CN104777085B - A kind of gas permeation rate multi-method measurement correction system of encapsulating material - Google Patents
A kind of gas permeation rate multi-method measurement correction system of encapsulating material Download PDFInfo
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Abstract
The present invention discloses a kind of gas permeation rate multi-method measurement correction system of encapsulating material, the test sample of polylith film-form is arranged on substrate, multiple reaction amount detecting devices detect the amount of the designated gas chemically reacted with each piece of test sample respectively, the amount for the designated gas that system chemically reacts according to each piece of test sample, surface area and testing time in conjunction with packing colloid calculate the transmitance for the designated gas for obtaining encapsulating material, the present invention verifies the accuracy for the transmitance that each test sample is measured according to the ratio of each piece of test sample, and the transmitance obtained to each test sample is weighted average, obtain corrected transmitance.The present invention increases measurement range using the different measurement sensitivity of multi-method.The system that the present invention constructs a multi-method, many test sample measurement results are mutually corrected, is able to verify that the Measurement reliability of every kind of method during each measurement, can further eliminate measurement error, improve the accuracy and resolution of measurement.
Description
Technical field
The present invention relates to moisture-vapor transmission fields of measurement, more particularly, to a kind of gas permeation rate of encapsulating material
Multi-method measures correction system.
Background technology
Organic Light Emitting Diode (OLED) is to be injected with after machine semiconductive thin film to be combined to produce by positive negative carrier to light
Luminescent device.Organic Light Emitting Diode (OLED) has actively luminous, high brightness, high-contrast, ultra-thin, inexpensive, low work(
Consumption, quick response, wide viewing angle, the advantages of can be flexible, with the potentiality for replacing traditional LCD.Flexible Displays have flexible, light
Thin and non-friable characteristic, is increasingly becoming the study hotspot that the whole world shows industry.OLED can flexibility characteristics promote OLED's
Technology develops and product marketization.However, OLED haves the shortcomings that device lifetime is short.Because vapor, oxygen are all
It can be chemically reacted to a certain extent with OLED electrode and luminous organic material, and then cause the performance of OLED special
Property change.For example：Blackspot effect, hot-spot, organic material aging etc..OLED water unstable has severely impacted OLED
The working life and exhibit stabilization of device, hinder the marketization of OLED Display Techniques.Research based on early stage, will make OLED
Device lifetime reaches the 10^4h of practicality, and the substrate and encapsulated layer of device should be less than 5 × 10^-6g/ to the infiltration rate of steam
m2D, its implication is the quality for the vapor that unit area is passed through daily.Therefore, in order to measure OLED encapsulation, backing material
High water resistance, precision reaches 10^-6g/m2D moisture-vapor transmission (WVTR) method of measuring seems increasingly important.Mesh
Before, more high-precision WVTR measuring methods of main flow, including sensor method, radioactive-tracer method, mass spectrography, based on Tunable
The steam detection method of Diode Laser Absorption Spectroscopy (TDLAS) technology, Ca methods.
The Mocon of MOCON companies of the U.S.Model 2WVTR testers employ the oxygen of coulomb electricity five
Change the method for two phosphorus AquatraceTM sensors measurement, its resolution has reached 5 × 10^-5g/m2d.Its principle is that structure is thin
Membrane sample works as two cavitys of connecting valve：The moist chamber and drying chamber of humidity, temperature-controllable.According to Fick's first law and henry
Sharp law, the vapour concentration gradient at film two ends causes steam to be spread from moist cavity to drying chamber.Steam is diffused into drying chamber,
Vapor into sensor very is converted into measurable electricity, and then calculates steam permeating rate.Two cavity type knots
Edge leakage problem occurs in the bonding limitation of structure measured material.When detection moisture is less than 10^-5g/m2During d, coulomb sensing
Technology is infeasible.
D.Ralf et al. uses reflectivity trace method, and its principle is the tracer measurement by the use of heavy water (tritium) as vapor
Through the steam permeating rate of measured material.Two cavity structures, gas compartment and the measuring chamber for being passed through methane full of HTO gases
Junction rubber seal measured material.By determining the other amounts of the HTO through measured material, measured material is calculated
WVTR.Reflectivity trace method equipment is complicated, expensive, and radwaste can be caused to pollute.
