CN118010597B - Device and method for testing helium permeability of glass material for quantum vacuum measurement standard - Google Patents
Device and method for testing helium permeability of glass material for quantum vacuum measurement standard Download PDFInfo
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- CN118010597B CN118010597B CN202410419353.9A CN202410419353A CN118010597B CN 118010597 B CN118010597 B CN 118010597B CN 202410419353 A CN202410419353 A CN 202410419353A CN 118010597 B CN118010597 B CN 118010597B
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- 238000012360 testing method Methods 0.000 title claims abstract description 125
- 239000001307 helium Substances 0.000 title claims abstract description 81
- 229910052734 helium Inorganic materials 0.000 title claims abstract description 81
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 title claims abstract description 78
- 239000000463 material Substances 0.000 title claims abstract description 72
- 239000011521 glass Substances 0.000 title claims abstract description 65
- 238000005259 measurement Methods 0.000 title claims abstract description 38
- 230000035699 permeability Effects 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 18
- 239000000725 suspension Substances 0.000 claims abstract description 47
- 238000005086 pumping Methods 0.000 claims description 12
- 230000035945 sensitivity Effects 0.000 claims description 10
- 238000001514 detection method Methods 0.000 claims description 6
- 238000013016 damping Methods 0.000 claims description 5
- 238000009530 blood pressure measurement Methods 0.000 abstract description 4
- 239000007789 gas Substances 0.000 description 8
- 230000003287 optical effect Effects 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 239000006094 Zerodur Substances 0.000 description 2
- 101100096624 Caenorhabditis elegans srg-3 gene Proteins 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000008358 core component Substances 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000005305 interferometry Methods 0.000 description 1
- 238000005339 levitation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
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Abstract
The application relates to a glass material helium permeability testing device and method for quantum vacuum measurement standard, comprising the following steps: the device comprises a first fine tuning vacuum valve, a capacitance film vacuum gauge, a plenum chamber, a second fine tuning vacuum valve, a magnetic suspension rotor vacuum gauge, a test chamber A, a first vacuum valve, a test chamber B, a quadrupole mass spectrometer, a helium bottle, a second vacuum valve, a first vacuum air extractor group, a third vacuum valve, a glass material to be tested, a fourth vacuum valve, a KF interface and a second vacuum air extractor group. According to the embodiment of the application, the helium partial pressure measurement mass spectrometer for testing is calibrated on line by utilizing the good stability of the magnetic suspension rotor vacuum gauge, so that the problem of overlarge helium partial pressure measurement deviation of the mass spectrometer caused by nonideal factors such as poor stability and repeatability is solved, and the uncertainty of the helium permeability measurement of the glass material for the quantum vacuum measurement standard is effectively reduced.
Description
Technical Field
The invention relates to the technical field of standard gas supply, in particular to a glass material helium permeability testing device and method for quantum vacuum metering standard.
Background
The literature 'nonpolar thin gas refractive index measurement research in quantum vacuum measurement standard, volume 70, 4 th period, 2021, 4 months, 040601-1-9 pages' describes a medium and low vacuum quantum measurement standard device and method based on an optical interferometry. The literature indicates that the Fabry-Perot optical resonant cavity is used as a core component of the device, the stability of the physical length of the Fabry-Perot optical resonant cavity has important relevance with the performance of the device, and the Fabry-Perot optical resonant cavity is required to have good thermal stability, so ULE (Ultra Low Expansion) and Zerodur glass materials are widely adopted for manufacturing the resonant cavity; meanwhile, in view of the fact that He is the gas with highest calculation precision of the current microscopic polarization parameters, helium is required to be adopted for experiments in the standard, but the glass material has higher adsorption and diffusion characteristics on helium and macroscopically shows permeability parameters, so that accurate measurement and evaluation of the parameters plays an important role in improving metering characteristics of the device. There is no unified and accepted method and device for testing the permeability of the material He at home and abroad.
Disclosure of Invention
The embodiment of the application provides a device and a method for testing helium permeability of a glass material for a quantum vacuum measurement standard. The following presents a simplified summary in order to provide a basic understanding of some aspects of the disclosed embodiments. This summary is not an extensive overview and is intended to neither identify key/critical elements nor delineate the scope of such embodiments. Its sole purpose is to present some concepts in a simplified form as a prelude to the more detailed description that is presented later.
