CN106289666B - Calibration device and method for vacuum leak at ambient temperature - Google Patents
Calibration device and method for vacuum leak at ambient temperature Download PDFInfo
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- CN106289666B CN106289666B CN201610794556.1A CN201610794556A CN106289666B CN 106289666 B CN106289666 B CN 106289666B CN 201610794556 A CN201610794556 A CN 201610794556A CN 106289666 B CN106289666 B CN 106289666B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01M—TESTING STATIC OR DYNAMIC BALANCE OF MACHINES OR STRUCTURES; TESTING OF STRUCTURES OR APPARATUS, NOT OTHERWISE PROVIDED FOR
- G01M3/00—Investigating fluid-tightness of structures
- G01M3/02—Investigating fluid-tightness of structures by using fluid or vacuum
- G01M3/04—Investigating fluid-tightness of structures by using fluid or vacuum by detecting the presence of fluid at the leakage point
- G01M3/20—Investigating fluid-tightness of structures by using fluid or vacuum by detecting the presence of fluid at the leakage point using special tracer materials, e.g. dye, fluorescent material, radioactive material
- G01M3/202—Investigating fluid-tightness of structures by using fluid or vacuum by detecting the presence of fluid at the leakage point using special tracer materials, e.g. dye, fluorescent material, radioactive material using mass spectrometer detection systems
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01M—TESTING STATIC OR DYNAMIC BALANCE OF MACHINES OR STRUCTURES; TESTING OF STRUCTURES OR APPARATUS, NOT OTHERWISE PROVIDED FOR
- G01M3/00—Investigating fluid-tightness of structures
- G01M3/02—Investigating fluid-tightness of structures by using fluid or vacuum
- G01M3/04—Investigating fluid-tightness of structures by using fluid or vacuum by detecting the presence of fluid at the leakage point
- G01M3/20—Investigating fluid-tightness of structures by using fluid or vacuum by detecting the presence of fluid at the leakage point using special tracer materials, e.g. dye, fluorescent material, radioactive material
- G01M3/207—Investigating fluid-tightness of structures by using fluid or vacuum by detecting the presence of fluid at the leakage point using special tracer materials, e.g. dye, fluorescent material, radioactive material calibration arrangements
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Abstract
The invention relates to a calibration device and method for a vacuum leak at ambient temperature, and belongs to the field of measurement. The device comprises a reference vacuum leak system mainly composed of a reference vacuum leak, a reference vacuum leak temperature sensor and a reference vacuum leak system valve, a to-be-corrected vacuum leak system mainly composed of a to-be-corrected vacuum leak, a to-be-corrected vacuum leak temperature sensor and a to-be-corrected vacuum leak system valve, and a mass spectrometry system and an air extraction system mainly composed of a calibration chamber, a vacuum gauge and a mass spectrometer. The leak rate of a reference vacuum leak hole at the laboratory temperature is corrected to the leak rate of the reference vacuum leak hole at the ambient temperature by using an index or linear temperature correction method through real-time measurement of a temperature sensor, so that the influence of different temperatures on the leak rate of the reference vacuum leak hole is avoided.
Description
Technical Field
The invention relates to a calibration device and method for a vacuum leak at ambient temperature, and belongs to the field of measurement.
Background
At present, the calibration of the vacuum leak is mainly performed in a laboratory, and the calibration environment of the laboratory generally requires: a) the environment temperature is (23 +/-3) DEG C, and the temperature fluctuation in the calibration process is not more than 1 ℃/h; b) relative humidity no greater than 80%; c) the ambient environment must not have additional heat source, strong electromagnetic field, strong vibration, etc. when calibrating, the calibration temperature that gives in the laboratory finally is the leak rate of the vacuum leak hole of waiting to calibrate under 23 ℃. The actual vacuum leak is mainly used in an open hall or workshop, the environmental temperature range generally changes at 15-40 ℃ due to seasonal changes and different south-north regions, the actual leak rate of the vacuum leak is the leak rate at the current temperature, the leak rate at the temperature of 23 ℃ is generally provided in a laboratory, the deviation range of the environmental temperature is-8 ℃ to +17 ℃, the influence of the environmental temperature on the leak rate of the vacuum leak is about 8-180%, and the leak rate of the vacuum leak can change due to the fact that the environmental temperature cannot meet the requirement of a calibration environment. The difference between the environmental temperature and the laboratory calibration temperature leads to the deviation of the leak rate of the vacuum leak hole, which can seriously affect the use result of the vacuum leak hole, so the vacuum leak hole needs to be calibrated at the environmental temperature, thereby fundamentally improving the use reliability of the vacuum leak hole.
