A kind of material radiation causes the online testing device deflated
Technical field
The utility model is related to field of measuring technique, more particularly, under a kind of vacuum condition material radiation cause deflate
Line test device.
Background technology
Any solid material, which is placed in vacuum environment, all can desorb and deflate, in satellite, airship, space and some semiconductors
Deng field, vacuum material produces acceleration deflation course due to the radiation by light, heat or electron beam etc., the portion gas of releasing
Original vacuum environment can be deteriorated, cause some optical components to fail.The deflation row of material under the conditions of Accurate Analysis vacuum radiation
To be the important evidence for evaluating material vacuum performance, including accurate obtain radiation and cause discharge quantity, deflation component and radiation to cause to deflate
Component.
Chinese granted patent " a kind of apparatus and method of dual testing room measured material outgassing rate measuring ", its Publication No.
CN101696923, as shown in figure 1, including high vacuum chamber (112), supervacuum chamber (102), extractor gauge (107), ultrahigh vacuum
Angle valve A (105), ultrahigh vacuum angle valve B (106), straight-through valve A (110) and straight-through valve B (111), bimolecular pump extract system
(101);Also include:Symmetrical test cabinet A (108) and test cabinet B (109).Bimolecular pump extract system (101) and ultrahigh vacuum
Room (102) is connected;Supervacuum chamber (102) passes through aperture respectively with two symmetrical test cabinet A (108) and test cabinet B (109)
It is connected, diameter range 5.7mm~14mm of aperture;Extractor gauge (107) bridges at supervacuum chamber (102) and test cabinet A
(108) on, and with supervacuum chamber (102) and test cabinet A (108) junction to be respectively provided with superelevation true for extractor gauge (107)
Empty angle valve A (105) and ultrahigh vacuum angle valve (106);Test cabinet A (108) and test cabinet B (109) pass through straight-through valve A respectively
(110), straight-through valve B (111) is connected with high vacuum chamber (112), heating plate built in high vacuum chamber (112).The apparatus structure is complicated,
Operation inconvenience, material is deflated using heating, and influence factor is more, and measurement accuracy is relatively low, involves great expense.
《Vacuum and low temperature》First phase paper of volume 20 in 2014 " material deflate under vacuum conditions Testing Technology Study "
Describing it uses static pressurizing method, constant conductance method and binary channels gas circuit transformation approach to test infrared radiation heating material in difference
At a temperature of deflation rate, and point out the rise with material temperature, deflation rate can increase.But it is not tested merely due to radiating production
Raw deflation rate.Tested according to said apparatus merely due to the deflation that radiation is produced, often needs the sample for identical material to exist
The deflation rate of sample when not radiating and radiating is tested under same operating mode respectively, both subtract each other acquisition.Due to the deflation rate of sample
It is closely bound up with pumpdown time, temperature, surface appearance and surrounding environment etc., therefore it is difficult to ensure that test condition complete one twice
Cause, cause deflation to bring difficulty to accurate testing radiation.
The partial pressure of each deflation component of current test material uses mass spectrograph mostly, is ionized by heat filament in surrounding environment
Gas molecule be ion, directly test obtains the size of ion stream, and partial pressure is obtained indirectly using the method for internal calculation.
China has authorized patent " the compound material deflation rate test system and method with self-calibration function ", open
Number it is CN201210431477, the device vacuum chamber is more, and structure is extremely complex, and system cost is very high.The system passes through
The method of calibrating mass spectrometry sensitivity increases measuring accuracy, but actual mass spectrograph partial pressure calculating except having outside the Pass with sensitivity,
Ionization probability, geometry factor, transforming factor and detection factor etc. are further related to, it is extremely complex;And most mass spectrograph in the market
Computation rule be also slightly different.Accordingly, it would be desirable to a kind of simple in construction, easy to operate material radiation causes the on-line testing deflated
Device so that test process is simple, result is more true accurate.
Utility model content
The purpose of this utility model is achieved through the following technical solutions.
