CN101654778A - Method for preparing insulating heat conducting ceramic coating from polymer precursor - Google Patents
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Abstract
The invention relates to a method for preparing an insulating heat conducting ceramic coating, which is prepared from one or more of polymer precursors such as polysilazane, polysiloxane and polycarbosilane serving as a base material, and multiple kinds of ceramic packing and active fillers as well as solvent and various auxiliary agents, and is prepared by the following steps of: 1, adding a certain amount of fillers, solvent and auxiliary agents into a polymer precursor, stirring the mixture evenly, and preparing the mixture into slurry after high-speed grinding; 2, coating the slurry on thesurface of a treated substrate material (comprising metal, ceramic, graphite, a C/C composite material and the like) in a brush coating or spray coating mode; 3, performing vacuum heat treatment on the substrate material with a coating at a temperature of between 100 and 300 DEG C for 1 to 2 hours to ensure that the polymer precursor performs a cross-linking reaction; and 4, performing high-temperature treatment on the treated material under the protection of a gas, namely treating the material at a temperature of between 400 and 1,000 DEG C for 1 to 5 hours, and then naturally cooling to obtain a ceramic coating on the surface of the substrate material. The insulating heat conducting ceramic coating has the characteristics of simple coating and heat treatment technology, excellent insulating property and heat conductivity, good high temperature resistance, excellent high-temperature cracking resistance and the like. The method can be widely applied in electronic and electrical industry.
Description
Technical field:
The present invention relates to the method that a kind of preparation has the ceramic coating of excellent insulation, heat conduction and mechanical property, reach ceramic coating, a kind of insulating heat-conductive coating that can be used for the electron and electrician industry according to method for preparing.Belong to the coating preparation field.
Background technology:
The advanced ceramics material has obtained using widely in various engineering machinery, equipment and member with high temperature resistant, corrosion-resistant, the abrasion resistance properties of its excellence.Along with the exploitation of high performance ceramic material and the expansion of new application, some stupaliths also more and more are subjected to the attention of electron and electrician industry with its excellent insulativity, thermotolerance, thermal conductivity and low-shrinkage energy simultaneously.Up to the present, the stupalith that has been successfully applied to the Electronic Packaging industry has LTCC (LTCC) and high temperature sintering aluminium nitride ceramics (AlN): LTCC has good thermotolerance and insulating property, but its heat conductivility is lower; The AlN pottery has excellent thermal conductivity, insulativity and low-shrinkage, but its sintering temperature causes its tooling cost can not to be in any more up to 1800 ℃.In actual applications, insulation is a pair of contradiction with heat conduction: metal is good heat conductor, is again good electro-conductive material simultaneously; Pottery has excellent insulativity, but will accomplish that good heat conduction is very difficult.How the thermal conductivity of metal and the insulativity of pottery are integrated, can significantly reduce cost again simultaneously, become a challenge of current type material exploitation.One of effective means that metallic surface ceramic coating technology addresses this problem beyond doubt.Metallic substance has played insulation, heat-resisting, corrosion-resistant, the effect of resistance to wearing by means of ceramic coating, also kept the advantage such as high strength, high thermal conductivity, high tenacity of self.
In the Electronic Packaging industry, the most crucial technology that is used for the insulating metal substrate of great-power electronic product heat radiation is exactly the design of the insulating layer material between circuit layer and the metal-based layer, the heat-conductive characteristic of insulation layer is good more, the diffusion of the heat that produces when just helping the device operation more also just helps reducing the operating temperature of device more.The insulativity of ceramic coating, thermotolerance and heat conductivility obviously are better than the resene coating, have become the main direction of studying of great-power electronic product heat transmission insulating metal substrate.In present stage, ceramic layer production method the most frequently used in the industrial production mainly contains: 1, and spraying method-comprise plasma spraying, thermospray, detonation flame spraying; 2, vapour deposition process-comprise chemical vapour deposition, physical vapor deposition; 3, burn method-comprise high temperature co-firing method, low temperature co-fired method altogether; 4, electrochemical process-comprise anonizing, differential arc oxidation method.Above-mentioned ceramic coating production technique mainly is in order to solve wear-resistant, high temperature resistant, the corrosion resistant application requiring of metallic substance.And for insulativity and thermal conductivity that the great-power electronic package application requires, mainly is at present the improvement that relies on technologies such as traditional low temperature co-fired method, anonizing and differential arc oxidation methods, adapting to the requirement of packaging process, but effect is still not remarkable.
