CN107492526A - A kind of flexible water oxygen Obstruct membrane with wide band antireflective effect and preparation method thereof - Google Patents
A kind of flexible water oxygen Obstruct membrane with wide band antireflective effect and preparation method thereof Download PDFInfo
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- CN107492526A CN107492526A CN201710528313.8A CN201710528313A CN107492526A CN 107492526 A CN107492526 A CN 107492526A CN 201710528313 A CN201710528313 A CN 201710528313A CN 107492526 A CN107492526 A CN 107492526A
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- obstruct membrane
- flexible
- membrane
- transparent
- water oxygen
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- 239000012528 membrane Substances 0.000 title claims abstract description 206
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 50
- 239000001301 oxygen Substances 0.000 title claims abstract description 50
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 50
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 230000003667 anti-reflective effect Effects 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000000758 substrate Substances 0.000 claims abstract description 62
- 239000010408 film Substances 0.000 claims abstract description 58
- 238000000034 method Methods 0.000 claims abstract description 51
- 230000003287 optical effect Effects 0.000 claims abstract description 41
- 230000008569 process Effects 0.000 claims abstract description 34
- 238000000427 thin-film deposition Methods 0.000 claims abstract description 24
- 238000010276 construction Methods 0.000 claims abstract description 12
- 239000000463 material Substances 0.000 claims description 48
- 239000002131 composite material Substances 0.000 claims description 22
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 21
- 238000002834 transmittance Methods 0.000 claims description 21
- 238000000151 deposition Methods 0.000 claims description 12
- 230000008021 deposition Effects 0.000 claims description 12
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 10
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 10
- 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
- 239000010703 silicon Substances 0.000 claims description 7
- 229910052710 silicon Inorganic materials 0.000 claims description 7
- 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
- 238000004062 sedimentation Methods 0.000 claims description 6
- 238000005240 physical vapour deposition Methods 0.000 claims description 5
- 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
- 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
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-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
- 229920003229 poly(methyl methacrylate) Polymers 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
- 238000005566 electron beam evaporation 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
- 239000004417 polycarbonate Substances 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
- 229920003207 poly(ethylene-2,6-naphthalate) Polymers 0.000 claims description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 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
- 238000004544 sputter deposition Methods 0.000 claims 1
- 230000004888 barrier function Effects 0.000 abstract description 36
- 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
- 241000894007 species Species 0.000 description 6
- 230000007935 neutral effect Effects 0.000 description 5
- 239000004642 Polyimide Substances 0.000 description 4
- 230000008901 benefit Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 229920001721 polyimide Polymers 0.000 description 4
- 238000009738 saturating Methods 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
- 230000009286 beneficial effect Effects 0.000 description 3
- 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
- 241001269238 Data Species 0.000 description 2
- 239000006117 anti-reflective coating Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000001755 magnetron sputter deposition Methods 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 silicon nitrides Chemical class 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000004425 Makrolon Substances 0.000 description 1
- 229910003978 SiClx Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 238000010923 batch production Methods 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
- 230000002349 favourable effect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 229920005573 silicon-containing polymer Polymers 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000007736 thin film deposition technique Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
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
Landscapes
- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Ceramic Engineering (AREA)
- Electromagnetism (AREA)
- Surface Treatment Of Optical Elements (AREA)
- Laminated Bodies (AREA)
Abstract
The invention discloses a kind of flexible and transparent water oxygen Obstruct membrane and preparation method thereof, the flexible and transparent water oxygen Obstruct membrane is located at more than flexible and transparent substrate；The Obstruct membrane has wide band antireflective effect.The Obstruct membrane is sandwich construction, and the thickness of each layer is in the range of 10nm to 400nm in the Obstruct membrane, and total number of plies of the Obstruct membrane is in the range of 2 to 20 layers.The present invention designs the membrane system mechanism of Obstruct membrane by using multilayer wide-band anti-reflection coating design method in Film Optics theory, the Obstruct membrane 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 Obstruct membrane with wide band antireflective effect that process costs are low, thus solve prior art and lack a kind of technical problem of the water oxygen Obstruct membrane 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
Obstruct membrane and preparation method thereof.
