CN111982885B - Non-contact type thin film water oxygen permeability test method - Google Patents
Non-contact type thin film water oxygen permeability test method Download PDFInfo
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- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
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- G01N21/66—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light electrically excited, e.g. electroluminescence
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- H10K50/11—OLEDs or polymer light-emitting diodes [PLED] characterised by the electroluminescent [EL] layers
- H10K50/125—OLEDs or polymer light-emitting diodes [PLED] characterised by the electroluminescent [EL] layers specially adapted for multicolour light emission, e.g. for emitting white light
- H10K50/13—OLEDs or polymer light-emitting diodes [PLED] characterised by the electroluminescent [EL] layers specially adapted for multicolour light emission, e.g. for emitting white light comprising stacked EL layers within one EL unit
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Abstract
The invention provides a non-contact film water-oxygen permeability test method, which is characterized in that an Al electrode and Al of a light-emitting device are provided with 2 O 3 An external power supply is connected to the substrate, an instrument is used for measuring an initial electroluminescence spectrogram of the device, peaks of red light and blue light in the spectrogram are recorded, the initial peak of the red light is recorded as h, voltage is applied to the device every other fixed time T, the electroluminescence spectrogram of the device is measured, the change delta h of the peak height of the red light under the condition that the peak of the blue light is unchanged is observed, and the thickness of the organic material which has reacted with water vapor is obtained
According to the molecular weight M [ H ] 2 0]And an average molecular weight M [ OEAM ] of the organic luminescent material]The invention provides a high-precision non-contact film water-oxygen permeability test method, which is characterized in that electroluminescent spectrum data of an organic light-emitting device is processed and corrected to obtain the water vapor permeability WVTR of a packaging material within T hours in a unit area, and the data correction of the water vapor permeability is corrected by adopting a water vapor permeability coefficient alpha according to the type of the organic light-emitting material.
Description
Technical Field
The invention relates to the technical field of water oxygen detection methods, in particular to a non-contact film water oxygen permeability test method.
Background
According to the principle of testing the water vapor transmittance of the infrared sensor, a prepared sample is clamped in a testing cavity, nitrogen with certain relative humidity flows on one side of the film, and dry nitrogen flows on the other side of the film; under the push of humidity gradient, water vapor can diffuse from the high humidity side to the low humidity side through the film; on the low humidity side, the permeated water vapor is sent to the infrared sensor by flowing dry nitrogen, and the same proportion of electric signals are generated when the water vapor enters the sensor, and parameters such as the water vapor transmittance of a sample are obtained through analysis and calculation of the electric signals of the sensor, but the range of the method for testing the WVTR is only 10 < -2 > -10 < -3 > g/m < 2 >/24 h at the minimum, the service life of the OLED device is determined to a great extent by the water vapor transmittance, the measuring method with higher accuracy is particularly important, and the requirement of the OLED device testing cannot be met by the infrared sensor, so that the effect of the thin film package is required to be detected by adopting a more accurate WVTR testing method.
Disclosure of Invention
(one) solving the technical problems
Aiming at the defects of the prior art, the invention provides a non-contact type film water-oxygen permeability testing method with high precision, which solves the problems in the background art.
(II) technical scheme
In order to achieve the above purpose, the invention is realized by the following technical scheme: the non-contact film water-oxygen permeability test method includes the following steps,
(1) At 500-550 ℃ under Al 2 O 3 Growing an undoped u-GaN layer with the thickness of about 5 mu m on the substrate at a low temperature;
(2) Heating to about 1200 ℃ to grow an Si doped n-GaN epitaxial layer with the thickness of about 3 mu m;
(3) Then the temperature is reduced to 700 to 750 ℃ to grow In for 8 to 9 periods 0.2 Ga 0.8 The N/GaN multi-quantum well layer, wherein the thickness of the InGaN quantum well layer is about 3nm, the thickness of the GaN quantum barrier layer is about 11.5nm, and finally annealing treatment is carried out at the temperature of 1000 ℃ by a high-temperature annealing furnace to obtain a blue light LED substrate;
(4) Will require vapor depositionPlacing various medicines on the blue light LED substrate on a boat source or a crucible source of an evaporation cabin, placing the processed blue light LED substrate on a mask plate in the evaporation cabin, closing the cabin door of the evaporation cabin, vacuumizing, and when the vacuum degree in the evaporation cabin reaches 10 -5 Starting vapor deposition below mbar, preheating boat source or crucible source corresponding to vapor deposition material before vapor deposition, starting vapor deposition after reaching a certain temperature and proper rate, and controlling current to make vapor deposition rate of organic matters at
According to the step, a layer of organic red light material and a layer of MoO are sequentially evaporated on the blue light LED substrate 3 A hole transport layer as a device;