Mass spectrography measurement is to measure the background partial pressure of vapor and satisfying after infiltration in vacuum chamber using QMS
And partial pressure, and the moisture vapor transmission of measured material is calculated using the analysis method of partial pressure device e measurement technology, successively
Built etc. by University of Electronic Science and Technology Li Jun and the proposition such as Germany Philip Hulsmann.Its detection accuracy can reach 10^-6g/m2d。
QMS make use of the ions of the different charge-mass ratios different principle of movement locus under electromagnetic field effect, point of detection gas
Pressure.Measuring system includes controllable gas compartment, pumped vacuum systems of the vacuum chamber equipped with QMS, humiture etc., structure
Complexity, it is costly.
Steam detection based on Tunable Diode Laser Absorption Spectroscopy (TDLAS) technology
Method.Tunable diode laser absorption spectroscopy analysis is the absorption according to gas to electromagnetic wave, and every kind of molecule is due to constituting and tying
Structure decision has specific energy state, and incident light is subsequently absorbed in the material when meeting bohr condition.Every kind of molecule has specific red
Outer absorption spectrum.TDLAS technologies are that the characteristic absorption area for passing through vapor is tuned using laser wavelength, and spectrum sensor is visited
The laser signal through gas measured is demodulated, and analyzes the component and concentration of gas, and then calculate the concentration of vapor.
TDLAS includes on signal detecting method：Direct absorption, wavelength modulation, frequency modulation(PFM) and balance Detection Techniques.TDLAS water steams
Gas detection accuracy can reach that 100ppb, detectable WVTR have reached 10^-7g/m2d.The HiBarSens of German SEMPA companies
Instrument is exactly that make use of TDLAS technologies, and resolution ratio reaches 10^-6g/m2d。
The method for being now widely used in the measurement of OLED encapsulating materials water vapor transmittance is Ca reaction methods.Ca reaction methods are to be based on
Ca chemical activity and vapor occurs to chemically react, and is characterized by detecting Ca extent of corrosions through encapsulating material and Ca
The steam vapour amount of reaction.The method of detection Ca extent of corrosions typically has two kinds：Conductivity measurement and optical means.The side of electricity
Method, is changed with time calculating moisture vapor transmission by detecting the electrical conductivity of Ca films.Optical method, passes through light microscope
Gather the Ca film images of different time points, and the ratio of image processing and analyzing clear area and corrosion region estimates the amount through water.
The estimation program water vapor transmittance limit that Paetzold R, Nisato G et al. are proposed can reach 3 × 10^-7g/m2d.However,
Ca reaction methods can not exclude oxygen and Ca reaction, it is impossible to distinguish oxygen and the respective transmitance of vapor.
At present, one kind is additionally provided by determining luminescent material luminous signal, so as to characterize the encapsulation of sealing luminescent material
The optical means of material water vapor transmittance.Formed under vacuum conditions after plugging meter sample, utilize optical measuring system first
The luminous signal intensity I of secondary measurement luminescent material0, measurement sample is stored in the controllable environment of humiture.At interval of identical
Individual hour t measures the luminescence generated by light optical signal of a luminescent material, obtains specifying the I under the time1、I2、I3........In.Return
One changes linear process, and unit interval t change in optical signal rate is：
Correspondingly, thickness is L0The reaction of luminescent material and vapor occur rotten to cause non-luminous amount of thickness Δ L to be
Unit interval, the luminescent material variable mass that area is B is：
In formula, WVTR [OLEM] is the water vapor transmittance of luminescent material, refers to the unit interval, and the steam that unit area is passed through is total
Amount.
The water vapor transmittance of encapsulating material is set as WVTR [H2O], unit interval area is saturating for the steam of A encapsulating material
It is excessively：
m[H2O]=WVTR*A
According to luminescent material and the chemical equation of steam, the amount of the luminescent material reacted with the steam through encapsulating material
For：
M[H2O] it is H2O molal weight, M [OLEM] is the molal weight of luminescent material used, and n is chemical equation
Proportioning number.
Try to achieve the water vapor transmittance of encapsulating material：
This method precision reaches OLED encapsulating materials WVTR requirements, measuring method simplicity, low cost, but draws during measurement
Enter external light source and interference necessarily is produced to the small-signal that luminescent material is produced, cause measurement result deviation.
