CN101949813A - Method and device for detecting water oxygen infiltration index in device packaging - Google Patents
Method and device for detecting water oxygen infiltration index in device packaging Download PDFInfo
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- CN101949813A CN101949813A CN 201010237106 CN201010237106A CN101949813A CN 101949813 A CN101949813 A CN 101949813A CN 201010237106 CN201010237106 CN 201010237106 CN 201010237106 A CN201010237106 A CN 201010237106A CN 101949813 A CN101949813 A CN 101949813A
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- water oxygen
- crystal oscillator
- quartz crystal
- oxygen infiltration
- film
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Abstract
The invention discloses a method and a device for detecting a water oxygen infiltration index in device packaging. The method comprises the following steps of: firstly, preparing a quartz crystal plated with an active metal layer; secondly, transferring the quartz crystal to a test box under the condition that air is isolated and sealing by using a packaging structure and a packaging method the same as the device packaging; and finally, connecting the test box with a crystal oscillator, a crystal controller and a power supply to form a quartz microbalance, switching on the power supply, sensing the piezoelectric effect and mass loading effect of the quartz crystal through the crystal controller, outputting the piezoelectric effect and mass loading effect to the microbalance in real time, calculating the increased mass of a metal film after infiltrated water is absorbed and then calculating the water oxygen infiltration rate and total infiltrated water oxygen content in unit time. The method and the device can be used for detecting the water oxygen infiltration rate in real time on line in the packaging of a water oxygen sensitive device, have the detection limit of lower than 5*10<-6>g.m<-2>/d, and can meet the limit detection requirement of packaging of organic photoelectric device products on water gas infiltration rate.
Description
Technical field
The present invention relates to a kind of method and pick-up unit thereof that is used to detect water oxygen infiltration index.Relate in particular to a kind of to water oxygen Sensitive Apparatus (as Organic Light Emitting Diode (OLED), organic photovoltaic devices, OTFT etc.) encapsulating structure under the water oxygen infiltration rate of reduced levels and infiltration total amount, carry out fast, accurate method and the pick-up unit thereof that detects.
Background technology
Fast-developing organic electronic device, all need to solve the problem of encapsulation as The Application of Technology such as OLED demonstration and white-light illuminating, organic solar batteries, OTFT, sensor and industrialization, this is because the water oxygen composition in the atmospheric environment can cause the quick aging of organic assembly.Studies show that, adopt the material and the encapsulation technology of the infiltration of high performance water proof oxygen can prolong the device mission life significantly.Calculating shows, reaches practical 1 * 10 device lifetime as making OLED
4More than hour, its encapsulating structure need be lower than 5 * 10 to the infiltration rate of steam
-6Gm
-2/ d, the infiltration rate of oxygen should be lower than 10
-5Cm
2M
-2/ d, current puzzlement scientific research personnel's a main difficult problem is, even prepare the substrate protective layer or the encapsulating structure of waterproof oxygen permeability, how the barrier property to them carries out quantitative test.Also do not have at present commercial apparatus can test so low infiltration rate, traditional sensor water oxygen pick-up unit can only detect 1 * 10
-3Gm
-2/ d.
The method that the general organic assembly water oxygen infiltration rate in laboratory detects is the method for testing of Ca reaction bonded CCD spectral analysis, and the area that vapor deposition 100nm is thick on substrate under vacuum tightness earlier is the Ca film of 5mm.At N
2In the glove box (the water oxygen content all is lower than 1ppm) with substrate to be measured or encapsulating structure and glass the Ca film with test cell of epoxy encapsulation composition, this test cell is placed under the constant environment of temperature and relative humidity, the Ca film can generate transparent calcium hydroxide with the water oxygen reaction that penetrates into, and the district can form transparent circular hole at the Ca film.Situation behind the Ca film reaction is sent into the CCD camera system by microscopic system, and CCD converts light signal digital signal to and do Flame Image Process in computing machine.By calculating the relative area that the Ca film is corroded, calculate the permeability of water oxygen again.If the test cell of full glass-encapsulated then records the permeability of the water oxygen that sees through from package edge epoxy resin.The method can be calculated the average velocity of the water oxygen infiltration in certain period, but the identification of the area that is corroded and estimation have certain difficulty, the Ca in district of particularly being corroded still has and a small amount of with under the situation of water oxygen reaction does not exist than mistake, and in addition, this method needs the long time.Therefore how finding a kind of not only economy but also reaching predetermined accuracy, the method that can also finish test within a short period of time and device is the problem that numerous scientific research personnel are concerned about most.
