CN102175624A - Method for testing water vapor transmittance - Google Patents
Method for testing water vapor transmittance Download PDFInfo
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- CN102175624A CN102175624A CN 201110062103 CN201110062103A CN102175624A CN 102175624 A CN102175624 A CN 102175624A CN 201110062103 CN201110062103 CN 201110062103 CN 201110062103 A CN201110062103 A CN 201110062103A CN 102175624 A CN102175624 A CN 102175624A
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Abstract
The invention relates to a method for testing water vapor transmittance, which is used for detecting a packing film, in particular to a film package process and test of an organic light-emitting device. The method is a molecule hygrometer method. In the principle of the test method, after an organic material absorbs water, the photoluminescence spectrum of the organic material is change, and the permeability of a film is obtained by quantitatively analyzing the change of photoluminescence spectrum of the organic material. The method comprises the following steps of: firstly manufacturing an organic functional layer on a substrate (a glass substrate, a flexible substrate and others); depositing a packing film on the organic layer; then testing the change of the photoluminescence spectrum of the organic material with time; and calculating the water vapor transmittance of the packing film according to the obtained spectrum and time data.
Description
Technical field
The present invention relates to a kind of organic electroluminescence device packaging film steam transmission measurement method, can be used for the detection of packaging film, relate in particular to the thin-film package technology and the test of organic electroluminescence device, is a kind of molecule hygrometer method.
Background technology
Organic electroluminescence device (Organic Light Emitting Device, OLED) because have that ultralight is thin, high brightness, response are fast, low-power consumption, efficient is high and make features such as simple, be widely used in flat-panel monitor, fields such as module backlight and illumination, its principle of luminosity is the extremely thin organic material of deposition between two electrodes, this luminous organic material is passed to direct current make it luminous.
Studies show that, compositions such as airborne steam and oxygen are very big to the life-span influence of OLED, its reason is mainly considered from the following aspect: will inject electronics from negative electrode during the work of OLED device, this just requires the negative electrode work function low more good more, but do these metals of negative electrode such as aluminium, magnesium, calcium etc., general relatively more active, easy steam of coming in infiltration reacts.In addition, chemical reaction also can take place with hole transmission layer and electron transfer layer (ETL) in steam, and these reactions all can cause component failure.Therefore OLED is effectively encapsulated, the steam in each functional layer that makes device and the atmosphere, oxygen etc. become to separate, and just can prolong device lifetime greatly.
Traditional OLED device is to go up at rigid substrates (glass, metal) to make electrode and each organic function layer, and the encapsulation that this class device is carried out generally is to add a cover plate to device, and substrate and lid is bonding.So just between substrate and cover plate, formed a cover, device and air are separated, compositions such as airborne water, oxygen can only permeate to device inside by the epoxy resin between substrate and the cover plate, therefore, prevented that more effectively compositions such as each functional layer of OLED and negative electrode and airborne water, oxygen from reacting.
To the used cover plate of encapsulation that OLED carries out, use two kinds of materials of glass and metal usually.Whole encapsulation process is finished in the glove box as nitrogen, hydrogen etc. at filling with inert gas.Moisture content should be less than 1 ppm in the glove box.Compositions such as metal cover board both can block water, oxygen can make device firm again, but its opaqueness have limited the application of this method for packing on organic electroluminescence device to the infiltration of device package.In addition, to pay special attention to the electrode that metal cover board can not touch device when encapsulating, in order to avoid cause short circuit with metal cover board.Need fluid sealant during the cover plate encapsulation, because the poriness of fluid sealant, therefore make airborne moisture penetration enter device inside easily, in this packaged type, generally add calcium oxide or baryta and be absorbed in when being coated with epoxy resin as drying agent and residual moisture during encapsulation at device inside.
ORGANIC ELECTROLUMINESCENCE DISPLAYS is compared with other forms of demonstration, has an important advantage can realize flexible the demonstration exactly.People such as Gustafsson had invented the OLED based on the flexible high molecular material on PET (the ploy ethylene terephthalate) substrate in 1992; People such as Forrest in 1997 have invented the OLED of flexible small molecule material.This class display spare softness can be out of shape and be not fragile, can be installed in curved surface, even can dress, thereby becomes the international research focus that shows industry day by day.For flexible OLED, traditional method for packing can not curl because of cover plate, thereby is invalid.With film directly encapsulation compare with traditional glass cover encapsulation, device is thinner, and needn't worry the wearing and tearing of polymer lid when flexibility shows, for the development of flexible OLED lays the first stone.
