CN107142466B - 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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- CN107142466B CN107142466B CN201710361310.XA CN201710361310A CN107142466B CN 107142466 B CN107142466 B CN 107142466B CN 201710361310 A CN201710361310 A CN 201710361310A CN 107142466 B CN107142466 B CN 107142466B
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- 239000011248 coating agent Substances 0.000 title claims abstract description 71
- 238000000034 method Methods 0.000 title claims abstract description 42
- 230000002633 protecting effect Effects 0.000 title claims abstract description 19
- 238000006243 chemical reaction Methods 0.000 claims abstract description 80
- 239000000463 material Substances 0.000 claims abstract description 74
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- 239000011261 inert gas Substances 0.000 claims abstract description 17
- 238000007747 plating Methods 0.000 claims abstract description 17
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- 239000002103 nanocoating Substances 0.000 claims description 22
- 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
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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
- 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
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- 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
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- 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
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- 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
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
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- 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
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- CERQOIWHTDAKMF-UHFFFAOYSA-M Methacrylate Chemical compound CC(=C)C([O-])=O CERQOIWHTDAKMF-UHFFFAOYSA-M 0.000 description 1
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- 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
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- 125000000217 alkyl group Chemical group 0.000 description 1
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- 230000000873 masking effect Effects 0.000 description 1
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- 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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- 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
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- 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
- 238000004078 waterproofing Methods 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)
- 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, the indoor vacuum of 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 movement 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 movement, improves coating deposition efficiency, and improve the uniformity and compactness of coating layer thickness.Prepared coating has the characteristic such as waterproof and dampproof, mould proof, acid and alkali resistance solvent, 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 environment is the most common factor that electronic device is destroyed.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, moisture-proof to electronic product, mould proof,
Corrosion resistance requires more and more stringenter.And in communication field, as technology is constantly progressive, the continuous lifting of communication frequency, to logical
Heat dissipation, the reliability requirement of signal transmission for interrogating equipment are also higher and higher.Can be to circuit therefore, it is necessary to reliable method
Plate and electronic component are effectively protected, 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 based on polymer coating, it is in electronic apparatus, circuit board surface shape
Into protective film can be effectively isolated wiring board, and can protect circuit exempted under corrosive environment erosion, destroy, 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 common circuit board waterproof method, can be effectively isolated wiring board,
And circuit can be protected to exempt from the erosion of adverse circumstances, destroy.In current conformal coat preparation process there is also some problems and
Drawback：Solvent easily causes to damage to circuit board components in liquid phase method；Heat-curable coating high temperature be easy to cause 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 are a kind of polymer of paraxylene, and there is low water, gas permeability, high screen effect can reach
Moisture-proof, waterproof, antirust, the effect of antiacid caustic corrosion.Research finds that Parylene is that deposition produces 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 vapour deposition conformal coat protection failure
In 3~7 micron thickness local corrosion failure easily occurs for coating, and coating layer thickness answers >=30 in the case of high-frequency dielectric loss is not influenced
Micron.The pre-processing requirements for the printed wiring board that parylene coating is protected for needs are higher, such as conductive component, signal transmission
Component, radio frequency component etc., need to do circuit board module masking pretreatment when being vapor-deposited conformal coat, avoid to component
It can impact.This drawback brings very big limitation to the application of parylene coating.Parylene coating preparing raw material is of high cost,
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) is a kind of use etc.
Gas ions activated reactive gas, promotes to be chemically reacted in matrix surface or near surface space, generates the technology of solid film.Deng
Gas ions chemical vapour deposition technique coating has the following advantages
(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 stablized.
(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, effectively avoid the damage of temperature sensitive device.
(6) plasma process can not only prepare thickness as 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 coating performance 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, 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 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
Generally by simply stacking with reference to film forming under the action of continuous discharge, obtained coating general structure is dredged for the chain rupture of activation
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.
Due to plasma density in reaction chamber and chemical raw material density, there are different zones difference, base material transfixion
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.
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
Discharge 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 exports, 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, real by controlling the relation between plasma discharge energy and monomer bond energy
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 net 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 be reacted
The indoor vacuum 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-
Answer and movement is produced in chamber；
(2) monomer vapours are passed through in reaction chamber, is 30~300 millitorrs to vacuum, opens plasma discharge, into
Row chemical vapor deposition, deposition process include 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 for 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, can improve coating and base with the surface of activated substrate
The combination power of material.