Summary of the invention
For overcoming the defective that exists in the prior art, purpose of the present invention aims to provide a kind of method and pick-up unit thereof that is used for detection means packaged water oxygen infiltration index.Utilize the crystal microbalance principle and, realize being lower than 5 * 10 in conjunction with deposition active metal film on the crystal-vibration-chip
-6Gm
-2The real-time online of/d water oxygen infiltration rate detects, and reaches organic electro-optic device product encapsulation such as OLED to the requirement that the water oxygen permeability limit detects, and further shortens sense cycle, improves degree of accuracy.
The technical scheme that realizes first purpose of the invention described above is:
Be used for the method for detection means packaged water oxygen infiltration index, it is characterized in that:
(1), at the metal film of the active region of quartz crystal oscillator sheet vacuum moulding machine one deck tool activity;
(2), described quartz crystal oscillator sheet is being transferred under the situation of secluding air among the glove box, the water oxygen content in the described glove box all is lower than 0.1ppm;
(3), in glove box with described quartz crystal oscillator sheet built-in test box, and with identical structure of device package and method sealing, described device encapsulation structure comprises that packaging film, moisture oxygen deaden the substrate of film and the cure package glue of encapsulation junction;
(4), testing cassete is linked to each other and constitutes crystal microbalance with crystal oscillator, brilliant control instrument, power supply, energized, piezoelectric effect and mass loading effect by crystalline substance control instrument sensing quartz crystal oscillator sheet, export to microprocessor in real time, calculate the quality that metal film absorbs to be increased behind the water oxygen that infiltrates, and then calculate water oxygen infiltration rate and the water oxygen total amount of having infiltrated in the unit interval.
Further, the aforementioned method that is used for detection means packaged water oxygen infiltration index, wherein the quartz crystal oscillator sheet is the crystal-vibration-chip that is applicable to crystal microbalance described in the step (1), crystal oscillator frequency is between 0.1MHz～55MHz; The material of crystal oscillator electrode is a kind of in gold, silver, the aluminium; Adopt the metal film of the mode of vacuum evaporation in the active region of quartz crystal oscillator sheet deposition tool activity.
Further, the aforementioned method that is used for detection means packaged water oxygen infiltration index, wherein this metal film is assist by film thickness gauge monitoring in real time to control thickness and vacuum-deposited.
The technical scheme that realizes second purpose of the invention described above is:
The pick-up unit that is used for detection means packaged water oxygen infiltration index, it is characterized in that comprising: testing cassete, provide device package to carry out the cavity that water oxygen infiltration index detects, described testing cassete is provided with the quartz crystal oscillator sheet of metal-coated membrane in the cavity and the crystal-vibration-chip connector on the wall of chamber, and described crystal-vibration-chip connector links to each other with two electrodes of quartz crystal oscillator sheet towards testing cassete cavity inboard; And described quartz crystal oscillator sheet is connected to form the loop of crystal microbalance, the output termination microprocessor of described brilliant control instrument by crystal-vibration-chip connector and lead and external crystal oscillator, brilliant control instrument, power supply.
Further, the aforementioned pick-up unit that is used for detection means packaged water oxygen infiltration index, wherein this metal film is the metallic film of any one or a few formation in tool activity calcium, magnesium, sodium, strontium, potassium, barium, caesium, yttrium, lanthanum, ytterbium, samarium, the erbium, and film thickness is between 10nm～1000nm.Preferred thickness is calcium (Ca) film of 100nm.
The present invention is used for the method and the pick-up unit thereof of detection means packaged water oxygen infiltration index, compares to the detection method of prior art, can be to being lower than 5 * 10
-6Gm
-2The water oxygen infiltration rate of/d carries out real-time online and detects, and reaches the requirement that organic electro-optic device product encapsulation such as Organic Light Emitting Diode detects the water vapor permeable rate limit; Further improve the detection degree of accuracy, and shortened the sense cycle of relative classic method greatly.
Following constipation closes accompanying drawing, the specific embodiment of the present invention is described in further detail, so that technical solution of the present invention is easier to understand, grasp.
Description of drawings
Fig. 1 is used for the system architecture synoptic diagram of pick-up unit one embodiment of detection means packaged water oxygen infiltration index for the present invention.
