CN107142466A - A kind of method that small-power continuous discharge prepares multi-functional nano protecting coating - Google Patents
A kind of method that small-power continuous discharge prepares multi-functional nano protecting coating Download PDFInfo
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- CN107142466A CN107142466A CN201710361310.XA CN201710361310A CN107142466A CN 107142466 A CN107142466 A CN 107142466A CN 201710361310 A CN201710361310 A CN 201710361310A CN 107142466 A CN107142466 A CN 107142466A
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- 238000000576 coating method Methods 0.000 title claims abstract description 73
- 239000011248 coating agent Substances 0.000 title claims abstract description 72
- 238000000034 method Methods 0.000 title claims abstract description 43
- 230000002633 protecting effect Effects 0.000 title claims abstract description 20
- 238000006243 chemical reaction Methods 0.000 claims abstract description 79
- 239000000178 monomer Substances 0.000 claims abstract description 74
- 239000000463 material Substances 0.000 claims abstract description 73
- 230000033001 locomotion Effects 0.000 claims abstract description 46
- 239000002253 acid Substances 0.000 claims abstract description 29
- 238000002360 preparation method Methods 0.000 claims abstract description 20
- 239000011261 inert gas Substances 0.000 claims abstract description 17
- 238000007747 plating Methods 0.000 claims abstract description 17
- 238000005229 chemical vapour deposition Methods 0.000 claims abstract description 16
- 238000000151 deposition Methods 0.000 claims abstract description 13
- 230000008021 deposition Effects 0.000 claims abstract description 12
- 239000002904 solvent Substances 0.000 claims abstract description 10
- 238000005137 deposition process Methods 0.000 claims abstract description 4
- 230000007246 mechanism Effects 0.000 claims abstract description 4
- 239000000758 substrate Substances 0.000 claims description 28
- 229930195735 unsaturated hydrocarbon Natural products 0.000 claims description 24
- 239000002103 nanocoating Substances 0.000 claims description 22
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical class FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 claims description 16
- 239000011347 resin Substances 0.000 claims description 16
- 229920005989 resin Polymers 0.000 claims description 16
- 239000011343 solid material Substances 0.000 claims description 16
- 239000000203 mixture Substances 0.000 claims description 15
- -1 polytetrafluoroethylene Polymers 0.000 claims description 15
- 239000000047 product Substances 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 150000002148 esters Chemical class 0.000 claims description 10
- 239000003960 organic solvent Substances 0.000 claims description 8
- KUDUQBURMYMBIJ-UHFFFAOYSA-N 2-prop-2-enoyloxyethyl prop-2-enoate Chemical compound C=CC(=O)OCCOC(=O)C=C KUDUQBURMYMBIJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000002537 cosmetic Substances 0.000 claims description 6
- LJRSZGKUUZPHEB-UHFFFAOYSA-N 2-[2-(2-prop-2-enoyloxypropoxy)propoxy]propyl prop-2-enoate Chemical compound C=CC(=O)OC(C)COC(C)COC(C)COC(=O)C=C LJRSZGKUUZPHEB-UHFFFAOYSA-N 0.000 claims description 5
- 238000007654 immersion Methods 0.000 claims description 5
- 210000004243 sweat Anatomy 0.000 claims description 5
- GTELLNMUWNJXMQ-UHFFFAOYSA-N 2-ethyl-2-(hydroxymethyl)propane-1,3-diol;prop-2-enoic acid Chemical class OC(=O)C=C.OC(=O)C=C.OC(=O)C=C.CCC(CO)(CO)CO GTELLNMUWNJXMQ-UHFFFAOYSA-N 0.000 claims description 4
- FIHBHSQYSYVZQE-UHFFFAOYSA-N 6-prop-2-enoyloxyhexyl prop-2-enoate Chemical compound C=CC(=O)OCCCCCCOC(=O)C=C FIHBHSQYSYVZQE-UHFFFAOYSA-N 0.000 claims description 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 4
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 claims description 4
- WIMBFQPYJQMSCP-UHFFFAOYSA-N (1,2,2,3,3,4,4,5,5,6,6-undecafluorocyclohexyl) 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OC1(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C1(F)F WIMBFQPYJQMSCP-UHFFFAOYSA-N 0.000 claims description 3
- 239000002202 Polyethylene glycol Substances 0.000 claims description 3
- 230000001351 cycling effect Effects 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 3
- 230000001788 irregular Effects 0.000 claims description 3
- 229920001223 polyethylene glycol Polymers 0.000 claims description 3
- 230000004044 response Effects 0.000 claims description 3
- SAMJGBVVQUEMGC-UHFFFAOYSA-N 1-ethenoxy-2-(2-ethenoxyethoxy)ethane Chemical compound C=COCCOCCOC=C SAMJGBVVQUEMGC-UHFFFAOYSA-N 0.000 claims description 2
- OTDGZDMGSFBZLI-UHFFFAOYSA-N 1-ethynyl-3,5-difluorobenzene Chemical class FC1=CC(F)=CC(C#C)=C1 OTDGZDMGSFBZLI-UHFFFAOYSA-N 0.000 claims description 2
- UZSRUNWVDBGNCD-UHFFFAOYSA-N 6,6,7,7,8,8,9,9,10,10,11,11,12,12,13,13,14,14,15,15,16,16,17,17,17-pentacosafluoroheptadec-2-ene Chemical class FC(C(C(C(C(C(C(C(C(C(C(C(F)(F)F)(F)F)(F)F)(F)F)(F)F)(F)F)(F)F)(F)F)(F)F)(F)F)(F)F)(CCC=CC)F UZSRUNWVDBGNCD-UHFFFAOYSA-N 0.000 claims description 2
- NTCKRBSOZLPJQP-UHFFFAOYSA-N 6,6,7,7,8,8,9,9,9-nonafluoronon-2-ene Chemical class FC(C(C(C(F)(F)F)(F)F)(F)F)(CCC=CC)F NTCKRBSOZLPJQP-UHFFFAOYSA-N 0.000 claims description 2
- 240000007594 Oryza sativa Species 0.000 claims description 2
- 235000007164 Oryza sativa Nutrition 0.000 claims description 2
- 238000000429 assembly Methods 0.000 claims description 2
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- 159000000011 group IA salts Chemical class 0.000 claims description 2
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- 235000009566 rice Nutrition 0.000 claims description 2
- 239000011265 semifinished product Substances 0.000 claims description 2
- 230000035939 shock Effects 0.000 claims description 2
- GETTZEONDQJALK-UHFFFAOYSA-N (trifluoromethyl)benzene Chemical compound FC(F)(F)C1=CC=CC=C1 GETTZEONDQJALK-UHFFFAOYSA-N 0.000 claims 1
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims 1
- 125000004386 diacrylate group Chemical group 0.000 claims 1
- 239000002585 base Substances 0.000 abstract description 55
- 239000003513 alkali Substances 0.000 abstract description 12
- 239000011247 coating layer Substances 0.000 abstract description 4
- 150000003839 salts Chemical class 0.000 abstract description 3
- 239000010408 film Substances 0.000 description 28
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 13
- 230000000694 effects Effects 0.000 description 12
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- 238000005260 corrosion Methods 0.000 description 9
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- 238000005516 engineering process Methods 0.000 description 8
- 238000006116 polymerization reaction Methods 0.000 description 8
- 239000007789 gas Substances 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 6
- 229920000052 poly(p-xylylene) Polymers 0.000 description 6
- 229920000642 polymer Polymers 0.000 description 6
- 230000006378 damage Effects 0.000 description 5
- 230000003628 erosive effect Effects 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
- 230000004888 barrier function Effects 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 238000004132 cross linking Methods 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 4
- 239000011159 matrix material Substances 0.000 description 4
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- 238000004891 communication Methods 0.000 description 3
- 230000005611 electricity Effects 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Natural products OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- 238000007781 pre-processing Methods 0.000 description 3
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 3
- 239000011253 protective coating Substances 0.000 description 3
- 150000003254 radicals Chemical class 0.000 description 3