Existing moisture-vapor transmission e measurement technology has that measurement accuracy is low, measuring method is complicated or cost is high etc. and lacked
Fall into, it is impossible to meet OLED encapsulating material moisture-vapor transmission measurement requests, and the method for these measurements all has some not
Variable error component, this produces negative interaction for the accuracy and precision of further lifting measurement.
The content of the invention
The present invention verifies every during measurement every time to overcome above-mentioned prior art measurement gas permeation rate to there is the defect of error
The Measurement reliability of the method for kind can eliminate a kind of envelope of measurement error, the accuracy for improving measurement and resolution there is provided a kind of
The gas permeation rate multi-method measurement correction system of package material, the system increases measurement using each method sensitivity difference
Scope.
In order to solve the above technical problems, technical scheme is as follows：
A kind of gas permeation rate multi-method measurement correction system of encapsulating material, the system is used to measure and correct encapsulation
The transmitance of the designated gas of material, the system includes substrate, encapsulating material, test sample and reaction amount detecting device, many
The test sample of block film-form is arranged on substrate, and encapsulating material encapsulates whole substrate, make test sample be located at encapsulating material with
In confined space between substrate, the test sample can chemically react with the designated gas, multiple reacting dose inspections
Survey the amount that device detects the designated gas chemically reacted with each piece of test sample respectively.
In a kind of preferred scheme, the test sample is using embedded photoluminescent material, electroluminescent material or active gold
One or more in category, when the test sample is embedded photoluminescent material or electroluminescent material, reaction amount detecting device inspection
Survey the weak amount of test sample optical excitation signal, and weak amount and test sample according to optical excitation signal and designated gas is anti-
Ratio is answered to calculate the amount of the designated gas chemically reacted with the test sample；When the test sample is active metal, instead
Answer amount detecting device to detect the resistance of active metal and calculate the amount of the designated gas chemically reacted with the test sample.
In a kind of preferred scheme, when the test sample is embedded photoluminescent material or electroluminescent material, its correspondence
Reaction amount detecting device include：
Excitation apparatus：Excited for use light or electrically excited mode makes test sample produce exciting light, the light is excited
Excited for laser reflection or laser transmission is excited；
Focused light passages：Exciting light for test sample to be produced converges to optical chopper.
Optical chopper：For being modulated with default reference frequency to exciting light；
Photo-detector：Optical signal is converted to electric signal after being modulated through optical chopper；
Lock-in amplifier：For extracting and exporting optical excitation signal, the lock-in amplifier is using reference frequency signal as ginseng
Signal is examined, the electric signal exported using photo-detector is input signal.
In a kind of preferred scheme, the substrate is flexible base board or rigid substrates, and the test sample of film-form is direct
Form on substrate.
In a kind of preferred scheme, the method that film-form measurement sample is formed on substrate uses wet method processing procedure or dry method
Processing procedure.
In a kind of preferred scheme, the packaged type of sample includes rigidity encapsulation and flexible package.
In a kind of preferred scheme, a variety of methods include photoluminescence method, electroluminescent method and active metal electric-resistivity method.
In a kind of preferred scheme, the designated gas that the system chemically reacts according to each piece of test sample
Amount, surface area and testing time in conjunction with packing colloid calculate the transmitance for the designated gas for obtaining encapsulating material, to each
The transmitance that test sample is obtained is weighted averagely, obtains corrected transmitance.
In a kind of preferred scheme, the designated gas that the system chemically reacts according to each piece of test sample
Amount, surface area and testing time in conjunction with packing colloid calculate the transmitance for the designated gas for obtaining encapsulating material, according to each
The ratio of block test sample verifies the accuracy for the transmitance that each test sample is measured.
In a kind of preferred scheme, the designated gas that the system chemically reacts according to each piece of test sample
Amount, surface area and testing time in conjunction with packing colloid calculate the transmitance for the designated gas for obtaining encapsulating material, sensitivity
Different a variety of methods correction measurements, because sensitivity is different, the high method of sensitivity can survey the situation of gas permeation rate very little,
The low method of sensitivity can survey gas permeation rate very big situation.Therefore, the different a variety of methods correction measurement of a variety of sensitivity,
Measurement range includes a variety of method measurement ranges, increases the scope of measurement..
