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CN108002827A - A kind of preparation method of insulated type ceramic heat-dissipating nanocomposite - Google Patents

A kind of preparation method of insulated type ceramic heat-dissipating nanocomposite Download PDF

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CN108002827A
CN108002827A CN201711098908.0A CN201711098908A CN108002827A CN 108002827 A CN108002827 A CN 108002827A CN 201711098908 A CN201711098908 A CN 201711098908A CN 108002827 A CN108002827 A CN 108002827A
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sapo
kaolin
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nano
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阚森
刘镇
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Xuzhou Sai'ou Electronic Technology Co Ltd
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Xuzhou Sai'ou Electronic Technology Co Ltd
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Abstract

The invention discloses a kind of preparation method of insulated type ceramic heat-dissipating nanocomposite, using 34 nano materials of kaolin/SAPO, montmorillonite, nano-calcium carbonate, modified urea-formaldehyde resin, polymeric modification phenolic resin, polysiloxanes, zirconium oxide, zinc dihydrogen phosphate, isopropyl acrylate as primary raw material, by the way that 34 nano material silanization treatments of kaolin/SAPO are modified the compound insulated type ceramic heat emission material for preparing excellent performance of Lauxite again;The present invention has excellent insulating properties and heat dissipation performance by the way that 34 nano material silanization treatments of kaolin/SAPO are modified the compound insulated type ceramic heat emission material prepared of Lauxite again.

Description

A kind of preparation method of insulated type ceramic heat-dissipating nanocomposite
Technical field
Invention is related to a kind of preparation method of insulated type ceramic nanocomposites, belongs to the standby neck of ceramic system Domain.
Background technology
LED is referred to as forth generation light source, has the advantages that energy-saving and environmental protection, safety, low energy consumption, high brightness, in daily life In be widely used, the heat dissipation performance of lamp body in itself is most important, directly influences the service life and illuminating effect of lamps and lanterns.It is existing Some heat sink materials mainly have metallic aluminium and aluminium alloy, aluminium oxide ceramics, heat-conducting plastic etc..Aluminium and aluminium alloy thermal conductivity are high, but Heat dissipation performance is not so good as aluminium oxide ceramics and heat-conducting plastic, and aluminium and aluminium alloy are the good conductors of electricity, are had necessarily as radiator Security risk.And ceramic heat emission material has insulation, heat-resisting, thermal coefficient of expansion is low, the characteristic such as stable, make the anti-height of radiator Press, is indeformable, not aoxidizing and there is similar thermal coefficient of expansion with chip, but ceramic substrate thermal conductivity factor is low, cannot meet big The radiating requirements of power.
The content of the invention
It is an object of the invention to provide a kind of insulated type ceramic heat-dissipating nanocomposite and preparation method thereof, by this Material prepared by method has excellent heat dissipation effect.
A kind of preparation method of insulated type ceramic heat-dissipating nanocomposite, this method comprise the following steps:
Step 1, by 30 parts of modified kaolins/SAPO-34 nano materials, 10 parts of montmorillonites, 20 parts of nano-calcium carbonates be scattered in 200 Mixed slurry is formed in part absolute ethyl alcohol, dry obtained complex sintering aids are spare;
Step 2, toward sequentially adding 25 parts of modified urea-formaldehyde resin, 10 parts of polysiloxanes, 12 parts of zirconium oxide, biphosphate in ball mill 15 parts of 6 parts of zinc, 10 parts of isopropyl acrylate and complex sintering aids made from step 1 progress wet ball grindings, when ball milling 2 is small, into Row is stirred under vacuum de-bubble, and ceramic slurry is made, spare;
Step 3, by ceramic slurry made from above-mentioned steps by mold bottom press-in die, place naturally and complete gel process, Ceramic green sheet is taken out when drying 2 is small under the conditions of temperature 60 C, ceramic body monolithic spreading alumina powder is then folded into 2 layers of placement On load bearing board, be put into hot pressing die be placed in hot pressing furnace at 1500 DEG C sintering 0.5 it is small when, continue to improve temperature to 1750 DEG C It is lower insulation 0.5 it is small when, cooling down obtains ceramic heat-dissipating nanocomposite.
