EP2235231A1 - Method for producing a workpiece surface and workpiece with predefinable hydrophilic wetting characteristics for said surface - Google Patents
Method for producing a workpiece surface and workpiece with predefinable hydrophilic wetting characteristics for said surfaceInfo
- Publication number
- EP2235231A1 EP2235231A1 EP08714780A EP08714780A EP2235231A1 EP 2235231 A1 EP2235231 A1 EP 2235231A1 EP 08714780 A EP08714780 A EP 08714780A EP 08714780 A EP08714780 A EP 08714780A EP 2235231 A1 EP2235231 A1 EP 2235231A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- substrate
- range
- areas
- layer
- plasma
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
- 238000009736 wetting Methods 0.000 title claims description 15
- 238000004519 manufacturing process Methods 0.000 title claims description 10
- 239000000758 substrate Substances 0.000 claims abstract description 115
- 239000010410 layer Substances 0.000 claims abstract description 95
- 239000011241 protective layer Substances 0.000 claims abstract description 50
- 239000002086 nanomaterial Substances 0.000 claims abstract description 41
- 150000002430 hydrocarbons Chemical class 0.000 claims abstract description 37
- 229930195733 hydrocarbon Natural products 0.000 claims abstract description 35
- 239000000463 material Substances 0.000 claims abstract description 26
- 238000009832 plasma treatment Methods 0.000 claims abstract description 17
- 238000004049 embossing Methods 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims description 62
- 239000007789 gas Substances 0.000 claims description 54
- 239000004215 Carbon black (E152) Substances 0.000 claims description 34
- 230000008569 process Effects 0.000 claims description 33
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 31
- 239000001301 oxygen Substances 0.000 claims description 31
- 229910052760 oxygen Inorganic materials 0.000 claims description 31
- 239000004033 plastic Substances 0.000 claims description 29
- 229920003023 plastic Polymers 0.000 claims description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 25
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 16
- -1 polypropylene Polymers 0.000 claims description 12
- 239000004743 Polypropylene Substances 0.000 claims description 11
- 229920001155 polypropylene Polymers 0.000 claims description 10
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 8
- 238000000151 deposition Methods 0.000 claims description 8
- 230000008021 deposition Effects 0.000 claims description 8
- 239000001257 hydrogen Substances 0.000 claims description 8
- 229910052739 hydrogen Inorganic materials 0.000 claims description 8
- 229910052751 metal Inorganic materials 0.000 claims description 8
- 239000002184 metal Substances 0.000 claims description 8
- 238000011282 treatment Methods 0.000 claims description 8
- 238000000992 sputter etching Methods 0.000 claims description 7
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 6
- 238000003486 chemical etching Methods 0.000 claims description 6
- 229910052756 noble gas Inorganic materials 0.000 claims description 6
- 229920001169 thermoplastic Polymers 0.000 claims description 4
- 239000004416 thermosoftening plastic Substances 0.000 claims description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 3
- 239000012528 membrane Substances 0.000 claims description 3
- 230000035699 permeability Effects 0.000 claims description 3
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical group O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 2
- 239000004744 fabric Substances 0.000 claims description 2
- 229920000642 polymer Polymers 0.000 claims description 2
- 239000004753 textile Substances 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims 1
- 230000005660 hydrophilic surface Effects 0.000 abstract description 8
- 238000000576 coating method Methods 0.000 description 15
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 12
- 239000011248 coating agent Substances 0.000 description 10
- 239000007788 liquid Substances 0.000 description 9
- 230000000694 effects Effects 0.000 description 8
- 239000000654 additive Substances 0.000 description 6
- 229910052786 argon Inorganic materials 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 6
- 238000004140 cleaning Methods 0.000 description 6
- 238000004806 packaging method and process Methods 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 230000002209 hydrophobic effect Effects 0.000 description 4
- 230000001681 protective effect Effects 0.000 description 4
- 238000012546 transfer Methods 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 229920000139 polyethylene terephthalate Polymers 0.000 description 3
- 239000005020 polyethylene terephthalate Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000012159 carrier gas Substances 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 229910003460 diamond Inorganic materials 0.000 description 2
- 239000010432 diamond Substances 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 238000013508 migration Methods 0.000 description 2
- 230000005012 migration Effects 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 229920000098 polyolefin Polymers 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 238000007639 printing Methods 0.000 description 2
