CN107523808A - A kind of preparation method of organic silicon nano protective coating - Google Patents
A kind of preparation method of organic silicon nano protective coating Download PDFInfo
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- CN107523808A CN107523808A CN201710729754.4A CN201710729754A CN107523808A CN 107523808 A CN107523808 A CN 107523808A CN 201710729754 A CN201710729754 A CN 201710729754A CN 107523808 A CN107523808 A CN 107523808A
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- 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
- C23C16/513—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 using plasma jets
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- 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
- C23C16/448—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 characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials
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Abstract
A kind of preparation method of organic silicon nano protective coating, belong to technical field of plasma, in this method, vacuum in reaction chamber is extracted into 10~200 millitorrs, and is passed through inert gas, opening movement mechanism, base material is set to produce motion, monomer vapours are passed through in reaction chamber, chemical vapor deposition is carried out, organic silicon nano coating is prepared in substrate surface chemical vapor deposition；Monomer vapours composition is：At least one organic silicon monomer and the mixture of at least one polyfunctionality unsaturated hydrocarbons and hydrocarbon derivative containing double bond, Si Cl, Si O C, Si N Si, Si O Si structures or cyclic structure.Traditional hydrocarbon oxygen organic compound monomer is replaced with organic silicon monomer by the present invention, each silicon atom provides at 14 avtive spots, with higher activity, plasma deposition method coating layer thickness can realize controllable precise from nanometer to micron, and solvent need not be used, while it also avoid the deficiencies of liquid phase organic silicon coating method produces waste water, waste liquid, waste gas.
Description
Technical field
The invention belongs to plasma chemical vapor deposition technique field, and in particular to a kind of system of nano protecting coating
Preparation Method.
Background technology
Corrosive atmosphere is the destroyed most common factor of electronic device.Cause because of environmental corrosion solid in electronic device
The phenomena of the failure such as the reduction of burn into conductor/semiconductor insulating properties and short circuit, open circuit or the loose contact of body material.At present, exist
In the product of the hi-tech industries such as national defence, space flight, the ratio that electronic unit occupies is increasing, moistureproof to electronic product, mould proof,
Corrosion resistance requires more and more stricter.And in communication field, as technology is constantly progressive, the continuous lifting of communication frequency, to logical
Interrogate the radiating of equipment, the reliability of signal transmission requires also more and more higher.Therefore, it is necessary to which reliable method can be to circuit
Plate and electronic component are effectively protected, and do not interfere with proper heat reduction and signal transmission again.
Polymer coating due to economic, easy application, it is applied widely the features such as be usually used in the protection of material surface, Ke Yifu
Give the good physics of material, chemical durability.Barrier based on polymer coating, it is in electronic apparatus, circuit board surface shape
Into diaphragm can be effectively isolated wiring board, and can protection circuit erosion is exempted under corrosive environment, is destroyed, so as to improve electricity
The reliability of sub- device, increase its safety coefficient, and ensure its service life, be 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, it is a kind of conventional circuit board waterproof method, wiring board can be effectively isolated,
And can protection circuit exempt from adverse circumstances erosion, 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 easily causes device failure；Light is consolidated
Change coating and be difficult to closed device inside.A kind of conformal parylene coating of HZO companies of U.S. development and application, Parylene apply
Layer is a kind of polymer of paraxylene, and there is low water, gas permeability, high screen effect can reach protection against the tide, waterproof, prevent
Rust, the effect of antiacid caustic corrosion.Research finds that Parylene is that deposition produces under vacuum conditions, can apply and be applied in liquid
Expect the protection of field such as high-frequency circuit, pole light current streaming system that can not be related to.Thin polymer film coating layer thickness is to influence poly- pair
The main reason for dimethylbenzene vapour deposition conformal coat protection failure, printed circuit board assembly polymer thin membrane coat is micro- 3~7
Local corrosion failure easily occurs for meter Hou Du, and coating layer thickness should be >=30 microns in the case of high-frequency dielectric loss is not influenceed.Parylene
The pre-processing requirements for the printed substrate that coating protects for needs are higher, such as conductive component, signal transmission assembly, radio frequency group
Part etc., need to do circuit board module masking pretreatment when being vapor-deposited conformal coat, avoid impacting assembly property.
This drawback brings very big limitation to the application of parylene coating.Parylene coating preparing raw material cost is high, coating prepares bar
Part harsh (high temperature, condition of high vacuum degree requirement), rate of film build are low, it is difficult to extensive use.In addition, thick coating is easily caused weak heat-dissipating, letter
Number transmission barrier, holiday the problems such as increasing.
Plasma activated chemical vapour deposition (plasma chemical vapor deposition, PCVD) is a kind of use etc.
Gas ions activated reactive gas, promote to be chemically reacted in matrix surface or near surface space, generate the technology of solid film.Deng
Gas ions chemical vapour deposition technique coating has advantages below：
(1) it is dry process, generation film is uniformly pin-free.
(2) chemistry such as the solvent resistance of plasma polymerization film, chemical resistance, heat resistance, abrasion resistance properties, physics
Property is stable.
(3) plasma polymerization film and matrix gluing are good.
(4) it may be made as homogeneous film in the substrate surface of concavo-convex irregular.
(5) coating preparation temperature is low, can be carried out under normal temperature condition, 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.
Base material is all fixed in existing plasma chemical vapor deposition coating preparation process, the motion 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 coating general structure that the chain rupture of activation typically, with reference to film forming, is obtained in the presence of continuous discharge by simply stacking is dredged
Pine, or even powdered degree are high, are unfavorable for the formation of the microcosmic compact texture of coating, therefore, the waterproof of coating, protection against the tide, it is corrosion-resistant,
The barrier propterties such as solvent resistant are poor.
Because different zones difference, base material transfixion be present in plasma density in reaction chamber and chemical raw material density
Some regions coating deposition rate can be caused slow, low production efficiency, but also uniformity be present and what compactness differed greatly shows
As.
In addition, most of plasma coatings are traditional hydrocarbon oxygen organic compound at present, it is organic compared to these tradition
Coating, organic silicon coating have the characteristics that the feature of environmental protection, hardness are high, wearability is good, good insulating, got in electronic product sector application
Come wider.Organic silicon monomer itself is nontoxic, and will not be decomposed into poisonous and harmful substance, monomer polymerization after, in polymer coating by
In inorganic SiO can be formed with silicon oxygen bond or in the coating2Nano particle, make it have high hardness, good insulating properties and
Heat resistance.But current most of organic silicon coatings are obtained by liquid phase method.Organic silicon monomer is hydrolyzed in the solution
After form colloidal sol, sol coating, finally by heat cure, one layer of dense coating is formed on model machine surface on processed exemplar.
