CN104596906B - The water oxygen air penetrability measuring system of many measurement heads - Google Patents
The water oxygen air penetrability measuring system of many measurement heads Download PDFInfo
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Abstract
The present invention relates to a kind of water oxygen air penetrability measuring system of many measurement heads, including a common cavity, the common cavity is a confined space being made up of upper substrate, infrabasal plate and side bucket, and high purity inert gas is filled with during work；The multiple and equidistant measuring probe chamber in upper substrate center is fixed with the upper substrate of common cavity, a shared vacuum evaporation chamber is fixed with the center of the infrabasal plate of public chamber；There is a mobile cavity being mated with each measuring probe chamber, the quartz crystal for having active metal film is deposited built with one for the mobile cavity, the upper/lower electrode of the quartz crystal is connected to oscillator formation oscillator signal through electric wire through the mobile cavity of mobile cavity and the side bucket of common cavity, film thickness measuring instrument is transferred to by respective electronic switch again, the film thickness measuring instrument connects computer.The utilization rate that multiple samples substantially increase instrument can be measured simultaneously by providing many measurement heads in the present invention.
Description
Technical field
The present invention relates to a kind of measuring system of the water oxygen air penetrability for encapsulating material, particularly a kind of many measurement heads
Water oxygen air penetrability measuring system.
Background technology
Due to Organic Light Emitting Diode（OLED）, OTFT（TFT）, organic photovoltaic cell（OPV）To water oxygen
Gas is especially sensitive, and the air penetrability of its water oxygen will be 10-6g/m2/ below d can just meet real requirement, and this is for flexible display
The flexible substrates and package used is a serious challenge.Need development substantial amounts of about flexible base board and plural layers for this
The highly sensitive air penetrability of water oxygen separation layer measurement, the measuring method of the water oxygen air penetrability used at present has：Existed with evaporation
The water oxygen solid/liquid/gas reactions of calcium film and transmission on transparency carrier generate the dot area of transparent calcium hydroxide to calculate its transmitance,
The shortcoming of the method is：Need time length and even if also may not be accurate come reference area using camera system and computer.Separately
A kind of outer method is to be thinned with the thickness of two interelectrode calcium films with increasing through water oxygen tolerance, and makes resistance with the time
Change to calculate the transmitance of aqueous vapor, the method advantage is can be with the monitoring of overall process, but its shortcoming is the detection piece of calcium film
Can only be with once.Do one-shot measurement：It need to be completed in an evaporator being connected with High Purity Nitrogen glove box to quartz crystal
Carry out gas sensing layer calcium film evaporation, after under the atmosphere of High Purity Nitrogen be moved into glove box, in glove box load measuring head after take out
Glove box is put into air or tested in climatic chamber, whole process swelling length and complete equipment costliness.
The method of thickness is surveyed with quartz crystal to determine the quality in the calcium film of evaporation thereon with through water oxygen gas
Amount and change to have been described in patent CN201010237106 come the method for the transmitance that calculates water oxygen gas, the method
Advantage is to repeat application many times as the quartz crystal of detector.But the method only one of which measurement cavity but also
The instrument of the volume production of energy convenient use is not formed.
The content of the invention
It is an object of the invention to the defect existed for prior art, there is provided a kind of survey of the water oxygen air penetrability of many measurement heads
Amount system, can carry out being evaporated in vacuo calcium film and can provide the measuring system of multiple measurement heads in a system.It can be used in
Organic Light Emitting Diode（OLED）, OTFT（OTFT）, organic film solar cell（OPV）Deng organic semiconductor,
The measurement of the water oxygen air penetrability of diaphragm and plural layers water oxygen barrier layer case chip in the thin-film package of photoelectric device.
