CN101553599A - Multilayered coatings for use on electronic devices or other articles - Google Patents
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- CN101553599A CN101553599A CNA2007800456525A CN200780045652A CN101553599A CN 101553599 A CN101553599 A CN 101553599A CN A2007800456525 A CNA2007800456525 A CN A2007800456525A CN 200780045652 A CN200780045652 A CN 200780045652A CN 101553599 A CN101553599 A CN 101553599A
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- 238000000576 coating method Methods 0.000 title claims abstract description 34
- 239000000463 material Substances 0.000 claims abstract description 75
- 239000002243 precursor Substances 0.000 claims abstract description 62
- 238000000034 method Methods 0.000 claims abstract description 53
- 238000006243 chemical reaction Methods 0.000 claims abstract description 49
- 239000000376 reactant Substances 0.000 claims abstract description 32
- 239000011248 coating agent Substances 0.000 claims abstract description 31
- 238000005229 chemical vapour deposition Methods 0.000 claims abstract description 21
- 230000008569 process Effects 0.000 claims abstract description 20
- 229910052814 silicon oxide Inorganic materials 0.000 claims abstract description 7
- 229920005573 silicon-containing polymer Polymers 0.000 claims abstract description 4
- 239000007789 gas Substances 0.000 claims description 43
- 239000002861 polymer material Substances 0.000 claims description 31
- 238000000151 deposition Methods 0.000 claims description 26
- 150000001875 compounds Chemical class 0.000 claims description 21
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 19
- 239000001301 oxygen Substances 0.000 claims description 19
- 229910052760 oxygen Inorganic materials 0.000 claims description 19
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 14
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 claims description 14
- 229910000077 silane Inorganic materials 0.000 claims description 14
- 230000008021 deposition Effects 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 239000000203 mixture Substances 0.000 claims description 12
- 239000000126 substance Substances 0.000 claims description 12
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 claims description 8
- -1 dimethyl siloxane Chemical class 0.000 claims description 8
- 230000008859 change Effects 0.000 claims description 7
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 6
- UIUXUFNYAYAMOE-UHFFFAOYSA-N methylsilane Chemical compound [SiH3]C UIUXUFNYAYAMOE-UHFFFAOYSA-N 0.000 claims description 6
- 238000004062 sedimentation Methods 0.000 claims description 6
- 238000007373 indentation Methods 0.000 claims description 5
- QBEXJDZIRVSLFV-UHFFFAOYSA-N N-ethyl-N-silyloxyethanamine Chemical compound CCN(CC)O[SiH3] QBEXJDZIRVSLFV-UHFFFAOYSA-N 0.000 claims description 4
- 239000004642 Polyimide Substances 0.000 claims description 4
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims description 4
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N diphenyl Chemical compound C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 claims description 4
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 claims description 4
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 4
- 229920001721 polyimide Polymers 0.000 claims description 4
- 239000001294 propane Substances 0.000 claims description 4
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims description 4
- 238000005096 rolling process Methods 0.000 claims description 4
- RSNQKPMXXVDJFG-UHFFFAOYSA-N tetrasiloxane Chemical compound [SiH3]O[SiH2]O[SiH2]O[SiH3] RSNQKPMXXVDJFG-UHFFFAOYSA-N 0.000 claims description 4
- 208000037656 Respiratory Sounds Diseases 0.000 claims description 3
- 230000004087 circulation Effects 0.000 claims description 3
- 230000001143 conditioned effect Effects 0.000 claims description 3
- 230000004044 response Effects 0.000 claims description 3
- 239000000758 substrate Substances 0.000 claims description 3
- BPMGYFSWCJZSBA-UHFFFAOYSA-N C[SiH](C)O[SiH3] Chemical compound C[SiH](C)O[SiH3] BPMGYFSWCJZSBA-UHFFFAOYSA-N 0.000 claims description 2
- DCERHCFNWRGHLK-UHFFFAOYSA-N C[Si](C)C Chemical compound C[Si](C)C DCERHCFNWRGHLK-UHFFFAOYSA-N 0.000 claims description 2
- 235000010290 biphenyl Nutrition 0.000 claims description 2
- 150000001718 carbodiimides Chemical class 0.000 claims description 2
- UBHZUDXTHNMNLD-UHFFFAOYSA-N dimethylsilane Chemical compound C[SiH2]C UBHZUDXTHNMNLD-UHFFFAOYSA-N 0.000 claims description 2
- PZPGRFITIJYNEJ-UHFFFAOYSA-N disilane Chemical compound [SiH3][SiH3] PZPGRFITIJYNEJ-UHFFFAOYSA-N 0.000 claims description 2
- GCSJLQSCSDMKTP-UHFFFAOYSA-N ethenyl(trimethyl)silane Chemical compound C[Si](C)(C)C=C GCSJLQSCSDMKTP-UHFFFAOYSA-N 0.000 claims description 2
- KCWYOFZQRFCIIE-UHFFFAOYSA-N ethylsilane Chemical compound CC[SiH3] KCWYOFZQRFCIIE-UHFFFAOYSA-N 0.000 claims description 2
- HTDJPCNNEPUOOQ-UHFFFAOYSA-N hexamethylcyclotrisiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O1 HTDJPCNNEPUOOQ-UHFFFAOYSA-N 0.000 claims description 2
- HZVOZRGWRWCICA-UHFFFAOYSA-N methanediyl Chemical compound [CH2] HZVOZRGWRWCICA-UHFFFAOYSA-N 0.000 claims description 2
- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 0.000 claims description 2
- OKHRRIGNGQFVEE-UHFFFAOYSA-N methyl(diphenyl)silicon Chemical compound C=1C=CC=CC=1[Si](C)C1=CC=CC=C1 OKHRRIGNGQFVEE-UHFFFAOYSA-N 0.000 claims description 2