Coating layer thickness is usually several microns to tens microns.Liquid phase organic silicon coating technology than traditional liquid phase coating technology although have
More preferable environment-friendly type, but there is also many deficiencies：
(1) water or organic matter is needed to use to have a negative impact as solvent, these solvents to electronic product；
(2) waste water, waste liquid and waste gas be present, it is necessary to be post-processed；
(3) coating layer thickness poor controllability, it is difficult to which Nano grade is arrived in control.
The content of the invention
The present invention provides a kind of preparation method of organic silicon nano protective coating to solve above-mentioned technical problem.This was prepared
Cheng Zhong, kinetic characteristic and plasma discharge energy the combination linkage of base material, while plasma discharge energy exports, base material
Keep motion state.It is extra to introduce that other monomers component with polyfunctional group cross-linked structure is introduced by energy of plasma
Crosslinking points to form cross-linked structure.Plasma discharge produces plasma, by controlling plasma discharge energy and list
Relation between body bond energy, realize that the effective activation of the low temperature plasma active group higher to energy in monomer component obtains
Avtive spot, meanwhile, the additional active point being introduced into is cross-linked with each other polymerization under plasma ambient, forms fine and close network structure.
In addition, traditional hydrocarbon oxygen organic compound monomer is replaced with organic silicon monomer by the present invention, due to organosilicon list
Hydrolysis or alcoholysis easily occur for the functional group being connected in body with silicon, and obtained structure is very easy to that condensation reaction occurs, and mutually
Crosslinking, each silicon atom provide at 1-4 avtive spot, have higher activity, therefore, in the case of low-temperature plasma more
Easily generate free radical and cross-linking reaction occurs, form the cross-linking compounds of densification, improve barrier propterty.Plasma deposition method
Coating layer thickness can realize controllable precise from nanometer to micron, and need not use solvent, while it is organic to it also avoid liquid phase
Silicon coating method produces the deficiencies of waste water, waste liquid, waste gas.
The technical solution adopted in the present invention is as follows：
A kind of preparation method of organic silicon nano protective coating, it is characterised in that：Comprise the following steps：
(1) pre-treatment：
Base material is placed in the reaction chamber of nano coating Preparation equipment, reaction chamber continuously vacuumized, by reaction chamber
Indoor vacuum is extracted into 10~200 millitorrs, and is passed through inert gas He, Ar or He and Ar mixed gas, opening movement mechanism,
Base material is set to produce motion in reaction chamber；
(2) prepared by organic silicon coating：
Monomer vapours are passed through in reaction chamber, is 30~300 millitorrs to vacuum, opens plasma discharge, carry out
Chemical vapor deposition, organic silicon nano coating is prepared in substrate surface chemical vapor deposition；
The monomer vapours composition is：
At least one organic silicon monomer containing double bond, Si-Cl, Si-O-C, Si-N-Si, Si-O-Si structure or cyclic structure
With at least one polyfunctionality unsaturated hydrocarbons and the mixture of hydrocarbon derivative, polyfunctionality unsaturated hydrocarbons in the monomer vapours
And the mass fraction shared by hydrocarbon derivative is 15~65%；
Monomer vapours are passed through to be atomized, being volatilized by charge pump by monomer and introduced by the millitorr of low pressure 10~200 anti-
Chamber is answered, the flow for being passed through monomer vapours is 10~1000 μ L/min；
(3) post-process：
Stopping is passed through monomer vapours, while stops plasma discharge, persistently vacuumizes, and holding reaction chamber vacuum is
Air is passed through after 10~200 1~5min of millitorr to an atmospheric pressure, stops the motion of base material, then takes out base material；
Or stop being passed through monomer vapours, while stop plasma discharge, air or inertia are filled with into reaction chamber
Then gas is evacuated to 10-200 millitorrs, carries out above-mentioned inflation and vacuum step at least one to pressure 2000-5000 millitorrs
It is secondary, air is passed through to an atmospheric pressure, is stopped the motion of base material, is then taken out base material.
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 higher product surface such as free radical, the free radical and mobile phone of excitation state of activity and is lived
Change group triggers polymerization to form nano water-proof film by way of chemical bonds, and forming organic silicon nano in substrate surface applies
Layer.Further, since the group being connected in organic silicon monomer with silicon has higher activity, it is easier in the case of low-temperature plasma
Simultaneously cross-linking reaction occurs for generation free radical, forms the cross-linking compounds of densification.
Base material produces motion in reaction chamber in the step (1), and substrate transport form is base material relative response chamber
Straight reciprocating motion or curvilinear motion are carried out, the curvilinear motion includes circular motion, ellipse circular motion, planetary motion, sphere
Motion or the curvilinear motion of other irregular routes.
Base material is solid material in the step (1), and the solid material is electronic product, electric component, Electronic Assemblies
Semi-finished product, pcb board, metallic plate, polytetrafluoroethylene (PTFE) sheet material or electronic component, and the substrate surface prepares organic silicon nano
Its any interface can be exposed to water environment, mould environment, acid, basic solvent environment, sour, alkaline salt mist environment, acidity after coating
Atmospheric environment, organic solvent immersion environment, cosmetics environment, sweat environment, cold cycling shock environment or damp and hot alternation environment
Middle use.
Reaction chamber is rotator shaped chamber or cube shaped chamber in the step (1), and volume is 50~1000L,
For the temperature control of reaction chamber at 30~60 DEG C, it is 5~300sccm that the inert gas, which is passed through flow,.
In the step (2)：Plasma discharge, carry out chemical vapor deposition, deposition process plasma discharge mistake
Journey includes small-power continuous discharge, pulsed discharge or cycle alternating discharge.
The deposition process plasma discharge process is small-power continuous discharge, specifically includes following deposition process extremely
Less once：
Deposition process include pretreatment stage and plating mem stage, pretreatment stage plasma discharge power be 150~
600W, 60~450s of continuous discharging time, subsequently into plating mem stage, adjustment plasma discharge power is 10~150W, is held
Continuous 600~3600s of discharge time.
