WO2019037446A1 - 一种具有调制结构的高绝缘纳米防护涂层的制备方法 - Google Patents
一种具有调制结构的高绝缘纳米防护涂层的制备方法 Download PDFInfo
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- 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
- C23C16/455—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 introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C16/45523—Pulsed gas flow or change of composition over time
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- B05D1/00—Processes for applying liquids or other fluent materials
- B05D1/62—Plasma-deposition of organic layers
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- 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
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- 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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- 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
- C23C16/455—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 introducing gases into reaction chamber or for modifying gas flows in reaction chamber
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- 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
- C23C16/458—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 supporting substrates in the reaction chamber
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- 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
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- 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
- C23C16/515—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 pulsed discharges
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- 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
- C23C16/517—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 a combination of discharges covered by two or more of groups C23C16/503 - C23C16/515
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- 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
- C23C16/56—After-treatment
Definitions
- the invention belongs to the technical field of plasma chemical vapor deposition, and in particular relates to a preparation method of a nano protective coating.
- Anti-mold, anti-moist and anti-salt spray (referred to as three-proof) is an important problem that needs to be solved in the process of storage, transportation and use of electronic devices. Mold, salt spray and moisture often cause electronic devices to fail due to short circuits. Therefore, for the protective coating applied to the electronics industry, in addition to the excellent "three-proof" performance, it must also have good insulation.
- the use of protective coatings to protect electronic products is an effective way to improve the service life of electronic products.
- the liquid phase method usually adopts three anti-paints. After coating the electronic products, it uses thermal curing or photocuring to form a dense organic coating on the circuit board to protect the circuit boards and related equipment from environmental pollution. .
- the three anti-paint has good resistance to high and low temperature; it forms a transparent protective film after curing, and has superior properties of insulation, moisture, leakage, shock, dust, corrosion, aging and corona resistance.
- the liquid phase method will produce waste water, waste gas and waste liquid.
- the solvent used will cause certain damage to the electronic device substrate itself.
- the thickness is mostly several tens of micrometers, which is difficult to control at the nanometer level. For some electrons requiring heat dissipation and signal transmission. Device features will have an impact.
- the gas phase method includes methods such as vapor deposition and plasma vapor deposition.
- the most typical vapor deposition coating is a parylene coating, developed by Union Carbide Co. of the United States and widely used in electronic product protection.
- the parylene coating is a p-xylene polymer that first heats para-xylene to 680 degrees Celsius to form an active para-xylene dimer. After the deposition chamber is lowered in temperature, the dimer is deposited in the electron. On the surface of the product, a polymer film is formed.
- the parylene coating Since the paraxylene structure is highly symmetrical, the dipole moment is 0, and due to the presence of the benzene ring, the polymer molecule has a large free volume; and at the same time, due to the relatively large molecular weight of the polymer, the coating is dense. Due to the above characteristics, the parylene coating has low water, gas permeability and high barrier effect to achieve moisture, water, rust and acid and alkali corrosion resistance. This parylene is deposited under vacuum and can be used in applications where liquid coatings cannot be involved, such as high frequency circuits and very weak current systems. The thickness of the polymer film coating is the main reason for the protection failure of the para-xylene vapor-deposited conformal coating.
- the polymer film coating of the printed circuit board component is prone to local rust failure at a thickness of 3 to 7 microns without affecting the high.
- the coating thickness should be ⁇ 30 ⁇ m in the case of frequency dielectric loss.
- Parylene coating requires high pretreatment of printed circuit boards that need protection, such as conductive components, signal transmission components, RF components, etc., in the vapor deposition of conformal coatings, it is necessary to pre-mask the circuit board components to avoid Affects component performance. This drawback has brought great limitations to the application of parylene coating.
- Pyrene coatings have high cost of raw materials, harsh coating preparation conditions (high temperature, high vacuum requirements), low film formation rate, and are difficult to be widely used.
- thick coatings tend to cause problems such as poor heat dissipation, signal rejection, and increased coating defects.
- Plasma chemical vapor deposition is a technique in which a reactive gas is activated by a plasma to promote a chemical reaction on a surface of a substrate or a near surface to form a solid film.
- Plasma chemical vapor deposition coatings have the following advantages:
- the plasma polymerization film is stable in chemical and physical properties such as solvent resistance, chemical corrosion resistance, heat resistance, and abrasion resistance.
- the plasma polymerization film has good adhesion to the substrate.
- a uniform film can also be formed on the surface of the substrate having irregular irregularities.
- the coating preparation temperature is low, and can be carried out under normal temperature conditions, thereby effectively avoiding damage to temperature sensitive devices.
- the plasma process can not only prepare a coating having a thickness of a micron order but also can prepare an ultra-thin nano-scale coating.
- the coating is highly configurable. Under plasma conditions, most of the organic monomers can be activated into highly active free radicals and form a coating on the surface of the electronic product.
- the screening and design of the monomer dipole moment, chemical inertness, and free volume is an important strategy for obtaining a coating with good insulation and excellent protection in a thin condition.
- the coating structure is highly controllable, and the composition and proportion of the monomer can be changed at any time, so that the coating has a special structure such as multilayer, gradient and modulation.
- the performance is relatively simple.
- the thickness must be increased, and the increase in thickness leads to a decrease in heat dissipation, signal transmission, and the like.
- the present invention provides a method for preparing a high-insulation nano-protective coating having a modulation structure in order to solve the above technical problems.
- the organic monomer with low dipole moment and high chemical inertness is screened, and the free volume and compactness of the coating are controlled by the polyfunctional monomer, so that the coating has high insulation and excellent protection at the same time.
- the low dipole moment organic coating and the silicone coating preparation or the organic fluorocarbon coating are alternately prepared to form a low dipole moment-silicone/fluorocarbon modulation multilayer dense structure, composite modulation
- the multi-layer structure is designed to achieve a significant increase in coating protection without sacrificing heat transfer and signal transmission.
- the composition and structure of the coating are optimized by the design of the monomer and the optimization of the process parameters.
- a nano-protective coating with a modulated structure can be designed.