The modified kaolin/SAPO-34 preparation method of nano material is as follows:
Step 1, the kaolin and 0.1kg SAPO-34 zeolite powders for drying 0.3kg, activate at 500 DEG C, are distributed to In 10L ethanol, the mixture of compound kaolin and ethanol is transferred in the three-necked flask equipped with 2L ammonium hydroxide after ball milling, will Temperature is increased to 60 DEG C, heats 1h, the TEOS of the 1L then added, continues stirring 6, the slurry mistake that will be obtained
Filter, is washed 3 times with ethanol, finally obtains kaolin/SAPO-34 filter cakes of short chain modifier modification;
Step 2, by 2mL gamma-aminopropyl-triethoxy-silanes be added to aquation 1h in the mixture of 0.5mL water and 10mL ethanol, PH is adjusted to 4 with acetic anhydride, 1h is stirred, obtains the hydrolyzate of gamma-aminopropyl-triethoxy-silane;
Step 3, by the kaolin/SAPO-34 filter cakes 0.2Kg for the short chain modifier modification that step 1 obtains be re-dispersed into ethanol In, the hydrolyzate for the 20ml gamma-aminopropyl-triethoxy-silanes that step 2 obtains is added, stirring reaction 1h, is filtered, ethanol
Three times, 110 DEG C of dry 12h, obtain the modified kaolin/SAPO-34 nanometers of material that surface carries amido functional group for washing Material.
The modified urea-formaldehyde resin preparation method is as follows:
20g urea, 30mL formaldehyde and 250mL ionized waters, be added in three-necked flask by step 1, with sodium carbonate by the PH of solution Value brings up to 8, and temperature is increased to 75 DEG C, continuously stirs 1h, obtains the prepolymer of Lauxite;
Step 2, take the polystyrene PS that 30g molecular weight is 190,000, molten after being mixed with 10g Chloromethyl polystyrenes CMPS
Solution adds the nano oxidized iron particle that 6g average diameters are 5nm, stirring in 200mL, N, N dimethyl formamides DMF It is set fully to dissolve obtained mixed solution;
Step 3, by the above-mentioned mixed liquors of 200mL, 100mL deionized waters and 8g neopelexes SDBS be added to three mouthfuls of burnings In bottle, 2h is stirred at room temperature;Then the Lauxite prepolymer that step 1 obtains is added in flask, 90 DEG C of stirring 3h, it After filter, wash, 120 DEG C of dry 12h, acquisition modified urea-formaldehyde resin.
Beneficial effect:Insulated type ceramic heat-dissipating nanocomposite prepared by the present invention, by kaolin/SAPO-34 nano materials It is compound that silanization treatment is modified Lauxite again, is formed and dissipated using nano-calcium carbonate and SAPO-34 nano molecular sieves material Hot particle, ensures that it all has high thermal conductivity and thermal diffusivity on radial and axial, and " bone is played in modified urea-formaldehyde resin Frame " acts on, and to form three-dimensional netted radiator structure, using the suction-operated of SAPO-34 zeolite nano materials, can overlap and change Property Lauxite can make it that the nano materials such as molecular sieve and calcium carbonate are attached on kaolin internal flaw and surface upper, So that composite material all has high thermal conductivity and thermal diffusivity on radial and axial;In addition, Lauxite and polyene are modified After material mixing, effect parcel could be formed with so that insulating materials covers comprehensively, forms active surface covering and is attacked with space, While so that ceramics have excellent heat conductivity, also possesses good insulating properties.
Embodiment
Embodiment 1
Comprise the following steps:
Step 1, by 30 parts of modified kaolins/SAPO-34 nano materials, 10 parts of montmorillonites, 20 parts of nano-calcium carbonates be scattered in 200 Mixed slurry is formed in part absolute ethyl alcohol, dry obtained complex sintering aids are spare;
Step 2, toward sequentially adding 25 parts of modified urea-formaldehyde resin, 10 parts of polysiloxanes, 12 parts of zirconium oxide, biphosphate in ball mill 15 parts of 6 parts of zinc, 10 parts of isopropyl acrylate and complex sintering aids made from step 1 progress wet ball grindings, when ball milling 2 is small, into Row is stirred under vacuum de-bubble, and ceramic slurry is made, spare;
Step 3, by ceramic slurry made from above-mentioned steps by mold bottom press-in die, place naturally and complete gel process, Ceramic green sheet is taken out when drying 2 is small under the conditions of temperature 60 C, ceramic body monolithic spreading alumina powder is then folded into 2 layers of placement On load bearing board, be put into hot pressing die be placed in hot pressing furnace at 1500 DEG C sintering 0.5 it is small when, continue to improve temperature to 1750 DEG C It is lower insulation 0.5 it is small when, cooling down obtains ceramic heat-dissipating nanocomposite.