Polymeric preceramic body material is by chemical process synthetic one class organic polymer, generally contains silicon, and it can cracking take place in certain temperature range, be converted into amorphous or xln ceramic.Vowed that the island sage makes in 1975 and wait the people to utilize Polycarbosilane (PCS), successfully prepare the SiC ceramic fiber, opened up the frontier of organic precursor method to the inorganic ceramic conversion.The development of the China's national defense University of Science and Technology and Chinese Academy of Sciences chemistry place precursor in recent years, and adopt aspects such as Stainless Steel via Precursor Pyrolysis ceramic fiber and ceramic matric composite to obtain bigger progress.Because the split product of precursor is a stupalith, it has stable high-temperature performance and is approaching with the thermal expansivity of ceramic base material; Simultaneously precursor has good fluidity again, is shaped convenient and structure, component such as can design at characteristics as organic polymer material, than the traditional preparation process technology, it is lower that the Stainless Steel via Precursor Pyrolysis ceramic product has a preparation temperature, the purity height of gained pottery, advantages such as convenient formation are pottery and ceramic matric composite one of the most promising preparation methods.
Summary of the invention:
The objective of the invention is that the polymeric preceramic body is changed into ceramic technology and ceramic coating technology and combine,, on substrate material surface, make one deck and have good insulativity, thermal conductivity and stable on heating ceramic coating with more easy method.This coating can be used as the circuit layer of insulating metal substrate and the insulation layer between the metal-based layer, is the critical material that preparation has the insulating metal substrate of high thermal conductivity.
The present invention is to be base-material with polymeric preceramic body such as polysilazane, polysiloxane and Polycarbosilane, in wherein adding ceramic packings such as aluminium nitride, silicon nitride, tantalum nitride, boron nitride, silicon carbide, norbide, silicon oxide, aluminum oxide one or more, and in the titanium, silicon, aluminium, boron isoreactivity filler one or more.Add certain amount of solvent simultaneously in order to the adjusting slurry viscosity, and add silane coupling agent to improve the wettability of polymeric preceramic body to filler.The polymeric preceramic body is overflowed having micro-molecular gas in the process of ceramic conversion, therefore mass loss takes place and causes volumetric shrinkage, makes can produce defectives such as hole and crackle in the ceramic product, has influence on the integrity and the bond strength of goods.Ceramic packing used in the present invention belongs to inert filler, wherein fillers such as aluminium nitride, tantalum nitride, boron nitride, silicon carbide play the effect that improves thermal conductivity on the one hand, its particle also has volume effect on the other hand, can reduce the volumetric shrinkage of precursor in the ceramic conversion process; Therefore silicon oxide can become molten state because its fusing point is lower under temperature of reaction, just can fill the precursor cracking and the crack and the hole that produce; Titanium, silicon, aluminium isoreactivity filler the polymeric preceramic body in the process of ceramic conversion can with its split product generation series of chemical, produce relevant carbide, nitride or oxide compound, be the effective way that reduces void content and shrinking percentage; Suitable surface reaction also can take place with the element in the base material in active filler, promotes the interface combination, improves the bond strength of coating.By adding suitable inert filler and active filler, can obviously reduce polymeric preceramic body defective such as the crackle that produces and hole in the process that is converted into pottery, obtain having good bond intensity, leakless and ceramic coating hole, surface compact.
The used polysilazane of the present invention be a kind of on main chain the polymkeric substance of Siliciumatom and the alternate Cheng Jian of nitrogen-atoms.Its structural unit is generally:
N in the formula, m are the polymerization degree.Polysilazane can be converted into the SiC/Si3N4 complex phase ceramic behind Pintsch process, itself just has good thermotolerance, insulativity and thermal conductivity, after adding the thermal conductive ceramic filler, by the thermal conductivity of its ceramic coating that makes (〉=30W/m.K) far above the thermal conductivity (1.1～2.2W/m.K) of the polymeric coating that contains heat conductive filler.
