CN206768216U - The equipment that a kind of substrate transport formula plasma discharge prepares nano coating - Google Patents
The equipment that a kind of substrate transport formula plasma discharge prepares nano coating Download PDFInfo
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- CN206768216U CN206768216U CN201720565383.6U CN201720565383U CN206768216U CN 206768216 U CN206768216 U CN 206768216U CN 201720565383 U CN201720565383 U CN 201720565383U CN 206768216 U CN206768216 U CN 206768216U
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Abstract
The equipment that a kind of substrate transport formula plasma discharge prepares nano coating, belongs to technical field of plasma, and equipment includes：Electrode, vacuum pumping hardware, base material fixing device, the gas piping being passed through for carrier gas and monomer vapours；Base material fixing device is arranged at the interior volume of electrode formation in a manner of revocable, base material is fixedly installed on base material fixing device, base material fixing device is provided with motion, and the interior volume that the base material fixing device can be formed under the drive of motion in electrode produces motion.In coating preparation process, kinetic characteristic and plasma discharge energy the combination linkage of base material.While preparation process plasma discharge, base material produces motion, improves coating deposition efficiency, and improve the uniformity and compactness of coating layer thickness.Prepared coating has the characteristics such as waterproof and dampproof, mould proof, acid and alkali resistance solvent, acid and alkali resistance salt fog.
Description
Technical field
The utility model belongs to plasma chemical vapor deposition technique field, and in particular to a kind of plasma discharge
Prepare the device and method of nano coating.
Background technology
Corrosive atmosphere is the destroyed most common factor of electronic device.Cause because of environmental corrosion solid in electronic device
The phenomena of the failure such as the reduction of burn into conductor/semiconductor insulating properties and short circuit, open circuit or the loose contact of body material.At present, exist
In the product of the hi-tech industries such as national defence, space flight, the ratio that electronic unit occupies is increasing, moistureproof to electronic product, mould proof,
Corrosion resistance requires more and more stricter.And in communication field, as technology 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
Solidify coating is difficult to closed device inside.A kind of new conformal painting of U.S. Union Carbide Co. development and application
Layer material, parylene coating are a kind of polymer of paraxylene, and there is low water, gas permeability, high screen effect can reach
To protection against the tide, waterproof, antirust, antiacid caustic corrosion effect.Research finds that Parylene is that deposition produces under vacuum conditions, can
To 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
Thickness is printed circuit board assembly polymer thin the main reason for influenceing Parylene vapour deposition conformal coat protection failure
In 3~7 micron thickness local corrosion failure easily occurs for membrane coat, in the case of high-frequency dielectric loss is not influenceed coating layer thickness should >=
30 microns.The pre-processing requirements for the printed substrate that parylene coating is protected for needs are higher, such as conductive component, signal pass
Defeated component, radio frequency component etc., need to do circuit board module masking pretreatment when being vapor-deposited conformal coat, avoid to component
Performance impacts.This drawback brings very big limitation to the application of parylene coating.Parylene coating preparing raw material cost
High, coating preparation condition harsh (high temperature, condition of high vacuum degree requirement), rate of film build are low, it is difficult to extensive use.In addition, thick coating is easy
The problems such as causing weak heat-dissipating, signal barrier, holiday to increase.
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.
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, it should can not be realized based on the preparation process of the method for specific small duty cycle pulse electric discharge
It is prepared to 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 electric equipment, and corrosion resistance caused by environment can not be solved effectively
Certainly.And fine and close protective coating prepared by the method based on specific small duty cycle pulse electric discharge has the shortcomings that 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 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.
Utility model content
The utility model provides a kind of substrate transport formula plasma discharge preparation nanometer painting to solve above-mentioned technical problem
The device and method of layer.In coating preparation process, base material relative response chamber, electrode, progress plane or three dimensions space are past
The fortune of motion, planar reciprocating, circular motion, ellipse circular motion, spheric motion, planetary motion or other irregular routes again
It is dynamic.
