CN105136389B - 10‑9The vacuum partial pressure calibrating installation and calibration factor acquisition methods of Pa magnitudes - Google Patents
10‑9The vacuum partial pressure calibrating installation and calibration factor acquisition methods of Pa magnitudes Download PDFInfo
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- CN105136389B CN105136389B CN201510428627.1A CN201510428627A CN105136389B CN 105136389 B CN105136389 B CN 105136389B CN 201510428627 A CN201510428627 A CN 201510428627A CN 105136389 B CN105136389 B CN 105136389B
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Abstract
The present invention provides one kind 10‑9The vacuum partial pressure calibrating installation of Pa magnitudes, it includes：Reset valve, source of the gas, with specimen chamber, eight valves, sampling room, secondary expansion room, compound vacuum gauge, separate vacuum meter, aperture, calibration chamber, piston manometer, Sample Room and by school mass spectrometers for partial pressure；Ancillary equipment is extract system.Present invention utilizes gas expansion method, by higher forepressure by being re-introduced into after gas expansion and aperture decay in calibration chamber, extends the calibration lower limit of mass spectrometers for partial pressure, solves 10‑9The calibration of the mass spectrometers for partial pressure of Pa magnitudes.In addition, by the use of high-precision piston manometer as forepressure normative reference, magnetic suspension spinning rotor vacuum gauge of the prior art is substituted for, reduces uncertainty of measurement, so as to improve calibration accuracy.
Description
Technical field
The invention belongs to vacuumatic measuring technical guarantee field, more particularly to one kind 10-9The vacuum partial pressure calibration of Pa magnitudes
Device and calibration factor acquisition methods.
Background technology
Mass spectrometers for partial pressure is widely used in industrial production every field, and its partial pressure measurement lower limit is mostly 10-9Pa.Point
The calibration of pressure mass spectrograph is an important research direction in vacuumatic measuring field.Document " Li get Tian, Li Zhenghai, Feng Yan, Zhang Di
Newly, Zhang Jianjun, Xu Hang, Gong Yueli, the development vacuum sciences and technology of Li Li Partial Pressure Mass Spectrometry Calibration Systems, 2001. " are situated between
Current China continued uniquely with Calibration System of Mass Spectrometers for Partial Pressure.
The calibrating installation realizes the calibration of mass spectrometers for partial pressure using two methods.One kind is：It is true using magnetic suspension rotor
The forepressure of sky meter measurement calibration indoor standard partial pressure, is directly compared with by school mass spectrometers for partial pressure, i.e., using straight
Connecing Comparison Method realizes mass spectrometers for partial pressure 10-4Pa~10-1Calibration in Pa pressure limits, as shown in Figure 1.Another kind is profit
With the pressure of magnetic suspension spinning rotor vacuum gauge measurement upstream chamber, calibration chamber will be introduced after the decline of pressure of upstream chamber by aperture, only
Know the decline of pressure ratio of aperture, the standard partial pressure of calibration chamber can be obtained, so as to realize mass spectrometers for partial pressure 10-6Pa
~10-4Calibration in Pa pressure limits, as shown in Figure 2.
The weak point of this system is limited by calibration method, and calibration range is confined to 10-6Pa~10-1Pa, it is empty at present
Between the measurement lower limit of mass spectrometers for partial pressure applied reached 10-9Pa magnitudes, the system can not realize 10-9Point of Pa magnitudes
The accurate alignment of pressure mass spectrograph；At present also it is not yet found that other systems or method can reach 10-9Pa magnitudes it is accurate
Calibration.In addition, the system uses magnetic suspension spinning rotor vacuum gauge, as normative reference, for measuring forepressure, uncertainty is big
In 1%, uncertainty is larger.
The content of the invention
To solve the above problems, the present invention provides one kind 10-9The vacuum partial pressure calibrating installation and calibration factor of Pa magnitudes
Acquisition methods, 10 can be realized-9The calibration of the mass spectrometers for partial pressure of Pa magnitudes.
The 10 of the present invention-9The vacuum partial pressure calibrating installation of Pa magnitudes, it includes：Reset valve, source of the gas, with specimen chamber, eight
Valve, sampling room, secondary expansion room, compound vacuum gauge, aperture, calibration chamber, piston manometer, Sample Room and by school partial pressure matter
Spectrum meter, separate vacuum meter；Ancillary equipment is extract system.