In a first aspect, an embodiment of the present application provides a device for testing helium permeability of a glass material for quantum vacuum measurement standards, the device comprising: the device comprises a first fine tuning vacuum valve, a capacitance film vacuum gauge, a plenum chamber, a second fine tuning vacuum valve, a magnetic suspension rotor vacuum gauge, a test chamber A, a first vacuum valve, a test chamber B, a quadrupole mass spectrometer, a helium bottle, a second vacuum valve, a first vacuum air extractor group, a third vacuum valve, a glass material to be tested, a fourth vacuum valve, a KF interface and a second vacuum air extractor group, wherein:
the helium bottle is connected with the plenum chamber, and the second vacuum valve and the first fine-tuning vacuum valve are sequentially arranged on a connected pipeline;
The plenum chamber is connected with the capacitance film vacuum gauge and the first vacuum air extractor group, and the pipeline connected with the first vacuum air extractor group is provided with the third vacuum valve;
The plenum chamber is connected with the test chamber A, a second fine-tuning vacuum valve is arranged on one connected pipeline, and the KF interface and the glass material to be tested are arranged on the other connected pipeline;
the test chamber A is connected with the magnetic suspension rotor vacuum gauge;
The test chamber A is connected with the test chamber B, and the first vacuum valve is arranged on a connected pipeline;
the testing chamber B is connected with the quadrupole mass spectrometer and the second vacuum air extractor group, and a pipeline connected with the second vacuum air extractor group is provided with the fourth vacuum valve;
the volume of the test chamber A is the same as that of the test chamber B, and the materials are the same.
According to a preferred embodiment, the glass material to be tested is in the shape of a circular sheet, the diameter range is 30 mm-40 mm, and the thickness range is 2 mm-3 mm.
According to a preferred embodiment, the minimum detectable partial pressure of the quadrupole mass spectrometer is less than or equal to 1 x 10 -10 Pa.
According to a preferred embodiment, the accuracy of the capacitance film vacuum gauge measurement should be within ±0.15%.
According to a preferred embodiment, the stability of the magnetic levitation rotor vacuum gauge is less than or equal to 1%/year.
According to another aspect of a preferred embodiment, the present embodiment provides a method for testing helium permeability of a glass material for quantum vacuum measurement standards, the method comprising:
Step 1, fixing the tested glass material on the KF interface;
Step 2, starting the first vacuum air extractor group and the second vacuum air extractor group, opening the first vacuum valve, the third vacuum valve and the fourth vacuum valve, exhausting the plenum chamber, the test chamber A, the test chamber B and the connecting pipeline, opening the capacitance film vacuum gauge connected with the plenum chamber and the magnetic suspension rotor vacuum gauge connected with the test chamber A, and opening the quadrupole mass spectrometer when the pressure in the test chamber A and the test chamber B is lower than 10 -2 Pa;
Step 3, continuously pumping air to enable the plenum chamber, the test chamber A and the test chamber B to reach the ultimate vacuum degree;
Step 4, after the quadrupole mass spectrometer, the capacitance film vacuum gauge and the magnetic suspension rotor vacuum gauge are stabilized for more than 24 hours, closing the third vacuum valve and the fourth vacuum valve, and respectively carrying out zeroing and residual damping deducting operations on the capacitance film vacuum gauge and the magnetic suspension rotor vacuum gauge;
Step 5, opening the second vacuum valve, adjusting the first fine-tuning vacuum valve, filling helium into the inflating chamber from the helium bottle, adjusting the air inlet pressure according to the test requirement, and recording the indication value of the corresponding capacitance film vacuum gauge;
Step 6, recording initial indication values of the magnetic suspension rotor vacuum gauge and initial values of helium partial pressure ion flows of the quadrupole mass spectrometer, adjusting the second fine tuning vacuum valve until the indication values of the magnetic suspension rotor vacuum gauge reach the magnitude of 10 -2 Pa, and recording the indication values of the magnetic suspension rotor vacuum gauge and the quadrupole mass spectrometer at the moment;
Step 7, calculating helium sensitivity of the quadrupole mass spectrometer according to the data measured in the step 6;
step 8, opening the fourth vacuum valve, and re-pumping the test chamber A and the test chamber B to the ultimate vacuum degree;
Step 9, closing the first vacuum valve and the fourth vacuum valve, and recording the variation of the ion flow of the quadrupole mass spectrometer within 5-180 min;
step 10, opening the first vacuum valve, and repeating the step 8;
Step 11, closing the fourth vacuum valve, recording the initial ion current value of the quadrupole mass spectrometer, and recording the value of the ion current rise of the quadrupole mass spectrometer caused by helium permeation of the glass material to be tested after the time used in the step 9;
And step 12, calculating the permeability of the tested glass material.
