CN106290106A - The steam of encapsulation coating and structure/measuring gas permebility System and method for - Google Patents

The steam of encapsulation coating and structure/measuring gas permebility System and method for Download PDF

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Publication number
CN106290106A
CN106290106A CN201610612736.3A CN201610612736A CN106290106A CN 106290106 A CN106290106 A CN 106290106A CN 201610612736 A CN201610612736 A CN 201610612736A CN 106290106 A CN106290106 A CN 106290106A
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CN
China
Prior art keywords
steam
coating
gas
encapsulation coating
permebility
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Pending
Application number
CN201610612736.3A
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Chinese (zh)
Inventor
王希祖
陈志宽
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Fangyuan Global Yancheng Photoelectric Technology Co Ltd
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Fangyuan Global Yancheng Photoelectric Technology Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
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Publication date
Application filed by Fangyuan Global Yancheng Photoelectric Technology Co Ltd filed Critical Fangyuan Global Yancheng Photoelectric Technology Co Ltd
Priority to CN201610612736.3A priority Critical patent/CN106290106A/en
Publication of CN106290106A publication Critical patent/CN106290106A/en
Pending legal-status Critical Current

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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00Investigating characteristics of particles; Investigating permeability, pore-volume, or surface-area of porous materials
    • G01N15/08Investigating permeability, pore-volume, or surface area of porous materials
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00Investigating characteristics of particles; Investigating permeability, pore-volume, or surface-area of porous materials
    • G01N15/08Investigating permeability, pore-volume, or surface area of porous materials
    • G01N2015/0813Measuring intrusion, e.g. of mercury

Abstract

The invention discloses a kind of steam/measuring gas permebility method of encapsulation coating and structure, can be used for the water oxygen permeability detection of various original position organic/inorganic encapsulation coating and structure, referring more particularly to the direct encapsulation coating of flexible device and the technology of the superelevation steam/oxygen barrier rate of organic electronic device, this is a kind of foundation metering method at molecular chemical reaction.Active metal detecting layer is utilized to touch, after steam/gas that testing sample passes through, produced reaction and the change curve of caused metal detection layer resistance value, then by quantitative analysis resistivity and the change of atomic layer level thickness and calibration, the steam/gas permeability of sample can be calculated.

