CN104777085A - Gas transmission rate multi-method measurement and correction system for packaging material - Google Patents
Gas transmission rate multi-method measurement and correction system for packaging material Download PDFInfo
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- CN104777085A CN104777085A CN201510129226.6A CN201510129226A CN104777085A CN 104777085 A CN104777085 A CN 104777085A CN 201510129226 A CN201510129226 A CN 201510129226A CN 104777085 A CN104777085 A CN 104777085A
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Abstract
The invention discloses a gas transmission rate multi-method measurement and correction system for a packaging material. A plurality of film-like test samples are disposed on a base plate, a plurality of reaction dose detection devices respectively detecting the dose of specified gas reacting chemically with each test sample, according to the dose of specified gas for chemical reaction of each test sample, the system combines the surface area and test time of packaging colloid to calculate the transmission rate of the specified gas for the packaging material. The system provided by the invention verifies the measured transmission rate's accuracy of each test sample according to the proportion of each test sample, and conducts weighted averaging on the measured transmission rate of each test sample so as to obtain a corrected transmission rate. According to the invention, different measuring sensitivities of multi-methods are utilized to increase the measurement range. The invention constructs the system able to realize mutual correction of multi-method and multi-test sample measurement results, can verify the measurement reliability of each method during each measurement, and can further eliminate measurement error and improve the measurement accuracy and resolution.
Description
Technical field
The present invention relates to moisture-vapor transmission fields of measurement, more specifically, relate to a kind of gas permeation rate multi-method measurement update system of encapsulating material.
Background technology
Organic Light Emitting Diode (OLED) produces luminous luminescent device by compound after positive and negative carrier injection organic semiconductor thin-film.Organic Light Emitting Diode (OLED) have active illuminating, high brightness, high-contrast, ultra-thin, low cost, low-power consumption, response fast, wide viewing angle, can be flexible etc. advantage, there are the potentiality of the traditional LCD of replacement.Flexible Displays has flexible, frivolous and non-friable characteristic, becomes the study hotspot of whole world display industry gradually.OLED flexibility characteristics can facilitate technical development and the product marketization of OLED.But there is short shortcoming device lifetime in OLED.This is because water vapor, oxygen all to a certain extent can with the electrode of OLED and luminous organic material generation chemical reaction, and then cause the Performance Characteristics of OLED to change.Such as: blackspot effect, local overheating, organic material are aging.The water unstable of OLED seriously have impact on mission life and the exhibit stabilization of OLED, hinders the marketization of OLED display technique.Based on early stage research, make the 10^4h that the OLED life-span reaches practical, the substrate of device and encapsulated layer should lower than 5 × 10^-6g/m to the infiltration rate of steam
2d, its implication be unit area every day through the quality of water vapor.Therefore, in order to measure the high water resistance of OLED encapsulation, backing material, precision reaches 10^-6g/m
2moisture-vapor transmission (WVTR) method of measuring of d seems especially important.At present, the comparatively high precision WVTR measuring method of main flow, comprises sensor method, radioactive-tracer method, mass spectroscopy, steam detection method, Ca method based on Tunable Diode Laser Absorption Spectroscopy (TDLAS) technology.
The Mocon of MOCON company of the U.S.
model 2WVTR tester have employed a coulomb method for electricity phosphorus pentoxide AquatraceTM sensor measurement, and its resolution reaches 5 × 10^-5g/m
2d.Its principle builds film sample when two cavitys connecting valve: the moist chamber of humidity, temperature-controllable and drying chamber.According to Fick's first law and Henry's law, the vapour concentration gradient at film two ends causes steam to spread from moist cavity to drying chamber.Steam is diffused into drying chamber, and the water vapor entering sensor very is converted into measurable electricity, and then calculates steam permeating rate.The bonding limitation of two cavity structure measured materials there will be edge leakage problem.When detection moisture is lower than 10^-5g/m
2during d, coulomb sensing technology is infeasible.