Carry out the continuous discharge of the corresponding power of plasma, the pulsed discharge of big space rate or power cycle alternation simultaneously
Electric discharge.Other monomers component with polyfunctional group cross-linked structure is introduced by energy of plasma to introduce extra crosslinking points
To form cross-linked structure.Plasma discharge produces plasma, by control plasma discharge energy and monomer bond energy it
Between relation, realize that the effective activation of the low temperature plasma active group higher to energy in monomer component obtains active sites
Point, meanwhile, the additional active point being introduced into is cross-linked with each other polymerization under plasma ambient, forms fine and close network structure.
Technical scheme is as follows used by the utility model：
The equipment that a kind of substrate transport formula plasma discharge prepares nano coating, including：Reaction chamber, its feature exist
In：Also include：
For the electrode of plasma discharge, the interior volume that reaction chamber is formed is arranged at；
For forming the air pumping out type vacuum exhaust apparatus of vacuum environment, the vacuum pumping hardware be connected to reaction chamber it
On, the vacuum pumping hardware includes blast pipe, one-level vavuum pump and two-stage vacuum pump, blast pipe and is connected with reaction chamber,
Blast pipe is sequentially connected two-stage vacuum pump and one-level vavuum pump；
The gas piping being passed through for carrier gas and monomer vapours；
For installing the base material fixing device of base material, the base material fixing device is arranged at the interior volume of electrode formation；
The base material fixing device is arranged at the interior volume of electrode formation in a manner of revocable, and base material is fixedly installed in
On base material fixing device, base material fixing device is provided with motion, and the base material fixing device can be in motion
The interior volume formed under drive in electrode produces motion, and its motion mode includes：Space reciprocating motion, planar reciprocating,
Circular motion, ellipse circular motion, spheric motion, planetary motion or the motion of other irregular routes.
The volume of the reaction chamber is 50~1000L, and the reaction chamber is rotator shaped chamber or cube shaped
Chamber.
The plasma discharge manner be radio frequency discharge, microwave discharge, intermediate frequency electric discharge, high-frequency discharge, spark discharge,
The high-frequency discharge and the waveform of intermediate frequency electric discharge are sinusoidal or bipolar pulse.
The method that a kind of substrate transport formula plasma discharge carried out using the said equipment prepares nano coating, its feature
It is：Comprise the following steps：
(1) base material is placed in the reaction chamber of the nano coating Preparation equipment described in claim 1, reaction chamber is connected
It is continuous to vacuumize, the vacuum in reaction chamber is extracted into 10~200 millitorrs, and be passed through inert gas He or Ar, opening movement
Mechanism, base material is set to produce motion in reaction chamber；
(2) monomer vapours are passed through in reaction chamber, is 30~300 millitorrs to vacuum, opens plasma discharge, enter
Row chemical vapor deposition, deposition process 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 is 10~
75W, continuous discharging time 600s~7200s, multi-functional nano coating is prepared in substrate surface chemical vapor deposition；
The monomer vapours composition 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 motion of base material, then take out base material.
Base material is solid material in the step (1), and the solid material is electronic product, electric component, Electronic Assemblies
Semi-finished product, pcb board, metallic plate, polytetrafluoroethylene (PTFE) sheet material or electronic component, and the substrate surface prepare multi-functional
Its any interface can be exposed to water environment after nano coating, mould environment, acid, basic solvent environment, sour, alkaline salt mist environment,
Acidic atmosphere environment, organic solvent immersion environment, cosmetics environment, sweat environment, cold cycling shock environment or damp and hot alternation
Used in environment.
The temperature control of reaction chamber is at 30~60 DEG C in the step (1), the inert gas be passed through flow for 5~
300sccm。
In the step (2)：Be passed through monomer vapours for monomer is atomized by charge pump, volatilize and by low pressure 10~
200 millitorrs introduce reaction chamber, and the flow for being passed through monomer is 10~1000 μ L/min；
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, the propylene of polyethylene glycol two
Acid esters, 1,6 hexanediol diacrylate, ethylene glycol diacrylate, diethylene glycol divinyl ether or diacrylate new penta 2
Alcohol ester.