To reach above-mentioned purpose, the present invention uses following technical proposals：
A kind of water oxygen air penetrability measuring system of many measurement heads, including a common cavity, the common cavity be by upper substrate,
The confined space that infrabasal plate and side bucket are constituted, is filled with high purity inert gas during work；It is fixed on the upper substrate of common cavity
Have multiple with the equidistant measuring probe chamber in upper substrate center, be fixed with the center of the infrabasal plate of public chamber one it is shared true
Empty evaporation cavity；There is a mobile cavity being mated with each measuring probe chamber, the mobile cavity is built with an evaporation
Have a quartz crystal of active metal film, the upper/lower electrode of the quartz crystal through electric wire through the mobile cavity of mobile cavity and
The side bucket of common cavity is connected to oscillator formation oscillator signal, is transferred to film thickness measuring instrument again by respective electronic switch, institute
State film thickness measuring instrument connection computer；The film thickness measuring instrument measurement testing sample piece thickness changes with time, and computer enters
After row data processing, the water oxygen transmitance of the testing sample piece on the measuring probe chamber is obtained；The mobile cavity connection turning handle,
The turning handle rotation drives the rotation of mobile cavity body mobile cavity is changed between measuring probe chamber and vacuum evaporation chamber, works as mobile cavity
When completing to go to the position docked with vacuum evaporation chamber after one-shot measurement, evaporate active by the evaporator crucible being evaporated in vacuo in chamber
Metal is to forming after new gas sensing layer on quartz crystal, then rotates back into original measuring probe chamber lower position and carry out next time
Measurement process.
The measuring probe chamber be by measuring probe cavity, sealing ring, testing sample piece, Intermediate Gray fenestra measurement cavity
Gland and the switch valve composition with cushion rubber；Atmosphere chamber outside a chamber is cased with the measurement cavity gland, in measuring probe
The bottom of cavity is provided with through hole and is communicated to mobile cavity, and the switch valve with cushion rubber is fitted with through hole, on measuring probe cavity
Also bleeding point and air inlet, the bleeding point connecting valve and vavuum pump, the air inlet connecting valve and high-purity indifferent gas
System is united, and the lower plane of the lower plane of the measuring probe cavity and the upper substrate of common cavity is in a smooth plane.
The outer atmosphere chamber of the chamber is the space formed by atmosphere cover with measurement cavity gland and testing sample piece, in atmosphere cover
On have atmosphere air inlet and atmosphere gas outlet, atmosphere air inlet is connected by valve with atmosphere generation device, atmosphere generation device
Constant temperature and humidity air, pure oxygen or pure water vapour are provided.
The vacuum evaporation chamber is drawn by vacuum evaporation cavity, the second sealing ring, equipped with upper evaporator crucible and heating furnace silk
Go out the lower cover of electrode and the second switch valve group of the cushion rubber of band second into, be evaporated in vacuo cavity upper bottom portion be provided with the second through hole,
Second through hole is communicated to the mobile cavity for rotating, and the second switch valve of the cushion rubber of band second is fitted with the second through hole, true
There are the second bleeding point and the second air inlet on empty evaporation cavity, the second bleeding point is connected with valve and high vacuum system, second
Air inlet is connected with valve and high purity inert gas system, the infrabasal plate of the upper plane for being evaporated in vacuo cavity and common cavity
Upper plane is in a smooth plane.
The mobile cavity moves cavity by the barrel-like structure of upper and lower opening and the 3rd sealing ring is constituted up and down, or by following
Mobile cavity and the sealing ring of top the 3rd composition of the tubular structure of closing, in order to guarantee to make to move cavity and measuring probe chamber
Body and the sealing for being evaporated in vacuo cavity, briquetting is provided with measuring probe cavity and the another side for being evaporated in vacuo cavity, when
Mobile cavity compresses briquetting to ensure air-tightness again after rotateing in place.
The public chamber has the 3rd bleeding point, the 3rd air inlet on the bucket of side, and the 3rd bleeding point is connected to very by valve
Empty pump, the 3rd air inlet is connected to high purity inert gas by valve；The rotating shaft is arranged on infrabasal plate.
The upper plane of the lower plane for being evaporated in vacuo cavity and the upper substrate of common cavity is in a smooth plane；And will be upper
Evaporator crucible changes lower evaporator crucible into.
The film thickness measuring instrument can be replaced with frequency meter.
The active metal be can be reacted at normal temperatures with water oxygen gas calcium metal, strontium, barium, caesium and they
Alloy.