The modified kaolin/SAPO-34 preparation method of nano material is as follows:
Step 1, the kaolin and 0.1kg SAPO-34 zeolite powders for drying 0.3kg, activate at 500 DEG C, are distributed to In 10L ethanol, the mixture of compound kaolin and ethanol is transferred in the three-necked flask equipped with 2L ammonium hydroxide after ball milling, will Temperature is increased to 60 DEG C, heats 1h, the TEOS of the 1L then added, continues stirring 6, the slurry mistake that will be obtained
Filter, is washed 3 times with ethanol, finally obtains kaolin/SAPO-34 filter cakes of short chain modifier modification;
Step 2, by 2mL gamma-aminopropyl-triethoxy-silanes be added to aquation 1h in the mixture of 0.5mL water and 10mL ethanol, PH is adjusted to 4 with acetic anhydride, 1h is stirred, obtains the hydrolyzate of gamma-aminopropyl-triethoxy-silane;
Step 3, by the kaolin/SAPO-34 filter cakes 0.2Kg for the short chain modifier modification that step 1 obtains be re-dispersed into ethanol In, the hydrolyzate for the 20ml gamma-aminopropyl-triethoxy-silanes that step 2 obtains is added, stirring reaction 1h, is filtered, ethanol
Three times, 110 DEG C of dry 12h, obtain the modified kaolin/SAPO-34 nanometers of material that surface carries amido functional group for washing Material.
The modified urea-formaldehyde resin preparation method is as follows:
20g urea, 30mL formaldehyde and 250mL ionized waters, be added in three-necked flask by step 1, with sodium carbonate by the PH of solution Value brings up to 8, and temperature is increased to 75 DEG C, continuously stirs 1h, obtains the prepolymer of Lauxite;
Step 2, take the polystyrene PS that 30g molecular weight is 190,000, molten after being mixed with 10g Chloromethyl polystyrenes CMPS
Solution adds the nano oxidized iron particle that 6g average diameters are 5nm, stirring in 200mL, N, N dimethyl formamides DMF It is set fully to dissolve obtained mixed solution;
Step 3, by the above-mentioned mixed liquors of 200mL, 100mL deionized waters and 8g neopelexes SDBS be added to three mouthfuls of burnings In bottle, 2h is stirred at room temperature;Then the Lauxite prepolymer that step 1 obtains is added in flask, 90 DEG C of stirring 3h, it After filter, wash, 120 DEG C of dry 12h, acquisition modified urea-formaldehyde resin.
Embodiment 2
Step 1, by 15 parts of modified kaolins/SAPO-34 nano materials, 18 parts of montmorillonites, 30 parts of nano-calcium carbonates be scattered in 200 Mixed slurry is formed in part absolute ethyl alcohol, dry obtained complex sintering aids are spare;
Step 2, toward sequentially adding 25 parts of modified urea-formaldehyde resin, 10 parts of polysiloxanes, 12 parts of zirconium oxide, biphosphate in ball mill 15 parts of 6 parts of zinc, 10 parts of isopropyl acrylate and complex sintering aids made from step 1 progress wet ball grindings, when ball milling 2 is small, into Row is stirred under vacuum de-bubble, and ceramic slurry is made, spare;
Step 3, by ceramic slurry made from above-mentioned steps by mold bottom press-in die, place naturally and complete gel process, Ceramic green sheet is taken out when drying 2 is small under the conditions of temperature 60 C, ceramic body monolithic spreading alumina powder is then folded into 2 layers of placement On load bearing board, be put into hot pressing die be placed in hot pressing furnace at 1500 DEG C sintering 0.5 it is small when, continue to improve temperature to 1750 DEG C It is lower insulation 0.5 it is small when, cooling down obtains ceramic heat-dissipating nanocomposite.
Remaining is prepared and embodiment 1 is identical.
Embodiment 3
Step 1, by 20 parts of modified kaolins/SAPO-34 nano materials, 20 parts of montmorillonites, 10 parts of nano-calcium carbonates be scattered in 200 Mixed slurry is formed in part absolute ethyl alcohol, dry obtained complex sintering aids are spare;
Step 2, toward sequentially adding 25 parts of modified urea-formaldehyde resin, 10 parts of polysiloxanes, 12 parts of zirconium oxide, biphosphate in ball mill 15 parts of 6 parts of zinc, 10 parts of isopropyl acrylate and complex sintering aids made from step 1 progress wet ball grindings, when ball milling 2 is small, into Row is stirred under vacuum de-bubble, and ceramic slurry is made, spare;
Step 3, by ceramic slurry made from above-mentioned steps by mold bottom press-in die, place naturally and complete gel process, Ceramic green sheet is taken out when drying 2 is small under the conditions of temperature 60 C, ceramic body monolithic spreading alumina powder is then folded into 2 layers of placement On load bearing board, be put into hot pressing die be placed in hot pressing furnace at 1500 DEG C sintering 0.5 it is small when, continue to improve temperature to 1750 DEG C It is lower insulation 0.5 it is small when, cooling down obtains ceramic heat-dissipating nanocomposite.