- GRJRKPMIRMSBNK-UHFFFAOYSA-N 3,3,4,4,5,5,6,6,7,7,8,8,8-tridecafluorooctan-1-ol Chemical compound OCCC(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F GRJRKPMIRMSBNK-UHFFFAOYSA-N 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 2
- 229910000851 Alloy steel Inorganic materials 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- JIGUQPWFLRLWPJ-UHFFFAOYSA-N Ethyl acrylate Chemical compound CCOC(=O)C=C JIGUQPWFLRLWPJ-UHFFFAOYSA-N 0.000 description 2
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 description 2
- URLKBWYHVLBVBO-UHFFFAOYSA-N Para-Xylene Chemical group CC1=CC=C(C)C=C1 URLKBWYHVLBVBO-UHFFFAOYSA-N 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 230000001458 anti-acid effect Effects 0.000 description 2
- 239000003518 caustics Substances 0.000 description 2
- 239000013064 chemical raw material Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 230000005284 excitation Effects 0.000 description 2
- 229930195733 hydrocarbon Natural products 0.000 description 2
- 230000008595 infiltration Effects 0.000 description 2
- 238000001764 infiltration Methods 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 239000002114 nanocomposite Substances 0.000 description 2
- 238000010422 painting Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 230000008054 signal transmission Effects 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- XTKBMZQCDBHHKY-UHFFFAOYSA-N 1-ethynyl-4-(trifluoromethyl)benzene Chemical compound FC(F)(F)C1=CC=C(C#C)C=C1 XTKBMZQCDBHHKY-UHFFFAOYSA-N 0.000 description 1
- LEJBBGNFPAFPKQ-UHFFFAOYSA-N 2-(2-prop-2-enoyloxyethoxy)ethyl prop-2-enoate Chemical compound C=CC(=O)OCCOCCOC(=O)C=C LEJBBGNFPAFPKQ-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 1
- 229910000906 Bronze Inorganic materials 0.000 description 1
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 1
- 241000255925 Diptera Species 0.000 description 1
- 206010013786 Dry skin Diseases 0.000 description 1
- CERQOIWHTDAKMF-UHFFFAOYSA-M Methacrylate Chemical compound CC(=C)C([O-])=O CERQOIWHTDAKMF-UHFFFAOYSA-M 0.000 description 1
- 235000008331 Pinus X rigitaeda Nutrition 0.000 description 1
- 235000011613 Pinus brutia Nutrition 0.000 description 1
- 241000018646 Pinus brutia Species 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- QYKIQEUNHZKYBP-UHFFFAOYSA-N Vinyl ether Chemical compound C=COC=C QYKIQEUNHZKYBP-UHFFFAOYSA-N 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 238000003916 acid precipitation Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000001154 acute effect Effects 0.000 description 1
- 238000004026 adhesive bonding Methods 0.000 description 1
- 238000005273 aeration Methods 0.000 description 1
- 150000001299 aldehydes Chemical class 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000010974 bronze Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000005234 chemical deposition Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- KUNSUQLRTQLHQQ-UHFFFAOYSA-N copper tin Chemical compound [Cu].[Sn] KUNSUQLRTQLHQQ-UHFFFAOYSA-N 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006477 desulfuration reaction Methods 0.000 description 1
- 230000023556 desulfurization Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 125000004177 diethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000003670 easy-to-clean Effects 0.000 description 1
- 230000005672 electromagnetic field Effects 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 230000005281 excited state Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000009851 ferrous metallurgy Methods 0.000 description 1
- 239000007792 gaseous phase 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
- 150000008282 halocarbons Chemical class 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000010687 lubricating oil Substances 0.000 description 1
- 230000000873 masking effect Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 230000036961 partial effect Effects 0.000 description 1
- QMMOXUPEWRXHJS-UHFFFAOYSA-N pent-2-ene Chemical group CCC=CC QMMOXUPEWRXHJS-UHFFFAOYSA-N 0.000 description 1
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 description 1
- 125000005459 perfluorocyclohexyl group Chemical group 0.000 description 1
- 125000005005 perfluorohexyl group Chemical group FC(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)* 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 230000002688 persistence Effects 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 229920006254 polymer film Polymers 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000013517 stratification Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 239000002345 surface coating layer Substances 0.000 description 1
- 235000007586 terpenes Nutrition 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 229960000834 vinyl ether Drugs 0.000 description 1
- KAKZBPTYRLMSJV-UHFFFAOYSA-N vinyl-ethylene Natural products C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 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
- C23C16/44—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 method of coating
- C23C16/50—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 method of coating using electric discharges
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Metallurgy (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Plasma & Fusion (AREA)
- Organic Chemistry (AREA)
- Nanotechnology (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Physical Vapour Deposition (AREA)
Abstract
A kind of method that small-power continuous discharge prepares multi-functional nano protecting coating, belong to technical field of plasma, in this method, vacuum in reaction chamber is extracted into 10~200 millitorrs, and it is passed through inert gas He or Ar, opening movement mechanism, base material is set to produce motion in reaction chamber, monomer vapours are passed through in reaction chamber, plasma discharge, carry out chemical vapor deposition, deposition process includes pretreatment stage and plating mem stage, pretreatment stage plasma discharge manner discharges for high power CW, plated film phase plasma discharge mode is small-power continuous discharge.In coating preparation process, kinetic characteristic and plasma discharge energy the combination linkage of base material.While preparation process plasma discharge, base material produces motion, improves coating deposition efficiency, and improve the uniformity and compactness of coating layer thickness.Prepared coating has waterproof and dampproof, mould proof, an acid and alkali resistance solvent, the characteristic such as acid and alkali resistance salt fog.
Description
Technical field
The invention belongs to plasma chemical vapor deposition technique field, and in particular to prepare multi-functional nanometer to one kind
The method of protective coating.
Background technology
Corrosive atmosphere is the destroyed most common factor of electronic device.Cause because of environmental corrosion solid in electronic device
The phenomena of the failure such as the reduction of burn into conductor/semiconductor insulating properties and short circuit, open circuit or the loose contact of body material.At present, exist
In the product of the hi-tech industries such as national defence, space flight, the ratio that electronic unit occupies is increasing, moistureproof to electronic product, mould proof,
Corrosion resistance requires more and more stricter.And in communication field, as technology constantly improves, the continuous lifting of communication frequency, to logical
Interrogate the radiating of equipment, the reliability of signal transmission and require also more and more higher.Accordingly, it would be desirable to which reliable method can be to circuit
Plate and electronic component are effectively protected, and proper heat reduction and signal transmission are not interfered with again.
