CN107492526B - A kind of flexible water oxygen barrier film and preparation method thereof with wide band antireflective effect - Google Patents
A kind of flexible water oxygen barrier film and preparation method thereof with wide band antireflective effect Download PDFInfo
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- CN107492526B CN107492526B CN201710528313.8A CN201710528313A CN107492526B CN 107492526 B CN107492526 B CN 107492526B CN 201710528313 A CN201710528313 A CN 201710528313A CN 107492526 B CN107492526 B CN 107492526B
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- water oxygen
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- 230000004888 barrier function Effects 0.000 title claims abstract description 182
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 239000001301 oxygen Substances 0.000 title claims abstract description 51
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 51
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 230000003667 anti-reflective effect Effects 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000010408 film Substances 0.000 claims abstract description 206
- 239000000758 substrate Substances 0.000 claims abstract description 62
- 239000012528 membrane Substances 0.000 claims abstract description 55
- 238000000034 method Methods 0.000 claims abstract description 53
- 230000003287 optical effect Effects 0.000 claims abstract description 41
- 230000008569 process Effects 0.000 claims abstract description 37
- 238000013461 design Methods 0.000 claims abstract description 31
- 238000000427 thin-film deposition Methods 0.000 claims abstract description 24
- 239000000463 material Substances 0.000 claims description 48
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 21
- 239000002131 composite material Substances 0.000 claims description 21
- 238000002834 transmittance Methods 0.000 claims description 21
- 238000000151 deposition Methods 0.000 claims description 16
- 230000008021 deposition Effects 0.000 claims description 15
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 12
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 11
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 11
- 230000005540 biological transmission Effects 0.000 claims description 9
- 230000009477 glass transition Effects 0.000 claims description 9
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 8
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 8
- 239000000377 silicon dioxide Substances 0.000 claims description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 6
- 230000008033 biological extinction Effects 0.000 claims description 6
- 238000005240 physical vapour deposition Methods 0.000 claims description 6
- 229910052710 silicon Inorganic materials 0.000 claims description 6
- 239000010703 silicon Substances 0.000 claims description 6
- 229920006254 polymer film Polymers 0.000 claims description 5
- 239000004695 Polyether sulfone Substances 0.000 claims description 4
- 239000005083 Zinc sulfide Substances 0.000 claims description 4
- 238000000231 atomic layer deposition Methods 0.000 claims description 4
- 238000005229 chemical vapour deposition Methods 0.000 claims description 4
- 229910000449 hafnium oxide Inorganic materials 0.000 claims description 4
- WIHZLLGSGQNAGK-UHFFFAOYSA-N hafnium(4+);oxygen(2-) Chemical compound [O-2].[O-2].[Hf+4] WIHZLLGSGQNAGK-UHFFFAOYSA-N 0.000 claims description 4
- 239000000395 magnesium oxide Substances 0.000 claims description 4
- 229910000476 molybdenum oxide Inorganic materials 0.000 claims description 4
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 claims description 4
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 claims description 4
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 claims description 4
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 4
- 229920003207 poly(ethylene-2,6-naphthalate) Polymers 0.000 claims description 4
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims description 4
- 239000004417 polycarbonate Substances 0.000 claims description 4
- 229920006393 polyether sulfone Polymers 0.000 claims description 4
- 239000011112 polyethylene naphthalate Substances 0.000 claims description 4
- 229920000139 polyethylene terephthalate Polymers 0.000 claims description 4
- 239000005020 polyethylene terephthalate Substances 0.000 claims description 4
- 239000004926 polymethyl methacrylate Substances 0.000 claims description 4
- 229910001936 tantalum oxide Inorganic materials 0.000 claims description 4
- 229910001930 tungsten oxide Inorganic materials 0.000 claims description 4
- 239000011787 zinc oxide Substances 0.000 claims description 4
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 claims description 4
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 3
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 3
- 235000013870 dimethyl polysiloxane Nutrition 0.000 claims description 3
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 3
- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 claims description 3
- 239000012994 photoredox catalyst Substances 0.000 claims description 3
- 238000004987 plasma desorption mass spectroscopy Methods 0.000 claims description 3
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 3
- 238000002207 thermal evaporation Methods 0.000 claims description 3
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 claims description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims 1
- 238000010894 electron beam technology Methods 0.000 claims 1
- 230000008020 evaporation Effects 0.000 claims 1
- 238000001704 evaporation Methods 0.000 claims 1
- 238000003682 fluorination reaction Methods 0.000 claims 1
- 229910052749 magnesium Inorganic materials 0.000 claims 1
- 239000011777 magnesium Substances 0.000 claims 1
- 229920003208 poly(ethylene sulfide) Polymers 0.000 claims 1
- 238000005452 bending Methods 0.000 abstract description 24
- 239000011248 coating agent Substances 0.000 abstract description 8
- 238000000576 coating method Methods 0.000 abstract description 8
- 230000007246 mechanism Effects 0.000 abstract description 2
- 239000010409 thin film Substances 0.000 description 11
- 229910052814 silicon oxide Inorganic materials 0.000 description 10