Disclosure of Invention
Aiming at the defect that the conventional vacuum calibrating device cannot realize calibration at ambient temperature, the invention aims to provide a calibrating device for a vacuum leak at ambient temperature; the second purpose of the invention is to provide a calibration method for vacuum leak hole under ambient temperature; the device and the method realize the accurate calibration of the vacuum leak hole at the ambient temperature.
In order to achieve the purpose of the invention, the following technical scheme is provided.
A calibrating device for a vacuum leak at ambient temperature mainly comprises a reference vacuum leak system, a vacuum leak system to be calibrated, a mass spectrometry system and an air pumping system.
The reference vacuum leak hole system mainly comprises a reference vacuum leak hole, a reference vacuum leak hole temperature sensor and a reference vacuum leak hole system valve; the reference vacuum leak hole temperature sensor is connected with the reference vacuum leak hole and used for measuring the temperature of the reference vacuum leak hole, the reference vacuum leak hole is connected with the calibration chamber through a pipeline and a reference vacuum leak hole system valve on the pipeline, and the reference vacuum leak hole system valve is used for communicating or blocking a connecting channel between the reference vacuum leak hole and the calibration chamber.
The system for the to-be-calibrated vacuum leak hole mainly comprises the to-be-calibrated vacuum leak hole, a temperature sensor of the to-be-calibrated vacuum leak hole and a valve of the system for the to-be-calibrated vacuum leak hole, wherein the system for the to-be-calibrated vacuum leak hole is more than one group, and the composition of each group of the system for the to-be-calibrated vacuum leak hole is the same; the temperature sensor of the to-be-calibrated vacuum leak hole is connected with the to-be-calibrated vacuum leak hole and used for measuring the temperature of the to-be-calibrated vacuum leak hole, the to-be-calibrated vacuum leak hole is connected with the calibration chamber through a pipeline and a valve of the to-be-calibrated vacuum leak hole system on the pipeline, and the valve of the to-be-calibrated vacuum leak hole system is used for communicating or blocking a connecting channel between the to-be-calibrated vacuum leak hole and the calibration chamber.
The mass spectrometry system mainly comprises a calibration chamber, a vacuum gauge and a mass spectrometer; the calibration chamber is used for comparing the amount of calibration gas flowing out of the reference vacuum leak and the to-be-calibrated vacuum leak, the vacuum gauge is connected with the calibration chamber and used for monitoring the vacuum degree of the calibration chamber, and the mass spectrometer is connected with the calibration chamber and used for measuring signals of the calibration gas.
The air pumping system is a device for pumping air to reach vacuum in the prior art, and can be a mechanical pump and a molecular pump or a combination of the mechanical pump and a double molecular pump; the air pumping system is connected with the calibration chamber through a pipeline and an air pumping system valve on the pipeline and is used for pumping air to the calibration chamber and maintaining the vacuum degree in the calibration chamber, and the air pumping system valve is used for communicating or blocking a connecting channel between the air pumping system and the calibration chamber.
Preferably, the reference vacuum leak system valve and the vacuum leak system valve to be calibrated are connected with the calibration chamber after being converged into a pipeline.
In the device, the leakage rate (Q) of the reference vacuum leak hole at the laboratory temperaturecal) Reference laboratory temperature (T) of vacuum leakcal) The constant (c) of the reference vacuum leak hole, which can be obtained by the method in "temperature correction of leak rate of helium leak type vacuum leak hole", vacuum and low temperature, 2007.6 ", is known, and the temperature coefficient (α) of the reference vacuum leak hole.
The reference vacuum leak hole and the vacuum leak hole to be calibrated can be provided with air sources or connected with the air sources so as to flow out calibration gas.
The calibration gas is a calibration gas commonly used in the art, such as helium (He), nitrogen (N)2) Or hydrogen (H)2)。
The mass spectrometer is preferably a quadrupole mass spectrometer.
Preferably, the valve is an all-metal ultrahigh vacuum valve.
When the calibration gas is helium, the mass spectrometry system, the air pumping system and the air pumping system valve can be replaced by a helium mass spectrometer leak detector, and the reference vacuum leak system valve and the vacuum leak system valve to be calibrated are connected with the helium mass spectrometer leak detector after being converged into a pipeline.
