CN102980832A - System and method for in-situ monitoring of quality loss of non-metallic material in vacuum - Google Patents
System and method for in-situ monitoring of quality loss of non-metallic material in vacuum Download PDFInfo
- Publication number
- CN102980832A CN102980832A CN2012104699590A CN201210469959A CN102980832A CN 102980832 A CN102980832 A CN 102980832A CN 2012104699590 A CN2012104699590 A CN 2012104699590A CN 201210469959 A CN201210469959 A CN 201210469959A CN 102980832 A CN102980832 A CN 102980832A
- Authority
- CN
- China
- Prior art keywords
- vacuum chamber
- sample
- quartz crystal
- crystal microbalance
- temperature
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 238000000034 method Methods 0.000 title claims abstract description 19
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 17
- 238000012544 monitoring process Methods 0.000 title claims abstract description 16
- 239000007769 metal material Substances 0.000 title claims abstract 7
- 238000003380 quartz crystal microbalance Methods 0.000 claims abstract description 35
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 10
- 239000007789 gas Substances 0.000 claims abstract description 3
- 238000000605 extraction Methods 0.000 claims abstract 3
- 238000005086 pumping Methods 0.000 claims abstract 2
- 238000005303 weighing Methods 0.000 claims abstract 2
- 238000001816 cooling Methods 0.000 claims 4
- 239000000463 material Substances 0.000 abstract description 17
- 238000012360 testing method Methods 0.000 abstract description 12
- 238000005259 measurement Methods 0.000 abstract description 2
- 229910052582 BN Inorganic materials 0.000 description 3
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 3
- 230000035945 sensitivity Effects 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 238000012806 monitoring device Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000009877 rendering Methods 0.000 description 1
Images
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
- Investigating Or Analyzing Materials Using Thermal Means (AREA)
Abstract
本发明涉及一种真空中非金属材料质量损失的原位监测系统及方法，属于材料特性测试领域。所述系统包括主真空室、连杆、抽气装置、副真空室、高真空插板阀、样品舟、石英晶体微量天平、低温冷沉；所述方法包括设定低温冷沉和石英晶体微量天平的温度，向副真空室内通入氮气；将试样称重后放入样品舟中，将样品舟装入副真空室后关闭副真空室，切断氮气开启抽气装置；将样品舟移入主真空室中石英晶体微量天平的正下方，关闭高真空插板阀；将试样加热至试样的出气温度，每隔设定时间记录一次石英晶体微量天平的频率变化Δf和温度T；计算试样的总质量损失。所述方法提高了测量精度，有效避免了装卸样品时大气对测试系统的影响。
The invention relates to an in-situ monitoring system and method for mass loss of non-metallic materials in vacuum, belonging to the field of material characteristic testing. The system includes a main vacuum chamber, a connecting rod, an air extraction device, a secondary vacuum chamber, a high vacuum plug valve, a sample boat, a quartz crystal microbalance, and a cryogenic cold sink; the method includes setting a low temperature cold sink and a quartz crystal micro balance. To adjust the temperature of the balance, feed nitrogen into the auxiliary vacuum chamber; put the sample into the sample boat after weighing, put the sample boat into the auxiliary vacuum chamber, close the auxiliary vacuum chamber, cut off the nitrogen and open the pumping device; move the sample boat into the main vacuum chamber. Directly below the quartz crystal microbalance in the vacuum chamber, close the high-vacuum plug-in valve; heat the sample to the gas outlet temperature of the sample, and record the frequency change Δf and temperature T of the quartz crystal microbalance every set time; calculate the test The total mass loss of the sample. The method improves the measurement accuracy and effectively avoids the influence of the atmosphere on the test system when loading and unloading samples.
Description
Technical field
The present invention relates to the in-situ monitoring system and method for nonmetallic materials mass loss in a kind of vacuum, belong to the material behavior field tests.