- WKWOFMSUGVVZIV-UHFFFAOYSA-N n-bis(ethenyl)silyl-n-trimethylsilylmethanamine Chemical compound C[Si](C)(C)N(C)[SiH](C=C)C=C WKWOFMSUGVVZIV-UHFFFAOYSA-N 0.000 claims description 2
- HMMGMWAXVFQUOA-UHFFFAOYSA-N octamethylcyclotetrasiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O1 HMMGMWAXVFQUOA-UHFFFAOYSA-N 0.000 claims description 2
- 230000035935 pregnancy Effects 0.000 claims description 2
- 238000006884 silylation reaction Methods 0.000 claims description 2
- CZDYPVPMEAXLPK-UHFFFAOYSA-N tetramethylsilane Chemical compound C[Si](C)(C)C CZDYPVPMEAXLPK-UHFFFAOYSA-N 0.000 claims description 2
- PQDJYEQOELDLCP-UHFFFAOYSA-N trimethylsilane Chemical compound C[SiH](C)C PQDJYEQOELDLCP-UHFFFAOYSA-N 0.000 claims description 2
- 229940094989 trimethylsilane Drugs 0.000 claims description 2
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 2
- 229920002554 vinyl polymer Polymers 0.000 claims description 2
- 229910010272 inorganic material Inorganic materials 0.000 claims 2
- 239000011147 inorganic material Substances 0.000 claims 2
- 150000003377 silicon compounds Chemical class 0.000 claims 1
- 230000007704 transition Effects 0.000 claims 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical class [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 abstract description 5
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 abstract description 2
- 230000003287 optical effect Effects 0.000 abstract description 2
- 150000003961 organosilicon compounds Chemical class 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 103
- 229920000642 polymer Polymers 0.000 description 46
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 description 12
- 229910004298 SiO 2 Inorganic materials 0.000 description 9
- 239000011541 reaction mixture Substances 0.000 description 9
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 8
- 230000004888 barrier function Effects 0.000 description 8
- 229910052710 silicon Inorganic materials 0.000 description 8
- 239000010703 silicon Substances 0.000 description 8
- 238000010586 diagram Methods 0.000 description 7
- 230000006866 deterioration Effects 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 4
- 229910052729 chemical element Inorganic materials 0.000 description 4
- 230000002950 deficient Effects 0.000 description 4
- 239000011888 foil Substances 0.000 description 4
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 4
- 238000003860 storage Methods 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 229920001296 polysiloxane Polymers 0.000 description 3
- 238000009736 wetting Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 229910018557 Si O Inorganic materials 0.000 description 2
- 229910052581 Si3N4 Inorganic materials 0.000 description 2
- 238000004630 atomic force microscopy Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 229920001577 copolymer Polymers 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 230000008595 infiltration Effects 0.000 description 2
- 238000001764 infiltration Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 230000003252 repetitive effect Effects 0.000 description 2
- 229910010271 silicon carbide Inorganic materials 0.000 description 2
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 2
- VFHJWQUCFQTIAR-UHFFFAOYSA-N 2-methylideneoxatrisiletane Chemical compound C=[Si]1O[SiH2][SiH2]1 VFHJWQUCFQTIAR-UHFFFAOYSA-N 0.000 description 1
- OPLQHQZLCUPOIX-UHFFFAOYSA-N 2-methylsilirane Chemical compound CC1C[SiH2]1 OPLQHQZLCUPOIX-UHFFFAOYSA-N 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 229910018540 Si C Inorganic materials 0.000 description 1
- 229910002808 Si–O–Si Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
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- 239000012080 ambient air Substances 0.000 description 1
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- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 229920003223 poly(pyromellitimide-1,4-diphenyl ether) Polymers 0.000 description 1
- 229920000548 poly(silane) polymer Polymers 0.000 description 1
- 229920003257 polycarbosilane Polymers 0.000 description 1
- 239000013047 polymeric layer Substances 0.000 description 1
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Abstract
A method for forming a multilayered coating over a surface is disclosed. The method comprises providing a single source of precursor material and transporting the precursor material to a reaction location adjacent a surface to be coated. A first layer is deposited over the surface by chemical vapor deposition using the single source of precursor material, under a first set of reaction conditions. A second layer is deposited over the surface by chemical vapor deposition using the single source of precursor material, under a second set of reaction conditions. The first layer may have a predominantly polymeric component and the second layer may have a predominantly non-polymeric component. The chemical vapor deposition process may be plasma-enhanced and may be performed using a reactant gas. The precursor material may be an organo-silicon compound, such as a siloxane. The first and second layers may comprise various types of polymeric materials, such as silicone polymers, and various types of non-polymeric materials, such as silicon oxides. The multilayered coating may have various characteristics suitable for use with organic light-emitting devices, such as optical transparency, impermeability, and/or flexibility.