The deposition process plasma discharge process is pulsed discharge, specifically includes following deposition process at least one
It is secondary：
Deposition process include pretreatment stage and plating mem stage, pretreatment stage plasma discharge power be 150~
600W, 60~450s of continuous discharging time, subsequently into plating mem stage, plating mem stage is pulsed discharge, 10~300W of power, when
Between 600s~3600s, the frequency of pulsed discharge is 1~1000HZ, and the dutycycle of pulse is 1:1~1:500.
The deposition process plasma discharge process is cycle alternating discharge, specifically includes following deposition process at least
Once：
Deposition process include pretreatment stage and plating mem stage, pretreatment stage plasma discharge power be 150~
600W, 60~450s of continuous discharging time, subsequently into plating mem stage, plated film phase plasma is cycle alternately change electric discharge
Output, 10~300W of power, time 600s~3600s, alternative frequency 1-1000Hz, the alternately change electric discharge of plasma cycle
Output waveform is zig-zag, sinusoidal waveform, square-wave waveform, current waveform in full-wave rectifier or half wave rectification wave.
The organic silicon monomer bag containing double bond, Si-Cl, Si-O-C, Si-N-Si, Si-O-Si structure or cyclic structure
Include：
Organic silicon monomer containing double bond structure：Allyltrimethoxysilanis, VTES, vinyl three
Methyl-monosilane, 3- cyclobutenyls trimethyl silane, vinyl tributyl ketoximyl silane, tetramethyl divinyl disiloxane, 1,2,
2- trifluoro vinyl tri-phenyl-silanes；
The organic silicon monomer of the key containing Si-Cl：Tri-phenyl chloride, methylvinyldichlorosilane, trifluoro propyl trichlorine silicon
Alkane, trifluoropropylmethyldichlorosilane, 3,5-dimethylphenyl chlorosilane, tributyl chlorosilane, benzyl dimethyl chlorosilane；
The organic silicon monomer of the structure containing Si-O-C：Tetramethoxy-silicane, trimethoxy hydrogen siloxane, n-octyl triethoxy
Silane, phenyl triethoxysilane, vinyl three (2- methoxy ethoxies) silane, triethylvinylsilane silane, Hexaethyl ring
Trisiloxanes, 3- (methacryloxypropyl) propyl trimethoxy silicane, phenyl three (trimethylsiloxane group) silane, diphenyl two
Ethoxysilane, dodecyltrimethoxysilane, n-octytriethoxysilane, dimethoxysilane, 3- chloropropyl front threes
TMOS；
The organic silicon monomer of the structure containing Si-N-Si or Si-O-Si：Hexamethyldisilane base amine, the silane ammonia of pregnancy basic ring three
Base, HMDS, hexamethyldisiloxane；
Organic silicon monomer containing cyclic structure：Hexamethyl cyclotrisiloxane, octamethylcy-clotetrasiloxane, the silicon of hexaphenyl ring three
Oxygen alkane, decamethylcyclopentaandoxane, octaphenylcyclotetrasiloxane, triphenyl silicol, Diphenylsilanediol, chromic acid are double
(trityl silylation) ester, trifluoro propyl methyl cyclotrisiloxane, the silicon of 2,2,4,4- tetramethyl -6,6,8,8- tetraphenyls ring four
Oxygen alkane, t etram-ethyltetravinylcyclotetrasiloxane, 3- glycydoxies triethoxysilane, γ-glycidol ether
Oxygen propyl trimethoxy silicane；
The polyfunctionality unsaturated hydrocarbons and hydrocarbon derivative include：
1,3- butadiene, isoprene, 1,4- pentadienes, ethoxylated trimethylolpropane triacrylate, two contractings three
Propylene glycol diacrylate, polyethyleneglycol diacrylate, 1,6 hexanediol diacrylate, ethylene glycol diacrylate, two
Ethylene glycol divinyl ether or diacrylic acid pentyl diol ester.
In the step (2), plasma discharge manner be radio frequency discharge, microwave discharge, intermediate frequency electric discharge, high-frequency discharge,
The waveform of spark discharge, the high-frequency discharge and intermediate frequency electric discharge is sinusoidal or bipolar pulse.Radio frequency plasma is to utilize height
Frequency electromagnetic field discharges and caused plasma.Microwave method is the energy excitation plasma using microwave, has energy utilization
The advantages of efficiency high, simultaneously because electrodeless discharge, plasma is pure, is prepared by current high quality, high-speed, large area
Excellent process.
In coating preparation process, kinetic characteristic and plasma discharge energy the combination linkage of base material.Preparation process is medium
While plasma discharge, base material produces motion, improves coating deposition efficiency, and improve uniformity and the cause of coating layer thickness
Close property.
Prepared coating has waterproof and dampproof, 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~+100 DEG C), wet-heat resisting alternation is (wet
Degree 75%~95%) etc. characteristic.For electronic product (mobile phone, earphone, Intelligent bracelet etc.), unmanned plane etc., coating is on possessing
While stating barrier propterty, thickness is in the case of 1~1000nm, to radio frequency communication signal of the frequency in the range of 10M~8G
Influence to be less than 5%, and coating does not interfere with the original heat dispersion of electronic product and electronic product in itself to current conduction
Requirement.
The above-mentioned technical proposal of the present invention has advantages below compared with prior art：
1st, plasma chemical vapor deposition technique method, it is more more environmentally friendly than liquid phase method three proofings coating coating method；And compare
Parylene method is deposited, depositing temperature is low, speed faster, the controllability of coating structure and composition it is strong, the alternative of monomer is strong.
2nd, base material moves in reaction chamber, the base material coating film thickness of diverse location is tended to consistent, solve by
In different zones monomer density difference causes substrate surface coating layer thickness uneven in reaction chamber the problem of.In preparation process,
Kinetic characteristic and plasma discharge energy the combination linkage of base material, while discharge energy exports, base material is moved, and is improved
Deposition efficiency, so as to get organic silicon nano protective coating compactness significantly improve.Simultaneously because the raising of deposition efficiency, single
The dosage of the chemical monomer raw material of body steam also only other in the prior art dosage 10%~15%, so as to reduce tail
The discharge of gas waste gas, it is more green, it is significant in actual production efficiency is improved.
3rd, general plasma polymerization selects the hydrocarbon oxygen organic compound monomer of single functionality, obtains that there is certain crosslinking to tie
Structure coating.Cross-linked structure be due to monomer occur in plasma discharge chain rupture formation numerous active sites pass through interactive connection
Mode and form cross-linked structure.But this cross-linked structure is more loose, containing more linear components, solvent resistant infiltration and
Dissolubility is poor.
