CN101451943B - Quartz crystal microbalance accuracy verification test system - Google Patents
Quartz crystal microbalance accuracy verification test system Download PDFInfo
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- CN101451943B CN101451943B CN2007101951964A CN200710195196A CN101451943B CN 101451943 B CN101451943 B CN 101451943B CN 2007101951964 A CN2007101951964 A CN 2007101951964A CN 200710195196 A CN200710195196 A CN 200710195196A CN 101451943 B CN101451943 B CN 101451943B
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- electronic balance
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- 238000003380 quartz crystal microbalance Methods 0.000 title claims abstract description 31
- 238000012360 testing method Methods 0.000 title claims abstract description 27
- 238000012795 verification Methods 0.000 title description 10
- 238000005303 weighing Methods 0.000 claims abstract description 34
- 238000005259 measurement Methods 0.000 claims abstract description 26
- 238000012546 transfer Methods 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 5
- 230000008021 deposition Effects 0.000 claims description 32
- 238000007689 inspection Methods 0.000 claims description 20
- 238000011065 in-situ storage Methods 0.000 claims description 15
- 239000007789 gas Substances 0.000 claims description 14
- 230000005540 biological transmission Effects 0.000 claims description 4
- 238000007872 degassing Methods 0.000 claims description 3
- 238000009792 diffusion process Methods 0.000 claims description 2
- 238000000790 scattering method Methods 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 238000011161 development Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 230000008020 evaporation Effects 0.000 description 4
- 238000001704 evaporation Methods 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000010943 off-gassing Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
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Abstract
The invention relates to a quartz crystal microbalance measuring accuracy testing device, comprising a vent chamber situ real-time weighing system, a deflation object cosine quantitation scattering system, an angle factor verifying system, wherein the vent chamber situ real-time weighing system realizes real-time measurement on quality variation of the deflation object, with measured value reaching national quality measurement norm through a gauged electronic balance; the deflation object cosine quantitation scattering system transfers gauged quality in an order of magnitude 10<-4> to gauged quality area density in an order of magnitude 10<-7> g/cm<2> on the surface of the quartz crystal microbalance through a quantitation scattering method, realizes quantitation loading of the quartz crystal microbalance, and the measurement accuracy of the loading quantity reaches quality norm of the superior and national measurement system; the angle factor verifying system is used for verifying accuracy of the angle factor of the scattering system, ensures that the whole quality transferring process is controllable. The inventive accuracy testing system has high testing accuracy, uncertainty precedes 40%, real-time direct weighing in vacuum of the deflation object is adopted, thereby realizing accurate measurement of deflation speed.
Description
Technical Field
The invention relates to a quartz crystal microbalance accuracy verification test system, and belongs to the technical field of material outgassing pollution tests.
Background
In the production process of the spacecraft, the pollution test of the quartz crystal microbalance is a main means for measuring the environmental pollution condition of the spacecraft development. The quartz crystal microbalance is applied to various stages of spacecraft development, and is applied to environmental pollution measurement in the stages of spacecraft part development and test, spacecraft assembly test, spacecraft thermal test and mechanical test, so that effective pollution control measures are provided, and development of the spacecraft is ensured to meet the requirement of pollution control.
However, the existing verification and calibration test device and verification standard of the quartz crystal microbalance are lacked in China, and the measurement accuracy of the quartz crystal microbalance cannot be traced back to a national metrological verification system, so that the reliability of the measurement result of the quartz crystal microbalance is influenced. The requirements of long service life and high reliability of the spacecraft cannot be met. At present, no relevant manufacturers carry out research and development in the aspect at home. In foreign countries, the American Lockheed Palo Alto Research Laboratories developed an accuracy analysis test device of a commercial quartz crystal microbalance, which adopts the saturated vapor pressure parameter of water to obtain the evaporation rate of water under a certain environment according to the thermodynamic characteristics of water; and obtaining the mass rate reaching the surface of the quartz crystal microbalance according to the scattering and transmission theory under the molecular vacuum. These quartz crystal microbalances were controlled at liquid nitrogen temperature. The water molecules that reach the balance surface are substantially completely absorbed. The measurement accuracy of a quartz crystal microbalance is traced back to the accuracy of the evaporation rate of water in a certain environment. Because the evaporation rate of water is influenced by multiple factors of the environment, especially the instability of the heat conduction rate seriously influences the accuracy of the evaporation rate of water, the foreign accuracy analysis test device can not realize higher accuracy, and the uncertainty of measurement is more than 80%.