Be the method that precursor prepares insulating heat conducting ceramic coating with the polysilazane among the present invention, calculate by weight and carry out as follows:
1) in 100 parts of polysilazane, add 10～30 parts of 0～10 part of 0～10 part of 0～10 part of 10～30 parts of aluminium nitride fillers, tantalum nitride filler, boron nitride filler, silicon nitride filler, silicon carbide filler, 0～10 part of the norbide filler handled with silane coupling agent in advance, 0～10 part of silica flour, 0～5 part in boron powder.Add 10～100 parts of aromatic solvent or ester solvents then, after the dispersed with stirring, use three-stage roll mill to grind, obtain the uniform slurry of packing material size between 0.01～10 micron;
2) base material is generally selected copper, aluminium, molybdenum-copper, aluminium/silicon carbide alloys, graphite etc. for use, adopts machinery or electrochemical method that substrate material surface is carried out pre-treatment, is cleaned, dry, smooth workpiece surface.With the mode of brushing or spray slurry is coated with then and is contained in the substrate material surface of handling;
3) with the base material of coating 100 ℃～300 ℃ following vacuum heat treatment 1～2 hour, remove the solvent in the coating paste, and make polysilazane generation crosslinking reaction;
4) under protective atmosphere, the material after handling is carried out pyroprocessing, promptly between 400 ℃～1000 ℃ temperature, handled 1～5 hour, slowly cooling obtains the ceramic coating on the base material afterwards.Described protective atmosphere is meant nitrogen, ammonia or rare gas element.
The used polysiloxane of the present invention is a kind of polymkeric substance that contains Siliciumatom and Sauerstoffatom on main chain.With methyl silsesquioxane (PSO
3/2) be example, its structural unit can be expressed as:
R1 and R2 are alkyl or phenyl in the formula, and n is the polymerization degree.Can find out PSO from following formula
3/2Si in the molecule: O=1: 1.5.The amorphous pottery of SiOC that cracking is converted into excellent property takes place in polysiloxane at a certain temperature, and the ceramic yield height, is the low-cost desirable precursor of making high performance ceramic material.
Be the method that precursor prepares insulating heat conducting ceramic coating with the polysiloxane among the present invention, calculate by weight and carry out as follows:
1) in 100 parts of polysiloxane, adds 10～30 parts of 10～30 parts of 10～20 parts of alumina packings, silicon carbide filler, norbide fillers, 0～20 part of the silica filler handled with silane coupling agent in advance, 0～10 part in AL powder, 0～5 part of silica flour.Add 10～100 parts of aromatic solvent or ester solvents then, after the dispersed with stirring, use three-stage roll mill to grind, obtain the uniform slurry of packing material size between 0.01～10 micron;
2) base material is generally selected copper, aluminium, molybdenum-copper, aluminium/silicon carbide alloys, graphite etc. for use, adopts machinery or electrochemical method that substrate material surface is carried out pre-treatment, is cleaned, dry, smooth workpiece surface.With the mode of brushing or spray slurry is coated with then and is contained in the substrate material surface of handling;
3) with the base material of coating 100 ℃～300 ℃ following vacuum heat treatment 1～2 hour, remove the solvent in the coating paste, and make polysiloxane generation crosslinking reaction;
4) under protective atmosphere, the material after handling is carried out pyroprocessing, promptly between 400 ℃～1000 ℃ temperature, handled 1～5 hour, slowly cooling obtains the ceramic coating on the base material afterwards.Described protective atmosphere is meant air, nitrogen or rare gas element.
The used Polycarbosilane of the present invention be a kind of on main chain the polymkeric substance of Siliciumatom and the alternate Cheng Jian of carbon atom.Its structural unit is:
N is the polymerization degree in the formula, and the quantity of n can be calculated according to molecular weight.Because Si: C=1 among the PCS: 2, make and contain too much free C in the final ceramic product, influence the interface intensity and the insulating property of ceramic coating, can improve the final performance of ceramic coating by adding active filler and use reactive atmosphere.