Description
[0001] the application incorporates the U.S. Patent application No._____ integral body that is entitled as " Mixed Composition Layers for Use as Coatings onElectronic Devices or Other Articles " of Sigurd Wagner and Prashant Mandlik into this paper by reference, and the attorney docket number of this application is No.10020/35301 and submits in same date with the application.
[0002] the present invention is supported under the contract No.W911QX-06-C-0017 that authorizes ground force research department (Army ResearchOffice) by United States Government to finish.United States Government can enjoy certain right in the present invention.
Technical field
[0003] the present invention relates to be used for the barrier coat of electron device.
Background technology
[0004] organic electronic devices for example organic luminescent device (OLED) when being exposed to water vapour or oxygen, be easy to deterioration.Its protectiveness barrier coat to the exposure of water vapour or oxygen of the last minimizing of OLED can help to improve the life-span and the performance of device.Considered that silicon oxide film, silicon nitride film or the pellumina that will successfully be used for food product pack are used as the barrier coat of OLED.Yet these mineral membranes tend to contain microdefect, and these microdefects allow water vapour and oxygen to diffuse through this film.In some cases, described defective is revealed as crackle in brittle film.Though this diffusing capacity is acceptable for edible product, it is unacceptable for OLED.For addressing this is that, on OLED, the multilayer barrier coating of using alternative inorganic layer and polymer layer is tested, find that the infiltration of water vapour and oxygen is had the resistivity of improvement.But the method for making these laminated coatings may be trouble and costliness.Therefore, there are the needs that manufacturing are applicable to other method of the laminated coating of protecting OLED.
General introduction
[0005] on the one hand, the invention provides the method that forms coating from the teeth outwards, comprising: the single precursor material source (a) is provided; (b) precursor material is transported to response location with surperficial adjacency to be coated; (c) use this single precursor material source to deposit the first layer by chemical vapour deposition in this surface under the first group reaction condition, this first layer has 100: 0-75: 25 polymer materials and non-polymer material weight ratio; (d) use this single precursor material source to deposit the second layer by chemical vapour deposition in this surface under the second group reaction condition, this second layer has 0: 100-25: 75 polymer materials and non-polymer material weight ratio.
[0006] chemical vapor deposition process can be the plasma body enhanced and can use reactant gas to carry out.Precursor material can be for example siloxanes of silicoorganic compound.Polymer layer can comprise for example silicone polymer of various types of polymer materialss, and non-polymer layer can comprise for example Si oxide of various types of non-polymer materials.This laminated coating can have and is suitable for the various performances used with organic luminescent device, for example optical transparence, impenetrability and/or snappiness.
The accompanying drawing summary
[0007] Fig. 1 has shown the synoptic diagram of the PE-CVD equipment that can be used for implementing certain embodiments of the invention.
[0008] Fig. 2 has shown the viewgraph of cross-section of the part of the OLED with multilayer barrier coating.
[0009] Fig. 3 has shown that contrast applies the experimental result of the deterioration of OLED and naked OLED.
Describe in detail
[0010] on the one hand, the invention provides the method that forms from the teeth outwards laminated coating. The method comprises by chemical vapour deposition (CVD) from the teeth outwards square deposited polymer layer and non-polymer Layer. Under the first group reaction condition, use the single precursor material source individually or add reaction Thing gas deposits non-polymer layer. Under the second group reaction condition, use identical single before The body material source individually or add reactant gas and come deposited polymer layer.
[0011] as in this article employed, term " non-polymer " refers to by having clear and definite Limit the material that the molecule of chemical formula consists of, that described molecule has is single, clearly limit Molecular weight. " non-polymer " molecule can have very large molecular weight. In some cases, Nonpolymer molecules can comprise repetitive. As in this article employed, term " polymerization Thing " refer to the material that consisted of by the molecule with repetition subunit (subunit) that covalency connects Material, and the molecular weight of described molecule can not wait between molecule and molecule, and this is because poly-Close the repetitive that reaction can produce for each molecule different numbers. Polymer comprises but not Be limited to homopolymers and copolymer for example block, grafting, the random or copolymer that replaces, and it Blend and variant. Polymer includes but not limited to the polymer of carbon or silicon.
[0012] " polymer layer " is made of polymer materials substantially, but can comprise the non-polymer material of even storage (at the most 5%).This idol storage is enough little, makes those skilled in the art can think that still this layer is polymkeric substance.Equally, " non-polymer layer " is made of non-polymer material substantially, but can comprise the polymer materials of even storage (at the most 5%).This idol storage is enough little, makes those skilled in the art can think that still this layer is non-polymer.