- 229910004205 SiNX Inorganic materials 0.000 description 9
- 230000008901 benefit Effects 0.000 description 5
- 230000007935 neutral effect Effects 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 239000004642 Polyimide Substances 0.000 description 4
- 238000010276 construction Methods 0.000 description 4
- 229920001721 polyimide Polymers 0.000 description 4
- MEYZYGMYMLNUHJ-UHFFFAOYSA-N tunicamycin Natural products CC(C)CCCCCCCCCC=CC(=O)NC1C(O)C(O)C(CC(O)C2OC(C(O)C2O)N3C=CC(=O)NC3=O)OC1OC4OC(CO)C(O)C(O)C4NC(=O)C MEYZYGMYMLNUHJ-UHFFFAOYSA-N 0.000 description 4
- 230000007547 defect Effects 0.000 description 3
- 230000006872 improvement Effects 0.000 description 3
- ORUIBWPALBXDOA-UHFFFAOYSA-L magnesium fluoride Chemical compound [F-].[F-].[Mg+2] ORUIBWPALBXDOA-UHFFFAOYSA-L 0.000 description 3
- 229910001635 magnesium fluoride Inorganic materials 0.000 description 3
- 238000009738 saturating Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 239000006117 anti-reflective coating Substances 0.000 description 2
- 238000005566 electron beam evaporation Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000012788 optical film Substances 0.000 description 2
- 229920003223 poly(pyromellitimide-1,4-diphenyl ether) Polymers 0.000 description 2
- -1 polyethylene terephthalate Polymers 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 229910003978 SiClx Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
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- 238000007254 oxidation reaction Methods 0.000 description 1
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- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 description 1
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- 229920005573 silicon-containing polymer Polymers 0.000 description 1
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Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L23/00—Details of semiconductor or other solid state devices
- H01L23/28—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L23/00—Details of semiconductor or other solid state devices
- H01L23/28—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection
- H01L23/29—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection characterised by the material, e.g. carbon
- H01L23/291—Oxides or nitrides or carbides, e.g. ceramics, glass
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/02—Details
- H01L31/0216—Coatings
Abstract
The invention discloses a kind of flexible and transparent water oxygen barrier film and preparation method thereof, which is located at flexible and transparent substrate or more；The barrier film has wide band antireflective effect.The barrier film is multilayered structure, and the thickness of each layer is within the scope of 10nm to 400nm in the barrier film, and total number of plies of the barrier film is within the scope of 2 to 20 layers.The present invention designs the membrane system mechanism of barrier film by using multilayer wide-band anti-reflection coating design method in Film Optics theory, the barrier film is deposited in flexible and transparent substrate using thin film deposition processes, one kind has been prepared and has taken into account barrier property, bending property and optical property, and the flexible water oxygen barrier film with wide band antireflective effect that process costs are low, thus solve the technical issues of prior art lacks a kind of water oxygen barrier film that both there is barrier property to meet optical performance requirements applied to flexible and transparent photoelectric device.
Description
Technical field
The invention belongs to field of photoelectric devices, more particularly, to a kind of flexible water oxygen with wide band antireflective effect
Barrier film and preparation method thereof.
Background technique
Emerging flexible and transparent photoelectric device, such as solar battery (solar cell), the organic light emission two of flexible and transparent
Pole pipe (OLED), Trackpad (touch panel) etc. have widely answer in people's lives because it is with unique advantage
With prospect, and the preparation of high-performance flexible substrates is exactly that photoelectric device realizes flexibility and transparence firstly the need of solution
Problem.Volume is frivolous, bending performance is good, type is abundant due to having for transparent polymer film, and compatible roll-to-roll large area
The many advantages such as batch production technique become the first choice of non-transparent flexible substrate.
However, thin polymer film due to its intrinsic loose porous surface and water and oxygen barrier property is low, it is difficult to meet light
The requirement of electrical part, and on the other hand, existing layer barrier film constructions due to only considering mostly when structure designs and makes
Barrier property and bending property, optical property are not able to satisfy the use demand of flexible and transparent photoelectric device.Therefore, the prior art
Lack a kind of water oxygen barrier film that not only there is barrier property but also meet optical performance requirements applied to flexible and transparent photoelectric device
And preparation method thereof.
Summary of the invention
Aiming at the above defects or improvement requirements of the prior art, the present invention provides a kind of with wide band antireflective effect
Flexible water oxygen barrier film and preparation method thereof, its object is to set by using multilayer wide-band anti-reflection coating in Film Optics theory
Meter method designs the membrane system mechanism of barrier film, the film thickness of each tunic material of reasonable set, and utilizes thin film deposition processes by the resistance
Diaphragm is deposited in flexible and transparent substrate, and one kind is prepared and takes into account barrier property, bending property and optical property, and technique at
This low flexible water oxygen barrier film with wide band antireflective effect, thus the solution prior art lacks one kind and is applied to flexibility thoroughly
The technical issues of water oxygen barrier film that not only there is barrier property but also meet optical performance requirements of Mingguang City's electrical part.