- 239000005871 repellent Substances 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000004544 sputter deposition Methods 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- ZUMHJAYVECWKLA-UHFFFAOYSA-N 3-dimethoxysilylpropan-1-ol Chemical compound CO[SiH](CCCO)OC ZUMHJAYVECWKLA-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000003666 anti-fingerprint Effects 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 239000007767 bonding agent Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 239000005025 cast polypropylene Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000004814 ceramic processing Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- NZZFYRREKKOMAT-UHFFFAOYSA-N diiodomethane Chemical compound ICI NZZFYRREKKOMAT-UHFFFAOYSA-N 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000005357 flat glass Substances 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 229920001600 hydrophobic polymer Polymers 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000007373 indentation Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000000976 ink Substances 0.000 description 1
- 239000002346 layers by function Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 description 1
- GQPLMRYTRLFLPF-UHFFFAOYSA-N nitrous oxide Inorganic materials [O-][N+]#N GQPLMRYTRLFLPF-UHFFFAOYSA-N 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 description 1
- 239000002985 plastic film Substances 0.000 description 1
- 229920006255 plastic film Polymers 0.000 description 1
- 229920001690 polydopamine Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000012552 review Methods 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/02—Pretreatment of the material to be coated
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C59/00—Surface shaping of articles, e.g. embossing; Apparatus therefor
- B29C59/02—Surface shaping of articles, e.g. embossing; Apparatus therefor by mechanical means, e.g. pressing
- B29C59/022—Surface shaping of articles, e.g. embossing; Apparatus therefor by mechanical means, e.g. pressing characterised by the disposition or the configuration, e.g. dimensions, of the embossments or the shaping tools therefor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C59/00—Surface shaping of articles, e.g. embossing; Apparatus therefor
- B29C59/14—Surface shaping of articles, e.g. embossing; Apparatus therefor by plasma treatment
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/02—Pretreatment of the material to be coated
- C23C16/0227—Pretreatment of the material to be coated by cleaning or etching
- C23C16/0245—Pretreatment of the material to be coated by cleaning or etching by etching with a plasma
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/02—Pretreatment of the material to be coated
- C23C16/0254—Physical treatment to alter the texture of the surface, e.g. scratching or polishing
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/26—Deposition of carbon only
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C59/00—Surface shaping of articles, e.g. embossing; Apparatus therefor
- B29C59/02—Surface shaping of articles, e.g. embossing; Apparatus therefor by mechanical means, e.g. pressing
- B29C59/022—Surface shaping of articles, e.g. embossing; Apparatus therefor by mechanical means, e.g. pressing characterised by the disposition or the configuration, e.g. dimensions, of the embossments or the shaping tools therefor
- B29C2059/023—Microembossing
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
- B29K2995/00—Properties of moulding materials, reinforcements, fillers, preformed parts or moulds
- B29K2995/0037—Other properties
- B29K2995/0092—Other properties hydrophilic
Definitions
- the invention relates to a method for producing a workpiece surface with predetermined wetting properties of the surface for hydrophilic behavior in which the water contact angle (WCA) in the range of 3 ° to 90 ° is set according to the preamble of claims 1 to 3, and to a Workpiece according to the preamble of claims 18 and 19.
- WCA water contact angle
- wetting is understood to mean the degree of adhesive contact of liquids on surfaces, in particular on solids. It refers to the ability of liquids to spread on a surface.
- An important case here is the hydrophilic behavior of a surface, ie the water-friendly behavior, whereby water is well accepted on the surface.
- the opposite is the hydrophobic behavior, ie the water-repellent behavior, in which the water is repelled at the surface and thereby form, for example, drops.
- This wetting behavior is measured and defined by the so-called water contact angle (WCA). The better the wettability, the smaller the contact angle that occurs during wetting.
- hydrophilic, well-wetting surfaces also leads to a better heat transfer behavior which is desirable in many technical applications where good thermal contact is to be created.
- hydrophilic surfaces can also be cleaned better.
- a workpiece having a hydrophilic surface with a selectable degree of hydrophilic behavior is to be provided by microstructuring the surface of a substrate material at least in partial areas by mechanical embossing and subsequently coating and producing a nanostructure with at least two-stage plasma treatment Microstructure is superimposed.
- the plasma treatment is preferably carried out in a sealed system in which the introduced process gases are pumped with a vacuum pump.
- the respective working pressure range is adjustable over a wide range and can reach atmospheric pressure. This targeted superimposition of different structures enables the targeted creation of surfaces with the desired degree of wettability.