The present invention compared with prior art, substantive distinguishing features and remarkable advantage is obviously protruded with following：
The vapo(u)rization system of measurement head and gas sensing layer is integrated into a complete system in the present invention and can be with small
Type, makes the evaporation process of the gas sensing layer of whole test and quartz crystal all complete in a high-purity inert gas system
Into, not only simplify process whole operation process and also greatly accumulate cost-saving.Each measurement head is provided in the present invention
One atmosphere cover provides the test condition required for testing sample piece, and it, which is accumulated, has saved the equipment such as climatic chamber and can reduce energy again
Amount consumption, and different test conditions can be provided each measurement head.Providing many measurement heads in the present invention can be with
Measure the utilization rate that multiple samples substantially increase instrument simultaneously.The public evaporation of multiple measuring heads is provided in the present invention
Cavity improves the utilization rate of evaporation cavity.This, which may be reused, in quartz crystal in the present invention can not only save into
This, it is often more important that make the simpler sustainability of test program.
Brief description of the drawings
Fig. 1 is the structure 3D schematic diagrames of many measurement head water oxygen transmission measurement systems in the present invention.
Fig. 2 is the structural representation of many measurement head water oxygen transmission measurement systems in the present invention.
Fig. 3 is the superincumbent many measurement head water oxygen transmission measurement system architectures signals of vacuum evaporation cavity in the present invention
Figure.
Embodiment
Details are as follows for the preferred embodiments of the present invention combination accompanying drawing：
Embodiment 1
Referring to Fig. 1 and Fig. 2, a kind of water oxygen air penetrability measuring system of many measurement heads, apply has one layer of energy and water in evaporation
The quartz crystal of the active metal film of oxygen reaction can react when running into water and oxygen to be generated oxide and increases weight, and
The increased principle of thickness can be measured, many spies of the transmitance of the water oxygen gas of flaky material are measured as water and oxygen sensor
Head system.Including a common cavity 59, the common cavity 59 is that by upper substrate 51, constitute one of infrabasal plate 52 and side bucket 50 is close
Space is closed, high purity inert gas is filled with during work；The multiple and center of upper substrate 51 is fixed with the upper substrate 51 of common cavity 59
Equidistant measuring probe chamber 19, a shared vacuum evaporation chamber 39 is fixed with the center of the infrabasal plate 52 of public chamber 59；
There is a mobile cavity being mated with each measuring probe chamber, the mobile cavity has active metal built with an evaporation
The quartz crystal 1 of film, the upper/lower electrode of the quartz crystal 1 passes through the mobile cavity 3 and common cavity of mobile cavity through electric wire 2
59 side bucket 50 is connected to the formation oscillator signal of oscillator 61, and film thickness measuring instrument is transferred to again by respective electronic switch 62
63, the film thickness measuring instrument 63 connects computer 64；The thickness of the measurement testing sample of film thickness measuring instrument 63 piece 17 is with the time
Change, after carrying out data processing through computer 64, obtains the water oxygen transmitance of the testing sample piece 17 on the measuring probe chamber；Institute
The mobile connection of cavity 3 turning handle 8 is stated, the rotation of turning handle 8 drives mobile cavity body 3 mobile cavity is steamed in measuring probe chamber 19 and vacuum
Conversion between chamber 39 is sent out, when mobile cavity completes to go to the position docked with vacuum evaporation chamber 39 after one-shot measurement, passes through vacuum
Evaporator crucible in evaporation cavity 39 evaporates active metal and formed to quartz crystal 1 after new gas sensing layer, then rotates back into original
Measuring probe chamber lower position carries out measurement process next time.
The measuring probe chamber 19 is by measuring probe cavity 10, sealing ring 16, testing sample piece 17, Intermediate Gray fenestra
Measurement cavity gland 18 and the switch valve 14 with cushion rubber 15 are constituted；A chamber outer gas is cased with the measurement cavity gland
Atmosphere chamber 79, is provided with through hole in the bottom 10 of measuring probe cavity and is communicated to mobile cavity 9, opening with cushion rubber 15 is fitted with through hole
Valve 14 is closed, also has bleeding point 12 and air inlet 13, the bleeding point connecting valve and vavuum pump, institute on measuring probe cavity 10
State air inlet connecting valve and high purity inert gas system, the lower plane of the measuring probe cavity and the upper substrate of common cavity 59
51 lower plane is in a smooth plane.