Therefore, it is necessary to develop a high-accuracy quartz crystal microbalance accuracy verification test system.
Disclosure of Invention
The invention aims to provide a quartz crystal microbalance measurement accuracy test system which has higher accuracy and can trace back to the national quality measurement standard.
The technical scheme of the invention is as follows: the quartz crystal microbalance measurement accuracy test system comprises an air release chamber in-situ real-time weighing system, an air release object cosine quantitative scattering system and an angle coefficient inspection system; the in-situ real-time weighing system of the air release chamber realizes the real-time measurement of the quality change of the air release, and the measured value is traced back to the national quality measurement standard through a calibrated electronic balance; bleed cosine quantitative scattering system 10 by quantitative scattering method-4Quantitative mass transfer of the order of g to the surface of a quartz crystal microbalance 10-7g/cm2The quantitative mass surface density of the order of magnitude realizes the quantitative loading of the quartz crystal microbalance, and the measuring accuracy of the loading amount can be traced back to the mass standard of the superior and national measuring systems; and the angle coefficient inspection system is used for verifying the accuracy of the angle coefficient of the scattering system and ensuring the control of the whole mass transfer process.
In the system, the in-situ real-time weighing system of the air release chamber comprises a calibrated electronic balance, an electronic balance loading and unloading device, the air release chamber and an air release chamber temperature control device. The calibrated electronic balance directly weighs the air discharge chamber in real time, and the electronic balance loading and unloading device realizes zero resetting of the calibrated electronic balance to ensure weighing accuracy. The air discharge chamber temperature control device performs non-contact temperature control on the air discharge chamber, and the mass value of the air discharge chamber is transmitted to the mass value of the air discharge object, so that the mass value transmission is realized.
In the system, the gas discharge object cosine quantitative scattering system comprises a gas discharge object, a scattering device and a deposition surface. The gas released by the outgasser passes through the scattering system to the deposition surface. The air discharge chamber in-situ real-time weighing system is used for transmitting the mass value of the air discharge rate of the air discharge object, and the scattering device is used for converting the mass value into a mass surface density value on the deposition surface. The accuracy of the mass surface density value can be traced upwards to the national mass measurement benchmark.
In the system, the angular coefficient inspection system comprises a calibrated electronic balance, an electronic balance loading and unloading device and a deposition amount inspection plate. The calibrated electronic balance directly weighs the deposition amount inspection plate in real time,the electronic balance loading and unloading device realizes zero resetting of the calibrated electronic balance and ensures the weighing accuracy. The deposition amount inspection plate receives deposition with the mass surface density which is the same as that of the deposition surface in the outgassing object cosine quantitative scattering system, and the mass surface density is weighed by an electronic balance, so that the scattering system can be accurately verified. The deposition amount of the deposition amount check plate is made larger than 10 by increasing the amount of the outgas-4And g, meeting the requirement of the calibrated electronic balance on the weighing range.
Wherein, the electronic balance in the in-situ real-time weighing system of the air release chamber and the electronic balance weighing resolution of the loading and unloading device thereof are 10-5g。
Furthermore, the quality of 1/1000 can be equally divided by the cosine diffusion mode adopted by the outgasse cosine quantitative scattering system.
Compared with the prior art, the invention has the following advantages:
(1) the mass transfer process of the invention is completely controlled, the gas release chamber in-situ real-time weighing system transfers the accuracy of national mass reference to the accuracy of gas release rate, and the gas release object cosine quantitative scattering system and the angular coefficient inspection system transfer the accuracy of gas release rate to the measurement value of the quartz crystal microbalance.
(2) The invention has high test precision, the uncertainty is better than 40%, and the accurate measurement of the deflation rate is realized by adopting real-time direct weighing of the deflation object under vacuum.
Drawings
FIG. 1 is a functional block diagram of the present invention;
FIG. 2 is a block diagram of the in-situ real-time weighing system of the degassing chamber of the present invention;
FIG. 3 is a block diagram of an outgassed cosine quantitative scattering system of the present invention;
FIG. 4 is a block diagram of an angular coefficient checking system of the present invention;
FIG. 5 is a flow chart of the test of the present invention.