A calibration method for a vacuum leak at ambient temperature is carried out by using the calibration device for the vacuum leak at ambient temperature, wherein a reference vacuum leak system valve, a to-be-calibrated vacuum leak system valve, a mass spectrometer, an air pumping system valve and an air pumping system are all in a closed state before calibration, and the method comprises the following steps:
(1) opening a valve of an air extraction system, starting the air extraction system, extracting gas from the calibration chamber, continuously extracting gas in the following steps to reach the required vacuum degree until all the steps are completed, monitoring the pressure in the calibration chamber by using a vacuum gauge, and opening the mass spectrometer to measure the calibration chamber after the pressure reaches the starting pressure of the mass spectrometer;
(2) when the limit pressure is reached in the calibration chamber, namely one position after the decimal point of the pressure value in the calibration chamber is monitored by the vacuum gauge does not change, the measurement of the mass spectrometerThe value is the background signal (I) of the calibration gas in the calibration chamber0)；
(3) Opening a valve of a reference vacuum leak hole system, introducing the calibration gas flowing out of the reference vacuum leak hole into a calibration chamber, and when the calibration gas is stabilized, taking the measurement value of a mass spectrometer as a calibration gas signal (I) generated by the reference vacuum leak hole in the calibration chamberS) The reference vacuum leak hole temperature sensor measures the environmental temperature (T) of the reference vacuum leak hole, and the leak rate (Q) of the reference vacuum leak hole at the laboratory temperature is corrected by an exponential temperature correction method or a linear temperature correction methodcal) Corrected to the leakage rate (Q) of the reference vacuum leak hole at ambient temperatureT) (ii) a Q corrected by exponential temperature correction method versus linear temperature correction methodTHas smaller deviation, so that Q is obtained by the exponential temperature correction method and the linear temperature correction methodTWhen the specific numerical values are inconsistent, an exponential temperature correction method is preferably selected;
wherein, the exponential temperature correction method is shown as formula (1):
in equation (1):
QT-leak rate of the reference vacuum leak at ambient temperature, in units of: pam3/s；
Qcal-leak rate of the reference vacuum leak at laboratory temperature in units of: pam3/s；
T-ambient temperature of the reference vacuum leak, unit is: k;
Tcalreference laboratory temperature of the vacuum leak in units of: K.
c-constant of reference vacuum leak.
The formula (1) can be obtained by the method in the document "temperature correction of leak rate of helium-permeated type vacuum leak hole", vacuum and low temperature, 2007.6 ";
the linear temperature correction method is shown in formula (2):
QT＝Qcal·[1+α×(T-Tcal)](2)
in equation (2):
QT-leak rate of the reference vacuum leak at ambient temperature, in units of: pam3/s；
Qcal-leak rate of the reference vacuum leak at laboratory temperature in units of: pam3/s；
T-ambient temperature of the reference vacuum leak, unit is: k;
Tcalreference laboratory temperature of the vacuum leak in units of: k;
α -temperature coefficient of reference vacuum leak hole, unit is:%/K.
Said formula (2) can be obtained by the method described in "temperature correction of leak rate of helium-permeated type vacuum leak hole", vacuum and low temperature, 2007.6 ".
(4) Closing a valve of a reference vacuum leak system, opening a valve of a vacuum leak system to be calibrated, introducing calibration gas flowing out of the vacuum leak to be calibrated into a calibration chamber, and when the calibration gas is stable, taking the measurement value of a mass spectrometer as a calibration gas signal (I) generated by the vacuum leak to be calibrated in the calibration chamberL) The temperature sensor of the vacuum leak hole to be calibrated measures the environmental temperature (T) of the vacuum leak hole to be calibratedL) Calculating the leakage rate (Q) of the vacuum leakage hole to be corrected at the ambient temperature by the formula (3)L)：
In equation (3):
QLthe leakage rate of the vacuum leak to be corrected at the ambient temperature is in units of: pam3/s，
IL-the calibration gas signal generated by the leak to be calibrated in the calibration chamber has the unit: a;
IS-a calibration gas signal generated in the calibration chamber with reference to the vacuum leak in units of: a;
I0-background signal of calibration gas in calibration chamber in units of: A.
when more than two groups of vacuum leak hole systems to be calibrated exist, the leak rate measured in the step (4) is the leak rate of the vacuum leak holes to be calibrated in the first group of vacuum leak hole systems to be calibrated at the ambient temperature; the leakage rate of the vacuum leakage holes to be corrected in the second group of vacuum leakage hole systems to be corrected at the ambient temperature is obtained by adopting the following method:
replacing the valve for closing the reference vacuum leak hole system in the step (4) with a valve for closing the first group of vacuum leak hole system to be corrected, opening a valve for opening the second group of vacuum leak hole system to be corrected, and performing the rest of the steps (4) to obtain the leak rate of the vacuum leak hole to be corrected in the second group of vacuum leak hole system to be corrected at the ambient temperature; by analogy, the leakage rate of the vacuum leakage holes to be corrected in the multiple groups of vacuum leakage hole systems to be corrected at the ambient temperature can be obtained.
The calibration gas is stabilized when the vacuum gauge monitors the pressure in the calibration chamber for a fraction of the time that is constant and the mass spectrometer has a stable fluctuation of less than 5%.