Be the method that precursor prepares insulating heat conducting ceramic coating with the Polycarbosilane among the present invention, calculate by weight and carry out as follows:
1) in 100 parts of Polycarbosilanes, adds 10～30 parts of 10～30 parts of silicon carbide filler, norbide fillers, 0～20 part of the silica filler handled with silane coupling agent in advance, 0～10 part of titanium valve, 0～10 part in boron powder.Add 10～100 parts of aromatic solvent or ester solvents then, after the dispersed with stirring, use three-stage roll mill to grind, obtain the uniform slurry of packing material size between 0.01～10 micron;
2) base material is generally selected copper, aluminium, molybdenum-copper, aluminium/silicon carbide alloys, graphite etc. for use, adopts machinery or electrochemical method that substrate material surface is carried out pre-treatment, is cleaned, dry, smooth workpiece surface.With the mode of brushing or spray slurry is coated with then and is contained in the substrate material surface of handling;
3) with the base material of coating 100 ℃～300 ℃ following vacuum heat treatment 1～2 hour, remove the solvent in the coating paste, and make Polycarbosilane generation crosslinking reaction;
4) under certain atmosphere, the material after handling is carried out pyroprocessing, promptly between 400 ℃～1000 ℃ temperature, handled 1～5 hour, slowly cooling obtains the ceramic coating on the base material afterwards.Described certain atmosphere is meant air or the rare gas element of the oxygen that mixed.
Compare with existing ceramic coating, ceramic coating of the present invention has following advantage:
1. preparation technology is simple: the preparation of slurry only need disperse and grind two steps, is applied at substrate surface by the mode that sprays or brush, and is applicable to abnormity component.Curing pre-treatment and the Pintsch process reaction that heats up can be carried out in same equipment, is convenient to operation.
2. heat conductivility excellence: traditional ceramic coating technology mainly is in order to solve wear-resistant, high temperature resistant, the corrosion resistant application of metallic substance, insulativity and thermal conductivity not to be done requirement.The thermal conductivity of the ceramic coating that makes by the present invention far above be used for the metal matrix insulcrete the thermal conductivity of polymeric coating.
3. insulating property are good: the ceramic insulating layer voltage breakdown of 80 micron thickness can reach more than the 10KV (AC), and insulation resistance is greater than 1 * 10
10Ω.
4. You Yi thermal shock resistance: no matter the ceramic coating that the present invention forms is the environment that is directly entered 300 ℃ (electron device maximum operation (service) temperatures) by room temperature, or put into process furnace at ambient temperature and be warming up to 300 ℃, coating is all intact, and the cooling back does not have cracking or foaming phenomenon.
Description of drawings
Fig. 1 is a vacuum heat treatment phase temperature control curve synoptic diagram
Fig. 2 is a high-temperature heat treatment phase temperature control curve synoptic diagram
Embodiment
Embodiment one
Get the polysilazane 1Kg of molecular weight between 1000～5000, add aluminium nitride filler 200g, the tantalum nitride filler 50g, boron nitride filler 100g, silicon carbide filler 200g, the norbide filler 100g that handled with the methacrylic acid group propyl trimethoxy silicane, silica flour 5g, boron powder 5g, stir the back and add dimethylbenzene 60g, continue to stir until evenly.With three-roll grinder slurry is ground 3～5 times repeatedly then.The slurry that obtains is sprayed at the surface of the surface-treated thick copper sheet of 1mm with spray gun, under vacuum state in 100 ℃～300 ℃ thermal treatments after 2 hours, feed nitrogen atmosphere, beginning slowly heats up up to 900 ℃, and 900 ℃ of insulations 1 hour, slowly be cooled to room temperature subsequently, obtaining with copper is the ceramic coating of base material, and thickness is about 80～100 μ m.Through experiment test, voltage breakdown can reach 10KV (AC), and insulation resistance is greater than 1 * 10
10Ω, thermal conductivity is greater than 30W/m.K.
Embodiment two
Get the polysilazane 1Kg of molecular weight between 1000～5000, add aluminium nitride filler 300g, the tantalum nitride filler 50g, boron nitride filler 100g, silicon carbide filler 200g, the norbide filler 200g that handled with the methacrylic acid group propyl trimethoxy silicane, silica flour 8g, boron powder 8g, stir the back and add dimethylbenzene 80g, continue to stir until evenly.With three-roll grinder slurry is ground 3～5 times repeatedly then.The slurry that obtains is sprayed at the surface of the surface-treated thick copper sheet of 1mm with spray gun, under vacuum state in 100 ℃～300 ℃ thermal treatments after 2 hours, feed ammonia atmosphere, beginning slowly heats up up to 900 ℃, and 900 ℃ of insulations 1 hour, slowly be cooled to room temperature subsequently, obtaining with copper is the ceramic coating of base material, and thickness is about 80～100 μ m.Through experiment test, voltage breakdown can reach 10KV (AC), and insulation resistance is greater than 1 * 10
10Ω, thermal conductivity is greater than 40W/m.K.