- the nanostructure is produced from a plastic material or a hydrocarbon-containing material by an at least two-stage plasma treatment in a plasma process, preferably under vacuum conditions.
- the plasma treatment causes structuring on the surface of the hydrocarbonaceous material, which generates structure dimensions in the nanometer range.
- the surface of a substrate can be directly treated, which at least on the surface consists of a plastic, preferably of a thermoplastic.
- a layer containing a hydrocarbon skeleton may be deposited on the substrate to subsequently nanostructure that layer with the plasma treatment.
- the substrate need not contain a plastic material, it may also consist of another material that can be embossed to produce the microstructure, such as a metal, preferably a ductile metal, such as copper or aluminum.
- a lattice-like microstructure with depressions is mechanically impressed into this plastic surface of the substrate, at least in planar partial regions, which is formed from a multiplicity of structure elements which hang one another and whose individual dimensions are in the range from 15 ⁇ m to 45 ⁇ m, and between the adjacent structural elements are trenched. formed shaped recesses which enclose the structural elements, wherein at least one open connection to the adjacent recess is made;
- the substrate is treated in a vacuum chamber at least in partial areas in at least two steps with a plasma discharge to produce a nanostructure in the plastic on the substrate surface, wherein in a first step the plasma at least oxygen or hydrogen is supplied to the chemical etching of the substrate surface and in the subsequent second step the plasma is added at least one noble gas for ion etching of the substrate surface;
- a hydrocarbon-containing protective layer in a chamber is deposited from a plasma discharge at least in portions on the substrate to which a hydrocarbon-containing gas is supplied, producing a layer thickness which is in the range of 1.0 to 500 nm;
- At least one cover layer in a chamber-preferably a vacuum chamber- is deposited from a plasma discharge at least in partial regions onto the substrate, to which a hydrocarbon-containing gas and additionally an oxygen-containing gas and / or a nitrogen-containing gas is supplied, producing a layer thickness which is in the range of 1.0 to 30nm.
- the nanostructure is generated from a hydrocarbon-containing layer which is deposited over the microstructured substrate surface.
- This hydrocarbon-containing layer simultaneously acts as a protective layer.
- the following steps are carried out for generating a desired hydrophilic workpiece surface in which a water contact angle (WCA) in the range of 3 ° to 90 ° is set:
- a lattice-like microstructure with indentations which is formed from a multiplicity of structure elements which hang one another and whose individual dimensions i, i 'lie in the range from 15 ⁇ m to 45 ⁇ m, is impressed mechanically on a surface, at least in planar partial areas, and that trench-shaped depressions are formed between the adjacent structural elements, which surround the structural elements and at least one open connection to the adjacent one
- a protective layer is deposited on the substrate in a vacuum chamber from a plasma discharge at least in partial areas, to which a hydrocarbon-containing gas is supplied, and a layer thickness is generated which lies in the range from 1.0 to 500 nm;
- the substrate is treated in at least partial areas with plasma discharge in at least two steps, wherein at least oxygen or hydrogen is supplied to the plasma for chemical etching of the surface of the protective layer and in the subsequent second step the plasma at least one noble gas is added to the ion etching of the substrate surface;
- At least in some areas at least one cover layer in a chamber - preferably in a vacuum chamber - deposited from a plasma discharge to the substrate, which is supplied to a hydrocarbon-containing gas and additionally an oxygen-containing gas and / or a nitrogen-containing gas, and that Layer thickness is generated, which is in the range of 1.0 to 30 nm.
- the microstructuring of the substrate with the superimposed nanostructure together with the cover layer makes it possible to achieve a workpiece surface which is hydrophilic, it being possible in this combination to easily set a water contact angle (WCA) which is less than 60 °, preferably even smaller in the range of 3 ° to 30 ° or preferably in the range of even 3 ° to 15 °.
- WCA water contact angle
- the adjustment is made by the choice of the microstructure and its dimensions, as well as by adjusting the dimensions of the nanostructure and by adjusting the hydrophilicity of the cover layer.
- the microstructure is advantageously embossed mechanically into the substrate material on the surface. Etching processes, such as chemical are also possible but less economical.
- the mechanical embossing can be done in a known manner, for example with stamp presses or rollers. For plastic substrates hot stamping is suitable.
- the structuring takes place with advantage with periodically repeating identical structural elements and is advantageously formed like a grid and should be at least in partial areas of a substrate surface.
- Particularly suitable as plastic are thermoplastics and preferably polypropylene.