Compared with prior art, the beneficial effect of technical solution of the present invention is：The gas permeation rate of encapsulating material of the present invention
Multi-method measures correction system, and the test sample of polylith film-form is arranged on substrate, and multiple reaction amount detecting devices are examined respectively
The amount of the designated gas chemically reacted with each piece of test sample is surveyed, it is anti-that according to each piece of test sample chemistry occurs for the system
The amount for the designated gas answered, surface area and testing time calculating in conjunction with packing colloid obtain the designated gas of encapsulating material
Transmitance, the present invention verifies the accuracy for the transmitance that each test sample is measured according to the ratio of each piece of test sample, and
The transmitance that each test sample is obtained is weighted averagely, obtains corrected transmitance.The present invention utilizes multi-method not
Same measurement sensitivity increases measurement range.The present invention constructs a multi-method, many test sample measurement results mutually school
Positive system, is able to verify that the Measurement reliability of every kind of method during each measurement, can further eliminate measurement error, improve measurement
Accuracy and resolution.
Brief description of the drawings
Fig. 1 is that mutually amplification WVTR optical measuring system schematic diagrames are locked in reflecting light photoluminescence.
Fig. 2 is that transmission-type luminescence generated by light locks mutually amplification WVTR optical measuring system schematic diagrames.
Fig. 3 is that mutually amplification WVTR optical measuring system schematic diagrames are locked in electroluminescent.
Fig. 4 is the test sample box schematic diagram of embodiment 1 and embodiment 2.
Fig. 5 is the test sample box schematic diagram of embodiment 3 and embodiment 4.
Fig. 6 is the structural representation of the reflective thin-film package test sample of the embodiment of the present invention 5.
Fig. 7 is the structural representation of the transmission-type thin-film package test sample of the embodiment of the present invention 5.
Wherein：1st, excitation apparatus；2nd, test sample box；3rd, focused light passages；4th, optical chopper；5th, photo-detector；6th, lock
Phase amplifier；7th, oscillograph or PC；22nd, material impervious to water；23rd, polyparaphenylene's acetylene PPV；24th, luminescent material PPV；25th, it is golden
Belong to electrode；26th, conductive layer；27th, encapsulating material；201st, substrate；202nd, luminescent material Alq3；203rd, metal electrode；204 encapsulation
Layer.
Embodiment
Accompanying drawing being given for example only property explanation, it is impossible to be interpreted as the limitation to this patent；
In order to more preferably illustrate the present embodiment, some parts of accompanying drawing have omission, zoomed in or out, and do not represent actual product
Size；
To those skilled in the art, it is to be appreciated that some known features and its explanation, which may be omitted, in accompanying drawing
's.
Technical scheme is described further with reference to the accompanying drawings and examples.
Embodiment 1
A kind of gas permeation rate multi-method measurement correction system of encapsulating material, the system is used to measure and correct encapsulation
The transmitance of the designated gas of material, the system includes substrate, encapsulating material, test sample and reaction amount detecting device, many
The test sample of block film-form is arranged on substrate, and encapsulating material encapsulates whole substrate, make test sample be located at encapsulating material with
In confined space between substrate, the test sample can chemically react with the designated gas, multiple reacting dose inspections
Survey the amount that device detects the designated gas chemically reacted with each piece of test sample respectively.
In specific implementation process, the test sample uses embedded photoluminescent material, electroluminescent material or active metal
In one or more, the test sample be embedded photoluminescent material or electroluminescent material when, reaction amount detecting device detection
The weak amount of test sample optical excitation signal, and the weak amount and test sample according to optical excitation signal and the reaction of designated gas
Ratio calculates the amount of the designated gas chemically reacted with the test sample；When the test sample is active metal, reaction
The resistance of amount detecting device detection active metal and the amount for calculating the designated gas chemically reacted with the test sample.