The implication of each Reference numeral is among the figure:
1～quartz crystal oscillator sheet, 2～calcium metal film, 3～epoxy resin, the airtight cavity of 4～testing cassete, 5～film-substrate to be measured, 6～test cavity, 7～lead, 8～oscillator, 9～crystalline substance control instrument.
Embodiment
The present invention has proposed a kind of method and pick-up unit thereof that is used for detection means packaged water oxygen infiltration index with innovating, can detect the total amount of water oxygen infiltration rate and infiltration fast, accurately, online, and sensitivity is up to 1.0 * 10
-6Gm
-2/ d.
The principal character content of this detection method comprises the steps:
(1), at the metal film of the active region of quartz crystal oscillator sheet vacuum moulding machine one deck tool activity;
(2), described quartz crystal oscillator sheet is being transferred under the situation of secluding air among the glove box, the water oxygen content in the described glove box all is lower than 0.1ppm;
(3), in glove box with described quartz crystal oscillator sheet built-in test box, and with encapsulating structure sealing, described encapsulating structure comprises substrate, packaging film or complete substrate and packaging film;
(4), testing cassete is linked to each other and constitutes crystal microbalance with crystal oscillator, brilliant control instrument, power supply, and energized, piezoelectric effect and mass loading effect by crystalline substance control instrument sensing quartz crystal oscillator sheet, export to microprocessor in real time, calculate the quality that metal film absorbs to be increased behind the water oxygen that infiltrates, and then calculate water oxygen infiltration rate and the water oxygen total amount of having infiltrated in the unit interval.
The detailed process of step (4) is: oscillator makes its vibration at high speed for the electric current of quartz crystal oscillator sheet by rapid change, an electronic signal is sent back to brilliant control instrument simultaneously, after receiving electronic signal, circuit in the brilliant control instrument is sent to microprocessor, calculate the per second vibration velocity of crystal-vibration-chip, when water oxygen infiltrates in the chamber to be measured by substrate or encapsulating structure, generate oxide or oxyhydroxide with the active metal film reaction on the quartz crystal oscillator sheet, the crystal-vibration-chip mass loading increases, thereby cause vibration frequency to descend, the value that descends is directly proportional with the water oxygen quality of infiltration, and these information are calculated water oxygen infiltration rate and total amount and the result is presented at crystalline substance by microprocessor and control on the instrument.
Technique scheme can further be optimized, and is embodied in:
This quartz crystal oscillator sheet is the crystal-vibration-chip that is applicable to crystal microbalance, and crystal oscillator frequency is between 0.1MHz～55MHz, and the material of crystal oscillator electrode is a kind of in gold, silver, the aluminium, the gold electrode of preferred crystal oscillator frequency 6MHz; Adopt the metal film of the mode of vacuum evaporation in the active region of quartz crystal oscillator sheet deposition tool activity.Wherein this metal film is assist by film thickness gauge monitoring in real time to control thickness and vacuum-deposited.
And the primary structure feature of this pick-up unit as shown in Figure 1, comprise testing cassete 4, provide device package to carry out the cavity 6 that water oxygen infiltration index detects, the impermeable water oxygen of cavity material itself, it is (not shown that described testing cassete 4 is provided with the quartz crystal oscillator sheet 1 and the crystal-vibration-chip connector on the wall of chamber of the metal-coated membrane 2 that is positioned at cavity 6, routine techniques for electrical control), this crystal-vibration-chip connector links to each other (not shown towards testing cassete 4 cavitys 6 inboards with two electrodes of quartz crystal oscillator sheet 1, routine techniques for electrical control), this testing cassete 4 uses epoxy resin 3 sealings of ultra-violet curing; And quartz crystal oscillator sheet 1 is connected to form the loop of crystal microbalance by crystal-vibration-chip connector and lead 7 and external crystal oscillator 8, brilliant control instrument 9, power supply, power supply connects the 220V electric main, and in addition, it is (not shown that the output terminal of this crystalline substance control instrument 9 also further connects microprocessor, routine techniques for electrical control), carry out high speed, accurate calculating and display result.
Deeply, wherein this metal film is the metallic film of any one or a few formation in tool activity calcium, magnesium, sodium, strontium, potassium, barium, caesium, yttrium, lanthanum, ytterbium, samarium, the erbium, and film thickness is between 10nm～1000nm.Preferred thickness is calcium (Ca) film of 100nm.