To achieve the above object, according to one aspect of the present invention, a kind of flexible and transparent water oxygen barrier film is provided, it is described
Flexible and transparent water oxygen barrier film is located at flexible and transparent substrate or more；The barrier film has wide band antireflective effect；The barrier
The error of the ordinate value of the CIE chromaticity coordinates of the ordinate value and standard white light of the CIE chromaticity coordinates of film is described no more than 0.1%
The error of the abscissa value of the CIE chromaticity coordinates of the abscissa value and standard white light of the CIE chromaticity coordinates of barrier film is no more than 0.1%.
Preferably, the barrier film is multilayered structure, and total number of plies of the barrier film is within the scope of 2 to 20 layers, the resistance
For the thickness of each layer within the scope of 10nm to 400nm, the overall thickness of the barrier film is not more than 3 microns in diaphragm.
Preferably, the available membrane material of each layer of the barrier film be silicon nitride, silica, silicon oxynitride, zirconium oxide,
Hafnium oxide, aluminium oxide, titanium oxide, zinc oxide, magnesia, magnesium fluoride, zinc sulphide, molybdenum oxide, tungsten oxide or tantalum oxide, the resistance
Diaphragm at least selects two different membrane materials.
Preferably, the flexible and transparent substrate is PI, PET, PEN, PES, PDMS, PMMA or PC transparent polymer film.
Preferably, the flexible and transparent substrate is PI.
Preferably, highest of the composite membrane that the barrier film and the flexible and transparent substrate are constituted in 430~730nm wave band
The difference of light transmittance and minimum light transmission rate is not more than 4.2%.
Other side according to the invention provides a kind of preparation method of flexible and transparent water oxygen barrier film, including such as
Lower step:
(1) flexible and transparent substrate, the membrane material type of barrier film and thin film deposition processes are selected, so that the flexible and transparent
The glass transition temperature of substrate is higher than the operating temperature of the thin film deposition processes, and the membrane material of the barrier film is at least two
Kind, the maximum refractive index and lowest refractive index of the membrane material that the refractive index of the flexible and transparent substrate is selected between the barrier film it
Between；
(2) deposition rate of thin film deposition processes described in demarcating steps (1), the optical constant of the flexible and transparent substrate
And the thin film deposition processes deposit the optical constant of film obtained；The optical constant includes refractive index n and delustring system
Number k；
(3) determine that the number of plies of target broadband range and barrier film, the barrier film are at least two layers, according to the target
Broadband range, reference wavelength, the membrane material type, the number of plies and step of the barrier film determined by the target broadband range
Suddenly (2) calibration optical constant, adjust the upper limit value and lower limit value of every a layer thickness so that final design obtain have multilayer
The overall thickness of the barrier film of structure is not less than 80nm, and is not higher than 3 microns, while making the barrier film and the flexible and transparent substrate
The peak of light transmittance of the composite membrane of composition in the target broadband range and the difference of minimum are no more than 4.2%, this is multiple
It closes absolute light transmittance of the film in the target broadband range and is not less than 85%；
(4) step (3) design is obtained according to step (2) deposition rate using the thin film deposition processes
Barrier film with multi-layer structure is deposited in the flexible and transparent substrate, obtains the flexible and transparent with wide band antireflective effect
Water oxygen barrier film.
Preferably, step (1) thin film deposition processes be physical vapour deposition (PVD) or chemical vapor deposition process, including etc.
One of plasma enhanced chemical vapor deposition, atomic layer deposition, electron beam evaporation, magnetron sputtering and/or vacuum thermal evaporation or
It is several.
Preferably, the upper limit value of step (3) each layer of the thickness is 100~150nm, and lower limit value is 20~30nm.
Preferably, step (3) reference wavelength is the central wavelength in the target broadband range.
In general, through the invention it is contemplated above technical scheme is compared with the prior art, can obtain down and show
Beneficial effect.
1) flexible and transparent water oxygen barrier film provided by the invention is located at flexible and transparent substrate or more, by the inorganic of multiple dense
Material is constituted, and by reasonably selecting the membrane material of barrier film, by means of the design method of traditional optical film, adjusts membrane system thickness
Setting, optimizes the broadband light transmittance for the composite membrane being prepared, the composite membrane finally obtained is in target broadband range iuuminting rate
The difference of peak and minimum is not more than 4.2%, and absolute light transmittance is not less than 85%, while flexible and transparent water prepared by the present invention
The absolute value of the difference of the longitudinal and transverse coordinate value of the CIE chromaticity coordinates of the longitudinal and transverse coordinate value and standard white light of oxygen barrier film CIE chromaticity coordinates
No more than 0.1%, it ensure that the good color of the barrier film is neutral, therefore flexible and transparent water oxygen barrier film of the invention combines
Optical property, barrier property and bending property are a kind of films for being ideally suited for emerging flexible and transparent photoelectric device
Material.