Compared to traditional single functionality Orqanics Monomer, under plasma conditions, being connected with silicon in organic silicon monomer
Functional group condensation reaction can occur between each other, therefore, solid netted crosslinking can occur between monomer and monomer, one can be entered
Step improves compactness, wearability and the corrosion resistance of coating.
(1) organic silicon monomer containing double bond, Si-Cl, Si-O-C, Si-N-Si, Si-O-Si structure or cyclic structure is utilized
The hydrocarbon oxygen organic compound monomer of traditional single functionality is substituted, under plasma condition, due to the functional group that is connected with silicon all
With higher reactivity, therefore, these organic silicon monomers have more cross-linking avtive spots；
(2) extra crosslinking points are introduced to be formed by introducing the other monomers component with polyfunctional group cross-linked structure
Cross-linked structure.,, will be single by effective control to energy and output under low temperature plasma effect during plasma discharge
The higher active group of energy interrupts to form active site in body component, and the additional active point being introduced into is mutual under plasma ambient
Cross-linked polymeric, form fine and close network structure.
For the coating structure more compared to loose linear components, network structure has more excellent compactness, Neng Gouyou
Effect improves the performance of the anticorrosive environment of film.Under plasma ambient, surface is activated obtaining numerous work plated film matrix 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 matrix material has excellent adhesion 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, obtain the structure for having the bottom dense skin roughness of special microstructure big, its environmental corrosion resisting
Combination property improve 45%~60%.Particularly, the organic silicon coating hardness of same thickness is higher 1-2 than conventional coatings hardness
Individual grade, salt spray resistance ability improve 30-50%.
4th, 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, both ensure that the hydrophobicity of film, and the resistance to environment for improving the products such as electronic product again is rotten
The performance of erosion.
Electronic equipment in daily life is easily damaged by the erosion of corrosive environment, is substantially at during use
In corrosive environment, if things go on like this, the irremediable infringement of electronic equipment can be caused.The film plating process of patent of the present invention greatly increases
Nanometer is significant in actual production efficiency is improved.Coating improves production in the service life of corrosive atmosphere
The protecting effect of product.It is mainly used in following product：
(1) portable equipment keyboard：Portable keyboard has the characteristics of small and light, is usually used in the equipment such as computer, mobile phone.Its
User can be easy to be handled official business 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, rainwater,
Sweat is impregnated with, and keyboard is easily short-circuit, and then damages.After carrying out plated film to it using such nano coating, when can protect
Hinder 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, the LED of workshop
Display screen control panel, road surface warning lamp, trade mark logo LED module, these adverse circumstances cause LED screen failure, and
And easy dust stratification, easy cleaning, after the nano coating, not can effectively solve the problem that above mentioned problem.
(3) intelligent fingerprint lock：Fingerprint Lock is intelligent lock, and it has gathered computer information technology, electronic technology, mechanical skill
Art 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) audiphone, bluetooth earphone, VR/AR glasses：For this kind of product after using the coating, user can be in a timing
It is interior to be used under water environment, such as have a bath, on rainy day, equipment will not infiltrate because of rainwater be damaged.Meanwhile applying coating
Afterwards, product has the function of certain salt spray resistance and resistance to sweat, ensures also can when user perspires in motion process
Normal use product.
(5) operative sensor：Operative sensor needs to work in liquid environment, such as hydraulic pressure, oil pressure sensor, Yi Jishui
The sensor used in lower implement, and working environment often meet the sensor of water, and these sensors are using the coating
Afterwards, can ensure will not cause faulty sensor because of liquid intrusion plant equipment internal structure.
(6) most of 3C Products：Such as mobile phone, computer, tablet personal computer, digital camera, PSP.
(7) unmanned plane product (agricultural/civilian/police)：Unmanned plane can run into different weather conditions in normal work,
Corrosive gas environment, rainy day and wet environment are inevitable, or even the contact with some agricultural chemicals reagents.Unmanned plane product
After the coating, its normal use under rainy day even soaked etc. environment can be effectively protected, without interiors of products
Water inlet causes wiring board short circuit or flies the phenomenon of control failure.
(8) other equipment for needing waterproof：Including needing the operation in wet environment, or it is likely encountered common liquid and sprinkles
The fortuitous event such as spill, the equipment of internal light current circuit normal operation can be influenceed.
The related production that organic silicon 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, audiphone.5 precision instruments and optical device：Mechanical watch, microscope.6 agricultures
With/police/civilian unmanned plane.
Acid and alkali resistance solvent, acid and alkali resistance salt fog, acid resistance air：
1 house inside gadget：Wallpaper, ceramic tile.2 safety devices：Acidproof (alkali) gloves, acidproof (alkali) protective garment.3 plant equipment
And pipeline：Flue desulfurization equipment, seal (acid/base lubricating oil), pipeline, valve, Large Diameter Pipeline sea conveyance conduit liner etc.
Place.4 various reactors, reactor.The production of 5 chemicals, storage；Sewage disposal, aeration tank；6 is other：Soda acid workshop, alkali prevention
The every profession and trades such as Aero-Space, electricity power, Ferrous Metallurgy, petrochemical industry, medical treatment, storage container, statue (reduce acid rain to its
Corrosion), sensor (under acid/base environment).
Organic solvent-resistant soaks, resistance to cosmetics, resistance to sweat：
1 such as alkane, alkene, alcohol, aldehyde, amine, ester, ether, ketone, aromatic hydrocarbon, hydrogenate hydrocarbon, terpene hydrocarbon, halogenated hydrocarbons, jeterocyclic chemistry
Thing, nitrogen-containing compound and sulfur-containing compound solvent etc.；2 toiletry bag packaging containers；3 Fingerprint Locks, earphone.
Cold-resistant thermal cycle impact (- 40 DEG C~+100 DEG C), wet-heat resisting alternation (humidity 75%~95%),：Electrician, electronics,
Car electrics, such as aviation, automobile, household electrical appliances, the equipment in scientific research field.
Embodiment
The present invention is described in detail with reference to specific embodiment, but the invention is not limited in specific embodiment.