Background technology
Emerging flexible and transparent photoelectric device, such as solar cell (solar cell), the organic light emission two of flexible and transparent
Pole pipe (OLED), Trackpad (touch panel) etc., because it has unique advantage, have in people live and widely should
With prospect, and to be exactly photoelectric device realize flexibility and transparence firstly the need of solution for the preparation of high-performance flexible substrates
Problem.Volume is frivolous, bending performance is good, species is enriched due to possessing for transparent polymer film, and compatible volume to volume 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 in structure design and making
Barrier property and bending property, its optical property can not meet the use demand of flexible and transparent photoelectric device.Therefore, prior art
Lack a kind of not only there is barrier property but also meet the water oxygen Obstruct membrane of optical performance requirements applied to flexible and transparent photoelectric device
And preparation method thereof.
The content of the invention
For the disadvantages described above or Improvement requirement of prior art, have what wide band antireflective acted on the invention provides a kind of
Flexible water oxygen Obstruct membrane 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 Obstruct membrane, the thickness of each tunic material of reasonable set, and utilizes thin film deposition processes by the resistance
Barrier film 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 into
This low flexible water oxygen Obstruct membrane with wide band antireflective effect, thus solution prior art shortage is a kind of applied to flexible saturating
Mingguang City's electrical part not only has barrier property but also meets the technical problem of the water oxygen Obstruct membrane of optical performance requirements.
To achieve the above object, according to one aspect of the present invention, there is provided a kind of flexible and transparent water oxygen Obstruct membrane, it is described
Flexible and transparent water oxygen Obstruct membrane is located at more than flexible and transparent substrate；The Obstruct membrane has wide band antireflective effect；The barrier
The error of the ordinate value of the ordinate value of the CIE chromaticity coordinates of film and the CIE chromaticity coordinates of standard white light is described no more than 0.1%
The error of the abscissa value of the CIE chromaticity coordinates of Obstruct membrane and the abscissa value of the CIE chromaticity coordinates of standard white light is no more than 0.1%.
Preferably, the Obstruct membrane is sandwich construction, and total number of plies of the Obstruct membrane is in the range of 2 to 20 layers, the resistance
For the thickness of each layer in the range of 10nm to 400nm, the gross thickness of the Obstruct membrane is not more than 3 microns in barrier film.
Preferably, the available membrane material of each layer of the Obstruct membrane be silicon nitride, silica, silicon oxynitride, zirconium oxide,
Hafnium oxide, aluminum oxide, titanium oxide, zinc oxide, magnesia, magnesium fluoride, zinc sulphide, molybdenum oxide, tungsten oxide or tantalum oxide, the resistance
Barrier film at least selects two kinds of 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 Obstruct membrane and the flexible and transparent substrate are formed in 430~730nm wave bands
The difference of light transmittance and minimum light transmission rate is not more than 4.2%.
According to another aspect of the present invention, there is provided a kind of preparation method of flexible and transparent water oxygen Obstruct membrane, including such as
Lower step：
(1) flexible and transparent substrate, the membrane material species of Obstruct membrane 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 Obstruct membrane 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 Obstruct membrane it
Between；
(2) sedimentation rate of the thin film deposition processes described in demarcating steps (1), the optical constant of the flexible and transparent substrate
And the optical constant of film made from the thin film deposition processes deposition；The optical constant includes refractive index n and delustring system
Number k；
(3) target broadband range and the number of plies of Obstruct membrane are determined, the Obstruct membrane is at least two layers, according to the target
Broadband range, the reference wavelength determined by the target broadband range, the membrane material species, the number of plies and step of the Obstruct membrane
Suddenly the optical constant of (2) demarcation, adjusts the higher limit and lower limit per a layer thickness so that what final design obtained has multilayer
The gross thickness of the Obstruct membrane of structure is not less than 80nm, and not higher than 3 microns, while make the Obstruct membrane 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%, and this is multiple
Close absolute light transmittance of the film in the target broadband range and be not less than 85%；
(4) step (3) design is obtained according to step (2) sedimentation rate using the thin film deposition processes
Obstruct membrane with sandwich construction is deposited in the flexible and transparent substrate, obtains the flexible and transparent that there is wide band antireflective to act on
Water oxygen Obstruct membrane.