The monomer vapours component is：
At least one single functionality unsaturation fluorocarbon resin and at least one polyfunctionality unsaturated hydrocarbons analog derivative it is mixed
Compound, the mass fraction in the monomer vapours shared by polyfunctionality unsaturated hydrocarbons analog derivative are 15~65%；
(3) stop being passed through monomer vapours, while stop 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 movement 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 the continuous discharge of 10~75W of small-power.What the process of continuous plasma discharge depositing produced etc.
Gas ions have deposition film certain etching；Be conducive to accelerate 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.
It is more active by effective output to energy, control molecular structure under low vacuum plasma discharge environment
Chemical bond in monomer is broken, and is formed the product surfaces such as the higher free radical of activity, the free radical and mobile phone of excitation state and 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 movement 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
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) plate 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 immersion environment, cosmetics environment, sweat environment, cold cycling shock environment or damp and hot alternation ring
Used in border.
The volume of reaction chamber is 50~1000L in the step (1), the temperature control of reaction chamber 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.
Monomer vapours are passed through to be atomized, being volatilized by charge pump by monomer and introduced by 10~200 millitorr of low pressure anti-
Chamber is answered, the flow for being passed through monomer is 10~1000 μ L/min；
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, the fluoro- 1- propine of 3,3,3- tri-, 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.
In the step (2), the plasma discharge manner is 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
The plasma that electromagnetic field of high frequency is discharged and produced.Microwave method is the energy excitation plasma using microwave, has energy profit
With it is efficient the advantages of, simultaneously because electrodeless discharge, plasma is pure, be current high quality, high-speed, large area prepare
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 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, an acid and alkali resistance solvent, acid and alkali resistance salt fog, and 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
Degree 75%~95%) etc. characteristic.While possessing above-mentioned barrier propterty, coating layer thickness exists frequency in the case of 1~1000nm
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 the following advantages compared with prior art：
1st, continuous small-power electric discharge is introduced in plating mem stage, can polymerize and carve at the same time during continuous discharge
Lose two processes, when 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, second, plasma can etch the strand of the low chemical bond energy of polymerization rear surface at the same time, while play the role 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 moves in reaction chamber, makes the base material coating film thickness of diverse location
Tend to consistent, solve since different zones monomer density difference causes substrate surface coating layer thickness non-uniform 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, improve deposition efficiency, 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 so as to reduce the discharge of tail gas exhaust, there is weight in actual production efficiency is improved
Big meaning.
4th, the introducing of polyfunctional group cross-linked structure promotes coating densification net structure in microstructure in monomer material
Formation, ensureing 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
Numerous active sites that chain rupture formation occurs in plasma discharge due to 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
Extra crosslinking points are introduced to form cross-linked structure by introducing the other monomers component with polyfunctional group cross-linked structure.Deng
During 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
Into fine and close net structure.
For the coating structure more compared to loose linear components, net structure has more preferably compactness, Neng Gouyou
Effect improves the performance of the anticorrosive environment of film.Under plasma ambient, surface is activated obtaining numerous work plated film basis material
Property site, the living radical of these avtive spots and the monomer material through plasma exciatiaon are mutually tied with stronger chemical bond
Close, form and the elementary reaction of wide variety occurs so that the nano thin-film of basis material has excellent combination power and machinery
Intensity.By controlling different monomers fit system, while regulate and control 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, its environmental corrosion resisting
Comprehensive performance 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, 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 infringement of electronic equipment can be caused.The film plating process of patent of the present invention greatly increases
Nanometer is of great significance in actual production efficiency is improved.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 the equipment such as computer, mobile phone.
It can handle official business easy to user in route.But when it runs into 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 easily short-circuit, and then are damaged.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 the purposes such as demonstration, StoreFront decoration, illumination, warning.Its partial use
The adverse circumstances in face of rainwater or more dust are needed, during such as rainy day, the outdoor LED advertisement screen curtain in market, road surface warning lamp is raw
The LED display control panel in workshop is produced, these adverse circumstances cause LED screen failure, and 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, 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), hearing aid, bluetooth headset：Hearing aid does not have connection, after the coating, Yong Huke with bluetooth headset
To be used within a certain period of time under water environment, such as have a bath, on rainy day, equipment will not be infiltrated because of rainwater to be damaged.