Embodiment 1
A kind of preparation method of organic silicon nano protective coating, comprises the following steps：
(1) pre-treatment：
Base material is placed in the reaction chamber of nano coating Preparation equipment, closed reaction chamber is simultaneously continuously taken out to reaction chamber
Vacuum, the vacuum in reaction chamber is extracted into 10 millitorrs, is passed through inert gas Ar, opening movement mechanism, is reacting base material
Motion is produced in chamber；
Base material is solid material in step (1), and the solid material is block polytetrafluoroethylene (PTFE) sheet material.
Reaction chamber is rotator shaped chamber in step (1), and the volume of reaction chamber is 50L, the temperature control of reaction chamber
For system at 30 DEG C, the flow for being passed through inert gas is 5sccm.
Base material produces motion in reaction chamber in step (1), and substrate transport form is carried out for base material relative response chamber
Circular motion, rotating speed are 1 turn/min.
(2) prepared by organic silicon coating：
Monomer vapours are passed through in reaction chamber, is 30 millitorrs to vacuum, opens plasma discharge, carry out chemical gas
Mutually deposit, organic silicon nano coating is prepared in substrate surface chemical vapor deposition；
The monomer vapours composition is：
A kind of organic silicon monomer and the mixture of two kinds of polyfunctionality unsaturated hydrocarbons and hydrocarbon derivative containing double bond structure,
Polyfunctionality unsaturated hydrocarbons and the mass fraction shared by hydrocarbon derivative are 15% in the monomer vapours；
In the step (2)：Plasma discharge, carry out chemical vapor deposition, deposition process plasma discharge mistake
Journey is small-power continuous discharge, specifically includes following deposition process once：
Deposition process includes pretreatment stage and plating mem stage, and pretreatment stage plasma discharge power is 150W, is held
Continuous discharge time 450s, subsequently into plating mem stage, adjustment plasma discharge power is 150W, continuous discharging time 600s.
In step (2)：
Monomer vapours are passed through to be atomized, being volatilized by charge pump by monomer, reaction chamber is introduced by the millitorr of low pressure 10,
The flow for being passed through monomer vapours is 1000 μ L/min；
A kind of organic silicon monomer containing double bond structure is：VTES；
Described two polyfunctionality unsaturated hydrocarbons and hydrocarbon derivative are：1,3-butadiene, ethylene glycol diacrylate；
Step (2) the plasma discharge mode is radio frequency discharge.
(3) post-process：
Stopping is passed through monomer vapours, while stops plasma discharge, persistently vacuumizes, and holding reaction chamber vacuum is
Air is passed through after 10 millitorr 1min to an atmospheric pressure, stops the motion of base material, then takes out base material.
Obtained deposition has the polyfluortetraethylene plate of organic silicon nano coating, is tested by GJB150.10A-2009 mould proof
Performance, effect are as follows：
Embodiment 2
A kind of preparation method of organic silicon nano protective coating, comprises the following steps：
(1) pre-treatment：
Base material is placed in nano coating Preparation equipment reaction chamber, closed reaction chamber is simultaneously continuously taken out true to reaction chamber
Sky, the vacuum in reaction chamber is extracted into 60 millitorrs, is passed through inert gas He, started motion, moved base material；
Base material is solid material in step (1), and the solid material is block aluminium alloy anode oxide material.
Reaction chamber is cube shaped chamber in step (1), and the volume of reaction chamber is 250L, the temperature control of reaction chamber
For system at 40 DEG C, the flow for being passed through inert gas 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) prepared by organic silicon coating：
Monomer vapours are passed through in reaction chamber, is 110 millitorrs to vacuum, opens plasma discharge, carry out chemistry
Vapour deposition, organic silicon nano coating is prepared in substrate surface chemical vapor deposition；
The monomer vapours composition is：
The mixing of the organic silicon monomer and three kinds of polyfunctionality unsaturated hydrocarbons and hydrocarbon derivative of two kinds of structures containing Si-Cl
Thing, polyfunctionality unsaturated hydrocarbons and mass fraction shared by hydrocarbon derivative are 29% in the monomer vapours；
In the step (2)：Plasma discharge, carry out chemical vapor deposition, deposition process plasma discharge mistake
Journey is small-power continuous discharge, specifically includes following deposition process three times：
Deposition process includes pretreatment stage and plating mem stage, and pretreatment stage plasma discharge power is 600W, is held
Continuous discharge time 60s, subsequently into plating mem stage, adjustment plasma discharge power is 10W, continuous discharging time 3600s.
In step (2)：
Monomer vapours are passed through to be atomized, being volatilized by charge pump by monomer, reaction chamber is introduced by the millitorr of low pressure 60,
The flow for being passed through monomer vapours is 700 μ L/min；
The organic silicon monomer of described two structures containing Si-Cl is：Tri-phenyl chloride and trifluoropropylmethyldichlorosilane.
Three kinds of polyfunctionality unsaturated hydrocarbons and hydrocarbon derivative are：1,4- pentadienes, the propylene of tripropylene glycol two
Acid esters, polyethyleneglycol diacrylate；
Step (2) plasma discharge mode is discharged for intermediate frequency.
(3) post-process：
Stopping is passed through monomer vapours, while stops plasma discharge, persistently vacuumizes, and holding reaction chamber vacuum is
80 millitorrs, air is passed through to an atmospheric pressure after 2min, then takes out base material.
After above-mentioned block aluminium alloy anode oxide material surface prepares organic silicon coating, in acid, alkali test environment
Its acid and alkali resistance is tested, effect is as follows：
Embodiment 3
A kind of preparation method of organic silicon nano protective coating, comprises the following steps：
(1) pre-treatment：
Base material is placed in the reaction chamber of nano coating Preparation equipment, closed reaction chamber is simultaneously continuously taken out to reaction chamber
Vacuum, the vacuum in reaction chamber is extracted into 130 millitorrs, is passed through inert gas Ar and He mixed gas, start fitness machine
Structure, moved base material；
Base material is solid material in step (1), and the solid material is bulk alloy steel plate materialses and PC plastic plate.
Reaction chamber is rotator shaped chamber in step (1), and the volume of reaction chamber is 480L, the temperature control of reaction chamber
For system at 50 DEG C, the flow for being passed through inert gas is 60sccm,.
Base material carries out circular motion in step (1), and rotating speed is 3 turns/min.