Preferably, step (1) described thin film deposition processes are physical vapour deposition (PVD) or chemical vapor deposition method, including etc.
Plasma enhanced chemical vapor deposition, ald, electron beam evaporation, magnetron sputtering and/or one kind in vacuum thermal evaporation or
It is several.
Preferably, the higher limit of the thickness of described each layer of step (3) is 100~150nm, and lower limit is 20~30nm.
Preferably, step (3) described reference wavelength is the centre wavelength in the target broadband range.
In general, by the contemplated above technical scheme of the present invention compared with prior art, it can obtain down and show
Beneficial effect.
1) flexible and transparent water oxygen Obstruct membrane provided by the invention is located at more than flexible and transparent substrate, by the inorganic of multiple dense
Material is formed, and by the membrane material of reasonable selection Obstruct membrane, by means of the design method of traditional optical film, adjusts membrane system thickness
Set, optimize 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 longitudinal and transverse coordinate value of oxygen Obstruct membrane CIE chromaticity coordinates and the CIE chromaticity coordinates of standard white light
No more than 0.1%, it ensure that the good color of the Obstruct membrane is neutral, therefore the flexible and transparent water oxygen Obstruct membrane of the present invention is taken into account simultaneously
Optical property, barrier property and bending property, it is a kind of film for being ideally suited for emerging flexible and transparent photoelectric device
Material.
2) preparation method of flexible and transparent water oxygen Obstruct membrane of the present invention seems the preparation method using traditional optical film, but
By dexterously setting, adjusting each layer film thickness, disposably it is prepared while meets optical property, barrier property and bending
The Obstruct membrane of performance, preparation technology is simple, and cost is low, efficiency high.
3) present invention is laid out the thickness of each layer in Obstruct membrane film structure by rationally designing, and limits Obstruct membrane gross thickness
No more than 3 microns, the Obstruct membrane so obtained has good bending property.
4) preparation method that the present invention has the flexible and transparent water oxygen Obstruct membrane of wide band antireflective effect uses thin film deposition
Technique, it is the common technology of field of photoelectric devices, cost is low, large area preparation and scale of mass production is adapted to, beneficial to industry
Change and promote.
5) preparation method of flexible and transparent water oxygen Obstruct membrane of the present invention is a kind of universal method, can be according to application
Device service band difference and convert the film structure of Obstruct membrane so that antireflective wave band matches with device service band.
6) present invention is using Obstruct membrane of the deposition with wide band antireflective effect, layer barrier film constructions in flexible and transparent substrate
Densification, flexible and transparent substrate is which overcomed in itself due to the water and oxygen barrier property difference caused by surface porosity is porous the defects of, this
The flexible and transparent water oxygen Obstruct membrane of invention not only remains the advantages of flexible and transparent substrate bending performance is good, and the Obstruct membrane
It is neutral with wide band antireflective effect and good color, therefore meet the application demand of current flexible and transparent photoelectric device, have
It is widely applied 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 substrates, and 430~
Rate that 730nm wave bands are anti-reflection averagely improves 4.82% than the pure anti-reflection rate of PI substrates, and anti-reflection rate is than pure PI substrates at 470nm wavelength
Improve at most, up to 5.97%.What deposition was prepared in PI substrates has barrier property and the wide band antireflective of bending property
Film will have a good application prospect in OLED display field.