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 adhesion of material.
In the continuous discharge that pretreatment stage plasma discharge form is high-power 120~400W, plating mem stage etc. from
Daughter discharge type is 10~75W of small-power continuous discharge.Caused by the process of continuous plasma discharge depositing etc.
Gas ions have certain etching to deposition film；Be advantageous to add in plating mem stage small-power continuous discharge combination substrate transport characteristic
The speed of fast chemistry deposition, relatively existing small duty cycle pulse discharge technology, the continuous discharge mode film within the regular hour
Thicker and finer and close, plated film is more efficient, so as to solve the P2i companies of Britain mentioned in background technology based on specific
The fatal defects of fine and close protective coating prepared by the method for small 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 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 multi-functional nanometer is formed in substrate surface
Coating.
Base material is solid material in the step (1), and the solid material is electronic product, electric component, Electronic Assemblies
Semi-finished product, pcb board, metallic plate, polytetrafluoroethylene (PTFE) sheet material or electronic component, and the substrate surface prepare multifunctionality and received
Its any interface can be exposed to water environment, mould environment, acid, basic solvent environment, sour, 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 temperature control of step (1) reaction chamber at 30~60 DEG C, the inert gas be passed through flow for 5~
300sccm。
In the step (2), the plasma discharge manner is radio frequency discharge, microwave discharge, intermediate frequency is discharged, high frequency is put
The waveform of electricity, spark discharge, the high-frequency discharge and intermediate frequency electric discharge is sinusoidal or bipolar pulse, and radio frequency plasma is to utilize
Discharge and caused plasma electromagnetic field of high frequency.Microwave method is the energy excitation plasma using microwave, has energy profit
The advantages of with efficiency high, simultaneously because electrodeless discharge, plasma is pure, is current high quality, high-speed, large area preparation
Excellent process.
In coating preparation process, kinetic characteristic and plasma discharge energy the combination linkage of base material, kinematic parameter is utilized
Solve coating with the combination configuration of plasma discharge energy and deposit uneven, unsound problem.Plasma in preparation process
While body discharges, base material produces motion, improves coating deposition efficiency, and improve uniformity and the densification of coating layer thickness
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 in the case of 1~1000nm to frequency
The influence of radio frequency communication signal in the range of 10M~8G is less than 5%.
Above-mentioned technical proposal of the present utility model has advantages below compared with prior art：
1st, continuous small-power electric discharge is introduced in plating mem stage, can polymerize and carve simultaneously during continuous discharge
Lose two processes, 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 in surface after polymerization simultaneously, while play a part of activation, two
The alternating action of person make it that the nano coating of polymerization is finer and close.
2nd, pre-process and plate mem stage, base material moves in reaction chamber, makes the base material coating film thickness of diverse location
Tend to consistent, solve because different zones monomer density difference causes substrate surface coating layer thickness uneven in reaction chamber
Problem.
3rd, in preparation process, kinetic characteristic and plasma discharge energy the combination linkage of base material, discharge energy output
Meanwhile base material is moved, 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 green so as to reduce the discharge of tail gas exhaust, in actual production efficiency is improved have weight
Big meaning.
4th, the introducing of polyfunctional group cross-linked structure promotes coating densification network 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.This practicality
It is new to introduce extra crosslinking points by introducing the other monomers component with polyfunctional group cross-linked structure to form crosslinking knot
Structure.During plasma discharge, under low temperature plasma effect, by effective control to energy and output, by monomer component
The higher active group of middle energy interrupts to form active site, and the additional active point being introduced into is cross-linked with each other poly- under plasma ambient
Close, 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 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, 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 the utility model patent is significantly
Nanometer is added to be significant in actual production efficiency is improved.Coating is in the service life of corrosive atmosphere, raising
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.
It can be easy to user to be handled official business in route.But when it runs into the pollution of common liquid, the unexpected 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 damage.After carrying out plated film to it using such nano coating, when can
Surface of keyboard easy to clean is ensured, 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, above mentioned problem can effectively solve the problem that.