Description

The steam of encapsulation coating and structure/measuring gas permebility System and method for
Technical field
The present invention relates to the method for testing of the steam/oxygen permeability of high impedance encapsulation coating and structure, refer more particularly to The performance test of the flexible package of the superelevation steam/oxygen barrier rate of organic electronic device the most directly encapsulating structure.
Background technology
Novel organic electronic device, organic light emission, organic electro-optic device and organic field-effect tube owing to himself is frivolous, The advantages such as energy-conservation and self-luminous, have broad application prospects in display and solid-state illumination field.Its outstanding characteristic is by shadow Ring the exploitation of next generation's display electronic product, be future of showing of flexible electronic.
But show according to the research of long-term organic electronics, the composition such as steam in air and oxygen is to organic electronic device Part has fatal impact, and its reason mainly has steam and oxygen that organic each thin layer is had various different reaction and impact, Thus there is the biggest harm in the integral device life-span.If organic electro-optic device can effectively can be sealed, stop steam/ Oxygen touches each organic function layer, it is possible to be greatly improved device lifetime.
A lot of novel encapsulation coating materials and direct combination encapsulating structure are invented and are used, but for efficient envelope Package material and encapsulation technology are it is also proposed that the harshest requirement, and existing means of testing and equipment are also a lack of and imperfection 's.Such as the coating the most directly encapsulated on the dependent coating material encapsulated and device and technology, existing equipment Just cannot accomplish with method directly to measure.Indirectly coating and direct encapsulating structure can only be prepared on different substrates, then Measure.But the method for this indirect measurement is equipment and method is difficulty with the high accuracy of steam and gas and accurately and has The measurement of effect, and measurement to transparent/non-transparent thin film simultaneously.Actual demand has claimed below to measuring system:
A. the detector layer being must have the sensitivity of superelevation;
B. detector will be in close proximity to coating to be measured and structure;
C. when detector runs, outside steam and gases affect measuring accuracy to be less than;
D. it is the change of detector layer can be observed effectively and measure;
E. the saturating rate of water oxygen of sample can be done qualitative and determined quantitative analysis.
Summary of the invention
It is an object of the invention to provide the steam/gas infiltration of a kind of effective high-acruracy survey encapsulation coating and structure Rate method, solves the problem that the steam/gas permeability of current most of dependent encapsulation coating and structure is difficult to measure.This Bright ultimate principle is based on some the water/gas body sensitive materials being inserted in coating and encapsulating structure, observes it gentle with water The increase of the resistance value that body causes after producing chemical reaction and change, I can be by the resistance of the whole detecting layer of quantitative analysis The relation of rate and atomic thickness calculates for stopping envelope coating that detector layer and water/gas body react and structure Steam/oxygen permeability.
Whole detector and encapsulation process are all in an inert atmosphere, and the glove box such as nitrogen, argon etc. completes.Glove Case water oxygen content is less than 1 Ppm.Glass/silicon substrate both can stop that he surveyed device to the compositions such as water/gas body from top to encapsulation Layer saturating, whole encapsulation coating and encapsulating structure can be fixed again, and directly prepare coating and encapsulating structure at substrate Design will not affect one another and be damaged to test layer.In order to ensure detector layer main measuring samples side infiltration in testing Steam/gas reaction also reduces external moisture/gas interference, then device structure design and encapsulation step such as figure are the heaviest Want: coating and encapsulating structure the most even to be completely covered detector layer, and the second coating and encapsulating structure must be insulant.I Pass through:
1. detector layer is directly prepared in the substrate at waterproof oxygen, covers coating material to be measured and encapsulation knot in pure glove box Structure.
2. survey coating material and encapsulating structure is completely covered detector layer, it is ensured that edge's steam infiltration probability is minimum.
3. can be by vacuum and the steam adding absorption in heat abstraction material and oxygen.
Accompanying drawing explanation
The test design structural representation of Fig. 1 high accuracy barrier film.
1. test substrate (silicon chip, glass);
2. leadout electrode;
3. encapsulation coating and multilayer encapsulation structure;
4. thin film active metal sensor layer;
5. resistance detecting circuit.
Fig. 2 example test result.
Detailed description of the invention
According to the design and processes of invention, one of them implementations is to use following steps:
The first step, be ready to treat can packaged glass or silicon chip substrate, surface can be carried out.And put into vacuum drying oven removal Steam and oxygen more than absorption.By incoming to glass or silicon chip fine vacuum cavity, utilize evaporating deposition technique (thermal evaporation, gas phase Deposition, sputtering, epitaxial growth, etc.) deposition one layer derivation silver electrode (low-resistance value).Again test zone grow one layer of steam/ Detection of gas layer (proper test area is 1X1 centimetre, the calcium film of 100 to 200 nanometers).
Second step, deposits one layer of encapsulated layer to be recorded or composite layered structure on the detector of the first step.
3rd step, it is also possible to biography sample, to glove box, utilizes other preparation methoies to be coated with one layer or several layers of thin film to be measured, this In use spin coating prepare the encapsulation oxidant layer of different-thickness on the detector.
4th step, is passed to packaged device in vacuum chamber, extracts unnecessary gas and cavity.
5th step, at glove box, utilizes UV lamp or vacuum oven cure package coating, detector layer and the external world is passed through Coating to be measured completely cuts off completely.
7th step, packaged after device, spread out of glove box.It is placed on external environment condition or the controlled test of humidity temperature In case (or in cavity of single atmosphere).
8th step, by connection electrode to the test system of resistance Yu time, observes whole device resistance value and time Change curve.
Wherein test result input system, according to qualitative and quantitative data base and parameter, calculates steam/gas Permeability through thin film.Result shows, at 40 degree, in 90% humidity measurement cavity, by the mensuration of resistivity, in sample 200 The nanometer calcium detector complete oxidation time is 56 hours, be converted into every square meter penetrate the hydrone of film have altogether 0.277 gram/flat Rice.Final steam permeability WVTR=0.277g/m2 × (24 ÷ 56)=1.2 × 10-1 gram/day. square meter.Thin film at 40 degree, In the environment of 90%, steam permeability is more than 1.2 × 10-1 gram/day. square meter.