In specific implementation process, when institute's test sample is embedded photoluminescent material or electroluminescent material, such as Fig. 1-3
Shown, its corresponding reaction amount detecting device includes：
Excitation apparatus 1：For being excited or electrically excited mode using light, make to be sealed in the luminescent material production in encapsulating material
Raw exciting light；
Test sample box 2：The test sample box includes encapsulating material and the luminescent material being sealed in encapsulating material,
The luminescent material can chemically react with designated gas；
Focused light passages 3：Exciting light for luminescent material to be produced converges to optical chopper；
Optical chopper 4：For being modulated with default reference frequency to exciting light；
Photo-detector 5：Optical signal is converted to electric signal after being modulated through optical chopper；
Lock-in amplifier 6：For extracting and exporting optical excitation signal, the lock-in amplifier is using reference frequency signal as ginseng
Signal is examined, the electric signal exported using photo-detector is input signal；
The present embodiment realizes luminescence generated by light (PL) measuring method, electroluminescent (EL) measuring method and electric-resistivity method mutually school
Just.As shown in figure 4, first, mask and active metal Ca reflecting layer and electroluminescent metal are formed on transparency carrier glass
Electrode A l.Secondly, luminous material layer Alq3 is formed on the metal layer.Then, metal electrode is formed in electroluminescent material layer
Al.Finally, encapsulation forms whole correcting structure.In identical environment, at the same using luminescence generated by light is reflective, it is resistance-type, electroluminescent
It is illuminated that water vapor transmittance is measured to respective sample.Luminescence generated by light reflective measuring system such as Fig. 1, electroluminescent measurement system
System such as Fig. 3.It can be calculated and lighting that water reacts by detecting the attenuation of Alq3 luminescence generated by lights and electroluminescence signal
Quantity of material, calculates the vapour quantity of participation reaction, so as to calculate water further according to the chemical reaction equation of luminescent material Alq3 and steam
Vapour transmitance.Electric-resistivity method calculates the amount of metal reacted with water by calculating metallic reflector Ca change in resistance, so as to count
Calculate water vapor transmittance.By repeatedly detecting the WVTR under same package using PL methods, EL methods, electric-resistivity method, three kinds of sides are determined
The sensitivity of three kinds of methods when method sample is packaged together.Sensitivity measures the ratio of WVTR values to represent by three kinds of methods.
The correction system can be used to verify the accuracy for measuring each method every time, add the reliability of measurement result.Measurement every time
It all can be the accuracy that can verify that three kinds of method measurements by the ratio of three kinds of methods.The correction system passing ratio is corrected in oxygen
It can be used to verify the accuracy for measuring each method every time under the interference of the other factors such as gas or ambient light, add measurement result
Reliability.Such as, when influence be can not ignore caused by ambient light when measuring, optical method for measuring value can deviate to be surveyed with electric-resistivity method
The ratio of value, so that it may verify that ambient light causes the inaccuracy of optical method for measuring.
Embodiment 2
The present embodiment realizes that PL measuring methods, EL measuring methods and electric-resistivity method are mutually corrected.According to Fig. 4, first, transparent
Mask and metallic reflector Li and hole transmission layer N, N- diphenyl-N, N- bis- (3- methylbenzenes are formed on substrate ito glass
Base) two units of -1,1- biphenyl -4,4- diamines (TPD).Secondly, all form luminous on metal level Li and hole transmission layer TPD
Then material strata Isosorbide-5-Nitrae-penylene CN-PPP, forms electron transfer layer quinoxaline derivant and metal in electroluminescent material layer
Electrode A l.Finally, encapsulation forms whole correcting structure.In identical environment, at the same using luminescence generated by light is reflective, resistance-type,
Electroluminescent formula measures water vapor transmittance to respective sample.Luminescence generated by light reflective measuring system such as Fig. 1, electroluminescent is surveyed
Amount system such as Fig. 2.It can be calculated by detecting the attenuation of CN-PPP luminescence generated by lights and electroluminescence signal and be reacted with water
Luminescent material CN-PPP amounts, further according to luminescent material CN-PPP and steam chemical reaction equation calculate participate in reaction steam
Amount, so as to calculate water vapor transmittance.Electric-resistivity method calculates what is reacted with water by calculating metallic reflector Li change in resistance
Amount of metal, so as to calculate water vapor transmittance.By repeatedly being detected using PL methods, EL methods, electric-resistivity method under same package
WVTR, determines that the sensitivity of three kinds of methods of ratio of three kinds of method measurement WVTR values is represented with ratio.What three kinds of methods were measured
Measurement range is determined that multi-method correction systematic survey scope is that the measurement range of three kinds of methods is added, and is conducive to increasing by sensitivity
The scope measured greatly.The correction system can be used to verify the accuracy for measuring each method every time, and add measurement result can
By property.Measurement all can be the accuracy that can verify that three kinds of method measurements by the ratio of three kinds of methods every time.The correction system is led to
Cross ratio adjustment and can be used to verify the accuracy for measuring each method every time under the interference of the other factors such as oxygen or ambient light, increase
The reliability of measurement result is added.