At present, encapsulated layer adopts SiNx, SiOx or Al usually
2O
3Etc. inorganic material or organic material, the encapsulated layer that also has is taked the mixed single or multiple lift structure that makes of organic-inorganic material.Make the life-span of OLED surpass 10000h, reach actual application requirements, so, this device be encapsulated in 39 ℃, relative humidity is that water vapor permeable rate (WVTR) is less than 10 under 95% the condition
-6* 10 g/m/day, OTR oxygen transmission rate (OTR) then is less than 10
-5Cm
3/ m
2/ day.The measurement of so little numerical value is a very big challenge concerning at present more popular measurement means.To measure the encapsulation characteristic of OLED, measuring system is had following requirement:
A. the measurement minimum value of system must can reach above-mentioned requirements.
B. system can measure the encapsulation characteristic of traditional OLED and flexible OLED.
C. can do qualitative and quantitative two kinds of analyses to the water oxygen permeability of device.
Summary of the invention
The object of the present invention is to provide a kind of method of effective measurement OLED encapsulation steam transmitance, solve the problem that present OLED packaging film steam transmitance is difficult to measure.Ultimate principle of the present invention is based on some organic materials and is easy to steam generation chemical reaction, and these organic materials with steam generation chemical reaction after photoluminescence spectra can die down, thereby our variation by the integrated intensity of quantitative test organic material photoluminescence spectra in the overall optical spectral limit calculates the steam transmitance that is used to stop the packaging film that organic material and steam reacts.
According to the foregoing invention design, the present invention adopts following technical step, and process flow diagram is seen Fig. 3:
A. be ready to substrate, and on substrate, utilize vacuum evaporation (perhaps method such as plasma enhanced chemical vapor deposition or magnetron sputtering) deposition one deck easily and the thickness of steam generation chemical reaction be h
0Organic material film.
B. on organic material again preparation (methods such as vacuum evaporation or plasma enhanced chemical vapor deposition or magnetron sputtering) one deck be used to the packaging film that stops organic material and steam to react, and pick up counting.
C. we measure photic spectral measurement to sample the time of fixed interval, and preserve the curve of spectrum data that obtain.
D. we suppose that the steam transmitance of glass substrate is 0, and the photic spectral intensity of definition organic material is
, will
Carry out normalization, the integrated intensity of organic material in the overall optical spectral limit is so
, on the unit interval unit area with the thickness of the organic material of steam generation chemical reaction
, then on the unit area in t hour the steam transmitance of packaging film can be expressed as
, wherein n is the wavelength of spectrum,
Be steam transmitance coefficient, size depends on the organic material that is used to test,
Be the molecular weight of hydrone,
Molecular weight for organic material.
This method is the steam transmitance of measuring packaging film according to the variation of photoluminescence spectra before and after some organic material and the steam generation chemical reaction.Its steam transmitance that both can be used for various packaging films on the glass substrate is measured, and the steam transmitance that also can be used for flexible base, board is measured.Its related organic material easy and steam generation chemical reaction includes the used red, green, blue three look materials of organic electro luminescent, small molecule material and macromolecular material.The packaging film steam method of testing of described organic electroluminescence device can prepare corresponding molecule hygrometer.
The present invention has following conspicuous outstanding substantive distinguishing features and remarkable advantage: (1) does not need special testing tool, can utilize existing fluorospectrophotometer to measure; (2) measure accurately, the steam that the method is measured is the steam that penetrates into organic material layer, and it is extensive not comprise that film itself absorbs moisture (3) the method test specification, is applied to various organic electroluminescence devices; (4) the method is simple and reliable, can reduce equipment investment significantly; (5) the method can realize real-time online measuring, monitoring in real time in the technological process of producing organic electroluminescent.
Description of drawings
Fig. 1 is the structures of samples synoptic diagram.Comprise glass substrate 1, electroluminescent organic material layer 2, encapsulated layer 3 compositions.Described electroluminescent organic material layer 2 is produced on the glass substrate 1, and encapsulated layer 3 is produced on the organic electro luminescent material layer 2.
Fig. 2 is the curve map of the photic spectrum of sample at the different time point measurement.T1, T2, T3, T4 represent Measuring Time respectively.
Fig. 3 is the test flow chart of method of testing of the present invention.
Embodiment
The present invention is described in detail below in conjunction with embodiment:
Embodiment one: concrete steps are as follows:
A. glass substrate is cleaned and oven dry, vacuum evaporation thickness is 100 nm's on substrate earlier
Organic film exists then
Preparing a layer thickness on the film again is the LiF packaging film of 200 nm, and structural representation is seen Fig. 1.
B. the sample for preparing is taken out in the test environment that is placed on fixedly humidity and oxygen content, the photoluminescence spectra of a sample of measurement is designated as
And preserve, pick up counting.
C. measured the photoluminescence spectra of a sample at interval in 12 hours, and the curve of spectrum data that obtain are preserved, the measurement result of sample in the time of 12,24,36 hours seen Fig. 2.
