CN108191429A - A kind of preparation method of insulating radiation type nano ceramic material - Google Patents
A kind of preparation method of insulating radiation type nano ceramic material Download PDFInfo
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- CN108191429A CN108191429A CN201711280800.3A CN201711280800A CN108191429A CN 108191429 A CN108191429 A CN 108191429A CN 201711280800 A CN201711280800 A CN 201711280800A CN 108191429 A CN108191429 A CN 108191429A
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- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 230000005855 radiation Effects 0.000 title claims abstract description 15
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 88
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 59
- 239000000919 ceramic Substances 0.000 claims abstract description 30
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 30
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 30
- 239000002086 nanomaterial Substances 0.000 claims abstract description 30
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 30
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 30
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910001928 zirconium oxide Inorganic materials 0.000 claims abstract description 18
- -1 methylene acrylamide Chemical compound 0.000 claims abstract description 14
- 238000005245 sintering Methods 0.000 claims abstract description 10
- 239000002245 particle Substances 0.000 claims abstract description 9
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims abstract description 8
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims abstract description 7
- 229920000058 polyacrylate Polymers 0.000 claims abstract description 7
- 239000002114 nanocomposite Substances 0.000 claims abstract description 3
- 238000002156 mixing Methods 0.000 claims description 41
- 239000002002 slurry Substances 0.000 claims description 26
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 23
- 238000000498 ball milling Methods 0.000 claims description 19
- 239000000243 solution Substances 0.000 claims description 14
- 239000003795 chemical substances by application Substances 0.000 claims description 12
- 239000013110 organic ligand Substances 0.000 claims description 7
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 claims description 7
- 239000000843 powder Substances 0.000 claims description 7
- 235000012239 silicon dioxide Nutrition 0.000 claims description 7
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 125000002382 camphene group Chemical group 0.000 claims description 6
- 150000003926 acrylamides Chemical class 0.000 claims description 5
- 230000001105 regulatory effect Effects 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 4
- 150000003639 trimesic acids Chemical class 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- 239000013084 copper-based metal-organic framework Substances 0.000 claims description 3
- SXTLQDJHRPXDSB-UHFFFAOYSA-N copper;dinitrate;trihydrate Chemical compound O.O.O.[Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O SXTLQDJHRPXDSB-UHFFFAOYSA-N 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000001746 injection moulding Methods 0.000 claims description 3
- 239000006193 liquid solution Substances 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- 229910052727 yttrium Inorganic materials 0.000 claims description 3
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims description 3
- 239000000463 material Substances 0.000 abstract description 16
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 4
- 238000000280 densification Methods 0.000 abstract description 3
- 239000000203 mixture Substances 0.000 abstract description 3
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 abstract description 2
- 239000011800 void material Substances 0.000 abstract description 2
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 abstract 2
- 229910001870 ammonium persulfate Inorganic materials 0.000 abstract 1
- 230000000694 effects Effects 0.000 description 13
- 230000017525 heat dissipation Effects 0.000 description 13
- 235000019441 ethanol Nutrition 0.000 description 12
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 6
- 238000000227 grinding Methods 0.000 description 5
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 5
- 239000006249 magnetic particle Substances 0.000 description 5
- 229910000838 Al alloy Inorganic materials 0.000 description 4
- QMKYBPDZANOJGF-UHFFFAOYSA-N benzene-1,3,5-tricarboxylic acid Chemical compound OC(=O)C1=CC(C(O)=O)=CC(C(O)=O)=C1 QMKYBPDZANOJGF-UHFFFAOYSA-N 0.000 description 4
- 238000009413 insulation Methods 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- 239000004411 aluminium Substances 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 239000011810 insulating material Substances 0.000 description 3
- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 description 3