Background technology
Nonmetallic materials such as organic, polymerization, inorganic material meeting volatilization gas under vacuum condition, thereby cause mass loss.The mass loss rate of nonmetallic materials is important performances of material, is one of foundation of selecting of space material.And existing home position testing method utilizes Cann type vacuum microbalance, and measuring sensitivity only is 10
-5G can't satisfy present request for utilization.And need to adopt non-contacting heating and temp measuring method, sample temperature control only can control to ± and 2.5 ℃.Therefore the in-situ monitoring system and the corresponding monitoring method that need nonmetallic materials mass loss in a kind of vacuum overcome the existing low deficiency of home position testing method measuring accuracy, improve the accuracy of temperature control of specimen.
Summary of the invention
The invention provides the in-situ monitoring system and method for nonmetallic materials mass loss in a kind of vacuum, can overcome the existing low deficiency of home position testing method measuring accuracy, improve the accuracy of temperature control of specimen.
For achieving the above object, technical scheme of the present invention is as follows:
The in-situ monitoring system of nonmetallic materials mass loss in a kind of vacuum, described system comprises: main vacuum chamber, connecting rod, air extractor, secondary vacuum chamber, high vacuum push-pull valve, example boat, quartz crystal microbalance, low temperature cold sink;
Wherein, main vacuum chamber is cylindrical structure; At the top of main vacuum chamber's inwall with to be respectively equipped with low temperature cold heavy in the position all around, quartz crystal microbalance be fixed on the low temperature cold at main vacuum chamber top heavy on; Example boat is placed on the main vacuum chamber bottom surface, and is staggered relatively with quartz crystal microbalance;
Be connected with the high vacuum push-pull valve by pipeline between main vacuum chamber and the secondary vacuum chamber;
Connecting rod communicates with main vacuum chamber and high vacuum push-pull valve; Connecting rod one end is positioned at secondary vacuum chamber, and the other end exposes secondary vacuum chamber, and the length of connecting rod is greater than the distance of example boat to secondary vacuum chamber; Described example boat, high vacuum push-pull valve, connecting rod are positioned on the straight line;
Air extractor respectively with main vacuum chamber be connected vacuum chamber and be connected;
The in-situ monitoring method of nonmetallic materials mass loss in a kind of vacuum, described method step is as follows:
Step 1, the quartz crystal microbalance temperature is made as≤-180 ℃, sets the temperature of the heavy temperature≤quartz crystal microbalance of low temperature cold, in secondary vacuum chamber, pass into nitrogen;
Step 2, put into example boat after sample weighed, example boat is packed into close secondary vacuum chamber behind the secondary vacuum chamber, cut off nitrogen, open air extractor, the pressure to the main vacuum chamber≤7 * 10
-3Pressure in the Pa, secondary vacuum chamber≤5 * 10
-3Pa;
Step 3, open the high vacuum push-pull valve, promote connecting rod, with example boat move into quartz crystal microbalance in the main vacuum chamber under, close the high vacuum push-pull valve;
Step 4, sample is heated to the air outlet temperature of sample, every frequency change Δ f and the temperature T of a quartz crystal microbalance of setting-up time record;
The total mass loss of step 5, calculating sample.
After reaching predetermined test duration, open the high vacuum push-pull valve, and example boat is moved to secondary vacuum chamber; In secondary vacuum chamber, pass into the dry nitrogen of cleaning, when the example boat temperature is cooled to below 35 ℃, take out example boat.