Advantageous effects
1. The invention provides a calibration device and a calibration method for a vacuum leak hole at ambient temperature, which are characterized in that the leak rate (Q) of a reference vacuum leak hole at the laboratory temperature is measured in real time by a temperature sensor by using an exponential temperature correction method and a linear temperature correction methodcal) Corrected to the leakage rate (Q) of the reference vacuum leak hole at ambient temperatureT) On the basis, when the reference vacuum leaking holes and the to-be-calibrated vacuum leaking holes are at the same environmental temperature, the leaking rate of the to-be-calibrated vacuum leaking holes at the environmental temperature can be obtained by adopting a comparison method, so that the accuracy of the leaking rate is improved, and the calibration efficiency is also improved.
Drawings
FIG. 1 is a schematic structural diagram of a calibrating apparatus for a vacuum leak at ambient temperature according to an embodiment.
In the figure: 1-reference vacuum leak hole, 2-reference vacuum leak hole temperature sensor, 3-reference vacuum leak hole system valve, 4-to-be-calibrated vacuum leak hole, 5-to-be-calibrated vacuum leak hole temperature sensor, 6-to-be-calibrated vacuum leak hole system valve, 7-calibration chamber, 8-vacuum gauge, 9-mass spectrometer, 10-pumping system valve, 11-pumping system, 12-helium mass spectrometer leak detector, 13-second to-be-calibrated vacuum leak hole, 14-second to-be-calibrated vacuum leak hole temperature sensor, 15-second to-be-calibrated vacuum leak hole system valve
Detailed Description
Example 1
As shown in FIG. 1, the calibrating device for the vacuum leak at the ambient temperature mainly comprises a reference vacuum leak system, a vacuum leak system to be calibrated, a mass spectrometry system and an air pumping system 11.
The reference vacuum leak hole system mainly comprises a reference vacuum leak hole 1, a reference vacuum leak hole temperature sensor 2 and a reference vacuum leak hole system valve 3; the reference vacuum leak hole temperature sensor 2 is connected with the reference vacuum leak hole 1 and used for measuring the temperature of the reference vacuum leak hole 1, the reference vacuum leak hole 1 is connected with the calibration chamber 7 through a pipeline and a reference vacuum leak hole system valve 3 on the pipeline, and the reference vacuum leak hole system valve 3 is used for communicating or blocking a connecting channel between the reference vacuum leak hole 1 and the calibration chamber 7.
The vacuum leak hole systems to be calibrated are divided into two groups, and the compositions of each group of vacuum leak hole systems to be calibrated are the same: the first group mainly comprises a to-be-corrected vacuum leak hole 4, a to-be-corrected vacuum leak hole temperature sensor 5 and a to-be-corrected vacuum leak hole system valve 6, wherein: the temperature sensor 5 of the vacuum leak hole to be calibrated is connected with the vacuum leak hole 4 to be calibrated and is used for measuring the temperature of the vacuum leak hole 4 to be calibrated, the vacuum leak hole 4 to be calibrated is connected with the calibration chamber 7 through a pipeline and a system valve 6 of the vacuum leak hole to be calibrated on the pipeline, and the system valve 6 of the vacuum leak hole to be calibrated is used for communicating or blocking a connecting channel between the vacuum leak hole 4 to be calibrated and the calibration chamber 7; the second group mainly comprises a second to-be-calibrated vacuum leak hole 13, a second to-be-calibrated vacuum leak hole temperature sensor 14 and a second to-be-calibrated vacuum leak hole system valve 15, wherein: the second to-be-calibrated vacuum leak hole temperature sensor 14 is connected with the second to-be-calibrated vacuum leak hole 13 and used for measuring the temperature of the second to-be-calibrated vacuum leak hole 13, the second to-be-calibrated vacuum leak hole 13 is connected with the calibration chamber 7 through a pipeline and a second to-be-calibrated vacuum leak hole system valve 15 on the pipeline, and the second to-be-calibrated vacuum leak hole system valve 15 is used for communicating or blocking a connecting channel between the second to-be-calibrated vacuum leak hole 13 and the calibration chamber 7.
The mass spectrometry system mainly comprises a calibration chamber 7, a vacuum gauge 8 and a mass spectrometer 9; wherein: the calibration chamber 7 is used for comparing the amounts of calibration gas flowing out of the reference vacuum leak hole 1, the to-be-calibrated vacuum leak hole 4 and the second to-be-calibrated vacuum leak hole 13, the vacuum gauge 8 is connected with the calibration chamber 7 and used for monitoring the vacuum degree of the calibration chamber 7, and the mass spectrometer 9 is connected with the calibration chamber 7 and used for measuring signals of the calibration gas.