[0013] can use various technology to determine the polymkeric substance of layer/non-polymer composition, these technology comprise moisten contact angle, infrared absorption, hardness and the snappiness of water droplet.For example, the moisten contact angle of the straight polymer layer that is formed by HMDSO is about 103 °.Like this, in some cases, the first layer has 60 °-115 °, preferred 75 °-115 ° moisten contact angle.The moisten contact angle of pure zirconia silicon layer is about 32 °.Like this, in some cases, the second layer has 0 °-60 ° moisten contact angle.If it should be noted that moisten contact angle is measured then it is measuring of forming on the surface of the film of firm sedimentation state.Because moisten contact angle can very big variation take place because of deposit post-treatment, the measurement of carrying out after such processing may accurately not reflect layer composition.It is believed that these moisten contact angles are applicable to the many layers that formed by organosilicon precursor.Preferably, the first layer has 1MPa-3GPa, the more preferably nano-indentation hardness of 0.2-2GPa.Preferably, the second layer has 10GPa-200GPa, the more preferably nano-indentation hardness of 10GPa-20GPa.In some cases, at least one layer has 0.1nm-10nm, the more preferably surfaceness of 0.2nm-0.35nm (rootmean-square).In some cases, at least one layer be when having enough snappinesies when being deposited on the thick layer of 4 μ m on the thick polyimide foil substrate of 50 μ m, makes not change observing microstructure under 0.2% the stretching strain (ε) after at least 55000 rollings circulations on the 1 inch diameter roll.In some cases, at least one layer has enough snappinesies, makes crackle not occur under at least 0.35% stretching strain (ε) (those skilled in the art thought can make usually 4 μ m pure zirconia silicon layer rimose stretching strain levels).
[0014] by pure non-polymer material for example the individual layer barrier coat made of silicon oxide can have the multiple advantage that relates to light transmission, good adhesion and good membrane stress.Yet these non-polymeric layers tend to contain microdefect, and described defective allows water vapour and oxygen to diffuse through this layer.Alternative polymer layer and non-polymer layer can reduce the permeability of coating.Be not intended to bound by theoryly, the inventor thinks, the defective in the non-polymeric layer that polymer layer will be close to is sheltered and/or planarization, thereby reduces the diffusion via described defective.
[0015] as used herein, " single precursor material source " is meant provides the source that forms polymer layer and necessary all precursor materials of non-polymer layer by CVD (adding or do not add reactant gas) precursors to deposit material the time.This is intended to get rid of the method for wherein using a kind of precursor material to form polymer layer and using different precursor materials formation non-polymer layers.By using the single precursor material source, this deposition method is simplified.For example, the single precursor material source can be eliminated the needs of the stream of precursor material independently and monitor the needs of following that this independently flows.
[0016] precursor material can be the mixture of simplification compound or multiple compound.In some cases, when the precursor material was the mixture of multiple compound, the every kind of different compounds self in the mixture can serve as precursor material independently.For example, precursor material can be the mixture of hexamethyldisiloxane (HMDSO) and dimethyl siloxane (DMSO).
[0017] in some cases, plasma enhanced CVD (PE-CVD) can be used for the deposition of each layer.For comprising that low temperature depositing, uniform coating form and the multiple reason of controllable process parameter, PE-CVD can be ideal.Be applicable to that various PE-CVD method of the present invention is well known in the art, comprise those methods of using the RF energy to produce plasma body.
[0018] precursor material is the material that can form polymer materials and non-polymer material when depositing by chemical vapour deposition.Various such precursor materials all are applicable to the present invention and with regard to their various characteristics it are selected.For example, precursor material can be selected with regard to the stoichiometric ratio of its chemical element content, its chemical element and/or the polymer materials that forms under CVD and non-polymer material.For example, silicoorganic compound such as siloxanes are compounds that is suitable as precursor material.The representative example of silicone compounds comprises hexamethyldisiloxane (HMDSO) and dimethyl siloxane (DMSO).When depositing by CVD, these silicone compounds can form for example silicone polymer and non-polymer material silicon oxide for example of polymer materials.Also can for example expense, nontoxicity, handling characteristics, the ability, volatility, molecular weight etc. of at room temperature keeping liquid phase be selected precursor material with regard to various other characteristics.
[0019] other silicoorganic compound that are suitable as precursor material comprise methyl-monosilane; Dimethylsilane; Vinyl trimethylsilane; Trimethyl silane; Tetramethylsilane; Ethylsilane; Disilane methylmethane (disilanomethane); Two (methyl-monosilane base) methane (bis (methyl-silano) methane); 1, and 2-disilane base ethane (1,2-disilanoethane); 1, two (methyl-monosilane base) ethane (1,2-bis (methylsilano) ethane) of 2-; 2, and 2-disilane base propane (2,2-disilanopropane); 1,3,5-three silylation-2,4, the 6-trimethylene (1,3,5-trisilano-2,4,6-trimethylene) and the fluorinated derivatives of these compounds.The silicoorganic compound that contain phenyl that are suitable as precursor material comprise: dimethylphenylsilaneand and diphenylmethylsilane.The oxygen silicoorganic compound that contain that are suitable as precursor material comprise: dimethyldimethoxysil,ne; 1,3,5, the 7-tetramethyl-ring tetrasiloxane; 1,1,3, the 3-tetramethyl disiloxane; 1, two (silylation methylene radical) sily oxide (1,3-bis (silanomethylene) disiloxane) of 3-; Two (1-methyl disiloxanyl-) methane; 2, two (the 1-methyl disiloxanyl-) propane of 2-; 2,4,6, the 8-tetramethyl-ring tetrasiloxane; Octamethylcyclotetrasiloxane; 2,4,6,8,10-pentamethyl-D5; 1,3,5,7-tetrasilane base-2,6-dioxy-4, the 8-dimethylene (1,3,5,7-tetrasilano-2,6-dioxy-4,8-dimethylene); Hexamethyl cyclotrisiloxane; 1,3-dimethyl sily oxide; 1,3,5,7,9-pentamethyl-D5; The fluorinated derivatives of hexa methoxy sily oxide and these compounds.The nitrogenous silicoorganic compound that are suitable as precursor material comprise: hexamethyldisilazane; The divinyl tetramethyl-disilazane; Pregnancy basic ring three silazane; Two (the N-methyl kharophen) silane of dimethyl; Dimethyl is two-(N-ethyl kharophen) silane; Two (the N-methyl kharophen) silane of methyl ethylene; Two (the N-butyl kharophen) silane of methyl ethylene; Methyl three (N-phenyl kharophen) silane; Vinyl three (N-ethyl kharophen) silane; Four (N-methyl kharophen) silane; Two (diethyl aminooxy) silane of phenylbenzene; Methyl three (diethyl aminooxy) silane; With two (trimethyl silicon based) carbodiimide.