(5) Evaporating each organic layer, evaporating one layer of Al as electrode of the device, and controlling the evaporation rate of Al to be equal to
Evaporating 300nm;
(6) Packaging the evaporated organic material layer and the metal electrode, and obtaining a complete light-emitting device after packaging;
(7) Al electrode and Al in inorganic-organic composite light emitting device 2 O 3 An external power supply is connected to the substrate, an inorganic unit of the device emits blue light after voltage is applied, an organic unit emits red light, an instrument is used for measuring an initial electroluminescence spectrogram of the device, peaks of the red light and the blue light in the spectrogram are recorded, and the initial peak of the red light is recorded as h;
(8) Applying voltage to the device at fixed time T and measuring electroluminescent spectrum of the device, observing that under the condition of unchanged blue light peak, the change of peak height delta h and d of red light refers to thickness of organic red light material, thereby obtaining thickness of organic material which has reacted with water vapor
(9) According to the molecular weight M [ H ] 2 0]And an average molecular weight M [ OEAM ] of the organic luminescent material]Organic light-emitting deviceThe electroluminescent spectrum data of (2) is processed and corrected to obtain the water vapor transmittance WVTR of the packaging material within T hours in unit area, the data correction of the water vapor transmittance is corrected by adopting the water vapor transmittance coefficient alpha according to the type of the organic luminescent material, and a specific calculation formula is as follows:
(III) beneficial effects
The invention has the following beneficial effects:
1. as the method judges how much organic material is corroded by water vapor according to the change of the wave crest of the organic material, the wave crest is measured by a measuring instrument connected with a computer, the data precision is high, and the calculated data is reliable, so the precision can reach 10 -6 g/m 2 On the order of/24 h, the defect of insufficient testing accuracy of the infrared sensor is overcome.
2. The radioactive substance of the radioisotope tracing method is not needed, the safety is better, the requirements on equipment and laboratory conditions are lower, and meanwhile, the experimental parameters are few and the control is easy.
3. The whole process has few steps, simple flow and high precision of the prepared device, and can be detected to 10 -6 g/m 2 Very high accuracy of 24 h.
4. The equipment cost of the test instrument is reduced, and the measurement of the electroluminescent spectrum can be completed by using the existing spectrum radiance meter.
Drawings
Fig. 1 is a schematic structural diagram of a light emitting device used in the non-contact thin film water-oxygen permeability test method of the present invention.
Labeling and describing: 1. al (Al) 2 O 3 A substrate; 2. a u-GaN buffer layer; 3. an n-GaN epitaxial layer; 4. In0.2Ga0.8N/GaN multiple quantum well layer; 5. an organic red light material layer; 6. a hole transport layer; 7. an electrode.
Detailed Description
Referring to FIG. 1, the non-contact film water-oxygen permeability test method of the invention is shown.
The contact film water-oxygen permeability test method includes the following steps, firstly, under the temperature of 500-550 deg.C, al 2 O 3 A layer of undoped u-GaN with the thickness of about 5 mu m is grown on the substrate at low temperature to relieve lattice mismatch between the sapphire substrate and the GaN, wherein the effect of relieving lattice mismatch between the substrate and the GaN can be achieved at the thickness of 5 mu m, and the performance of a device is not lost; heating to about 1200 ℃, growing a Si doped n-GaN epitaxial layer with the thickness of about 3 mu m, and growing a multi-quantum well layer above the Si doped n-GaN epitaxial layer, wherein the Si doped n-GaN is better matched with the multi-quantum well, and the thickness of 3 mu m is used for growing the multi-quantum well layer above the Si doped n-GaN epitaxial layer, so that the performances such as light transmittance of a device cannot be influenced by excessive thickness; then the temperature is reduced to 700 to 750 ℃ to grow In for 8 to 9 periods 0.2 Ga 0.8 N/GaN multiple quantum well layer, in 0.2 Ga 0.8 The N/GaN multiple quantum well layer is a blue light emitting layer, in 0.2 Ga 0.8 N/GaN is used as a control group of the organic red light emitting layer, wherein the thickness of the InGaN quantum well layer is about 3nm, the thickness of the GaN quantum barrier layer is about 11.5nm, and finally annealing treatment is carried out at the temperature of 1000 ℃ by a high-temperature annealing furnace to obtain a blue light LED substrate; placing various medicines to be evaporated on the blue light LED substrate on a boat source or a crucible source of an evaporation cabin, placing the processed blue light LED substrate on a mask plate in the evaporation cabin, closing an evaporation cabin door, vacuumizing, and when the vacuum degree in the evaporation cabin reaches 10 - 5 Starting vapor deposition below mbar, preheating boat source or crucible source corresponding to vapor deposition material before vapor deposition, starting vapor deposition after reaching a certain temperature and proper rate, and controlling current to make vapor deposition rate of organic matters at
According to the step, a layer of organic red light material and a layer of MoO are sequentially evaporated on the blue light LED substrate 3 As a hole transport layer of the device, a device with emergent light having red light wave crest and blue light wave crest is prepared, and an organic red light material is evaporated on a prepared blue light LED substrate to obtain the required device, wherein the vacuum degree reaches 10 -5 The mbar is as follows: only when this condition is reached at the vacuum level,organic matters can escape from the heated boat or crucible and deposit on the device, and the evaporation rate of the organic matters is that