(2) prepared by organic silicon coating：
Monomer vapours are passed through in reaction chamber, is 170 millitorrs to vacuum, opens plasma discharge, carry out chemistry
Vapour deposition, organic silicon nano coating is prepared in substrate surface chemical vapor deposition；
The monomer vapours composition is：
The organic silicon monomer and the mixture of a kind of polyfunctionality unsaturated hydrocarbons and hydrocarbon derivative of three kinds of Si-O-C structures,
Polyfunctionality unsaturated hydrocarbons and the mass fraction shared by hydrocarbon derivative are 42% in the monomer vapours；
Plasma discharge, chemical vapor deposition is carried out, deposition process plasma discharge process is pulsed discharge, tool
Body includes following deposition process three times：
Deposition process includes pretreatment stage and plating mem stage, and pretreatment stage plasma discharge power is 150W, is held
Continuous discharge time 450s, subsequently into plating mem stage, plating mem stage is pulsed discharge, power 300W, time 600s, pulsed discharge
Frequency be 1HZ, the dutycycle of pulse is 1:1.
In step (2)：
Monomer vapours are passed through to be atomized, being volatilized by charge pump by monomer, reaction chamber is introduced by the millitorr of low pressure 130
Room, the flow for being passed through monomer vapours are 550 μ L/min；
The organic silicon monomer of three kinds of structures containing Si-O-C is：Phenyl triethoxysilane, triethylvinylsilane silane,
Hexaetcycletrisiloxane；
The polyfunctionality unsaturated hydrocarbons analog derivative is：1,6 hexanediol diacrylate；
Step (2) plasma discharge mode is high-frequency discharge, and the waveform of high-frequency discharge is bipolar pulse.
(3) stop being passed through monomer vapours, while stop plasma discharge, persistently vacuumize, keep reaction chamber vacuum
Spend for 160 millitorrs, be passed through air to an atmospheric pressure after 3min, then take out base material.
After above-mentioned alloy-steel plate material and PC plastic plate deposition organic silicon coating, in organic solvent Soak Test its resistance to have
Solvent performance, effect are as follows：
Embodiment 4
A kind of preparation method of organic silicon nano protective coating, comprises the following steps：
(1) pre-treatment：
Base material is placed in nano coating Preparation equipment reaction chamber, closed reaction chamber is simultaneously continuously taken out true to reaction chamber
Sky, the vacuum in reaction chamber is extracted into 160 millitorrs, is passed through inert gas He, started motion, transported base material
It is dynamic；
Base material is solid material in step (1), and the solid material is block aluminum material and pcb board.
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) prepared by organic silicon coating：
Monomer vapours are passed through in reaction chamber, is 210 millitorrs to vacuum, opens plasma discharge, carry out chemistry
Vapour deposition, organic silicon nano coating is prepared in substrate surface chemical vapor deposition；
The monomer vapours composition is：
The organic silicon monomer and four kinds of polyfunctionality unsaturated hydrocarbons and hydro carbons of two kinds of structures containing Si-N-Si or Si-O-Si spread out
The mixture of biology, polyfunctionality unsaturated hydrocarbons and mass fraction shared by hydrocarbon derivative are 65% in the monomer vapours；
Plasma discharge, chemical vapor deposition is carried out, deposition process plasma discharge process is pulsed discharge, tool
Body includes following deposition process once：
Deposition process includes pretreatment stage and plating mem stage, and pretreatment stage plasma discharge power is 600W, is held
Continuous discharge time 60s, subsequently into plating mem stage, plating mem stage is pulsed discharge, power 10W, time 3600s, pulsed discharge
Frequency be 1000HZ, the dutycycle of pulse is 1:500.
In step (2)：
Monomer vapours are passed through to be atomized, being volatilized by charge pump by monomer, reaction chamber is introduced by the millitorr of low pressure 160
Room, the flow for being passed through monomer vapours are 220 μ L/min；
The organic silicon monomer of described two structures containing Si-N-Si or Si-O-Si is：The silane amino of pregnancy basic ring three, pregnancy
Base disilazane；
Four kinds of polyfunctionality unsaturated hydrocarbons and hydrocarbon derivative are：Isoprene, ethoxylated trimethylolpropane
Triacrylate, tri (propylene glycol) diacrylate, polyethyleneglycol diacrylate；
Step (2) plasma discharge mode is microwave discharge.
(3) post-process：
Stopping is passed through monomer vapours, while stops plasma discharge, persistently vacuumizes, and holding reaction chamber vacuum is
200 millitorrs, air is passed through to an atmospheric pressure after 5min, then takes out base material.
Block aluminum material and pcb board after above-mentioned plated film, cold cycling is carried out in hot and cold loop test environment
Impact test, test effect are as follows：
Embodiment 5
A kind of preparation method of organic silicon nano protective coating, comprises the following steps：
(1) pre-treatment：
Base material is placed in nano coating Preparation equipment reaction chamber, closed reaction chamber is simultaneously continuously taken out true to reaction chamber
Sky, the vacuum in reaction chamber is extracted into 200 millitorrs, is passed through inert gas Ar, started motion, transported base material
It is dynamic；
Base material is solid material in step (1), and the solid material is electronic component.
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) prepared by organic silicon coating：
Monomer vapours are passed through in reaction chamber, is 300 millitorrs to vacuum, opens plasma discharge, carry out chemistry
Vapour deposition, organic silicon nano coating is prepared in substrate surface chemical vapor deposition；
The monomer vapours composition is：
Three kinds of organic silicon monomers and the mixture of five kinds of polyfunctionality unsaturated hydrocarbons and hydrocarbon derivative containing cyclic structure,
Polyfunctionality unsaturated hydrocarbons and the mass fraction shared by hydrocarbon derivative are 52% in the monomer vapours；
Plasma discharge, carries out chemical vapor deposition, and deposition process plasma discharge process is alternately to put in the cycle
Electricity, specifically includes following deposition process four times：
Deposition process includes pretreatment stage and plating mem stage, and pretreatment stage plasma discharge power is 150W, is held
Continuous discharge time 450s, subsequently into plating mem stage, plated film phase plasma is alternately to change electric discharge output, power in the cycle
300W, time 600s, alternative frequency 1Hz, the plasma cycle, alternately change electric discharge output waveform was zig-zag；
In step (2)：
Monomer vapours are passed through to be atomized, being volatilized by charge pump by monomer, reaction chamber is introduced by the millitorr of low pressure 200
Room, the flow for being passed through monomer vapours are 10 μ L/min；
Three kinds of organic silicon monomers containing cyclic structure are：Double (the trityl silane of octaphenylcyclotetrasiloxane, chromic acid
Base) ester, t etram-ethyltetravinylcyclotetrasiloxane；
Five kinds of polyfunctionalities unsaturated hydrocarbons analog derivative is：1,4- pentadienes, tri (propylene glycol) diacrylate,
Polyethyleneglycol diacrylate, ethylene glycol diacrylate, diethylene glycol divinyl ether；
Step (2) plasma discharge mode is spark discharge.