The outer atmosphere chamber 79 of the chamber is the space formed by atmosphere cover 70 with measurement cavity gland 18 and testing sample piece 17,
There are atmosphere air inlet 71 and atmosphere gas outlet 72 on atmosphere cover, atmosphere air inlet is connected by valve with atmosphere generation device,
Atmosphere generation device provides constant temperature and humidity air, pure oxygen or pure water vapour.
The vacuum evaporation chamber 39 is by vacuum evaporation cavity 30, the second sealing ring 36, equipped with upper evaporator crucible 40 and added
Hot the stove silk lower cover 37 of extraction electrode 38 and the second switch valve 34 of the second cushion rubber of band 35 are constituted, and are being evaporated in vacuo the upper of cavity 30
Bottom is provided with the second through hole 33, and the second through hole 33 is communicated to the mobile cavity 9 for rotating, and band the is fitted with the second through hole 33
The second switch valve 34 of two cushion rubbers 35, also has the second bleeding point 32 and the second air inlet 31 being evaporated in vacuo on cavity 30, and second
Bleeding point 32 is connected with valve and high vacuum system, and the second air inlet 31 is connected with valve and high purity inert gas system, described
The upper plane for being evaporated in vacuo the upper plane of cavity 30 and the infrabasal plate 52 of common cavity 59 is in a smooth plane.
The mobile cavity 9 moves cavity 3 by the barrel-like structure of upper and lower opening and the 3rd sealing ring 4 is constituted up and down, in order to
Guarantee the sealing for making to move cavity and measuring probe cavity and vacuum evaporation cavity 30, in measuring probe cavity and vacuum
The another side of evaporation cavity 30 is provided with briquetting, compresses briquetting again after mobile cavity rotate in place to ensure air-tightness.
The public chamber 59 has the 3rd bleeding point 53, the 3rd air inlet 54 on side bucket 50, and the 3rd bleeding point 53 passes through
Valve is connected to vavuum pump, and the 3rd air inlet 54 is connected to high purity inert gas by valve；The rotating shaft 8 is arranged on infrabasal plate 52
On.
The active metal be can be reacted at normal temperatures with water oxygen gas calcium metal, strontium, barium, caesium and they
Alloy.
Whole process is the gas for first all measuring probe chambers, vacuum evaporation chamber and common cavity being maintained at ultra-pure nitrogen
The content of the water oxygen of its in atmosphere will be between 0.1ppm to 1ppm, then the switch valve pass for the measuring probe chamber to be measured
Close, corresponding mobile cavity is turned to the position for being evaporated in vacuo chamber, compress briquetting, open switch valve, be evacuated to after high vacuum
The evaporation of calcium is carried out, 10 to 1000 nanometers of calcium film is deposited on quartz crystal, the switch valve for being evaporated in vacuo cavity is closed,
Unclamp briquetting and mobile cavity is rotated back into measuring probe cavity and pushed and press block, the High Purity Nitrogen of renewal measuring probe chamber again
Air to close closes the valve of bleeding point and air inlet afterwards, and the switch valve for opening measuring probe cavity proceeds by measurement.If desired in spy
Its transmitance is observed in fixed atmosphere then the constant temperature and humidity atmosphere needed for being passed on the atmosphere enclosure.Then it can be carried out
The operation of his measuring probe chamber.
Embodiment 2
Referring to Fig. 3, most of structure of the present embodiment is same as Example 1, goes main difference to have：It is described to be evaporated in vacuo
Chamber 39 is arranged on the center of the upper substrate 51 of common cavity 59, the lower plane of the vacuum evaporation cavity 30 and the upper base of common cavity 59
The upper plane of plate 51 is in a smooth plane；And change upper evaporator crucible 40 into lower evaporator crucible 41.The mobile cavity is under
Mobile cavity 6 and the sealing ring of top the 3rd composition of the tubular structure of face closure.