According to a preferred embodiment, before step 2, further comprises: and carrying out leak detection on the tested glass material and the KF interface to ensure that the leak detection meets the requirements.
The technical scheme provided by the embodiment of the application can have the following beneficial effects:
In an embodiment of the present application, the device for testing helium permeability of glass material for quantum vacuum measurement standard includes: the device comprises a first fine tuning vacuum valve, a capacitance film vacuum gauge, a plenum chamber, a second fine tuning vacuum valve, a magnetic suspension rotor vacuum gauge, a test chamber A, a first vacuum valve, a test chamber B, a quadrupole mass spectrometer, a helium bottle, a second vacuum valve, a first vacuum air extractor group, a third vacuum valve, a glass material to be tested, a fourth vacuum valve, a KF interface and a second vacuum air extractor group, wherein: the helium bottle is connected with the plenum chamber, and the second vacuum valve and the first fine-tuning vacuum valve are sequentially arranged on a connected pipeline; the plenum chamber is connected with the capacitance film vacuum gauge and the first vacuum air extractor group, and the pipeline connected with the first vacuum air extractor group is provided with the third vacuum valve; the plenum chamber is connected with the test chamber A, a second fine-tuning vacuum valve is arranged on one connected pipeline, and the KF interface and the glass material to be tested are arranged on the other connected pipeline; the test chamber A is connected with the magnetic suspension rotor vacuum gauge; the test chamber A is connected with the test chamber B, and the first vacuum valve is arranged on a connected pipeline; the testing chamber B is connected with the quadrupole mass spectrometer and the second vacuum air extractor group, and a pipeline connected with the second vacuum air extractor group is provided with the fourth vacuum valve; the volume of the test chamber A is the same as that of the test chamber B, and the materials are the same. The method for testing the helium permeability of the glass material for the quantum vacuum measurement standard comprises the following steps: step 1, fixing the tested glass material on the KF interface; step 2, starting the first vacuum air extractor group and the second vacuum air extractor group, opening the first vacuum valve, the third vacuum valve and the fourth vacuum valve, exhausting the plenum chamber, the test chamber A, the test chamber B and the connecting pipeline, opening the capacitance film vacuum gauge connected with the plenum chamber and the magnetic suspension rotor vacuum gauge connected with the test chamber A, and opening the quadrupole mass spectrometer when the pressure in the test chamber A and the test chamber B is lower than 10 -2 Pa; step 3, continuously pumping air to enable the plenum chamber, the test chamber A and the test chamber B to reach the ultimate vacuum degree; step 4, after the quadrupole mass spectrometer, the capacitance film vacuum gauge and the magnetic suspension rotor vacuum gauge are stabilized for more than 24 hours, closing the third vacuum valve and the fourth vacuum valve, and respectively carrying out zeroing and residual damping deducting operations on the capacitance film vacuum gauge and the magnetic suspension rotor vacuum gauge; step 5, opening the second vacuum valve, adjusting the first fine-tuning vacuum valve, filling helium into the inflating chamber from the helium bottle, adjusting the air inlet pressure according to the test requirement, and recording the indication value of the corresponding capacitance film vacuum gauge; step 6, recording initial indication values of the magnetic suspension rotor vacuum gauge and initial values of helium partial pressure ion flows of the quadrupole mass spectrometer, adjusting the second fine tuning vacuum valve until the indication values of the magnetic suspension rotor vacuum gauge reach the magnitude of 10 -2 Pa, and recording the indication values of the magnetic suspension rotor vacuum gauge and the quadrupole mass spectrometer at the moment; step 7, calculating helium sensitivity of the quadrupole mass spectrometer according to the data measured in the step 6; step 8, opening the fourth vacuum valve, and re-pumping the test chamber A and the test chamber B to the ultimate vacuum degree; step 9, closing the first vacuum valve and the fourth vacuum valve, and recording the variation of the ion flow of the quadrupole mass spectrometer within 5-180 min; step 10, opening the first vacuum valve, and repeating the step 8; step 11, closing the fourth vacuum valve, recording the initial ion current value of the quadrupole mass spectrometer, and recording the value of the ion current rise of the quadrupole mass spectrometer caused by helium permeation of the glass material to be tested after the time used in the step 9; and step 12, calculating the permeability of the tested glass material. According to the device and the method for testing the helium permeability of the glass material for the quantum vacuum measurement standard, disclosed by the embodiment of the application, a more accurate test pressure indication value is provided for helium permeability test in an in-situ calibration mode, so that the accurate measurement of the helium permeability of the glass material for the quantum vacuum measurement standard is realized, and the problem that the helium permeability characteristic of the glass material for the traditional quantum vacuum measurement standard is difficult to evaluate is solved; according to the embodiment of the application, the helium partial pressure measurement mass spectrometer for testing is calibrated on line by utilizing the good stability of the magnetic suspension rotor vacuum gauge, so that the problem of overlarge helium partial pressure measurement deviation of the mass spectrometer caused by nonideal factors such as poor stability and repeatability is solved, and the uncertainty of measuring the helium permeability of the glass material for the quantum vacuum measurement standard is effectively reduced.