[0020] when using PE-CVD, precursor material can be used in combination with the reactant gas that reacts with this precursor material in PE-CVD technology.The use of reactant gas is well known in the art among the PE-CVD, and multiple reactant gas is applicable to the present invention, comprises oxygen-containing gas (O for example
2, ozone, water) and nitrogenous gas (for example ammonia).Reactant gas can be used for changing the stoichiometric ratio of the chemical element that exists in the reaction mixture.For example, when the silxoane precursors material when containing oxygen or nitrogenous reactant gas and use, reactant gas will change oxygen in the reaction mixture or the nitrogen stoichiometric ratio with respect to silicon and carbon.This stoichiometric relation between the various chemical elements in the reaction mixture (for example silicon, carbon, oxygen, nitrogen) can change by some modes.A kind of mode is the concentration that changes precursor material in the reaction or reactant gas.Another kind of mode is that change precursor material or reactant gas enter the flow velocity of reaction.Another mode is to change the precursor material be used to react or the type of reactant gas.
[0021] material type that forms of the chemical vapour deposition by precursor material will depend on that carrying out CVD handles residing reaction conditions.Can limit described reaction conditions by the composition of reaction mixture, this composition comprises the type of employed precursor material and reactant gas and the amount of these materials.For example, reaction mixture can contain siloxane gas (for example HMDSO or DMSO) as precursor material and contain aerobic as reactant gas.Can come the amount of conditioned reaction mixture material by the flow velocity that changes these materials.For example, by changing the flow velocity of precursor material and reactant gas, can deposit dissimilar materials.In some cases, there is not reactant gas (for example the flow velocity with reactant gas is made as zero) in the reaction mixture.Other parameter of defined reaction condition comprises various processing parameters for example RF power and frequency, deposition pressure, temperature and depositing time.
[0022] in the method for the invention, using the first group reaction condition to have by the CVD deposition mainly is the first layer of polymeric constituent.Depend on employed reaction conditions, precursor material can form various types of non-polymer materials.Non-polymer material can be inorganic or organic.For example, silicoorganic compound as precursor material and with contain oxygen reactant gas when combination, non-polymer material can comprise Si oxide for example SiO, SiO
2With mixed valence oxide S iO
xWhen depositing with nitrogenous reactant gas, non-polymer material can comprise silicon nitride (SiN
x).Other non-polymer material that can form comprises the oxycarbide of silicon carbide, silicon and the oxynitride of silicon.Preferably, the first layer has 100: 0-75: 25 polymkeric substance and non-polymer weight ratio.
[0023] using the second group reaction condition to have by the CVD deposition mainly is the second layer of non-polymeric ingredients.Depend on employed reaction conditions, precursor material can form various types of polymer materialss.Polymer materials can be inorganic or organic.For example, when using silicoorganic compound as precursor material, sedimentary mixolimnion can comprise that the polymer chain of Si-O key, Si-C key or Si-O-C key is to form polysiloxane, Polycarbosilane and polysilane and organic polymer.Preferably, the second layer has 0: 100-25: 75 polymkeric substance and non-polymer weight ratio.
[0024] therefore, the method for the application of the invention, can form have alternative mainly be polymkeric substance the layer and mainly be non-polymer the layer laminated coating.This coating can possess the characteristic of the various uses of being applicable to.Such characteristic comprises light transmission, impenetrability, snappiness, thickness, tack and other mechanical property.For example, total thickness that can be by changing coating, the thickness of polymer layer are regulated in these characteristics one or more with respect to the number of the thickness of non-polymer layer and alternating layer.For example, this coating can have the impenetrability that 3 to 5 pairs of polymkeric substance/non-polymer layers obtain desired level.In some cases, polymer layer can have the thickness of 0.1 μ m-10 μ m, and non-polymer layer can have the thickness of 0.05 μ m-10 μ m.Other number of layers and thickness also are possible and can change the thickness of each layer independently.