(3), intelligent fingerprint lock：Fingerprint Lock is intelligent lock, and it has gathered computer information technology, electronic technology, machinery
Technology and modern five gold process, are widely used in police criminal detection and judicial domain.But 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：Audiphone does not have connection, after the coating, Yong Huke with bluetooth earphone
To be used within a certain period of time under water environment, such as have a bath, on rainy day, equipment will not infiltrate 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, and these sensors are using the painting
After layer, can ensure will not cause faulty sensor because of liquid intrusion plant equipment internal structure.
(6), most of 3C Products：Such as mobile phone, notebook, PSP.
(7), other 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 influenceed.
Multi-functional nano coating prepared by this method can be applicable to following different environment and its correlation being related to
Product：
It is waterproof and dampproof mould proof：
1 house interior trim：Toilet top surface, wallpaper, pendent lamp, curtain, window screening.2 daily necessitiess：Mosquito net, desk lamp cover, chopsticks
Basket, automobile rearview mirror.3 historical relics and the art work：Copybook, antiques, woodcarving, leather, bronze ware, silk, ancient costume, ancient books.4 electronics member
Device and electronic product：Sensor (operation in moist or dirty environment), each electronic product (electronic sphygmomanometer, intelligent hand
Table) chip, wiring board, mobile phone, LED screen, audiphone.5 precision instruments and optical device：Mechanical watch, microscope.
Acid and alkali resistance solvent, acid and alkali resistance salt fog, acid resistance air：
1 house inside gadget：Wallpaper, ceramic tile.2 safety devices：Acidproof (alkali) gloves, acidproof (alkali) protective garment.3 plant equipment
And pipeline：Flue desulfurization equipment, seal (acid/base lubricating oil), pipeline, valve, Large Diameter Pipeline sea conveyance conduit liner etc.
Place.4 various reactors, reactor.The production of 5 chemicals, storage；Sewage disposal, aeration tank；6 is other：Soda acid workshop, alkali prevention
The every profession and trades such as Aero-Space, electricity power, Ferrous Metallurgy, petrochemical industry, medical treatment, storage container, statue (reduce acid rain to its
Corrosion), sensor (under acid/base environment).
Organic solvent-resistant soaks, resistance to cosmetics, resistance to sweat：
1 such as alkane, alkene, alcohol, aldehyde, amine, ester, ether, ketone, aromatic hydrocarbon, hydrogenate hydrocarbon, terpene hydrocarbon, halogenated hydrocarbons, jeterocyclic chemistry
Thing, nitrogen-containing compound and sulfur-containing compound solvent etc.；2 toiletry bag packaging containers；3 Fingerprint Locks, earphone.
Cold-resistant thermal cycle impact (- 40 DEG C~+75 DEG C), wet-heat resisting alternation (humidity 75%~95%)：Electrician, electronics, vapour
Car electrical equipment, such as aviation, automobile, household electrical appliances, the equipment in scientific research field.
Brief description of the drawings
Fig. 1 is that base material carries out the device structure front view that circular motion plasma discharge prepares nano coating.
Fig. 2 is Fig. 1 top view.
Fig. 3 is that base material carries out the device structure front view that planetary motion plasma discharge prepares nano coating.
Fig. 4 is Fig. 3 top view.
Fig. 5 is that base material carries out the device structure front view that space reciprocating motion plasma discharge prepares nano coating.
Fig. 6 is Fig. 5 top view.
Fig. 7 is that base material carries out the device structure front view that planar reciprocating plasma discharge prepares nano coating.
Fig. 8 is Fig. 7 top views.
In figure, 1, reaction chamber, 2, electrode, 3, circumference pivoted frame, 4, workpiece, 5, planet pivoted frame, 6, planetary turntable, 7, space
Move back and forth platform, 8, planar reciprocating platform
Embodiment
Describe the utility model in detail with specific embodiment below in conjunction with the accompanying drawings, but the utility model is not limited to specifically
Embodiment.