- the nanostructure is generated in an at least two-stage vacuum plasma process.
- the structure is set by selecting the process parameters, such as the discharge conditions of the gas discharge, the reactor configuration and the gas flow with the operating pressures.
- process parameters such as the discharge conditions of the gas discharge, the reactor configuration and the gas flow with the operating pressures.
- cover layer already has a share of hydrophilic behavior, with a WCA of less than 60 °. Only by the combination of all measures it is surprisingly possible to reproducibly achieve such a low WCA value and thus to realize outstanding hydrophilic behavior or high wettability of the workpiece surface.
- the protective layer serves to protect against environmental influences and enables a stable behavior of the surface, so that degradation over several months to years can essentially be avoided or at least kept extremely low.
- the protective layer may be omitted, and after the nanostructuring, a capping layer similar to that in the two cases described above is deposited. This is preferably deposited in a vacuum chamber from a plasma discharge on the substrate over the nanostructure as the outermost layer, wherein the plasma discharge is a hydrocarbon-containing working gas and additionally an oxygen-containing working gas and / or a nitrogen-containing working gas is supplied, and that a layer thickness is generated, which is in the range of 1.0 to 100 nm.
- the hydrophilic cover layer simultaneously has a protective effect, similar to the protective layer. However, it is more difficult to achieve the same good properties (hydrophilicity, protective effect, etc.) in this single-stage coating process as in the first variant.
- the layer properties in this variant depend more strongly on the choice of material of the substrate.
- This embodiment comprises only three basic process steps. Although the setup is simpler, the litigation is a little less secure than the first two cases presented. Since no separate protective layer is present, the top layer must take over part of the protective layer function. This can be increased by increasing the hydrocarbon content compared to the first two embodiments. In addition, the layer thickness should be increased. This design is only suitable for workpiece applications because of the lower protective effect, where the requirements are lower or the choice of workpiece material permits this.
- the substrate surface, the nanostructure and the cover layer it is possible to carry out further process steps or coatings between the substrate surface, the nanostructure and the cover layer, as long as the microstructure and the nanostructure are effectively imaged on the workpiece surface.
- mixed forms of the first and second or the first and third inventive embodiments are possible if the coatings are sufficiently thin and the plasma can also act on the substrate.
- the nanostructure becomes through the substrate and the protective layer or protective Cover layer formed.
- further functional layers over the cover layer as long as the microstructure and the nanostructure are effectively imaged on the workpiece surface, such as further protective layers or photocatalytically active layers.
- Fig. 1 is a schematic representation of a production device for producing a workpiece with a hydrophilic surface
- FIG. 2 shows in cross-section a substrate which is at least on the surface of a plastic with a microstructured surface for the first case of an embodiment according to the invention
- FIG. 3 shows in cross-section the substrate according to FIG. 2 with a superposed nanostructured surface
- FIG. 4 shows in cross-section the substrate according to FIG. 3 with a protective layer on the nanostructured surface
- FIG. 5 shows in cross section the substrate according to FIG. 4 with the covering layer deposited on the protective layer, forming the workpiece with a hydrophilic surface
- FIG. 6 shows an example of an inventive and preferred layer structure with nanostructuring on a plastic substrate surface for the first case
- 7 shows in cross section a substrate with a microstructured surface and with a hydrocarbon-containing protective layer deposited thereon for the second case of an embodiment according to the invention
- FIG. 8 shows in cross section the substrate according to FIG. 7 with a processed nanostructured protective layer
- FIG. 10 is a plan view of a microstructured substrate surface with differently sized and differently shaped structural elements
- FIG. 11 shows in plan view an example of a microstructured substrate surface with square equal and staggered structural elements
- FIG. 12 shows in plan view another example of a microstructured substrate surface with square, equal, non-offset structural elements
- FIG. 13 shows in plan view a further example of a microstructured substrate surface with triangular, equally large structural elements
- FIG. 14 shows in plan view an example of a nanostructured substrate surface or a hydrocarbon-containing layer.
- the substrate 1 is first provided with a microstructure on its surface by preferably mechanical embossing and then in A vacuum system 20 plasma treated and / or coated, as shown schematically in Figure 1.
- the embossing is carried out by known methods by embossing or pressing into the substrate surface 4 of the substrate 1 lying on a substrate carrier 27 with an embossing tool 27, such as an embossing punch or an embossing roll.
- an embossing tool 27 such as an embossing punch or an embossing roll.