[0025] a kind of method that can characterize layer is the moisten contact angle of water droplet, and this is a kind of technology as known in the art.Determine that a kind of method whether laminated coating has a following alternating layer is to measure wetting angle, described alternating layer has mainly to be the component of polymkeric substance and mainly to be the component of non-polymer.For example, if the first layer has the wetting angle greater than 60 ° (or 60 °-115 °), and the second layer has the wetting angle less than 60 ° (or 60 °-0 °), can think that then the first layer has than the remarkable more polymkeric substance of the second layer.As an example, the contact angle of polymkeric substance pp-HMDSO is 103 °, and non-polymer SiO
2Contact angle be 32 °.In some cases, if the moisten contact angle between the first layer and the second layer differs a certain amount of, can think that then this laminated coating has alternating layer.For example, the feature of laminated coating can be for having alternating layer, and the first layer mostly are polymkeric substance, wherein the first layer has the moisten contact angle bigger at least 15 ° than the second layer.
[0026] polymer layer and non-polymer layer can deposit by any order.In some cases, before the deposition polymerization layer, deposit non-polymer layer.In other situation, deposited polymer layer before the deposition non-polymer layer.For example, can be from the teeth outwards at first deposited polymer layer serve as planarization layer.
[0027] can on all kinds goods, deposit this laminated coating.In some cases, these goods can be for example OLED of organic electronic devices.For OLED, this laminated coating can serve as the barrier coat of opposing water vapour and oxygen infiltration.For example, have less than 10
-6G/m
2/ day steam permeating rate and/or less than 10
-3G/m
2The laminated coating of the oxygen transmission rates in/sky can be suitable for protecting OLED.In some cases, the thickness of laminated coating can be 0.5-10 μ m, but depends on that purposes also can use other thickness.In addition, having the thickness of the light transmission of giving and the laminated coating of material composition can be suitable for using with OLED.In order to use, laminated coating can be designed to have the snappiness of aequum with flexible OLED.In some cases, can be to using this laminated coating on other goods of deterioration sensitivity when being exposed to environment, described goods are pharmaceuticals, medicine equipment, biological reagent, biological sample, biosensor or other sensitive measurement equipment for example.
[0028] can use any reactor in all kinds CVD reactor to implement method of the present invention.As an embodiment, Fig. 1 has shown the PE-CVD equipment 10 that can be used for implementing certain embodiments of the invention.PE-CVD equipment 10 comprises reaction chamber 20, and electron device 30 is loaded on the anchor clamps 24 in this reaction chamber.Reaction chamber 20 is designed to contain vacuum and vacuum pump 70 is connected to reaction chamber 20 to produce and/or to keep suitable pressure.N
2Gas tank 50 provides N
2Gas is with treating plant 10.Reaction chamber 20 can also comprise that cooling system is to reduce the heat that anti-x should produce.
[0029] in order to control gas flow, equipment 10 also comprises can be in various flow control mechanisms (for example mass flow controller 80, shut-off valve 82 and vacuum breaker 84) manual or that control automatically.Precursor material source 40 provides precursor material (for example HMDSO of liquid form), and this precursor material is evaporated and fills in the reaction chamber 20.In some cases, can use carrier gas for example argon precursor material is transported to reaction chamber 20.Reactant gas jar 60 provides reactant gas (for example oxygen), and this reactant gas is also charged in the reaction chamber 20.Precursor material and reactant gas flow in the reaction chamber 20 so that produce reaction mixture 42 near electron device 30.Conditioned reaction chamber 20 pressure inside are to obtain deposition pressure in addition.Reaction chamber 20 comprises the one group of electrode 22 that is installed on the electrode support (standoff) 26, and described electrode support can be conductor or isolator.The various configurations of device 30 and electrode 22 all are feasible.Can use diode or triode electrode or electrode (remote electrode) far away.Device 30 can perhaps can be installed on one or two electrode of diode structure by placing at a distance shown in Fig. 1.
[0030] provide RF power in reaction mixture 42, to produce condition of plasma for electrode 22.The reaction product of plasma generation is deposited on the electron device 30.Make reaction be enough to the time period of settled layer on electron device 30.Reaction times will be depended on multiple factor, and for example device 30 is with respect to the position of electrode 22, the type for the treatment of settled layer, reaction conditions, required layer thickness, precursor material and reactant gas.Reaction times can continue 5 seconds to 5 hour, but can also use the longer or shorter time according to purposes.Can be provided with at different reaction conditionss then and repeat previous step down to deposit dissimilar layers.Device 30 may need heating or cooling so that its temperature or keep its temperature to be in desirable value.
[0031] Fig. 2 has shown the viewgraph of cross-section of the part of OLED 100, this OLED comprise the OLED body that is on the substrate 150 140 and use HMDSO as precursor material and use oxygen as reactant gas by the sedimentary multilayer barrier coating 160 of PE-CVD.In following table 1, shown the characteristic and their reaction conditions of deposition of each layer in the laminated coating.Reaction conditions shown in the use is silicon oxide layer deposited 110 on OLED body 140.Use different reaction conditionss to be arranged on layer 110 top depositing silicon polymer layer 120, described reaction conditions setting comprises the oxygen flow speed of higher H MDSO flow velocity and reduction.At last, use reaction conditions layer 120 above the silicon oxide layer deposited 130 identical with layers 110.