Wherein, described sample is nonmetallic materials;
Preferably with sample at 25.0 ℃ ± 5.0 ℃, relative humidity is after placing more than 24 hours under 20% ~ 60% the environment, to carry out step 1;
In the preferred steps three, the venthole of example boat is positioned on the axis of quartz crystal microbalance;
In the preferred steps four, every frequency change Δ f and the temperature T of 10s ~ quartz crystal microbalance of 10min record;
Beneficial effect
1. the invention provides in-situ monitoring device and the method for nonmetallic materials mass loss in a kind of vacuum, described device adopts quartz crystal microbalance, will measure sensitivity and bring up to 10
-9G/Hz has improved measuring accuracy;
2. described device adopts the dual-vacuum chamber setting, and atmosphere is on the impact of test macro when effectively having avoided the loading and unloading sample;
3. at main vacuum chamber's inwall low temperature cold to be set heavy for described device, can avoid the outer molecule of giving vent to anger of quartz crystal microbalance angular field of view to condense in its surface through the reflection of vacuum chamber inwall, thus the measuring error that causes.
Description of drawings
Fig. 1 is the structural representation of the in-situ monitoring device of nonmetallic materials mass loss in the vacuum of the present invention.
Fig. 2 is among the embodiment, the relation curve of boron nitride amount loss rate and test duration.
Wherein, 1-main vacuum chamber, 2-connecting rod, 3-air extractor, the secondary vacuum chamber of 4-, 5-high vacuum push-pull valve, 6-example boat, 7-quartz crystal microbalance, 8-low temperature cold sink.
Embodiment
Embodiment
The in-situ monitoring system of nonmetallic materials mass loss in the vacuum as shown in Figure 1, described system comprises: main vacuum chamber 1, connecting rod 2, air extractor 3, secondary vacuum chamber 4, high vacuum push-pull valve 5, example boat 6, quartz crystal microbalance 7, low temperature cold heavy 8;
Wherein, main vacuum chamber 1 is cylindrical structure; At the top of main vacuum chamber's 1 inwall with to be respectively equipped with low temperature cold heavy 8 in the position all around, quartz crystal microbalance 7 is fixed on the low temperature cold heavy 8 at main vacuum chamber 1 top; Example boat 6 is placed on main vacuum chamber 1 bottom surface, and is staggered relatively with quartz crystal microbalance 7;
Are connected connection with the high vacuum push-pull valve by pipeline between main vacuum chamber 1 and the secondary vacuum chamber 4;
Connecting rod 2 communicates with main vacuum chamber 1 and high vacuum push-pull valve 5; Connecting rod 2 one ends are positioned at secondary vacuum chamber 4, and the other end exposes secondary vacuum chamber 4, and the length of connecting rod 2 is greater than the distance of example boat 6 to secondary vacuum chamber 4; Described example boat 6, high vacuum push-pull valve 5, connecting rod 2 are positioned on the straight line;
Air extractor 3 respectively with main vacuum chamber 1 be connected vacuum chamber 4 and be connected.
With the in-situ monitoring of described system for the mass loss of vacuum nonmetallic materials, described method step is as follows:
Step 1, choosing boron nitride coating 10g, put into climatic chamber after the sample preparation, is 23.0 ℃ ± 2.0 ℃ in temperature, and relative humidity is under 45% ~ 55% the condition, to place 24 hours; Quartz crystal microbalance 7 temperature are made as-183 ℃, and the temperature of setting low temperature cold heavy 8 is-183 ℃, passes into nitrogen in secondary vacuum chamber 4;
Step 2, after 0.1g ~ the 0.3g sample is weighed, put into example boat 6; With the example boat 6 secondary vacuum chamber 4 of packing into, close secondary vacuum chamber, cut off nitrogen, open air extractor 3, main vacuum chamber 1 is evacuated to 7 * 10
-3Pa, secondary vacuum chamber 4 is evacuated to 5 * 10
-3Pa;
Step 3, unlatching high vacuum push-pull valve 5; Promote connecting rod 2, with example boat 6 move into quartz crystal microbalance 7 in the main vacuum chamber 1 under, the venthole of example boat 6 is positioned on the axis of quartz crystal microbalance 7, is 150mm apart from the distance of quartz crystal microbalance 7 sensing surfaces; Close high vacuum push-pull valve 5;
Step 4, sample is heated to 125 ℃ of the air outlet temperatures of sample, every frequency change Δ f and the temperature T of a quartz crystal microbalance 7 of 5min record;
The total mass loss m of step 5, calculating sample
t, computing method are as follows:
m
t1＝F·Ks·Δf
In the formula:
Ks---the used mass measurement sensitivity of quartz crystal microbalance 7 under adiabatic condensation temperature, unit is g/cm
2Hz;
The viewing factor of 7 pairs of ventholes of F---quartz crystal microbalance, under geometric relationship of the present invention, F=353.50cm
2
Calculate the mass loss of sample boron nitride under different time, and divided by its initial mass, obtain mass loss rate, the relation curve of rendering quality loss percentage and test duration, as shown in Figure 2.