Brief description of the drawings
Fig. 1 is the optical constant of PECVD deposited silicon nitrides in embodiment 1, silica and PI films used；
Fig. 2 is the layer barrier film constructions schematic diagram used in embodiment 1；
Fig. 3 is the light transmittance of flexible and transparent substrate and prepared layer barrier film constructions in embodiment 1.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, it is right below in conjunction with drawings and Examples
The present invention is further elaborated.It should be appreciated that specific embodiment described herein is only to explain the present invention, not
For limiting the present invention.As long as in addition, technical characteristic involved in each embodiment of invention described below that
Conflict can is not formed between this to be mutually combined.
Flexible and transparent water oxygen Obstruct membrane provided by the invention, the Obstruct membrane are located at more than flexible and transparent substrate；The Obstruct membrane
Acted on wide band antireflective, the composite membrane that the Obstruct membrane is formed with the flexible and transparent substrate is in 430~730nm wave bands
The difference of highest light transmittance and minimum light transmission rate is not more than 4.2%.The CIE chromaticity coordinates (chromaticity coordinates of CIE 1931) of the Obstruct membrane
Longitudinal and transverse coordinate value and standard white light CIE chromaticity coordinates longitudinal and transverse coordinate value difference absolute value be no more than 0.1%, ensure that
The good color of Obstruct membrane is neutral；The Obstruct membrane is sandwich construction, and total number of plies is in the range of 2 to 20 layers, and the thickness of each layer is in 10nm
To 400nm, and the gross thickness of the Obstruct membrane is not more than 3 microns, can so ensure that the Obstruct membrane has well curved
Qu Xingneng.
The membrane material of the Obstruct membrane can be silicon nitride, silica, silicon oxynitride, zirconium oxide, hafnium oxide, aluminum 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 (PEN), PES (polyether sulfone),
PDMS (dimethyl silicone polymer), PMMA (polymethyl methacrylate) or PC (makrolon) transparent polymer film.Barrier
Membrane material at least selects two kinds of different materials, and meets that the refractive index size of base material is located at selected membrane material and (obstructed
The material of each layer film of film) refractive index size between.
The preparation method of flexible and transparent water oxygen Obstruct membrane 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 Obstruct membrane, is interfered using optical thin film and managed in film optical theory
By writing with reference to conventional optical thin film design software (such as TFcalc, Macleod) or voluntarily 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 having what wide band antireflective acted on
The film structure of Obstruct membrane, then the film structure is deposited in flexible and transparent substrate using thin film deposition processes.
Specifically, the preparation method comprises the following steps：
(1) flexible and transparent substrate, the membrane material species of Obstruct membrane 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 Obstruct membrane at least selects two
Kind different materials, maximum refractive index in the membrane material that the refractive index of the flexible and transparent substrate is selected between the Obstruct membrane and
Between lowest refractive index.
Specifically, the selected principle of flexible and transparent substrate and thin film deposition processes is included following aspects：Obstruct membrane
Material at least selects two kinds of different materials, and the refractive index size of base material should (i.e. Obstruct membrane be each positioned at selected membrane material
The material of layer film) refractive index between the refractive index of maximum refractive index and minimum, could so meet optical property
It is required that；Membrane material need to be transparent in visible light wave range, to ensure relatively low extinction coefficient；The operating temperature of the thin film deposition processes of selection
Glass transition temperature (the T of base material should be less thang)；The thermal expansion of barrier membrane material and flexible and transparent substrate to be deposited
Coefficient needs as far as possible close, otherwise can cause the film breaks of deposition, come off or substrate and Obstruct membrane it is compound obtain later answer
It is Texturized to close film generation；A variety of membrane material depositions can be sequentially completed in same equipment by being chosen as far as possible in the selection of membrane material
The membrane material of Obstruct membrane.