The people such as D.Ralf adopt reflectivity trace method, and its principle utilizes heavy water (tritium) to measure through the steam permeating rate of measured material as the tracer agent of water vapor.Two cavity structures, the junction rubber seal measured material of the gas compartment being full of HTO gas and the measuring chamber that passes into methane.By measuring other amounts through the HTO of measured material, calculate the WVTR of measured material.Reflectivity trace method equipment is complicated, expensive, and radioactive waste can be caused to pollute.
Mass spectroscopy measurement utilizes quadrupole mass spectroscope to measure the background partial pressure of water vapor in vacuum chamber and the saturated partial pressure after permeating, and utilize the analytical approach of partial pressure device measuring technique to calculate the moisture vapor transmission of measured material, successively to be built etc. by University of Electronic Science and Technology Li Jun and the proposition such as German Philip Hulsmann.Its detection accuracy can reach 10^-6g/m
2d.Quadrupole mass spectroscope make use of the ion principle that movement locus is different under electromagnetic field effect of different specific charge, detects the partial pressure of gas.Measuring system comprises vacuum chamber, humiture that quadrupole mass spectroscope is housed controlled gas compartment, pumped vacuum systems etc., complex structure, costly.
Based on the steam detection method of Tunable Diode Laser Absorption Spectroscopy (TDLAS) technology.Tunable diode laser absorption spectroscopy analysis is according to gas to electromagnetic absorption, and often kind of molecule determines to have specific energy state due to the Nomenclature Composition and Structure of Complexes, is subsequently absorbed in the material when incident light meets bohr condition.Often kind of molecule has specific infrared absorption spectrum.TDLAS technology utilizes the tuning characteristic absorption district by water vapor of laser wavelength, carries out demodulation, the component of analytical gas and concentration, and then calculate the concentration of water vapor to the laser signal through gas that spectrum sensor detects.TDLAS comprises on signal detecting method: directly absorption, wavelength-modulated, frequency modulation (PFM) and balance Detection Techniques.TDLAS water vapor detection accuracy can reach 100ppb, and detectable WVTR reaches 10^-7g/m
2d.The HiBarSens instrument of SEMPA company of Germany make use of TDLAS technology exactly, and resolution reaches 10^-6g/m
2d.
The method being widely used in the measurement of OLED encapsulating material water vapor transmittance is at present Ca reaction method.Ca reaction method is that occur based on the chemical activity of Ca and water vapor can chemical reaction, characterizes by detecting Ca extent of corrosion the steam vapour amount reacted through encapsulating material and Ca.The method detecting Ca extent of corrosion generally has two kinds: conductivity measurement and optical means.The method of electricity, calculates moisture vapor transmission over time by the conductivity detecting Ca film.The method of optics, gathered the Ca film image of different time points, and the ratio of image processing and analyzing clear area and corrosion region estimates the amount through water by optical microscope.The estimation program water vapor transmittance limit that the people such as Paetzold R, NisatoG propose can reach 3 × 10^-7g/m
2d.But Ca reaction method can not get rid of the reaction of oxygen and Ca, oxygen and water vapor transmitance separately cannot be distinguished.
At present, additionally provide a kind of by measuring luminescent material luminous signal, thus characterize the optical means of the encapsulating material water vapor transmittance of sealed light emitting material.After forming plugging meter sample under vacuum conditions, optical measuring system first time is utilized to measure the luminous signal intensity I of luminescent material
0, by measurement sample storage in the environment that humiture is controlled.Measure the photoluminescence light signal of a luminescent material at interval of identical hour t, obtain the I under the fixed time
1, I
2, I
3... ..I
n.Normalization linear process, unit interval t change in optical signal rate is:
Correspondingly, thickness is L
0luminescent material and water vapor react and occur rotten to cause non-luminous amount of thickness Δ L to be
Unit interval, to be the luminescent material variable mass of B be area:
In formula, the water vapor transmittance that WVTR [OLEM] is luminescent material, refers to the unit interval, unit area through total precipitable water.