2) preparation method of flexible and transparent water oxygen barrier film of the present invention seems the preparation method using traditional optical film, but
By being dexterously arranged, adjusting each layer film thickness, optical property, barrier property and bending are disposably prepared while met
The barrier film of performance, preparation process is simple, at low cost, high-efficient.
3) present invention is by rationally designing the thickness of each layer in layout barrier film film structure, and limits barrier film overall thickness
No more than 3 microns, the barrier film obtained in this way has good bending property.
4) there is the present invention preparation method of the flexible and transparent water oxygen barrier film of wide band antireflective effect to be deposited using film
Technique is the common technology of field of photoelectric devices, at low cost, is adapted to large area preparation and scale of mass production, is conducive to industry
Change and promotes.
5) preparation method of flexible and transparent water oxygen barrier film of the present invention is a kind of universal method, can be according to application
The difference of device service band and convert the film structure of barrier film so that antireflective wave band matches with device service band.
6) present invention is using barrier film of the deposition with wide band antireflective effect, layer barrier film constructions in flexible and transparent substrate
Densification, which overcome flexible and transparent substrate itself due to surface porosity it is porous caused by water and oxygen barrier property difference defect, this
The flexible and transparent water oxygen barrier film of invention not only remains the good advantage of flexible and transparent substrate bending performance, but also the barrier film
It is neutral with wide band antireflective effect and good color, therefore meet the application demand of current flexible and transparent photoelectric device, have
Broad application prospect.
7) PI is a kind of flexible base material with good thermal property and solvent resistance, and the present invention is flexible saturating
Deposition obtains taking into account the wide-band anti-reflection coating of optical property, bending property and barrier property in bright PI substrate, and 430~
Rate that 730nm wave band is anti-reflection is more anti-reflection than pure PI substrate, and rate averagely improves 4.82%, and anti-reflection rate is than pure PI substrate at 470nm wavelength
It improves at most, up to 5.97%.The wide band antireflective with barrier property and bending property being prepared is deposited in PI substrate
Film will have a good application prospect in OLED display field.
Detailed description of the invention
Fig. 1 is the optical constant of PECVD deposited silicon nitride in embodiment 1, silica and PI film used；
Fig. 2 is layer barrier film constructions schematic diagram used in Example 1；
Fig. 3 is the light transmittance of flexible and transparent substrate and prepared layer barrier film constructions in embodiment 1.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further elaborated.It should be appreciated that described herein, specific examples are only used to explain the present invention, not
For limiting the present invention.As long as in addition, technical characteristic involved in the various embodiments of the present invention described below that
Not constituting conflict between this can be combined with each other.
Flexible and transparent water oxygen barrier film provided by the invention, the barrier film are located at flexible and transparent substrate or more；The barrier film
With wide band antireflective effect, the composite membrane that the barrier film and the flexible and transparent substrate are constituted is in 430~730nm wave band
The difference of highest light transmittance and minimum light transmission rate is not more than 4.2%.The CIE chromaticity coordinates (1931 chromaticity coordinate of CIE) of the barrier film
Longitudinal and transverse coordinate value and standard white light CIE chromaticity coordinates longitudinal and transverse coordinate value absolute value of the difference be no more than 0.1%, ensure that
The good color of barrier film is neutral；The barrier film is multilayered structure, and total number of plies is within the scope of 2 to 20 layers, and the thickness of each layer is in 10nm
To 400nm, and the overall thickness of the barrier film is not more than 3 microns, and it is good curved can to guarantee that the barrier film has in this way
Qu Xingneng.
The membrane material of the barrier film can be silicon nitride, silica, silicon oxynitride, zirconium oxide, hafnium oxide, aluminium oxide, oxidation
At least two in titanium, zinc oxide, magnesia, magnesium fluoride, zinc sulphide, molybdenum oxide, tungsten oxide and tantalum oxide.Flexible and transparent substrate
For PI (polyimides), PET (polyethylene terephthalate), PEN (polyethylene naphthalate), PES (polyether sulfone),
PDMS (dimethyl silicone polymer), PMMA (polymethyl methacrylate) or PC (polycarbonate) transparent polymer film.Barrier
Membrane material at least selects two kinds of different materials, and the refractive index size for meeting base material is located at selected membrane material and (obstructs
The material of each layer film of film) refractive index size between.
The preparation method of flexible and transparent water oxygen barrier film provided by the invention with wide band antireflective effect is using thin
The film structure of multilayer wide-band anti-reflection coating design method design barrier film, is interfered using optical thin film and is managed in film optical theory
By in conjunction with common optical thin film design software (such as TFcalc, Macleod) or voluntarily writing program (such as MATLAB, C language
Speech etc.), by rationally designing the thickness of each layer and the order of high low-index layer, it can obtain that there is wide band antireflective effect
Then the film structure is deposited in flexible and transparent substrate by the film structure of barrier film using thin film deposition processes.
Specifically, which includes the following steps:
(1) flexible and transparent substrate, the membrane material type of barrier film and thin film deposition processes are selected, so that the flexible and transparent
The glass transition temperature of substrate is higher than the operating temperature of the thin film deposition processes, and the membrane material of the barrier film at least selects two
Kind different materials, maximum refractive index of the refractive index of the flexible and transparent substrate in the membrane material that the barrier film is selected and
Between lowest refractive index.