Embodiment three
Get the polysilazane 1Kg of molecular weight between 1000～5000, add aluminium nitride filler 200g, the tantalum nitride filler 50g, boron nitride filler 100g, silicon carbide filler 200g, the norbide filler 200g that handled with the methacrylic acid group propyl trimethoxy silicane, silica flour 8g, boron powder 8g, stir the back and add dimethylbenzene 80g, continue to stir until evenly.With three-roll grinder slurry is ground 3～5 times repeatedly then.The slurry that obtains is sprayed at the surface of the surface-treated thick aluminium flake of 1mm with spray gun, under vacuum state in 100 ℃～300 ℃ thermal treatments after 2 hours, feed ammonia atmosphere, beginning slowly heats up up to 500 ℃, and 500 ℃ of insulations 2 hours, slowly be cooled to room temperature subsequently, obtaining with aluminium is the ceramic coating of base material, and thickness is about 80～100 μ m.Through experiment test, voltage breakdown can reach 10KV (AC), and insulation resistance is greater than 1 * 10
10Ω, thermal conductivity is greater than 30W/m.K.
Embodiment four
Get the polysiloxane 1Kg of molecular weight between 2000～10000, add alumina packing 100g, the silicon carbide filler 200g, norbide filler 200g, the silica filler 100g that handled with the methacrylic acid group propyl trimethoxy silicane, AL powder 8g, silica flour 5g, stir the back and add dimethylbenzene 100g, continue to stir until evenly.With three-roll grinder slurry is ground 3～5 times repeatedly then.The slurry that obtains is sprayed at the surface of the surface-treated thick aluminium flake of 1mm with spray gun, under vacuum state in 100 ℃～300 ℃ thermal treatments after 2 hours, feed nitrogen atmosphere, beginning slowly heats up up to 500 ℃, and 500 ℃ of insulations 2 hours, slowly be cooled to room temperature subsequently, obtaining with aluminium is the ceramic coating of base material, and thickness is about 80～100 μ m.Through experiment test, voltage breakdown can reach 10KV (AC), and insulation resistance is greater than 1 * 10
10Ω, thermal conductivity is greater than 20W/m.K.
Embodiment five
Get the polysiloxane 1Kg of molecular weight between 2000～10000, add alumina packing 50g, the silicon carbide filler 250g, norbide filler 250g, the silica filler 50g that handled with the methacrylic acid group propyl trimethoxy silicane, AL powder 5g, silica flour 5g, stir the back and add dimethylbenzene 100g, continue to stir until evenly.With three-roll grinder slurry is ground 3～5 times repeatedly then.The slurry that obtains is sprayed at the surface of the surface-treated thick aluminium flake of 1mm with spray gun, under vacuum state in 100 ℃～300 ℃ thermal treatments after 2 hours, feed nitrogen atmosphere, beginning slowly heats up up to 500 ℃, and 500 ℃ of insulations 2 hours, slowly be cooled to room temperature subsequently, obtaining with aluminium is the ceramic coating of base material, and thickness is about 80～100 μ m.Through experiment test, voltage breakdown can reach 10KV (AC), and insulation resistance is greater than 1 * 10
10Ω, thermal conductivity is greater than 20W/m.K.
Embodiment six
Get the polysiloxane 1Kg of molecular weight between 2000～10000, add alumina packing 50g, the silicon carbide filler 200g, norbide filler 200g, the silica filler 50g that handled with the methacrylic acid group propyl trimethoxy silicane, AL powder 5g, boron powder 5g, stir the back and add dimethylbenzene 100g, continue to stir until evenly.With three-roll grinder slurry is ground 3～5 times repeatedly then.The slurry that obtains is sprayed at the surface of surface-treated 4mm graphite flake with spray gun, under vacuum state in 100 ℃～300 ℃ thermal treatments after 2 hours, feed nitrogen atmosphere, beginning slowly heats up up to 800 ℃, and 800 ℃ of insulations 1 hour, slowly be cooled to room temperature subsequently, obtaining with aluminium is the ceramic coating of base material, and thickness is about 100～120 μ m.Through experiment test, voltage breakdown can reach 10KV (AC), and insulation resistance is greater than 1 * 10
10Ω, thermal conductivity is greater than 10W/m.K.