- the use of the interface between the layers prevents the longitudinal diffusion of corrosion; at the same time, due to the superlattice effect of the modulation of the nano-layered structure, the accumulation of dislocations between the layers makes the coating less likely to be broken down, and is resistant to underwater energization. The ability has been effectively improved.
- This modulation structure coating has superior protection and insulation properties at the same thickness than existing coatings such as parylene. Protection and insulation can be achieved at lower thicknesses, thus solving many problems existing in the current coatings such as parylene, such as thick coating thickness, low production efficiency, poor heat dissipation, and signal blocking.
- a method for preparing a high-insulation nano-protective coating having a modulation structure comprising: the following steps:
- the substrate is placed in a reaction chamber of the nano-coating preparation device, and the reaction chamber is continuously evacuated, and the vacuum in the reaction chamber is pumped to 10 to 200 mTorr, and an inert gas of He, Ar or He and Ar is introduced. Mixing the gas, opening the moving mechanism to cause the substrate to move in the reaction chamber;
- the monomer A vapor component comprises:
- the monomer B vapor component comprises:
- the monomer C vapor component comprises:
- the passage of monomer A, monomer B and monomer C vapor is carried out by atomizing, volatilizing and introducing a monomer into a reaction chamber from a low pressure of 10 to 200 mTorr, the monomer A, single
- the flow rate of the body B and the monomer C is 10 to 1000 ⁇ L / min;
- Stop the plasma discharge continue to vacuum, keep the vacuum of the reaction chamber at 10 ⁇ 200 mTorr, and then pass air to an atmospheric pressure after 1 to 5 minutes to stop the movement of the substrate, and then take out the substrate;
- stop the plasma discharge fill the reaction chamber with air or inert gas to a pressure of 2000-5000 mTorr, then evacuate to 10-200 mTorr, perform the above aeration and vacuum steps at least once, and pass air to a At atmospheric pressure, stop the movement of the substrate and then remove the substrate.
- the substrate generates motion in the reaction chamber, and the substrate moves in the form of a linear reciprocating motion or a curved motion of the substrate relative to the reaction chamber, the curved motion including circular motion, elliptical motion, planetary motion, Curved motion of spherical motion or other irregular routes.
- the substrate in the step (1) is a solid material
- the solid material is an electronic product, an electrical component, an electronic assembly semi-finished product, a PCB board, a metal plate, a polytetrafluoroethylene plate or an electronic component, and the surface of the substrate
- any interface can be exposed to water environment, mold environment, acid, alkaline solvent environment, acid, alkaline salt spray environment, acidic atmospheric environment, organic solvent soaking environment, cosmetic environment, sweat environment, Use in cold or hot cycle impact environment or wet heat alternating environment.
- the reaction chamber is a rotating body chamber or a cubic chamber, the volume of which is 50-1000 L, the temperature of the reaction chamber is controlled at 30-60 ° C, and the flow rate of the inert gas is 5 ⁇ . 300sccm.
- step (2) introducing a monomer A vapor, introducing a monomer B vapor or introducing a monomer C vapor, plasma discharge, performing chemical vapor deposition, and the plasma discharge process includes a low power continuous discharge during the deposition process. , pulse discharge or periodic discharge.
- the plasma discharge process during the deposition process is a low power continuous discharge, specifically including the following deposition process at least once:
- the deposition process includes a pretreatment stage and a coating stage.
- the plasma discharge power in the pretreatment stage is 150-600 W
- the continuous discharge time is 60-450 s
- the plasma discharge power is adjusted to 10 to 150 W
- the continuous discharge time is 600 to 3600 s. .
- the plasma discharge process during the deposition is a pulse discharge, specifically including the following deposition process at least once:
- the deposition process includes a pretreatment stage and a coating stage.
- the plasma discharge power of the pretreatment stage is 150-600 W, and the continuous discharge time is 60-450 s, and then enters the coating stage.
- the coating stage is pulse discharge, the power is 10 to 300 W, and the time is 600 s to 3600 s.
- the frequency of the pulse discharge is 1 to 1000 Hz, and the duty ratio of the pulse is 1:1 to 1:500.
- the plasma discharge process during the deposition process is a periodic alternating discharge, specifically including the following deposition process at least once:
- the deposition process includes a pretreatment stage and a coating stage.
- the plasma discharge power in the pretreatment stage is 150-600 W, and the continuous discharge time is 60-450 s, and then enters the coating stage.
- the plasma in the coating stage is a periodic alternating discharge output with a power of 10 to 300 W.
- the time is 600s ⁇ 3600s, the frequency conversion rate is 1-1000Hz, and the plasma cycle alternately changes.
- the discharge output waveform is a sawtooth waveform, a sinusoidal waveform, a square wave waveform, a full-wave rectified waveform or a half-wave rectified waveform.