Remaining is prepared and embodiment 1 is identical.
Embodiment 4
Step 1, by 10 parts of modified kaolins/SAPO-34 nano materials, 10 parts of montmorillonites, 20 parts of nano-calcium carbonates be scattered in 200 Mixed slurry is formed in part absolute ethyl alcohol, dry obtained complex sintering aids are spare;
Step 2, toward sequentially adding 15 parts of modified urea-formaldehyde resin, 10 parts of polysiloxanes, 12 parts of zirconium oxide, biphosphate in ball mill 15 parts of 6 parts of zinc, 10 parts of isopropyl acrylate and complex sintering aids made from step 1 progress wet ball grindings, when ball milling 2 is small, into Row is stirred under vacuum de-bubble, and ceramic slurry is made, spare;
Step 3, by ceramic slurry made from above-mentioned steps by mold bottom press-in die, place naturally and complete gel process, Ceramic green sheet is taken out when drying 2 is small under the conditions of temperature 60 C, ceramic body monolithic spreading alumina powder is then folded into 2 layers of placement On load bearing board, be put into hot pressing die be placed in hot pressing furnace at 1500 DEG C sintering 0.5 it is small when, continue to improve temperature to 1750 DEG C It is lower insulation 0.5 it is small when, cooling down obtains ceramic heat-dissipating nanocomposite.
Remaining is prepared and embodiment 1 is identical.
Embodiment 5
Step 1, by 20 parts of modified kaolins/SAPO-34 nano materials, 10 parts of montmorillonites, 20 parts of nano-calcium carbonates be scattered in 200 Mixed slurry is formed in part absolute ethyl alcohol, dry obtained complex sintering aids are spare;
Step 2, toward sequentially adding 35 parts of modified urea-formaldehyde resin, 20 parts of polysiloxanes, 12 parts of zirconium oxide, biphosphate in ball mill 15 parts of 6 parts of zinc, 10 parts of isopropyl acrylate and complex sintering aids made from step 1 progress wet ball grindings, when ball milling 2 is small, into Row is stirred under vacuum de-bubble, and ceramic slurry is made, spare;
Step 3, by ceramic slurry made from above-mentioned steps by mold bottom press-in die, place naturally and complete gel process, Ceramic green sheet is taken out when drying 2 is small under the conditions of temperature 60 C, ceramic body monolithic spreading alumina powder is then folded into 2 layers of placement On load bearing board, be put into hot pressing die be placed in hot pressing furnace at 1500 DEG C sintering 0.5 it is small when, continue to improve temperature to 1750 DEG C It is lower insulation 0.5 it is small when, cooling down obtains ceramic heat-dissipating nanocomposite.
Remaining is prepared and embodiment 1 is identical.
Embodiment 6
Step 1, by 10 parts of modified kaolins/SAPO-34 nano materials, 20 parts of montmorillonites, 20 parts of nano-calcium carbonates be scattered in 200 Mixed slurry is formed in part absolute ethyl alcohol, dry obtained complex sintering aids are spare;
Step 2, toward sequentially adding 15 parts of modified urea-formaldehyde resin, 10 parts of polysiloxanes, 22 parts of zirconium oxide, biphosphate in ball mill 15 parts of 16 parts of zinc, 10 parts of isopropyl acrylate and complex sintering aids made from step 1 progress wet ball grindings, when ball milling 2 is small, into Row is stirred under vacuum de-bubble, and ceramic slurry is made, spare;
Step 3, by ceramic slurry made from above-mentioned steps by mold bottom press-in die, place naturally and complete gel process, Ceramic green sheet is taken out when drying 2 is small under the conditions of temperature 60 C, ceramic body monolithic spreading alumina powder is then folded into 2 layers of placement On load bearing board, be put into hot pressing die be placed in hot pressing furnace at 1500 DEG C sintering 0.5 it is small when, continue to improve temperature to 1750 DEG C It is lower insulation 0.5 it is small when, cooling down obtains ceramic heat-dissipating nanocomposite.
Remaining is prepared and embodiment 1 is identical.