The utility model discloses the online testing device that a kind of material radiation causes to deflate, and described device includes:Vacuum chamber
System, radiant chamber system, extract system, air supply system, detection components and numerical control collecting unit, wherein,
The vacuum chamber system includes placing testing sample inside a vacuum chamber (1), the vacuum chamber (1)
(3);
The radiant chamber system is connected with the vacuum chamber system by flange window (4);
The extract system is connected with the vacuum chamber system;
The air supply system is connected with the vacuum chamber system, and all kinds of gases are passed through to the vacuum chamber (1);
The detection components include vacuum gauge (19) and mass spectrograph (20);
The numerical control collecting unit is used for the switch for controlling vacuum pump group, radiation source (6) and detection components, adopts in real time online
Collect vacuum data, the data gathered are preserved and calculated.
Preferably, the vacuum chamber system includes:Vacuum chamber (1), sample stage (2), sample (3) and flange window
(4), sample stage (2) is fixed on above the side of vacuum chamber (1), rather than bleeding point, and sample (3) is placed on sample stage (2),
Flange window (4) is on vacuum chamber (1).
Preferably, the radiant chamber system includes:Radiant chamber (5), radiation source (6) and radiant flux (7), radiation source
(6) it is placed in radiant chamber (5), is light, heat or electron beam irradiation, radiant flux (7) is radiated sample through flange window (4)
(3) on.
Preferably, the extract system includes:Dry-type mechanical pump (8), maglev molecular pump (9), current limliting aperture (10),
One angle valve (11), push-pull valve (12) and the second angle valve (13), wherein dry-type mechanical pump (8) and the second angle valve (13) composition first is taken out
Gas passage, thick for vacuum chamber (1) is taken out;Dry-type mechanical pump (8), maglev molecular pump (9) and push-pull valve (12) composition the
Two bleed-off passages, the essence for vacuum chamber (1) is taken out;Dry-type mechanical pump (8), maglev molecular pump (9), current limliting aperture (10) and
First angle valve (11) constitutes the 3rd bleed-off passage, and test of deflating is caused for sample emission.
Preferably, the air supply system includes:Source of the gas (14), the first stop valve (15), reset valve (16), the second stop valve
And gas flow controller (18), (17) wherein source of the gas (14), the first stop valve (15) and reset valve (16) composition first are supplied
Passage, makes vacuum chamber (1) formation dynamic stability air-flow;Source of the gas (14), the first stop valve (15) and the second stop valve (17) group
Into the second air supply channel, for being filled with protective gas to vacuum chamber (1);Source of the gas (14), the first stop valve (15) and gas stream
Amount controller (18) constitutes the 3rd air supply channel, the air-flow known and controllable for being filled with flow into vacuum chamber (1);Wherein
Gas flow controller (18) passes through accurate calibration.
Preferably, the detection components include:Vacuum gauge (19), mass spectrograph (20), the third angle valve (21) and fourth angle valve
(22).Vacuum gauge (19) passes through accurate calibration, is connected to by the third angle valve (21) on vacuum chamber (1);Mass spectrograph (20) leads to
Fourth angle valve (22) is crossed to be connected on vacuum chamber (1).
Compared with prior art, the on-line testing dress deflated is caused the utility model proposes material radiation under a set of vacuum condition
Put, the apparatus structure is simple, and only one of which vacuum chamber, the problem of overcoming many vacuum chambers in the prior art is easy to operate;
And the radiation effect of vacuum gauge and mass spectrograph hot filament is effectively prevent, reduce influence of the test sample to effective pumping speed;And
Mass spectrograph and effective pumping speed can be calibrated, overcome the problem of accurate testing radiation causes to deflate difficult in the prior art, surveyed
Test result is more true accurate.
Brief description of the drawings
By reading the detailed description of hereafter preferred embodiment, various other advantages and benefit is common for this area
Technical staff will be clear understanding.Accompanying drawing is only used for showing the purpose of preferred embodiment, and is not considered as to this practicality
New limitation.And in whole accompanying drawing, identical part is denoted by the same reference numerals.In the accompanying drawings:
Fig. 1 is a kind of existing device of dual testing room measured material outgassing rate measuring;
Fig. 2 is the test device of material radiation cause deflation under a kind of vacuum condition of the present utility model;
Fig. 3 is that polyimides sample laser emission of the present utility model causes deflation composition chromatograph chart;
Fig. 4 is deflation total amount and the deflation component that laser emission polyimides sample of the present utility model causes to deflate.