It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory only and are not restrictive of the invention as claimed.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments consistent with the invention and together with the description, serve to explain the principles of the invention.
FIG. 1 is a schematic diagram of a glass material helium permeability test device for quantum vacuum measurement standard according to an embodiment of the present application;
fig. 2 is a schematic flow chart of a method for testing helium permeability of a glass material for quantum vacuum measurement standard according to an embodiment of the present application.
Reference numerals: 1-a first fine tuning vacuum valve; 2-capacitance film vacuum gauge; 3-plenum; 4-a second fine tuning vacuum valve; 5-a magnetic suspension rotor vacuum gauge; 6-a test chamber A; 7-a first vacuum valve; 8-a test chamber B; 9-quadrupole mass spectrometer; 10-helium bottle; 11-a second vacuum valve; 12-a first vacuum air extractor group; 13-a third vacuum valve; a 14-KF interface; 15-glass material to be tested; 16-fourth vacuum valve; 17-a second vacuum air extractor group.
Detailed Description
The following description and the drawings sufficiently illustrate specific embodiments of the invention to enable those skilled in the art to practice them.
It should be understood that the described embodiments are merely some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
When the following description refers to the accompanying drawings, the same numbers in different drawings refer to the same or similar elements, unless otherwise indicated. The implementations described in the following exemplary examples do not represent all implementations consistent with the invention. Rather, they are merely examples of systems and methods that are consistent with aspects of the invention as detailed in the accompanying claims.
In the description of the present invention, it should be understood that the terms "first," "second," and the like are used for descriptive purposes only and are not to be construed as indicating or implying relative importance. The specific meaning of the above terms in the present invention will be understood in specific cases by those of ordinary skill in the art. Furthermore, in the description of the present invention, unless otherwise indicated, "a plurality" means two or more. "and/or", describes an association relationship of an association object, and indicates that there may be three relationships, for example, a and/or B, and may indicate: a exists alone, A and B exist together, and B exists alone. The character "/" generally indicates that the context-dependent object is an "or" relationship.
The following describes in detail a device and a method for testing helium permeability of glass material for quantum vacuum measurement standard according to an embodiment of the present application with reference to fig. 1-fig. 2.