Polymer coating due to economic, easy application, it is applied widely the features such as be usually used in the protection of material surface, Ke Yifu
Give the good physics of material, chemical durability.Barrier based on polymer coating, it is in electronic apparatus, circuit board surface shape
Into diaphragm can be effectively isolated wiring board, and can protection circuit erosion, destruction are exempted under corrosive environment, so as to improve electricity
The reliability of sub- device, increases its safety coefficient, and ensures its service life, is used as erosion shield.
Conformal coating (Conformal coating) is that certain material is coated on PCB, is formed and the external shape of coated article
The technical process for the insulating protective layer being consistent, is a kind of conventional circuit board waterproof method, can be effectively isolated wiring board,
And can protection circuit exempt from adverse circumstances erosion, destruction.In current conformal coat preparation process there is also some problems and
Drawback：Solvent easily causes damage to circuit board components in liquid phase method；Heat-curable coating high temperature easily causes device failure；Light is consolidated
Change coating and be difficult to closed device inside.A kind of new conformal coat of U.S. Union Carbide Co. development and application
Material, parylene coating is a kind of polymer of paraxylene, can be reached with low water, gas permeability, high screen effect
Protection against the tide, waterproof, antirust, the effect of antiacid caustic corrosion.Research finds that Parylene is that deposition is produced under vacuum conditions, can be with
Apply the protection of the field such as high-frequency circuit, pole light current streaming system that can not be related in liquid coating.Polymer thin membrane coat is thick
Degree is to influence the main cause of Parylene vapour deposition conformal coat protection failure, printed circuit board assembly thin polymer film
In 3~7 micron thickness local corrosion failure easily occurs for coating, and coating layer thickness answers >=30 in the case of not influenceing high-frequency dielectric to be lost
Micron.The pre-processing requirements of printed substrate of the parylene coating for needing to protect are higher, and such as conductive component, signal are transmitted
Component, radio frequency component etc., need to do circuit board module masking pretreatment, it is to avoid to component when being vapor-deposited conformal coat
It can impact.This drawback brings very big limitation to the application of parylene coating.Parylene coating preparing raw material cost height,
Coating preparation condition harsh (high temperature, condition of high vacuum degree requirement), rate of film build are low, it is difficult to extensive use.In addition, thick coating is easily caused
The problems such as weak heat-dissipating, signal barrier, holiday increase.
Plasma activated chemical vapour deposition (plasma chemical vapor deposition, PCVD) is a kind of use etc.
Gas ions activated reactive gas, promotion is chemically reacted in matrix surface or near surface space, generates the technology of solid film.Deng
Gas ions chemical vapour deposition technique coating has advantages below
(1) it is dry process, generation film is uniformly pin-free.
(2) chemistry such as the solvent resistance of plasma polymerization film, chemical resistance, heat resistance, abrasion resistance properties, physics
Property is stable.
(3) plasma polymerization film and matrix gluing are good.
(4) it may be made as homogeneous film in the substrate surface of concavo-convex irregular.
(5) coating preparation temperature is low, can be carried out under normal temperature condition, be prevented effectively from the damage of temperature sensitive device.
(6) plasma process can not only prepare thickness for micron-sized coating but also can prepare ultra-thin nanoscale
Coating.
P2i companies of Britain are developed a kind of based on specific small duty cycle pulse electric discharge using chemical vapour deposition technique
Polymer nanocomposite coating prepared by method, should can not be realized based on the preparation process of the method for specific small duty cycle pulse electric discharge
It is prepared to the effective cooperation and control of not isoplastic bond distance, bond energy, the molecular weight of material with providing energy in chemical raw material
The scratch resistance and persistence effect of coating are undesirable.Also just because of coating performance limit, current coating only electronics,
A kind of nano coating of lyophobicity is formed on electric equipment, and the corrosion resistance brought to environment can not be solved effectively
Certainly.And had the shortcomings that based on fine and close protective coating prepared by the method that specific small duty cycle pulse is discharged fatal：From micro-
See for angle, less power density is unfavorable for the shaping of compact texture in coating process, or even can not form stable film
Structure；For macroscopically, the big speed that less power density is unfavorable for coating increases, and efficiency is relatively low in actual production,
Limit its application.
Base material is all fixed, the motion shape of base material in existing plasma chemical vapor deposition coating preparation process
The discharge energy of state and plasma does not have relevance；With base material static in the method processing chamber housing of continuous discharge, in monomer
The chain rupture of activation typically combines film forming in the presence of continuous discharge by simply stacking, and obtained coating general structure is dredged
Pine, or even powdered degree are high, are unfavorable for the formation of the microcosmic compact texture of coating, therefore, the waterproof of coating, protection against the tide, it is corrosion-resistant,
The barrier propterties such as solvent resistant are poor.
Because there is different zones difference, base material transfixion in plasma density in reaction chamber and chemical raw material density
Some regions coating deposition rate can be caused slow, low production efficiency, but also there is uniformity and compactness differs greatly shows
As.
The content of the invention
The present invention provides a kind of small-power continuous discharge preparation multi-functional nano protecting painting to solve above-mentioned technical problem
The method of layer.In the preparation process, technique mainly includes pre-processing and plating mem stage, pretreatment stage plasma discharge manner
Discharged for high power CW, plated film phase plasma discharge mode is small-power continuous discharge.And by the kinetic characteristic of base material
Combine and link with plasma discharge energy, while plasma discharge energy is exported, base material keeps motion state.Pass through
Gas ions energy introduces the other monomers component with polyfunctional group cross-linked structure and introduces extra crosslinking points to form crosslinking
Structure.Plasma discharge produces plasma, by controlling the relation between plasma discharge energy and monomer bond energy, real
The effective activation of the existing low temperature plasma active group higher to energy in monomer component obtains avtive spot, meanwhile, drawn
The additional active point entered is cross-linked with each other polymerization under plasma ambient, forms fine and close network structure.
The technical solution adopted in the present invention is as follows：
A kind of method that small-power continuous discharge prepares multi-functional nano protecting coating, it is characterised in that：Including following
Step：
(1) base material is placed in the reaction chamber of nano coating Preparation equipment, reaction chamber is continuously vacuumized, will reacted
Vacuum in chamber is extracted into 10~200 millitorrs, and is passed through inert gas He or Ar, and opening movement mechanism makes base material anti-
Answer and motion is produced in chamber；
(2) monomer vapours are passed through in reaction chamber, is 30~300 millitorrs to vacuum, opens plasma discharge, enter
Row chemical vapor deposition, deposition process includes pretreatment stage and plating mem stage, and pretreatment stage plasma discharge power is
120~400W, 60~900s of continuous discharging time, subsequently into plating mem stage, adjustment plasma discharge power is 10~
75W, continuous discharging time 600s~7200s, multi-functional nano coating is prepared in substrate surface chemical vapor deposition；
The purpose of pretreatment stage is activated substrate surface, and numerous avtive spots are formed in substrate surface.The bombardment is pre-
Processing can clear up the impurity of substrate surface, while, beneficial to the deposition of coating, coating and base can be improved with the surface of activated substrate
The adhesion of material.
The monomer vapours composition is：
The unsaturated fluorocarbon resin of at least one single functionality and at least one polyfunctionality unsaturated hydrocarbons analog derivative it is mixed
Mass fraction in compound, the monomer vapours shared by polyfunctionality unsaturated hydrocarbons analog derivative is 15~65%；
(3) stop being passed through monomer vapours, while stopping plasma discharge, persistently vacuumize, keep reaction chamber vacuum
Spend to be passed through air after 10~200 1~5min of millitorr to an atmospheric pressure, stop the motion of base material, then take out base material.