- the low dipole moment organic monomer includes:
- the monofunctional unsaturated fluorocarbon resin includes:
- the silicone monomer containing a double bond, a Si—Cl, a Si—O—C, a Si—N—Si, a Si—O—Si structure or a ring structure includes:
- Silicone monomer containing double bond structure allyl trimethoxy silane, vinyl triethoxy silane, vinyl trimethyl silane, 3-butenyl trimethyl silane, vinyl tributyl ketone fluorenyl Silane, tetramethyldivinyldisiloxane, 1,2,2-trifluorovinyltriphenylsilane;
- Silicone monomer containing Si-Cl bond triphenylchlorosilane, methylvinyldichlorosilane, trifluoropropyltrichlorosilane, trifluoropropylmethyldichlorosilane, dimethylphenylchlorosilane , tributylchlorosilane, benzyldimethylchlorosilane;
- Silicone monomer containing Si-OC structure tetramethoxysilane, trimethoxyhydrogensiloxane, n-octyltriethoxysilane, phenyltriethoxysilane, vinyltris(2-methoxy Ethyl ethoxy) silane, triethyl vinyl silane, hexaethylcyclotrisiloxane, 3-(methacryloyloxy)propyl trimethoxy silane, phenyl tris(trimethyl siloxane group Silane, diphenyldiethoxysilane, dodecyltrimethoxysilane, n-octyltriethoxysilane, dimethoxysilane, 3-chloropropyltrimethoxysilane;
- Silicone monomer containing Si-N-Si or Si-O-Si structure hexamethyldisilazide, hexamethylcyclotrisilylamino, hexamethyldisilazane, hexamethyldisiloxane;
- Silicone monomer containing cyclic structure hexamethylcyclotrisiloxane, octamethylcyclotetrasiloxane, hexaphenylcyclotrisiloxane, decamethylcyclopentasiloxane, octaphenyl ring Tetrasiloxane, triphenylhydroxysilane, diphenyldihydroxysilane, bis(tritylsilyl) chromate, trifluoropropylmethylcyclotrisiloxane, 2,2,4,4 -tetramethyl-6,6,8,8-tetraphenylcyclotetrasiloxane, tetramethyltetravinylcyclotetrasiloxane, 3-glycidoxypropyltriethoxysilane, ⁇ - glycidyloxypropyltrimethoxysilane;
- the polyfunctional unsaturated hydrocarbons and hydrocarbon derivatives include:
- the plasma discharge mode is radio frequency discharge, microwave discharge, intermediate frequency discharge, high frequency discharge, and electric spark discharge, and the waveforms of the high frequency discharge and the intermediate frequency discharge are sinusoidal or bipolar pulses, and the radio frequency is A plasma is a plasma generated by discharge of a high-frequency electromagnetic field.
- the microwave method utilizes the energy of the microwave to excite the plasma, and has the advantages of high energy utilization efficiency.
- the electrodeless discharge and the plasma are pure, it is an excellent method for high-quality, high-rate, large-area preparation.
- the motion characteristics of the substrate and the plasma discharge energy are combined.
- the substrate generates motion, improves the deposition efficiency of the coating, and improves the uniformity and compactness of the coating thickness.
- the prepared coating has insulation, waterproof and moisture proof, anti-mold, acid and alkaline solvents, acid and alkali salt spray, acid atmosphere, organic solvent immersion, cosmetics resistance, sweat resistance, cold and heat cycle impact resistance (-40 °C ⁇ +75 ° C), resistance to heat and humidity (humidity 75% ⁇ 95%) and other characteristics.
- the coating thickness is between 1 and 1000 nm, and the influence on the RF communication signal in the range of 10M to 8G is less than 5%.
- the plasma chemical vapor deposition method is more environmentally friendly than the liquid phase three-coating coating method; and the deposition temperature is lower, the speed is faster, and the coating structure and composition are controllable compared to the vapor deposition parylene method. Strong, the monomer is highly selective.
- the substrate moves in the reaction chamber, so that the coating thickness of the substrate at different positions tends to be uniform, which solves the problem that the thickness of the coating on the surface of the substrate is not uniform due to the difference in monomer density in different regions of the reaction chamber.
- the amount of chemical monomer raw materials used in monomer steam is only 10% to 15% of the amount in other prior art, thereby reducing emissions of exhaust gas, making it more environmentally friendly and improving actual production efficiency. It has great significance.
- the present invention screens organic monomers having low dipole moment and high chemical inertness, and controls the free volume and compactness of the coating by the polyfunctional monomer, so that the coating has high insulation and excellent protection at the same time.
- the present invention selects a benzene ring having a high symmetry and a benzene derivative or a perfluoro compound as a monomer, and the polymer after polymerization is symmetrical or each carbon atom is coated with a large amount of fluorine atoms, and the polarity is low, and the dielectric is low.
- the constant is very low, less than 2.7, and the insulation is high;
- the formed polymer has excellent chemical stability
- the invention adopts a method of alternately performing low dipole moment organic coating and silicone coating preparation or organic fluorocarbon coating to form a low dipole moment-silicone/fluorocarbon modulation multilayer dense structure, which can be reduced
- the stress of the coating increases the toughness of the coating.
- the corrosive medium corrodes the coating. When the transverse interface is encountered, the corrosion will develop laterally.
- the present invention employs plasma chemical vapor deposition to obtain a nano-protective coating having a modulated structure by controlling the structure of the monomer and the coating.
- This coating has the following advantages: each cycle consists of a layer of nano-scale low dipole moment and nano-scale silicone coating or organic fluorocarbon coating, the total thickness of the coating is controlled between 20nm-10 ⁇ m; hardness Controllable between HB-4H; excellent insulation performance, underwater resistance and low surface energy; excellent three-proof performance.
- the method of the invention is more than a single long-time coating, and the obtained coating has a bonding strength and a density which are at least 40%-50% and 35%-50%, respectively, and the underwater electric resistance is increased by 40%-50%. .
- the modulation structure coating obtained by alternately circulating the cycle has excellent performance and strong practicability.
- General plasma polymerization uses a monofunctional hydrocarbon-hydrogen organic compound monomer to obtain a coating having a certain cross-linking structure.
- the crosslinked structure is formed by a plurality of active sites formed by chain scission of a monomer during plasma discharge by cross-linking.
- this crosslinked structure is relatively loose, contains more linear components, and is resistant to solution penetration and solubility.
- the silicon-bonded functional groups in the silicone monomer can undergo a condensation reaction with each other, and therefore, a three-dimensional network can occur between the monomer and the monomer.
- Cross-linking can further improve the compactness, wear resistance and corrosion resistance of the coating.
- the hardness of the silicone coating of the same thickness is 1-2 grades higher than that of the conventional coating, and the salt spray resistance is increased by 30-50%.
- portable device keyboard has small and light features, commonly used in computers, mobile phones and other equipment. It makes it easy for users to work on the journey. However, when it encounters the contamination of common liquids, such as the accidental overturn of the water cup, the soaking of rain and sweat, the inside of the keyboard is easily short-circuited and damaged. After coating with this type of nano-coating, it can ensure that the surface of the keyboard is easy to clean and function properly after being exposed to water, so that the keyboard can adapt to a more severe environment.