The air pumping system 11 is a combination of a mechanical pump and a molecular pump; the air pumping system 11 is connected with the calibration chamber 7 through a pipeline and an air pumping system valve 10 on the pipeline, and is used for pumping air to the calibration chamber 7 and maintaining the vacuum degree in the calibration chamber 7, and the air pumping system valve 10 is used for communicating or blocking a connecting channel between the air pumping system 11 and the calibration chamber 7.
The reference vacuum leak system valve 3, the to-be-calibrated vacuum leak system valve 6 and the second to-be-calibrated vacuum leak system valve 15 are respectively connected with the calibration chamber 7 after being converged into a pipeline.
In the device, the leakage rate (Q) of the reference vacuum leak hole 1 at the laboratory temperaturecal) Is 1.28X 10-9Pam3S, laboratory temperature (T) of reference vacuum leak 1cal) The constant (c) of the reference vacuum leak hole 1, which is 296K and is-2635.5, and the temperature coefficient (α) of the reference vacuum leak hole 1, which is 3.63%, are known, and can be obtained by the method described in "temperature correction of leak rate of helium infiltration type vacuum leak hole", vacuum and low temperature, 2007.6 ".
The reference vacuum leak hole 1, the to-be-calibrated vacuum leak hole 4 and the second to-be-calibrated vacuum leak hole 13 are provided with gas sources to flow out calibration gas.
The calibration gas is helium (He).
The mass spectrometer 9 is a quadrupole mass spectrometer.
The valve is an all-metal ultrahigh vacuum valve.
The mass spectrometry system, the gas-extracting system 11 and the gas-extracting system valve 10 can also be replaced by a helium mass spectrometer leak detector 12, and the reference vacuum leak system valve 3, the to-be-corrected vacuum leak system valve 6 and the second to-be-corrected vacuum leak system valve 15 are respectively connected with the helium mass spectrometer leak detector 12 after being converged into a pipeline.
A calibration method for a vacuum leak at ambient temperature is carried out by using the calibration device for the vacuum leak at ambient temperature, wherein a reference vacuum leak system valve 3, a to-be-calibrated vacuum leak system valve 6, a second to-be-calibrated vacuum leak system valve 15, a mass spectrometer 9, an air pumping system valve 10 and an air pumping system 11 are all in a closed state before calibration, and the method comprises the following steps:
(1) opening a valve 10 of the air extraction system, starting a mechanical pump in the air extraction system 11, extracting gas from the calibration chamber 7 until the pressure in the calibration chamber 7 measured by the vacuum gauge 8 reaches 1Pa, starting a molecular pump in the air extraction system 11, continuously extracting gas in the following steps to reach the required vacuum degree until all the steps are completed, monitoring the pressure in the calibration chamber 7 by the vacuum gauge 8, and opening the mass spectrometer 9 to measure the calibration chamber 7 after the pressure reaches the starting pressure of the mass spectrometer 9;
(2) when the limit pressure is reached in the calibration chamber 7, i.e. the vacuum gauge 8 monitors the decimal point of the pressure value in the calibration chamber 7 and then one bit does not change, the measurement value of the mass spectrometer 9 is the background signal (I) of the calibration gas in the calibration chamber 70) Is 1.63X 10-13A；
(3) Opening a valve 3 of the reference vacuum leak hole system, introducing the calibration gas flowing out of the reference vacuum leak hole 1 into a calibration chamber 7, and when the calibration gas is stabilized, taking the measured value of a mass spectrometer 9 as a calibration gas signal (I) generated by the reference vacuum leak hole 1 in the calibration chamber 7S) Is 1.72X 10-10A, measuring by a reference vacuum leak hole temperature sensor 2 to obtain the environment temperature (T) of a reference vacuum leak hole 1 to be 298K, and performing exponential temperature correction or linear temperature correction on the leak rate (Q) of the reference vacuum leak hole 1 at the laboratory temperaturecal) Corrected to the leakage rate (Q) of the reference vacuum leak hole 1 at ambient temperatureT)；
Wherein, the exponential temperature correction method is shown as formula (1):
in the formula:
QTthe leak rate of the reference vacuum leak orifice 1 at ambient temperature, in units of: pam3/s；