It is connected with source of the gas by reset valve with specimen chamber, is connected by the first valve with sampling room；Sampling room passes through the second valve
Door is connected with Sample Room, is connected by the 7th valve with piston manometer；Sample Room is connected by the 3rd valve and secondary expansion room
Connect, be connected by the 4th valve with compound vacuum gauge, and be connected after connecting aperture by the 5th valve with calibration chamber；Calibration chamber is led to
Cross the 8th valve to be connected with by school mass spectrometers for partial pressure, be connected by the 6th valve with separate vacuum meter；And vacuum partial pressure school
The pipeline of standard apparatus is connected with extract system.
Further, the reset valve is ultrahigh vacuum all-metal reset valve.
Further, the source of the gas is multiple pure gas sources of the gas or the mixed gas of main constituent.
Further, described with specimen chamber is stainless steel spherical structure, volume 10L.
Further, eight valves are ultrahigh vacuum all-metal ball valve.
Further, the sampling room, secondary expansion room, Sample Room are stainless steel spherical structure.
Further, the Sample Room and secondary expansion room volumetric ratio are 10.
Further, the decline of pressure ratio of the aperture is 1/1000.
Further, vacuumized with specimen chamber, Sample Room, calibration chamber by three sets of different extract systems.
The present invention also provides one kind 10-9The calibration factor acquisition methods of the vacuum partial pressure calibrating installation of Pa magnitudes, it is wrapped
Include following steps：
Step 1, the volumetric ratio of sampling room and Sample Room is measured
Step 2, extract the gas in vacuum partial pressure calibrating installation and its in pipeline, and close reset valve, the first valve,
Second valve, the 3rd valve, the 4th valve, the 5th valve, the 6th valve, the 7th valve and the 8th valve；
Step 3, reset valve and the first valve are opened, by the gas in source of the gas by being incorporated into specimen chamber in sampling room, is treated
The first valve is closed after pressure stability, then opens the 7th valve, the pressure that gas is filled with sampling room is measured by piston manometer
Power p；
Step 4, the second valve is opened, it is after pressure stabilisation to close second by gas expansion in sampling room into Sample Room
Valve, because of VSample introduction>>VSampling, then Sample Room gas pressure be
Step 5, the 3rd valve is opened, it is after pressure stabilisation by gas expansion into secondary expansion room, open the 4th valve
Door, reads the gas pressure of compound vacuum gauge, judges whether the gas pressure in Sample Room meets to calibrate according to the gas pressure
Demand, if not satisfied, continuing gas expansion to secondary expansion room, until meeting calibration requirements；If the gas pressure in Sample Room
Power meets calibration requirements, then closes the 3rd valve, and now Sample Room gas pressure is
Step 6, the 5th valve is opened, gas is incorporated into calibration chamber by aperture, it is after pressure stabilisation, open the 6th
Valve reads the gas pressure of separate vacuum meter, and judges whether the gas pressure in calibration chamber meets school according to the gas pressure
Quasi need, if not satisfied, continuing gas introducing calibration chamber by aperture, until meeting calibration requirements；If in calibration chamber
Gas pressure meets calibration requirements, then closes the 5th valve, and now the standard partial pressure of calibration chamber is
Step 8, the 8th valve is opened, it is after pressure stabilisation, read by the pressure reading of school mass spectrometers for partial pressure, close the
Eight valves；
Step 9, the standard partial pressure is compared with by the pressure reading of school mass spectrometers for partial pressure, obtained by school point
The calibration factor of pressure mass spectrograph.
Beneficial effect：
Present invention utilizes gas expansion method, by higher forepressure by being re-introduced into after gas expansion and aperture decay
Into calibration chamber, the calibration lower limit of mass spectrometers for partial pressure is extended, solves 10-9The calibration of the mass spectrometers for partial pressure of Pa magnitudes.
In addition, by the use of high-precision piston manometer as standard vacuum gauge, magnetic suspension spinning rotor vacuum gauge of the prior art is substituted for, is subtracted
Small uncertainty of measurement, so as to improve calibration accuracy.
Brief description of the drawings
Fig. 1 is direct comparison method schematic device of the prior art；
Fig. 2 is pressure-decay method schematic device of the prior art；
Fig. 3 is the 10 of the present invention-9The structure design principle schematic diagram of the vacuum partial pressure calibrating installation of Pa magnitudes.