Specifically, the selected principle of flexible and transparent substrate and thin film deposition processes includes following aspects: barrier film
Material at least selects two kinds of different materials, and the refractive index size of base material should (i.e. barrier film be each positioned at selected membrane material
The material of layer film) refractive index between maximum refractive index and the smallest refractive index, be just able to satisfy optical property in this way
It is required that；Membrane material need to be transparent in visible light wave range, to ensure lower extinction coefficient；The operating temperature of the thin film deposition processes of selection
Glass transition temperature (the T of base material should be lower thang)；The thermal expansion of barrier membrane material and flexible and transparent substrate to be deposited
Coefficient needs to approach as far as possible, otherwise will cause the film breaks of deposition, fall off or substrate and barrier film it is compound after obtain answer
It is Texturized to close film generation；A variety of membrane material depositions can be sequentially completed in same equipment by choosing as far as possible in the selection of membrane material
The membrane material of barrier film.
(2) deposition rate of thin film deposition processes described in demarcating steps (1), the optical constant of the flexible and transparent substrate
And the thin film deposition processes deposit the optical constant of film obtained；Optical constant is that each wavelength is corresponding in visible light wave range
Refractive index n and extinction coefficient k；
(3) determine that the number of plies of target broadband range and barrier film, the barrier film are at least two layers, according to the target
Broadband range, the reference wavelength λ determined by the target broadband range0, selected membrane material type, the number of plies of barrier film and step
Suddenly the optical constant of (2) calibration is set using the upper and lower limit that multilayer wide band antireflective design software adjusts described every a layer thickness
Value so that the overall thickness for the barrier film with multi-layer structure that final design obtains is not less than 80nm, and is not higher than 3 microns, together
When constitute the barrier film and the flexible and transparent substrate light transmittance of the composite membrane in the target broadband range highest
Value and the difference of minimum are no more than 4.2%, and absolute light transmittance of the composite membrane in the target broadband range is not less than 85%.
Wherein target broadband range, membrane material type, the number of plies of barrier film, every a layer thickness upper and lower limit can be according to need
Sets itself is wanted to choose；Reference wavelength λ0The general central value for choosing target broadband range, i.e. central wavelength；Using optically thin
When wide band antireflective method design software in film theory carries out the structure design of barrier film, the minimum value of general wavelength is than choosing
Target broadband range the small 20~30nm of minimum value, maximum value is bigger by 20 than the maximum value of the target broadband range of selection~
30nm may insure that the composite membrane wide band antireflective effect designed in target broadband range is more preferable in this way.Target broadband
It may range from visible light wave range, but be not limited to visible light wave range.
The upper limit value and lower limit value of each layer of thickness can be adjusted according to the number of plies of the barrier film of setting, it preferably can be with
For the upper limit value range of the every a layer thickness set as 100~150nm, lower limit value range is 20~30nm, in the preferred scope,
Available barrier property and the good composite membrane of bending property.
(4) step (3) barrier film is deposited according to the deposition rate using step (2) thin film deposition processes
In the flexible and transparent substrate, the flexible and transparent water oxygen barrier film with wide band antireflective effect is obtained.
(5) optical property, water and oxygen barrier property and bending property is carried out to deposition gained composite membrane to characterize.
Wherein, thin film deposition processes are physical vapour deposition (PVD) or chemical vapor deposition process, including plasma-reinforced chemical
Be vapor-deposited (PECVD), atomic layer deposition (ALD), electron beam evaporation, one of magnetron sputtering and/or vacuum thermal evaporation or
It is several.
Barrier film of the present invention film structure design be one it is multifactor compromise, comprehensively consider as a result, utilize gained light
It is multiple in order to balance when the design method of constant combination film optics middle width strip antireflective coating designs the film structure of the barrier film
Bending property, barrier property and the process costs of film are closed, and the integral thickness for controlling barrier film is no more than 3 microns, preferably controls
System is further preferably controlled in 0.5 micron range, total number of plies is between 2~20 layers in the range of 1 micron.
The design method of multilayer wide-band anti-reflection coating is commonly used in optical thin film design in Film Optics theory, designs mesh
Be so that thin-film material have wide band antireflective effect, do not required particularly generally for the thickness of the thin-film material.Benefit
It is theoretical with optics film interference, in conjunction with common optical thin film design software (such as TFcalc, Macleod) or voluntarily write journey
When the order of thickness and high low-index layer that sequence (such as MATLAB, C language) designs each layer carries out film structure design, generally
User's sets itself according to demand is needed there are two parameter, one is each layer film upper thickness limit, the other is each layer film
Lower thickness limit, in traditional optical thin film design, the setting of the two parameters is primary concern is that meeting optical property
Under the premise of film layer powder injection molding and technique realize.