- band-shaped substrates for example plastic films, can also be processed in a continuous process. Thereafter, the further processing steps are carried out in a vacuum system 20.
- the substrate 1 is transported into the vacuum system 20 through a lock 23 and stored there on a support or directly on an electrode 22 '.
- the vacuum system is evacuated via a pumping system 24.
- the working gas and possibly a carrier gas such as preferably inert gases, such as argon or helium, are introduced via gas inlet systems 25, 26 into the vacuum chamber with the desired gas flow and working pressure in the chamber.
- a second electrode 22 is disposed opposite the first electrode 22 'and both electrodes are connected to a power supply 21 for generating the plasma.
- the plasma discharge can be fed in individual process steps with a direct current (DC) - power supply 21 as long as materials are involved, which have at least a certain electrical conductivity.
- DC direct current
- DC pulsed feeds or AC feeds 21 are advantageously used.
- the height of the DC pulse frequency or the AC frequency is selected. Frequencies from 5OkHz to 50OkHz can be used for DC pulses with both unipolar and bipolar pulses. Bipolar pulses may be asymmetric with only a small negative or positive contribution, with the turn-on time greater than the turn-off time.
- the AC supply can use frequencies from 10 kHz to 1.0 MHz. Frequently used frequencies for the AC supply are in the RF range, which includes a range from 1.0 MHz to about 1.0 GHz. In certain cases, the use of microwaves is possible, with frequencies the above 1.OGHz. It may be advantageous to use magnetic-field-assisted plasma reactors.
- sputtering sources preferably magne- tron sources
- PECVD plasma deposition
- metal oxide-containing layers such as TiO 2
- a reactive process is preferably used in which the material to be sputtered consists of titanium and oxygen as working gas 26 and a carrier gas 25, for example argon, are introduced into the process chamber 20.
- the sputtering sources are operated with DC or AC power supplies, according to the above-mentioned information.
- the individual steps of the vacuum processes can also be carried out in different systems, but they are advantageously all carried out in the same system or in multi-chamber systems, if different lhe process conditions are necessary or even a full automation is provided.
- FIG. 2 shows diagrammatically and in cross section and in FIG. 10 a top view of how a microstructure is mechanically embossed into the surface of the substrate 1 in order to obtain a surface 4 which is microstructured at least in TeN regions.
- the substrate 1 may consist of different materials.
- the substrate 1 includes, for example, at the bottom of another material 1b, such as a metal, as the upper portion 1a, which adjoins the substrate surface.
- the upper part consists of a plastic 1a, preferably a thermoplastic, and is the material part in which the microstructure 2, 3 is embossed.
- a plastic polypropylene is particularly suitable.
- the microstructure consists of a lattice-like structure with mechanically impressed depressions 2, which consist of a plurality of the hanging structural elements 3 is formed, the individual expansions I, P are in the range of 15 .mu.m to 45 .mu.m. Between the adjacent structural elements 3, the recesses 2 are trench-shaped, so that they enclose the structural elements 3 and at least one open connection to the adjacent recess 2 is produced.
- These enclosing depressions 2 can also have interruptions in the circumference and form a kind of bridge 12 from one structural element 3 to the next, as long as there is at least one connection of a recess 2 of a structural element 3 with the depression 2 of the adjacent structural element 2, as in the plan view in FIG FIG. 10 is shown.
- the depth t, the trench-shaped depressions 2 is in the range of 0.5 .mu.m to 10 .mu.m, preferably 1 .mu.m to 5 .mu.m.
- the recesses may be different in a workpiece.
- the cross-sectional shape of the recess 2 is not particularly important and can be selected on the basis of practical, manufacturing-technical aspects.
- the width b of the trench-shaped depression 2 on the substrate surface 4 is in the range of 0.5 ⁇ m to 6 ⁇ m, preferably 2 ⁇ m to 4 ⁇ m.
- the dimensions I, P of the structural elements 3, that is to say the longest extent I and the smallest extent P of the surface of the structural element 3 are within the range of 15 ⁇ m to 45 ⁇ m.
- the structural elements may have different shapes and sizes, as shown in Figures 2 and 10. Periodically, repeating patterns are advantageous for the practical realization, as shown for example in the schematic figures 11 to 13 in the plan view.
- FIG. 11 shows a microstructure with periodically arranged rectangular or square structural elements 3 with an arrangement offset from one another in a line.