- LED display has product promotion, store decoration, lighting, warning and other purposes. Some of its uses need to face the harsh environment of rain or dust, such as the rainy days, the mall's open-air LED advertising screen, road warning lights, LED display control panel in the production workshop, these harsh environments lead to LED screen failure, and easy to accumulate dust, It is difficult to clean, and after using the nano-coating, the above problems can be effectively solved.
- fingerprint lock is a smart lock, which integrates computer information technology, electronic technology, mechanical technology and modern hardware technology, is widely used in public security criminal investigation and judicial field. However, after it meets water, its internal circuit is short-circuited, difficult to repair, and requires violent de-locking. This coating can be used to avoid this problem.
- Some sensors need to work in a liquid environment, such as water pressure, oil pressure sensors, and sensors used in underwater operation equipment, as well as sensors that often encounter water in the working environment. These sensors use this coating. After the layer, it can guarantee that the sensor will not malfunction due to the liquid invading the internal structure of the mechanical device.
- the silicone nano-coating prepared by the method can also be applied to the following different environments and related products:
- Acid and alkaline solvents, acid and alkali salt spray, acid resistant atmosphere are acids and alkaline solvents, acid and alkali salt spray, acid resistant atmosphere:
- 1 such as paraffin, olefin, alcohol, aldehyde, amine, ester, ether, ketone, aromatic hydrocarbon, hydrogenated hydrocarbon, terpene olefin, halogenated hydrocarbon, heterocyclic compound, nitrogen-containing compound and sulfur compound solvent; 2 cosmetic packaging container ; 3 fingerprint lock, headphones.
- Resistance to cold and heat cycle (-40 ° C ⁇ +75 ° C), resistance to heat and humidity (humidity 75% ⁇ 95%): electrical, electronic, automotive electrical, such as aviation, automotive, home appliances, scientific research and other fields of equipment.
- a method for preparing a high-insulation nano-protective coating having a modulation structure comprising the steps of:
- the substrate is placed in a reaction chamber of the nano-coating preparation device, the reaction chamber is closed, and the reaction chamber is continuously evacuated, and the vacuum in the reaction chamber is pumped to 10 mTorr, and an inert gas Ar is introduced to open the moving mechanism. , causing the substrate to generate motion in the reaction chamber;
- the substrate in the step (1) is a solid material, the solid material is a bulk aluminum material and a PCB board, and the surface of the substrate is prepared to be exposed to cold and heat after being subjected to a cold and heat resistant cyclic impact coating. In a loop test environment.
- the reaction chamber is a rotating body chamber
- the volume of the reaction chamber is 50 L
- the temperature of the reaction chamber is controlled at 30 ° C
- the flow rate of the inert gas is 5 sccm.
- the substrate moves in the reaction chamber, and the substrate moves in the form of a circular motion of the substrate relative to the reaction chamber at a rotation speed of 10 rpm.
- the monomer A vapor component comprises:
- the low dipole moment organic monomer is: 1,8-diiodo perfluorooctane,
- the two polyfunctional unsaturated hydrocarbons and hydrocarbon derivatives are: 1,3-butadiene, ethoxylated trimethylolpropane triacrylate;
- the monomer B vapor component comprises:
- the monofunctional unsaturated fluorocarbon resin is: 2-(perfluorododecyl)ethyl acrylate
- the three polyfunctional unsaturated hydrocarbons and hydrocarbon derivatives are: 1,4-pentadiene, tripropylene glycol diacrylate, 1,6-hexanediol diacrylate;
- the flow of the monomer A and the monomer B is carried out by atomizing and volatilizing the monomer through a feed pump and introducing into the reaction chamber from a low pressure of 10 mTorr, wherein the flow rates of the monomer A and the monomer B are both 10 ⁇ L/min;
- the monomer A vapor or the monomer B vapor is introduced, the plasma is discharged, and the chemical vapor deposition is performed.
- the plasma discharge process is a small power continuous discharge, specifically including the following deposition process. :
- the deposition process includes the pretreatment stage and the coating stage.
- the plasma discharge power of the pretreatment stage is 150W, the discharge time is 450s, and then enters the coating stage.
- the plasma discharge power is adjusted to 10W and the continuous discharge time is 3600s.
- the plasma discharge mode is radio frequency discharge
- the plasma discharge is stopped, the vacuum is continuously applied, and the vacuum of the reaction chamber is maintained at 10 mTorr. After 1 min, air is introduced to an atmospheric pressure, and then the substrate is taken out.
- the dielectric constant of the coating obtained by the above process is 2.73. After coating the aluminum material and PCB board, the cold and thermal cycle impact test results are as follows:
- a method for preparing a high-insulation nano-protective coating having a modulation structure comprising the steps of:
- the substrate in the step (1) is a solid material, and the solid material is a bulk aluminum material, and any interface of the surface of the substrate after the preparation of the moisture-resistant heat alternating coating can be exposed to the damp heat test environment.
- the reaction chamber is a cubic chamber, the volume of the reaction chamber is 270 L, the temperature of the reaction chamber is controlled at 42 ° C, and the flow rate of the inert gas is 18 sccm.
- the substrate is subjected to planetary motion, the revolution speed is 4 rpm, and the rotation speed is 10 rpm.
- the monomer A vapor is introduced into the reaction chamber to a vacuum of 70 mTorr, plasma discharge is started, chemical vapor deposition is performed, the monomer A vapor is stopped, the monomer C vapor is introduced, and the plasma discharge is continued. Chemical vapor deposition, stopping the passage of monomer C vapor;
- the monomer A vapor component comprises:
- the three low dipole moment organic monomers are: polydimethylsiloxane having a molecular weight of 50,000, decafluorobiphenyl ketone, and hexafluoropropylene;
- the polyfunctional unsaturated hydrocarbon and hydrocarbon derivative are: ethylene glycol diacrylate;
- the monomer C vapor component comprises:
- the organosilicon monomer containing a double bond structure is: vinyl tributol sulfonyl silane,
- the four polyfunctional unsaturated hydrocarbons and hydrocarbon derivatives are: isoprene, 1,4-pentadiene, tripropylene glycol diacrylate, diethylene glycol divinyl ether;
- the flow of the monomer A and the monomer C is carried out by atomizing and volatilizing the monomer through a feed pump and introducing the reaction chamber into the reaction chamber by a low pressure of 30 mTorr, wherein the flow rates of the monomer A and the monomer C are both 85 ⁇ L/min;
- a monomer A vapor or a monomer C vapor is introduced, a plasma discharge is performed, and a chemical vapor deposition is performed.