The water vapor transmittance of setting encapsulating material is WVTR [H
2o], to be the steam transit dose of the encapsulating material of A be unit interval area:
m[H
2O]＝WVTR*A
According to the chemical equation of luminescent material and steam, the amount of the luminescent material reacted with the steam through encapsulating material is:
M [H
2o] be H
2the molal weight of O, the molal weight that M [OLEM] is luminescent material used, n is the proportioning number of chemical equation.
Try to achieve the water vapor transmittance of encapsulating material:
This method precision reaches OLED encapsulating material WVTR requirement, measuring method is easy, cost is low, but introducing external light source when measuring must produce interference to the feeble signal of luminescent material generation, cause measurement result deviation.
Existing moisture-vapor transmission measuring technique also exists that measuring accuracy is low, measuring method is complicated or high in cost of production defect, OLED encapsulating material moisture-vapor transmission cannot be met and measure requirement, and these methods measured all also exist some immutable error components, this is for promoting the accuracy and precision generation negative interaction measured further.
Summary of the invention
The present invention overcomes the defect that above-mentioned prior art measurement gas transmitance exists error, the Measurement reliability of method is often planted when checking is measured at every turn, the gas permeation rate multi-method measurement update system of a kind of encapsulating material provide a kind of and can eliminate measuring error, improving accuracy and the resolution measured, described system utilizes each method sensitivity difference to increase measurement range.
For solving the problems of the technologies described above, technical scheme of the present invention is as follows:
A kind of gas permeation rate multi-method measurement update system of encapsulating material, described system is for measuring and correcting the transmitance of the designated gas of encapsulating material, described system comprises substrate, encapsulating material, test sample and reacting dose pick-up unit, the test sample of polylith film-form is arranged on substrate, encapsulating material encapsulates whole substrate, make in the confined space of test specimens product between encapsulating material and substrate, described test sample can with described designated gas generation chemical reaction, multiple reacting dose pick-up unit detects the amount of the designated gas testing sample generation chemical reaction with each piece respectively.
In the preferred scheme of one, described test sample adopt in embedded photoluminescent material, electroluminescent material or active metal one or more, described test sample be embedded photoluminescent material or electroluminescent material time, reacting dose pick-up unit detects the weak amount of test sample optical excitation signal, and calculates the amount with the designated gas of this test sample generation chemical reaction according to the weak amount of optical excitation signal and the reaction ratio of test sample and designated gas; When described test sample is active metal, reacting dose pick-up unit detects the resistance of active metal and calculates the amount with the designated gas of this test sample generation chemical reaction.
In the preferred scheme of one, described test sample be embedded photoluminescent material or electroluminescent material time, the reacting dose pick-up unit of its correspondence comprises:
Excitation apparatus: for adopting optical excitation or electrically excited mode to make test sample book produce exciting light, described optical excitation is that laser reflection excites or laser-transmitting excites;
Focused light passages: the exciting light for test sample book being produced converges to optical chopper.
Optical chopper: for modulating exciting light with the reference frequency preset;
Photo-detector: electric signal will be converted to by light signal after optical chopper modulation;
Lock-in amplifier: for extracting and exporting optical excitation signal, described lock-in amplifier take reference frequency signal as reference signal, and the electric signal exported with photo-detector is for input signal.
In the preferred scheme of one, described substrate is flexible base, board or rigid substrates, and the test sample direct forming of film-form is on substrate.
In the preferred scheme of one, substrate forms method employing wet method processing procedure or dry method processing procedure that film-form measures sample.
In the preferred scheme of one, the packaged type of sample comprises rigidity encapsulation and flexible package.
In the preferred scheme of one, multiple method comprises photoluminescence method, electroluminescence method and active metal electric-resistivity method.
In the preferred scheme of one, described system is according to the amount of the designated gas of each piece of test sample generation chemical reaction, the transmitance of the designated gas of encapsulating material is calculated again in conjunction with the surface area of packing colloid and test duration, the transmitance that each test sample obtains is weighted on average, obtains corrected transmitance.