This glove box and metal film vacuum evaporation chamber link to each other by a valve (not shown, as to be the routine techniques of electrical control); Glove box is commercial glove box, and the water oxygen content is lower than 0.1ppm, is to use high purity inert gas N
2Or Ar is in conjunction with the interior circulatory function realization of glove box.And being sealed in the mode that encapsulating structure adopted to be measured, the crystal-vibration-chip that will be coated with the active metal film is to use the epoxy resin ultra-violet curing.
Oscillator makes the crystal-vibration-chip vibration at high speed for the electric current of crystal-vibration-chip by rapid change, an electronic signal is sent back to brilliant control instrument simultaneously, after circuit in the brilliant control instrument is received electronic signal, calculate the per second vibration velocity of crystal-vibration-chip, when water oxygen infiltrates in the chamber to be measured by substrate or encapsulating structure, generate oxide or oxyhydroxide with the active metal reaction on the crystal-vibration-chip, the crystal-vibration-chip mass loading increases, thereby cause vibration frequency to descend, the value that descends is directly proportional with the water oxygen quality of infiltration, these information are sent to a microprocessor, calculate water oxygen infiltration rate and total amount and the result is presented at brilliant the control on the instrument.
The case introduction that water oxygen infiltration index detects:
At first at quartz crystal oscillator sheet active region mask vacuum deposited metal Ca film, the quartz crystal oscillator sheet that is coated with the Ca film is transferred to glove box (water oxygen content＜0.1ppm) under situation about not being exposed in the atmosphere, the quartz crystal oscillator sheet that is coated with the Ca film is placed in the special test box, and solidify sealing with film sample epoxy resin UV to be measured, and in atmosphere, the quartz crystal oscillator sheet of testing cassete is linked to each other with oscillator (or claiming oscillator tank), brilliant control instrument (or claiming crystal counter) and power supply, water oxygen can only penetrate in the chamber from film at this moment.Following reaction takes place in the calcium film on the instant and quartz crystal oscillator sheet of the water oxygen that infiltrates:
2Ca+O
2→2CaO
2CaO+H
2O→2Ca(OH)
2
Ca+2H
2O→Ca(OH)
2+H
2
Be that the Ca film can fully absorb the nearly all water oxygen that infiltrates through in the annular seal space, cause the crystal-vibration-chip mass loading to increase.Present embodiment crystal-vibration-chip frequency is 6MHz, and the crystal oscillator frequency counting can be accurate to 0.1Hz, can accurately be weighed to the weight of Δ m=1ng.Encapsulating structure to the Organic Light Emitting Diode product detects, and water oxygen infiltration rate is exceeded standard (＞5 * 10
-6Gm
-2/ d) encapsulating structure, can be observed the descend per half an hour continuous variation of 0.1Hz of frequency, only need a couple of days can accurately record water oxygen permeability state, and the traditional calcium film in laboratory need the above time of several weeks just can estimate the total amount of water outlet oxygen infiltration in conjunction with the CCD method at least; Increase the area of organic light-emitting diode packaging structure to be measured in the testing cassete, can further improve detection efficiency; Also can connect the machine counting and calculate during the test of this dress system, realize that the infiltration of full-automatic water oxygen detects with PC.
In sum, the detection method of a kind of water oxygen infiltration of the present invention index and pick-up unit thereof are by the specific descriptions of embodiment, and its architectural feature and detection principle are by publicity at length.Yet; more than the embodiment of Xiang Ximiaoshuing only innovates essence and provides for deeply understanding the present invention; it is not the diversity that limits the specific embodiment of the invention with this; in every case equivalence replacement or the simple modification of doing based on the foregoing description and detection method thereof all should be contained within the scope of patent protection of patent request of the present invention.
Claims (6)
1. be used for the method for detection means packaged water oxygen infiltration index, it is characterized in that:
(1), at the metal film of the active region of quartz crystal oscillator sheet vacuum moulding machine one deck tool activity;
(2), described quartz crystal oscillator sheet is being transferred under the situation of secluding air among the glove box, the water oxygen content in the described glove box all is lower than 0.1ppm;
(3), in glove box with described quartz crystal oscillator sheet built-in test box, and with identical structure of device package and method sealing, described device encapsulation structure comprises that packaging film, moisture oxygen deaden the substrate of film and the cure package glue of encapsulation junction;
(4), testing cassete is linked to each other and constitutes crystal microbalance with crystal oscillator, brilliant control instrument, power supply, energized, piezoelectric effect and mass loading effect by crystalline substance control instrument sensing quartz crystal oscillator sheet, export to microprocessor in real time, calculate the quality that metal film absorbs to be increased behind the water oxygen that infiltrates, and then calculate water oxygen infiltration rate and the water oxygen total amount of having infiltrated in the unit interval.