After reaching predetermined test duration, open high vacuum push-pull valve 5, and example boat 6 is moved to secondary vacuum chamber 4; In secondary vacuum chamber 4, pass into the dry nitrogen of cleaning, when example boat 6 temperature are cooled to below 35 ℃, take out example boat 6.
In sum, more than be preferred embodiment of the present invention only, be not for limiting protection scope of the present invention.Within the spirit and principles in the present invention all, any modification of doing, be equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (5)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210469959.0A CN102980832B (en) | 2012-11-20 | 2012-11-20 | System and method for in-situ monitoring of quality loss of non-metallic material in vacuum |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210469959.0A CN102980832B (en) | 2012-11-20 | 2012-11-20 | System and method for in-situ monitoring of quality loss of non-metallic material in vacuum |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102980832A true CN102980832A (en) | 2013-03-20 |
| CN102980832B CN102980832B (en) | 2014-11-05 |
Family
ID=47855054
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210469959.0A Active CN102980832B (en) | 2012-11-20 | 2012-11-20 | System and method for in-situ monitoring of quality loss of non-metallic material in vacuum |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102980832B (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104215598A (en) * | 2014-09-30 | 2014-12-17 | 北京卫星环境工程研究所 | On-line Infrared Absorption Spectrum Detection System for Outgassing Components of Spacecraft Materials |
| 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 |
| CN109828300A (en) * | 2019-01-31 | 2019-05-31 | 兰州空间技术物理研究所 | A kind of miniaturization omnidirectional particles detection |
| CN109917080A (en) * | 2019-04-12 | 2019-06-21 | 中国科学院上海技术物理研究所 | A vacuum pollution prevention and control test system for precision optical instruments |
| CN113237789A (en) * | 2021-05-12 | 2021-08-10 | 雅安百图高新材料股份有限公司 | Method for detecting content of organic modifier on surface of alumina powder |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3863495A (en) * | 1973-04-16 | 1975-02-04 | Exxon Research Engineering Co | Quartz crystal solute mass detector |
| CN101776557A (en) * | 2009-12-17 | 2010-07-14 | 中国航天科技集团公司第五研究院第五一○研究所 | Device for testing grease evaporation rate in vacuum environment |
| CN101876612A (en) * | 2009-12-17 | 2010-11-03 | 中国航天科技集团公司第五研究院第五一○研究所 | An in-situ monitoring method for outgassing pollution of non-metallic materials on the optical surface of spacecraft |
| CN102744654A (en) * | 2012-07-30 | 2012-10-24 | 中国人民解放军国防科学技术大学 | Double-vacuum chamber ion beam polishing system and polishing method |
-
2012
- 2012-11-20 CN CN201210469959.0A patent/CN102980832B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3863495A (en) * | 1973-04-16 | 1975-02-04 | Exxon Research Engineering Co | Quartz crystal solute mass detector |
| CN101776557A (en) * | 2009-12-17 | 2010-07-14 | 中国航天科技集团公司第五研究院第五一○研究所 | Device for testing grease evaporation rate in vacuum environment |
| CN101876612A (en) * | 2009-12-17 | 2010-11-03 | 中国航天科技集团公司第五研究院第五一○研究所 | An in-situ monitoring method for outgassing pollution of non-metallic materials on the optical surface of spacecraft |
| CN102744654A (en) * | 2012-07-30 | 2012-10-24 | 中国人民解放军国防科学技术大学 | Double-vacuum chamber ion beam polishing system and polishing method |
Non-Patent Citations (1)
| Title |
|---|