In figure：
1- reset valves, 2- sources of the gas, 3- are with specimen chamber, the valves of 4- first, the valves of 6- second, the valves of 7- the 3rd, the valves of 10- the 4th
Door, the valves of 12- the 5th, the valves of 14- the 6th, the valves of 15- the 7th, the valves of 19- the 8th, 5- sampling rooms, 8- secondary expansions room, 9- are multiple
Vacuum meter, 11- apertures, 13- calibration chambers, 16- piston manometers, 17- Sample Rooms, 18- is closed by school mass spectrometers for partial pressure, 20- to be divided
From vacuum meter, 21- valves；22- magnetic suspension spinning rotor vacuum gauges, 23- upstream chambers.
Embodiment
As shown in figure 3, the 10 of the present invention-9The vacuum partial pressure calibrating installation and calibration factor acquisition methods of Pa magnitudes, its
Middle device includes：Reset valve 1, source of the gas 2, with 3, eight valves of specimen chamber, sampling room 5, secondary expansion room 8, compound vacuum gauge 9, small
Hole 11, calibration chamber 13, piston manometer 16, Sample Room 17, by school mass spectrometers for partial pressure 18, separate vacuum meter 20.
Wherein, eight valves are respectively the first valve 4, the second valve 6, the 3rd valve 7, the 4th valve 10, the 5th valve
12nd, the 6th valve 14, the 7th valve 15 and the 8th valve 19.
Reset valve 1 is ultrahigh vacuum all-metal reset valve, and leak rate is less than 10-9Pam3/ s magnitudes.
The mixed gas of main constituent for multiple single high-purity gas combinations or of source of the gas 2.
It is 316L stainless steel spherical structures with specimen chamber 3, volume 10L, the gas for source of the gas 2 to be provided is sufficiently mixed,
Calibration gas needed for being formed.
Sampling room 5, the calibration gas of pressure needed for acquisition from specimen chamber 3；Wherein calibration gas forepressure is by piston
Pressure gauge 16 measures.
Eight valves are ultrahigh vacuum all-metal ball valve.
The sampling room 5, secondary expansion room 8, Sample Room 17 are 316L stainless steel spherical structures；Sample Room and auxiliary are swollen
Swollen room volumetric ratio is 10；CV is much smaller than Sample Room volume, and volumetric ratio is according to by the calibration model of school mass spectrometers for partial pressure
Enclose selection.Above-mentioned 316L is a kind of stainless steel material trade mark.
Sample Room 17 completes the once expansion of calibration gas, gas pressure is once reduced.
The reexpansion of calibration gas is completed in secondary expansion room 8, makes the secondary reduction of gas pressure.
The attenuation ratio of aperture 11 is 1/1000, gas pressure is reduced three times.
Calibration chamber 13 obtains the standard partial pressure of calibration gas, with being carried out by the partial pressure shown in school mass spectrometers for partial pressure 18
Compare, obtain calibration factor.
Compound vacuum gauge 9 is used to monitor the gas pressure in Sample Room 17；Separate vacuum meter 20 is used to monitor calibration chamber 13
In gas pressure.
Source of the gas 2 is connected by reset valve 1 with specimen chamber 3；Sampling room 5 is connected by the first valve 4 with specimen chamber 3, is passed through
Second valve 6 is connected with Sample Room 17；Piston manometer 16 is connected by the 7th valve 15 with sampling room 5, is sampled for measuring
Gas pressure in room 5；Secondary expansion room 8 is connected by the 3rd valve 7 with Sample Room 17；Compound vacuum gauge 9 passes through the 4th valve
Door 10 is connected with Sample Room 17, for measuring the gas pressure in Sample Room 17；The valve 12 of aperture 11 and the 5th is connected to sample introduction
Between room 17 and calibration chamber 13；It is connected by school mass spectrometers for partial pressure 18 by the 8th valve 19 with calibration chamber 13；Separate vacuum meter
20 are connected by the 8th valve 19 with calibration chamber 13, for measuring the gas pressure in calibration chamber 13；With specimen chamber 3 and sampling room 5
Vacuumized by the first extract system, secondary expansion room 8 and Sample Room 17 are vacuumized by the second extract system, and calibration chamber 13 is logical
The 3rd extract system is crossed to vacuumize.