Embodiment 3
The present embodiment is realized that PL is reflective and mutually corrected with transmission-type, optimizes transmission-type measurement result.The reflective methods of PL
Compared to PL transmission-type methods, because employing reflected light path, only need to ensure that outer light source optical signal reaches makes luminescent material fully send out
Light, the influence produced to measurement is less.However, PL transmission-type methods use linear light path, ensureing that laser signal reaches
Luminescent material is fully lighted outer, small may should also avoid producing considerable influence to measurement unexpectedly.Swash when therefore, it can change measurement
The size of optical signal, can be with by the way that to two methods, measured obtained WVTR is compared under different size laser signal
Optimize PL transmission-type measuring methods.On the same substrate, two regions are averagely divided into：Echo area and transmission area.With reference to figure
5, the sample of reflection measurement is made on echo area, the sample of transmission measurement is made.First, base-plate cleaning and substrate is divided
Area is simultaneously separated out with material impervious to water 22.As shown in figure 5, forming luminescent material polyparaphenylene's acetylene on substrate echo area
Luminescent material PPV24 is formed on PPV23, transmission area.Then, metal electrode 25 is formed on luminescent material 23 with reference to Fig. 5.Most
Afterwards, the substrate after film forming is entirely encapsulated using encapsulating material 27.Using Fig. 1 and Fig. 2 measuring systems, by changing laser
The size of signal, multiple WVTR values to reflective measurement are averaging, and transmission-type corresponding with each laser signal size is surveyed
Amount result is compared.Corresponding laser signal is that transmission-type measures optimal laser signal when difference is minimum, and measurement result is more accurate
Really.
Embodiment 4
The present embodiment realizes that luminescence generated by light is mutually corrected with electroluminescent measuring method.On the same substrate, it is average to draw
It is divided into two regions：PL areas and EL areas.With reference to Fig. 5 structures, the sample of reflection measurement is made in PL areas, EL is made in EL areas
The sample of measurement.First, ito substrate cleans and carries out subregion to substrate and separated out with material impervious to water 22.With reference to Fig. 5 knots
Structure, forms in substrate 81PL areas and luminescent material PPV24 is formed in luminescent material polyparaphenylene's acetylene PPV23, EL areas.Then,
Metal electrode 25 is formed on luminescent material polyparaphenylene acetylene PPV23 on PL is gone with reference to Fig. 5, PEDOT/ is formed in EL areas
PSS conductive layers 26.Finally, the substrate after film forming is entirely encapsulated using encapsulating material 27.Utilize PL and EL measuring systems
Fig. 1 and Fig. 2 are respectively in PL areas and the WVTR of EL region measurement samples.Two obtained WVTR are measured for the first time to average WVTR1。
Change the voltage of EL measurements, and by measured value and WVTR1It is averaging WVTR2.Change the laser signal size of PL measurements, and will survey
Value and WVTR2.Change the voltage of EL measurements, and by measured value and WVTR2It is averaging WVTR3.Change the survey of two methods successively
Amount condition, until the EL results measured compare WVTRnSmall or PL measurement results compare WVTRnIt is big.Now, WVTRnIt is exactly the environment
It is lower, the WVTR of encapsulating material.The WVTR obtained by the mutual correction of PL and EL measuring methods, it is contemplated that two kinds of measuring methods
Limitation obtained more accurate result.
Embodiment 5
Make respectively for the emanant measurement of luminescence generated by light, the measurement of luminescence generated by light transmission-type, electroluminescent measurement, active gold
Belong to the measurement sample of 4 kinds of measuring methods of resistance measurement, measurement sample is all packaged with identical transparent encapsulation material.
Fig. 6 is the structural representation of the reflective thin-film package test sample of the embodiment of the present invention.
First, base-plate cleaning.The material of substrate 201 flexibility such as the rigid substrates and plastics base such as including glass in embodiment
Plate.Luminescent material Alq3 202 is formed on substrate 201.In the present embodiment, luminescent material Alq3 202 method bag is formed
Include wet method processing procedure and dry method processing procedure.Wet method processing procedure may include spin-coating method, ink-jet method, roller rubbing method, silk-screen printing, stamped method,
Scraper for coating, dry method processing procedure includes chemical vapor deposition (CVD), sputtering, evaporation, ald.The species bag of luminescent material
Include organic and inorganic, high molecular polymer and small molecule.