Referring to fig. 1, a schematic structural diagram of a glass material helium permeability testing device for quantum vacuum measurement standard is provided in an embodiment of the present application. As shown in fig. 1, a glass material helium permeability test device for quantum vacuum measurement standard according to an embodiment of the present application may include: the device comprises a first fine tuning vacuum valve 1, a capacitance film vacuum gauge 2, a plenum chamber 3, a second fine tuning vacuum valve 4, a magnetic suspension rotor vacuum gauge 5, a test chamber A6, a first vacuum valve 7, a test chamber B8, a quadrupole mass spectrometer 9, a helium bottle 10, a second vacuum valve 11, a first vacuum pumping unit 12, a third vacuum valve 13, a glass material 15 to be tested, a fourth vacuum valve 16, a KF interface 14 and a second vacuum pumping unit 17, wherein:
the helium bottle 10 is connected with the plenum chamber 3, and the second vacuum valve 11 and the first fine-tuning vacuum valve 1 are sequentially arranged on the connected pipeline;
The plenum chamber 3 is connected with a capacitance film vacuum gauge 2 and a first vacuum air extractor group 12, and a third vacuum valve 13 is arranged on a pipeline connected with the first vacuum air extractor group 12;
the plenum chamber 3 is connected with the test chamber A6, a second fine-tuning vacuum valve 4 is arranged on one connected pipeline, and a KF interface 14 and a glass material 15 to be tested are arranged on the other connected pipeline;
The test chamber A6 is connected with a magnetic suspension rotor vacuum gauge 5;
the test chamber A6 is connected with the test chamber B8, and a first vacuum valve 7 is arranged on a connected pipeline;
The testing chamber B8 is connected with a quadrupole mass spectrometer 9 and a second vacuum air extractor group 17, and a fourth vacuum valve 16 is arranged on a pipeline connected with the second vacuum air extractor group 17;
the test chamber A6 has the same volume and the same material as the test chamber B8.
Specifically, in the embodiment of the application, the glass material 15 to be measured is in a shape of a circular sheet, the diameter range is 30 mm-40 mm, the thickness range is 2 mm-3 mm, and the material adopted in the embodiment of the application is Zerodur, the diameter is 40mm, and the thickness is 2mm; the first vacuum air extractor group 12 and the second vacuum air extractor group 17 are respectively LEYBOLD SC D and LEYBOLD i600; the first vacuum valve 7, the third vacuum valve 13 and the fourth vacuum valve 16 are all VAT 54; PFEIFFER QMG220 and 220 are selected as the quadrupole mass spectrometer 9, and the minimum detectable partial pressure of the quadrupole mass spectrometer 9 is less than or equal to 1 multiplied by 10 -10 Pa; the capacitance film vacuum gauge 2 is INFICON CUBE to 1000Torr, and the accuracy of the measurement of the capacitance film vacuum gauge 2 is within +/-0.15 percent; the magnetic suspension rotor vacuum gauge 5 is selected from MKS SRG-3, and the stability of the magnetic suspension rotor vacuum gauge 5 is less than or equal to 1%/year; the first fine tuning vacuum valve 1 is a VARIAN DN40.
Example 1:
The embodiment of the application provides a flow diagram of a glass material helium permeability test method for a quantum vacuum measurement standard. As shown in fig. 2, the method according to the embodiment of the present application may include the following steps:
Step 1, fixing a glass material 15 to be tested on a KF interface 14;
Step 2, opening a first vacuum air extractor group 12 and a second vacuum air extractor group 17, opening a first vacuum valve 7, a third vacuum valve 13 and a fourth vacuum valve 16, exhausting air from a plenum chamber 3, a test chamber A6, a test chamber B8 and a connecting pipeline, opening a capacitance film vacuum gauge 2 connected to the plenum chamber 3 and a magnetic suspension rotor vacuum gauge 5 connected to the test chamber A6, and opening a quadrupole mass spectrometer 9 when the pressure in the test chamber A6 and the test chamber B8 is pumped to 8.7X10 -3 Pa, wherein the steps further comprise:
The leak detection of the glass material 15 to be detected and the KF interface 14 meets the requirements, and in the embodiment of the application, the detected leak rate is 5.2 multiplied by 10 -12 Pam3/s, which meets the requirements;
Step 3, continuously pumping to enable the plenum chamber 3, the test chamber A6 and the test chamber B8 to reach the ultimate vacuum degree of 1.8x -6 Pa;
Step4, after the quadrupole mass spectrometer 9, the capacitance film vacuum gauge 2 and the magnetic suspension rotor vacuum gauge 5 are stabilized for 28 hours, closing the third vacuum valve 13 and the fourth vacuum valve 16, and respectively carrying out zero setting and residual damping deduction operation on the capacitance film vacuum gauge 2 and the magnetic suspension rotor vacuum gauge 5;