(3) post-process：
Stopping is passed through monomer vapours, while stops plasma discharge, and inert gas is filled with into reaction chamber to pressure
2000 millitorrs, 10 millitorrs are then evacuated to, carry out above-mentioned inflation and vacuum step once, be passed through air to an air
Pressure, stops the motion of base material, then takes out base material.Electronic component after above-mentioned plated film, exposed to damp and hot test environment
Middle its wet-heat resisting alternation performance of test, test result are as follows：
Embodiment 6
A kind of preparation method of organic silicon nano protective coating, comprises the following steps：
(1) pre-treatment：
Base material is placed in nano coating Preparation equipment reaction chamber, closed reaction chamber is simultaneously continuously taken out true to reaction chamber
Sky, the vacuum in reaction chamber is extracted into 180 millitorrs, is passed through inert gas Ar, started motion, transported base material
It is dynamic；
Step (1) base material is solid material, and the solid material is electric component.
The volume of reaction chamber is 880L in step (1), and the temperature control of reaction chamber is passed through inert gas at 50 DEG C
Flow is 200sccm.
Base material carries out curved reciprocating movement, speed 200mm/min in step (1).
(2) prepared by organic silicon coating：
Monomer vapours are passed through in reaction chamber, is 250 millitorrs to vacuum, opens plasma discharge, carry out chemistry
Vapour deposition, organic silicon nano coating is prepared in substrate surface chemical vapor deposition；
The monomer vapours composition is：
The mixing of the organic silicon monomer and three kinds of polyfunctionality unsaturated hydrocarbons and hydrocarbon derivative of four kinds of structures containing Si-O-C
Thing, polyfunctionality unsaturated hydrocarbons and mass fraction shared by hydrocarbon derivative are 57% in the monomer vapours；
Plasma discharge, carries out chemical vapor deposition, and deposition process plasma discharge process is alternately to put in the cycle
Electricity, specifically include following deposition process once：
Deposition process includes pretreatment stage and plating mem stage, and pretreatment stage plasma discharge power is 600W, is held
Continuous discharge time 60s, subsequently into plating mem stage, plated film phase plasma is alternately to change electric discharge output, power in the cycle
10W, time 3600s, alternative frequency 1000Hz, the plasma cycle, alternately change electric discharge output waveform was full-wave rectification ripple
Shape；
In step (2)：
Monomer vapours are passed through to be atomized, being volatilized by charge pump by monomer, reaction chamber is introduced by the millitorr of low pressure 180
Room, the flow for being passed through monomer vapours are 35 μ L/min；
The organic silicon monomer of four kinds of structures containing Si-O-C is：Hexaetcycletrisiloxane, diphenyl diethoxy silicon
Alkane, dodecyltrimethoxysilane, 3- r-chloropropyl trimethoxyl silanes；
Three kinds of polyfunctionalities unsaturated hydrocarbons analog derivative is：Polyethyleneglycol diacrylate, diacrylate ethylene glycol
Ester, diacrylic acid pentyl diol ester.
Step (2) plasma discharge mode is discharged for intermediate frequency, and the waveform of intermediate frequency electric discharge is sine.
(3) post-process：
Stopping is passed through monomer vapours, while stops plasma discharge, and air is filled with into reaction chamber to pressure 5000
Millitorr, 200 millitorrs are then evacuated to, carry out above-mentioned inflation and vacuum step 12 times, be passed through air to an atmospheric pressure, stop
The only motion of base material, then takes out base material.Electric component after above-mentioned plated film, in International Industry classification of waterproof standard IPX7
Resistance to underwater powered is tested under described environment and resistance to underwater soaking, experiment effect are as follows：
Following table is that coating manufactured in the present embodiment reaches time test used in 1mA in different voltage, currents：
| Voltage | 3.8V | 5V | 12.5V |
| Time | >48h | ＞ 48h | ＞ 48h |
Obtained deposition has the classification of waterproof of electric component IPX 7 test (the underwater 1m immersions examination of waterproof electrical breakdown withstand coating
Test 30min) effect is as follows：
Claims (10)
- A kind of 1. preparation method of organic silicon nano protective coating, it is characterised in that：Comprise the following steps：(1) pre-treatment：Base material is placed in the reaction chamber of nano coating Preparation equipment, reaction chamber continuously vacuumized, by reaction chamber Vacuum be extracted into 10~200 millitorrs, and be passed through inert gas He, Ar or He and Ar mixed gas, opening movement mechanism, make base Material produces motion in reaction chamber；(2) prepared by organic silicon coating：Monomer vapours are passed through in reaction chamber, is 30~300 millitorrs to vacuum, opens plasma discharge, carry out chemistry Vapour deposition, organic silicon nano coating is prepared in substrate surface chemical vapor deposition；The monomer vapours composition is：It is at least one containing double bond, the organic silicon monomer of Si-Cl, Si-O-C, Si-N-Si, Si-O-Si structure or cyclic structure and extremely A kind of few mixture of polyfunctionality unsaturated hydrocarbons and hydrocarbon derivative, polyfunctionality unsaturated hydrocarbons and hydrocarbon in the monomer vapours Mass fraction shared by analog derivative is 15~65%；The flow for being passed through monomer vapours is 10~1000 μ L/min；(3) post-process：Stopping is passed through monomer vapours, while stops plasma discharge, persistently vacuumizes, keep reaction chamber vacuum be 10~ Air is passed through after 200 1~5min of millitorr to an atmospheric pressure, stops the motion of base material, then takes out base material；Or stop being passed through monomer vapours, while stop plasma discharge, air or inert gas are filled with into reaction chamber To pressure 2000-5000 millitorrs, 10-200 millitorrs are then evacuated to, carry out above-mentioned inflation and vacuum step at least once, Air is passed through to an atmospheric pressure, stops the motion of base material, then takes out base material.