D. we suppose that the steam transmitance of glass substrate is 0, and the photic spectral intensity of sample is when defining 36 hours
, will
Carry out normalization, the integrated intensity of organic material in the overall optical spectral limit is so
, on the unit interval unit area with the thickness of the organic material of steam generation chemical reaction
, then on the unit area in t hour the steam transmitance of packaging film can be expressed as
, wherein
Be 0.15,
Be 18,
Be 459.43,
Be 0.2 as calculated,
Be 100 nm, t is 36 hours, calculates WVTR at last and is about 0.078 g/m/day.
Behind the print that completes, between measure the photoluminescence spectra of print at regular intervals, obtain a series of photoluminescence spectra data, by calculating the integrated intensity of organic material photoluminescence spectra in the overall optical spectral limit as can be seen As time goes on, the organic material photoluminescence spectra obviously weakens, and we can draw the steam transmitance of packaging film by further calculating.
Embodiment two: present embodiment and embodiment one are basic identical, and different is: the organic film material easy and steam generation chemical reaction of vacuum evaporation is the Rubrene of thickness 100 nm on substrate.
Embodiment three: present embodiment and embodiment one are basic identical, and different is: the encapsulated layer material that deposits on organic film is the ZnS of 200 nm.
Embodiment four: present embodiment and embodiment one are basic identical, and different is: the encapsulated layer material that deposits on organic film is the SiNx of 200 nm.
Embodiment five: present embodiment and embodiment one are basic identical, and different is: the encapsulated layer material that deposits on organic film is the SiOx of 200 nm.
Claims (2)
1. the method for testing of a steam transmitance is characterized in that testing procedure is as follows:
A. be ready to substrate, and on substrate, utilize method deposition one deck thickness easy and steam generation chemical reaction of vacuum evaporation or plasma enhanced chemical vapor deposition or magnetron sputtering to be h
0Organic material film utilizes the method for vacuum evaporation or plasma enhanced chemical vapor deposition or magnetron sputtering to prepare one deck then on organic material again and is used to the packaging film that stops organic material and steam to react;
B. the sample for preparing is taken out in the test environment that is placed on fixedly humidity and oxygen content, measure the photoluminescence spectra of a sample and also preserve, pick up counting;
C. the time of fixed interval is measured photic spectral measurement to sample, and preserves the curve of spectrum data that obtain;
D. the steam transmitance of supposing glass substrate is 0, and the photic spectral intensity of definition organic material is
, will
Carry out normalization, the integrated intensity of organic material in the overall optical spectral limit is so
, on the unit interval unit area with the thickness of the organic material of steam generation chemical reaction
, then on the unit area in t hour the steam transmitance of packaging film can be expressed as
, wherein
Be steam transmitance coefficient, size depends on the organic material that is used to test,
Be the molecular weight of hydrone,
Molecular weight for organic material.
2. film steam transmission measurement method according to claim 1 is characterized in that among the described step C, regulates and selects different excitation wavelengths to measure.
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|---|---|---|---|
| CN 201110062103 CN102175624A (en) | 2011-03-16 | 2011-03-16 | Method for testing water vapor transmittance |
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|---|---|---|---|
| CN 201110062103 CN102175624A (en) | 2011-03-16 | 2011-03-16 | Method for testing water vapor transmittance |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102636441A (en) * | 2012-05-02 | 2012-08-15 | 厦门华联电子有限公司 | Test evaluation method of LED (light emitting diode) packaging adhesive |
| DE102013022032A1 (en) | 2013-12-19 | 2015-06-25 | Technische Universität Ilmenau | Method for detecting foreign substances or degradation products in encapsulated systems and its use |
| CN104777085A (en) * | 2015-03-23 | 2015-07-15 | 中山大学 | Gas transmission rate multi-method measurement and correction system for packaging material |
| CN104777084A (en) * | 2015-03-23 | 2015-07-15 | 中山大学 | Lock-in amplifier based gas transmission rate optical measurement method and system |
| CN105973548A (en) * | 2016-05-07 | 2016-09-28 | 上海大学 | Water vapor transmittance testing clamp based on active metal electrical method |
| CN106338462A (en) * | 2016-08-25 | 2017-01-18 | 泰通(泰州)工业有限公司 | Semi-quantitative testing apparatus and semi-quantitative testing method for water vapor permeation capability of double-glass module edge |