Description of reference numerals
The sample stage of 1 vacuum chamber 2
The flange window of 3 sample 4
The radiation source of 5 radiant chamber 6
The dry-type mechanical pump of 7 radiant flux 8
The current limliting aperture of 9 maglev molecular pump 10
The push-pull valve of 11 first angle valve 12
The source of the gas of 13 second angle valve 14
The reset valve of 15 first stop valve 16
The gas flow controller of 17 second stop valve 18
The mass spectrograph of 19 vacuum gauge 20
The fourth angle valve of 21 the third angle valve 22
23 numerical control collecting units
The supervacuum chamber of 101 bimolecular pump extract system 102
The aperture B of 103 aperture A 104
The ultrahigh vacuum angle valve B of 105 ultrahigh vacuum angle valve A 106
The test cabinet A of 107 extractor gauge 108
The straight-through valve A of 109 test cabinet B 110
The high vacuum chambers of 111 straight-through valve B 112
113 sample materials
Embodiment
The illustrative embodiments of the disclosure are more fully described below with reference to accompanying drawings.Although showing this public affairs in accompanying drawing
The illustrative embodiments opened, it being understood, however, that may be realized in various forms the disclosure without the reality that should be illustrated here
The mode of applying is limited.Conversely it is able to be best understood from the disclosure there is provided these embodiments, and can be by this public affairs
The scope opened completely convey to those skilled in the art.
The utility model embodiment is described in detail below in conjunction with accompanying drawing.
As shown in Fig. 2 the utility model embodiment, which discloses material radiation under a kind of vacuum condition, causes the on-line testing deflated
Device, the device includes vacuum chamber system, radiant chamber system, extract system, air supply system, detection components and numerical control collection
Unit.
The vacuum chamber system only one of which vacuum chamber, interior placement testing sample, and sample should avoid being placed directly within
On bleeding point;
The radiant chamber system is connected with vacuum chamber system by flange window, for radiation sample, radiant chamber
Can be vacuum or antivacuum, radiation source can be light, heat or electron beam etc.;
The extract system is connected with vacuum chamber system, for being vacuumized to vacuum chamber system;
The air supply system is connected with vacuum chamber system, and all kinds of gases are passed through to vacuum chamber, adjustable mass spectrograph and
Effective pumping speed;
The detection components include vacuum gauge and mass spectrograph, the position of optimizing detection component, it is to avoid its filament directly hot spoke
Penetrate sample;
The numerical control collecting unit can easily control the switch of vacuum pump group, radiation source and detection components, can be real online
When gather vacuum data, bring convenience to operation.
Specifically, the vacuum chamber system includes:Vacuum chamber 1, sample stage 2, sample 3 and flange window 4.Vacuum chamber
Room 1 is cylinder, and typical sizes are Φ 200mm × 250mm, and the requirement of its final vacuum reaches 1 × 10-7Pa.Sample stage 2 is fixed
In the side of vacuum chamber 1, it is to avoid be placed directly within bleeding point and influence the effective pumping speed of vavuum pump, thermometric platinum is installed thereon
Resistance, the temperature for test sample.Sample 3 is placed on sample stage, and typical sizes are 100mm × 100mm square piece shape.Method
Blue window 4 can be furnished with water cooling plant thereon on vacuum chamber 1 by radiant flux, prevent the temperature distortion of flange window from rupturing.
The radiant chamber system includes:Radiant chamber 5, radiation source 6 and radiant flux 7.Radiant chamber 5 can be vacuum or non-
Vacuum chamber.Radiation source 6 is placed in radiant chamber 5, can be light, heat or electron beam irradiation, radiant flux 7 is through the spoke of flange window 4
It is mapped on sample 3.
The extract system includes:Dry-type mechanical pump 8, maglev molecular pump 9, current limliting aperture 10, the first angle valve 11, plate
The angle valve 13 of valve 12 and second.The wherein pumping speed of maglev molecular pump 9 is about 300L/s.The angle valve 13 of dry-type mechanical pump 8 and second is constituted
First bleed-off passage, thick for vacuum chamber 1 is taken out;Dry-type mechanical pump 8, maglev molecular pump 9 and the composition of push-pull valve 12 second
Bleed-off passage, the essence for vacuum chamber 1 is taken out;Dry-type mechanical pump 8, maglev molecular pump 9, the angle valve 11 of current limliting aperture 10 and first
The 3rd bleed-off passage is constituted, deflates and tests for sample, wherein a diameter of 20~100mm of current limliting aperture 10 can be according to application
The diameter of required effective pumping speed selection current limliting aperture 10.