- FIG. 12 shows an example with square structural elements 3 in a non-staggered arrangement, and
- FIG. 13 shows a microstructure with periodically arranged triangles, here equilateral triangles, as structural elements 3.
- the figures also show that the width b of the depressions 2 is always smaller as the extension I, I 'of the adjacent structural elements 3.
- a nanostructure 5 is produced which is directly superimposed on the microstructure at least in partial areas and is produced from the surface 4 made of plastic, here from the substrate surface made of plastic, with an at least two-stage plasma treatment as shown in Figure 3 in cross section.
- FIG. 14 shows by way of example a nanostructured surface 5, 5 'with randomly distributed worm-like structures as resulting from this method.
- the nano-structure 5 is designed in such a way that the height h of its elevations is set in the range from 20 nm to 120 nm and the distances or the extent w of the elevations lie in the range from 40 nm to 200 nm.
- the substrate 1 is treated in a vacuum chamber 20 in two steps with a plasma discharge, wherein in a first step the plasma at least oxygen or hydrogen is supplied to the chemical etching of the substrate surface 4 and at the subsequent second step the plasma at least one Noble gas, preferably argon, is added to the ion etching of the substrate surface 4.
- a plasma process is preferably used in which oxygen, hydrogen or another corrosive working gas is supplied. Other methods of purification, such as ion etching, are also possible.
- a hydrocarbon-containing protective layer 6 is deposited in a vacuum chamber 20 from a plasma discharge onto the substrate 1, at least in some areas, as shown in FIG.
- a hydrocarbon-containing gas is supplied to the plasma, wherein a layer thickness 6 is generated, which is in the range of 1.0 to 500 nm, preferably in the range of 2.0 to 50 nm lies.
- Such a protective layer 6 is advantageously formed as a dense, three-dimensionally highly crosslinked, plasma-polymerized hydrocarbon layer which is flexible and soft or as a hard DLC layer (Diamond Like Carbon) which protects against mechanical damage (scratch protection, etc.).
- the protective layer 6 should advantageously lower the permeability of oxygen by at least a factor of 10 compared to the uncoated substrate 1. The migration of additives to the plastic surface and their penetration into directly contacting environment is also prevented by this diffusion barrier. Or it is additionally advantageous if the oxygen permeability is less than 15 ml / m 2 xTagxbar, if a 12 micron thick, microstructured embossed polyethylene terephthalate film is used as the substrate 1 and over this protective layer 6 is deposited.
- At least one covering layer 7 is deposited, which itself already has hydrophilic properties on its own, but alone achieves only a WCA of 20 to 60 °, as shown in FIG.
- the at least one cover layer 7 is deposited in a chamber 20 - preferably a vacuum chamber - from a plasma discharge onto the substrate 1 via the protective layer 6 by supplying a hydrocarbon-containing gas and additionally an oxygen-containing gas and / or a nitrogen-containing gas, wherein a layer thickness is generated which is in the range of 1.0 to 30 nm.
- the cover layer 7 is preferably also formed as an oxygen- and / or nitrogen-containing plasma-polymerized hydrocarbon coating or oxygen- and / or nitrogen-containing DLC coating.
- FIG. 6 shows an enlarged and cross-section of a finished and coated workpiece 10 with a microstructured substrate surface 2, 3 made of a plastic with superimposed nanostructure 5 machined thereon, with overlying protective layer 6 and a final covering layer 7 Workpiece surface 9.
- a WCA is advantageously set which is in the range of 3 ° to 30 °, or preferably in the range of 3 ° to 15 °.
- an additional important function is, for example, the addition of the hydrophilic workpiece 10 with a photoactive layer which, for example, allows self-cleaning effects on the workpiece surface.
- a TiO 2 layer preferably having a thickness in the range from 5 nm to 500 nm, is deposited.
- Another suitable coating is carried out by deposition of a SiO 2 layer with a thickness in the range of 5 nm to 500 nm. This transparent layer allows additional protection, in particular from mechanical damage, and has inherent hydrophilic properties.
- the layer thickness it is important, for example by choosing the layer thickness, to ensure that the microstructure 2, 3 and in particular also the nanostructure 5 on the workpiece surface 9 is at least still imaged in order to be able to fulfill the function.
- a thicker layer should be chosen, which ranges from 1.0nm to 100nm.
- FIG. 7 shows in cross-section an example in which the carbon-containing protective layer 6 with its surface 8 is deposited directly onto the substrate 1 with the microstructure 2, 3.
- the hydrocarbon-containing protective layer 6 can likewise be advantageously formed here as a DLC layer.