(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, these sensors are using the painting
After layer, can ensure will not cause 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 needing the operation in wet environment, or it is likely encountered common liquid
The fortuitous event such as splash, the equipment of internal light current circuit normal operation can be influenced.
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, 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, seal (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 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, 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
Car electric appliance, such as aviation, automobile, household electrical appliances, the equipment in scientific research field.
Embodiment
With reference to the present invention will be described in detail with 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 reaction chamber
It is continuous to vacuumize, the indoor vacuum of reaction chamber is extracted into 10 millitorrs, is passed through inert gas Ar, opening movement mechanism, makes base material exist
Movement 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 its any interface after mould proof nano coating and can be exposed to GJB150.10A-2009 moulds and surveys
Test ring uses 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 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) 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 include pretreatment stage and plate 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)：
Monomer vapours are passed through to be atomized, being volatilized by charge pump by monomer, 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 component 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 15%；
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 (2) the plasma discharge mode is continuous radio frequency discharge.
(3) plated film terminates, and stopping is passed through starting monomer steam, while stops plasma discharge, persistently vacuumizes, and keeps
Reaction cavity vacuum is 10 millitorrs, and air is passed through after 1min to an atmospheric pressure, 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 indoor vacuum of reaction chamber is extracted into 60 millitorrs, be passed through inert gas He, start motion, carry out base material
Movement；
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 exposed 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 vapour deposition, pretreatment stage power 200W, time 700s, subsequently into plating mem stage, discharge power 30W, time
6000s, the nano coating of acid and alkali resistance environment is prepared in substrate surface chemical vapor deposition.
In step (2)：
Monomer vapours are passed through to be atomized, being volatilized by charge pump by monomer, reaction cavity is introduced by 60 millitorr of low pressure,
The flow for being passed through monomer vapours is 700 μ L/min；
Monomer vapours component 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 35%；
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 (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 stops plasma discharge, persistently vacuumizes, and keeps
Reaction cavity vacuum is 80 millitorrs, and air is passed through after 2min to an atmospheric pressure, 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 indoor vacuum of reaction chamber is extracted into 130 millitorrs, be passed through inert gas Ar, start motion, carry out base material
Movement；
Base material is solid material in step (1), and the solid material is bulk alloy steel plate materials, and the substrate surface
Its any interface can be exposed in organic solvent test environment after preparing organic solvent-resistant immersion and the coating of resistance to cosmetics.
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 vapour deposition, pretreatment stage power 250W, time 580s, subsequently into plating mem stage, discharge power 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)：
Monomer vapours are passed through to be atomized, being volatilized by charge pump by monomer, 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 component 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 (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 stops plasma discharge, persistently vacuumizes, and keeps
Reaction cavity vacuum is 130 millitorrs, and air is passed through after 3min to an atmospheric pressure, 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 indoor vacuum of reaction chamber is extracted into 160 millitorrs, be passed through inert gas He, start motion, carry out base material
Movement；
Base material is solid material in step (1), and the solid material is block aluminum material and pcb board, and the base material
Its any interface can be exposed in hot and cold loop test environment after surface prepares cold-resistant thermal cycle impact coating.
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, movement velocity 20mm/min in step (1).
(2) monomer vapours are passed through in reaction chamber, when vacuum is 190 millitorr, plasma discharge is opened, is changed
Learn vapour deposition, pretreatment stage power 300W, time 350s, subsequently into plating mem stage, discharge power 55W, time
2200s, the nano coating of cold-resistant thermal cycle impact is prepared in substrate surface chemical vapor deposition.
In step (2)：
Monomer vapours are passed through to be atomized, being volatilized by charge pump by monomer, 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 component 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 55%；
The single functionality unsaturation fluorocarbon resin 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 stops plasma discharge, persistently vacuumizes, and keeps
Reaction cavity vacuum is 160 millitorrs, and air is passed through after 4min to an atmospheric pressure, 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 indoor vacuum of reaction chamber is extracted into 200 millitorrs, be passed through inert gas Ar, start motion, carry out base material
Movement；
Base material is solid material in step (1), and the solid material is 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, speed 100mm/min in step (1).
(2) monomer vapours are passed through in reaction chamber, when vacuum is 300 millitorr, plasma discharge is opened, is changed
Learn vapour deposition, pretreatment stage power 400W, time 60s, subsequently into plating mem stage, discharge power 75W, time
600s, the nano coating of wet-heat resisting alternation is prepared in substrate surface chemical vapor deposition.