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- CRPUJAZIXJMDBK-UHFFFAOYSA-N camphene Chemical compound C1CC2C(=C)C(C)(C)C1C2 CRPUJAZIXJMDBK-UHFFFAOYSA-N 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- 241001465382 Physalis alkekengi Species 0.000 description 1
- PXRCIOIWVGAZEP-UHFFFAOYSA-N Primaeres Camphenhydrat Natural products C1CC2C(O)(C)C(C)(C)C1C2 PXRCIOIWVGAZEP-UHFFFAOYSA-N 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- XCPQUQHBVVXMRQ-UHFFFAOYSA-N alpha-Fenchene Natural products C1CC2C(=C)CC1C2(C)C XCPQUQHBVVXMRQ-UHFFFAOYSA-N 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229930006739 camphene Natural products 0.000 description 1
- ZYPYEBYNXWUCEA-UHFFFAOYSA-N camphenilone Natural products C1CC2C(=O)C(C)(C)C1C2 ZYPYEBYNXWUCEA-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 150000001860 citric acid derivatives Chemical class 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical class O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 description 1
- 239000007783 nanoporous material Substances 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- RUDFQVOCFDJEEF-UHFFFAOYSA-N oxygen(2-);yttrium(3+) Chemical class [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
- C04B35/481—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates containing silicon, e.g. zircon
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
- C04B2235/3225—Yttrium oxide or oxide-forming salts thereof
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- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3418—Silicon oxide, silicic acids or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
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- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
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Abstract
The invention discloses a kind of preparation method of insulating radiation type nano ceramic material, acrylamide, methylene acrylamide, ammonium polyacrylate, Cu BTC SiO2Nano material, zirconium oxide, silica, zirconium oxide, tetramethylammonium hydroxide, ammonium persulfate are primary raw material, due to Cu BTC SiO2Nano material grain size is small, accordingly, its large specific surface area can cause the sintering densification degree of material to improve so that the composition structure of material is more fine and close, and fill Zirconium powder void among particles, in sintering, it can equally so that material is fine and close, uniform, so as to improve the intensity of material, while the logical nano composite ceramic prepared of the present invention has excellent heat conductivity, also has good insulating properties.
Description
Technical field
The present invention relates to a kind of preparation methods of insulating radiation type nano ceramic material, belong to field of ceramic preparation.
Background technology
LED is referred to as forth generation light source, has many advantages, such as 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 centainly as radiator
Security risk.And ceramic heat emission material has that insulation, heat-resisting, coefficient of thermal expansion is low, the characteristics such as stable, makes the anti-height of radiator
It presses, is indeformable, not aoxidizing and there is similar coefficient of thermal expansion, but ceramic substrate thermal conductivity factor is low with chip, cannot meet big
The radiating requirements of power.
Invention content
The purpose of the present invention is to provide a kind of insulating radiation type nano ceramic materials and preparation method thereof, pass through this method
The material of preparation has excellent heat dissipation effect.
A kind of preparation method of insulating radiation type nano ceramic material, this method include the following steps：
2 parts of acrylamides, 5 parts of methylene acrylamides and 10 parts of ammonium polyacrylates are added water to mix, and regulated value is extremely by step 1
9, obtain pre-mixing liquor；
Step 2, again by 45 parts of Cu-BTC-SiO2Nano material, 100 parts of zirconium oxides and 3 parts of fluxing agent silica are added to ball
In grinding jar, pre-mixing liquor ball milling mixing is then added in 30 hours, obtain slurry；
Step 3 adds in 2 parts of tetramethylammonium hydroxide and 3 parts of ammonium persulfates into above-mentioned slurry, by pulp gel injection moulding,
Again with the heating rate of 3 DEG C/min from room temperature to 1450 DEG C, and heat preservation sintering 2 hours at 1450 DEG C；
Above-mentioned sintered product from normal temperature and pressure increasing temperature and pressure 4 hours to 1450 DEG C of pressure of temperature is 120MPa by step 4, and
1450 DEG C, hip treatment is carried out under conditions of 120MPa 4 hours, then decrease temperature and pressure 3 hours is normal to room temperature
Pressure obtains insulating radiation type ceramics.