Realize that step is as follows：
(1) according to by the calibration range of school quadrupole mass spectrometer 18, selection induction pathway, measurement sampling room 5 and Sample Room 17
Volumetric ratio
(2) start the first extract system, the second extract system, the 3rd extract system, extract vacuum partial pressure calibrating installation
Gas in interior and its pipeline；And close the first valve 4, the second valve 6, the 3rd valve 7, the 4th valve 10, the 5th valve 12,
6th valve 14, the 7th valve 15 and the 8th valve 19；
(3) extract system is closed, the valve 4 of reset valve 1 and first is opened, by gas by introducing sampling room 5 with specimen chamber 3
In, first valve 4 of closing after pressure stabilisation, the 7th valve 15 is then opened, gas is filled with by the measurement of piston manometer 16
Pressure p=1 × 104Pa；
(4) the second valve 6 is opened, by gas expansion into Sample Room 17, second valve 6 of closing after pressure stabilisation, then
The gas pressure of Sample Room 17 is 1 × 10-5Pa；
(5) the 3rd valve 7 is opened, it is after pressure stabilisation by gas expansion into secondary expansion room 8, open the 4th valve
10, the gas pressure of compound vacuum gauge 9 is read, judges whether the gas pressure in Sample Room 17 meets school according to the gas pressure
Quasi need, if not satisfied, continuing gas expansion to secondary expansion room 8, until meeting calibration requirements；If the gas in Sample Room 17
Body pressure meets calibration requirements, then closes the 3rd valve 7, now the gas pressure 9.1 × 10 of Sample Room 17-6Pa；
(6) the 5th valve 12 is opened, gas is incorporated into calibration chamber 13 by aperture 11, it is after pressure stabilisation, open
6th valve 14 reads the gas pressure of separate vacuum meter 20, and judges the gas pressure in calibration chamber 13 according to the gas pressure
Whether calibration requirements are met, if not satisfied, continuing gas introducing calibration chamber 13 by aperture 11, until meeting to calibrate need
Ask；If the gas pressure in calibration chamber 13 meets calibration requirements, valve 12 is closed, now the standard partial pressure of calibration chamber 13 is
9.1×10-9Pa；
(7) the 8th valve 19 is opened, it is after pressure stabilisation, read by the pressure reading of school mass spectrometers for partial pressure 18, close
8th valve 19；
(8) standard partial pressure is compared with by the partial pressure reading of school mass spectrometers for partial pressure 18, obtained by school partial pressure
The calibration factor of power mass spectrograph.
It is using the reason for three kinds of extract systems with the gas pressure requirement in specimen chamber 3, Sample Room 17 and calibration chamber 13
Difference, and it is distant between three, if using an extract system, higher is required to pipeline, thus cost is higher.
Certainly, the present invention can also have other various embodiments, ripe in the case of without departing substantially from spirit of the invention and its essence
Know those skilled in the art when can be made according to the present invention it is various it is corresponding change and deformation, but these corresponding change and become
Shape should all belong to the protection domain of appended claims of the invention.
Claims (10)
1. one kind 10-9The vacuum partial pressure calibrating installation of Pa magnitudes, it is characterised in that including：Reset valve (1), source of the gas (2), match somebody with somebody
Specimen chamber (3), eight valves (4,6,7,10,12,14,15,19), sampling room (5), secondary expansion room (8), compound vacuum gauge (9),
Aperture (11), calibration chamber (13), piston manometer (16), Sample Room (17) and by school mass spectrometers for partial pressure (18), separate vacuum
Count (20)；Ancillary equipment is extract system；
It is connected with source of the gas (2) by reset valve (1) with specimen chamber (3), is connected by the first valve (4) with sampling room (5)；Sampling room
(5) it is connected with Sample Room (17) by the second valve (6), is connected by the 7th valve (15) with piston manometer (16)；Sample introduction
Room (17) is connected by the 3rd valve (7) with secondary expansion room (8), is connected by the 4th valve (10) with compound vacuum gauge (9),
And it is connected after connection aperture (11) by the 5th valve (12) with calibration chamber (13)；Calibration chamber (13) by the 8th valve (19) with
Connected by school mass spectrometers for partial pressure (18), be connected by the 6th valve (14) with separate vacuum meter (20)；And vacuum partial pressure school
The pipeline of standard apparatus is connected with extract system.