Claims (9)
1. the water oxygen air penetrability measuring system of a kind of many measurement heads, it is characterised in that including a common cavity（59）, it is described public
Chamber（59）It is by upper substrate（51）, infrabasal plate（52）With side bucket（50）The confined space constituted, is filled with high-purity lazy during work
Property gas；In common cavity（59）Upper substrate（51）On be fixed with multiple and upper substrate（51）The equidistant measuring probe chamber in center
（19）, in public chamber（59）Infrabasal plate（52）Center be fixed with a shared vacuum evaporation chamber（39）；At each
There is a mobile cavity being mated with measuring probe chamber, the quartz for having active metal film is deposited built with one for the mobile cavity
Crystal-vibration-chip（1）, the quartz crystal（1）Upper/lower electrode through electric wire（2）Through the mobile cavity of mobile cavity（3）And common cavity
（59）Side bucket（50）It is connected to oscillator（61）Oscillator signal is formed, passes through respective electronic switch（62）Thickness is transferred to again
Measuring instrument（63）, the film thickness measuring instrument（63）Connect computer（64）；The film thickness measuring instrument（63）Measure testing sample piece
（17）Thickness changes with time, through computer（64）Carry out after data processing, obtain the testing sample on the measuring probe chamber
Piece（17）Water oxygen transmitance；The mobile cavity（3）Connect turning handle（8）, the turning handle（8）Rotation drives mobile cavity body（3）
Rotation makes mobile cavity in measuring probe chamber（19）With vacuum evaporation chamber（39）Between change, when mobile cavity complete one-shot measurement after turn
To with being evaporated in vacuo chamber（39）During the position of docking, by being evaporated in vacuo chamber（39）In evaporator crucible evaporate active metal to stone
English crystal-vibration-chip（1）It is upper to be formed after new gas sensing layer, then rotate back into the measurement of original measuring probe chamber lower position progress next time
Process.
2. the water oxygen air penetrability measuring system of many measurement heads according to claim 1, the measuring probe chamber（19）Be by
Measuring probe cavity（10）, sealing ring（16）, testing sample piece（17）, Intermediate Gray fenestra measurement cavity gland（18）With band glue
Circle（15）Switch valve（14）Composition；Atmosphere chamber outside a chamber is cased with the measurement cavity gland（79）, visited in measurement
Head cavity body（10）Bottom be provided with through hole and be communicated to mobile cavity（9）, band cushion rubber is fitted with through hole（15）Switch valve（14）,
In measuring probe cavity（10）It is upper to also have bleeding point（12）And air inlet（11）, the bleeding point connecting valve and vavuum pump, institute
State air inlet connecting valve and high purity inert gas system, the lower plane and common cavity of the measuring probe cavity（59）Upper base
Plate（51）Lower plane be in a smooth plane.
3. the water oxygen air penetrability measuring system of many measurement heads according to claim 2, it is characterised in that the outer atmosphere of the chamber
Chamber（79）It is by atmosphere cover（70）With measurement cavity gland（18）With testing sample piece（17）The space of formation, has on atmosphere cover
Atmosphere air inlet（71）With atmosphere gas outlet（72）, atmosphere air inlet is connected by valve with atmosphere generation device, and atmosphere is produced
Device provides constant temperature and humidity air, pure oxygen or pure water vapour.
4. the water oxygen air penetrability measuring system of many measurement heads according to claim 1, it is characterised in that the vacuum evaporation
Chamber（39）It is by vacuum evaporation cavity（30）, the second sealing ring（36）, equipped with upper evaporator crucible（40）Electricity is drawn with heating furnace silk
Pole（38）Lower cover（37）With the cushion rubber of band second（35）Second switch valve（34）Composition, is being evaporated in vacuo cavity（30）Upper bottom
Portion is provided with the second through hole（33）, the second through hole（33）It is communicated to the mobile cavity for rotating（9）, in the second through hole（33）Fill above
There is the cushion rubber of band second（35）Second switch valve（34）, it is being evaporated in vacuo cavity（30）It is upper to also have the second bleeding point（32）With second
Air inlet（31）, the second bleeding point（32）It is connected with valve and high vacuum system, the second air inlet（31）With valve and high-purity lazy
Property gas system be connected, the vacuum evaporation cavity（30）Upper plane and common cavity（59）Infrabasal plate（52）Upper plane be in
One smooth plane.
5. the water oxygen air penetrability measuring system of many measurement heads according to claim 1, it is characterised in that the mobile cavity
（9）It is that cavity is moved by the barrel-like structure of upper and lower opening（3）3rd sealing ring up and down（4）Composition, or by the cylinder of lower face closure
The mobile cavity of shape structure（6）With the sealing ring of top the 3rd（4）Composition, in order to guarantee to make to move cavity and measuring probe cavity
And it is evaporated in vacuo cavity（30）Sealing, measuring probe cavity and be evaporated in vacuo cavity（30）Another side pressure is installed
Block, compresses briquetting to ensure air-tightness again after mobile cavity rotate in place.