Table 1
[0032] Fig. 3 has shown the experimental result of the deterioration of coating OLED in the comparison diagram 2 and naked OLED.Two kinds of OLED all worked in ambient air 17 days in room temperature under the 6.5V galvanic current.Than naked OLED, apply OLED and suffer obviously littler deterioration.These results prove that method of the present invention can provide environmental exposure deterioration influence is had the coating of effective protective.
[0033] Fig. 4 has shown and uses HMDSO under the flow velocity of 33 ℃ source temperature and 1.5sccm and O
2Flow velocity is that 50sccm, deposition pressure are in 150 millitorrs, RF power is that 60W and depositing time are the optical transmission spectrum of the layer of 135 minutes sedimentary 6 μ m.This layer is in the transparence that has near ultraviolet near infrared spectrum greater than 90%.
[0034] Fig. 5 has shown how to measure the contact angle of water droplet on film.Fig. 6 is at various O
2The contact angle of the several layers that/HMDSO gas flow ratio forms down is than pure SiO
2The coordinate diagram of the contact angle of film and straight polymer.When the oxygen flow speed in depositing treatment increased, the contact angle of described layer was near pure SiO
2The contact angle of film.
[0035] Fig. 7 is the coordinate diagram of the contact angle of the several layers that forms down in the various power levels that applied during PE-CVD handles.When power level increased, the contact angle of described layer was near pure SiO
2The contact angle of film, this may be because higher power level makes O
2Become stronger oxygenant.Fig. 8 has shown the high relatively O of use
2Flow and relative low O
2The layer that flow forms is than pure SiO
2The infrared absorption spectra of the film of (thermal oxide) or the film of straight polymer.High O
2Layer demonstrates strong peak at the Si-O-Si band.Think thermal oxide (pure SiO
2) Si-CH of film
3Nominal peak in the band is relevant with the Si-O vibration.Fig. 9 is at various O
2The nano-indentation hardness of the various layers that/HMDSO gas flow ratio forms down is than pure SiO
2The coordinate diagram of the hardness of film.The hardness of this layer increases with the increase of oxygen flow speed in the depositing treatment, and these layers can almost hard as pure SiO
2Film, but tough and tensile and unusual softish.
[0036] Figure 10 is at various O
2The coordinate diagram of the surfaceness (rootmean-square) that the several layers that/HMDSO gas flow ratio forms down records by atomic force microscopy, and show that this surfaceness is with the O that is used for depositing treatment
2Flow velocity increases and reduces.Figure 11 is the coordinate diagram of the surfaceness (rootmean-square) that records by atomic force microscopy of the several layers that forms under various power levels, and shows that this surfaceness increases with the power level that is used for depositing treatment and reduce.
[0037] Figure 12 A and 12B have shown on the thick Kapton polyimide foil of 50 μ m in 33 ℃ source temperature, the HMDSO gas flow rate of 1.5sccm, the O of 50sccm
2The light micrograph on the surface of 4 μ m layers of the RF power deposit of the pressure of flow velocity, 150 millitorrs and 60W.In Figure 12 A, make the coated foils rolling (stretching strain ε=0.2%) that on 1 inch diameter roll, stands to circulate obtain image before and afterwards.Not observing microstructure after 58600 rolling circulations changes.In Figure 12 B, the stretching strain that makes coated foils stand to increase gradually, and occurring first cracking (roller diameter of 14mm) obtains image afterwards and at a large amount of crackings (roller diameters of 2mm) afterwards.These snappinesies result proves that method of the present invention can provide the coating of high degree of flexibility.
Claims (33)
1. form the method for coating from the teeth outwards, comprising:
The single precursor material source is provided;
Precursor material is transported to response location with surperficial adjacency to be coated;
Under the first group reaction condition, use this single precursor material source to deposit the first layer in this surface by chemical vapour deposition, this first layer has 100: 0-75: 25 polymer materials and non-polymer material weight ratio; With
Under the second group reaction condition, use this single precursor material source to deposit the second layer in this surface by chemical vapour deposition, this second layer has 0: 100-25: 75 polymkeric substance and non-polymer material weight ratio.
2. the process of claim 1 wherein that the chemical vapour deposition under the described first and second group reaction conditions is the plasma body enhanced.
3. the method for claim 2, also being included in the first group reaction condition, the second group reaction conditioned disjunction its both provides reactant gas and this reactant gas is transported to response location.
4. the method for claim 3, wherein reactant gas is an oxygen.
5. wherein there is reactant gas in the method for claim 3 under two group reaction conditions, and the flow velocity of this reactant gas greatly at least 10% in the velocity ratio second group reaction condition of this reactant gas in the first group reaction condition wherein.
6. the process of claim 1 wherein that the described first group reaction condition and the second group reaction condition comprise independently of one another is selected from following parameter: gas flow rate, gaseous tension, processing pressure, DC power, RF power, RF frequency, underlayer temperature and depositing time.
7. the process of claim 1 wherein that described precursor material includes organic silicon compound.
8. the method for claim 7, wherein said precursor material comprises single silicoorganic compound.
9. the method for claim 7, wherein said precursor material comprises the mixture of multiple silicoorganic compound.