Embodiment seven
Get the Polycarbosilane 1Kg of molecular weight between 2000～8000, add the silicon carbide filler 100g, norbide filler 150g, the silica filler 100g that handled with the methacrylic acid group propyl trimethoxy silicane, titanium valve 10g, boron powder 10g, stir the back and add dimethylbenzene 100g, continue to stir until evenly.With three-roll grinder slurry is ground 3～5 times repeatedly then.The slurry that obtains is sprayed at the surface of the surface-treated thick aluminium of 1mm with spray gun, under vacuum state in 100 ℃～300 ℃ thermal treatments after 2 hours, feed nitrogen atmosphere, beginning slowly heats up up to 500 ℃, and 500 ℃ of insulations 2 hours, slowly be cooled to room temperature subsequently, obtaining with aluminium is the ceramic coating of base material, and thickness is about 80～100 μ m.Through experiment test, voltage breakdown can reach 10KV (AC), and insulation resistance is greater than 1 * 10
10Ω, thermal conductivity is greater than 20W/m.K.
Claims (10)
1. one kind is equipped with the method for insulating heat conducting ceramic coating by polymer precursor, it is characterized in that, calculates by weight and carries out as follows:
A) in 100 parts of polymeric preceramic bodies, 0～40 part of 0～50 part of nitride ceramics filler, the carbide ceramics filler that adding was handled with silane coupling agent, 0～30 part of oxide filler, and 0～10 part of active filler, the solvent that adds 10～100 parts simultaneously is to regulate viscosity.After the dispersed with stirring, use three-stage roll mill to grind, obtain the uniform slurry of packing material size between 0.01 μ m～10 μ m;
B) base material is generally selected copper, aluminium, molybdenum-copper, aluminium/silicon carbide alloys, graphite etc. for use, adopts machinery or electrochemical method that substrate material surface is carried out pre-treatment, is cleaned, dry, smooth workpiece surface.With the mode of brushing or spray slurry is coated with then and is contained in the substrate material surface of handling;
C) with the base material of coating 100 ℃～300 ℃ following vacuum heat treatment 1～2 hour, remove the solvent in the coating paste, and make polysilazane generation crosslinking reaction;
D) under protective atmosphere, the material after handling is carried out pyroprocessing, promptly between 400 ℃～1000 ℃ temperature, handled 1～5 hour, slowly reduce to room temperature afterwards, obtain the ceramic coating on the base material.
2. according to the preparation method of claim 1, it is characterized in that: described polymeric preceramic body is polysilazane, polysiloxane or Polycarbosilane, and its molecular weight is between 1000～10000.
3. according to the preparation method of claim 1, it is characterized in that: described silane coupling agent is aminosilane, styryl amido functional group silane, epoxy radicals silicone hydride or vinyl silanes.
4. according to the preparation method of claim 1, it is characterized in that: described nitride ceramics filler is aluminium nitride, silicon nitride, tantalum nitride or boron nitride, and its granularity is between 0.1 μ m～10 μ m.
5. according to the preparation method of claim 1, it is characterized in that: described carbide ceramics filler is silicon carbide or norbide, and its granularity is between 0.1 μ m～10 μ m.
6. according to the preparation method of claim 1, it is characterized in that: described oxide filler is silicon-dioxide or aluminum oxide, and its granularity is between 1 μ m～10 μ m.
7. according to the preparation method of claim 1, it is characterized in that: described active filler is titanium, silicon, aluminium, boron, and its granularity is between 0.01 μ m～10 μ m.
8. according to the preparation method of claim 1, it is characterized in that: described solvent is aromatic hydrocarbon solvent or esters solvent.
9. according to the preparation method of claim 1, it is characterized in that: described employing machinery or electrochemical method carry out pre-treatment to substrate material surface, are meant that sandblast processing, surperficial anodic oxidation treatment and differential arc oxidation of surface handle.
10. according to the preparation method of claim 1, it is characterized in that: described protective atmosphere is nitrogen, ammonia, helium, argon gas, air, oxygen.
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