In the preferred scheme of one, described system is according to the amount of the designated gas of each piece of test sample generation chemical reaction, calculate the transmitance of the designated gas of encapsulating material again in conjunction with the surface area of packing colloid and test duration, verify the accuracy of the transmitance that each test sample records according to the ratio of each piece of test sample.
In the preferred scheme of one, described system is according to the amount of the designated gas of each piece of test sample generation chemical reaction, the transmitance of the designated gas of encapsulating material is calculated again in conjunction with the surface area of packing colloid and test duration, the multiple method correcting measuring that sensitivity is different, because sensitivity is different, highly sensitive method can survey the very little situation of gas permeation rate, and the low method of sensitivity can survey the very large situation of gas permeation rate.Therefore, the multiple method correcting measuring that multiple sensitivity is different, measurement range includes multiple method measurement range, increases the scope of measurement.。
Compared with prior art, the beneficial effect of technical solution of the present invention is: the gas permeation rate multi-method measurement update system of encapsulating material of the present invention, the test sample of polylith film-form is arranged on substrate, multiple reacting dose pick-up unit detects the amount of the designated gas testing sample generation chemical reaction with each piece respectively, described system is according to the amount of the designated gas of each piece of test sample generation chemical reaction, the transmitance of the designated gas of encapsulating material is calculated again in conjunction with the surface area of packing colloid and test duration, the present invention verifies the accuracy of the transmitance that each test sample records according to the ratio of each piece of test sample, and be weighted on average to the transmitance that each test sample obtains, obtain corrected transmitance.The measurement sensistivity that the present invention utilizes multi-method different increases measurement range.The system that the present invention constructs a multi-method, many test sample measurement results correct mutually, often plants the Measurement reliability of method, can eliminate measuring error further, improves the accuracy and resolution measured when can verify each measurement.
Accompanying drawing explanation
Fig. 1 is reflecting light photoluminescence lock-in amplify WVTR optical measuring system schematic diagram.
Fig. 2 is transmission-type photoluminescence lock-in amplify WVTR optical measuring system schematic diagram.
Fig. 3 is electroluminescence lock-in amplify WVTR optical measuring system schematic diagram.
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 embodiment of the present invention 5 reflective thin-film package test sample.
Fig. 7 is the structural representation of the embodiment of the present invention 5 transmission-type thin-film package test sample.
Wherein: 1, excitation apparatus; 2, sample box is tested; 3, focused light passages; 4, optical chopper; 5, photo-detector; 5, lock-in amplifier; 7, oscillograph or PC; 21, substrate; 22, material impervious to water; 23, polyparaphenylene's acetylene PPV; 24, luminescent material PPV; 25, metal electrode; 26, conductive layer; 27, encapsulating material; 201, substrate; 202, luminescent material Alq3; 203, metal electrode; 204 encapsulated layers.
Embodiment
Accompanying drawing, only for exemplary illustration, can not be interpreted as the restriction to this patent;
In order to better the present embodiment is described, some parts of accompanying drawing have omission, zoom in or out, and do not represent the size of actual product;
To those skilled in the art, in accompanying drawing, some known features and explanation thereof may be omitted is understandable.
Below in conjunction with drawings and Examples, technical scheme of the present invention is described further.
Embodiment 1
A kind of gas permeation rate multi-method measurement update system of encapsulating material, described system is for measuring and correcting the transmitance of the designated gas of encapsulating material, described system comprises substrate, encapsulating material, test sample and reacting dose pick-up unit, the test sample of polylith film-form is arranged on substrate, encapsulating material encapsulates whole substrate, make in the confined space of test specimens product between encapsulating material and substrate, described test sample can with described designated gas generation chemical reaction, multiple reacting dose pick-up unit detects the amount of the designated gas testing sample generation chemical reaction with each piece respectively.
In specific implementation process, described test sample adopt in embedded photoluminescent material, electroluminescent material or active metal one or more, described test sample be embedded photoluminescent material or electroluminescent material time, reacting dose pick-up unit detects the weak amount of test sample optical excitation signal, and calculates the amount with the designated gas of this test sample generation chemical reaction according to the weak amount of optical excitation signal and the reaction ratio of test sample and designated gas; When described test sample is active metal, reacting dose pick-up unit detects the resistance of active metal and calculates the amount with the designated gas of this test sample generation chemical reaction.