(2) sedimentation rate of the thin film deposition processes described in demarcating steps (1), the optical constant of the flexible and transparent substrate
And the optical constant of film made from the thin film deposition processes deposition；Optical constant is that each wavelength is corresponding in visible light wave range
Refractive index n and extinction coefficient k；
(3) target broadband range and the number of plies of Obstruct membrane are determined, the Obstruct membrane is at least two layers, according to the target
Broadband range, the reference wavelength λ determined by the target broadband range0, selected membrane material species, the number of plies of Obstruct membrane and step
Suddenly the optical constant of (2) demarcation, set using the multilayer wide band antireflective design software adjustment upper and lower limit per a layer thickness
Value so that the gross thickness for the Obstruct membrane with sandwich construction that final design obtains is not less than 80nm, and not higher than 3 microns, together
When make the highest of the light transmittance of composite membrane that the Obstruct membrane and the flexible and transparent substrate form in the target broadband range
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 species, the number of plies of Obstruct membrane, the upper and lower limit per a layer thickness can be according to need
Sets itself is wanted to choose；Reference wavelength λ0The general central value for choosing target broadband range, i.e. centre wavelength；Using optically thin
When wide band antireflective method design software in film theory carries out the structure design of Obstruct membrane, the minimum value of general wavelength is than choosing
Target broadband range the small 20~30nm of minimum value, maximum is bigger by 20 than the maximum of the target broadband range of selection~
30nm, it so may insure that the composite membrane wide band antireflective effect that designs to obtain in target broadband range is more preferable.Target broadband
Visible light wave range is may range from, but is not limited to visible light wave range.
The higher limit and lower limit of each layer of thickness can be adjusted according to the number of plies of the Obstruct membrane of setting, preferably can be with
For the higher limit scope of the every a layer thickness set as 100~150nm, lower limit scope is 20~30nm, in the preferred scope,
Barrier property and the good composite membrane of bending property can be obtained.
(4) step (3) Obstruct membrane is deposited according to the sedimentation rate using step (2) thin film deposition processes
In the flexible and transparent substrate, the flexible and transparent water oxygen Obstruct membrane that there is wide band antireflective to act on 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 method, including plasma-reinforced chemical
Be vapor-deposited (PECVD), ald (ALD), electron beam evaporation, magnetron sputtering and/or one kind in vacuum thermal evaporation or
It is several.
The result that the film structure design of Obstruct membrane of the present invention is a multifactor compromise, considered, utilizes gained light
It is multiple in order to take into account when the design method of constant combination film optics middle width strip antireflective coating designs the film structure of the Obstruct membrane
Bending property, barrier property and the process costs of film are closed, and control the integral thickness of Obstruct membrane to be no more than 3 microns, are preferably controlled
System is further preferably controlled in 0.5 micrometer 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 generally used for optical thin film design in Film Optics theory, and it designs mesh
Be so that thin-film material has wide band antireflective effect, do not required particularly generally for the thickness of the thin-film material.Profit
It is theoretical with optics film interference, write with reference to conventional optical thin film design software (such as TFcalc, Macleod) or voluntarily 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, typically
There is two parameter persons of needing to use sets itself according to demand, one is each layer film upper thickness limit, and another 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 the defects of control and technique realize.
However, the present invention flexible and transparent water oxygen Obstruct membrane 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.Obstruct membrane is thicker or the number of plies is more more more is beneficial to resistance
The improvement of separating performance, but this bending property to Obstruct membrane and saving process costs are unfavorable.The present invention utilizes optically thin
Film interference theory, write with reference to conventional optical thin film design software (such as TFcalc, Macleod) or voluntarily 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, the bending property of Obstruct membrane made from guarantee, the thickness per layer film need to set a suitable higher limit；The opposing party
Face, in order to reduce film defects to obtain more preferable barrier property, and the shadow that thickness deviation caused by reducing fabrication error is brought
Ring, the lower limit of the thickness per tunic is also required to rationally give.Inventors herein have recognized that the thickness when each layer is set as
During 20~120nm scopes, namely the lower thickness limit value of every tunic is set as 20nm, when higher limit is set as 120nm, is prepared
Obstruct membrane can meet optical property, barrier property, bending property and relatively low process costs simultaneously.