- the protective layer 6 assumes the task of the embossed plastic substrate 1 in comparison with the first exemplary embodiment of the invention presented above.
- the substrate material can be chosen freely, as long as it can be embossed for the introduction of a microstructure 2, 3. It is thus for the substrate 1, for example, ductile metals and alloys such as aluminum, magnesium, copper, gold, silver, steel, etc. usable, although plastics are preferred.
- the nanostructuring on this protective layer surface 8 takes place in turn with the at least two-stage plasma treatment (b) already described above, as shown in cross section in FIG.
- the nanostructure 5 ' has thus been worked out at least partially from the protective layer 6' with the at least two-stage plasma treatment, wherein only the nanostructure of the surface 4 of the substrate 1 embossed with the microstructure 2, 3 can be changed.
- mixed forms are possible.
- At least one cover layer 7 is now deposited over this nanostructured protective layer 6 as described above.
- further treatment steps and / or coating steps can take place between the individual method steps or over the cover layer 7, if this is necessary and desired.
- all the steps of the first described case can also be used for this second case.
- the area of use of workpieces 10 with hydrophilic surfaces 9 is extremely wide.
- the non-fogging effect of the workpieces is particularly advantageous for ensuring transparency for transparent or indicating uses such as packaging and optical components, mirrors, windows, screens, PDAs, cell phones, navigation systems, photovoltaics, etc.
- a more intensive solar irradiation in greenhouses is made possible.
- the top layer of photocatalytically active TiO 2 plays an important role, because the workpiece surface in addition to the anti-fogging effect in addition to an active self-cleaning effect (anti-fingerprint, anti-bacterial, etc.) is equipped.
- Another possible application is the transfer or transport of liquids or condensed water in the membrane and packaging industry.
- the condensed water can also be directed to intended locations.
- the content of a package is transferred by the variation of the hydrophilicity of the workpiece surface in the intended sub-areas without loss (residual emptying).
- the development of plastic surface - especially of polypropylene - allows the preservation of the sealing of the workpiece. If necessary, the preservation of the sealing properties can be increased by omitting treatment steps in these subareas.
- Step 2 A vacuum chamber is evacuated to reach a base pressure of less than about 10 "2 mbar than the following working pressure, after which the working gases are introduced into the vacuum chamber via mass flow controllers and the working pressure is checked with a pressure gauge.
- a worm-like nanostructure of the microstructure is deposited on the microstructured substrate at least in some areas at room temperature.
- the low molecular weight polymer chains, additives (ingredients, additives, etc.) and impurities are removed.
- the second process step the worm-like nanostructure is worked out by ion etching.
- 1st process stage RF plasma, room temperature, grounded substrate
- Power range 200 to 700 watts, typically at 400 watts
- Operating Pressure about 1.0 x 10 -2 mbar
- Working gas 10 to 60 sccm of oxygen
- Power range 100 to 600 watts, typically at 300 watts
- Working pressure approx. 5 x 10 '4 mbar
- Working gas 10 to 50 sccm argon
- Step 3 The workpiece surface, which has been enlarged by the structuring, is provided with a three-dimensionally highly cross-linked, plasma polymerized hydrocarbon layer or DLC layer.
- the structures are thereby fixed and protected from direct contact with the environment.
- Example of process conditions RF plasma, room temperature, substrate grounded, with or without bias voltage
- Power range 50 to 400 watts, typically at 100 watts
- Working pressure 9 x 10 '3 mbar
- Gas mixture 30 sccm C 2 H 2 , 15 sccm He • 4th step: deposition of a wafer-thin, hydrophilic, plasma polymerized hydrocarbon layer, which the workpiece gives a hydrophilic surface.
- Example of process conditions RF plasma, room temperature, substrate grounded, with or without bias voltage: Power range: 400 to 800 watts, typically at 500 watts Working pressure: 6 x 10 2 mbar
- Step 5 deposition of a photocatalytically active TiO 2 film (anatase containing) subsequent to step 4 or step 4 in place at a substrate temperature of ⁇ 100 0 C.
- Example of process conditions pulsed, reactive DC magnetron sputtering process with process grounded substrate and variable magnetic field strength: power: 2000 watts
- Working pressure range 1 x 10 "2 mbar to a few mbar, typically 5 x 10 -2 mbar gas mixture: 35 sccm of argon and 13 sccm of oxygen
- a working pressure range of 5 ⁇ 10 4 mbar to a few mbar is preferred; if necessary, the working pressure can reach one atmosphere.