In specific implementation process, described test sample be embedded photoluminescent material or electroluminescent material time, as Figure 1-3, the reacting dose pick-up unit of its correspondence comprises:
Excitation apparatus 1: for adopting optical excitation or electrically excited mode, makes the luminescent material be sealed in encapsulating material produce exciting light;
Test sample box 2: described test sample box comprises encapsulating material and is sealed in the luminescent material in encapsulating material, described luminescent material can with designated gas generation chemical reaction;
Focused light passages 3: the exciting light for being produced by luminescent material converges to optical chopper;
Optical chopper 4: for modulating exciting light with the reference frequency preset;
Photo-detector 5: electric signal will be converted to by light signal after optical chopper modulation;
Lock-in amplifier 6: for extracting and exporting optical excitation signal, described lock-in amplifier take reference frequency signal as reference signal, and the electric signal exported with photo-detector is for input signal;
The present embodiment realizes photoluminescence (PL) measuring method, electroluminescence (EL) measuring method and electric-resistivity method and mutually corrects.As shown in Figure 4, first, mask form Ca reflection horizon, active metal and electroluminescent metal electrode Al on transparency carrier glass.Secondly, luminous material layer Alq3 is formed on the metal layer.Then, electroluminescent material layer forms metal electrode Al.Finally, encapsulation forms whole correcting structure.In equivalent environment, use photoluminescence reflective, resistance-type, electroluminescence formula to carry out measurement water vapor transmittance to respective sample simultaneously.The reflective measuring system of photoluminescence is as Fig. 1, and electroluminescence measuring system is as Fig. 3.Can calculate by the damping capacity of detection Alq3 photoluminescence and electroluminescence signal the luminescent material amount reacted with water, then calculate according to the chemical reaction equation of luminescent material Alq3 and steam the vapour quantity participating in reacting, thus calculate water vapor transmittance.Electric-resistivity method is calculated and the amount of metal that water reacts by the change in resistance calculating metallic reflector Ca, thus calculates water vapor transmittance.By repeatedly utilizing the WVTR under PL method, EL method, electric-resistivity method detection same package, the sensitivity of three kinds of methods when determining that three kinds of method samples are packaged together.The ratio that sensitivity measures WVTR value by three kinds of methods represents.This corrective system can be used to verify each accuracy measuring each method, adds the reliability of measurement result.Each measurement all can verify by the ratio of three kinds of methods the accuracy that three kinds of methods are measured.This corrective system passing ratio corrects and can be used to verify each accuracy measuring each method under the interference of other factors such as oxygen or ambient light, adds the reliability of measurement result.Such as, when the impact that ambient light causes when measuring be can not ignore, optical method for measuring value can depart from the ratio with resistance measurement value, just can verify that ambient light causes the inaccuracy of optical method for measuring.