Detailed Description
As shown in figure 1, an air discharge chamber in-situ real-time weighing system 1 of a quartz crystal microbalance measurement accuracy test system provides a quantitative value of the air discharge rate of an air discharge object for an air discharge object cosine quantitative scattering system 2, the accuracy of the quantitative value can be traced back to the national mass measurement standard, and the air discharge object cosine quantitative scattering system 2 measures 10-4Conversion of the g-quality value to 10-7g/cm2The mass surface density value is provided for the quartz crystal microbalance 4 to be tested, and the quantitative mass loading on the surface of the quartz crystal microbalance is realized; the angular coefficient inspection system 3 inspects the accuracy of converting the mass value into the mass surface density value in the gas discharge cosine quantitative scattering system 2, and the accuracy can be traced back to the national mass measurement standard.
As shown in fig. 2, the in-situ real-time weighing system 1 of the air release chamber of the invention comprises a calibrated electronic balance 11, an electronic balance loading and unloading device 12, an air release chamber 13 and an air release chamber temperature control device 14. The calibrated electronic balance 11 directly weighs the air discharge chamber 13 in real time, and the electronic balance loading and unloading device 12 realizes zero resetting of the calibrated electronic balance 11 to ensure weighing accuracy. The air-release-chamber temperature control device 14 performs non-contact temperature control of the air release chamber 13, and the mass value of the air release chamber 13 is transmitted to the mass value of the air release object 21, thereby realizing mass value transmission.
As shown in FIG. 3, the system 2 for quantitatively scattering outgassed cosine of the present invention comprises an outgassed 21, a scattering device 22, and a deposition surface 23. The gas released by the outgas 21 passes through the scattering means 22 to the deposition surface 23. The mass value of the bleed rate of the bleed 21 is transmitted by the bleed chamber 13 in the bleed chamber in-situ real-time weighing system 1, and the scattering device 22 converts the mass value into a mass areal density value on the deposition surface 23. The accuracy of the mass surface density value can be traced upwards to the national mass metering standard.
As shown in fig. 4, the angular coefficient inspection system 3 of the present invention includes a calibrated electronic balance 31, an electronic balance loading and unloading device 32, and a deposition amount inspection plate 33. The calibrated electronic balance 31 directly weighs the deposition amount inspection plate 33 in real time, and the electronic balance loading and unloading device 32 realizes zero resetting of the calibrated electronic balance 31 to ensure weighing accuracy. The deposition amount check plate 33 receives deposition with the same mass area density as the deposition surface 23 in the outgassed cosine quantitative scattering system 2, and the mass area density is weighed by the electronic balance 31, so that the accurate verification of the scattering system is realized. The deposition amount check plate 33 is deposited more than 10 by increasing the amount of the off-gas-4And g, meeting the requirement of the calibrated weighing range of the electronic balance 31.
As shown in fig. 5, in the test procedure of the present invention, an angular coefficient verification test or a quartz balance accuracy verification test is first selected. Installing a deposition amount inspection plate or a quartz crystal microbalance according to test requirements, installing an outgas material, weighing an initial value of the outgas, simultaneously weighing the deposition amount inspection plate or recording an initial value of the frequency of the quartz crystal microbalance, starting an outgas scattering test process, weighing the outgas again after the test is finished, and simultaneously weighing the deposition amount inspection plate again or recording a final value of the frequency of the quartz crystal microbalance. And determining the angle coefficient and the accuracy of the quartz crystal microbalance according to the weighing and recording results.
Although particular embodiments of the present invention have been described and illustrated in detail, it should be noted that various changes and modifications could be made to the above-described embodiments without departing from the spirit of the invention and the scope of the appended claims.
Claims (6)
1. The quartz crystal microbalance measurement accuracy test system comprises an air release chamber in-situ real-time weighing system (1), an air release object cosine quantitative scattering system (2) and an angle coefficient inspection system (3); wherein,
the in-situ real-time weighing system (1) of the air release chamber is characterized by comprising an electronic balance (11), an electronic balance loading and unloading device (12), an air release chamber (13) and an air release chamber temperature control device (14) which are calibrated; the electronic balance (11) directly weighs the air release chamber (13) in real time, and the electronic balance loading and unloading device (12) realizes zero resetting of the electronic balance (11) to ensure weighing accuracy; the air discharge chamber temperature control device (14) performs non-contact temperature control on an air discharge chamber (13), and the mass value of the air discharge chamber (13) is transmitted to the mass value of the air discharge object (21) to realize mass value transmission;
the gas discharge object cosine quantitative scattering system (2) comprises a gas discharge object (21), a scattering device (12) and a deposition surface (13); the gases released by the outgas (21) pass through a scattering system (22) to reach the deposition surface (23); -mass quantity transfer of the rate of deflation of the outgassed (21) by the deflation chamber (13) of the in situ real-time deflation system (1), the scattering device (12) converting the mass value into a mass areal density value on the deposition surface (23); the accuracy of the mass surface density value can be traced back to the national mass measurement standard;
the angular coefficient inspection system (3) comprises an electronic balance (31) which is calibrated, an electronic balance loading and unloading device (32) and a deposition amount inspection plate (33); the electronic balance (31) directly weighs the deposition amount inspection plate (33) in real time, and the electronic balance loading and unloading device (32) realizes zero resetting of the calibrated electronic balance (11) to ensure weighing accuracy; the deposition amount inspection plate (33) receives deposition with the same mass surface density as that of a deposition surface (23) in the outgassed cosine quantitative scattering system (2), and the mass surface density is weighed by an electronic balance (31), so that the scattering system can be accurately verified; the deposition amount of the deposition amount check plate (33) is made larger than 10 by increasing the amount of the off-gas-4And g, meeting the weighing range requirement of the calibrated electronic balance (31).