At this rate, the organic deposition is more uniform on the device; evaporating each organic layer, evaporating a layer of Al as electrode of the device, and controlling the evaporation rate of Al to +.>
Evaporating 300nm; packaging the evaporated organic material layer and the metal electrode, and obtaining a complete light-emitting device after packaging; al electrode and Al in inorganic-organic composite light emitting device 2 O 3 An external power supply is connected to the substrate, an inorganic unit of the device emits blue light after voltage is applied, an organic unit emits red light, an instrument is used for measuring an initial electroluminescence spectrogram of the device, peaks of the red light and the blue light in the spectrogram are recorded, and the initial peak of the red light is recorded as h; applying a voltage to the device at fixed time T and measuring the electroluminescent spectrum of the device to observe the change delta h of the peak height of red light under the condition of unchanged blue light peak, thereby obtaining the thickness of the organic material which has reacted with water vapor +>
According to the molecular weight M [ H ] 2 0]And an average molecular weight M [ OEAM ] of the organic luminescent material]Processing and correcting electroluminescent spectrum data of the organic light-emitting device to obtain the water vapor transmittance WVTR of the packaging material within T hours in unit area, wherein the data correction of the water vapor transmittance is corrected by adopting a water vapor transmittance coefficient alpha according to the type of the organic light-emitting material, and a specific calculation formula is as follows: />
According to the method, since the method judges how much organic material is corroded by water vapor according to the change of the wave crest of the organic material, the wave crest is measured by a measuring instrument connected with a computer, the data precision is high,the calculated data is reliable, so the accuracy can reach 10 -6 g/m 2 On the order of/24 h, the defect of insufficient testing accuracy of the infrared sensor is overcome.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (1)
1. The non-contact film water-oxygen permeability test method is characterized in that: comprises the following steps of the method,
(1) At 500-550 ℃ under Al 2 O 3 Growing an undoped u-GaN layer with the thickness of about 5 mu m on the substrate at a low temperature;
(2) Heating to about 1200 ℃ to grow an Si doped n-GaN epitaxial layer with the thickness of about 3 mu m;
(3) Then the temperature is reduced to 700 to 750 ℃ to grow In for 8 to 9 periods 0.2 Ga 0.8 The N/GaN multi-quantum well layer, wherein the thickness of the InGaN quantum well layer is about 3nm, the thickness of the GaN quantum barrier layer is about 11.5nm, and finally annealing treatment is carried out at the temperature of 1000 ℃ by a high-temperature annealing furnace to obtain a blue light LED substrate;
(4) Placing various medicines to be evaporated on the blue light LED substrate on a boat source or a crucible source of an evaporation cabin, placing the processed blue light LED substrate on a mask plate in the evaporation cabin, closing an evaporation cabin door, vacuumizing, and when the vacuum degree in the evaporation cabin reaches 10 -5 Starting vapor deposition below mbar, preheating boat source or crucible source corresponding to vapor deposition material before vapor deposition, starting vapor deposition after reaching a certain temperature and proper rate, and controlling current to make vapor deposition rate of organic matters at
According to the step, a layer of organic red light material and a layer of MoO are sequentially evaporated on the blue light LED substrate 3 A hole transport layer as a device;
(5) Vapor deposition is goodAfter each organic layer, evaporating a layer of Al as the electrode of the device, and controlling the evaporation rate of Al to be equal to
Evaporating 300nm;
(6) Packaging the evaporated organic material layer and the metal electrode, and obtaining a complete light-emitting device after packaging;
(7) Al electrode and Al in inorganic-organic composite light emitting device 2 O 3 An external power supply is connected to the substrate, an inorganic unit of the device emits blue light after voltage is applied, an organic unit emits red light, an instrument is used for measuring an initial electroluminescence spectrogram of the device, peaks of the red light and the blue light in the spectrogram are recorded, and the initial peak of the red light is recorded as h;
(8) Applying voltage to the device at fixed time T, measuring electroluminescent spectrum of the device, observing peak height change deltah of red light and thickness d of organic red light material under the condition of unchanged blue light peak, thereby obtaining thickness of organic material which has reacted with water vapor
(9) According to the molecular weight M [ H ] 2 0]And an average molecular weight M [ OEAM ] of the organic luminescent material]Processing and correcting electroluminescent spectrum data of the organic light-emitting device to obtain the water vapor transmittance WVTR of the packaging material within T hours in unit area, wherein the data correction of the water vapor transmittance is corrected by adopting a water vapor transmittance coefficient alpha according to the type of the organic light-emitting material, and a specific calculation formula is as follows:
/>
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