Step 5, opening a second vacuum valve 11, adjusting the first fine-tuning vacuum valve 1, filling helium gas into the plenum chamber 3 through a helium bottle 10, adjusting the inlet pressure according to the test requirement, and recording the indication value of the corresponding capacitance film vacuum gauge 2 as 1.03X10 5 Pa;
Step 6, recording an initial indication value p SRG0=4.5623×10-5 Pa of the magnetic suspension rotor vacuum gauge 5 and an initial value I 0=1.6984×10-13 A of helium partial pressure ion flow of the quadrupole mass spectrometer 9, adjusting the second fine tuning vacuum valve 4 until the indication value p SRG=2.8182×10-2 Pa of the magnetic suspension rotor vacuum gauge 5, and recording indication values I= 6.0862 ×10 -5 A of helium partial pressure ion flow of the quadrupole mass spectrometer 9 and simultaneously recording indication values of the magnetic suspension rotor vacuum gauge 5 and the quadrupole mass spectrometer 9;
Step 7, according to the data measured in the step 6, calculating the helium sensitivity of the quadrupole mass spectrometer 9, wherein in the embodiment of the application, the helium sensitivity S He=2.16×10-3 A/Pa of the quadrupole mass spectrometer 9 is calculated according to a formula ①;
step 8, opening a fourth vacuum valve 16, and re-pumping the test chamber A6 and the test chamber B8 to the limit vacuum degree of 1.9 multiplied by 10 -6 Pa;
Step 9, closing the first vacuum valve 7 and the fourth vacuum valve 16, and recording the variation of the ion flow of the quadrupole mass spectrometer 9 within 5min =2.5367×10-13 A；
Step 10, opening the first vacuum valve 7, and repeating the step 8;
Step 11, closing the fourth vacuum valve 16, recording an initial ion current value I i=1.8225×10-13 A of the quadrupole mass spectrometer 9, and after 5 minutes, recording a magnitude I f=5.5395×10-12 A of the ion current of the quadrupole mass spectrometer 9, which is caused by helium permeation of the glass material to be tested;
In step 12, the permeability of the glass material 15 to be measured is calculated, specifically, according to the formula ②, and k=1.18×10 -15cm2/s is calculated.
Example 2:
the method of the embodiment of the application can comprise the following steps:
Step 1, fixing a glass material 15 to be tested on a KF interface 14;
Step 2, opening a first vacuum air extractor group 12 and a second vacuum air extractor group 17, opening a first vacuum valve 7, a third vacuum valve 13 and a fourth vacuum valve 16, exhausting air from a plenum chamber 3, a test chamber A6, a test chamber B8 and a connecting pipeline, opening a capacitance film vacuum gauge 2 connected to the plenum chamber 3 and a magnetic suspension rotor vacuum gauge 5 connected to the test chamber A6, and opening a quadrupole mass spectrometer 9 when the pressure in the test chamber A6 and the test chamber B8 is pumped to 9.97X10 -3 Pa, wherein the steps further comprise:
The leak detection of the glass material 15 to be detected and the KF interface 14 meets the requirements, and in the embodiment of the application, the detected leak rate is 4.9 multiplied by 10 -12 Pam3/s, and meets the requirements;
Step 3, continuously pumping to enable the plenum chamber 3, the test chamber A6 and the test chamber B8 to reach the ultimate vacuum degree of 1.5 multiplied by 10 -6 Pa;
Step4, after the quadrupole mass spectrometer 9, the capacitance film vacuum gauge 2 and the magnetic suspension rotor vacuum gauge 5 are stabilized for 25 hours, closing the third vacuum valve 13 and the fourth vacuum valve 16, and respectively carrying out zero setting and residual damping deduction operation on the capacitance film vacuum gauge 2 and the magnetic suspension rotor vacuum gauge 5;
Step 5, opening a second vacuum valve 11, adjusting the first fine-tuning vacuum valve 1, filling helium gas into the plenum chamber 3 through a helium bottle 10, adjusting the inlet pressure according to the test requirement, and recording the indication value of the corresponding capacitance film vacuum gauge 2 as 1.03X10 5 Pa;
Step 6, recording an initial indication value p SRG0=4.3461×10-5 Pa of the magnetic suspension rotor vacuum gauge 5 and an initial value I 0=1.5538×10-13 A of helium partial pressure ion flow of the quadrupole mass spectrometer 9, adjusting the second fine tuning vacuum valve 4 until the indication value p SRG=2.7998×10-2 Pa of the magnetic suspension rotor vacuum gauge 5, and recording indication values I= 5.9425 ×10 -5 A of helium partial pressure ion flow of the quadrupole mass spectrometer 9 and simultaneously recording indication values of the magnetic suspension rotor vacuum gauge 5 and the quadrupole mass spectrometer 9;
Step 7, according to the data measured in the step 6, calculating the helium sensitivity of the quadrupole mass spectrometer 9, wherein in the embodiment of the application, the helium sensitivity S He=2.13×10-3 A/Pa of the quadrupole mass spectrometer 9 is calculated according to a formula ①;