However, the present invention flexible and transparent water oxygen barrier film with wide band antireflective effect to be designed not only needs to meet
Optical property, while also its barrier property and bending property are required.Barrier film is thicker or the number of plies the more more are conducive to resistance
The improvement of separating performance, but this is to the bending property of barrier film and to save the process cost be unfavorable.The present invention utilizes optically thin
Film interference theory in conjunction with common optical thin film design software (such as TFcalc, Macleod) or voluntarily writes program (such as
MATLAB, C language etc.) each layer of design thickness and high low-index layer order when, on the one hand, in order to control the entirety of membrane system
Thickness, guarantees the bending property of barrier film obtained, and the thickness of every layer film needs to set a suitable upper limit value；Another party
Face in order to reduce film defects to obtain better barrier property, and reduces film thickness deviation bring shadow caused by fabrication error
It rings, the lower limit value of the thickness of every tunic is also required to rationally given.The inventors of the present application found that the thickness when each layer is set as
When 20~120nm range namely the lower thickness limit value of every tunic is set as 20nm, when upper limit value is set as 120nm, is prepared
Barrier film can meet optical property, barrier property, bending property and lower process costs simultaneously.
By taking the barrier film of four-layer structure as an example, a kind of structure of typical four layers of wide-band anti-reflection coating is λ0/4-λ0/4-λ0/
2-λ0/ 4 wherein λ0It indicating reference wavelength (such as 550nm), the overall thickness of barrier film obtained in this way is 687.5nm, but when setting
For each thickness degree in 20~120nm, the barrier film overall thickness designed is only 210nm in barrier film, ensure that good bending
Performance, while its color is neutral and barrier property is all fine.
PI (polyimides) is a kind of with good thermal property (glass transition temperature is 356 DEG C) and solvent resistance
Flexible base material, as one of preferred scheme, the present invention provides a kind of flexible and transparent water oxygen barrier film, the flexibilities
Transparent water oxygen barrier film is located at flexible and transparent substrate PI or more；The barrier film have wide band antireflective effect, the barrier film with it is soft
Property transparent substrates constitute composite membrane averagely improve 4.82% in the anti-reflection rate of the anti-reflection rate ratio PI substrate of 430~730nm wave band, should
The ordinate value of the CIE chromaticity coordinates of the ordinate value and standard white light of the CIE chromaticity coordinates of barrier film absolute value of the difference do not surpass
Cross 0.1%, the abscissa value of the CIE chromaticity coordinates of the abscissa value and standard white light of the CIE chromaticity coordinates of the barrier film difference
Absolute value be no more than 0.1%.The barrier film is multilayered structure, and total number of plies is within the scope of 2 to 20 layers, each layer in the barrier film
Thickness within the scope of 10nm to 400nm, the overall thickness of the barrier film is not more than 3 microns.Each layer of the barrier film can
The material of selection be silicon nitride, silica, silicon oxynitride, zirconium oxide, hafnium oxide, aluminium oxide, titanium oxide, zinc oxide, magnesia,
Magnesium fluoride, zinc sulphide, molybdenum oxide, tungsten oxide or tantalum oxide, the barrier film preferably at least have two different materials.
Deposition obtains taking into account the wide band antireflective of optical property, bending property and barrier property in flexible and transparent PI substrate
Film, the composite membrane averagely improve 4.82% in the light transmittance of the light transmittance ratio PI substrate of 430~730nm wave band, the composite membrane
It is 4.17% in the difference of the wave band highest light transmittance and minimum light transmission rate, anti-reflection rate is improved than pure PI substrate at 470nm wavelength
At most, up to 5.97%.The wide-band anti-reflection coating with barrier property and bending property that deposition is prepared in PI substrate will
It has a good application prospect in OLED display field.
The industrialization of transparent flexible photoelectric device of the present invention towards large area is introduced into multilayer broadband in Film Optics theory
Antireflecting coating design method has designed and prepared the transparent flexible resistance with favorable optical performance, bending property and barrier property
The design of barrier film and optical thin film design are combined into one, effectively simplify device architecture and preparation process, have by diaphragm
Very high application value.
The following are embodiments:
Embodiment 1
Embodiment 1 is to be deposited in the clear polyimides PI substrate that glass transition temperature is 356 DEG C with pecvd process
The step of nitridation silicon/oxidative silicon alternating structure, use, is as follows:
1) transparent polyimides PI film is prepared, on the glass substrate with a thickness of 20 microns.
2) it according to thermal properties such as the glass transition temperature of above-mentioned Kapton, thermal expansion coefficients, and selects
The optical properties such as refractive index, the extinction coefficient of membrane material, select pecvd process deposition.
Specifically, since the glass transition temperature of the PI substrate of selection is 356 DEG C, the membrane material of selection is silicon nitride SiNx
And silicon oxide siox(silicon nitride and silica atomic ratio deposited due to different thin film deposition processes is not a fixation
Numerical value, therefore silicon nitride SiN herexAnd silicon oxide sioxContain subscript x) in molecular formula, in the same band silicon nitride SiNxFolding
The refractive index for penetrating rate ratio PI film is high, and silicon oxide sioxRefractive index ratio PI film refractive index it is low, and silicon nitride SiNxAnd oxygen
SiClx SiOxIt is transparent (extinction coefficient is low) in visible light wave range, therefore meet the requirement of optical property.Due to both membrane materials
It can disposably be prepared with furnace using pecvd process at 300 DEG C, which is lower than the glass transition temperature of PI film,
Therefore PECVD has been selected to carry out thin-film technique deposition.