Embodiment 7
Step 1, by 10 parts of modified kaolins/SAPO-34 nano materials, 30 parts of montmorillonites, 5 parts of nano-calcium carbonates be scattered in 200 Mixed slurry is formed in part absolute ethyl alcohol, dry obtained complex sintering aids are spare;
Step 2, toward sequentially adding 5 parts of modified urea-formaldehyde resin, 20 parts of polysiloxanes, 12 parts of zirconium oxide, biphosphate in ball mill 15 parts of 6 parts of zinc, 15 parts of isopropyl acrylate and complex sintering aids made from step 1 progress wet ball grindings, when ball milling 2 is small, into Row is stirred under vacuum de-bubble, and ceramic slurry is made, spare;
Step 3, by ceramic slurry made from above-mentioned steps by mold bottom press-in die, place naturally and complete gel process, Ceramic green sheet is taken out when drying 2 is small under the conditions of temperature 60 C, ceramic body monolithic spreading alumina powder is then folded into 2 layers of placement On load bearing board, be put into hot pressing die be placed in hot pressing furnace at 1500 DEG C sintering 0.5 it is small when, continue to improve temperature to 1750 DEG C It is lower insulation 0.5 it is small when, cooling down obtains ceramic heat-dissipating nanocomposite.
Remaining is prepared and embodiment 1 is identical.
Embodiment 8
Step 1, by 30 parts of modified kaolins/SAPO-34 nano materials, 10 parts of montmorillonites, 20 parts of nano-calcium carbonates be scattered in 200 Mixed slurry is formed in part absolute ethyl alcohol, dry obtained complex sintering aids are spare;
Step 2, toward sequentially adding 35 parts of modified urea-formaldehyde resin, 20 parts of polysiloxanes, 12 parts of zirconium oxide, biphosphate in ball mill 25 parts of 6 parts of zinc, 10 parts of isopropyl acrylate and complex sintering aids made from step 1 progress wet ball grindings, when ball milling 2 is small, into Row is stirred under vacuum de-bubble, and ceramic slurry is made, spare;
Step 3, by ceramic slurry made from above-mentioned steps by mold bottom press-in die, place naturally and complete gel process, Ceramic green sheet is taken out when drying 2 is small under the conditions of temperature 60 C, ceramic body monolithic spreading alumina powder is then folded into 2 layers of placement On load bearing board, be put into hot pressing die be placed in hot pressing furnace at 1500 DEG C sintering 0.5 it is small when, continue to improve temperature to 1750 DEG C It is lower insulation 0.5 it is small when, cooling down obtains ceramic heat-dissipating nanocomposite.
Remaining is prepared and embodiment 1 is identical.
Embodiment 9
Step 1, by 10 parts of modified kaolins/SAPO-34 nano materials, 30 parts of montmorillonites, 20 parts of nano-calcium carbonates be scattered in 200 Mixed slurry is formed in part absolute ethyl alcohol, dry obtained complex sintering aids are spare;
Step 2, toward sequentially adding 15 parts of modified urea-formaldehyde resin, 20 parts of polysiloxanes, 10 parts of zirconium oxide, biphosphate in ball mill 15 parts of 6 parts of zinc, 5 parts of isopropyl acrylate and complex sintering aids made from step 1 progress wet ball grindings, when ball milling 2 is small, carry out De-bubble is stirred under vacuum, ceramic slurry is made, it is spare;
Step 3, by ceramic slurry made from above-mentioned steps by mold bottom press-in die, place naturally and complete gel process, Ceramic green sheet is taken out when drying 2 is small under the conditions of temperature 60 C, ceramic body monolithic spreading alumina powder is then folded into 2 layers of placement On load bearing board, be put into hot pressing die be placed in hot pressing furnace at 1500 DEG C sintering 0.5 it is small when, continue to improve temperature to 1750 DEG C It is lower insulation 0.5 it is small when, cooling down obtains ceramic heat-dissipating nanocomposite.
Remaining is prepared and embodiment 1 is identical.
Embodiment 10
Step 1, by 15 parts of modified kaolins/SAPO-34 nano materials, 15 parts of montmorillonites, 10 parts of nano-calcium carbonates be scattered in 200 Mixed slurry is formed in part absolute ethyl alcohol, dry obtained complex sintering aids are spare;
Step 2, toward sequentially adding 25 parts of modified urea-formaldehyde resin, 10 parts of polysiloxanes, 12 parts of zirconium oxide, biphosphate in ball mill 35 parts of 6 parts of zinc, 20 parts of isopropyl acrylate and complex sintering aids made from step 1 progress wet ball grindings, when ball milling 2 is small, into Row is stirred under vacuum de-bubble, and ceramic slurry is made, spare;
Step 3, by ceramic slurry made from above-mentioned steps by mold bottom press-in die, place naturally and complete gel process, Ceramic green sheet is taken out when drying 2 is small under the conditions of temperature 60 C, ceramic body monolithic spreading alumina powder is then folded into 2 layers of placement On load bearing board, be put into hot pressing die be placed in hot pressing furnace at 1500 DEG C sintering 0.5 it is small when, continue to improve temperature to 1750 DEG C It is lower insulation 0.5 it is small when, cooling down obtains ceramic heat-dissipating nanocomposite.