10. the method for claim 7, wherein said silicoorganic compound are hexamethyldisiloxane or dimethyl siloxane.
11. the method for claim 7, wherein said silicoorganic compound are selected from: methyl-monosilane; Dimethylsilane; Vinyl trimethylsilane; Trimethyl silane; Tetramethylsilane; Ethylsilane; The disilane methylmethane; Two (methyl-monosilane base) methane; 1,2-disilane base ethane; 1, two (methyl-monosilane base) ethane of 2-; 2,2-disilane base propane; 1,3,5-three silylation-2,4,6-trimethylene; Dimethylphenylsilaneand; Diphenylmethylsilane; Dimethyldimethoxysil,ne; 1,3,5, the 7-tetramethyl-ring tetrasiloxane; 1,3-dimethyl sily oxide; 1,1,3, the 3-tetramethyl disiloxane; 1, two (silylation methylene radical) sily oxide of 3-; Two (1-methyl disiloxanyl-) methane; 2, two (the 1-methyl disiloxanyl-) propane of 2-; 2,4,6, the 8-tetramethyl-ring tetrasiloxane; Octamethylcyclotetrasiloxane; 2,4,6,8,10-pentamethyl-D5; 1,3,5,7-tetrasilane base-2,6-dioxy-4,8-dimethylene; Hexamethyl cyclotrisiloxane; 1,3,5,7,9-pentamethyl-D5; The hexa methoxy sily oxide; Hexamethyldisilazane; The divinyl tetramethyl-disilazane; Pregnancy basic ring three silazane; Two (the N-methyl kharophen) silane of dimethyl; Dimethyl is two-(N-ethyl kharophen) silane; Two (the N-methyl kharophen) silane of methyl ethylene; Two (the N-butyl kharophen) silane of methyl ethylene; Methyl three (N-phenyl kharophen) silane; Vinyl three (N-ethyl kharophen) silane; Four (N-methyl kharophen) silane; Two (diethyl aminooxy) silane of phenylbenzene; Methyl three (diethyl aminooxy) silane; With two (trimethyl silicon based) carbodiimide.
12. the process of claim 1 wherein that described non-polymer material is made of inorganic materials substantially.
13. the method for claim 12, wherein said inorganic materials is a silicon oxide.
14. the process of claim 1 wherein that described polymer materials is made of silicone polymer substantially.
15. the method for claim 1 also is included under the 3rd group reaction condition, uses this single precursor material source to deposit the 3rd layer by chemical vapour deposition above the first layer and the second layer.
16. the process of claim 1 wherein and before the deposition the first layer, deposit the second layer.
17. the method for claim 1, also comprise and repeat following steps in an alternating manner at least one time: deposition has 100: 0-75: the layer of 25 polymer materials and non-polymer material weight ratio and have 0: 100-25: the layer of 75 polymer materials and non-polymer material weight ratio, wherein selection is used to deposit the reaction conditions of each layer independently.
18. the process of claim 1 wherein at the material of the transition period deposition of deposition between each layer less than 10nm.
19. the process of claim 1 wherein that described surface is the surface that is used for the substrate of electron device.
20. the method for claim 19, wherein said electron device is an organic luminescent device.
21. the method for claim 19, wherein said electron device is a solar cell.
22. the process of claim 1 wherein that described surface is the surface of electron device.
23. the method for claim 22, wherein said electron device is an organic luminescent device.
24. the method for claim 22, wherein said electron device is a solar cell.
25. the process of claim 1 wherein that the first layer of firm sedimentation state has 60 °-115 ° water droplet moisten contact angle.
26. the process of claim 1 wherein that the first layer of firm sedimentation state has 75 °-115 ° water droplet moisten contact angle.
27. the process of claim 1 wherein that the second layer of firm sedimentation state has 0 °-60 ° water droplet moisten contact angle.
28. the process of claim 1 wherein that the first layer of firm sedimentation state and the just moisten contact angle of the second layer of sedimentation state differ at least 15 °.
29. the process of claim 1 wherein that described the first layer has the nano-indentation hardness of 0.2-2GPa.
30. the process of claim 1 wherein that the described second layer has the nano-indentation hardness of 10-20GPa.
31. the process of claim 1 wherein that at least one has the surfaceness (rootmean-square) of 0.1-10nm in the described layer.
32. the method for claim 1, have enough snappinesies during the 4 μ m layers of at least one in the wherein said layer on being deposited as 50 μ m thick polyimide paper tinsels, make not change after at least 55000 rollings circulations under 0.2% stretching strain (ε), observing microstructure on the 1 inch diameter roll.
33. have enough snappinesies when the process of claim 1 wherein 4 μ m layers on being deposited as 50 μ m thick polyimide paper tinsels of in the described layer at least one, make under at least 0.35% stretching strain (ε), crackle not occur.
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| CN104846350A (en) * | 2014-02-18 | 2015-08-19 | 中国科学院苏州纳米技术与纳米仿生研究所 | Organic-inorganic hybrid high barrier film and preparation method thereof |
| CN104733641B (en) | 2015-04-03 | 2017-01-18 | 京东方科技集团股份有限公司 | OLED packaging method and structure and display device |
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