Embodiment 2
The present embodiment realizes PL measuring method, EL measuring method and electric-resistivity method and mutually corrects.According to Fig. 4, first, mask on transparency carrier ito glass form metallic reflector Li and hole transmission layer N, N-diphenyl-N, N-bis-(3-aminomethyl phenyl)-1,1-biphenyl-4,4-diamines (TPD) two unit.Secondly, metal level Li and hole transmission layer TPD form luminescent material strata Isosorbide-5-Nitrae-penylene CN-PPP then, electroluminescent material layer is formed electron transfer layer quinoxaline derivant and metal electrode Al.Finally, encapsulation forms whole correcting structure.In equivalent environment, use photoluminescence reflective, resistance-type, electroluminescence formula to carry out measurement water vapor transmittance to respective sample simultaneously.The reflective measuring system of photoluminescence is as Fig. 1, and electroluminescence measuring system is as Fig. 2.Can calculate by the damping capacity detecting CN-PPP photoluminescence and electroluminescence signal the luminescent material CN-PPP reacted with water to measure, calculate according to the chemical reaction equation of luminescent material CN-PPP and steam the vapour quantity participating in reacting again, thus calculate water vapor transmittance.Electric-resistivity method is calculated and the amount of metal that water reacts by the change in resistance calculating metallic reflector Li, thus calculates water vapor transmittance.By repeatedly utilizing the WVTR under PL method, EL method, electric-resistivity method detection same package, determining that the sensitivity of ratio three kinds of methods of three kinds of methods measurement WVTR values represents by ratio.The measurement range of three kinds of method measurements is determined by sensitivity, and multi-method corrective system measurement range is that the measurement range of three kinds of methods is added, and is conducive to increasing the scope measured.This corrective system can be used to verify each accuracy measuring each method, adds the reliability of measurement result.Each measurement all can verify by the ratio of three kinds of methods the accuracy that three kinds of methods are measured.This corrective system passing ratio corrects and can be used to verify each accuracy measuring each method under the interference of other factors such as oxygen or ambient light, adds the reliability of measurement result.
Embodiment 3
The present embodiment realizes that PL is reflective to be corrected mutually with transmission-type, optimizes transmission-type measurement result.The reflective method of PL compares PL transmission-type method, because have employed reflected light path, only need ensure that outer light source light signal reaches and make luminescent material fully luminous, on measuring, the impact produced is less.But PL transmission-type method adopts linear light path, make outside the abundant luminescence of luminescent material ensureing that laser signal reaches, also should unexpectedly may littlely avoid producing considerable influence to measurement.Therefore, the size of laser signal during measurement can being changed, by comparing the WVTR obtained measured by two kinds of methods are under different size laser signal, PL transmission-type measuring method can be optimized.On the same substrate, two regions are on average divided into: echo area and transmission area.With reference to figure 5, echo area makes the sample of reflection measurement, makes the sample of transmission measurement.First, base-plate cleaning subregion separating out with material impervious to water 22 is carried out to substrate.As shown in Figure 5, substrate 21 echo area is formed luminescent material polyparaphenylene acetylene PPV23, transmission area is formed luminescent material PPV24.Then, on luminescent material 23, metal electrode 25 is formed with reference to figure 5.Finally, the substrate after film forming is adopted encapsulating material 27 is whole is encapsulated.Utilizing Fig. 1 and Fig. 2 measuring system, by changing the size of laser signal, multiple WVTR values of reflective measurement are averaging, and the transmission-type measurement result corresponding with each laser signal size comparing.Laser signal corresponding when difference is minimum is that transmission-type measures best laser signal, and measurement result is more accurate.Embodiment 4
The present embodiment realizes photoluminescence and electroluminescence measuring method corrects mutually.On the same substrate, two regions are on average divided into: PL district and EL district.With reference to figure 5 structure, PL district makes the sample of reflection measurement, in EL district, makes the sample of EL measurement.First, ito substrate 21 cleans and carries out subregion to substrate and separate out with material impervious to water 22.With reference to figure 5 structure, substrate 81 PL district is formed luminescent material polyparaphenylene acetylene PPV23, EL district is formed luminescent material PPV24.Then, on PL goes, luminescent material polyparaphenylene acetylene PPV23 forms metal electrode 25 with reference to figure 5, EL district is formed PEDOT/PSS conductive layer 26.Finally, the substrate after film forming is adopted encapsulating material 27 is whole is encapsulated.Utilize PL and EL measuring system Fig. 1 and Fig. 2 respectively at the WVTR of PL district and EL region measurement sample.Measure two WVTR obtained for the first time to average WVTR
1.Change the voltage that EL measures, and by measured value and WVTR
1be averaging WVTR
2.Change the laser signal size that PL measures, and by measured value and WVTR
2.Change the voltage that EL measures, and by measured value and WVTR
2be averaging WVTR
3.Change the measuring condition of two kinds of methods successively, until the result that EL measures compares WVTR
nlittle or PL measurement result compares WVTR
nlarge.Now, WVTR
nbe exactly under this environment under, the WVTR of encapsulating material.By the WVTR that the mutual correction of PL and EL measuring method obtains, the limitation considering two kinds of measuring methods obtains more accurate result.