In step (2)：
Monomer vapours are passed through to be atomized, being volatilized by charge pump by monomer, 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 component 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 (2) plasma discharge mode is spark discharge.
(3) plated film terminates, and stopping is passed through starting monomer steam, while stops plasma discharge, persistently vacuumizes, and keeps
Reaction cavity vacuum is 200 millitorrs, and air is passed through after 5min to an atmospheric pressure, 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 with the processing step that embodiment 1 is basic, and different technological parameters is as follows：
1st, the indoor vacuum 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 electric component, and substrate surface preparation waterproof is resistance to
The environment that its any interface can be exposed to described in International Industry waterproofing grade standard IPX7 after electrical breakdown coating uses.
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 vapour deposition, pretreatment stage power 380W, time 400s, subsequently into plating mem stage, discharge power 20W, time
3600s, the resistance to nano coating being powered under water is prepared in substrate surface chemical vapor deposition.
In step (2)：Monomer vapours are passed through to be atomized, being volatilized by charge pump by monomer, are 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 component 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 48%；
The single functionality unsaturation fluorocarbon resin 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 underwater powered, underwater soaking experiment effect are as follows：
Following table reaches time test used in 1mA for coating manufactured in the present embodiment electric current under different voltages：
| Voltage | 3.8V | 5V | 12.5V |
| Time | >48h | ＞ 24h | ＞ 24h |
It is working properly that IPX 7 tests (underwater 1m submerging test 30min) electric component.
Claims (7)
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 includes pretreatment stage and plating mem stage, pretreatment stage plasma discharge power for 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 component 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, 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 diacrylate neopentyl glycol
Ester；
(3) stop being passed through monomer vapours, while stop 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 movement 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 characterized in that：Base material produces movement 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
Movement 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 characterized in that：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) plate 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 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 characterized in that：The volume of reaction chamber is 50~1000L in the step (1), the temperature control of reaction chamber at 30~60 DEG C,
It is 5~300sccm that the inert gas, which is passed through flow,.
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 characterized in that：In the step (2)：Monomer vapours are passed through to be atomized, being volatilized and by low pressure 10 by charge pump by monomer
~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 characterized in that：In the step (2), plasma discharge manner for 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.
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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 |
| 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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| 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 |
| US11270871B2 (en) | 2017-05-21 | 2022-03-08 | Jiangsu Favored Nanotechnology Co., LTD | Multi-layer protective 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 |
| 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 |
| 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 |
| 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 |
| 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 |
| CN114438478B (en) * | 2022-01-27 | 2024-04-26 | 深圳市技高美纳米科技有限公司 | Preparation method of silicon-based nano coating, silicon-based nano coating and printed circuit board assembly |
| CN115449775B (en) * | 2022-08-25 | 2024-06-25 | 武汉理工大学 | Corrosion-resistant special air pipe with silicon carbide coating coated on inner wall and preparation method thereof |
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| US4382985A (en) * | 1980-10-11 | 1983-05-10 | Daikin Kogyo Co., Ltd. | Process for forming film of fluoroalkyl acrylate polymer on substrate and process for preparing patterned resist from the film |
| CN1367721A (en) * | 1999-09-07 | 2002-09-04 | 宝洁公司 | Process for hydrophobic treatment of water vapour permeable substrates |
| GB0208261D0 (en) * | 2002-04-10 | 2002-05-22 | Dow Corning | An atmospheric pressure plasma assembly |
| CN101369631B (en) * | 2008-09-26 | 2010-11-17 | 电子科技大学 | Organic opto-electronic device with composite protection layer and preparation method thereof |
| US8852693B2 (en) * | 2011-05-19 | 2014-10-07 | Liquipel Ip Llc | Coated electronic devices and associated methods |
| GB201112516D0 (en) * | 2011-07-21 | 2011-08-31 | P2I Ltd | Surface coatings |
| CN203174194U (en) * | 2012-11-12 | 2013-09-04 | 广东世创金属科技有限公司 | Multifunctional plasma body enhanced coat system |
| 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 |
| 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 |
| CN106958012A (en) * | 2017-05-21 | 2017-07-18 | 无锡荣坚五金工具有限公司 | A kind of substrate transport formula plasma discharge prepares the device and method of nano 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 |
| 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 |
| 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 |
| 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 |
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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 |