Remaining is prepared and embodiment 1 is identical.
Embodiment 11
Step 1, by 30 parts of modified kaolins/SAPO-34 nano materials, 10 parts of montmorillonites, 10 parts of modified magnesium carbonate, 20 parts of nanometers Calcium carbonate, which is scattered in 200 parts of absolute ethyl alcohols, forms mixed slurry, dry obtained complex sintering aids, spare;
Step 2, toward sequentially adding 25 parts of modified urea-formaldehyde resin, 10 parts of polysiloxanes, 12 parts of zirconium oxide, biphosphate in ball mill 15 parts of 6 parts of zinc, 10 parts of isopropyl acrylate and complex sintering aids made from step 1 progress wet ball grindings, when ball milling 2 is small, into Row is stirred under vacuum de-bubble, and ceramic slurry is made, spare;
Step 3, by ceramic slurry made from above-mentioned steps by mold bottom press-in die, place naturally and complete gel process, Ceramic green sheet is taken out when drying 2 is small under the conditions of temperature 60 C, ceramic body monolithic spreading alumina powder is then folded into 2 layers of placement On load bearing board, be put into hot pressing die be placed in hot pressing furnace at 1500 DEG C sintering 0.5 it is small when, continue to improve temperature to 1750 DEG C It is lower insulation 0.5 it is small when, cooling down obtains ceramic heat-dissipating nanocomposite.
The modification magnesium carbonate preparation method is as follows:
The nano-calcium carbonate magnesium that 200g particle diameters are 30nm is put into aqueous solution, with the mixing speed machine of 3000rpm at 20 DEG C After tool stirring 15min, the aqueous dispersions of nano-calcium carbonate magnesium are obtained;15g is added into the aqueous dispersions of obtained nano-calcium carbonate magnesium Modifer L monothio salicylic acid, at a temperature of 80 DEG C, is stirred under the rotating speed of 3000rpm, obtains the suspension of modified nano-meter caco 3 magnesium Liquid;The suspension of gained is spray-dried, the rotating speed of spray drying is 16000rpm, and the temperature of spray drying is 100 DEG C, Obtain nano-calcium carbonate magnesium base composite material, average grain diameter 330nm.
Reference examples 1
It is with 1 difference of embodiment:In step 1 prepared by modified kaolin/SAPO-34 nano materials, the height of 0.1kg dryings Ridge soil and 0.3kg SAPO-34 zeolite powders, remaining step are identical with embodiment 1.
Reference examples 2
It is with 1 difference of embodiment:In step 1 prepared by modified kaolin/SAPO-34 nano materials, 0.3 dry kaolin It is identical with embodiment 1 with 0.3kg SAPO-34 zeolite powders, remaining step.
Reference examples 3
It is with 1 difference of embodiment:, will with acetic anhydride in step 2 prepared by modified kaolin/SAPO-34 nano materials PH is adjusted to 7, remaining step is identical with embodiment 1.
Reference examples 4
It is with 1 difference of embodiment:, will with acetic anhydride in step 2 prepared by modified kaolin/SAPO-34 nano materials PH is adjusted to 12, remaining step is identical with embodiment 1.
Reference examples 5
It is with 1 difference of embodiment:In step 3 prepared by modified kaolin/SAPO-34 nano materials, add step 2 and obtain 10ml gamma-aminopropyl-triethoxy-silanes hydrolyzate, remaining step is identical with embodiment 1.
Reference examples 6
It is with 1 difference of embodiment:In step 3 prepared by modified kaolin/SAPO-34 nano materials, add step 2 and obtain 's:The hydrolyzate of 40ml gamma-aminopropyl-triethoxy-silanes, remaining step are identical with embodiment 1.
Reference examples 7
It is with 1 difference of embodiment:Modified urea-formaldehyde resin prepare step 1 in, by 10g urea, 30mL formaldehyde and 250mL from Sub- water is added in three-necked flask, remaining step is identical with embodiment 1.