- the plasma discharge process is a small power continuous discharge, specifically including the following deposition process 5 Times:
- the deposition process includes a pretreatment stage and a coating stage.
- the plasma discharge power of the pretreatment stage is 600 W, the discharge time is 60 s, and then enters the coating stage.
- the plasma discharge power is adjusted to 150 W and the continuous discharge time is 600 s.
- the plasma discharge mode is microwave discharge
- the plasma discharge is stopped, the vacuum is continuously applied, and the vacuum of the reaction chamber is maintained at 60 mTorr. After 2 minutes, the air is introduced to an atmospheric pressure, and then the substrate is taken out.
- the dielectric constant of the coating obtained by the above process is 2.45.
- the thermal and thermal cycling impact test results are as follows:
- a method for preparing a high-insulation nano-protective coating having a modulation structure comprising the steps of:
- the substrate in the step (1) is a solid material
- the solid material is a bulk polytetrafluoroethylene plate and an electrical component
- any interface of the block-shaped polytetrafluoroethylene plate is exposed after the preparation of the anti-fungal coating.
- the surface of the electrical component can be exposed to the environment described in the international industrial waterproof rating standard IPX7 after the waterproof and electrical breakdown coating is prepared.
- the reaction chamber is a rotating body chamber
- the volume of the reaction chamber is 580 L
- the temperature of the reaction chamber is controlled at 53 ° C
- the flow rate of the inert gas is 65 sccm.
- the substrate was subjected to a circular motion at a rotation speed of 12 rpm.
- the monomer A vapor component comprises:
- the four low dipole moment organic monomers are: toluene, ⁇ -methyl styrene, dimethyl siloxane, decafluorobiphenyl ketone,
- the two polyfunctional unsaturated hydrocarbons and hydrocarbon derivatives are: isoprene, neopentyl glycol diacrylate;
- the monomer C vapor component comprises:
- the five Si-Cl-containing silicone monomers are: triphenylchlorosilane, trifluoropropylmethyldichlorosilane, dimethylphenylchlorosilane, tributylchlorosilane, benzyl dimethyl Chlorosilane,
- the two polyfunctional unsaturated hydrocarbons and hydrocarbon derivatives are: polyethylene glycol diacrylate, 1,6-hexanediol diacrylate;
- the flow of the monomer A and the monomer C is carried out by atomizing and volatilizing the monomer through a feed pump and introducing into the reaction chamber from a low pressure of 80 mTorr, wherein the flow rates of the monomer A and the monomer C are both 440 ⁇ L/min;
- a monomer A vapor is introduced or a monomer C vapor is introduced, and a plasma discharge is performed to perform chemical vapor deposition.
- the plasma discharge process is a pulse discharge during the deposition process, and specifically includes the following deposition process:
- the deposition process includes pretreatment stage and coating stage.
- the plasma discharge power of the pretreatment stage is 150W, the discharge time is 450s, and then enters the coating stage.
- the coating stage is pulse discharge, power 10W, time 3600s, pulse discharge frequency is 1HZ, pulse The duty cycle is 1:500;
- the plasma discharge mode is an electric spark discharge
- the plasma discharge is stopped, the vacuum is continuously applied, the vacuum of the reaction chamber is maintained at 100 mTorr, and after 3 minutes, air is introduced to an atmospheric pressure, and then the substrate is taken out.
- the dielectric constant of the coating obtained by the above process was 2.46, and the GJB150.10A-2009 mold test result after coating the polytetrafluoroethylene plate:
- IPX 7 waterproof rating test (underwater 1m water immersion test 30min) results:
- a method for preparing a high-insulation nano-protective coating having a modulation structure comprising the steps of:
- the substrate in the step (1) is a solid material
- the solid material is a bulk polytetrafluoroethylene plate and an electrical component
- any interface of the block-shaped polytetrafluoroethylene plate is exposed after the preparation of the anti-fungal coating.
- the surface of the electrical component can be exposed to the environment described in the international industrial waterproof rating standard IPX7 after the waterproof and electrical breakdown coating is prepared.
- the volume of the reaction chamber in the step (1) was 640 L, the temperature of the reaction chamber was controlled at 54 ° C, and the flow rate of the inert gas was 240 sccm.
- the substrate was linearly reciprocated at a moving speed of 23 mm/min.
- the monomer A vapor component comprises:
- the five low dipole moment organic monomers are: p-xylene, 1H, 1H-perfluorooctylamine, 2-(perfluorooctyl)ethyl methacrylate, 1,1,2,2- Tetrahydroperfluorohexyl iodide, 2,4,6-tris(perfluoroheptyl)-1,3,5-triazine,
- the three polyfunctional unsaturated hydrocarbons and hydrocarbon derivatives are: isoprene, tripropylene glycol diacrylate, polyethylene glycol diacrylate;
- the monomer B vapor component comprises:
- the four monofunctional unsaturated fluorocarbon resins are: 2-(perfluorobutyl)ethyl acrylate, (perfluorocyclohexyl) methacrylate, 3,3,3-trifluoro-1-propene Alkyne, 4-ethynyl trifluorotoluene,
- the four polyfunctional unsaturated hydrocarbons and hydrocarbon derivatives are: isoprene, 1,4-pentadiene, polyethylene glycol diacrylate, 1,6-hexanediol diacrylate;
- the flow of the monomer A and the monomer B is carried out by atomizing and volatilizing the monomer through a feed pump and introducing the reaction chamber into the reaction chamber by a low pressure of 100 mTorr, wherein the flow rates of the monomer A and the monomer B are both 1000 ⁇ L/min;
- a monomer A vapor is introduced or a monomer B vapor is introduced, and a plasma discharge is performed to perform chemical vapor deposition.