In the continuous discharge that pretreatment stage plasma discharge form is high-power 120~400W, plating mem stage etc. from
Daughter discharge type is 10~75W of small-power continuous discharge.What the process of continuous plasma discharge depositing was produced etc.
Gas ions have certain etching to deposition film；Be conducive to accelerating in plating mem stage small-power continuous discharge combination substrate transport characteristic
The speed of chemical deposition, relatively existing small duty cycle pulse discharge technology, the continuous discharge mode thickness within the regular hour
Thicker and finer and close, plated film is more efficient, thus solve the P2i companies of Britain mentioned in background technology based on specific small
The fatal defects of fine and close protective coating prepared by the method for duty cycle pulse electric discharge.
Under low vacuum plasma discharge environment, by effective output to energy, control molecular structure is more active
Chemical bond in monomer is broken, the higher free radical of formation activity, and the product surface such as free radical and mobile phone of excitation state is lived
Change group triggers polymerization to form nano water-proof film by way of chemical bonds, and multi-functional nanometer is formed in substrate surface
Coating.
Base material produces motion in reaction chamber in the step (1), and substrate transport form is base material relative response chamber
Straight reciprocating motion or curvilinear motion are carried out, the curvilinear motion includes circular motion, ellipse circular motion, planetary motion, sphere
Motion or the curvilinear motion of other irregular routes.
Base material is solid material in the step (1), and the solid material is electronic product, electric component, Electronic Assemblies
Semi-finished product, pcb board, metallic plate, polytetrafluoroethylene (PTFE) sheet material or electronic component, and the substrate surface prepare multifunctionality and received
Its any interface can be exposed to water environment, mould environment, acid, basic solvent environment, acid, alkaline salt mist environment, acid after rice coating
Property atmospheric environment, organic solvent immersion environment, cosmetics environment, sweat environment, cold cycling shock environment or damp and hot alternation ring
Used in border.
In the step (1) volume of reaction chamber be 50~1000L, the temperature control of reaction chamber at 30~60 DEG C,
The inert gas is passed through flow for 5~300sccm.
The reaction chamber is rotator shaped chamber or cube shaped chamber.
Monomer vapours are passed through to be atomized monomer by charge pump, volatilize and introduce anti-by the millitorr of low pressure 10~200
Chamber is answered, the flow for being passed through monomer is 10~1000 μ L/min；
The unsaturated fluorocarbon resin of the single functionality includes：
3- (perfluor -5- methylhexyls) -2- hydroxy propyl methacrylates, 2- (perfluoro decyl) ethyl methacrylate
Ester, 2- (perfluoro hexyl) ethylmethyl acrylate, 2- (perfluorododecyl) ethyl propylenes acid esters, 2- perfluoro capryl acrylic acid
Ethyl ester, 1H, 1H, 2H, 2H- perfluorooctanols acrylate, 2- (perfluoro butyl) ethyl propylenes acid esters, (2H- perfluoro propyls) -2-
Acrylate, (perfluorocyclohexyl) methacrylate, the fluoro- 1- propine of 3,3,3- tri-, 1- acetenyl -3,5- difluorobenzenes or 4-
Acetenyl benzotrifluoride；
The polyfunctionality unsaturated hydrocarbons analog derivative includes：
Ethoxylated trimethylolpropane triacrylate, tri (propylene glycol) diacrylate, the propylene of polyethylene glycol two
Acid esters, 1,6 hexanediol diacrylate, ethylene glycol diacrylate, diethylene glycol divinyl ether or diacrylate new penta 2
Alcohol ester.
In the step (2), the plasma discharge manner is radio frequency discharge, microwave discharge, intermediate frequency is discharged, high frequency is put
The waveform of electricity, spark discharge, the high-frequency discharge and intermediate frequency electric discharge is sinusoidal or bipolar pulse, and radio frequency plasma is to utilize
The plasma that electromagnetic field of high frequency is discharged and produced.Microwave method is the energy excitation plasma using microwave, with energy profit
It is prepared by current high-quality, high-speed, large area simultaneously because electrodeless discharge, plasma is pure with the advantage of efficiency high
Excellent process.
In coating preparation process, kinetic characteristic and plasma discharge energy the combination linkage of base material.Preparation process is medium
While plasma discharge, base material produces motion, improves coating deposition efficiency, and improve uniformity and the cause of coating layer thickness
Close property.
Prepared coating has waterproof and dampproof, and mould proof, acid and alkali resistance solvent, acid and alkali resistance salt fog, acid resistance is big
Gas, organic solvent-resistant immersion, resistance to cosmetics, resistance to sweat, cold-resistant thermal cycle impact (- 40 DEG C~+75 DEG C), wet-heat resisting alternation is (wet
95%) etc. degree 75%~characteristic.While possessing above-mentioned barrier propterty, coating layer thickness exists in the case of 1~1000nm to frequency
The influence of radio frequency communication signal in the range of 10M~8G is less than 5%.
The above-mentioned technical proposal of the present invention has advantages below compared with prior art：
1st, continuous small-power electric discharge is introduced in plating mem stage, can polymerize and carve simultaneously during continuous discharge
Lose two processes, one be the excited state molecule end of the chain that interrupts of plasma by way of chemical bond with substrate surface avtive spot
With reference to, two be plasma while the strand of the low chemical bond energy in surface after polymerization can be etched, while play a part of activation, two
The alternating action of person make it that the nano coating of polymerization is finer and close.
2nd, pre-process and plate mem stage, base material is moved in reaction chamber, makes the base material coating film thickness of diverse location
Tend to consistent, solve because different zones monomer density difference causes substrate surface coating layer thickness uneven in reaction chamber
Problem.
3rd, in preparation process, kinetic characteristic and plasma discharge energy the combination linkage of base material, discharge energy output
Meanwhile, base material is moved, and improves deposition efficiency, so as to get multi-functional nano protecting coating compactness significantly improve.
Simultaneously because the raising of deposition efficiency, the consumption of the chemical monomer raw material of monomer vapours also only has other consumptions in the prior art
10%~15%, so as to reduce the discharge of tail gas exhaust, more environmental protection, there is weight in actual production efficiency is improved
Big meaning.
4th, the introducing of polyfunctional group cross-linked structure promotes the fine and close network structure of coating in microstructure in monomer material
Formation, ensure it is hydrophobic while improving antiacid/caustic corrosion performance of the coating to environment.
General plasma polymerization selects monofunctional monomer, obtains with certain cross-linked structure coating.Cross-linked structure is
Because numerous active sites that chain rupture formation occurs in plasma discharge for monomer form crosslinking by way of interactive connection
Structure.But this cross-linked structure is more loose, containing more linear components, solvent resistant infiltration and dissolubility are poor.The present invention
The other monomers component of polyfunctional group cross-linked structure is carried by introducing and introduces extra crosslinking points to form cross-linked structure.Deng
During plasma discharge, under low temperature plasma effect, by effective control to energy and output, by energy in monomer component
Higher active group interrupts to form active site, and the additional active point being introduced into is cross-linked with each other polymerization, shape under plasma ambient
Into fine and close network structure.