Reference examples 8
It is with 1 difference of embodiment::In step 1 prepared by modified urea-formaldehyde resin, by 30g urea, 10mL formaldehyde and 250mL Ionized water is added in three-necked flask, remaining step is identical with embodiment 1.
Reference examples 9
It is with 1 difference of embodiment:In step 2 prepared by modified urea-formaldehyde resin, the polystyrene that 10g molecular weight is 190,000 is taken PS, is dissolved in 200mL after being mixed with 20g Chloromethyl polystyrenes CMPS, in N, N dimethyl formamides DMF, remaining step with Embodiment 1 is identical.
Reference examples 10
It is with 1 difference of embodiment:In step 2 prepared by modified urea-formaldehyde resin, the polystyrene that 50g molecular weight is 190,000 is taken PS, is dissolved in 200mL after being mixed with 30g Chloromethyl polystyrenes CMPS, in N, N dimethyl formamides DMF, remaining step with Embodiment 1 is identical.
Choose the insulated type ceramic heat emission material being prepared and carry out performance detection respectively,
Test result
Test result indicates that insulation thermal Ceramics radiation nano composite material provided by the invention has good heat dissipation effect, material Under national standard test condition, mechanical strength is certain, and thermal conductivity is higher, illustrates that heat dissipation effect is better, conversely, effect is poorer; Embodiment 1 arrives embodiment 10, and volume resistivity reaches insulating materials standard, and thermal conductivity more than 150 W/ (mk), changes respectively Become the proportioning of each raw material composition in ceramic heat-dissipating nanocomposite, have different degrees of shadow to the heat dissipation performance of material Ring, be 5 in modified urea-formaldehyde resin, complex sintering aids quality proportioning:3, when other dispensing dosages are fixed, heat dissipation effect is best; It is worth noting that embodiment 11 adds modified Nano magnesia, heat dissipation effect significantly improves, and illustrates modified Nano magnesia pair The heat dissipation performance of ceramic packing structure has more preferable optimization function;Reference examples 1 to reference examples 4 change kaolin/SAPO-34 nanometers Kaolin and SAPO-34 dosages and mixed solution PH, heat dissipation effect prepared by material is decreased obviously, and illustrates kaolin and molecular sieve The modification of dosage and mixed liquor PH to composite material has an important influence on;Reference examples 5 change γ-aminopropyl three to reference examples 6 The dosage of Ethoxysilane, effect is also bad, illustrates that silane modifier dosage plays an important role composite modification;Reference examples 7 change the proportioning of Lauxite modified feedstock urea and formaldehyde to example 10, and heat dissipation effect substantially reduces, and illustrates urea and formaldehyde Composite modified influence of the dosage on ceramic packing structure is very big;Therefore the insulated type ceramic heat-dissipating nanometer prepared using the present invention is answered Condensation material has excellent heat dissipation effect.

Claims (3)

1. a kind of preparation method of insulated type ceramic heat-dissipating nanocomposite, it is characterised in that this method comprises the following steps:
Step 1, by 30 parts of modified kaolins/SAPO-34 nano materials, 10 parts of montmorillonites, 20 parts of nano-calcium carbonates be scattered in 200 Mixed slurry is formed in part absolute ethyl alcohol, dry obtained complex sintering aids are spare;
Step 2, toward sequentially adding 25 parts of modified urea-formaldehyde resin, 10 parts of polysiloxanes, 12 parts of zirconium oxide, biphosphate in ball mill 15 parts of 6 parts of zinc, 10 parts of isopropyl acrylate and complex sintering aids made from step 1 progress wet ball grindings, when ball milling 2 is small, into Row is stirred under vacuum de-bubble, and ceramic slurry is made, spare;
Step 3, by ceramic slurry made from above-mentioned steps by mold bottom press-in die, place naturally and complete gel process, Ceramic green sheet is taken out when drying 2 is small under the conditions of temperature 60 C, ceramic body monolithic spreading alumina powder is then folded into 2 layers of placement On load bearing board, be put into hot pressing die be placed in hot pressing furnace at 1500 DEG C sintering 0.5 it is small when, continue to improve temperature to 1750 DEG C It is lower insulation 0.5 it is small when, cooling down obtains ceramic heat-dissipating nanocomposite.