2. The system according to claim 1, characterized in that the in-situ real-time weighing system (1) of the degassing chamber enables real-time measurement of the quality variation of the degassing gas, the measurement values of which are traced back to the national quality measurement reference by means of a calibrated electronic balance.
3. The system according to claim 1, wherein the outgassed cosine quantitative scattering system (2) scatters 10 by a quantitative scattering method-4Quantitative mass transfer of the order of g to the surface of a quartz crystal microbalance 10-7g/cm2Quantitative quality of order of magnitudeThe surface density is measured, the quantitative loading of the quartz crystal microbalance is realized, and the accuracy of measuring the loading amount can be traced back to the quality standard of superior and national measuring systems.
4. The system according to claim 1, characterized by said angular coefficient inspection system (3) for verifying the accuracy of the angular coefficient of the scattering system, ensuring the control of the whole mass transfer process.
5. The system according to any one of claims 1-4, wherein: the electronic balance (11) in the in-situ real-time gas release chamber weighing system (1) and the electronic balance weighing resolution of the loading and unloading device (12) of the electronic balance are 10-5g。
6. The system according to any one of claims 1-4, wherein: the bleed matter cosine quantitative scattering system adopts a cosine diffusion mode, and mass equal division of 1/1000 can be realized.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2007101951964A CN101451943B (en) | 2007-12-04 | 2007-12-04 | Quartz crystal microbalance accuracy verification test system |
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| CN2007101951964A CN101451943B (en) | 2007-12-04 | 2007-12-04 | Quartz crystal microbalance accuracy verification test system |
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| CN101451943A CN101451943A (en) | 2009-06-10 |
| CN101451943B true CN101451943B (en) | 2011-02-16 |
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| CN2007101951964A Expired - Fee Related CN101451943B (en) | 2007-12-04 | 2007-12-04 | Quartz crystal microbalance accuracy verification test system |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102455211B (en) * | 2010-10-20 | 2014-01-01 | 北京卫星环境工程研究所 | Performance testing system for quartz crystal microbalance (QCM) |
| CN104237057A (en) * | 2014-09-05 | 2014-12-24 | 兰州空间技术物理研究所 | Characteristic testing method of condensable and volatile matters in non-metal material in vacuum |
| CN104237142B (en) * | 2014-09-29 | 2016-09-14 | 北京卫星环境工程研究所 | Material outgassing is to optical transmittance impact analysis pilot system |
| CN107677563A (en) * | 2017-10-11 | 2018-02-09 | 北京航空航天大学 | Quartz crystal temperature probe, quartz crystal microbalance and its application method |
Citations (2)
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|---|---|---|---|---|
| CN2549444Y (en) * | 2002-05-10 | 2003-05-07 | 武汉大学 | Quatrz micro-balance analyzer |
| CN1646902A (en) * | 2002-04-22 | 2005-07-27 | 纳尔科公司 | Measuring deposit forming capacity with microbalance |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1646902A (en) * | 2002-04-22 | 2005-07-27 | 纳尔科公司 | Measuring deposit forming capacity with microbalance |
| CN2549444Y (en) * | 2002-05-10 | 2003-05-07 | 武汉大学 | Quatrz micro-balance analyzer |
Non-Patent Citations (5)
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| JP特开2004-184256A 2004.07.02 |
| 杨东升等.低温石英天平在材料放气污染特性测试中的应用.《航天器环境工程》.2005,第22卷(第5期),300-303. * |
| 杨昭毅.质量量值传递原理是校准砝码的基本依据.《北京师范学院学报(自然科学版)》.1989,第10卷(第2期),76,77. * |
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