2. one kind 10 as claimed in claim 1-9The vacuum partial pressure calibrating installation of Pa magnitudes, it is characterised in that the fine setting
Valve (1) is ultrahigh vacuum all-metal reset valve.
3. one kind 10 as claimed in claim 1-9The vacuum partial pressure calibrating installation of Pa magnitudes, it is characterised in that the source of the gas
(2) mixed gas of main constituent for the combination of multiple pure gases or.
4. one kind 10 as claimed in claim 1-9The vacuum partial pressure calibrating installation of Pa magnitudes, it is characterised in that the sample
Room (3) is stainless steel spherical structure, volume 10L.
5. one kind 10 as claimed in claim 1-9The vacuum partial pressure calibrating installation of Pa magnitudes, it is characterised in that described eight
Valve is ultrahigh vacuum all-metal ball valve.
6. one kind 10 as claimed in claim 1-9The vacuum partial pressure calibrating installation of Pa magnitudes, it is characterised in that the sampling
Room (5), secondary expansion room (8), Sample Room (17) are stainless steel spherical structure.
7. one kind 10 as claimed in claim 1-9The vacuum partial pressure calibrating installation of Pa magnitudes, it is characterised in that the sample introduction
Room (17) is 10 with secondary expansion room (8) volumetric ratio.
8. one kind 10 as claimed in claim 1-9The vacuum partial pressure calibrating installation of Pa magnitudes, it is characterised in that the aperture
(11) decline of pressure ratio is 1/1000.
9. one kind 10 as claimed in claim 1-9The vacuum partial pressure calibrating installation of Pa magnitudes, it is characterised in that with specimen chamber
(3), Sample Room (17), calibration chamber (13) are vacuumized by three sets of different extract systems.
10. 10 described in a kind of claim 1-9The calibration factor acquisition methods of the vacuum partial pressure calibrating installation of Pa magnitudes, its
It is characterised by, comprises the following steps：
Step 1, the volumetric ratio of sampling room (5) and Sample Room (17) is measured
Step 2, the gas in vacuum partial pressure calibrating installation and its in pipeline is extracted, and closes reset valve (1), the first valve
(4), the second valve (6), the 3rd valve (7), the 4th valve (10), the 5th valve (12), the 6th valve (14), the 7th valve
And the 8th valve (19) (15)；
Step 3, reset valve (1) and the first valve (4) are opened, by the gas in source of the gas (2) by introducing sampling with specimen chamber (3)
In room (5), first valve of closing after pressure stabilisation (4), the 7th valve (15) is then opened, measured by piston manometer (16)
The pressure p of gas is filled with sampling room (5)；
Step 4, the second valve (6), by gas expansion is into Sample Room (17) in sampling room (5), pass after pressure stabilisation are opened
The second valve (6) is closed, because of VSample introduction>>VSampling, then Sample Room (17) gas pressure be
Step 5, the 3rd valve (7) is opened, it is after pressure stabilisation by gas expansion in secondary expansion room (8), open the 4th valve
Door (10), the gas pressure of compound vacuum gauge (9) is read, judges that the gas pressure in Sample Room (17) is according to the gas pressure
It is no to meet calibration requirements, if not satisfied, continuing gas expansion to secondary expansion room (8), until meeting calibration requirements；If sample introduction
Gas pressure in room (17) meets calibration requirements, then closes the 3rd valve (7), and now Sample Room (17) gas pressure is
Step 6, the 5th valve (12) is opened, gas is incorporated into calibration chamber (13) by aperture (11), it is after pressure stabilisation,
Open the 6th valve (14) and read the gas pressure of separate vacuum meter (20), and judged according to the gas pressure in calibration chamber (13)
Gas pressure whether meet calibration requirements, if not satisfied, continuing gas introducing calibration chamber (13) by aperture (11), directly
To meeting calibration requirements；If the gas pressure in calibration chamber (13) meets calibration requirements, the 5th valve (12) is closed, now school
The standard partial pressure of quasi- room (13) is
Step 7, the 8th valve (19) is opened, it is after pressure stabilisation, read by the pressure reading of school mass spectrometers for partial pressure (18), close
Close the 8th valve (19)；
Step 8, the standard partial pressure is compared with by the pressure reading of school mass spectrometers for partial pressure (18), obtained by school point
The calibration factor of pressure mass spectrograph.
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