QcalThe leak rate of the reference vacuum leak orifice 1 at laboratory temperature, in units of: pam3/s；
T-the ambient temperature of the reference vacuum leak 1, with the unit: k;
Tcalreference laboratory temperature of the vacuum leak 1, in units of: k;
c-constant of the reference vacuum leak 1,
e is the natural base number;
calculating to obtain QTIs 1.37X 10-9Pam3/s。
The formula (1) can be obtained by the method in the document "temperature correction of leak rate of helium-permeated type vacuum leak hole", vacuum and low temperature, 2007.6 ";
the linear temperature correction method formula (2) is as follows:
QT＝Qcal·[1+α×(T-Tcal)](2)
in the formula:
QTthe leak rate of the reference vacuum leak orifice 1 at ambient temperature, in units of: pam3/s；
QcalThe leak rate of the reference vacuum leak orifice 1 at laboratory temperature, in units of: pam3/s；
T-the ambient temperature of the reference vacuum leak 1, with the unit: k;
Tcalreference laboratory temperature of the vacuum leak 1, in units of: k;
α -temperature coefficient of the reference vacuum leak hole 1, unit is:%/K;
calculating to obtain QTIs 1.37X 10-9Pam3/s。
Said formula (2) can be obtained by the method in "temperature correction of leak rate of helium-permeated type vacuum leak hole", vacuum and low temperature, 2007.6 ";
in this example, Q at an ambient temperature of 298K obtained by exponential temperature correction and linear temperature correctionTThe specific values are consistent; but with temperature variation, Q obtained by exponential temperature correction and linear temperature correctionTThe specific values may not be consistent, and the preferred choice is the exponential temperature correction method, the exponential temperature correction method than the linear temperature correction methodTLess deviation of (d);
(4) closing the valve 3 of the reference vacuum leak system, opening the valve 6 of the vacuum leak system to be calibrated, introducing the calibration gas flowing out of the vacuum leak 4 to be calibrated into the calibration chamber 7, and when the calibration gas is stable, the measurement value of the mass spectrometer 9 is the calibration gas signal (I) generated by the vacuum leak 4 to be calibrated in the calibration chamber 7L) Is 1.85X 10-10A; the temperature sensor 5 of the vacuum leak hole to be calibrated measures the environmental temperature (T) of the vacuum leak hole 4 to be calibratedL) 298K; calculating the leakage rate (Q) of the vacuum leakage hole 4 to be corrected at the ambient temperature by the formula (3)L)：
In the formula:
QLthe leakage rate of the vacuum leak 4 to be calibrated at the ambient temperature is given by the unit: pam3/s，
ILThe calibration gas signal generated by the leak 4 to be calibrated in the calibration chamber 7 has the unit: a;
ISthe calibration gas signal generated in the calibration chamber 7 with reference to the vacuum leak 1 has the unit: a;
I0the background signal of the calibration gas in the calibration chamber 7 is given by: A.
calculating to obtain QLIs 1.47X 10-9Pam3/s。
(5) Closing the valve 6 of the vacuum leak system to be calibrated, opening the valve 15 of the second vacuum leak system to be calibrated, introducing the calibration gas flowing out of the second vacuum leak 13 to be calibrated into the calibration chamber 7, and measuring by the mass spectrometer 9 when the calibration gas is stableThe value of the calibration gas signal (I) generated by the second leak hole 13 to be calibrated in the calibration chamber 7L’) Is 2.75X 10-10A; the temperature sensor 14 of the second vacuum leak hole to be calibrated measures the ambient temperature (T) of the second vacuum leak hole 13 to be calibratedL’) 298K; calculating the leakage rate (Q) of the second vacuum leakage hole 13 to be calibrated at the ambient temperature through the formula (4)L’)：
In the formula:
QL’the leakage rate of the second to-be-calibrated vacuum leak hole 13 at the ambient temperature is given by: pam3/s，
IL’The calibration gas signal generated by the second leak to be calibrated 13 in the calibration chamber 7 has the unit: a;
ISthe calibration gas signal generated in the calibration chamber 7 with reference to the vacuum leak 1 has the unit: a;
I0the background signal of the calibration gas in the calibration chamber 7 is given by: a;
calculating to obtain QL’Is 2.20X 10-9Pam3/s。
The calibration gas is stabilized when the vacuum gauge 8 monitors the pressure in the calibration chamber 7 for a fraction of the time that is constant and the mass spectrometer 9 has a stable fluctuation of less than 5%.