Embodiment 1
The equipment that a kind of substrate transport formula plasma discharge as illustrated in figs. 1 and 2 prepares nano coating, including：Instead
Answer chamber 1, it is characterised in that：Also include：
For the electrode 2 of plasma discharge, the interior volume that reaction chamber is formed is arranged at；
For forming the air pumping out type vacuum exhaust apparatus of vacuum environment, the vacuum pumping hardware be connected to reaction chamber it
On, the vacuum pumping hardware includes blast pipe, one-level vavuum pump and two-stage vacuum pump, blast pipe and is connected with reaction chamber,
Blast pipe is sequentially connected two-stage vacuum pump and one-level vavuum pump；
The gas piping being passed through for carrier gas and monomer vapours；
For installing the base material fixing device of base material, the base material fixing device is arranged at the interior volume of electrode formation；
The base material fixing device is arranged at the interior volume of electrode formation in a manner of revocable, and base material is fixedly installed in
On base material fixing device, base material fixing device is provided with motion, and the base material fixing device can be in motion
The interior volume formed under drive in electrode produces motion, and its motion mode is circular motion.Set in the space that electrode is formed
There is circumference pivoted frame, workpiece is fixed on circumference pivoted frame；
The volume of reaction chamber is 50L, and the reaction chamber is rotator shaped chamber.
Plasma discharge manner is continuous radio frequency discharge.
A kind of method that substrate transport formula plasma discharge prepares nano coating, comprises the following steps：
(1) base material is placed in the reaction chamber of nano coating Preparation equipment, closed reaction chamber simultaneously connects to reaction chamber
It is continuous to vacuumize, the vacuum in reaction chamber is extracted into 10 millitorrs, inert gas Ar is passed through, opening movement mechanism, base material is existed
Motion is produced in reaction chamber；Base material is solid material in step (1), and the solid material is block polyfluortetraethylene plate
Material, and the substrate surface prepares 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 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) 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 the millitorr of low pressure 10
Room, the flow for being passed through monomer vapours are 1000 μ L/min；
Monomer vapours composition 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；
(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
The equipment that a kind of substrate transport formula plasma discharge as described in fig. 3 and fig. 4 prepares nano coating, including：Instead
Answer chamber 1, it is characterised in that：Also include：
For the electrode 2 of plasma discharge, the interior volume that reaction chamber is formed is arranged at；
For forming the air pumping out type vacuum exhaust apparatus of vacuum environment, the vacuum pumping hardware be connected to reaction chamber it
On, the vacuum pumping hardware includes blast pipe, one-level vavuum pump and two-stage vacuum pump, blast pipe and is connected with reaction chamber,
Blast pipe is sequentially connected two-stage vacuum pump and one-level vavuum pump；
The gas piping being passed through for carrier gas and monomer vapours；
For installing the base material fixing device of base material, the base material fixing device is arranged at the interior volume of electrode formation；
The base material fixing device is arranged at the interior volume of electrode formation in a manner of revocable, and base material is fixedly installed in
On base material fixing device, base material fixing device is provided with motion, and the base material fixing device can be in motion
The interior volume formed under drive in electrode produces motion, and its motion mode is planetary motion.Set in the space that electrode is formed
There is planet pivoted frame 5, planetary turntable 6 is provided with planet pivoted frame, workpiece 4 is fixed on planetary turntable.
The volume of reaction chamber is 250L, and the reaction chamber is rotator shaped chamber.
Plasma discharge manner is intermediate frequency continuous discharge, and the waveform of intermediate frequency electric discharge is sinusoidal.