Then SiN is deposited to the PECVD of proposed adoptionxAnd SiOxRate and gained film and Kapton light
Learning constant, (refractive index n and extinction coefficient k) are demarcated, as a result as shown in Figure 1.
3) determine target broadband range in 430~730nm wave band, reference wavelength λ0Be chosen to be 550nm, set barrier film as
By SiNxAnd SiOxAlternate four layer series structure, using gained optical constant, combination film optics middle width strip antireflective coating is set
Meter method, a kind of typical structure that design obtains four layers of broadband anti-reflection film is λ0/4-λ0/4-λ0/2-λ0/ 4, wherein λ0Indicate reference
Wavelength.Under the premise of taking into account barrier property, optical property, bending property and process costs, the thickness of every tunic is constantly adjusted
Upper limit value and lower limit value, eventually by setting each layer in barrier film of upper thickness limit value as 120nm, lower limit value 20nm, obtained film
Architecture is: PI/SiNx(35nm)/SiOx(25nm)/SiNx(50nm)/SiOx(100nm), the barrier film share four layers, total thickness
Degree is 210nm, as shown in Fig. 2, the structure and the barrier film of thickness have good bending property.
4) pecvd process is utilized, above structure is deposited in transparent PI substrate, technological parameter used is as shown in table 1.SiNx
Deposition process in adjust the stress of film by the way of the low-and high-frequency modulation.
Process conditions used in 1 PECVD deposited silicon nitride silica of table
5) composite membrane is removed from glass substrate.
The barrier film that 2 embodiment 1 of table is prepared is in 430~730nm wave band iuuminting rate test data
| Maximum transmission rate %@wavelength | Maximum transmission rate %@wavelength | Average transmittance | |
| Design result | 93.48%@650nm | 89.31%@430nm | 92.84% |
| Experimental result | 92.28%@641nm | 86.71%@430nm | 91.68% |
The structure of composite membrane that Fig. 3, which is the flexible and transparent water oxygen barrier film that is prepared of the present embodiment, to be constituted with PI substrate it is saturating
Light rate, table 2 are the barrier film in 430~730nm wave band iuuminting rate test data, design result and practical preparation experimental result
Very close to either design result or experimental result, average transmittance values all reach 91% or more；As can be seen from Figure 2
After depositing barrier film, the light transmittance of composite membrane is all significantly increased in entirely design wave band (430~730nm).Wherein 430
The anti-reflection rate of~730nm wave band barrier film averagely improves 4.82% than the anti-reflection rate of pure PI substrate, increases at 470nm wavelength
Saturating rate improves at most than pure PI substrate, and up to 5.97%, which is in the difference of the wave band highest light transmittance and minimum light transmission rate
4.17%；The corresponding CIE chromaticity coordinates of the composite membrane is expressed as (0.336,0.338), the CIE chromaticity coordinates with standard white light
(0.333,0.333) closely, shows that the barrier film has good color neutral.
This reality is measured under conditions of 38 DEG C and 100% relative humidity using 3/33 moisture-inhibiting instrument of MOCON Permatran W
The water vapor transmittance (WVTR) for applying the composite membrane (the thick PI film with water oxygen barrier film) that example is prepared is 1.58 × 10-2g/
(m2·day).It is to test under conditions of gas to measure again with purity oxygen using 2/21 oxygen flow instrument of MOCON OxTran at 23 DEG C
The OTR oxygen transmission rate (OTR) for closing film is 5.96 × 10-2cm3/(m2·day).And 20 microns thick of pure PI under the conditions of same test
The water vapor transmittance and OTR oxygen transmission rate test result of film are respectively 85.3g/ (m2) and 200cm day3/(m2·day).Thus
It can be seen that there is good water oxygen barrier property using the flexible and transparent water oxygen barrier film that preparation method of the invention is prepared
Energy.
The present embodiment deposits barrier film in PI substrate and obtains composite membrane PI/SiNx(35nm)/SiOx(25nm)/SiNx
(50nm)/SiOx(100nm) has wide band antireflective effect, and antireflective effect is very significant, and water and oxygen barrier property is good, and total thickness
Degree is only 210nm, and bending property is good, which meets the use demand of existing flexible and transparent photoelectric device, has
Huge potential using value.
As it will be easily appreciated by one skilled in the art that the foregoing is merely illustrative of the preferred embodiments of the present invention, not to
The limitation present invention, any modifications, equivalent substitutions and improvements made within the spirit and principles of the present invention should all include
Within protection scope of the present invention.