Claims (7)
1. A calibrating device for vacuum leak at ambient temperature characterized by: the device comprises a reference vacuum leak hole system, a vacuum leak hole system to be calibrated, a mass spectrometry system and an air pumping system (11);
the reference vacuum leak hole system mainly comprises a reference vacuum leak hole (1), a reference vacuum leak hole temperature sensor (2) and a reference vacuum leak hole system valve (3); the device comprises a reference vacuum leak hole temperature sensor (2), a calibration chamber (7), a calibration valve and a calibration valve, wherein the reference vacuum leak hole temperature sensor (2) is connected with a reference vacuum leak hole (1), and the reference vacuum leak hole (1) is connected with the calibration chamber (7) through a pipeline and a reference vacuum leak hole system valve (3) on the pipeline;
the system for the vacuum leak holes to be corrected mainly comprises the vacuum leak holes to be corrected (4), a temperature sensor for the vacuum leak holes to be corrected (5) and a valve for the system for the vacuum leak holes to be corrected (6), wherein the system for the vacuum leak holes to be corrected is more than one group, and the composition of each group of the system for the vacuum leak holes to be corrected is the same; wherein, the temperature sensor (5) of the leak hole to be calibrated is connected with the leak hole (4) to be calibrated, and the leak hole (4) to be calibrated is connected with the calibration chamber (7) through a pipeline and a system valve (6) of the leak hole to be calibrated on the pipeline;
the mass spectrometry system mainly comprises a calibration chamber (7), a vacuum gauge (8) and a mass spectrometer (9); wherein the vacuum gauge (8) and the mass spectrometer (9) are respectively connected with the calibration chamber (7);
the air pumping system (11) is connected with the calibration chamber (7) through a pipeline and an air pumping system valve (10) on the pipeline;
in the device, the leakage rate, the laboratory temperature, the constant and the temperature coefficient of the reference vacuum leakage hole (1) at the laboratory temperature are known;
the reference vacuum leak hole (1) and the vacuum leak hole (4) to be calibrated are provided with air sources or connected with the air sources;
in the calibration process, the leakage rate Q of the reference vacuum leakage hole (1) at the ambient temperature is obtained by adopting an exponential temperature correction method or a linear temperature correction methodTThe calculation formulas are respectively shown in formula (1) and formula (2), wherein the leakage rate Q of the reference vacuum leakage hole (1) at the laboratory temperaturecalLaboratory temperature TcalThe constant c and the temperature coefficient α are known;
the exponential temperature correction method is shown in formula (1):
in equation (1):
QT-leak rate of the reference vacuum leak hole (1) at ambient temperature;
Qcal-leak rate of the reference vacuum leak (1) at laboratory temperature;
t is the ambient temperature of the reference vacuum leak hole (1);
Tcalreference vacuum leak(1) The laboratory temperature of (a);
c-constant of the reference vacuum leak hole (1);
the linear temperature correction method is shown in formula (2):
QT＝Qcal·[1+α×(T-Tcal)](2)
in equation (2):
α -temperature coefficient of reference vacuum leak hole (1);
QT-leak rate of the reference vacuum leak hole (1) at ambient temperature;
Qcal-leak rate of the reference vacuum leak (1) at laboratory temperature;
t is the ambient temperature of the reference vacuum leak hole (1);
Tcal-reference laboratory temperature of the vacuum leak (1).
2. A calibration device for an ambient temperature vacuum leak, as defined in claim 1, wherein: the calibration gas is helium, nitrogen or hydrogen; when the calibration gas is helium, the mass spectrometry system, the air pumping system (11) and the air pumping system valve (10) are replaced by a helium mass spectrometer leak detector (12), and the reference vacuum leak system valve (3) and the vacuum leak system valve (6) to be calibrated are connected with the helium mass spectrometer leak detector (12) after being combined into a pipeline.
3. A calibration device for an ambient temperature vacuum leak, as defined in claim 1, wherein: the valve is an all-metal ultrahigh vacuum valve.
4. A calibration device for an ambient temperature vacuum leak, as defined in claim 1, wherein: the mass spectrometer (9) is a four-stage mass spectrometer.
5. A calibration device for an ambient temperature vacuum leak, as defined in claim 1, wherein: and the pipelines of the reference vacuum leakage hole system valve (3) and the to-be-calibrated vacuum leakage hole system valve (6) are converged into one pipeline and then are connected with the calibration chamber (7).
6. A calibration device for an ambient temperature vacuum leak, as defined in claim 1, wherein: the calibration gas is helium, nitrogen or hydrogen; the valve is an all-metal ultrahigh vacuum valve; the mass spectrometer (9) is a four-stage mass spectrometer; and the pipelines of the reference vacuum leakage hole system valve (3) and the to-be-calibrated vacuum leakage hole system valve (6) are converged into one pipeline and then are connected with the calibration chamber (7).