Step 8, opening a fourth vacuum valve 16, and re-pumping the test chamber A6 and the test chamber B8 to the limit vacuum degree of 1.6X10 -6 Pa;
Step 9, closing the first vacuum valve 7 and the fourth vacuum valve 16, and recording the variation of the ion flow of the quadrupole mass spectrometer 9 within 180 minutes =9.1283×10-12 A；
Step 10, opening the first vacuum valve 7, and repeating the step 8;
Step 11, closing the fourth vacuum valve 16, recording an initial ion current value I i=1.7133×10-13 A of the quadrupole mass spectrometer 9, and after 180 minutes, recording a magnitude I f=1.9142×10-10 A of the ion current of the quadrupole mass spectrometer 9, which is caused by helium permeation of the glass material to be tested;
in step 12, the permeability of the glass material 15 to be measured is calculated, specifically, according to the formula ②, and k=1.19×10 -15cm2/s is calculated.
The formulas in the above embodiments are as follows:
①
in formula ①: the unit is Pa and the unit is the pressure indication value of the magnetic suspension rotor vacuum gauge 5 The initial pressure indication value of the magnetic suspension rotor vacuum gauge 5 is shown in Pa;/(I)An initial helium ion flow in a unit of a for a quadrupole mass spectrometer 9;/(I)Helium ion flow in a unit of a for a quadrupole mass spectrometer 9;
②
In formula ②: The unit is A for the value of the ion flow after the ion flow rises in the step 11;/(I) The initial ion current value in step 11 is expressed in the unit of A; -The unit is A for the change amount of the test chamber B8 in the step 9 in a period of time; /(I)The volume of the test chamber B8 is m 3; /(I)The unit is m for the thickness of the glass material 15 to be measured; /(I)For a period of time in step 9, in s; a is the area of the glass material 15 to be measured, and the unit is m 2; /(I)Is the pressure of helium in the plenum chamber 3 in Pa.
In the embodiment of the application, the sensitivity of the gas of the quadrupole mass spectrometer 9 is affected by the type of the gas, and the sensitivity is different for different gases, so that the helium sensitivity is calibrated on line in the step 7, experimental errors are reduced, and the accuracy of a measurement result is ensured; in addition, in the embodiment of the application, in the step 9, the helium permeation quantity of the test chamber B8 in the idle state is measured by utilizing the quadrupole mass spectrometer 9, and the characteristics of the test chamber A6 and the test chamber B8 that the volumes are the same and the materials are the same are utilized, so that the helium permeation quantity of the two test chambers is subtracted when the permeation rate of the glass material 15 to be measured is calculated, the influence of the helium attached to the test chambers on experimental results is eliminated, and the accuracy of the measurement results is ensured.
The foregoing embodiment numbers of the present application are merely for the purpose of description, and do not represent the advantages or disadvantages of the embodiments.
The foregoing disclosure is illustrative of the present application and is not to be construed as limiting the scope of the application, which is defined by the appended claims.
Claims (7)
1. A glass material helium permeability testing device for quantum vacuum measurement standard, which is characterized by comprising: the device comprises a first fine tuning vacuum valve, a capacitance film vacuum gauge, a plenum chamber, a second fine tuning vacuum valve, a magnetic suspension rotor vacuum gauge, a test chamber A, a first vacuum valve, a test chamber B, a quadrupole mass spectrometer, a helium bottle, a second vacuum valve, a first vacuum air extractor group, a third vacuum valve, a glass material to be tested, a fourth vacuum valve, a KF interface and a second vacuum air extractor group, wherein:
the helium bottle is connected with the plenum chamber, and the second vacuum valve and the first fine-tuning vacuum valve are sequentially arranged on a connected pipeline;
The plenum chamber is connected with the capacitance film vacuum gauge and the first vacuum air extractor group, and the pipeline connected with the first vacuum air extractor group is provided with the third vacuum valve;
The plenum chamber is connected with the test chamber A, a second fine-tuning vacuum valve is arranged on one connected pipeline, and the KF interface and the glass material to be tested are arranged on the other connected pipeline;
the test chamber A is connected with the magnetic suspension rotor vacuum gauge;
The test chamber A is connected with the test chamber B, and the first vacuum valve is arranged on a connected pipeline;
the testing chamber B is connected with the quadrupole mass spectrometer and the second vacuum air extractor group, and a pipeline connected with the second vacuum air extractor group is provided with the fourth vacuum valve;
the volume of the test chamber A is the same as that of the test chamber B, and the materials are the same.