- the plasma discharge process is a pulse discharge during the deposition process, specifically including the following deposition process seven times. :
- the deposition process includes pretreatment stage and coating stage.
- the plasma discharge power of the pretreatment stage is 600W, the discharge time is 60s, and then enters the coating stage.
- the coating stage is pulse discharge, power 300W, time 600s, pulse discharge frequency is 1000HZ, pulse The duty ratio is 1:1;
- the plasma discharge mode is a high frequency discharge, and the waveform of the high frequency discharge is a sine;
- the dielectric constant of the coating obtained by the above process was 2.48. After the coating of the polytetrafluoroethylene plate, the GJB150.10A-2009 mold test results:
- IPX 7 waterproof rating test (underwater 1m water immersion test 30min) results:
- a method for preparing a high-insulation nano-protective coating having a modulation structure comprising the steps of:
- the substrate in the step (1) is a solid material, and the solid material is a bulk aluminum material, and any interface of the substrate surface can be exposed to an acid or alkali test environment after preparing an acid-proof and alkaline environment coating. .
- the volume of the reaction chamber in the step (1) was 1000 L, the temperature of the reaction chamber was controlled at 60 ° C, and the flow rate of the inert gas was 300 sccm.
- the substrate was subjected to a curve reciprocating motion at a speed of 50 mm/min.
- the monomer A vapor is introduced into the reaction chamber to a vacuum of 300 mTorr, plasma discharge is started, chemical vapor deposition is performed, the monomer A vapor is stopped, the monomer C vapor is introduced, and the plasma discharge is continued. Chemical vapor deposition, stopping the passage of monomer C vapor;
- the monomer A vapor component comprises:
- the six low dipole moment organic monomers are: benzene, ⁇ -methylstyrene, dimethylsiloxane, allylbenzene, 2-(perfluorobutyl)ethyl methacrylate, 1, 1,2,2-tetrahydroperfluorohexyl iodide,
- the three polyfunctional unsaturated hydrocarbons and hydrocarbon derivatives are: 1,4-pentadiene, polyethylene glycol diacrylate, 1,6-hexanediol diacrylate;
- the monomer C vapor component comprises:
- the four Si-OC structure-containing silicone monomers are: trimethoxyhydrogensiloxane, n-octyltriethoxysilane, triethylvinylsilane, 3-(methacryloyloxy)propane Trimethoxysilane,
- the three polyfunctional unsaturated hydrocarbons and hydrocarbon derivatives are: 1,4-pentadiene, ethoxylated trimethylolpropane triacrylate, polyethylene glycol diacrylate;
- the flow of the monomer A and the monomer C is carried out by atomizing and volatilizing the monomer through a feed pump and introducing into the reaction chamber from a low pressure of 200 mTorr, wherein the flow rates of the monomer A and the monomer C are both 780 ⁇ L/min;
- a monomer A vapor is introduced or a monomer C vapor is introduced, and a plasma discharge is performed to perform chemical vapor deposition.
- the plasma discharge process is alternately discharged periodically, specifically including the following deposition process. :
- the deposition process includes the pretreatment stage and the coating stage.
- the plasma discharge power of the pretreatment stage is 150W
- the continuous discharge time is 450s
- the coating stage is the periodic alternating discharge output, power 10W, time 3600s, alternating frequency At 1 Hz, the plasma cycle alternates with the discharge output waveform as a sawtooth waveform.
- the plasma discharge mode is an intermediate frequency discharge, and the waveform of the intermediate frequency discharge is a bipolar pulse;
- the substrate obtained after the removal of the substrate can be obtained by the above process and the aluminum material after the coating, and the test results are as follows:
- a method for preparing a high-insulation nano-protective coating having a modulation structure comprising the steps of:
- the substrate is a solid material, which is a bulk aluminum material and an electrical component, and any interface of the substrate surface after the preparation of the high insulating coating can be exposed to the organic solvent test environment.
- the volume of the reaction chamber in the step (1) was 400 L, the temperature of the reaction chamber was controlled at 40 ° C, and the flow rate of the inert gas was 150 sccm.
- the substrate was subjected to a curve reciprocating motion at a speed of 30 mm/min.
- the monomer A vapor is introduced into the reaction chamber to a vacuum of 230 mTorr, plasma discharge is started, chemical vapor deposition is performed, the monomer A vapor is stopped, the monomer C vapor is introduced, and the plasma discharge is continued. Chemical vapor deposition, stopping the passage of monomer C vapor;
- the monomer A vapor component comprises:
- the five low dipole moment organic monomers are: allylbenzene, decafluorobiphenyl ketone, hexafluoropropylene, 1H, 1H-perfluorooctylamine, perfluorooctyl iodine,
- the four polyfunctional unsaturated hydrocarbons and hydrocarbon derivatives are: 1,4-pentadiene, ethoxylated trimethylolpropane triacrylate, polyethylene glycol diacrylate, 1,6- Hexanediol diacrylate;
- the monomer C vapor component comprises:
- silicone monomers containing a cyclic structure hexaphenylcyclotrisiloxane, octaphenylcyclotetrasiloxane, diphenyldihydroxysilane, bis(tritylsilyl) chromate Ester, trifluoropropylmethylcyclotrisiloxane, 2,2,4,4-tetramethyl-6,6,8,8-tetraphenylcyclotetrasiloxane,
- the four polyfunctional unsaturated hydrocarbons and hydrocarbon derivatives are: 1,3-butadiene, isoprene, ethoxylated trimethylolpropane triacrylate, ethylene glycol diacrylate;
- the flow of the monomer A and the monomer C is carried out by atomizing and volatilizing the monomer through a feed pump and introducing into the reaction chamber from a low pressure of 160 mTorr, wherein the flow rates of the monomer A and the monomer C are both 460 ⁇ L/min;
- a monomer A vapor is introduced or a monomer C vapor is introduced, and a plasma discharge is performed to perform chemical vapor deposition.
- the plasma discharge process is periodically alternately discharged, specifically including the following deposition process. Times:
- the deposition process includes the pretreatment stage and the coating stage.