- A kind of 2. preparation method of organic silicon nano protective coating according to claim 1, it is characterised in that：The step (1) base material produces motion in reaction chamber in, and substrate transport form is that base material relative response chamber carries out straight reciprocating motion Or curvilinear motion, the curvilinear motion includes circular motion, ellipse circular motion, planetary motion, spheric motion or other are irregular The curvilinear motion of route.
- A kind of 3. preparation method of organic silicon nano protective coating according to claim 1, it is characterised in that：The step (1) base material is solid material in, and the solid material is electronic product, electric component, Electronic Assemblies semi-finished product, pcb board, metal Plate, polytetrafluoroethylene (PTFE) sheet material or electronic component, and the substrate surface prepares its any interface after organic silicon nano coating Water environment, mould environment, acid, basic solvent environment, sour, alkaline salt mist environment, acidic atmosphere environment, organic solvent can be exposed to Environment is soaked, cosmetics environment, sweat environment, is used in cold cycling shock environment or damp and hot alternation environment.
- A kind of 4. preparation method of organic silicon nano protective coating according to claim 1, it is characterised in that：The step (1) reaction chamber is rotator shaped chamber or cube shaped chamber in, and its volume is 50~1000L, the temperature of reaction chamber At 30~60 DEG C, it is 5~300sccm that the inert gas, which is passed through flow, for control.
- A kind of 5. preparation method of organic silicon nano protective coating according to claim 1, it is characterised in that：The step (2) in：Plasma discharge, chemical vapor deposition is carried out, it is continuous that deposition process plasma discharge process includes small-power Electric discharge, pulsed discharge or cycle alternating discharge.
- A kind of 6. preparation method of organic silicon nano protective coating according to claim 5, it is characterised in that：The deposition During plasma discharge processes be small-power continuous discharge, specifically include following deposition process at least once：Deposition process includes pretreatment stage and plating mem stage, and pretreatment stage plasma discharge power is 150~600W, is held Continuous 60~450s of discharge time, subsequently into plating mem stage, adjustment plasma discharge power is 10~150W, during continuous discharge Between 600~3600s.
- A kind of 7. preparation method of organic silicon nano protective coating according to claim 5, it is characterised in that：The deposition During plasma discharge processes be pulsed discharge, specifically include following deposition process at least once：Deposition process includes pretreatment stage and plating mem stage, and pretreatment stage plasma discharge power is 150~600W, is held Continuous 60~450s of discharge time, subsequently into plating mem stage, plating mem stage is pulsed discharge, 10~300W of power, time 600s ~3600s, the frequency of pulsed discharge is 1~1000HZ, and the dutycycle of pulse is 1:1~1:500.
- A kind of 8. preparation method of organic silicon nano protective coating according to claim 5, it is characterised in that：The deposition During plasma discharge processes be cycle alternating discharge, specifically include following deposition process at least once：Deposition process includes pretreatment stage and plating mem stage, and pretreatment stage plasma discharge power is 150~600W, is held Continuous 60~450s of discharge time, subsequently into plating mem stage, plated film phase plasma is alternately to change electric discharge output, work(in the cycle 10~300W of rate, time 600s~3600s, alternative frequency 1-1000Hz, plasma cycle alternately change electric discharge output wave Shape is zig-zag, sinusoidal waveform, square-wave waveform, current waveform in full-wave rectifier or half wave rectification wave.
- A kind of 9. preparation method of organic silicon nano protective coating according to claim 1, it is characterised in that：The organic silicon monomer containing double bond, Si-Cl, Si-O-C, Si-N-Si, Si-O-Si structure or cyclic structure includes：Organic silicon monomer containing double bond structure：Allyltrimethoxysilanis, VTES, vinyl trimethyl Silane, 3- cyclobutenyls trimethyl silane, vinyl tributyl ketoximyl silane, tetramethyl divinyl disiloxane, 1,2,2- tri- Fluoride-based tri-phenyl-silane；The organic silicon monomer of the key containing Si-Cl：Tri-phenyl chloride, methylvinyldichlorosilane, trifluoro propyl trichlorosilane, three Fluoropropyl dimethyl dichlorosilane (DMCS), 3,5-dimethylphenyl chlorosilane, tributyl chlorosilane, benzyl dimethyl chlorosilane；The organic silicon monomer of the structure containing Si-O-C：Tetramethoxy-silicane, trimethoxy hydrogen siloxane, n-octyl triethoxysilicane Alkane, phenyl triethoxysilane, vinyl three (2- methoxy ethoxies) silane, triethylvinylsilane silane, Hexaethyl ring three Siloxanes, 3- (methacryloxypropyl) propyl trimethoxy silicane, phenyl three (trimethylsiloxane group) silane, diphenyl diethyl TMOS, dodecyltrimethoxysilane, n-octytriethoxysilane, dimethoxysilane, 3- chloropropyl trimethoxies Base silane；The organic silicon monomer of the structure containing Si-N-Si or Si-O-Si：Hexamethyldisilane base amine, the silane amino of pregnancy basic ring three, six Methyl disilazane, hexamethyldisiloxane；Organic silicon monomer containing cyclic structure：Hexamethyl cyclotrisiloxane, octamethylcy-clotetrasiloxane, the silica of hexaphenyl ring three Alkane, decamethylcyclopentaandoxane, octaphenylcyclotetrasiloxane, triphenyl silicol, Diphenylsilanediol, chromic acid are double (trityl silylation) ester, trifluoro propyl methyl cyclotrisiloxane, the silicon of 2,2,4,4- tetramethyl -6,6,8,8- tetraphenyls ring four Oxygen alkane, t etram-ethyltetravinylcyclotetrasiloxane, 3- glycydoxies triethoxysilane, γ-glycidol ether Oxygen propyl trimethoxy silicane；The polyfunctionality unsaturated hydrocarbons and hydrocarbon derivative include：1,3- butadiene, isoprene, 1,4- pentadienes, ethoxylated trimethylolpropane triacrylate, two contractings 3 the third two Alcohol diacrylate, polyethyleneglycol diacrylate, 1,6 hexanediol diacrylate, ethylene glycol diacrylate, diethyl two Alcohol divinyl ether or diacrylic acid pentyl diol ester.
- A kind of 10. preparation method of organic silicon nano protective coating according to claim 1, it is characterised in that：The step Suddenly in (2), plasma discharge manner be radio frequency discharge, microwave discharge, intermediate frequency electric discharge, high-frequency discharge, spark discharge, it is described High-frequency discharge and the waveform of intermediate frequency electric discharge are sinusoidal or bipolar pulse.
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