Embodiment 5
Make the measurement sample being used for the emanant measurement of photoluminescence, the measurement of photoluminescence transmission-type, electroluminescence measurement, active metal resistance measurement 4 kinds of measuring methods respectively, measure sample and all encapsulate by identical transparent encapsulation material.
Fig. 6 is the structural representation of the embodiment of the present invention reflective thin-film package test sample.
First, base-plate cleaning.In embodiment, the material of substrate 201 comprises the flexible base, boards such as rigid substrates and plastics such as glass.Substrate 201 is formed luminescent material Alq3 202.In the present embodiment, the method forming luminescent material Alq3 202 comprises wet method processing procedure and dry method processing procedure.Wet method processing procedure can comprise spin-coating method, ink-jet method, roller rubbing method, serigraphy, stamped method, scraper for coating, and dry method processing procedure comprises chemical vapor deposition (CVD), sputtering, evaporation, ald.The kind of luminescent material comprises organic and inorganic, high molecular polymer and Small molecular.
Then, on luminescent material Alq3 202, metal electrode is formed with reference to figure 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.In embodiment, the material of substrate 201 comprises the flexible base, boards such as rigid substrates and plastics such as glass.
With reference to figure 7 structure, substrate 201 forms luminescent material Alq3 202.In the present embodiment, the method forming luminescent material Alq3 202 comprises wet method processing procedure and dry method processing procedure.Wet method processing procedure can comprise spin-coating method, ink-jet method, roller rubbing method, serigraphy, stamped method, scraper for coating, and dry method processing procedure comprises chemical vapor deposition (CVD), sputtering, evaporation, ald.The kind of luminescent material comprises organic and inorganic, high molecular polymer and Small molecular.
Finally, on luminescent material Alq3 202, thin-film package transparent encapsulated layer 204.
In addition, the sample measured for electroluminescence optical measurement and Ca reaction method is made respectively according to the structure of common OLED and Ca reaction method.
By above-mentioned flow process preparation test sample, and be stored in the controlled environment of humiture.At interval of within 2 hours, just utilizing the lock-in amplify WVTR electroluminescence measuring system shown in the lock-in amplify WVTR optical transmission measuring system shown in the lock-in amplify WVTR optical reflection measuring system shown in Fig. 1, Fig. 2, Fig. 3, Ca response measurement system to test in 4 different environment sample, and calculate the WVTR of the same package material being used for 4 kinds of different method of testings.
The WVTR result recorded for 4 kinds of method of testings is analyzed: reflecting light photoluminescence measuring method introduces ambient light signal, introduces noise and makes measurement structure less than normal.Penetration photoluminescence measurement method, introduces ambient light signal, although add filter plate to carry out filtering to light signal, filter plate filter range may exist with photoluminescence signal occurs simultaneously, so deviation appears in measurement result.Owing to not having external light source, there is not the interference of other light signals in electroluminescence signal, the aging of local overheating accelerated luminescence material can be caused to cause measurement bigger than normal when being carried in the voltage on sample.Time Ca reaction method is that steam reacts also simultaneously and oxygen reaction, cause measurement result bigger than normal.So need the WVTR obtained above 4 kinds of method measurements to carry out mutually correcting obtaining right value.Bearing calibration adopts average weighted mode: the equation that 4 WVTR value formations 4 that 4 kinds of measuring methods under 4 varying environments obtain are corresponding, solves 4 equation and can obtain advising corresponding to often kind of method, namely to measurement result correction for drift ratio.
The corresponding same or analogous parts of same or analogous label;
The term describing position relationship in accompanying drawing, only for exemplary illustration, can not be interpreted as the restriction to this patent;
Obviously, the above embodiment of the present invention is only for example of the present invention is clearly described, and is not the restriction to embodiments of the present invention.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here exhaustive without the need to also giving all embodiments.All any amendments done within the spirit and principles in the present invention, equivalent to replace and improvement etc., within the protection domain that all should be included in the claims in the present invention.