For the coating structure more compared to loose linear components, network structure has more excellent compactness, Neng Gouyou
Effect improves the performance of the anticorrosive environment of film.Plated film matrix material is under plasma ambient, and surface is activated obtaining numerous work
Property site, the living radical of these avtive spots and the monomer material through plasma exciatiaon is mutually tied with stronger chemical bond
Close, occur the elementary reaction of form and wide variety so that the nano thin-film of matrix material has excellent adhesion and machinery
Intensity.By controlling different monomers fit system, while the different process conditions of regulation and control, to realize to the anticorrosive of material surface
The Effective Regulation of environment, obtains the big structure of the bottom dense skin roughness with special microstructure, its environmental corrosion resisting
Combination property improve 20%~35%.
5th, by the other monomers of introducing crosslinked structure, monomer ratio is controlled, according to the molecular bond energy of different monomers, bond distance
Difference, the difference of vapourizing temperature, give the Significant Change of the output of equipment corresponding energy and technological parameter, be combined, gradually
The polymer nanocomposite coating of structure changes, both ensure that the hydrophobicity of film, and the resistance to environment that the products such as electronic product are improved again is rotten
The performance of erosion.
Electronic equipment in daily life is easily damaged by the erosion of corrosive environment, is substantially at during use
In corrosive environment, if things go on like this, the irremediable infringement of electronic equipment can be caused.The film plating process of patent of the present invention is greatly increased
Nanometer is significant in actual production efficiency is improved.Coating improves production in the service life of corrosive atmosphere
The protecting effect of product.It is mainly used in following product：
(1), portable equipment keyboard：The characteristics of portable keyboard has small and light, is usually used in computer, the equipment such as mobile phone.
It can be easy to user to be handled official business in route.But when it runs into the pollution of common liquid, the unexpected overturning for the teacup that is such as filled with water, rain
Water, sweat are impregnated with, and keyboard is easily short-circuit, and then damage.It is carried out after plated film using such nano coating, when can
Ensure that function is intact after surface of keyboard easy to clean, chance water so that keyboard can adapt to more acute environment.
(2), LED display：LED display has demonstration, and StoreFront decoration is illuminated, the purposes such as warning.Its partial use
When needing the adverse circumstances, such as rainy day in face of rainwater or many dust, the outdoor LED advertisement screen curtain in market, road surface warning lamp,
The LED display control panel of workshop, these adverse circumstances cause LED screen failure, and easily dust stratification, are difficult clear
Wash, after the nano coating, can effectively solve the problem that above mentioned problem.
(3), intelligent fingerprint lock：Fingerprint Lock is intelligent lock, and it has gathered computer information technology, electronic technology, machinery
Technology and modern five gold process, are widely used in police criminal detection and judicial domain.But it is met after water, its inner wire Louis is short
Road, it is difficult to repair, it is necessary to lock is torn in violence open, after the coating, this problem can be avoided.
(4), audiphone, bluetooth earphone：Audiphone is with bluetooth earphone without connection, after the coating, Yong Huke
To be used within a certain period of time under water environment, such as have a bath, rainy day, equipment will not be damaged because of rainwater infiltration.
(5), operative sensor：Operative sensor needs to work in liquid environment, such as hydraulic pressure, oil pressure sensor, and
The sensor used in underwater operation equipment, and working environment often meet the sensor of water, and these sensors are using the painting
After layer, can ensure will not cause faulty sensor because of liquid intrusion plant equipment internal structure.
(6), most of 3C Products：Such as mobile phone, notebook, PSP.
(7), other need the equipment of waterproof：Including needing the operation in wet environment, or it is likely encountered common liquid
The fortuitous event, the equipment that internal light current circuit can be influenceed normally to run such as splash.
Multi-functional nano coating prepared by this method can be applicable to following different environment and its correlation being related to
Product：
It is waterproof and dampproof mould proof：
1 house interior trim：Toilet top surface, wallpaper, pendent lamp, curtain, window screening.2 daily necessitiess：Mosquito net, desk lamp cover, chopsticks
Basket, automobile rearview mirror.3 historical relics and the art work：Copybook, antiques, woodcarving, leather, bronze ware, silk, ancient costume, ancient books.4 electronics member
Device and electronic product：Sensor (operation in moist or dirty environment), each electronic product (electronic sphygmomanometer, intelligent hand
Table) chip, wiring board, mobile phone, LED screen, audiphone.5 precision instruments and optical device：Mechanical watch, microscope.
Acid and alkali resistance solvent, acid and alkali resistance salt fog, acid resistance air：
1 house inside gadget：Wallpaper, ceramic tile.2 safety devices：Acidproof (alkali) gloves, acidproof (alkali) protective garment.3 plant equipment
And pipeline：Flue desulfurization equipment, seal (acid/base lubricating oil), pipeline, valve, Large Diameter Pipeline sea conveyance conduit liner etc.
Place.4 various reactors, reactor.The production of 5 chemicals, storage；Sewage disposal, aeration tank；6 is other：Soda acid workshop, alkali prevention
The every profession and trades such as Aero-Space, electricity power, Ferrous Metallurgy, petrochemical industry, medical treatment, storage container, statue (reduce acid rain to its
Corrosion), sensor (under acid/base environment).
Organic solvent-resistant soaks, resistance to cosmetics, resistance to sweat：
1 such as alkane, alkene, alcohol, aldehyde, amine, ester, ether, ketone, aromatic hydrocarbon, hydrogenate hydrocarbon, terpene hydrocarbon, halogenated hydrocarbons, jeterocyclic chemistry
Thing, nitrogen-containing compound and sulfur-containing compound solvent etc.；2 toiletry bag packaging containers；3 Fingerprint Locks, earphone.
Cold-resistant thermal cycle impact (- 40 DEG C~+75 DEG C), wet-heat resisting alternation (humidity 75%~95%)：Electrician, electronics, vapour
Car electrical equipment, such as aviation, automobile, household electrical appliances, the equipment in scientific research field.
Embodiment
The present invention is described in detail with reference to specific embodiment, but the invention is not limited in specific embodiment.
Embodiment 1
A kind of method that small-power continuous discharge prepares multi-functional nano protecting coating, comprises the following steps：
(1) base material is placed in the reaction chamber of nano coating Preparation equipment, closed reaction chamber simultaneously connects to reaction chamber
It is continuous to vacuumize, the vacuum in reaction chamber is extracted into 10 millitorrs, inert gas Ar is passed through, opening movement mechanism makes base material exist
Motion is produced in reaction chamber；Base material is solid material in step (1), and the solid material is block polyfluortetraethylene plate
Material, and the substrate surface prepares after mould proof nano coating its any interface and can be surveyed exposed to GJB150.10A-2009 moulds
Test ring is used in border.
The volume of reaction chamber is 50L in step (1), and the temperature control of reaction chamber is passed through inert gas at 30 DEG C
Flow is 5sccm.
Base material produces motion in reaction chamber in step (1), and substrate transport form is carried out for base material relative response chamber
Circular motion, rotating speed is 1 turn/min.
(2) monomer vapours are passed through in reaction chamber, when to vacuum being 30 millitorr, plasma discharge is opened, carries out
Chemical vapor deposition, deposition process includes pretreatment stage and plates mem stage, pretreatment stage plasma discharge power 120W,
Time 900s, subsequently into plating mem stage, plasma discharge power is 10W, time 7200s, in substrate surface chemical gaseous phase
Deposition prepares mould proof nano coating.
