 1 × 10
-3open quadrupole mass spectrometer 16 during Pa, in pressure stabilizing chamber 10 and mass spectrometric analysis chamber 5, vacuum tightness is less than 1 × 10
-4open true 5th vacuum valve 21, the 6th vacuum valve 24 during Pa, be less than 5 × 10 in the indicated value of the 3rd vacuum gauge 22
-6pa, and after the first vacuum gauge 9 works 3 hours, the background of setting magnetic suspension rotor gauge;
S4, to work more than 3 hours at quadrupole mass spectrometer 16, and the indicated value of the second vacuum gauge 15 is less than 1 × 10
-6during Pa, close after the first vacuum valve 4 and measure the change of probe gas background ions stream I along with time t by quadrupole mass spectrometer, after Δ t after a while, according to the slope that ion current increased along with the time
S5, open the first vacuum valve 4 pairs of mass spectrometric analysis chambers 5 and bleed, when probe gas ion current drops to initial background ions stream, slowly opening the 4th vacuum valve 17 will be calibrated in vacuum leak probe gas introducing mass spectrometric analysis chamber 5, when quadrupole mass spectrometer 16 detect ion current stable after, to close after the first vacuum valve 4 and writing time, after Δ t after a while, the slope increased along with the time of small opening ion current
S6, open the first vacuum valve 4 pairs of mass spectrometric analysis chambers 5 to bleed, close the second vacuum valve 7, 3rd vacuum valve 11, 4th vacuum valve 17, in pressure stabilizing chamber 10, the gas of certain pressure is introduced by fine tuning valve 20, when the ion current of probe gas in mass spectrometric analysis chamber 5 be reduced to background ions stream and after the first vacuum gauge 9 pressure stability time, opening the second vacuum valve 7 introduces in mass spectrometric analysis chamber 5 by gas by aperture 6, after probe gas ion current is stable, close the first vacuum valve 4 simultaneously writing time, record the indicated value P of the first vacuum gauge 9, after 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, being then calibrated leak hole leak rate is
Be placed in constant temperature system by vacuum leak 18 in step S1, in experimentation, its temperature variation is no more than 0.5 degree.
In step S3, magnetic suspension rotor gauge measures 10
-1~ 10
-3during Pa pressure, the sampling time is set as 10 seconds, when measurement 10
-4during Pa pressure, the sampling time is set as 30 seconds.
Get in step S5
the mean value measured for more than at least six times is as measurement result.
Get in step S6
the mean value measured for more than at least six times is as measurement result.
In step S7, C is known, and its combined standard uncertainty is less than 2%.
Embodiment 1
(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) machine first mechanical pump 1, second mechanical pump 14 is opened, then open the first electric valve valve 2, first vacuum valve 4, second vacuum valve 7, the 3rd vacuum valve 11, second solenoid valve 13 pairs of mass spectrometric analysis chambers 5 and valve pipe to bleed, open the second vacuum gauge 15, when the second vacuum gauge 15 measured value is less than 10pa (1.2Pa), open the first molecular pump 3 and the second molecular pump 12 vacuumizes, keep environment temperature to be 23 ± 3 DEG C (23 ± 0.5 DEG C);
(3) open the first vacuum gauge 9 when gaseous tension in pressure stabilizing chamber 10 is less than 1Pa (0.1Pa), in pressure stabilizing chamber 10, vacuum tightness is less than 1 × 10
-4pa (6.2 × 10
-5pa) the 5th vacuum valve 21 is opened time, when in mass spectrometric analysis chamber 5, vacuum tightness is less than 1 × 10
-3pa (8.5 × 10
-5pa) open quadrupole mass spectrometer 16 time, be less than 5 × 10 in the indicated value of the 3rd vacuum gauge 22
-6pa (1.2 × 10
-6pa), and after the first vacuum gauge 9 works 3 hours (3.4 hours), the background (1.1231 × 10 of magnetic suspension rotor gauge is set
-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), measured the change of probe gas background ions stream by quadrupole mass spectrometer, close the first vacuum valve 4 writing time simultaneously, after Δ t after a while (300 seconds), according to the slope of the growth of ion current
(1.1 × 10
-15a/min).