The air supply system includes:Source of the gas 14, the first stop valve 15, reset valve 16, the second stop valve 17 and gas flow
Controller 18.Wherein source of the gas 14 can be all kinds of gases, such as He, N2、CO2Deng gas flow controller 18 passes through accurate calibration.Gas
Source 14, the first stop valve 15 and reset valve 16 constitute the first air supply channel, make the formation dynamic stability air-flow of vacuum chamber 1, pressure
Adjustable extent is 10-7Pa~1Pa;Source of the gas 14, the first stop valve 15 and the second stop valve 17 constitute the second air supply channel, for
Vacuum chamber 1 is filled with protective gas (such as N2);Source of the gas 14, the first stop valve 15 and the composition of gas flow controller 18 the 3rd are supplied
Passage, for being filled with air-flow known to flow and controllable into vacuum chamber 1, flow-control scope is 7 × 10-2~7 × 10- 5Pa·m3/s。
The detection components include:Vacuum gauge 19, mass spectrograph 20, the third angle valve 21 and fourth angle valve 22.Vacuum gauge 19 is used
In the pressure of measurement vacuum chamber 1, by accurate calibration;From Penning gauge, filament is iridium filament;Pass through the third angle valve
21 are connected on vacuum chamber 1, and filament is not directly to sample 3, the connection end for making it be slightly above the third angle valve 21 and vacuum chamber 1
Mouthful, radiation of the hot filament (1000 DEG C of >) to chamber wall and sample is reduced to greatest extent.Mass spectrograph 20 is used to measure vacuum chamber
Gas component and partial pressure in room 1;Mass number scope 1-200amu, preferably QMG220 models, filament are iridium filament;Pass through the 4th
Angle valve 22 is connected on vacuum chamber 1, makes the connection end of filament not directly to sample 3, slightly above fourth angle valve 22 and vacuum chamber 1
Mouthful, the heat radiation to chamber wall and sample is reduced to greatest extent.
The numerical control collecting unit 23 passes through on the one hand control radiation source 6, dry-type mechanical pump 8, the magnetic suspension of industrial computer software
Startup, stopping and the signal feedback of molecular pump 9 and mass spectrograph 20, on the other hand gather the test number of vacuum gauge 19 and mass spectrograph 20
According to, and data preservation and simple computation can be carried out.
Using utility model device shown in Fig. 2, mass spectrograph 20 can be calibrated.Calibrating quality numerical digit is needed to put and peak first
It is worth shape:Vacuum chamber 1 for reaching end vacuum, enables the first air supply channel and the 3rd bleed-off passage, to vacuum chamber 1
In be passed through high-purity He gas (4amu) of low quality number, it is 5 × 10 to keep dynamic stability air-flow-6Pa, adjusts source parameters, makes peak
Value is shaped as gaussian-shape, and is centrally located at 4amu;Similarly, high-purity Xe gas of high-quality number is passed through into vacuum chamber 1
(132amu), it is 5 × 10 to keep dynamic stability air-flow-6Pa, adjusts source parameters, makes peak shape for gaussian-shape, and center
Positioned at 132amu.Secondly as vacuum gauge 19 is calibrated, by mass spectrograph 20 and the comparison calibration of vacuum gauge 19, it is ensured that test knot
The uniformity and reliability of fruit.Vacuum chamber 1 for reaching end vacuum, enables the first air supply channel and the 3rd pumping is logical
Road, high-purity gas i is passed through into vacuum chamber 1, keeps dynamic stability air-flow, vacuum is about 10-6Pa;Treat in chamber 95% with
When upper gas is i, the stagnation pressure P that record vacuum gauge 19 is measuredionThe gas i measured with mass spectrograph 20 partial pressure Pi, ratio between two obtains
The modifying factor P of partial pressure is tested to mass spectrograph 20ion/Pi。
, can be to effective pumping speed S using utility model device shown in Fig. 2e(m3/ s) calibrated.For reaching end vacuum
Vacuum chamber 1, enable the 3rd air supply channel and the 3rd bleed-off passage, adjusting gas flow controller 18, with certain flow velocity
Qi(Pa·m3/ s) gas i is passed through to vacuum chamber 1, reach after dynamic equilibrium, vacuum chamber is tested with calibrated mass spectrograph 20
Gas i partial pressure P in 1i, then effective pumping speed S of the extract system to gas iei=Qi/Pi。
Thus, by accurate calibration mass spectrograph and system effective pumping speed, can conveniently and efficiently, it is accurate truly and online real
When measure the radiation of material under vacuum condition and cause deflation total amount, deflation component and deflation component.