Claims (7)

1. the steam of an encapsulation coating and structure/measuring gas permebility system, it is characterised in that including: deposition compact serves as a contrast Electrode layer at the end, and the conduction detector layer relying on steam/gas sensitive material to prepare being deposited on testing sample, its The change of resistivity of material can be caused when touching the gas such as steam or oxygen;Preparation coating to be measured on electrode is tied with thin film Structure and can monitored resistance value change detector.
The steam of encapsulation coating the most according to claim 1 and structure/measuring gas permebility system, it is characterised in that Described dense substrate is selected from metal-oxide, silicon oxide, glass, silicon chip.
The steam of encapsulation coating the most according to claim 1 and structure/measuring gas permebility system, it is characterised in that Described electrode layer, its material is selected from high connductivity thin-film material, gold, silver, copper, ITO, FTO, ZAO.
The steam of encapsulation coating the most according to claim 1 and structure/measuring gas permebility system, it is characterised in that Described steam/gas sensitive material is selected from calcium metal or magnesium.
The steam of encapsulation coating the most according to claim 1 and structure/measuring gas permebility system, it is characterised in that Described steam/gas sensitive material is selected from conducting polymer, metal alloy, metal-oxide and mixture.
The steam of encapsulation coating the most according to claim 1 and structure/measuring gas permebility system, it is characterised in that The solution manufacturing methods such as described coating to be measured and the preparation of membrane structure can pass through spin coating, evaporation, chemical deposition.
7. the steam of encapsulation coating and structure/measuring gas permebility method, described method includes: make steam/gas only Detector layer contact surface, observation detector layer resistivity and the change of time is permeated, according to survey from testing coating and structure side Amount result calculates steam/gas permeability coefficient.
CN201610612736.3A 2016-07-29 2016-07-29 The steam of encapsulation coating and structure/measuring gas permebility System and method for Pending CN106290106A (en)

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CN201610612736.3A CN106290106A (en) 2016-07-29 2016-07-29 The steam of encapsulation coating and structure/measuring gas permebility System and method for

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CN201610612736.3A CN106290106A (en) 2016-07-29 2016-07-29 The steam of encapsulation coating and structure/measuring gas permebility System and method for

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CN106290106A true CN106290106A (en) 2017-01-04

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108074833A (en) * 2017-12-18 2018-05-25 武汉华星光电半导体显示技术有限公司 A kind of testing film and for assessing the gauge of thin-film package performance and test method
CN109142185A (en) * 2018-08-30 2019-01-04 上海大学 A kind of testing vapor transmission system and method
WO2021036043A1 (en) * 2019-08-26 2021-03-04 武汉华星光电半导体显示技术有限公司 Method for testing thin film encapsulation performance
US11569447B2 (en) 2019-08-26 2023-01-31 Wuhan China Star Optoelectronics Semiconductor Display Technology Co., Ltd. Method for testing performance of thin-film encapsulation

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108074833A (en) * 2017-12-18 2018-05-25 武汉华星光电半导体显示技术有限公司 A kind of testing film and for assessing the gauge of thin-film package performance and test method
CN108074833B (en) * 2017-12-18 2021-03-02 武汉华星光电半导体显示技术有限公司 Test film, jig for evaluating film packaging performance and test method
CN109142185A (en) * 2018-08-30 2019-01-04 上海大学 A kind of testing vapor transmission system and method
CN109142185B (en) * 2018-08-30 2020-05-05 上海大学 Water vapor transmittance testing system and method
WO2021036043A1 (en) * 2019-08-26 2021-03-04 武汉华星光电半导体显示技术有限公司 Method for testing thin film encapsulation performance
US11569447B2 (en) 2019-08-26 2023-01-31 Wuhan China Star Optoelectronics Semiconductor Display Technology Co., Ltd. Method for testing performance of thin-film encapsulation

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Application publication date: 20170104