(5) open the first vacuum valve 4 pairs of mass spectrometric analysis chambers 5 to bleed, when probe gas ion current drops to background ions stream, slowly open the 4th vacuum valve 17, when quadrupole mass spectrometer 16 detect ion current stable after, close the first vacuum valve 4 simultaneously writing time, after Δ t after a while (300 seconds), according to the slope of the growth of ion current
(9.3 × 10
-13a/min).
(6) open the first vacuum valve 4 pairs of mass spectrometric analysis chambers 5 to bleed, close the second vacuum valve 7, the 3rd vacuum valve 11, the 4th vacuum valve 17, open the gas that micrometering valve 20 introduces certain pressure in pressure stabilizing chamber 10.When the ion current of probe gas in mass spectrometric analysis chamber 5 be reduced to background ions stream and after the first vacuum gauge 9 pressure stability time, opening the second vacuum valve 7 introduces in mass spectrometric analysis chamber 5 by gas by aperture 6, after probe gas ion current is stable, close the first vacuum valve 4 simultaneously writing time, record the indicated value P (2.3151 × 10 of the first vacuum gauge 9
-4pa), after 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, being then calibrated leak hole leak rate is
(C=9.2 × 10
-10m
3/ s, Q
l=4.2 × 10
-13pa m
3/ s).
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the prerequisite not departing from the technology of the present invention principle; can also make some improvement and replacement, these improve and replace and also should be considered as protection scope of the present invention.
Claims (8)
1. gas micro calibration lower limit is extended to 10 by one kind
-14pam
3the system of/s, this system comprises: the first mechanical pump (1), the first vacuum valve (4), the 3rd vacuum valve (11), the 4th vacuum valve (17), the first molecular pump (3), mass spectrometric analysis chamber (5), aperture (6), pressure stabilizing chamber (10), the first vacuum gauge (9), micrometering valve (20), quadrupole mass spectrometer (16) and vacuum leak (18); It is characterized in that, this system also comprises: the second mechanical pump (14), the first solenoid valve (2), the second solenoid valve (13), the second vacuum valve (7), the 5th vacuum valve (21), the 6th vacuum valve (24), the second molecular pump (12), the first getter pump (8), the second getter pump (23), the second vacuum gauge (15), the 3rd vacuum gauge (22), gas bomb (19);
Within the system, the first mechanical pump (1) is connected with the first solenoid valve (2), and the first molecular pump (3) one end is connected with the first solenoid valve (2), and the other end is connected with the first vacuum valve (4); Mass spectrometric analysis chamber (5) is provided with the second vacuum gauge (15), quadrupole mass spectrometer (16), 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 second vacuum valve (7) is connected with aperture (6), 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); Pressure stabilizing chamber (10) there are six interfaces, 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); 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) is connected with the second mechanical pump (14).
2. gas micro calibration lower limit is extended to 10 by one as claimed in claim 1
-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), and the diameter of aperture (6) is 2um, and before measuring, magnetic suspension rotor gauge (SRG) stablizes more than 3 hours; Described first getter pump (8), the second getter pump (23) to inert gas without pumping speed; Source of the gas in gas bomb (19) is inert gas; Quadrupole mass spectrometer (16) works more than 3 hours before measuring.