In step (2)：
It is passed through monomer vapours be atomized monomer by charge pump, volatilize, reaction chamber is introduced by the millitorr of low pressure 10,
The flow for being passed through monomer vapours is 1000 μ L/min；
Monomer vapours composition is：
The mixture of two kinds of unsaturated fluorocarbon resins of single functionality and two kinds of polyfunctionality unsaturated hydrocarbons analog derivatives, monomer
Mass fraction in steam shared by polyfunctionality unsaturated hydrocarbons analog derivative is 15%；
The unsaturated fluorocarbon resin of the single functionality is：2- perfluoro capryls ethyl acrylate, 2- (perfluoro hexyl) ethyl first
Base acrylate；
The polyfunctionality unsaturated hydrocarbons analog derivative is：Ethylene glycol diacrylate, 1,6 hexanediol diacrylate；
Step (2) the plasma discharge mode is continuous radio frequency discharge.
(3) plated film terminates, and stopping is passed through starting monomer steam, while stopping plasma discharge, persistently vacuumizes, and keeps
Reaction cavity vacuum is 10 millitorrs, is passed through air to an atmospheric pressure after 1min, then takes out base material.
Obtained deposition has the polyfluortetraethylene plate performance test effect of mould proof coating as follows：
Embodiment 2
A kind of method that small-power continuous discharge prepares multi-functional nano protecting coating, comprises the following steps：
(1) base material is placed in nano coating Preparation equipment reaction chamber, closed reaction chamber is simultaneously continuous to reaction chamber
Vacuumize, the vacuum in reaction chamber is extracted into 60 millitorrs, be passed through inert gas He, start motion, carry out base material
Motion；
Base material is solid material in step (1), and the solid material is block aluminum alloy materials, and the substrate surface system
Its any interface can be in acid, alkali test environment after standby acid and alkali resistance environment coating.
The volume of reaction chamber is 250L in step (1), and the temperature control of reaction chamber is passed through inert gas at 40 DEG C
Flow is 15sccm.
Base material carries out planetary motion in step (1), and revolution speed is 1 turn/min, and rotational velocity is 1.5 turns/min.
(2) monomer vapours are passed through in reaction chamber, when vacuum is 90 millitorr, plasma discharge is opened, is changed
Learn and be vapor-deposited, pretreatment stage power 200W, time 700s, subsequently into plating mem stage, discharge power is 30W, time
6000s, the nano coating of acid and alkali resistance environment is prepared in substrate surface chemical vapor deposition.
In step (2)：
It is passed through monomer vapours be atomized monomer by charge pump, volatilize, reaction cavity is introduced by the millitorr of low pressure 60,
The flow for being passed through monomer vapours is 700 μ L/min；
Monomer vapours composition is：
The mixture of three kinds of unsaturated fluorocarbon resins of single functionality and two kinds of polyfunctionality unsaturated hydrocarbons analog derivatives, monomer
Mass fraction in steam shared by polyfunctionality unsaturated hydrocarbons analog derivative is 35%；
The unsaturated fluorocarbon resin of the single functionality is：2- (perfluoro decyl) ethylmethyl acrylate, 2- (perfluors 12
Alkyl) ethyl propylene acid esters, (perfluorocyclohexyl) methacrylate；
The polyfunctionality unsaturated hydrocarbons analog derivative is：Tri (propylene glycol) diacrylate and the propylene of polyethylene glycol two
Acid esters；
Step (2) plasma discharge mode is intermediate frequency continuous discharge, and the waveform of intermediate frequency electric discharge is sinusoidal.
(3) plated film terminates, and stopping is passed through starting monomer steam, while stopping plasma discharge, persistently vacuumizes, and keeps
Reaction cavity vacuum is 80 millitorrs, is passed through air to an atmospheric pressure after 2min, then takes out base material.
After above-mentioned aluminum alloy materials plated film, acid, alkalescence test effect are as follows：
Embodiment 3
A kind of method that small-power continuous discharge prepares multi-functional nano protecting coating, comprises the following steps：
(1) base material is placed in nano coating Preparation equipment reaction chamber, closed reaction chamber is simultaneously continuous to reaction cavity
Vacuumize, the vacuum in reaction chamber is extracted into 130 millitorrs, be passed through inert gas Ar, start motion, carry out base material
Motion；
Base material is solid material in step (1), and the solid material is bulk alloy steel plate materialses, and the substrate surface
Preparing its any interface after organic solvent-resistant immersion and the coating of resistance to cosmetics can be exposed in organic solvent test environment.
The volume of reaction chamber is 480L in step (1), and the temperature control of reaction chamber is passed through inert gas at 50 DEG C
Flow is 60sccm,.
Base material carries out circular motion in step (1), and rotating speed is 3 turns/min.
(2) monomer vapours are passed through in reaction chamber, when vacuum is 150 millitorr, plasma discharge is opened, is changed
Learn and be vapor-deposited, pretreatment stage power 250W, time 580s, subsequently into plating mem stage, discharge power is 45W, time
4000s, the nano coating of organic solvent-resistant immersion and resistance to cosmetics is prepared in substrate surface chemical vapor deposition.
In step (2)：
It is passed through monomer vapours be atomized monomer by charge pump, volatilize, reaction cavity is introduced by the millitorr of low pressure 10,
The flow for being passed through monomer vapours is 550 μ L/min；
Monomer vapours composition is：
The mixture of two kinds of unsaturated fluorocarbon resins of single functionality and two kinds of polyfunctionality unsaturated hydrocarbons analog derivatives, monomer
Mass fraction in steam shared by polyfunctionality unsaturated hydrocarbons analog derivative is 45%；
The unsaturated fluorocarbon resin of the single functionality is：(perfluorocyclohexyl) methacrylate and 2- (perfluoro hexyl) second
Methyl acrylate；
The polyfunctionality unsaturated hydrocarbons analog derivative is：Ethoxylated trimethylolpropane triacrylate and diethyl two
Alcohol divinyl ether；
Step (2) plasma discharge mode is high frequency continuous discharge, and the waveform of high-frequency discharge is bipolar pulse.
(3) plated film terminates, and stopping is passed through starting monomer steam, while stopping plasma discharge, persistently vacuumizes, and keeps
Reaction cavity vacuum is 130 millitorrs, is passed through air to an atmospheric pressure after 3min, then takes out base material.
After above-mentioned alloy-steel plate material film plating, organic solvent-resistant test effect is as follows：
Embodiment 4
A kind of method that small-power continuous discharge prepares multi-functional nano protecting coating, comprises the following steps：
(1) base material is placed in nano coating Preparation equipment reaction chamber, closed reaction chamber is simultaneously continuous to reaction cavity
Vacuumize, the vacuum in reaction chamber is extracted into 160 millitorrs, be passed through inert gas He, start motion, carry out base material
Motion；
Base material is solid material in step (1), and the solid material is block aluminum material and pcb board, and the base material
Surface, which prepares its any interface after cold-resistant thermal cycle impact coating, to be exposed in hot and cold loop test environment.
The volume of reaction chamber is 680L in step (1), and the temperature control of reaction chamber is passed through inert gas at 50 DEG C
Flow is 160sccm.