Vacuum material radiation causes the online testing device deflated with reference to shown in Fig. 2, and the invention also discloses material spoke
Penetrate cause discharge quantity, deflation component and material radiation cause deflation component on-line testing method, the method for testing include dynamic method and
Mass spectrography, is on air real time test.The radiation that two methods test same sample is respectively adopted in set of system causes discharge quantity, just
Compare in the superiority-inferiority for carrying out each method of testing.Using mass spectrography can also on-line testing material radiation cause deflate each gas component
With deflation component.Explanation exemplified by the laser emission to test polyimides causes to deflate below.
Dynamic method testing procedure is as follows:S1:Vacuum chamber 1 for reaching end vacuum, closes all bleed-off passages, opens
The second air supply channel is used, 1.2atm drying N is filled with to vacuum chamber 12, polyimides sample to be measured is put into vacuum chamber 1
In, close the second air supply channel.S2:Start the first bleed-off passage slightly to take out vacuum chamber 1, be then switched to the second bleed-off passage
Essence is taken out.S3:Vacuum gauge 19 is opened, vacuum chamber 1 is evacuated to the limit true by the pressure P of on-line real-time measuremen vacuum chamber 1 again
Sky, switches to the 3rd bleed-off passage.S4:Radiation source 6 is opened, radiated time is t (s), and the pressure of vacuum gauge 19 rises Δ P
(Pa).S5:The bleed-off passage of radiation source 6 and the 3rd is closed, 1.2atm drying N is filled with to vacuum chamber 12, polyamides will have been surveyed sub-
Amine sample takes out, and is completed.Then unit interval polyimides sample discharge quantity Q (moleculars-1) calculating see formula
1.Wherein SeN2(m3/ s) for the 3rd bleed-off passage to N2Effective pumping speed, NA(mol-1) it is Avgadro constant, T (K) is spoke
Temperature when penetrating, R (Pam3·K-1·mol-1) it is gas constant.The material outgassing amount Q of gained is to be equivalent to N2Equivalent value.
Mass spectrography testing procedure is as follows:The same dynamic methods of step S1-S2.S3:Open mass spectrograph 20, on-line real-time measuremen vacuum
The deflation component of chamber 1 and each component i partial pressure Pi(Pa) vacuum chamber 1, is evacuated to end vacuum again, the 3rd is switched to and takes out
Gas passage.S4:Radiation source 6 is opened, radiated time is t (s), and the partial pressure that mass spectrograph 20 measures gas component i rises to Δ Pi
(Pa).S5:The bleed-off passage of radiation source 6 and the 3rd is closed, 1.2atm drying N is filled with to vacuum chamber 12, polyamides will have been surveyed sub-
Amine sample takes out, and is completed.Then unit interval polyimides sample deflation component Qi(molecular·s-1) calculating see public affairs
Formula 2, unit interval polyimides sample deflation total amount Q (moleculars-1) calculating see formula 3.Wherein Sei(m3/ s) be
3rd bleed-off passage is to gas i effective pumping speed, NA(mol-1) it is Avgadro constant, temperature when T (K) is radiation, R
(Pa·m3·K-1·mol-1) it is gas constant, n is the gas component number that the polyimides sample that mass spectrograph 20 is measured is deflated.
Fig. 3 is the deflation composition chromatograph chart that mass spectrography measures polyimides sample, mainly there is H2(2amu)、H2O(18amu)、N2
(CO)(28amu)、O2(32amu), Ar (40amu) and CO2(44amu).Fig. 4 is that laser emission polyimides sample causes what is deflated
Deflation total amount and deflation component, the deflation total amount of dynamic method test is nitrogen equivalent value, mass spectrography test for actual value.Use
Dynamic method and mass spectrography can test the deflation total amount of same sample, and both can contrast.Mass spectrography can test specific deflation group
The deflation component divided.
It is described above, only the utility model preferably embodiment, but protection domain of the present utility model is not
This is confined to, any one skilled in the art can readily occur in the technical scope that the utility model is disclosed
Change or replacement, should all cover within protection domain of the present utility model.Therefore, protection domain of the present utility model should be with
Protection domain described in claim is defined.