7. A calibration method for a vacuum leak at ambient temperature, characterized by: the method is completed by using a calibration device for vacuum leaks at ambient temperature according to any one of claims 1 to 5, the reference vacuum leak system valve (3), the vacuum leak system valve (6) to be calibrated, the mass spectrometer (9), the gas exhaust system valve (10) and the gas exhaust system (11) are all in a closed state before calibration, and the method comprises the following steps:
(1) opening a valve (10) of the gas extraction system, starting the gas extraction system (11), extracting gas from the calibration chamber (7), continuously extracting gas in the following steps to reach the required vacuum degree until all the steps are completed, and after monitoring that the pressure in the calibration chamber (7) reaches the starting pressure of the mass spectrometer (9) by the vacuum gauge (8), opening the mass spectrometer (9) to measure the calibration chamber (7);
(2) when the limit pressure is reached in the calibration chamber (7), the measurement value of the mass spectrometer (9) is the background signal of the calibration gas in the calibration chamber (7);
(3) opening a valve (3) of a reference vacuum leak hole system, introducing calibration gas flowing out of a reference vacuum leak hole (1) into a calibration chamber (7), when the calibration gas is stable, measuring values of a mass spectrometer (9) are calibration gas signals generated by the reference vacuum leak hole (1) in the calibration chamber (7), measuring by a reference vacuum leak hole temperature sensor (2) to obtain the ambient temperature of the reference vacuum leak hole (1), and correcting the leak rate of the reference vacuum leak hole (1) at the laboratory temperature to the leak rate of the reference vacuum leak hole (1) at the ambient temperature by an exponential temperature correction method or a linear temperature correction method; q corrected by exponential temperature correction method versus linear temperature correction methodTHas smaller deviation, so that Q is obtained by the exponential temperature correction method and the linear temperature correction methodTWhen the specific numerical values are inconsistent, selecting an exponential temperature correction method;
wherein, the exponential temperature correction method is shown as formula (1):
in equation (1):
c-constant of the reference vacuum leak hole (1);
the linear temperature correction method is shown in formula (2):
QT＝Qcal·[1+α×(T-Tcal)](2)
in equation (2):
α -temperature coefficient of reference vacuum leak hole (1);
in formula (1) and formula (2):
QT-leak rate of the reference vacuum leak hole (1) at ambient temperature;
Qcal-leak rate of the reference vacuum leak (1) at laboratory temperature;
t is the ambient temperature of the reference vacuum leak hole (1);
Tcal-laboratory temperature of the reference vacuum leak (1);
(4) closing a reference vacuum leak hole system valve (3), opening a to-be-corrected vacuum leak hole system valve (6), introducing calibration gas flowing out of a to-be-corrected vacuum leak hole (4) into a calibration chamber (7), when the calibration gas reaches a stable state, measuring values of a mass spectrometer (9) are calibration gas signals generated in the calibration chamber (7) of the to-be-corrected vacuum leak hole (4), measuring an ambient temperature of the to-be-corrected vacuum leak hole (4) by a temperature sensor of the to-be-corrected vacuum leak hole (4), and calculating the leak rate of the to-be-corrected vacuum leak hole (4) at the ambient temperature through a formula (3):
in equation (3):
QLthe leakage rate of the vacuum leakage hole (4) to be calibrated at the ambient temperature,
IL-a calibration gas signal generated in the calibration chamber (7) by the leak (4) to be calibrated,
IS-referring to the calibration gas signal generated by the vacuum leak (1) in the calibration chamber (7),
I0-a background signal of the calibration gas in the calibration chamber (7),
when more than two groups of vacuum leak hole systems to be calibrated exist, the leak rate measured in the step (4) is the leak rate of the vacuum leak holes (4) to be calibrated in the first group of vacuum leak hole systems to be calibrated at the ambient temperature; the leakage rate of a second vacuum leak hole (13) to be calibrated in a second group of vacuum leak hole systems to be calibrated at the ambient temperature is obtained by adopting the following method:
replacing the reference vacuum leakage hole system closing valve (3) in the step (4) with a first group of vacuum leakage hole system valves to be corrected (6), opening a second group of vacuum leakage hole system valves to be corrected, and performing the rest of the steps (4) to obtain the leakage rate of a second vacuum leakage hole (13) to be corrected in the second group of vacuum leakage hole system to be corrected at the ambient temperature; by analogy, the leakage rate of the vacuum leakage holes to be corrected in the multiple groups of vacuum leakage hole systems to be corrected at the ambient temperature is obtained;
the calibration gas is stabilized when the vacuum gauge (8) monitors the pressure in the calibration chamber (7) for a fraction of the time that is constant and the mass spectrometer (9) has a stable fluctuation of less than 5%.
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| CN108593216B (en) * | 2018-03-27 | 2020-06-23 | 兰州空间技术物理研究所 | Portable dynamic comparison positive pressure leak hole calibration device and method |
| CN108982021A (en) * | 2018-07-13 | 2018-12-11 | 北京东方计量测试研究所 | A kind of lower limit is 10-10Pam3The PRESSURE LEAK CALIBRATION System and method for of/s |
| 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 |
| CN109752139B (en) * | 2018-12-14 | 2020-08-18 | 兰州空间技术物理研究所 | Device and method for calibrating vacuum leak of nitrogen-hydrogen mixed gas |
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