By taking the Obstruct membrane 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 λ0Reference wavelength (such as 550nm) is represented, the gross thickness of so obtained Obstruct membrane is 687.5nm, but when setting
For each thickness degree in 20~120nm, the Obstruct membrane gross thickness designed is only 210nm, ensure that good bending in Obstruct membrane
Performance, while its color is neutral and barrier 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 the preferable scheme of one of which, the invention provides a kind of flexible and transparent water oxygen Obstruct membrane, the flexibility
Transparent water oxygen Obstruct membrane is located at more than flexible and transparent substrate PI；The Obstruct membrane has wide band antireflective effect, the Obstruct membrane with it is soft
Property transparent substrates form composite membrane averagely improve 4.82% in the anti-reflection rate of 430~730nm wave bands rate more anti-reflection than PI substrate, should
The ordinate value of the ordinate value of the CIE chromaticity coordinates of Obstruct membrane and the CIE chromaticity coordinates of standard white light the absolute value of difference do not surpass
Cross 0.1%, the abscissa value of the abscissa value of the CIE chromaticity coordinates of the Obstruct membrane and the CIE chromaticity coordinates of standard white light difference
Absolute value be no more than 0.1%.The Obstruct membrane is sandwich construction, and total number of plies is in the range of 2 to 20 layers, each layer in the Obstruct membrane
Thickness in the range of 10nm to 400nm, the gross thickness of the Obstruct membrane is not more than 3 microns.Each layer of the Obstruct membrane can
The material of selection be silicon nitride, silica, silicon oxynitride, zirconium oxide, hafnium oxide, aluminum oxide, titanium oxide, zinc oxide, magnesia,
Magnesium fluoride, zinc sulphide, molybdenum oxide, tungsten oxide or tantalum oxide, the Obstruct membrane preferably at least have two kinds of different materials.
Deposition obtains taking into account the wide band antireflective of optical property, bending property and barrier property in flexible and transparent PI substrates
Film, the composite membrane averagely improve 4.82% in the light transmittance of 430~730nm wave bands than the light transmittance of PI substrate, 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 improves than pure PI substrates at 470nm wavelength
At most, up to 5.97%.What deposition was prepared in PI substrates has barrier property and the wide-band anti-reflection coating of bending property will
Had a good application prospect in OLED display field.
The present invention is introduced into multilayer broadband in Film Optics theory towards the industrialization of the transparent flexible photoelectric device of large area
Antireflecting coating design method, design and be prepared for have the transparent flexible of favorable optical performance, bending property and barrier property to hinder
Barrier film, the design of Obstruct membrane and optical thin film design are combined into one, effectively simplify device architecture and preparation technology, is had
Very high application value.
It is embodiment below：
Embodiment 1
Embodiment 1 is to be deposited in the clear polyimides PI substrates that glass transition temperature is 356 DEG C with pecvd process
Silicon/oxidative silicon alternating structure is nitrogenized, it is as follows the step of use：
1) transparent polyimides PI films are prepared on the glass substrate, and thickness is 20 microns.
2) according to thermal properties such as the glass transition temperature of above-mentioned Kapton, thermal coefficient of expansions, and select
The refractive index of membrane material, the optical property such as extinction coefficient, deposited from pecvd process.
Specifically, because the glass transition temperature of the PI substrates of selection is 356 DEG C, the membrane material of selection is silicon nitride SiNx
And silicon oxide siox(it is not a fixation because different thin film deposition processes deposit obtained silicon nitride and silica atomic ratio
Numerical value, therefore silicon nitride SiN herexAnd silicon oxide sioxContain subscript x) in molecular formula, in the same band silicon nitride SiNxFolding
It is higher than the refractive index of PI film to penetrate rate, and silicon oxide sioxRefractive index it is lower than the refractive index of PI film, 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
Pecvd process can be used disposably to be prepared at 300 DEG C with stove, the technological temperature is less than the glass transition temperature of PI films,
Therefore PECVD has been selected to carry out thin-film technique deposition.