6. the water oxygen air penetrability measuring system of many measurement heads according to claim 1, it is characterised in that the public chamber
（59）In side bucket（50）On have the 3rd bleeding point（53）, the 3rd air inlet（54）, the 3rd bleeding point（53）It is connected to very by valve
Empty pump, the 3rd air inlet（54）High purity inert gas is connected to by valve；Rotating shaft（8）Installed in infrabasal plate（52）On.
7. the water oxygen air penetrability measuring system of many measurement heads according to claim 1, it is characterised in that the vacuum evaporation
Chamber（39）Installed in common cavity（59）Upper substrate（51）Center, the vacuum evaporation cavity（30）Lower plane and common cavity
（59）Upper substrate（51）Upper plane be in a smooth plane；And by upper evaporator crucible（40）Change lower evaporator crucible into（41）.
8. the water oxygen air penetrability measuring system of many measurement heads according to claim 1, it is characterised in that the film thickness measuring
Instrument（63）Replaced with frequency meter.
9. the water oxygen air penetrability measuring system of many measurement heads according to claim 1, it is characterised in that the active metal
It is calcium metal, strontium, barium, caesium and their alloy that can be reacted at normal temperatures with water oxygen gas.
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| TWI661193B (en) * | 2018-03-15 | 2019-06-01 | Southern Taiwan University Of Science And Technology | Water vapor and oxygen transmission sensing structure of silverless electrode |
| CN112461732A (en) * | 2020-12-14 | 2021-03-09 | 赣州优膜科技有限公司 | Testing arrangement of super high barrier film's steam transmissivity |
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| EP0022444B1 (en) * | 1979-07-04 | 1983-10-12 | Kidde-Graviner Limited | Improvements in and relating to the detection of particles in a gaseous medium |
| US4366703A (en) * | 1981-01-19 | 1983-01-04 | General Electric Company | Method and apparatus for determining permeability and thickness of refractory coatings on foundry molds and cores |
| US5548991A (en) * | 1995-03-09 | 1996-08-27 | Ritson; Marc J. | Permeameter probe |
| US7235214B2 (en) * | 2003-04-23 | 2007-06-26 | Particle Measuring Systems, Inc. | System and method for measuring molecular analytes in a measurement fluid |
| CN100507510C (en) * | 2004-09-30 | 2009-07-01 | 清华大学 | Testing method for water oxygen permeability and its testing equipment |
| KR101245296B1 (en) * | 2005-04-06 | 2013-03-19 | 바이오스케일, 아이엔씨. | Electrically responsive device |
| CN101949813B (en) * | 2010-07-27 | 2012-01-11 | 中国科学院苏州纳米技术与纳米仿生研究所 | Method and device for detecting water oxygen infiltration index in device packaging |
| CN102011096B (en) * | 2010-12-29 | 2012-07-04 | 上海大学 | Vacuum evaporation system capable of controlling evaporating airflow distribution and components |
| CN102185074A (en) * | 2011-04-07 | 2011-09-14 | 上海大学 | Light emitting diode of Ag/zinc-oxide-based composite transparent electrode and preparation method thereof |
| PL2667159T3 (en) * | 2012-05-24 | 2022-05-02 | Air Products And Chemicals, Inc. | Method of, and Apparatus for, Measuring the Mass Flow Rate of a Gas |
| US9541488B2 (en) * | 2012-09-21 | 2017-01-10 | Msp Corporation | Particle sampling and measurement in the ambient air |
| CN203405395U (en) * | 2013-06-21 | 2014-01-22 | 徐州市沃土农业科技发展有限公司 | Permeable rate tester |
| CN203479652U (en) * | 2013-09-12 | 2014-03-12 | 广州标际包装设备有限公司 | Water vapor transmission rate tester employing desiccant method |
| CN103575630B (en) * | 2013-10-23 | 2016-04-27 | 中国广州分析测试中心 | A kind of Simultaneously test combination gas respectively forms the assay method of the membrane permeability of gas |
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