Then, metal electrode is formed on luminescent material Alq3 202 with reference to Fig. 6.
Finally, on metal electrode 203, thin-film package encapsulated layer 204.
Fig. 7 is the structural representation of embodiment of the present invention transmission-type thin-film package test sample.
First, base-plate cleaning.The material of substrate 201 flexibility such as the rigid substrates and plastics base such as including glass in embodiment
Plate.
With reference to Fig. 7 structures, luminescent material Alq3 202 is formed on substrate 201.In the present embodiment, luminescent material is formed
Alq3 202 method includes wet method processing procedure and dry method processing procedure.Wet method processing procedure may include spin-coating method, ink-jet method, roller rubbing method,
Silk-screen printing, stamped method, scraper for coating, dry method processing procedure include chemical vapor deposition (CVD), sputtering, evaporation, ald.
The species of luminescent material includes organic and inorganic, high molecular polymer and small molecule.
Finally, on luminescent material Alq3 202, thin-film package transparent encapsulated layer 204.
Reacted in addition, being made respectively according to the structure of common OLED and Ca reaction methods for the measurement of electroluminescent optics and Ca
The sample of method measurement.
Test sample is prepared by above-mentioned flow, and is stored in the controllable environment of humiture.Just utilized at interval of 2 hours
Lock shown in Fig. 1 mutually amplification WVTR optical reflections measuring system, the lock shown in Fig. 2 mutually amplify WVTR optical transmissions measuring system,
Lock shown in Fig. 3 mutually to sample in 4 different environment enter by amplification WVTR electroluminescent measuring system, Ca response measurements system
Row test, and calculate the WVTR of the same package material for 4 kinds of different method of testings.
Analyzed for the WVTR results that 4 kinds of method of testings are measured：Reflecting light photoluminescence measuring method introduces outer
Carry out optical signal, introducing noise makes measurement structure less than normal.Penetration photoluminescence measurement method, introduces external optical signal, although
Filter plate is added to filter light signal, but filter plate filter range may have common factor, institute with luminescence generated by light signal
There is deviation with measurement result.Electroluminescence signal, in the absence of the interference of other optical signals, works as loading due to not external light source
Voltage on sample can cause the aging of hot-spot accelerated luminescence material to cause measurement bigger than normal.Ca reaction methods are that steam is anti-
Should when also simultaneously and oxygen reaction, cause measurement result bigger than normal.So needing the WVTR that 4 kinds of method measurements are obtained to more than
Carry out mutually correction and obtain right value.Bearing calibration uses average weighted mode：4 kinds of measuring methods under 4 varying environments
4 obtained WVTR values constitute 4 corresponding equations, solve 4 equations and can obtain advising corresponding to every kind of method,
I.e. to measurement result correction for drift ratio.
The same or analogous part of same or analogous label correspondence；
Term the being given for example only property explanation of position relationship described in accompanying drawing, it is impossible to be interpreted as the limitation to this patent；
Obviously, the above embodiment of the present invention is only intended to clearly illustrate example of the present invention, and is not pair
The restriction of embodiments of the present invention.For those of ordinary skill in the field, may be used also on the basis of the above description
To make other changes in different forms.There is no necessity and possibility to exhaust all the enbodiments.It is all this
Any modification, equivalent and improvement made within the spirit and principle of invention etc., should be included in the claims in the present invention
Protection domain within.
Claims (10)
1. a kind of gas permeation rate multi-method measurement correction system of encapsulating material, the system is used to measure and correct package material
The transmitance of the designated gas of material, it is characterised in that the system includes substrate, encapsulating material, test sample and reacting dose inspection
Device is surveyed, the test sample of polylith film-form is arranged on substrate, encapsulating material encapsulates whole substrate, test sample is located at envelope
In confined space between package material and substrate, the test sample can chemically react with the designated gas, multiple
Reaction amount detecting device detects the amount of the designated gas chemically reacted with each piece of test sample respectively.