Then SiN is deposited to the PECVD for intending usingxAnd SiOxSpeed, and the light of gained film and Kapton
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 bands, reference wavelength λ0Be chosen to be 550nm, set Obstruct membrane 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 λ0Represent reference
Wavelength.On the premise of barrier property, optical property, bending property and process costs are taken into account, the thickness per tunic is constantly adjusted
Upper limit value and lower limit value, eventually through setting each layer in Obstruct membrane of upper thickness limit value as 120nm, lower limit 20nm, obtained film
Architecture is：PI/SiNx(35nm)/SiOx(25nm)/SiNx(50nm)/SiOx(100nm), the Obstruct membrane share four layers, total thickness
Spend for 210nm, as shown in Fig. 2 the Obstruct membrane of the structure and thickness has good bending property.
4) pecvd process is utilized, said structure is deposited in transparent PI substrates, technological parameter used is as shown in table 1.SiNx
Deposition process in adjust the stress of film by the way of low-and high-frequency modulation.
Process conditions used in the PECVD deposited silicon nitride silica of table 1
5) composite membrane is peeled off from glass substrate.
The Obstruct membrane that the embodiment 1 of table 2 is prepared is in 430~730nm wave band iuuminting rate test datas
| 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% |
Fig. 3 is the saturating of the structure of composite membrane that the flexible and transparent water oxygen Obstruct membrane that the present embodiment is prepared is formed with PI substrates
Light rate, table 2 are the Obstruct membrane in 430~730nm wave band iuuminting rate test datas, design result and actual preparation experimental result
Very close to either design result or experimental result, its average transmittance values all reach more than 91%；As can be seen from Figure 2
After Obstruct membrane is deposited, 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 bands Obstruct membrane averagely improves 4.82% than the anti-reflection rate of pure PI substrates, increases at 470nm wavelength
Saturating rate improves most than pure PI substrates, and up to 5.97%, the composite membrane is in the difference of the wave band highest light transmittance and minimum light transmission rate
4.17%；CIE chromaticity coordinates is expressed as (0.336,0.338) corresponding to the composite membrane, the CIE chromaticity coordinates with standard white light
(0.333,0.333) closely, shows that the Obstruct membrane has good color neutral.
This reality is measured under conditions of 38 DEG C and 100% relative humidity using the moisture-inhibiting instrument of MOCON Permatran W 3/33
The water vapor transmittance (WVTR) for applying the composite membrane (the thick PI films with water oxygen Obstruct membrane) that example is prepared is 1.58 × 10-2g/
(m2·day).Using the oxygen flow instrument of MOCON OxTran 2/21 at 23 DEG C, using purity oxygen as test gas under conditions of measure it is multiple
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 the flexible and transparent water oxygen Obstruct membrane being prepared using the preparation method of the present invention has good water oxygen barrier
Energy.
The present embodiment deposits Obstruct membrane in PI substrates and obtains composite membrane PI/SiNx(35nm)/SiOx(25nm)/SiNx
(50nm)/SiOx(100nm), there is wide band antireflective effect, antireflective effect is very notable, and water and oxygen barrier property is good, and total thickness
Degree is only 210nm, and bending property is good, and the Obstruct membrane 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, all any modification, equivalent and improvement made within the spirit and principles of the invention etc., all should be included
Within protection scope of the present invention.
Claims (10)
- A kind of 1. flexible and transparent water oxygen Obstruct membrane, it is characterised in that：The flexible and transparent water oxygen Obstruct membrane is located at flexible and transparent base It is more than bottom；The Obstruct membrane has wide band antireflective effect；The ordinate value of the CIE chromaticity coordinates of the Obstruct membrane and standard white light CIE chromaticity coordinates ordinate value difference absolute value be no more than 0.1%, the abscissa of the CIE chromaticity coordinates of the Obstruct membrane Value and the abscissa value of the CIE chromaticity coordinates of standard white light difference absolute value no more than 0.1%.
- 2. flexible and transparent water oxygen Obstruct membrane as claimed in claim 1, it is characterised in that the Obstruct membrane is sandwich construction, institute Total number of plies of Obstruct membrane is stated in the range of 2 to 20 layers, the thickness of each layer is in the range of 10nm to 400nm in the Obstruct membrane, institute The gross thickness for stating Obstruct membrane is not more than 3 microns.