A kind of method that substrate transport formula plasma discharge prepares nano coating, comprises the following steps：
(1) base material is placed in nano coating Preparation equipment reaction chamber, closed reaction chamber is simultaneously continuous to reaction chamber
Vacuumize, the vacuum in reaction chamber is extracted into 60 millitorrs, be passed through inert gas He, start motion, carry out base material
Motion；
Base material is solid material in step (1), and the solid material is block aluminum alloy materials, and the substrate surface system
Its any interface can be 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 the millitorr of low pressure 60,
The flow for being passed through monomer vapours is 700 μ L/min；
Monomer vapours composition is：
The mixture of three kinds of 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：Tri (propylene glycol) diacrylate and the propylene of polyethylene glycol two
Acid esters；
(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
The equipment that a kind of substrate transport formula plasma discharge as described in the fig 5 and 6 prepares nano coating, including：Instead
Answer chamber 1, it is characterised in that：Also include：
For the electrode 2 of plasma discharge, the interior volume that reaction chamber is formed is arranged at；
For forming the air pumping out type vacuum exhaust apparatus of vacuum environment, the vacuum pumping hardware be connected to reaction chamber it
On, the vacuum pumping hardware includes blast pipe, one-level vavuum pump and two-stage vacuum pump, blast pipe and is connected with reaction chamber,
Blast pipe is sequentially connected two-stage vacuum pump and one-level vavuum pump；
The gas piping being passed through for carrier gas and monomer vapours；
For installing the base material fixing device of base material, the base material fixing device is arranged at the interior volume of electrode formation；
The base material fixing device is arranged at the interior volume of electrode formation in a manner of revocable, and base material is fixedly installed in
On base material fixing device, base material fixing device is provided with motion, and the base material fixing device can be in motion
The interior volume formed under drive in electrode produces motion, and its motion mode moves back and forth for space.In the space that electrode is formed
It is provided with space and moves back and forth platform 7.
The volume of reaction chamber is 480L, and the reaction chamber is cube shaped chamber.
Plasma discharge manner is high frequency continuous discharge, and the waveform of high-frequency discharge is bipolar pulse.
A kind of method that substrate transport formula plasma discharge prepares nano coating, comprises the following steps：
(1) base material is placed in nano coating Preparation equipment reaction chamber, closed reaction chamber is simultaneously continuous to reaction cavity
Vacuumize, the vacuum in reaction chamber is extracted into 130 millitorrs, be passed through inert gas Ar, start motion, enter base material
Row motion；
Base material is solid material in step (1), and the solid material is bulk alloy steel plate materialses, 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 space reciprocating motion in step (1), and its speed to move up and down is 5mm/min, its side-to-side movement
Speed is 3mm/min, and its speed moved forward and backward is 6mm/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 the millitorr of low pressure 10,
The flow for being passed through monomer vapours is 550 μ L/min；
Monomer vapours composition is：
The mixture of two kinds of 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 38%；
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；
(3) plated film terminates, and stopping is passed through starting monomer steam, while stops plasma discharge, persistently vacuumizes, and protects
It is 130 millitorrs to hold reaction cavity vacuum, 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
The equipment that a kind of substrate transport formula plasma discharge as described in Fig. 7 and Fig. 8 prepares nano coating, including：Instead
Answer chamber 1, it is characterised in that：Also include：
For the electrode 2 of plasma discharge, the interior volume that reaction chamber is formed is arranged at；
For forming the air pumping out type vacuum exhaust apparatus of vacuum environment, the vacuum pumping hardware be connected to reaction chamber it
On, the vacuum pumping hardware includes blast pipe, one-level vavuum pump and two-stage vacuum pump, blast pipe and is connected with reaction chamber,
Blast pipe is sequentially connected two-stage vacuum pump and one-level vavuum pump；
The gas piping being passed through for carrier gas and monomer vapours；
For installing the base material fixing device of base material, the base material fixing device is arranged at the interior volume of electrode formation；
The base material fixing device is arranged at the interior volume of electrode formation in a manner of revocable, and base material is fixedly installed in
On base material fixing device, base material fixing device is provided with motion, and the base material fixing device can be in motion
The interior volume formed under drive in electrode produces motion, and its motion mode is planar reciprocating.In the space that electrode is formed
It is provided with planar reciprocating platform 7.
The volume of reaction chamber is 680L, and the reaction chamber is cube shaped chamber.
Plasma discharge manner discharges for microwave continuous.