2. the method that is used for detection means packaged water oxygen infiltration index according to claim 1, it is characterized in that: the quartz crystal oscillator sheet is the crystal-vibration-chip that is applicable to crystal microbalance described in the step (1), and crystal oscillator frequency is between 0.1MHz～55MHz; The material of crystal oscillator electrode is a kind of in gold, silver, the aluminium.
3. the method that is used for detection means packaged water oxygen infiltration index according to claim 1 is characterized in that: adopt the metal film of the mode of vacuum evaporation in the active region of quartz crystal oscillator sheet deposition tool activity in the step (1).
4. according to claim 1 or the 3 described methods that are used for detection means packaged water oxygen infiltration index, it is characterized in that: described metal film is assist by film thickness gauge monitoring in real time to control thickness and vacuum-deposited.
5. the pick-up unit that is used for detection means packaged water oxygen infiltration index, it is characterized in that comprising: testing cassete, provide encapsulating structure to carry out the cavity that water oxygen infiltration index detects, described testing cassete is provided with the quartz crystal oscillator sheet of metal-coated membrane in the cavity and the crystal-vibration-chip connector on the wall of chamber, and described crystal-vibration-chip connector links to each other with two electrodes of quartz crystal oscillator sheet towards testing cassete cavity inboard; And described quartz crystal oscillator sheet is connected to form the loop of crystal microbalance, the output termination microprocessor of described brilliant control instrument by crystal-vibration-chip connector and lead and external crystal oscillator, brilliant control instrument, power supply.
6. the pick-up unit that is used for detection means packaged water oxygen infiltration index according to claim 5, it is characterized in that: described metal film is the metallic film of any one or a few formation in tool activity calcium, magnesium, sodium, strontium, potassium, barium, caesium, yttrium, lanthanum, ytterbium, samarium, the erbium, and film thickness is between 10nm～1000nm.
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|---|---|---|---|
| CN2010102371065A CN101949813B (en) | 2010-07-27 | 2010-07-27 | Method and device for detecting water oxygen infiltration index in device packaging |
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|---|---|---|---|
| CN2010102371065A CN101949813B (en) | 2010-07-27 | 2010-07-27 | Method and device for detecting water oxygen infiltration index in device packaging |
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| CN101949813A true CN101949813A (en) | 2011-01-19 |
| CN101949813B CN101949813B (en) | 2012-01-11 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103033455A (en) * | 2012-12-12 | 2013-04-10 | 东莞南玻光伏科技有限公司 | Permeable rate test method of solar photovoltaic assembly |
| CN104330345A (en) * | 2014-11-24 | 2015-02-04 | 云南云天化股份有限公司 | Method and device for detecting gas permeability of PVA membrane |
| CN104596906A (en) * | 2015-01-16 | 2015-05-06 | 上海大学 | Water and oxygen air permeability measuring system with multiple measuring heads |
| CN113466101A (en) * | 2021-06-24 | 2021-10-01 | 华中科技大学 | Permeability detection equipment and detection method |
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2010
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Patent Citations (4)
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| WO2003104810A1 (en) * | 2002-06-07 | 2003-12-18 | Sensor Research And Development Corporation | Biological warfare sensor using molecularly imprinted polymers |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103033455A (en) * | 2012-12-12 | 2013-04-10 | 东莞南玻光伏科技有限公司 | Permeable rate test method of solar photovoltaic assembly |
| CN104330345A (en) * | 2014-11-24 | 2015-02-04 | 云南云天化股份有限公司 | Method and device for detecting gas permeability of PVA membrane |
| CN104596906A (en) * | 2015-01-16 | 2015-05-06 | 上海大学 | Water and oxygen air permeability measuring system with multiple measuring heads |
| CN113466101A (en) * | 2021-06-24 | 2021-10-01 | 华中科技大学 | Permeability detection equipment and detection method |
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| Publication number | Publication date |
|---|---|
| CN101949813B (en) | 2012-01-11 |
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