- the plasma processes are carried out at room temperature, the workpiece is grounded or provided with an optionally pulsed bias voltage. The layer thickness is varied over the treatment time.
- Table 1 summarizes process parameters for selected plasma processes for fabricating the nanostructure on the workpiece surface to increase wettability.
- PP polypropylene PET: polyethylene terephthalate
- protective layer 6 as hard diamond-like DLC carbon layer (Diamond Like Carbon) or soft three-dimensionally cross-linked plasma polymerized hydrocarbon layer.
- Table 2 the importance of the combination of the microstructure, the nanostructure and the hydrophilic cover layer 7 is clarified, because the desired water contact angle of WCA ⁇ 20 ° is already achieved with a significantly lower surface energy by the MikroVNano Modell than when the same hydrophilic cover layer 7 on a non-structured workpiece is deposited.
- the wetting properties were determined using a contact angle meter using the test liquids distilled water, diiodomethane, ethylene glycol, according to standards ASTM D5725-95 and ASTM D724 at 23 ° C and at 50% relative humidity.
- the surface energy [mN / m] is a measure of the total energy content of a smooth solid surface and is determined by measuring contact angles for different liquids.
- a nano / micro structure in combination with a plasma coating enables a stable, highly wetting workpiece surface with a WCA ⁇ 20 °.
- This workpiece surface is characterized by a surface energy of 55 to 70mN / m, which is stable over a longer period of time. If now the nanostructure and the subsequent plasma coatings are only superimposed on a partial area of the microstructured polypropylene surface, a workpiece surface can be created which is partially hydrophilic (WCA ⁇ 60 °) and partially hydrophobic (WCA> 90 °).
- WCA> 110 ° is on the microstructured, but not plasma-treated workpiece surface, on the micro / nanostructured and plasma-treated workpiece surface the WCA is ⁇ 40 °.
- the anti-fogging effect is not only found in water-based fluids, but also in oily fluids. Accordingly, the surface of a packaging can also be modified with suitable structuring and coating in such a way that the oily liquid propagates like a film. The surface energy of the substrate surface is then adjusted according to the surface tension of the wetting liquid. This optimizes the transfer of the filling material (residual emptying). Likewise, the interface of two contacting materials in large rem w to be wetted by the described method. This is particularly important in the metal and ceramic processing industry.
- the nanostructure advantageously has structural heights in the range of 20 to 200 nm.
- the nanostructure can also be embossed in a process step following the microstructure. The generation of the nanostructure 5 with a plasma discharge is replaced in this case by an embossing process. As a result, the generation of the nanostructure by the plasma treatment is unnecessary, although the plasma treatment is preferred, in particular for polyolefins and in particular for the substrate polypropylene.
- the substrate surface or the DLC-coated material surface wettable by activation in a plasma discharge with addition of at least one oxygen-containing and / or nitrogen-containing gas and thereby the long-term stable hydrophilic thin layer 7 to replace.
- the hydrocarbon-containing protective layer 6 can be activated in a vacuum chamber 20 from a plasma discharge, to which an at least oxygen-containing gas and / or a nitrogen-containing gas is supplied, thereby replacing the cover layer 7.
- the substrate surface is simultaneously structured, cleaned and oxidized and / or provided with nitrogen-containing compounds.
- the microstructured and nanostructured substrate 1 is activated in a vacuum chamber 20 from a plasma discharge, to which at least one oxygen-containing gas and / or a nitrogen-containing gas is supplied and thereby the protective layer 6 and the cover layer 7 is replaced.
- the substrate surface becomes readily wettable to water and subsequent surface treatments such as coating or printing with inks stick excellent.
- the deposition of the protective layer 6 and the hydrophilic cover layer 7 is unnecessary. This behavior is of great importance in the case of the inherently hydrophobic polymers, such as the polyolefins, especially in the case of polypropylene.
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Abstract
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CN104626529A (en) * | 2014-12-30 | 2015-05-20 | 西安建筑科技大学 | Preparation method of super-hydrophilic self-cleaning membrane structure |
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CN102143810A (en) * | 2008-08-07 | 2011-08-03 | 尤尼-皮克塞尔显示器有限公司 | Microstructures to reduce the apperance of fingerprints on surfaces |
DE102011054789A1 (en) * | 2011-10-25 | 2013-04-25 | Universität Kassel | Nano-shape structure |
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