Claims (10)
1. the gas permeation rate multi-method measurement update system of an encapsulating material, described system is for measuring and correcting the transmitance of the designated gas of encapsulating material, it is characterized in that, described system comprises substrate, encapsulating material, test sample and reacting dose pick-up unit, the test sample of polylith film-form is arranged on substrate, encapsulating material encapsulates whole substrate, make in the confined space of test specimens product between encapsulating material and substrate, described test sample can with described designated gas generation chemical reaction, multiple reacting dose pick-up unit detects the amount of the designated gas testing sample generation chemical reaction with each piece respectively.
2. the gas permeation rate multi-method measurement update system of encapsulating material according to claim 1, it is characterized in that, described test sample adopt in embedded photoluminescent material, electroluminescent material or active metal one or more, described test sample be embedded photoluminescent material or electroluminescent material time, reacting dose pick-up unit detects the weak amount of test sample optical excitation signal, and calculates the amount with the designated gas of this test sample generation chemical reaction according to the weak amount of optical excitation signal and the reaction ratio of test sample and designated gas; When described test sample is active metal, reacting dose pick-up unit detects the resistance of active metal and calculates the amount with the designated gas of this test sample generation chemical reaction.
3. the gas permeation rate multi-method measurement update system of encapsulating material according to claim 2, is characterized in that, described test sample be embedded photoluminescent material or electroluminescent material time, the reacting dose pick-up unit of its correspondence comprises:
Excitation apparatus: for adopting optical excitation or electrically excited mode to make test sample book produce exciting light, described optical excitation is that laser reflection excites or laser-transmitting excites;
Focused light passages: the exciting light for test sample book being produced converges to optical chopper.
Optical chopper: for modulating exciting light with the reference frequency preset;
Photo-detector: electric signal will be converted to by light signal after optical chopper modulation;
Lock-in amplifier: for extracting and exporting optical excitation signal, described lock-in amplifier take reference frequency signal as reference signal, and the electric signal exported with photo-detector is for input signal.
4. the gas permeation rate multi-method measurement update system of encapsulating material according to claim 1, it is characterized in that, described substrate is flexible base, board or rigid substrates, and the test sample direct forming of film-form is on substrate.
5. the gas permeation rate multi-method measurement update system of encapsulating material according to claim 4, is characterized in that, substrate is formed method employing wet method processing procedure or dry method processing procedure that film-form measures sample.
6. the gas permeation rate multi-method measurement update system of encapsulating material according to claim 1, is characterized in that, the packaged type of sample comprises rigidity encapsulation and flexible package.
7. the gas permeation rate multi-method measurement update system of encapsulating material according to claim 1, it is characterized in that, multiple method comprises photoluminescence method, electroluminescence method and active metal electric-resistivity method.
8. the gas permeation rate multi-method measurement update system of encapsulating material according to claim 1, it is characterized in that, described system is according to the amount of the designated gas of each piece of test sample generation chemical reaction, the transmitance of the designated gas of encapsulating material is calculated again in conjunction with the surface area of packing colloid and test duration, the transmitance that each test sample obtains is weighted on average, obtains corrected transmitance.
9. the gas permeation rate multi-method measurement update system of encapsulating material according to claim 1, it is characterized in that, described system is according to the amount of the designated gas of each piece of test sample generation chemical reaction, calculate the transmitance of the designated gas of encapsulating material again in conjunction with the surface area of packing colloid and test duration, verify the accuracy of the transmitance that each test sample records according to the ratio of each piece of test sample.
10. the gas permeation rate multi-method measurement update system of encapsulating material according to claim 1, it is characterized in that, described system is according to the amount of the designated gas of each piece of test sample generation chemical reaction, the transmitance of the designated gas of encapsulating material is calculated again in conjunction with the surface area of packing colloid and test duration, utilize each method sensitivity different, increase measurement range.
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