A kind of method that substrate transport formula plasma discharge prepares nano coating, comprises the following steps：
(1) base material is placed in nano coating Preparation equipment reaction chamber, closed reaction chamber is simultaneously continuous to reaction cavity
Vacuumize, the vacuum in reaction chamber is extracted into 160 millitorrs, be passed through inert gas He, start motion, carry out base material
Motion；
Base material is solid material in step (1), and the solid material is block aluminum material and pcb board, and the base material
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 planar reciprocating in step (1), and the speed of its side-to-side movement is 6mm/min, what it was moved forward and backward
Speed is 9mm/min.
(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 the millitorr of low pressure 160
Room, the flow for being passed through monomer vapours are 220 μ L/min；
Monomer vapours composition 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 52%；
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；
(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
The equipment that a kind of substrate transport formula plasma discharge as illustrated in figs. 1 and 2 prepares nano coating, including：Instead
Answer chamber 1, it is characterised in that：Also include：
For the electrode 2 of plasma discharge, the interior volume that reaction chamber is formed is arranged at；
For forming the air pumping out type vacuum exhaust apparatus of vacuum environment, the vacuum pumping hardware is connected to reaction chamber
On, the vacuum pumping hardware includes blast pipe, one-level vavuum pump and two-stage vacuum pump, blast pipe and is connected with reaction chamber
Connect, blast pipe is sequentially connected two-stage vacuum pump and one-level vavuum pump；
The gas piping being passed through for carrier gas and monomer vapours；
For installing the base material fixing device of base material, the base material fixing device is arranged at the interior volume of electrode formation；
The base material fixing device is arranged at the interior volume of electrode formation in a manner of revocable, and base material is fixedly installed in
On base material fixing device, base material fixing device is provided with motion, and the base material fixing device can be in motion
The interior volume formed under drive in electrode produces motion, and its motion mode is circular motion.Set in the space that electrode is formed
There is circumference pivoted frame, workpiece is fixed on circumference pivoted frame；
The volume of reaction chamber is 580L, and the reaction chamber is rotator shaped chamber.
Plasma discharge manner is continuous radio frequency discharge.
A kind of method that substrate transport formula plasma discharge prepares nano coating, comprises the following steps：
(1) base material is placed in nano coating Preparation equipment reaction chamber, closed reaction chamber is simultaneously continuous to reaction cavity
Vacuumize, the vacuum in reaction chamber is extracted into 200 millitorrs, be passed through inert gas Ar, start motion, carry out base material
Motion；
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 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) 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 the millitorr of low pressure 200
Body, the flow for being passed through monomer vapours are 10 μ L/min；
Monomer vapours composition 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：
。
Claims (3)
1. the equipment that a kind of substrate transport formula plasma discharge prepares nano coating, including：Reaction chamber (1), its feature exist
In：Also include：
For the electrode (2) of plasma discharge, the interior volume that reaction chamber is formed is arranged at；
For forming the air pumping out type vacuum exhaust apparatus of vacuum environment, the vacuum pumping hardware is connected on reaction chamber,
The vacuum pumping hardware includes blast pipe, one-level vavuum pump and two-stage vacuum pump, blast pipe and is connected with reaction chamber, is vented
Pipe is sequentially connected two-stage vacuum pump and one-level vavuum pump；
The gas piping being passed through for carrier gas and monomer vapours；
For installing the base material fixing device of base material, the base material fixing device is arranged at the interior volume of electrode formation；
The base material fixing device is arranged at the interior volume of electrode formation in a manner of revocable, and base material is fixedly installed in base material
On fixing device, base material fixing device is provided with motion, and the base material fixing device can be in the drive of motion
Under the interior volume that is formed in electrode produce motion, its motion mode includes：Space reciprocating motion, planar reciprocating, circumference
Motion, ellipse circular motion, spheric motion, planetary motion or the motion of other irregular routes.
2. the equipment that a kind of substrate transport formula plasma discharge according to claim 1 prepares nano coating, its feature
It is：The volume of the reaction chamber is 50~1000L, and the reaction chamber is rotator shaped chamber or cube shaped chamber
Room.
