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
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- 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
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Abstract
The invention relates to a system and a method for in-situ monitoring of a quality loss of a non-metallic material in vacuum and belongs to the field of a material characteristic test. The system comprises a main vacuum chamber, a connection rod, an air extractor, an ancillary vacuum chamber, a high-vacuum gate valve, a sample boat, a quartz crystal microbalance and a low-temperature cryoprecipitation device. The method comprises the following steps of arranging temperatures of the low-temperature cryoprecipitation device and the quartz crystal microbalance, feeding nitrogen into the ancillary vacuum chamber, weighing a sample, putting the sample into the sample boat, putting the sample boat into the ancillary vacuum chamber, closing the ancillary vacuum chamber, stopping nitrogen feeding, starting the air extractor, transferring the sample boat into the main vacuum chamber, arranging the sample boat right below the quartz crystal microbalance, closing the high-vacuum gate valve, heating the sample to an outlet temperature of the sample, recording a frequency change delta f and a temperature T of the quartz crystal microbalance once at a set time interval, and calculating a total mass loss of the sample. The method improves a measurement precision and effectively avoids the influence produced by air on the system in loading and unloading of a sample.
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)
1. the in-situ monitoring system of nonmetallic materials mass loss in the vacuum, it is characterized in that: 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; The top of main vacuum chamber (1) inwall and all around the position be respectively equipped with low temperature cold heavy (8), 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);
Be connected 5 by pipeline with the high vacuum push-pull valve between main vacuum chamber (1) and the secondary vacuum chamber (4)) connect;
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.
2. the in-situ monitoring method of nonmetallic materials mass loss in the vacuum, it is characterized in that: described method is used as claimed in claim 1 system, and described method step is as follows:
Step 1, quartz crystal microbalance (7) temperature is made as≤-180 ℃, sets the temperature of the temperature≤quartz crystal microbalance (7) of low temperature cold heavy (8), in secondary vacuum chamber (4), pass into nitrogen;
Step 2, put into example boat (6) after sample weighed, example boat (6) is packed into close secondary vacuum chamber (4) behind the secondary vacuum chamber (4), cut off nitrogen, open air extractor (3), the pressure to the main vacuum chamber (1)≤7 * 10
-3Pressure in the Pa, secondary vacuum chamber (4)≤5 * 10
-3Pa;
Step 3, unlatching high vacuum push-pull valve (5) promote connecting rod (2), under quartz crystal microbalance (7) in example boat (6) the immigration main vacuum chamber (1), close high vacuum push-pull valve (5);
Step 4, sample is heated to the air outlet temperature of sample, every frequency change Δ f and the temperature T of a setting-up time quartz crystal microbalance of record (7);
The total mass loss of step 5, calculating sample.
3. the in-situ monitoring method of nonmetallic materials mass loss in a kind of vacuum according to claim 2 is characterized in that: at 25.0 ℃ ± 5.0 ℃, relative humidity is after placing more than 24 hours under 20% ~ 60% the environment, to carry out step 1 with sample.
4. the in-situ monitoring method of nonmetallic materials mass loss in a kind of vacuum according to claim 2, it is characterized in that: in the step 3, the venthole of example boat (6) is positioned on the axis of quartz crystal microbalance (7).
5. the in-situ monitoring method of nonmetallic materials mass loss in a kind of vacuum according to claim 2 is characterized in that: in the step 4, every frequency change Δ f and the temperature T of 10s ~ 10min quartz crystal microbalance of record (7).
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| 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 |
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| CN102980832B CN102980832B (en) | 2014-11-05 |
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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 | Online infrared absorption spectrum detecting system for gas composition released from spacecraft material |
| 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 kind of vacuum pollution prevention and control test macro of precision optical instrument |
| 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 |
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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 |
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| 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 kind of vacuum pollution prevention and control test macro of precision optical instrument |
| 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 |
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| CN102980832B (en) | 2014-11-05 |
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