Claims (8)
1. a kind of flexible and transparent water oxygen barrier film, it is characterised in that: the flexible and transparent water oxygen barrier film is located at flexible and transparent base
It is more than bottom；The barrier film has wide band antireflective effect；The ordinate value and standard white light of the CIE chromaticity coordinates of the barrier film
CIE chromaticity coordinates ordinate value absolute value of the difference be no more than 0.1%, the abscissa of the CIE chromaticity coordinates of the barrier film
Value and the abscissa value of the CIE chromaticity coordinates of standard white light absolute value of the difference be no more than 0.1%；
The preparation method of the flexible and transparent water oxygen barrier film, includes the following steps:
(1) flexible and transparent substrate, the membrane material type of barrier film and thin film deposition processes are selected, so that the flexible and transparent substrate
Glass transition temperature be higher than the operating temperatures of the thin film deposition processes, the membrane material of the barrier film is at least two kinds, institute
The refractive index of flexible and transparent substrate is stated between the maximum refractive index and lowest refractive index for the membrane material that the barrier film is selected；
(2) deposition rate of thin film deposition processes described in demarcating steps (1), the optical constant of the flexible and transparent substrate and
The thin film deposition processes deposit the optical constant of film obtained；The optical constant includes refractive index n and extinction coefficient k；
(3) determine that the number of plies of target broadband range and barrier film, the barrier film are at least two layers, according to the target broadband
Range, reference wavelength, the membrane material type, the number of plies and step of the barrier film determined by the target broadband range
(2) demarcate optical constant, adjust the upper limit value and lower limit value of every a layer thickness so that final design obtain have multilayer knot
The overall thickness of the barrier film of structure is not less than 80nm, and is not higher than 3 microns, while making the barrier film and the flexible and transparent substrate structure
At the peak of light transmittance of the composite membrane in the target broadband range and the difference of minimum be no more than 4.2%, this is compound
Absolute light transmittance of the film in the target broadband range is not less than 85%；The barrier film and the flexible and transparent substrate are constituted
Composite membrane 430~730nm wave band highest light transmittance and minimum light transmission rate difference be not more than 4.2%；
(4) had according to step (2) deposition rate by what step (3) design obtained using the thin film deposition processes
The barrier film of multilayered structure is deposited in the flexible and transparent substrate, obtains the flexible and transparent water oxygen with wide band antireflective effect
Barrier film.
2. flexible and transparent water oxygen barrier film as described in claim 1, which is characterized in that the barrier film is multilayered structure, institute
Total number of plies of barrier film is stated within the scope of 2 to 20 layers, the thickness of each layer is within the scope of 10nm to 400nm in the barrier film, institute
The overall thickness of barrier film is stated no more than 3 microns.
3. flexible and transparent water oxygen barrier film as claimed in claim 2, which is characterized in that each layer of the barrier film can be selected
Membrane material be silicon nitride, silica, silicon oxynitride, zirconium oxide, hafnium oxide, aluminium oxide, titanium oxide, zinc oxide, magnesia, fluorination
Magnesium, zinc sulphide, molybdenum oxide, tungsten oxide or tantalum oxide, the barrier film at least select two different membrane materials.
4. flexible and transparent water oxygen barrier film as described in claim 1, which is characterized in that the flexible and transparent substrate be PI,
PET, PEN, PES, PDMS, PMMA or PC transparent polymer film.
5. flexible and transparent water oxygen barrier film as described in claim 1, which is characterized in that the flexible and transparent substrate is PI.
6. flexible and transparent water oxygen barrier film as described in claim 1, which is characterized in that step (1) described thin film deposition processes
For physical vapour deposition (PVD) or chemical vapor deposition process, including plasma reinforced chemical vapour deposition, atomic layer deposition, electron beam
One or more of evaporation, magnetron sputtering and/or vacuum thermal evaporation.
7. flexible and transparent water oxygen barrier film as described in claim 1, which is characterized in that step (3) described reference wavelength is institute
State the central wavelength in target broadband range.
8. flexible and transparent water oxygen barrier film as described in claim 1, which is characterized in that step (3) each layer of the thickness
Upper limit value be 100~150nm, lower limit value be 20~30nm.
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| JPH0868990A (en) * | 1994-08-29 | 1996-03-12 | Mitsui Toatsu Chem Inc | Gas barrier type low moisture permeable insulating transparent substrate for electrode and its use |
| CN1700826A (en) * | 2004-05-20 | 2005-11-23 | 株式会社半导体能源研究所 | Light-emitting element and display device |
| CN105637453A (en) * | 2013-10-18 | 2016-06-01 | 应用材料公司 | Layer stack for a touch panel and method for forming a layer stack |
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|---|---|---|---|---|
| JPH0868990A (en) * | 1994-08-29 | 1996-03-12 | Mitsui Toatsu Chem Inc | Gas barrier type low moisture permeable insulating transparent substrate for electrode and its use |
| CN1700826A (en) * | 2004-05-20 | 2005-11-23 | 株式会社半导体能源研究所 | Light-emitting element and display device |
| CN105637453A (en) * | 2013-10-18 | 2016-06-01 | 应用材料公司 | Layer stack for a touch panel and method for forming a layer stack |
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