Base material carries out straight reciprocating motion in step (1), and movement velocity is 20mm/min.
(2) monomer vapours are passed through in reaction chamber, when vacuum is 190 millitorr, plasma discharge is opened, is changed
Learn and be vapor-deposited, pretreatment stage power 300W, time 350s, subsequently into plating mem stage, discharge power is 55W, time
2200s, the nano coating of cold-resistant thermal cycle impact is prepared in substrate surface chemical vapor deposition.
In step (2)：
It is passed through monomer vapours be atomized monomer by charge pump, volatilize, reaction chamber is introduced by the millitorr of low pressure 160
Room, the flow for being passed through monomer vapours is 220 μ L/min；
Monomer vapours composition is：
The mixture of three kinds of unsaturated fluorocarbon resins of single functionality and three kinds of polyfunctionality unsaturated hydrocarbons analog derivatives, monomer
Mass fraction in steam shared by polyfunctionality unsaturated hydrocarbons analog derivative is 55%；
The unsaturated fluorocarbon resin of the single functionality is：The fluoro- 1- propine of 3,3,3- tri-, 3- (perfluor -5- methylhexyls) -2-
Hydroxy propyl methacrylate, 1H, 1H, 2H, 2H- perfluorooctanol acrylate；
The polyfunctionality unsaturated hydrocarbons analog derivative is：Ethoxylated trimethylolpropane triacrylate, two propylene
Sour glycol ester and 1,6 hexanediol diacrylate；
Step (2) plasma discharge mode is discharged for microwave continuous.
(3) plated film terminates, and stopping is passed through starting monomer steam, while stopping plasma discharge, persistently vacuumizes, and keeps
Reaction cavity vacuum is 160 millitorrs, is passed through air to an atmospheric pressure after 4min, then takes out base material.
Block aluminum material and pcb board after above-mentioned plated film, cold cycling shock-testing effect are as follows：
Embodiment 5
A kind of method that small-power continuous discharge prepares multi-functional nano protecting coating, comprises the following steps：
(1) base material is placed in nano coating Preparation equipment reaction chamber, closed reaction chamber is simultaneously continuous to reaction cavity
Vacuumize, the vacuum in reaction chamber is extracted into 200 millitorrs, be passed through inert gas Ar, start motion, carry out base material
Motion；
In step (1) base material be solid material, the solid material be electronic component, and the substrate surface prepare it is resistance to
Its any interface can be exposed in damp and hot test environment after damp and hot alternation coating.
The volume of reaction chamber is 1000L in step (1), and the temperature control of reaction chamber is passed through inert gas at 60 DEG C
Flow be 300sccm.
Base material carries out curved reciprocating movement in step (1), and speed is 100mm/min.
(2) monomer vapours are passed through in reaction chamber, when vacuum is 300 millitorr, plasma discharge is opened, is changed
Learn and be vapor-deposited, pretreatment stage power 400W, time 60s, subsequently into plating mem stage, discharge power is 75W, time
600s, the nano coating of wet-heat resisting alternation is prepared in substrate surface chemical vapor deposition.
In step (2)：
It is passed through monomer vapours be atomized monomer by charge pump, volatilize, reaction chamber is introduced by the millitorr of low pressure 200
Body, the flow for being passed through monomer vapours is 10 μ L/min；
Monomer vapours composition is：
The mixture of three kinds of unsaturated fluorocarbon resins of single functionality and two kinds of polyfunctionality unsaturated hydrocarbons analog derivatives, monomer
Mass fraction in steam shared by polyfunctionality unsaturated hydrocarbons analog derivative is 65%；
The unsaturated fluorocarbon resin of the single functionality is：1H, 1H, 2H, 2H- perfluorooctanol acrylate, 3,3,3- tri-
Fluoro- 1- propine and 2- (perfluoro hexyl) ethylmethyl acrylate；
The polyfunctionality unsaturated hydrocarbons analog derivative is：Tri (propylene glycol) diacrylate and diacrylate ethylene glycol
Ester；
Step (2) plasma discharge mode is spark discharge.
(3) plated film terminates, and stopping is passed through starting monomer steam, while stopping plasma discharge, persistently vacuumizes, and keeps
Reaction cavity vacuum is 200 millitorrs, is passed through air to an atmospheric pressure after 5min, then takes out base material.
Electronic component after above-mentioned plated film, damp and hot alternation test effect is as follows：
Embodiment 6
The present embodiment is identical with the processing step that embodiment 1 is basic, and different technological parameters is as follows：
1st, the vacuum in reaction chamber is extracted into 120 millitorrs by step (1), is passed through inert gas Ar；
Step (1) base material is solid material, and the solid material is electric component, and substrate surface preparation waterproof is resistance to
Its any interface can be used exposed to the environment described in International Industry classification of waterproof standard IPX7 after electrical breakdown coating.
The volume of reaction chamber is 400L in step (1), and the temperature control of reaction chamber is passed through inert gas at 40 DEG C
Flow is 150sccm.
(2) monomer vapours are passed through in reaction chamber, when vacuum is 160 millitorr, plasma discharge is opened, is changed
Learn and be vapor-deposited, pretreatment stage power 380W, time 400s, subsequently into plating mem stage, discharge power is 20W, time
3600s, the resistance to nano coating being powered under water is prepared in substrate surface chemical vapor deposition.
In step (2)：It is passed through monomer vapours be atomized monomer by charge pump, volatilize, by the millitorr of low pressure 160
Reaction chamber is introduced, the flow for being passed through monomer vapours is 200 μ L/min；
Monomer vapours composition is：
The mixture of four kinds of unsaturated fluorocarbon resins of single functionality and two kinds of polyfunctionality unsaturated hydrocarbons analog derivatives, monomer
Mass fraction in steam shared by polyfunctionality unsaturated hydrocarbons analog derivative is 48%；
The unsaturated fluorocarbon resin of the single functionality is：2- (perfluoro decyl) ethylmethyl acrylate, 1H, 1H, 2H,
The fluoro- 1- propine of 2H- perfluorooctanols acrylate, 3,3,3- tri- and 2- (perfluoro hexyl) ethylmethyl acrylate；
The polyfunctionality unsaturated hydrocarbons analog derivative is：Tri (propylene glycol) diacrylate and diethylene glycol divinyl
Base ether；
2nd, step (3) keeps reaction cavity vacuum to be passed through air to an atmospheric pressure after 160 millitorr 5min.
Electric component after above-mentioned plated film, resistance to powered under water, underwater soaking experiment effect is as follows：
Following table is that coating manufactured in the present embodiment reaches time test used in 1mA in different voltage, currents：
| Voltage | 3.8V | 5V | 12.5V |
| Time | >48h | ＞ 24h | ＞ 24h |
It is working properly that IPX 7 tests (1m submerging test 30min under water) electric component.
Claims (8)
1. a kind of method that small-power continuous discharge prepares multi-functional nano protecting coating, it is characterised in that：Including following step
Suddenly：
(1) base material is placed in the reaction chamber of nano coating Preparation equipment, reaction chamber is continuously vacuumized, by reaction chamber
Interior vacuum is extracted into 10~200 millitorrs, and is passed through inert gas He or Ar, and opening movement mechanism makes base material in reaction chamber
Indoor generation campaign；
(2) monomer vapours are passed through in reaction chamber, is 30~300 millitorrs to vacuum, opens plasma discharge, changed
Learn vapour deposition, deposition process include pretreatment stage and plating mem stage, pretreatment stage plasma discharge power be 120~
400W, 60~900s of continuous discharging time, subsequently into plating mem stage, adjustment plasma discharge power is 10~75W, is continued
Discharge time 600s~7200s, multi-functional nano coating is prepared in substrate surface chemical vapor deposition；
The monomer vapours composition is：
The mixture of the unsaturated fluorocarbon resin of at least one single functionality and at least one polyfunctionality unsaturated hydrocarbons analog derivative,
Mass fraction in the monomer vapours shared by polyfunctionality unsaturated hydrocarbons analog derivative is 15~65%；
(3) stop being passed through monomer vapours, while stopping plasma discharge, persistently vacuumize, holding reaction chamber vacuum is
Air is passed through after 10~200 1~5min of millitorr to an atmospheric pressure, stops the motion of base material, then takes out base material.
2. the method that a kind of small-power continuous discharge according to claim 1 prepares multi-functional nano protecting coating, its
It is characterised by：Base material produces motion in reaction chamber in the step (1), and substrate transport form is base material relative response chamber
Straight reciprocating motion or curvilinear motion are carried out, the curvilinear motion includes circular motion, ellipse circular motion, planetary motion, sphere
Motion or the curvilinear motion of other irregular routes.
3. the method that a kind of small-power continuous discharge according to claim 1 prepares multi-functional nano protecting coating, its
It is characterised by：Base material is solid material in the step (1), and the solid material is electronic product, electric component, Electronic Assemblies
Semi-finished product, pcb board, metallic plate, polytetrafluoroethylene (PTFE) sheet material or electronic component, and the substrate surface prepare multifunctionality and received
Its any interface can be exposed to water environment, mould environment, acid, basic solvent environment, acid, alkaline salt mist environment, acid after rice coating
Property atmospheric environment, organic solvent immersion environment, cosmetics environment, sweat environment, cold cycling shock environment or damp and hot alternation ring
Used in border.
4. the method that a kind of small-power continuous discharge according to claim 1 prepares multi-functional nano protecting coating, its
It is characterised by：In the step (1) volume of reaction chamber be 50~1000L, the temperature control of reaction chamber at 30~60 DEG C,
The inert gas is passed through flow for 5~300sccm.
5. the method that a kind of small-power continuous discharge according to claim 1 or 4 prepares multi-functional nano protecting coating,
It is characterized in that：The reaction chamber is rotator shaped chamber or cube shaped chamber.
6. the method that a kind of small-power continuous discharge according to claim 1 prepares multi-functional nano protecting coating, its
It is characterised by：In the step (2)：Monomer vapours are passed through to be atomized monomer by charge pump, volatilize and by low pressure 10
~200 millitorrs introduce reaction chamber, and the flow for being passed through monomer is 10~1000 μ L/min.
7. the method that a kind of small-power continuous discharge according to claim 1 prepares multi-functional nano protecting coating, its
It is characterised by：
The unsaturated fluorocarbon resin of the single functionality includes：
3- (perfluor -5- methylhexyls) -2- hydroxy propyl methacrylates, 2- (perfluoro decyl) ethylmethyl acrylate,
2- (perfluoro hexyl) ethylmethyl acrylate, 2- (perfluorododecyl) ethyl propylenes acid esters, 2- perfluoro capryl acrylic acid second
Ester, 1H, 1H, 2H, 2H- perfluorooctanols acrylate, 2- (perfluoro butyl) ethyl propylenes acid esters, (2H- perfluoro propyls) -2- propylene
Acid esters, (perfluorocyclohexyl) methacrylate, the fluoro- 1- propine of 3,3,3- tri-, 1- acetenyl -3,5- difluorobenzenes or 4- acetenyls
Benzotrifluoride；
The polyfunctionality unsaturated hydrocarbons analog derivative includes：
Ethoxylated trimethylolpropane triacrylate, tri (propylene glycol) diacrylate, polyethyleneglycol diacrylate,
1,6 hexanediol diacrylate, ethylene glycol diacrylate, diethylene glycol divinyl ether or diacrylic acid pentyl diol ester.
8. the method that a kind of small-power continuous discharge according to claim 1 prepares multi-functional nano protecting coating, its
It is characterised by：In the step (2), plasma discharge manner be radio frequency discharge, microwave discharge, intermediate frequency electric discharge, high-frequency discharge,
The waveform of spark discharge, the high-frequency discharge and intermediate frequency electric discharge is sinusoidal or bipolar pulse.
Priority Applications (5)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710361310.XA CN107142466B (en) | 2017-05-21 | 2017-05-21 | A kind of method that small-power continuous discharge prepares multi-functional nano protecting coating |
| PCT/CN2017/113188 WO2018214446A1 (en) | 2017-05-21 | 2017-11-27 | Method for preparing multi-functional protective nano coating by means of low-power continuous discharge |
| US16/688,845 US11742186B2 (en) | 2017-05-21 | 2019-11-19 | Multi-functional protective coating |
| US16/688,589 US11270871B2 (en) | 2017-05-21 | 2019-11-19 | Multi-layer protective coating |
| US17/653,401 US11587772B2 (en) | 2017-05-21 | 2022-03-03 | Multi-layer protective coating |
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| CN201710361310.XA CN107142466B (en) | 2017-05-21 | 2017-05-21 | A kind of method that small-power continuous discharge prepares multi-functional nano protecting coating |
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Cited By (8)
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| WO2018214447A1 (en) * | 2017-05-21 | 2018-11-29 | 江苏菲沃泰纳米科技有限公司 | Method for preparing multi-functional protective nano coating by means of cyclical low-power continuous discharge |
| WO2018214450A1 (en) * | 2017-05-21 | 2018-11-29 | 江苏菲沃泰纳米科技有限公司 | Method for preparing multi-functional protective nano coating by means of periodic alternating discharge |
| WO2018214446A1 (en) * | 2017-05-21 | 2018-11-29 | 江苏菲沃泰纳米科技有限公司 | Method for preparing multi-functional protective nano coating by means of low-power continuous discharge |
| WO2018214448A1 (en) * | 2017-05-21 | 2018-11-29 | 江苏菲沃泰纳米科技有限公司 | Method for preparing multifunctional protective nano coating by means of large-duty-ratio pulse discharge |
| WO2018214451A1 (en) * | 2017-05-21 | 2018-11-29 | 江苏菲沃泰纳米科技有限公司 | Method for preparing multi-functional protective nano coating by means of cyclical periodic alternating discharge |
| WO2020082681A1 (en) * | 2018-10-24 | 2020-04-30 | 江苏菲沃泰纳米科技有限公司 | High-transparency low-color-difference nano coating and preparation method therefor |
| US11270871B2 (en) | 2017-05-21 | 2022-03-08 | Jiangsu Favored Nanotechnology Co., LTD | Multi-layer protective coating |
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| CN107142466B (en) | 2018-05-11 |
| WO2018214446A1 (en) | 2018-11-29 |
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Denomination of invention: A method for preparing multifunctional nano protective coatings using low-power continuous discharge Granted publication date: 20180511 Pledgee: Wuxi Branch of China CITIC Bank Co.,Ltd. Pledgor: Jiangsu feiwotai nanotechnology Co.,Ltd. Registration number: Y2024980016337 |