- 3. flexible and transparent water oxygen Obstruct membrane as claimed in claim 2, it is characterised in that each layer of the Obstruct membrane can be selected Membrane material for silicon nitride, silica, silicon oxynitride, zirconium oxide, hafnium oxide, aluminum oxide, titanium oxide, zinc oxide, magnesia, fluorination Magnesium, zinc sulphide, molybdenum oxide, tungsten oxide or tantalum oxide, the Obstruct membrane at least select two kinds of different membrane materials.
- 4. flexible and transparent water oxygen Obstruct membrane as claimed in claim 1, it is characterised 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 Obstruct membrane as claimed in claim 1, it is characterised in that the flexible and transparent substrate is PI.
- 6. flexible and transparent water oxygen Obstruct membrane as claimed in claim 1, it is characterised in that the Obstruct membrane and the flexible and transparent The composite membrane that substrate is formed is not more than 4.2% in the highest light transmittance of 430~730nm wave bands and the difference of minimum light transmission rate.
- 7. a kind of preparation method of flexible and transparent water oxygen Obstruct membrane, it is characterised in that comprise the following steps：(1) flexible and transparent substrate, the membrane material species of Obstruct membrane 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 Obstruct membrane is at least two kinds, institute Between the maximum refractive index and lowest refractive index of stating the membrane material that the refractive index of flexible and transparent substrate is selected between the Obstruct membrane；(2) sedimentation rate of the thin film deposition processes described in demarcating steps (1), the optical constant of the flexible and transparent substrate and The optical constant of film made from the thin film deposition processes deposition；The optical constant includes refractive index n and extinction coefficient k；(3) target broadband range and the number of plies of Obstruct membrane are determined, the Obstruct membrane is at least two layers, according to the target broadband Scope, the reference wavelength determined by the target broadband range, the membrane material species, the number of plies and step of the Obstruct membrane (2) optical constant of demarcation, higher limit and lower limit per a layer thickness are adjusted so that what final design obtained has multilayer knot The gross thickness of the Obstruct membrane of structure is not less than 80nm, and not higher than 3 microns, while make the Obstruct membrane and the flexible and transparent substrate structure Into 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%；(4) had using the thin film deposition processes according to step (2) sedimentation rate by what step (3) design obtained The Obstruct membrane of sandwich construction is deposited in the flexible and transparent substrate, obtains the flexible and transparent water oxygen that there is wide band antireflective to act on Obstruct membrane.
- 8. preparation method as claimed in claim 7, it is characterised in that step (1) described thin film deposition processes are physical vapor Deposition or chemical vapor deposition method, including plasma reinforced chemical vapour deposition, ald, electron beam evaporation, magnetic control One or more in sputtering and/or vacuum thermal evaporation.
- 9. preparation method as claimed in claim 7, it is characterised in that step (3) described reference wavelength is the target broadband In the range of centre wavelength.
- 10. preparation method as claimed in claim 7, it is characterised in that the higher limit of the thickness of described each layer of step (3) is 100~150nm, lower limit are 20~30nm.
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| CN110172674A (en) * | 2019-05-29 | 2019-08-27 | 汕头万顺新材集团股份有限公司 | A kind of high transparency barrier film and preparation method thereof |
| CN111474607A (en) * | 2020-04-21 | 2020-07-31 | Tcl华星光电技术有限公司 | Coating for reducing reflectivity, display panel and display device |
| CN111712929A (en) * | 2018-02-23 | 2020-09-25 | 中建材蚌埠玻璃工业设计研究院有限公司 | Solar module with uniform color impression |
| CN112277416A (en) * | 2020-10-29 | 2021-01-29 | 合肥乐凯科技产业有限公司 | Barrier film and preparation method thereof |
| CN112640087A (en) * | 2018-08-28 | 2021-04-09 | 深圳市柔宇科技股份有限公司 | Display panel and display device |
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