3. the equipment that a kind of substrate transport formula plasma discharge according to claim 1 prepares nano coating, its feature
It is：The plasma discharge manner be radio frequency discharge, microwave discharge, intermediate frequency electric discharge, high-frequency discharge, spark discharge, institute
The waveform for stating high-frequency discharge and intermediate frequency electric discharge is sinusoidal or bipolar pulse.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109554690A (en) * | 2019-01-04 | 2019-04-02 | 朱广智 | A kind of microwave plasma vacuum coating equipment and application method |
| CN112538617A (en) * | 2019-09-20 | 2021-03-23 | 江苏菲沃泰纳米科技股份有限公司 | Film coating equipment |
| CN112981373A (en) * | 2019-12-18 | 2021-06-18 | 江苏菲沃泰纳米科技股份有限公司 | Film coating equipment and film coating method thereof |
| CN114836735A (en) * | 2021-02-01 | 2022-08-02 | 江苏菲沃泰纳米科技股份有限公司 | ICP-based plasma coating device and method |
| US11555247B2 (en) | 2019-09-20 | 2023-01-17 | Jiangsu Favored Nanotechnology Co., Ltd. | Coating apparatus and movable electrode arrangement, movable support arrangement, and application thereof |
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2017
- 2017-05-21 CN CN201720565383.6U patent/CN206768216U/en active Active
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109554690A (en) * | 2019-01-04 | 2019-04-02 | 朱广智 | A kind of microwave plasma vacuum coating equipment and application method |
| CN112538617A (en) * | 2019-09-20 | 2021-03-23 | 江苏菲沃泰纳米科技股份有限公司 | Film coating equipment |
| CN112538617B (en) * | 2019-09-20 | 2022-02-22 | 江苏菲沃泰纳米科技股份有限公司 | Film coating equipment |
| US11555247B2 (en) | 2019-09-20 | 2023-01-17 | Jiangsu Favored Nanotechnology Co., Ltd. | Coating apparatus and movable electrode arrangement, movable support arrangement, and application thereof |
| CN112981373A (en) * | 2019-12-18 | 2021-06-18 | 江苏菲沃泰纳米科技股份有限公司 | Film coating equipment and film coating method thereof |
| CN112981375A (en) * | 2019-12-18 | 2021-06-18 | 江苏菲沃泰纳米科技股份有限公司 | Film coating equipment and film coating method thereof |
| CN112981375B (en) * | 2019-12-18 | 2023-09-22 | 江苏菲沃泰纳米科技股份有限公司 | Coating equipment and coating method thereof |
| US11898248B2 (en) | 2019-12-18 | 2024-02-13 | Jiangsu Favored Nanotechnology Co., Ltd. | Coating apparatus and coating method |
| CN114836735A (en) * | 2021-02-01 | 2022-08-02 | 江苏菲沃泰纳米科技股份有限公司 | ICP-based plasma coating device and method |
| CN114836735B (en) * | 2021-02-01 | 2024-01-19 | 江苏菲沃泰纳米科技股份有限公司 | Plasma coating device and method based on ICP |
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Effective date of registration: 20180111 Address after: Yuqi Industrial Park East Ring Road 214183 Jiangsu city of Wuxi Province Patentee after: Jiangsu Feiwotai Nano Technology Co. Ltd. Address before: 214000 Jiangsu Province, Wuxi city Huishan District Qi Zhen Yu Yuqi Industrial Park East Ring Road Patentee before: Wuxi RJ Industries Co., Ltd. |
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| CP03 | Change of name, title or address | ||
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Address after: No.182, East Ring Road, Yuqi supporting area, Huishan Economic Development Zone, Wuxi City, Jiangsu Province, 214000 Patentee after: Jiangsu feiwotai nanotechnology Co.,Ltd. Address before: 214183 East Ring Road, Yuqi Industrial Park, Wuxi City, Jiangsu Province Patentee before: Jiangsu Favored Nanotechnology Co.,Ltd. |