A kind of 2. preparation method of insulated type ceramic heat-dissipating nanocomposite according to claim 1, it is characterised in that
The modified kaolin/SAPO-34 preparation method of nano material is as follows:
Step 1, the kaolin and 0.1kg SAPO-34 zeolite powders for drying 0.3kg, activate at 500 DEG C, are distributed to In 10L ethanol, the mixture of compound kaolin and ethanol is transferred in the three-necked flask equipped with 2L ammonium hydroxide after ball milling, will Temperature is increased to 60 DEG C, heats 1h, the TEOS of the 1L then added, continues stirring 6, the slurry mistake that will be obtained
Filter, is washed 3 times with ethanol, finally obtains kaolin/SAPO-34 filter cakes of short chain modifier modification;
Step 2, by 2mL gamma-aminopropyl-triethoxy-silanes be added to aquation 1h in the mixture of 0.5mL water and 10mL ethanol, PH is adjusted to 4 with acetic anhydride, 1h is stirred, obtains the hydrolyzate of gamma-aminopropyl-triethoxy-silane;
Step 3, by the kaolin/SAPO-34 filter cakes 0.2Kg for the short chain modifier modification that step 1 obtains be re-dispersed into ethanol In, the hydrolyzate for the 20ml gamma-aminopropyl-triethoxy-silanes that step 2 obtains is added, stirring reaction 1h, is filtered, ethanol
Three times, 110 DEG C of dry 12h, obtain the modified kaolin/SAPO-34 nanometers of material that surface carries amido functional group for washing Material.
A kind of 3. preparation method of insulated type ceramic heat-dissipating nanocomposite according to claim 1, it is characterised in that institute The modified urea-formaldehyde resin preparation method stated is as follows:
20g urea, 30mL formaldehyde and 250mL ionized waters, be added in three-necked flask by step 1, with sodium carbonate by the PH of solution Value brings up to 8, and temperature is increased to 75 DEG C, continuously stirs 1h, obtains the prepolymer of Lauxite;
Step 2, take the polystyrene PS that 30g molecular weight is 190,000, molten after being mixed with 10g Chloromethyl polystyrenes CMPS
Solution adds the nano oxidized iron particle that 6g average diameters are 5nm, stirring in 200mL, N, N dimethyl formamides DMF It is set fully to dissolve obtained mixed solution;
Step 3, by the above-mentioned mixed liquors of 200mL, 100mL deionized waters and 8g neopelexes SDBS be added to three mouthfuls of burnings In bottle, 2h is stirred at room temperature;Then the Lauxite prepolymer that step 1 obtains is added in flask, 90 DEG C of stirring 3h, it After filter, wash, 120 DEG C of dry 12h, acquisition modified urea-formaldehyde resin.
CN201711098908.0A 2017-11-09 2017-11-09 A kind of preparation method of insulated type ceramic heat-dissipating nanocomposite Pending CN108002827A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109233033A (en) * 2018-07-26 2019-01-18 合肥峰腾节能科技有限公司 A kind of energy saving and environment friendly insulating materials and preparation method thereof
CN110028259A (en) * 2019-04-26 2019-07-19 湖南腾达岩土工程技术有限公司 A kind of steel slag neutral activated cementitious material and its preparation method and application
WO2020109759A1 (en) * 2018-11-29 2020-06-04 Johnson Matthey Public Limited Company Method to modify the surface of a molecular sieve with an aminosilane
CN113861694A (en) * 2021-10-26 2021-12-31 广东电网有限责任公司 High-voltage cable joint insulating silicone grease with high barrier property and preparation method thereof

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109233033A (en) * 2018-07-26 2019-01-18 合肥峰腾节能科技有限公司 A kind of energy saving and environment friendly insulating materials and preparation method thereof
WO2020109759A1 (en) * 2018-11-29 2020-06-04 Johnson Matthey Public Limited Company Method to modify the surface of a molecular sieve with an aminosilane
GB2580513A (en) * 2018-11-29 2020-07-22 Johnson Matthey Plc Method
US11192793B2 (en) 2018-11-29 2021-12-07 Johnson Matthey Public Limited Company Method
GB2580513B (en) * 2018-11-29 2022-01-12 Johnson Matthey Plc Method for preparing modified molecular sieve
GB2602722A (en) * 2018-11-29 2022-07-13 Johnson Matthey Plc Modified molecular sieve
CN110028259A (en) * 2019-04-26 2019-07-19 湖南腾达岩土工程技术有限公司 A kind of steel slag neutral activated cementitious material and its preparation method and application
CN110028259B (en) * 2019-04-26 2023-08-29 湖南腾达岩土工程技术有限公司 Neutral steel slag activated cementing material and preparation method and application thereof
CN113861694A (en) * 2021-10-26 2021-12-31 广东电网有限责任公司 High-voltage cable joint insulating silicone grease with high barrier property and preparation method thereof

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