| 李丹明等: "应用材料可凝挥发物测试装置测量油脂饱和蒸气压", 《真空与低温》, vol. 9, no. 04, 30 December 2003 (2003-12-30), pages 195 - 198 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN104215598A (en) * | 2014-09-30 | 2014-12-17 | 北京卫星环境工程研究所 | On-line Infrared Absorption Spectrum Detection System for Outgassing Components of Spacecraft Materials |
| CN109828300A (en) * | 2019-01-31 | 2019-05-31 | 兰州空间技术物理研究所 | A kind of miniaturization omnidirectional particles detection |
| CN109828300B (en) * | 2019-01-31 | 2023-05-05 | 兰州空间技术物理研究所 | Miniaturized omnidirectional space particle detector |
| CN109917080A (en) * | 2019-04-12 | 2019-06-21 | 中国科学院上海技术物理研究所 | A vacuum pollution prevention and control test system for precision optical instruments |
| CN113237789A (en) * | 2021-05-12 | 2021-08-10 | 雅安百图高新材料股份有限公司 | Method for detecting content of organic modifier on surface of alumina powder |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102980832B (en) | 2014-11-05 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102980832A (en) | System and method for in-situ monitoring of quality loss of non-metallic material in vacuum | |
| CN103091180B (en) | Thermograde frozen soil uniaxial static creep test method | |
| CN100533133C (en) | Heat pipe plate type thermal conductivity tester | |
| CN102944358B (en) | High and low temperature vacuum calibrating device and method | |
| CN105044147B (en) | A kind of nearly phase change zone thermal conductivity of frozen soils measure apparatus and method | |
| CN101482526A (en) | Measuring method for thermal expansion coefficient of early-age concrete | |
| CN105004479B (en) | Ion gauge and mass spectrograph calibrating installation and method based on normal pressure measurement | |
| CN104180929B (en) | A kind of calibration steps of TR heat flow transducer | |
| WO2012097488A1 (en) | Calibration device for on-line sulfur hexafluoride humidity meters and calibration method therefor | |
| CN104062201B (en) | Measure the experimental provision of vacuum drying and vacuum lyophilization process parameter | |
| Nemanič et al. | New organic fiber-based core material for vacuum thermal insulation | |
| CN103808457A (en) | Low-temperature vacuum calibration device and method | |
| CN107607411A (en) | A kind of high-temperature tensile testing machine | |
| CN104215749A (en) | Realization method of combined temperature gradient in frozen earth | |
| CN104215655B (en) | A kind of frozen soil three-dimensional heat conducting coefficient measurement device and method | |
| CN102455211A (en) | Quartz crystal microbalance performance test system | |
| CN104215654A (en) | New method for measuring heat conductivity coefficient of micro powder sample under variable temperature and variable pressure conditions | |
| CN107966474B (en) | Device for measuring heat conductivity coefficient of block based on steady-state method | |
| CN104374667B (en) | Device for testing volatizing property of material at ultrahigh vacuum thermal environment | |
| CN206656979U (en) | It is a kind of to be used to measure rubber and the experimental provision of intermetallic contact thermal resistance | |
| CN104237057A (en) | Characteristic testing method of condensable and volatile matters in non-metal material in vacuum | |
| CN111948253A (en) | Concrete adiabatic temperature rise measuring device and method | |
| CN204925002U (en) | Frozen soil coefficient of heat conductivity apparatus | |
| CN110865002A (en) | High-precision material outgassing rate testing system and testing method thereof | |
| CN101788443B (en) | Prediction method for service life of vacuum thermal-insulation plate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |