CN107142465B - A method of cycle small-power continuous discharge prepares multi-functional nano protecting coating - Google Patents
A method of cycle small-power continuous discharge prepares multi-functional nano protecting coating Download PDFInfo
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- CN107142465B CN107142465B CN201710360355.5A CN201710360355A CN107142465B CN 107142465 B CN107142465 B CN 107142465B CN 201710360355 A CN201710360355 A CN 201710360355A CN 107142465 B CN107142465 B CN 107142465B
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- 238000000576 coating method Methods 0.000 title claims abstract description 87
- 239000011248 coating agent Substances 0.000 title claims abstract description 74
- 238000000034 method Methods 0.000 title claims abstract description 40
- 230000002633 protecting effect Effects 0.000 title claims abstract description 20
- 238000006243 chemical reaction Methods 0.000 claims abstract description 80
- 239000000178 monomer Substances 0.000 claims abstract description 74
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- 239000002253 acid Substances 0.000 claims abstract description 28
- 239000002103 nanocoating Substances 0.000 claims abstract description 23
- 238000005229 chemical vapour deposition Methods 0.000 claims abstract description 21
- 239000011261 inert gas Substances 0.000 claims abstract description 17
- 229930195735 unsaturated hydrocarbon Natural products 0.000 claims description 24
- 238000002360 preparation method Methods 0.000 claims description 18
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical compound 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
- -1 2- (perfluoro decyl) ethylmethyl Chemical group 0.000 claims description 15
- 239000000047 product Substances 0.000 claims description 15
- 238000007599 discharging Methods 0.000 claims description 14
- 150000002148 esters Chemical class 0.000 claims description 11
- 239000002904 solvent Substances 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
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- 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
- 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
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- 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
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- 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
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- GETTZEONDQJALK-UHFFFAOYSA-N (trifluoromethyl)benzene Chemical compound FC(F)(F)C1=CC=CC=C1 GETTZEONDQJALK-UHFFFAOYSA-N 0.000 claims description 2
- 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
- 159000000011 group IA salts Chemical class 0.000 claims description 2
- 239000011265 semifinished product Substances 0.000 claims description 2
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- 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
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- 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
- 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
- 230000009471 action Effects 0.000 description 2
- 150000001336 alkenes Chemical class 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
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- 230000007613 environmental effect Effects 0.000 description 2
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- 239000011159 matrix material Substances 0.000 description 2
- 239000002114 nanocomposite Substances 0.000 description 2
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- 150000003839 salts Chemical class 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 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
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 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
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- 150000001299 aldehydes Chemical class 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
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- KUNSUQLRTQLHQQ-UHFFFAOYSA-N copper tin Chemical compound [Cu].[Sn] KUNSUQLRTQLHQQ-UHFFFAOYSA-N 0.000 description 1
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- 125000004177 diethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
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- 238000009851 ferrous metallurgy Methods 0.000 description 1
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- 125000000524 functional group Chemical group 0.000 description 1
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- 229910052737 gold Inorganic materials 0.000 description 1
- 150000008282 halocarbons Chemical class 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
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- 238000001764 infiltration Methods 0.000 description 1
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- 239000007791 liquid phase Substances 0.000 description 1
- 239000010687 lubricating oil Substances 0.000 description 1
- 230000000873 masking effect Effects 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
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- 238000010422 painting 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
- 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
- 238000002203 pretreatment Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000010865 sewage Substances 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
- 210000003462 vein Anatomy 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
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Metallurgy (AREA)
- Nanotechnology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Plasma & Fusion (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- General Physics & Mathematics (AREA)
- Physical Vapour Deposition (AREA)
- Application Of Or Painting With Fluid Materials (AREA)
- Laminated Bodies (AREA)
Abstract
A method of cycle small-power continuous discharge prepares multi-functional nano protecting coating,Belong to technical field of plasma,In this method,By the indoor suction of reaction chamber and it is passed through inert gas,Base material is set to generate movement in reaction chamber,It is passed through in monomer vapours to reaction chamber,Carry out chemical vapor deposition,Deposition 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,Circulating repetition pretreatment stage and plating mem stage are at least once,During coating process,Cycle, which introduces, makes substrate surface introduce more active sites,Increase effective plated film,Membrane structure is finer and close,Obtain the nano coating of multi-layer compound structure,Multilayer proofing is provided for product itself,More fine and close coating structure is shown as on microcosmic,From macroscopically showing excellent hydrophobicity,Adhesive force,Acid and alkali-resistance,Mechanical performance and wet-hot aging performance.
Description
Technical field
The invention belongs to plasma chemical vapor deposition technique fields, and in particular to prepare multi-functional nanometer to a kind of
The method of protective coating.
Background technology
Corrosive environment is the most common factor that electronic device is destroyed.Cause because of environmental corrosion solid in electronic device
The burn into conductor/semiconductor insulating properties of body material reduces and the phenomena of the failure such as short-circuit, open circuit or poor contact.Currently,
In the product of the hi-tech industries such as national defence, space flight, the ratio that electronic unit occupies is increasing, moisture-proof to electronic product, mould proof,
Corrosion resistance requires to be increasingly stringenter.And in communication field, as technology is constantly progressive, the continuous of communication frequency is promoted, to logical
The reliability of the heat dissipation, signal transmission of interrogating equipment requires also higher and higher.Therefore, it is necessary to reliable methods can be to circuit
Plate and electronic component carry out effective protection, and do not interfere with proper heat reduction and signal transmission.
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 property based on polymer coating, in electronic apparatus, circuit board surface shape
At protective film can be effectively isolated wiring board, and can protect circuit under corrosive environment from corroding, destroying, 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 common circuit board waterproof method, can be effectively isolated wiring board,
And erosion, destruction of the circuit from adverse circumstances can be protected.In current conformal coat preparation process there is also some problems and
Drawback：Solvent is easy to cause to damage to circuit board components in liquid phase method；Heat-curable coating high temperature be easy to cause device failure；Light is solid
Change coating and is difficult to closed device inside.A kind of novel conformal coat of U.S. Union Carbide Co. development and application
Material, parylene coating are a kind of polymer of paraxylene, and there is low water, gas permeability, high screen effect can reach
Moisture-proof, waterproof, antirust, antiacid caustic corrosion effect.Research finds that Parylene is that deposition generates under vacuum conditions, can be with
Apply the protection in the field that liquid coating can not be related to such as high-frequency circuit, pole light current streaming system.Polymer thin membrane coat is thick
Degree is printed circuit board assembly thin polymer film the main reason for influencing Parylene vapor deposition conformal coat protection failure
In 3~7 micron thickness local corrosion failure easily occurs for coating, and >=30 are answered in the case that not influencing high-frequency dielectric loss coating layer thickness
Micron.Parylene coating is higher for the pre-processing requirements for the printed wiring board that needs protect, such as conductive component, signal transmission
Component, radio frequency component etc. are needed to do masking pretreatment to circuit board module when being vapor-deposited conformal coat, be avoided to component
It can impact.This drawback brings very big limitation to the application of parylene coating.Parylene coating prepare cost of material it is high,
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 led to
The problems such as weak heat-dissipating, signal barrier, holiday increase.
Plasma activated chemical vapour deposition (plasma chemical vapor deposition, PCVD) be it is a kind of with etc.
Gas ions activated reactive gas, promotion are chemically reacted in matrix surface or near surface space, generate the technology of solid film.Deng
Gas ions chemical vapour deposition technique coating has the following advantages：
(1) it is dry process, it is uniformly pin-free generates film.
(2) chemistry such as the solvent resistance of plasma polymerization film, chemical resistance, heat resistance, abrasion resistance properties, physics
Property is stablized.
(3) plasma polymerization film and matrix gluing are good.
(4) it may be made as uniform film in the substrate surface of concave-convex irregular.
(5) coating preparation temperature is low, can be carried out under normal temperature condition, effectively avoid the damage of temperature sensitive device.
(6) plasma process can not only prepare thickness and be 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 be can not achieve based on the preparation process of the method for specific small duty cycle pulse electric discharge
It is prepared to not isoplastic bond distance, bond energy, the molecular weight of material and effective cooperation of offer energy and control in chemical raw material
The scratch resistance and persistence effect of coating are undesirable.Also just because of the performance of coating limit, at present coating only electronics,
A kind of nano coating of lyophobicity is formed on electrical equipment, and corrosion resistance caused by environment cannot 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-
For seeing angle, smaller power density is unfavorable for the molding of compact texture in coating process, or even can not form stable film
Structure；For macroscopically, the big rate that smaller power density is unfavorable for coating increases, and efficiency is relatively low in actual production,
Limit its application.
Base material is all fixed in existing plasma chemical vapor deposition coating preparation process, the movement shape of base material
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 is generally dredged by simply stacking the coating general structure obtained in conjunction with film forming under the action of continuous discharge
Pine or even powdered degree are high, are unfavorable for the formation of the microcosmic compact texture of coating, therefore, the waterproof of coating, it is moisture-proof, corrosion-resistant,
The barrier propterties such as solvent resistant are poor.
Since plasma density in reaction chamber and chemical raw material density are there are different zones difference, base material is stationary
Some regions coating deposition rate can be caused slow, low production efficiency, but also there are what uniformity and compactness differed greatly to show
As.
Invention content
It is anti-that the present invention provides a kind of multi-functional nanometer of cycle small-power continuous discharge preparation to solve above-mentioned technical problem
The method for protecting coating.In the preparation process, technique includes mainly pre-processing and plating mem stage, pretreatment stage plasma discharge
Mode be high power CW electric discharge, plated film phase plasma discharge mode be small-power continuous discharge, and the pretreatment and
Coating process is at least repeated 2 times, and forms the compact texture of multilayer.And by the kinetic characteristic of base material and plasma discharge energy bins
Linkage is closed, while plasma discharge energy exports, base material keeps motion state.It is introduced with more by energy of plasma
The other monomers component of functional group's cross-linked structure and introduce additional crosslinking points to form cross-linked structure.Plasma discharge generates
Plasma realizes low temperature plasma to monomer by controlling the relationship between plasma discharge energy and monomer bond energy
The effective activation of the higher active group of energy obtains active site in component, meanwhile, the additional active point being introduced into wait from
Be cross-linked with each other polymerization under subenvironment, forms fine and close reticular structure.
The technical solution adopted in the present invention is as follows：
A method of cycle small-power continuous discharge prepares multi-functional nano protecting coating, it is characterised in that：Including
Following steps：
(1) base material is placed in the reaction chamber of nano coating Preparation equipment, reaction chamber is continuously vacuumized, will be reacted
The indoor vacuum degree of chamber is extracted into 10~200 millitorrs, and is passed through inert gas He or Ar, and opening movement mechanism makes base material anti-
It answers and generates movement in chamber；
(2) it is passed through in monomer vapours to reaction chamber, until vacuum degree is 30~300 millitorrs, opens plasma discharge, into
Row chemical vapor deposition；
(3) deposition process include pretreatment stage and plating mem stage, pretreatment stage plasma discharge power be 120~
400W, 60~450s of continuous discharging time, subsequently into plating mem stage, adjustment plasma discharge power is 10~75W, is continued
600~3600s of discharge time；
(4) in circulating repetition step (3) pretreatment stage and plating mem stage at least once, in substrate surface chemical vapor deposition
Product prepares multi-functional nano coating；
The purpose of pretreatment stage is activated substrate surface, and numerous active sites are formed in substrate surface.The bombardment is pre-
Processing can clear up the impurity of substrate surface, while can be conducive to the deposition of coating with the surface of activated substrate, improve coating and base
The binding force of material, in repeated pretreatment and coating process, the high-power pretreated bombardment process after each plated film can
Further to form numerous active sites in film surface, the surface of film layer is activated, is conducive to the further deposition of coating, improves film
Binding force between layer, formation binding force and the higher laminated coating structure of consistency, more general single long-time plated film,
20%-40% and 15%-30% has at least been respectively increased in binding force and consistency, and the mode effect of the cycle small-power plated film is bright
Aobvious, practicability is stronger.
The monomer vapours ingredient is：
At least one single functionality unsaturation fluorocarbon resin and at least one polyfunctionality unsaturated hydrocarbons analog derivative it is mixed
Object is closed, the mass fraction in the monomer vapours shared by polyfunctionality unsaturated hydrocarbons analog derivative is 15~65%；
(5) stop being passed through monomer vapours, be simultaneously stopped plasma discharge, persistently vacuumize, keep reaction chamber vacuum
Degree is passed through air to an atmospheric pressure after being 10~200 1~5min of millitorr, stops the movement of base material, then takes 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 the continuous discharge of 10~75W of small-power.The process of continuous plasma discharge depositing generate it is equal from
Daughter has deposition film certain etching；Be conducive to quickeningization in plating mem stage small-power continuous discharge combination substrate transport characteristic
The speed of deposition is learned, relatively existing small duty cycle pulse discharge technology, continuous discharge mode film thickness is more within the regular hour
Thick and finer and close, plated film is more efficient, to solve being accounted for based on specifically small for the P2i companies of Britain mentioned in background technology
Fatal defects of the sky than fine and close protective coating prepared by the method for pulsed discharge.
Under low vacuum plasma discharge environment, by effective output to energy, control molecular structure is more active
Chemical bond in monomer is broken, and forms the higher free radical of activity, and the product surfaces such as free radical and mobile phone of excitation state are lived
Change group is caused polymerization by way of chemical bonds and forms nano water-proof film, and multi-functional nanometer is formed in substrate surface
Coating.
Base material generates movement in reaction chamber in the step (1), and substrate transport form is base material relative response chamber
It includes circular motion, ellipse circular motion, planetary motion, spherical surface to carry out straight reciprocating motion or curvilinear motion, the curvilinear motion
Movement 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) plank or electronic component, and the substrate surface prepare multifunctionality and receive
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 impregnates environment, cosmetics environment, sweat environment, cold cycling shock environment or damp and hot alternation ring
It is used in border.
The volume of reaction chamber is 50~1000L in the step (1), and the temperature of reaction chamber is controlled at 30~60 DEG C,
It is 5~300sccm that the inert gas, which is passed through flow,.
The reaction chamber is rotator shaped chamber or cube shaped chamber.
It is to be atomized monomer by charge pump, volatilize and introduced by 10~200 millitorr of low pressure anti-to be passed through monomer vapours
It is 10~1000 μ L/min to answer chamber, the flow for being passed through monomer；
The single functionality unsaturation fluorocarbon resin 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- third
Olefin(e) acid ester, (perfluorocyclohexyl) methacrylate, tri- fluoro- 1- propine of 3,3,3-, 1- acetenyl -3,5- difluorobenzenes or 4- acetylene
Base benzotrifluoride；
The polyfunctionality unsaturated hydrocarbons analog derivative includes：
Ethoxylated trimethylolpropane triacrylate, tri (propylene glycol) diacrylate, two propylene of polyethylene glycol
Acid esters, 1,6 hexanediol diacrylate, ethylene glycol diacrylate, diethylene glycol divinyl ether or diacrylate new penta 2
Alcohol ester.
The step (3) and (4) plasma discharge mode are radio frequency discharge, microwave discharge, intermediate frequency discharges, 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
Electromagnetic field of high frequency is discharged and the plasma of generation.Microwave method is the energy excitation plasma using microwave, has energy profit
With efficient advantage, simultaneously because electrodeless discharge, plasma is pure, is current high quality, high-speed, large area preparation
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 generates movement, improves coating deposition efficiency, and improve uniformity and the cause of coating layer thickness
Close property.
Prepared coating has waterproof and dampproof, mould proof, acid and alkali resistance solvent, and acid and alkali resistance salt fog, acid resistance is big
Gas, organic solvent-resistant impregnate, and resistance to cosmetics, resistance to sweat, cold-resistant thermal cycle impact (- 40 DEG C~+75 DEG C), wet-heat resisting alternation is (wet
Degree 75%~95%) etc. characteristics.While having above-mentioned barrier propterty, coating layer thickness exists to frequency in 1~1000nm
The influence of radio frequency communication signal within the scope of 10M~8G is less than 5%.
The above-mentioned technical proposal of the present invention has the following advantages compared with prior art：
1, cycle plated film introduces the powerful pre-treatment and activation stage in process stage, and the cycle in the stage introduces
Be conducive to introduce more active sites in the substrate surface in this stage, increase effective plated film, membrane structure is finer and close, to corrosivity
The better protecting effect of environment.During coating process, using cycle coating process, the nanometer of multi-layer compound structure is obtained
Coating provides multilayer proofing for product itself, it is microcosmic on show as more fine and close coating structure, it is excellent from macroscopically showing
Different hydrophobicity, adhesive force, acid and alkali-resistance, mechanical performance and wet-hot aging performance.
2, in cycle coating process process, continuous small-power electric discharge is introduced in plating mem stage, in the process of continuous discharge
In can occur simultaneously polymerize and etch two processes, first, the side that the excited state molecule end of the chain that plasma interrupts passes through chemical bond
Formula is combined with substrate surface active site, second is that plasma can etch the strand of the low chemical bond energy of polymerization rear surface simultaneously,
Play the role of activation simultaneously, the alternating action of the two makes the nano coating of polymerization finer and close.
3, it pre-processes and plates mem stage, base material moves in reaction chamber, makes the base material coating film thickness of different location
Tend to consistent, solves since different zones monomer density difference causes substrate surface coating layer thickness non-uniform in reaction chamber
Problem.
4, in preparation process, kinetic characteristic and plasma discharge energy the combination linkage of base material, discharge energy output
Meanwhile base material is moved, and deposition efficiency is improved, so as to get multi-functional nano protecting coating compactness significantly improve.
Simultaneously because the raising of deposition efficiency, the dosage of the chemical monomer raw material of monomer vapours also only has other dosages in the prior art
10%~15%, it is more environmentally protective to reduce the discharge of tail gas exhaust, in improving actual production efficiency have weight
Big meaning.
5, the introducing of polyfunctional group cross-linked structure promotes coating densification reticular structure 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 having certain cross-linked structure coating.Cross-linked structure is
Since 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
Additional crosslinking points are introduced to form cross-linked structure with the other monomers component of polyfunctional group cross-linked structure by introducing.Deng
When plasma discharge, under low temperature plasma effect, by the effective control and output to energy, 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 under plasma ambient, shape
At fine and close reticular structure.
For the coating structure more compared to loose linear components, reticular structure has more preferably compactness, Neng Gouyou
Effect improves the performance of the anticorrosive environment of film.Under plasma ambient, surface is activated to obtain numerous work plated film basis material
Property site, the living radical of these active sites and the monomer material through plasma exciatiaon are mutually tied with stronger chemical bond
It closes, the elementary reaction of form and wide variety occurs so that the nano thin-film of basis material has excellent binding force and machinery
Intensity.By controlling different monomers fit system, while regulating and controlling different process conditions, to realize to the anticorrosive of material surface
The Effective Regulation of environment obtains the structure for having the bottom dense skin roughness of special microstructure big, environmental corrosion resisting
Comprehensive performance improve 25%~45%.
6, 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, obtain compound, gradually
The polymer nanocomposite coating of structure changes, not only ensure that the hydrophobicity of film, but also improve the resistance to environment corruption of the products such as electronic product
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 damage of electronic equipment can be caused.The film plating process of patent of the present invention greatly increases
Nanometer is of great significance in improving actual production efficiency.Coating improves production in the service life of corrosive environment
The protecting effect of product.It is mainly used in following product：
(1), portable equipment keyboard：Portable keyboard has the characteristics that small and light, is usually used in computer, the equipment such as mobile phone.
It can handle official business convenient for user in route.But when it encounters the pollution of common liquid, the unexpected of the teacup that is such as filled with water overturns, rain
Water, sweat are impregnated with, and keyboard is easy short circuit, and then damages.After carrying out plated film to it using such nano coating, when can
Ensure surface of keyboard easy to clean, function is intact after meeting water so that keyboard can adapt to more acute environment.
(2), LED display：LED display has demonstration, StoreFront decoration, illumination, the purposes such as warning.Its partial use
The adverse circumstances in face of rainwater or more dust are needed, when such as rainy day, the outdoor LED advertisement screen curtain in market, road surface warning lamp, life
The LED display control panel in workshop is produced, these adverse circumstances lead to LED screen failure, and are easy dust stratification, not easy cleaning,
After the nano coating, the above problem can effectively solve the problem that.
(3), intelligent fingerprint lock：Fingerprint Lock is intelligent lock, 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 after it meets water, inner wire Louis is short
Road, it is difficult to repair, violence is needed to tear lock open, after the coating, this problem can be avoided.
(4), hearing aid, bluetooth headset：Hearing aid is with bluetooth headset without connection, after the coating, Yong Huke
It to be used under water environment within a certain period of time, such as has a bath, on rainy day, equipment will not be infiltrated because of rainwater to be damaged.
(5), operative sensor：Operative sensor needs work in liquid environment, such as hydraulic pressure, oil pressure sensor, and
The sensor and working environment used in underwater operation equipment often meet the sensor of water, these sensors are using the painting
After layer, can ensure will not lead to faulty sensor because of liquid intrusion mechanical equipment internal structure.
(6), most of 3C Products：Such as mobile phone, notebook, PSP.
(7), other equipment for needing waterproof：Including needs operation in wet environment, or it is likely encountered common liquid
It splashes and waits fortuitous events, the equipment of internal light current circuit normal operation can be influenced.
The correlation that multi-functional nano coating prepared by this method can be applicable to following different environment and its be 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, hearing aid.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 mechanical equipments
And pipeline：Flue desulfurization equipment, sealing element (acid/base lubricating oil), pipeline, valve, Large Diameter Pipeline sea conveyance conduit liner etc.
Place.4 various reaction kettles, 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 aerospace, 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 impregnates, 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
Object, nitrogenous 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
Vehicle electric appliance, such as aviation, automobile, household electrical appliances, scientific research field equipment.
Specific implementation mode
The present invention will be described in detail for specific embodiment below, but the invention is not limited in specific embodiments.
Embodiment 1
A method of cycle small-power continuous discharge prepares multi-functional nano protecting coating, includes the following steps：
(1) base material is placed in the reaction chamber of nano coating Preparation equipment, closed reaction chamber simultaneously connects reaction chamber
It is continuous to vacuumize, the indoor vacuum degree of reaction chamber is extracted into 10 millitorrs, is passed through inert gas Ar, opening movement mechanism makes base material exist
Movement is generated in reaction chamber；
In step (1) base material be solid material, the solid material be block-like polyfluortetraethylene plate and electric component, and
Its any interface can be exposed in GJB150.10A-2009 mould test environments and use after the substrate surface prepares coating, institute
Environment described in International Industry waterproofing grade standard IPX7 can be exposed to by stating its any interface after the prepares coating of electric component surface
It uses.
The volume of reaction chamber is 50L in step (1), and the temperature of reaction chamber is controlled at 30 DEG C, is passed through inert gas
Flow is 5sccm.
Base material generates movement in reaction chamber in step (1), and substrate transport form carries out for base material relative response chamber
Circular motion, rotating speed are 1 turn/min.
(2) it is passed through in monomer vapours to reaction chamber, until when vacuum degree is 30 millitorr, opens plasma discharge, carry out
Chemical vapor deposition；
(3) deposition process includes pretreatment stage and plating mem stage, and pretreatment stage plasma discharge power is 400W,
Continuous discharging time 60s, subsequently into plating mem stage, adjustment plasma discharge power is 75W, continuous discharging time 600s；
(4) pretreatment stage and plating mem stage 11 times in circulating repetition step (3), in substrate surface chemical vapor deposition system
Standby multifunctionality nano coating；
In step (2)：
It is to be atomized monomer by charge pump, volatilize to be passed through monomer vapours, and reaction chamber is introduced by 10 millitorr of low pressure,
The flow for being passed through monomer vapours is 1000 μ L/min；
Monomer vapours ingredient is：
The mixture of two kinds of single functionality unsaturation fluorocarbon resins and two kinds of polyfunctionality unsaturated hydrocarbons analog derivatives, monomer
Mass fraction in steam shared by polyfunctionality unsaturated hydrocarbons analog derivative is 30%；
The single functionality unsaturation fluorocarbon resin 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 (3) and (4) plasma discharge mode are continuous radio frequency discharge.
(5) plated film terminates, and stopping is passed through starting monomer steam, is simultaneously stopped plasma discharge, persistently vacuumizes, and keeps
Reaction cavity vacuum degree 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：
Obtained deposition has the electric component of waterproof electrical breakdown withstand coating to test underwater soaking effect such as under different voltages
Under：
Obtained deposition has 7 waterproofing grade of electric component IPX test (the underwater 1m immersions examination of waterproof electrical breakdown withstand coating
Test 30min) effect is as follows：
Embodiment 2
A method of cycle small-power continuous discharge prepares multi-functional nano protecting coating, includes the following steps：
(1) base material is placed in nano coating Preparation equipment reaction chamber, closed reaction chamber is simultaneously continuous to reaction chamber
It vacuumizes, the indoor vacuum degree of reaction chamber is extracted into 60 millitorrs, be passed through inert gas He, start motion, base material is made to carry out
Movement；
In step (1) base material be solid material, the solid material be block-like polyfluortetraethylene plate and electric component, and
Its any interface can be exposed in GJB150.10A-2009 mould test environments and use after the substrate surface prepares coating, institute
Environment described in International Industry waterproofing grade standard IPX7 can be exposed to by stating its any interface after the prepares coating of electric component surface
It uses.
The volume of reaction chamber is 250L in step (1), and the temperature of reaction chamber is controlled at 40 DEG C, is passed through inert gas
Flow is 15sccm.
Base material carries out planetary motion in step (1), and revolution speed is 2 turns/min, and rotational velocity is 2.5 turns/min.
(2) it is passed through in monomer vapours to reaction chamber, until when vacuum degree is 90 millitorr, opens plasma discharge, carry out
Chemical vapor deposition；
(3) deposition process includes pretreatment stage and plating mem stage, and pretreatment stage plasma discharge power is 120W,
Continuous discharging time 450s, subsequently into plating mem stage, adjustment plasma discharge power is 10W, continuous discharging time
3600s；
(4) pretreatment stage and plating mem stage 1 time in circulating repetition step (3), in substrate surface chemical vapor deposition system
Standby multifunctionality nano coating；
In step (2)：
It is to be atomized monomer by charge pump, volatilize to be passed through monomer vapours, and reaction cavity is introduced by 60 millitorr of low pressure,
The flow for being passed through monomer vapours is 500 μ L/min；
Monomer vapours ingredient is：
The mixture of three kinds of single functionality unsaturation fluorocarbon resins and two kinds of polyfunctionality unsaturated hydrocarbons analog derivatives, monomer
Mass fraction in steam shared by polyfunctionality unsaturated hydrocarbons analog derivative is 45%；
The single functionality unsaturation fluorocarbon resin is：2- (perfluoro decyl) ethylmethyl acrylate, 2- (perfluors 12
Alkyl) ethyl propylene acid esters, (perfluorocyclohexyl) methacrylate；
The polyfunctionality unsaturated hydrocarbons analog derivative is：Two propylene of tri (propylene glycol) diacrylate and polyethylene glycol
Acid esters；
Step (3) and (4) plasma discharge mode are intermediate frequency continuous discharge, and the waveform of intermediate frequency electric discharge is bipolar arteries and veins
Punching.
(5) plated film terminates, and stopping is passed through starting monomer steam, is simultaneously stopped plasma discharge, persistently vacuumizes, and keeps
Reaction cavity vacuum degree is 80 millitorrs, is passed through air to an atmospheric pressure after 2min, then takes out base material.
Obtained deposition has the polyfluortetraethylene plate performance test effect of mould proof coating as follows：
Obtained deposition has the electric component of waterproof electrical breakdown withstand coating to test underwater soaking effect such as under different voltages
Under：
Obtained deposition has 7 waterproofing grade of electric component IPX test (the underwater 1m immersions examination of waterproof electrical breakdown withstand coating
Test 30min) effect is as follows：
Embodiment 3
A method of cycle small-power continuous discharge prepares multi-functional nano protecting coating, includes the following steps：
(1) base material is placed in nano coating Preparation equipment reaction chamber, closed reaction chamber is simultaneously continuous to reaction cavity
It vacuumizes, the indoor vacuum degree of reaction chamber is extracted into 130 millitorrs, be passed through inert gas Ar, start motion, base material is made to carry out
Movement；
Base material is solid material in step (1), and the solid material is bulk alloy steel plate materials, and the substrate surface
Preparing organic solvent-resistant and impregnating can be exposed to its any interface after the coating of resistance to cosmetics in organic solvent test environment.
The volume of reaction chamber is 480L in step (1), and the temperature of reaction chamber is controlled at 50 DEG C, is passed through inert gas
Flow is 50sccm,.
Base material carries out circular motion in step (1), and rotating speed is 4 turns/min.
(2) it is passed through in monomer vapours to reaction chamber, until when vacuum degree is 150 millitorr, opens plasma discharge, carry out
Chemical vapor deposition；
(3) deposition process includes pretreatment stage and plating mem stage, and pretreatment stage plasma discharge power is 200W,
Continuous discharging time 150s, subsequently into plating mem stage, adjustment plasma discharge power is 20W, continuous discharging time
1000s；
(4) pretreatment stage and plating mem stage 6 times in circulating repetition step (3), in substrate surface chemical vapor deposition system
Standby multifunctionality nano coating；
In step (2)：
It is to be atomized monomer by charge pump, volatilize to be passed through monomer vapours, and reaction cavity is introduced by 10 millitorr of low pressure,
The flow for being passed through monomer vapours is 550 μ L/min；
Monomer vapours ingredient is：
The mixture of two kinds of single functionality unsaturation fluorocarbon resins and two kinds of polyfunctionality unsaturated hydrocarbons analog derivatives, monomer
Mass fraction in steam shared by polyfunctionality unsaturated hydrocarbons analog derivative is 45%；
The single functionality unsaturation fluorocarbon resin 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 (3) and (4) plasma discharge mode are high frequency continuous discharge, and the waveform of high-frequency discharge is sinusoidal.
(5) plated film terminates, and stopping is passed through starting monomer steam, is simultaneously stopped plasma discharge, persistently vacuumizes, and keeps
Reaction cavity vacuum degree 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, it is as follows that organic solvent-resistant tests effect：
Embodiment 4
A method of cycle small-power continuous discharge prepares multi-functional nano protecting coating, includes the following steps：
(1) base material is placed in nano coating Preparation equipment reaction chamber, closed reaction chamber is simultaneously continuous to reaction cavity
It vacuumizes, the indoor vacuum degree of reaction chamber is extracted into 160 millitorrs, be passed through inert gas He, start motion, base material is made to carry out
Movement；
Base material is solid material in step (1), and the solid material is blocky aluminum alloy materials, and the substrate surface system
Its any interface can be exposed in acid, alkali test environment after standby acid and alkali resistance environment coating.
The volume of reaction chamber is 680L in step (1), and the temperature of reaction chamber is controlled at 50 DEG C, is passed through inert gas
Flow is 160sccm.
Base material carries out straight reciprocating motion, movement velocity 20mm/min in step (1).
(2) it is passed through in monomer vapours to reaction chamber, until when vacuum degree is 190 millitorr, opens plasma discharge, carry out
Chemical vapor deposition；
(3) deposition process includes pretreatment stage and plating mem stage, and pretreatment stage plasma discharge power is 300W,
Continuous discharging time 250s, subsequently into plating mem stage, adjustment plasma discharge power is 35W, continuous discharging time
2000s；
(4) pretreatment stage and plating mem stage 3 times in circulating repetition step (3), in substrate surface chemical vapor deposition system
Standby multifunctionality nano coating；
In step (2)：
It is to be atomized monomer by charge pump, volatilize to be passed through monomer vapours, and reaction chamber is introduced by 160 millitorr of low pressure
Room, the flow for being passed through monomer vapours are 220 μ L/min；
Monomer vapours ingredient is：
The mixture of three kinds of single functionality unsaturation fluorocarbon resins and three kinds of polyfunctionality unsaturated hydrocarbons analog derivatives, monomer
Mass fraction in steam shared by polyfunctionality unsaturated hydrocarbons analog derivative is 35%；
The single functionality unsaturation fluorocarbon resin is：Tri- fluoro- 1- propine of 3,3,3-, 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 (3) and (4) plasma discharge mode are discharged for microwave continuous.
(5) plated film terminates, and stopping is passed through starting monomer steam, is simultaneously stopped plasma discharge, persistently vacuumizes, and keeps
Reaction cavity vacuum degree is 160 millitorrs, is passed through air to an atmospheric pressure after 4min, then takes out base material.
Blocky aluminum alloy materials after above-mentioned plated film, it is as follows that effect is tested in acid and alkali resistance：
Embodiment 5
A method of cycle small-power continuous discharge prepares multi-functional nano protecting coating, includes the following steps：
(1) base material is placed in nano coating Preparation equipment reaction chamber, closed reaction chamber is simultaneously continuous to reaction cavity
It vacuumizes, the indoor vacuum degree of reaction chamber is extracted into 200 millitorrs, be passed through inert gas Ar, start motion, base material is made to carry out
Movement；
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 of reaction chamber is controlled at 60 DEG C, is passed through inert gas
Flow be 300sccm.
In step (1) base material carry out planetary motion, planet revolution speed be 1 turn/min, planetary rotation speed be 1.5 turns/
min。
(2) it is passed through in monomer vapours to reaction chamber, until when vacuum degree is 300 millitorr, opens plasma discharge, carry out
Chemical vapor deposition；
(3) deposition process includes pretreatment stage and plating mem stage, and pretreatment stage plasma discharge power is 150W,
Continuous discharging time 400s, subsequently into plating mem stage, adjustment plasma discharge power is 55W, continuous discharging time
3000s；
(4) pretreatment stage and plating mem stage 2 times in circulating repetition step (3), in substrate surface chemical vapor deposition system
Standby multifunctionality nano coating；
In step (2)：
It is to be atomized monomer by charge pump, volatilize to be passed through monomer vapours, and reaction chamber is introduced by 200 millitorr of low pressure
Body, the flow for being passed through monomer vapours are 10 μ L/min；
Monomer vapours ingredient is：
The mixture of three kinds of single functionality unsaturation fluorocarbon resins and two kinds of polyfunctionality unsaturated hydrocarbons analog derivatives, monomer
Mass fraction in steam shared by polyfunctionality unsaturated hydrocarbons analog derivative is 65%；
The single functionality unsaturation fluorocarbon resin is：1H, 1H, 2H, 2H- perfluorooctanol acrylate, 3,3,3- tri- are 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 (3) and (4) plasma discharge mode are spark discharge.
(5) plated film terminates, and stopping is passed through starting monomer steam, is simultaneously stopped plasma discharge, persistently vacuumizes, and keeps
Reaction cavity vacuum degree 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 are as follows：
Embodiment 6
The present embodiment is identical as the processing step that embodiment 1 is basic, and different technological parameters is as follows：
1, the indoor vacuum degree of 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 blocky aluminum material and printed wiring board, and the base
Its any interface can be exposed in hot and cold loop test environment after material surface prepares cold-resistant thermal cycle impact coating.
The volume of reaction chamber is 400L in step (1), and the temperature of reaction chamber is controlled at 40 DEG C, is passed through inert gas
Flow is 150sccm.
(2) it is passed through in monomer vapours to reaction chamber, when vacuum degree is 160 millitorr, opens plasma discharge, changed
Learn vapor deposition；
(3) deposition process includes pretreatment stage and plating mem stage, and pretreatment stage plasma discharge power is 180W,
Continuous discharging time 200s, subsequently into plating mem stage, adjustment plasma discharge power is 60W, continuous discharging time
1500s；
(4) pretreatment stage and plating mem stage 3 times in circulating repetition step (3), in substrate surface chemical vapor deposition system
Standby multifunctionality nano coating；
In step (2)：It is to be atomized monomer by charge pump, volatilize to be passed through monomer vapours, is drawn by 160 millitorr of low pressure
Enter reaction chamber, the flow for being passed through monomer vapours is 200 μ L/min；
Monomer vapours ingredient is：
The mixture of four kinds of single functionality unsaturation fluorocarbon resins and two kinds of polyfunctionality unsaturated hydrocarbons analog derivatives, monomer
Mass fraction in steam shared by polyfunctionality unsaturated hydrocarbons analog derivative is 45%；
The single functionality unsaturation fluorocarbon resin is：2- (perfluoro decyl) ethylmethyl acrylate, 1H, 1H, 2H,
2H- perfluorooctanols acrylate, tri- fluoro- 1- propine of 3,3,3- and 2- (perfluoro hexyl) ethylmethyl acrylate；
The polyfunctionality unsaturated hydrocarbons analog derivative is：Tri (propylene glycol) diacrylate and diethylene glycol divinyl
Base ether；
2, step (5) keeps reaction cavity vacuum degree to be passed through air to an atmospheric pressure after 160 millitorr 5min.
Aluminum material after above-mentioned plated film and printed wiring board, cold cycling shock-testing effect are as follows：
Claims (7)
1. a kind of method that cycle small-power continuous discharge prepares multi-functional nano protecting coating, it is characterised in that：Including with
Lower step：
(1) base material is placed in the reaction chamber of nano coating Preparation equipment, reaction chamber is continuously vacuumized, by reaction chamber
Interior vacuum degree 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) it is passed through in monomer vapours to reaction chamber, until vacuum degree is 30~300 millitorrs, opens plasma discharge, changed
Learn vapor deposition；
(3) deposition process include pretreatment stage and plating mem stage, pretreatment stage plasma discharge power be 120~
400W, 60~450s of continuous discharging time, subsequently into plating mem stage, adjustment plasma discharge power is 10~75W, is continued
600~3600s of discharge time；
(4) in circulating repetition step (3) pretreatment stage and plating mem stage at least once, in substrate surface chemical vapor deposition system
Standby multifunctionality nano coating；
The monomer vapours ingredient is：
The mixture of at least one single functionality unsaturation fluorocarbon resin 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%；
The single functionality unsaturation fluorocarbon resin 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, tri- fluoro- 1- propine of 3,3,3-, 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；
(5) stop being passed through monomer vapours, be simultaneously stopped plasma discharge, persistently vacuumize, holding reaction chamber vacuum degree is
It is passed through air after 10~200 1~5min of millitorr to an atmospheric pressure, stops the movement of base material, then takes out base material.
2. a kind of cycle small-power continuous discharge according to claim 1 prepares the side of multi-functional nano protecting coating
Method, it is characterised in that：Base material generates movement in reaction chamber in the step (1), and substrate transport form is that base material is relatively anti-
Chamber is answered to carry out straight reciprocating motion or curvilinear motion, the curvilinear motion includes circular motion, ellipse circular motion, planet fortune
Dynamic, spheric motion or the curvilinear motion of other irregular routes.
3. a kind of cycle small-power continuous discharge according to claim 1 prepares the side of multi-functional nano protecting coating
Method, it is characterised in that：Base material is solid material in the step (1), and the solid material is electronic product, electric component, electricity
Subgroup fills semi-finished product, pcb board, metallic plate, polytetrafluoroethylene (PTFE) plank or electronic component, and the substrate surface prepares more work(
Its any interface can be exposed to water environment, mould environment, acid, basic solvent environment, acid, alkaline salt fog ring after energy property nano coating
Border, acidic atmosphere environment, organic solvent impregnate environment, cosmetics environment, sweat environment, cold cycling shock environment or damp and hot friendship
It is used in changing environment.
4. a kind of cycle small-power continuous discharge according to claim 1 prepares the side of multi-functional nano protecting coating
Method, it is characterised in that：The volume of reaction chamber is 50~1000L in the step (1), the temperature control of reaction chamber 30~
60 DEG C, it is 5~300sccm that the inert gas, which is passed through flow,.
5. a kind of cycle small-power continuous discharge according to claim 1 or 4 prepares multi-functional nano protecting coating
Method, it is characterised in that：The reaction chamber is rotator shaped chamber or cube shaped chamber.
6. a kind of cycle small-power continuous discharge according to claim 1 prepares the side of multi-functional nano protecting coating
Method, it is characterised in that：In the step (2)：It is to be atomized monomer by charge pump, volatilize and by low to be passed through monomer vapours
10~200 millitorrs are pressed to introduce reaction chamber, the flow for being passed through monomer is 10~1000 μ L/min.
7. a kind of cycle small-power continuous discharge according to claim 1 prepares the side of multi-functional nano protecting coating
Method, it is characterised in that：In the step (3) and (4), plasma discharge manner is that radio frequency discharge, microwave discharge, intermediate frequency are put
The waveform of electricity, high-frequency discharge or spark discharge, the high-frequency discharge and intermediate frequency electric discharge is sinusoidal or bipolar pulse.
Priority Applications (5)
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| CN201710360355.5A CN107142465B (en) | 2017-05-21 | 2017-05-21 | A method of cycle small-power continuous discharge prepares multi-functional nano protecting coating |
| PCT/CN2017/113189 WO2018214447A1 (en) | 2017-05-21 | 2017-11-27 | Method for preparing multi-functional protective nano coating by means of cyclical low-power continuous discharge |
| US16/688,589 US11270871B2 (en) | 2017-05-21 | 2019-11-19 | Multi-layer protective coating |
| US16/688,845 US11742186B2 (en) | 2017-05-21 | 2019-11-19 | Multi-functional protective coating |
| US17/653,401 US11587772B2 (en) | 2017-05-21 | 2022-03-03 | Multi-layer protective coating |
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| CN201710360355.5A CN107142465B (en) | 2017-05-21 | 2017-05-21 | A method of cycle small-power continuous discharge prepares multi-functional nano protecting coating |
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| CN107142466B (en) * | 2017-05-21 | 2018-05-11 | 江苏菲沃泰纳米科技有限公司 | A kind of method that small-power continuous discharge prepares multi-functional nano protecting coating |
| CN107201511B (en) * | 2017-05-21 | 2018-07-13 | 江苏菲沃泰纳米科技有限公司 | A kind of method that cycle period alternating discharge prepares multi-functional nano protecting coating |
| CN107217243B (en) * | 2017-05-21 | 2018-07-13 | 江苏菲沃泰纳米科技有限公司 | A kind of method that big space rate pulsed discharge prepares multi-functional nano protecting coating |
| CN107201510B (en) * | 2017-05-21 | 2018-09-21 | 江苏菲沃泰纳米科技有限公司 | A kind of method that period alternating discharge prepares multi-functional nano protecting coating |
| CN107142465B (en) * | 2017-05-21 | 2018-07-13 | 江苏菲沃泰纳米科技有限公司 | A method of cycle small-power continuous discharge prepares multi-functional nano protecting coating |
| US11742186B2 (en) | 2017-05-21 | 2023-08-29 | Jiangsu Favored Nanotechnology Co., LTD | Multi-functional protective coating |
| CN108031500B (en) * | 2017-12-27 | 2020-02-11 | 北京百奥芯科技有限公司 | Hydrophobic modification method for micro-channel in micro-fluidic chip |
| JP2021520446A (en) * | 2018-05-04 | 2021-08-19 | ジアンスゥ フェイバード ナノテクノロジー カンパニー リミテッドＪｉａｎｇｓｕ Ｆａｖｏｒｅｄ Ｎａｎｏｔｅｃｈｎｏｌｏｇｙ Ｃｏ．，Ｌｔｄ． | How to protect electrical equipment with nano-coating |
| CN109354941B (en) * | 2018-10-24 | 2020-01-24 | 江苏菲沃泰纳米科技有限公司 | High-adhesion anti-aging nano coating and preparation method thereof |
| CN109354903B (en) * | 2018-10-24 | 2020-01-17 | 江苏菲沃泰纳米科技有限公司 | High-transparency low-chromatic-aberration nano coating and preparation method thereof |
| CN109267041B (en) * | 2018-10-24 | 2020-04-21 | 江苏菲沃泰纳米科技有限公司 | Anti-static liquid-proof nano coating and preparation method thereof |
| CN114438477A (en) * | 2020-11-02 | 2022-05-06 | 江苏菲沃泰纳米科技股份有限公司 | Cyclic coating method, coating and product |
| CN116180029B (en) * | 2023-04-26 | 2023-07-21 | 电子科技大学 | Layered magnetron sputtering coating device for flexible film and preparation method thereof |
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| EP1777691A3 (en) * | 2005-10-21 | 2010-08-11 | Semiconductor Energy Laboratory Co., Ltd. | Display device and method of driving the same |
| GB2434369B (en) * | 2006-01-20 | 2010-08-25 | P2I Ltd | Plasma coated electrical or electronic devices |
| US20080146734A1 (en) * | 2006-11-30 | 2008-06-19 | Youngblood Jeffrey P | Stimuli-responsive polymeric surface materials |
| US8852693B2 (en) * | 2011-05-19 | 2014-10-07 | Liquipel Ip Llc | Coated electronic devices and associated methods |
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| CN103160786A (en) * | 2013-03-07 | 2013-06-19 | 苏州睿研纳米医学科技有限公司 | Nano coating preparation method and antibiosis nano coating prepared by nano coating |
| US9988536B2 (en) * | 2013-11-05 | 2018-06-05 | E I Du Pont De Nemours And Company | Compositions for surface treatments |
| CN107201510B (en) * | 2017-05-21 | 2018-09-21 | 江苏菲沃泰纳米科技有限公司 | A kind of method that period alternating discharge prepares multi-functional nano protecting coating |
| CN107177835B (en) * | 2017-05-21 | 2018-06-19 | 江苏菲沃泰纳米科技有限公司 | A kind of method for recycling big space rate pulsed discharge and preparing multi-functional nano protecting coating |
| CN107142466B (en) * | 2017-05-21 | 2018-05-11 | 江苏菲沃泰纳米科技有限公司 | A kind of method that small-power continuous discharge prepares multi-functional nano protecting coating |
| CN107201511B (en) * | 2017-05-21 | 2018-07-13 | 江苏菲沃泰纳米科技有限公司 | A kind of method that cycle period alternating discharge prepares multi-functional nano protecting coating |
| CN107142465B (en) * | 2017-05-21 | 2018-07-13 | 江苏菲沃泰纳米科技有限公司 | A method of cycle small-power continuous discharge prepares multi-functional nano protecting coating |
| CN107217243B (en) * | 2017-05-21 | 2018-07-13 | 江苏菲沃泰纳米科技有限公司 | A kind of method that big space rate pulsed discharge prepares multi-functional nano protecting coating |
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