2. the gas permeation rate multi-method measurement correction system of encapsulating material according to claim 1, it is characterised in that institute
Test sample is stated using the one or more in embedded photoluminescent material, electroluminescent material or active metal, the test sample
During for embedded photoluminescent material or electroluminescent material, reaction amount detecting device detects the weak amount of test sample optical excitation signal,
And the weak amount and test sample and the reaction ratio of designated gas according to optical excitation signal are calculated and the test sample
Learn the amount of the designated gas of reaction；When the test sample is active metal, reaction amount detecting device detects the electricity of active metal
Hinder and calculate the amount of the designated gas chemically reacted with the test sample.
3. the gas permeation rate multi-method measurement correction system of encapsulating material according to claim 2, it is characterised in that institute
When stating test sample for embedded photoluminescent material or electroluminescent material, its corresponding reaction amount detecting device includes：
Excitation apparatus：Excited for use light or electrically excited mode makes test sample produce exciting light, it is sharp that the light, which is excited,
Light reflection is excited or laser transmission is excited；
Focused light passages：Exciting light for test sample to be produced converges to optical chopper；
Optical chopper：For being modulated with default reference frequency to exciting light；
Photo-detector：Optical signal is converted to electric signal after being modulated through optical chopper；
Lock-in amplifier：For extracting and exporting optical excitation signal, the lock-in amplifier is using reference frequency signal as with reference to letter
Number, the electric signal exported using photo-detector is input signal.
4. the gas permeation rate multi-method measurement correction system of encapsulating material according to claim 1, it is characterised in that institute
Substrate is stated for flexible base board or rigid substrates, the test sample direct forming of film-form is on substrate.
5. the gas permeation rate multi-method measurement correction system of encapsulating material according to claim 4, it is characterised in that,
The method that film-form measurement sample is formed on substrate uses wet method processing procedure or dry method processing procedure.
6. the gas permeation rate multi-method measurement correction system of encapsulating material according to claim 1, it is characterised in that, sample
The packaged type of product includes rigidity encapsulation and flexible package.
7. the gas permeation rate multi-method measurement correction system of encapsulating material according to claim 1, it is characterised in that many
The method of kind includes photoluminescence method, electroluminescent method and active metal electric-resistivity method.
8. the gas permeation rate multi-method measurement correction system of encapsulating material according to claim 1, it is characterised in that institute
The amount for the designated gas that system chemically reacts according to each piece of test sample is stated, surface area and test in conjunction with packing colloid
Time Calculation obtains the transmitance of the designated gas of encapsulating material, the transmitance that each test sample is obtained is weighted flat
, corrected transmitance is obtained.
9. the gas permeation rate multi-method measurement correction system of encapsulating material according to claim 1, it is characterised in that institute
The amount for the designated gas that system chemically reacts according to each piece of test sample is stated, surface area and test in conjunction with packing colloid
Time Calculation obtains the transmitance of the designated gas of encapsulating material, and each test sample is verified according to the ratio of each piece of test sample
The accuracy of the transmitance measured.
10. the gas permeation rate multi-method measurement correction system of encapsulating material according to claim 1, it is characterised in that
The amount for the designated gas that the system chemically reacts according to each piece of test sample, surface area and survey in conjunction with packing colloid
Examination Time Calculation obtains the transmitance of the designated gas of encapsulating material, different using each method sensitivity, increases measurement range.
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| CN106092854B (en) * | 2016-06-21 | 2019-01-22 | 武汉华星光电技术有限公司 | A kind of testing vapor transmission device and method of encapsulating material |
| CN106814019B (en) * | 2017-01-19 | 2019-05-14 | 红河雄风印业有限责任公司 | A kind of measurement method of paper coating material imbibition characteristic |
| CN108398369A (en) * | 2018-03-21 | 2018-08-14 | 广东电网有限责任公司电力科学研究院 | A kind of GIS rubber packing materials selection method and system |
| CN109142284B (en) * | 2018-09-03 | 2021-10-01 | 重庆惠科金渝光电科技有限公司 | Penetration rate detection method, device and computer readable storage medium |
| US10859494B2 (en) | 2018-09-03 | 2020-12-08 | Chongqing Hkc Optoelectronics Technology Co., Ltd. | Transmittance measuring method, device and computer readable storage medium |
| CN113686758B (en) * | 2021-10-27 | 2022-03-18 | 江苏英瑞世家实业有限公司 | Jean cloth gas permeability check out test set |
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