- the plasma discharge power of the pretreatment stage is 600W
- the discharge time is 60s
- the plasma in the coating stage is the cycle alternating discharge output, power 300W, time 600s, alternating frequency At 1000 Hz, the plasma cycle alternately changes the discharge output waveform to a half-wave rectified waveform.
- the plasma discharge mode is microwave discharge
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Abstract
Description
Claims (10)
- 一种具有调制结构的高绝缘纳米防护涂层的制备方法,其特征在于:包括以下步骤:(1)前处理:将基材置于纳米涂层制备设备的反应腔室内,对反应腔室连续抽真空,将反应腔室内的真空度抽到10~200毫托,并通入惰性气体He、Ar或He和Ar混合气体,开启运动机构,使基材在反应腔室内产生运动;(2)高绝缘纳米涂层的制备:进行以下步骤至少一次,在基材表面制备高绝缘调制结构的纳米涂层:通入单体A蒸汽到反应腔室内,至真空度为30~300毫托,开启等离子体放电,进行化学气相沉积,停止通入单体A蒸汽,通入单体B或单体C蒸汽,继续等离子体放电,进行化学气相沉积,停止通入单体B或单体C蒸汽;所述单体A蒸汽成分包括:至少一种低偶极矩有机物单体和至少一种多官能度不饱和烃及烃类衍生物的混合物,所述单体A蒸汽中多官能度不饱和烃及烃类衍生物所占的质量分数为15~65%;所述单体B蒸汽成分包括:至少一种单官能度不饱和氟碳树脂和至少一种多官能度不饱和烃及烃类衍生物的混合物,所述单体B蒸汽中多官能度不饱和烃及烃类衍生物所占的质量分数为15~65%;所述单体C蒸汽成分包括:至少一种含双键、Si-Cl、Si-O-C、Si-N-Si、Si-O-Si结构或环状结构的有机硅单体和至少一种多官能度不饱和烃及烃类衍生物的混合物,所述单体C蒸汽中多官能度不饱和烃类衍生物所占的质量分数为15~65%;所述通入单体A、单体B和单体C的流量均为10~1000μL/min;(3)后处理:停止等离子体放电,持续抽真空,保持反应腔室真空度为10~200毫托,1~5min后通入空气至一个大气压,停止基材的运动,然后取出基材即可;或者,停止等离子体放电,向反应腔室内充入空气或惰性气体至压力2000-5000毫托,然后抽真空至10-200毫托,进行上述充气和抽真空步骤至少一次,通入空气至一个大气压,停止基材的运动,然后取出基材即可。
- 根据权利要求1所述的一种具有调制结构的高绝缘纳米防护涂层的制备方法,其特征在于:所述步骤(1)中基材在反应腔室内产生运动,基材运动形式为基材相对反应腔室进行直线往复运动或曲线运动,所述曲线运动包括圆周运动、椭圆周运动、行星运动、球面运动或其他不规则路线的曲线运动。
- 根据权利要求1所述的一种具有调制结构的高绝缘纳米防护涂层的制备方法,其特征在于:所述步骤(1)中基材为固体材料,所述固体材料为电子产品、电器部件、电子组装半成品,PCB板、金属板、聚四氟乙烯板材或者电子元器件,且所述基材表面制备有机硅纳米涂层后其任一界面可暴露于水环境,霉菌环境,酸、碱性溶剂环境,酸、碱性盐雾环境,酸性大气环境,有机溶剂浸泡环境,化妆品环境,汗液环境,冷热循环冲击环境或湿热交变环境中使用。
- 根据权利要求1所述的一种具有调制结构的高绝缘纳米防护涂层的制备方法,其特征在于:所述步骤(1)中反应腔室为旋转体形腔室或者立方体形腔室,其容积为50~1000L,反应腔室的温度控制在30~60℃,所述惰性气体通入流量为5~300sccm。
- 根据权利要求1所述的一种具有调制结构的高绝缘纳米防护涂层的制备方法,其特征在于:所述步骤(2)中:通入单体A蒸汽、通入单体B蒸汽或通入单体C蒸汽,等离子体放电,进行化学气相沉积,沉积过程中等离子体放电过程包括小功率连续放电、脉冲放电或周期交替放电。
- 根据权利要求5所述的一种具有调制结构的高绝缘纳米防护涂层的制备方法,其特征在于:所述沉积过程中等离子体放电过程为小功率连续放电,具体包括以下沉积过程至少一次:沉积过程包括预处理阶段和镀膜阶段,预处理阶段等离子体放电功率为150~600W,持续放电时间60~450s,然后进入镀膜阶段,调整等离子体放电功率为10~150W,持续放电时间600~3600s。
- 根据权利要求5所述的一种具有调制结构的高绝缘纳米防护涂层的制备方法,其特征在于:所述沉积过程中等离子体放电过程为脉冲放电,具体包括以下沉积过程至少一次:沉积过程包括预处理阶段和镀膜阶段,预处理阶段等离子体放电功率为150~600W,持续放电时间60~450s,然后进入镀膜阶段,镀膜阶段为脉冲放电,功率10~300W,时间600s~3600s,脉冲放电的频率为1~1000HZ,脉冲的占空比为1:1~1:500。
- 根据权利要求5所述的一种具有调制结构的高绝缘纳米防护涂层的制备方法,其特征在于:所述沉积过程中等离子体放电过程为周期交替放电,具体包括以下沉积过程至少一次:沉积过程包括预处理阶段和镀膜阶段,预处理阶段等离子体放电功率为150~600W,持续放电时间60~450s,然后进入镀膜阶段,镀膜阶段等离子体为周期交替变化放电输出,功率10~300W,时间600s~3600s,交变频率为1-1000Hz,等离子体周期交替变化放电输出波形为锯齿波形、正弦波形、方波波形、全波整流波形或半波整流波形。