3. gas micro calibration lower limit is extended to 10 by one kind
-14pam
3the method of the system of/s, is characterized in that, comprises step:
S1, the vacuum leak be calibrated (18) to be connected with the 4th vacuum valve (17), and to check sealing, then close the 4th vacuum valve (17);
S2, open the first mechanical pump (1), second mechanical pump (14) is bled, then the first solenoid valve (2) is opened, first vacuum valve (4), second vacuum valve (7), 3rd vacuum valve (11), second solenoid valve (13) is bled to mass spectrometric analysis chamber (5) and valve pipe, open the second vacuum gauge (15), 3rd vacuum gauge (22), when the second vacuum gauge (15), when 3rd vacuum gauge (22) measured value is less than 10Pa, open the first molecular pump (3), second molecular pump (12) vacuumizes, environment temperature is kept to be 23 ± 3 DEG C around,
S3, open the first vacuum gauge (9) when gaseous tension is less than 1Pa in pressure stabilizing chamber 10, when in mass spectrometric analysis chamber (5), vacuum tightness is less than 1 × 10
-3open quadrupole mass spectrometer (16) during Pa, in pressure stabilizing chamber (10) and mass spectrometric analysis chamber (5), vacuum tightness is less than 1 × 10
-4open true 5th vacuum valve (21), the 6th vacuum valve (24) during Pa, be less than 5 × 10 in the indicated value of the 3rd vacuum gauge (22)
-6pa, and in the first vacuum gauge (9) work after 3 hours, the background of setting magnetic suspension rotor gauge;
S4, quadrupole mass spectrometer (16) work more than 3 hours, and the indicated value of the second vacuum gauge (15) was less than 1 × 10
-6during Pa, close after the first vacuum valve (4) and measure the change of probe gas background ions stream I along with time t by quadrupole mass spectrometer, after Δ t after a while, according to the slope that ion current increased along with the time
S5, open the first vacuum valve (4) mass spectrometric analysis chamber (5) is bled, when probe gas ion current drops to initial background ions stream, slowly opening the 4th vacuum valve (17) will be calibrated in vacuum leak probe gas introducing mass spectrometric analysis chamber (5), after quadrupole mass spectrometer (16) detection ion current is stable, close the first vacuum valve (4) afterwards and writing time, after Δ t after a while, the slope increased along with the time of small opening ion current
S6, open the first vacuum valve (4) to bleed to mass spectrometric analysis chamber (5), close the second vacuum valve (7), 3rd vacuum valve (11), 4th vacuum valve (17), in pressure stabilizing chamber (10), the gas of certain pressure is introduced by fine tuning valve (20), when the ion current of probe gas in mass spectrometric analysis chamber (5) be reduced to background ions stream and after the first vacuum gauge (9) pressure stability time, opening the second vacuum valve (7) introduces in mass spectrometric analysis chamber (5) by gas by aperture (6), after probe gas ion current is stable, close the first vacuum valve (4) simultaneously writing time, record the indicated value P of the first vacuum gauge (9), after 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, being then calibrated leak hole leak rate is
wherein C is conductance.
4. gas micro calibration lower limit is extended to 10 by one as claimed in claim 3
-14pam
3the method of the system of/s, is characterized in that, the vacuum leak (18) be calibrated in described step S1 is placed in constant temperature system, and in experimentation, its temperature variation is no more than 0.5 degree.
5. gas micro calibration lower limit is extended to 10 by one as claimed in claim 3
-14pam
3the method of the system of/s, is characterized in that, in described step S3, magnetic suspension rotor gauge measures 10
-1~ 10
-3during Pa pressure, the sampling time is set as 10 seconds, when measurement 10
-4during Pa pressure, the sampling time is set as 30 seconds.
6. gas micro calibration lower limit is extended to 10 by one as claimed in claim 3
-14pam
3the method of the system of/s, is characterized in that, gets in described step S5
the mean value measured for more than at least six times is as measurement result.
7. gas micro calibration lower limit is extended to 10 by one as claimed in claim 3
-14pam
3the method of the system of/s, is characterized in that, gets in described step S6
the mean value measured for more than at least six times is as measurement result.
8. gas micro calibration lower limit is extended to 10 by one as claimed in claim 3
-14pam
3the method of the system of/s, is characterized in that, in described step S7, C is known, and its combined standard uncertainty is less than 2%.
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| 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 |
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| 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 |
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| 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 |
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| 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 |
| 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 |
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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 |
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