| CN107449704A (en) * | 2017-05-22 | 2017-12-08 | 茆胜 | The method of testing of film water vapor transmittance |
| CN109238940A (en) * | 2018-09-29 | 2019-01-18 | 汉能新材料科技有限公司 | A kind of packaging film method for testing vapor transmission |
| CN109696390A (en) * | 2019-01-28 | 2019-04-30 | 中山大学 | The device of electric-resistivity method testing film gas permeation rate and its production, test method |
| CN109890287A (en) * | 2016-10-04 | 2019-06-14 | 特里邦美公司 | The method of Non-invasive measurement blood hemoglobin concentration and oxygen concentration |
| CN111781120A (en) * | 2020-06-24 | 2020-10-16 | 吉林大学 | Testing method for thin film package |
| CN111982885A (en) * | 2020-07-10 | 2020-11-24 | 绍兴秀朗光电科技有限公司 | Non-contact type film water oxygen transmission performance testing method |
| CN111987235A (en) * | 2020-07-10 | 2020-11-24 | 绍兴秀朗光电科技有限公司 | Non-contact type film water oxygen transmission performance testing device and production process thereof |
| US11508932B2 (en) | 2017-07-19 | 2022-11-22 | Beijing Boe Technology Development Co., Ltd. | Package structure, display panel, display device, and method for detecting package structure |
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| CN1976088A (en) * | 2006-12-29 | 2007-06-06 | 清华大学 | Organic electro luminescent device |
| US20090110896A1 (en) * | 2007-10-30 | 2009-04-30 | Fujifilm Corporation | Silicon -nitrogen compound film, and gas-barrier film and thin-film device using the silicon-nitrogen compound film |
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| CN1976088A (en) * | 2006-12-29 | 2007-06-06 | 清华大学 | Organic electro luminescent device |
| US20090110896A1 (en) * | 2007-10-30 | 2009-04-30 | Fujifilm Corporation | Silicon -nitrogen compound film, and gas-barrier film and thin-film device using the silicon-nitrogen compound film |
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Cited By (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102636441A (en) * | 2012-05-02 | 2012-08-15 | 厦门华联电子有限公司 | Test evaluation method of LED (light emitting diode) packaging adhesive |
| DE102013022032A1 (en) | 2013-12-19 | 2015-06-25 | Technische Universität Ilmenau | Method for detecting foreign substances or degradation products in encapsulated systems and its use |
| CN104777085B (en) * | 2015-03-23 | 2017-07-18 | 中山大学 | A kind of gas permeation rate multi-method measurement correction system of encapsulating material |
| CN104777085A (en) * | 2015-03-23 | 2015-07-15 | 中山大学 | Gas transmission rate multi-method measurement and correction system for packaging material |
| CN104777084A (en) * | 2015-03-23 | 2015-07-15 | 中山大学 | Lock-in amplifier based gas transmission rate optical measurement method and system |
| CN104777084B (en) * | 2015-03-23 | 2018-02-16 | 中山大学 | A kind of gas permeation rate measuring method and system based on lock-in amplifier |
| CN105973548A (en) * | 2016-05-07 | 2016-09-28 | 上海大学 | Water vapor transmittance testing clamp based on active metal electrical method |
| CN106338462A (en) * | 2016-08-25 | 2017-01-18 | 泰通(泰州)工业有限公司 | Semi-quantitative testing apparatus and semi-quantitative testing method for water vapor permeation capability of double-glass module edge |
| CN109890287A (en) * | 2016-10-04 | 2019-06-14 | 特里邦美公司 | The method of Non-invasive measurement blood hemoglobin concentration and oxygen concentration |
| CN109890287B (en) * | 2016-10-04 | 2021-11-02 | 特里邦美公司 | Method for non-invasive determination of hemoglobin concentration and oxygen concentration in blood |
| CN107449704A (en) * | 2017-05-22 | 2017-12-08 | 茆胜 | The method of testing of film water vapor transmittance |
| US11508932B2 (en) | 2017-07-19 | 2022-11-22 | Beijing Boe Technology Development Co., Ltd. | Package structure, display panel, display device, and method for detecting package structure |
| CN109238940A (en) * | 2018-09-29 | 2019-01-18 | 汉能新材料科技有限公司 | A kind of packaging film method for testing vapor transmission |
| CN109696390A (en) * | 2019-01-28 | 2019-04-30 | 中山大学 | The device of electric-resistivity method testing film gas permeation rate and its production, test method |
| CN111781120A (en) * | 2020-06-24 | 2020-10-16 | 吉林大学 | Testing method for thin film package |
| CN111781120B (en) * | 2020-06-24 | 2021-06-18 | 吉林大学 | Testing method for thin film package |
| CN111982885A (en) * | 2020-07-10 | 2020-11-24 | 绍兴秀朗光电科技有限公司 | Non-contact type film water oxygen transmission performance testing method |
| CN111987235A (en) * | 2020-07-10 | 2020-11-24 | 绍兴秀朗光电科技有限公司 | Non-contact type film water oxygen transmission performance testing device and production process thereof |
| CN111987235B (en) * | 2020-07-10 | 2023-12-01 | 绍兴秀朗光电科技有限公司 | Non-contact type thin film water-oxygen permeability testing device and production process thereof |
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Application publication date: 20110907 |