- 根据权利要求1所述的一种具有调制结构的高绝缘纳米防护涂层的制备方法,其特征在于:所述低偶极矩有机物单体包括:对二甲苯、苯、甲苯、四氟化碳、α-甲基苯乙烯、聚对二氯甲苯、二甲基硅氧烷、分子量500-50000的聚二甲基硅氧烷、烯丙苯、十氟联苯、十氟联苯酮、全氟烯丙基苯、四氟乙 烯、六氟丙烯、1H,1H-全氟辛基胺、全氟碘代十二烷、全氟三丁胺、1,8-二碘代全氟辛烷、全氟己基碘烷、全氟碘代丁烷、全氟碘代癸烷、全氟辛基碘烷、1,4-二(2',3'-环氧丙基)全氟丁烷、十二氟-2-甲基-2-戊烯、2-(全氟丁基)乙基甲基丙烯酸酯、2-(全氟辛基)乙基甲基丙烯酸酯、2-(全氟辛基)碘代乙烷、全氟癸基乙基碘、1,1,2,2-四氢全氟己基碘、全氟丁基乙烯、1H,1H,2H-全氟-1-癸烯、2,4,6-三(全氟庚基)-1,3,5-三嗪、全氟己基乙烯、3-(全氟正辛基)-1,2-环氧丙烷、全氟环醚、全氟十二烷基乙烯、全氟十二烷基乙基碘、二溴对二甲苯、1,1,4,4-四苯基-1,3-丁二烯;所述单官能度不饱和氟碳树脂包括:3-(全氟-5-甲基己基)-2-羟基丙基甲基丙烯酸酯、2-(全氟癸基)乙基甲基丙烯酸酯、2-(全氟己基)乙基甲基丙烯酸酯、2-(全氟十二烷基)乙基丙烯酸酯、2-全氟辛基丙烯酸乙酯、1H,1H,2H,2H-全氟辛醇丙烯酸酯、2-(全氟丁基)乙基丙烯酸酯、(2H-全氟丙基)-2-丙烯酸酯、(全氟环己基)甲基丙烯酸酯、3,3,3-三氟-1-丙炔、1-乙炔基-3,5-二氟苯或4-乙炔基三氟甲苯;所述含双键、Si-Cl、Si-O-C、Si-N-Si、Si-O-Si结构或环状结构的有机硅单体包括:含双键结构的有机硅单体:烯丙基三甲氧基硅烷、乙烯基三乙氧基硅烷、乙烯基三甲基硅烷、3-丁烯基三甲基硅烷、乙烯基三丁酮肟基硅烷、四甲基二乙烯基二硅氧烷、1,2,2-三氟乙烯基三苯基硅烷;含Si-Cl键的有机硅单体:三苯基氯硅烷、甲基乙烯基二氯硅烷、三氟丙基三氯硅烷、三氟丙基甲基二氯硅烷、二甲基苯基氯硅烷、三丁基氯硅烷、苄基二甲基氯硅烷;含Si-O-C结构的有机硅单体:四甲氧基硅烷、三甲氧基氢硅氧烷、正辛基三乙氧基硅烷、苯基三乙氧基硅烷、乙烯基三(2-甲氧基乙氧基)硅烷、三乙基乙烯基硅烷、六乙基环三硅氧烷、3-(甲基丙烯酰氧)丙基三甲氧基硅烷、苯基三(三甲基硅氧烷基)硅烷、二苯基二乙氧基硅烷、十二烷基三甲氧基硅烷、正辛基三乙氧基硅烷、二甲氧基硅烷、3-氯丙基三甲氧基硅烷;含Si-N-Si或Si-O-Si结构的有机硅单体:六甲基二硅烷基胺、六甲基环三硅烷氨基、六甲基二硅氮烷、六甲基二硅醚;含环状结构的有机硅单体:六甲基环三硅氧烷、八甲基环四硅氧烷、六苯基环三硅氧烷、十甲基环五硅氧烷、八苯基环四硅氧烷、三苯基羟基硅烷、二苯基二羟基硅烷、铬酸双(三苯甲基硅烷基)酯、三氟丙基甲基环三硅氧烷、2,2,4,4-四甲基-6,6,8,8-四苯基环四硅氧烷、四甲基四乙烯基环四硅氧烷、3-缩水甘油醚氧基丙基三乙氧基硅烷、γ-缩水甘油醚氧丙基三甲氧基硅烷;所述多官能度不饱和烃及烃类衍生物包括:1,3-丁二烯、异戊二烯、1,4-戊二烯、乙氧基化三羟甲基丙烷三丙烯酸酯、二缩三丙二醇二丙烯酸酯、聚乙二醇二丙烯酸酯、1,6-己二醇二丙烯酸酯、二丙烯酸乙二醇酯、二乙二醇二乙烯基醚或二丙烯酸新戊二醇酯。
- 根据权利要求1所述的一种具有调制结构的高绝缘纳米防护涂层的制备方法,其特 征在于:所述步骤(2)中,等离子体放电方式为射频放电、微波放电、中频放电、高频放电、电火花放电,所述高频放电和中频放电的波形为正弦或双极脉冲。
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CN113943933B (zh) * | 2020-07-16 | 2023-09-29 | 江苏菲沃泰纳米科技股份有限公司 | 多层结构的复合膜及其制备方法和产品 |
CN114552201A (zh) * | 2022-04-22 | 2022-05-27 | 中国电子科技集团公司第二十九研究所 | 一种适用于高频印制天线的高透波高防腐涂层制备方法 |
CN114552201B (zh) * | 2022-04-22 | 2022-07-05 | 中国电子科技集团公司第二十九研究所 | 一种适用于高频印制天线的高透波高防腐涂层制备方法 |
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JP6937430B2 (ja) | 2021-09-22 |
BR112020003338B1 (pt) | 2024-03-12 |
BR112020003338A2 (pt) | 2020-09-15 |
KR102373702B1 (ko) | 2022-03-11 |
EP3674438A4 (en) | 2020-09-02 |
EP3674438B1 (en) | 2023-03-29 |
EP3674438A1 (en) | 2020-07-01 |
CN107587120A (zh) | 2018-01-16 |
KR20200045480A (ko) | 2020-05-04 |
JP2020531690A (ja) | 2020-11-05 |
CN107587120B (zh) | 2018-12-18 |
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