2. The device for testing helium permeability of glass materials for quantum vacuum measurement standards according to claim 1, wherein the glass materials to be tested are in a round sheet shape, the diameter range is 30 mm-40 mm, and the thickness range is 2 mm-3 mm.
3. The device for testing helium permeability of glass materials for quantum vacuum measurement standards according to claim 1, wherein the minimum detectable partial pressure of the quadrupole mass spectrometer is 1 x 10 -10 Pa or less.
4. The device for testing helium permeability of glass materials for quantum vacuum measurement standards according to claim 1, wherein the accuracy of measurement of the capacitance film vacuum gauge is within +/-0.15%.
5. The device for testing helium permeability of glass materials for quantum vacuum measurement standards according to claim 1, wherein the stability of the magnetic suspension rotor vacuum gauge is less than or equal to 1%/year.
6. A method for testing helium permeability of glass material for quantum vacuum measurement standard, characterized in that the device for testing helium permeability of glass material for quantum vacuum measurement standard according to any one of claims 1 to 5 comprises:
Step 1, fixing the tested glass material on the KF interface;
Step 2, starting the first vacuum air extractor group and the second vacuum air extractor group, opening the first vacuum valve, the third vacuum valve and the fourth vacuum valve, exhausting the plenum chamber, the test chamber A, the test chamber B and the connecting pipeline, opening the capacitance film vacuum gauge connected with the plenum chamber and the magnetic suspension rotor vacuum gauge connected with the test chamber A, and opening the quadrupole mass spectrometer when the pressure in the test chamber A and the test chamber B is lower than 10 -2 Pa;
Step 3, continuously pumping air to enable the plenum chamber, the test chamber A and the test chamber B to reach the ultimate vacuum degree;
Step 4, after the quadrupole mass spectrometer, the capacitance film vacuum gauge and the magnetic suspension rotor vacuum gauge are stabilized for more than 24 hours, closing the third vacuum valve and the fourth vacuum valve, and respectively carrying out zeroing and residual damping deducting operations on the capacitance film vacuum gauge and the magnetic suspension rotor vacuum gauge;
Step 5, opening the second vacuum valve, adjusting the first fine-tuning vacuum valve, filling helium into the inflating chamber from the helium bottle, adjusting the air inlet pressure according to the test requirement, and recording the indication value of the corresponding capacitance film vacuum gauge;
Step 6, recording initial indication values of the magnetic suspension rotor vacuum gauge and initial values of helium partial pressure ion flows of the quadrupole mass spectrometer, adjusting the second fine tuning vacuum valve until the indication values of the magnetic suspension rotor vacuum gauge reach the magnitude of 10 -2 Pa, and recording the indication values of the magnetic suspension rotor vacuum gauge and the quadrupole mass spectrometer at the moment;
Step 7, calculating helium sensitivity of the quadrupole mass spectrometer according to the data measured in the step 6;
step 8, opening the fourth vacuum valve, and re-pumping the test chamber A and the test chamber B to the ultimate vacuum degree;
Step 9, closing the first vacuum valve and the fourth vacuum valve, and recording the variation of the ion flow of the quadrupole mass spectrometer within 5-180 min;
step 10, opening the first vacuum valve, and repeating the step 8;
Step 11, closing the fourth vacuum valve, recording the initial ion current value of the quadrupole mass spectrometer, and recording the value of the ion current rise of the quadrupole mass spectrometer caused by helium permeation of the glass material to be tested after the time used in the step 9;
And step 12, calculating the permeability of the tested glass material.
7. The method for testing helium permeability of glass materials for quantum vacuum measurement standards according to claim 6, further comprising, before step 2: and carrying out leak detection on the tested glass material and the KF interface to ensure that the leak detection meets the requirements.
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