The Cu-BTC-SiO2Preparation method of nano material is as follows：
Step 1 aoxidizes 10 parts of silicon dioxide powders, 0.3 part of Sodium Polyacrylate, 19.4 parts of camphenes, 2.9 parts of tert-butyl alcohols and 0.5 part
Yttrium mixing is put into flask, and the uniform stirring at 75 DEG C obtains slurry；
Step 2 pours into slurry in mold, is placed at -16 DEG C, obtains being shaped to columnar SiO 2-ceramic particle modeling
Base；
SiO 2-ceramic particle preform is first placed 12h by step 3 at -16 DEG C, is then put it into freeze drier
The dry 6h under the conditions of -60 DEG C, is finally heated up with the speed of 4 DEG C/min and carries out high temperature sintering, be warming up to 1000 DEG C, keep the temperature 3h,
Porous silica ceramic monolith is obtained after cooling；
Step 4,2 parts of trimesic acids are mixed with 25 parts of the ethanol solution that mass fraction is 95%, are stirred evenly, are obtained organic match
Liquid solution takes 5 parts of porous silica ceramic monoliths to be put into organic ligand solution obtained above, impregnates 12h, filters, will
Gained sample is put into the ethanol solution that 25 parts of mass fractions are 95% after filtering, is added in 4.8 parts of nitrate trihydrate copper, is stirred evenly,
It is reacted at 80 DEG C, filters, cleans, and the drying and processing at 100 DEG C, obtain porous silica ceramic load Cu-MOF, i.e.,
Nano material Cu-BTC-SiO2。
Advantageous effect：Insulating radiation type nano ceramic material prepared by the present invention, due to Cu-BTC-SiO2Nano material grain size
Small, accordingly, large specific surface area can cause the sintering densification degree of material to improve so that the composition structure of material is more
For densification, and Zirconium powder void among particles are filled, in sintering, can equally so that material is fine and close, uniformly, so as to carry
The intensity of high material；Using nano zircite and Cu-BTC-SiO2Nano-porous materials form heat dissipation particle, ensure it radially
With in axial direction all have high thermal conductivity and thermal diffusivity；In addition, by the slurry after pre-mixing liquor ball milling, effect packet could be formed with
It wraps up in so that insulating materials covers comprehensively, forms active surface covering and is invaded with space so that ceramics have the same of excellent heat conductivity
When, also have good insulating properties.
Specific embodiment
Embodiment 1
A kind of preparation method of insulating radiation type nano ceramic material, this method include the following steps：
2 parts of acrylamides, 5 parts of methylene acrylamides and 10 parts of ammonium polyacrylates are added water to mix, and regulated value is extremely by step 1
9, obtain pre-mixing liquor；
Step 2, again by 45 parts of Cu-BTC-SiO2Nano material, 100 parts of zirconium oxides and 3 parts of fluxing agent silica are added to ball
In grinding jar, pre-mixing liquor ball milling mixing is then added in 30 hours, obtain slurry；
Step 3 adds in 2 parts of tetramethylammonium hydroxide and 3 parts of ammonium persulfates into above-mentioned slurry, by pulp gel injection moulding,
Again with the heating rate of 3 DEG C/min from room temperature to 1450 DEG C, and heat preservation sintering 2 hours at 1450 DEG C；
Above-mentioned sintered product from normal temperature and pressure increasing temperature and pressure 4 hours to 1450 DEG C of pressure of temperature is 120MPa by step 4, and
1450 DEG C, hip treatment is carried out under conditions of 120MPa 4 hours, then decrease temperature and pressure 3 hours is normal to room temperature
Pressure obtains insulating radiation type ceramics.
The Cu-BTC-SiO2Preparation method of nano material is as follows：
Step 1 aoxidizes 10 parts of silicon dioxide powders, 0.3 part of Sodium Polyacrylate, 19.4 parts of camphenes, 2.9 parts of tert-butyl alcohols and 0.5 part
Yttrium mixing is put into flask, and the uniform stirring at 75 DEG C obtains slurry；
Step 2 pours into slurry in mold, is placed at -16 DEG C, obtains being shaped to columnar SiO 2-ceramic particle modeling
Base；
SiO 2-ceramic particle preform is first placed 12h by step 3 at -16 DEG C, is then put it into freeze drier
The dry 6h under the conditions of -60 DEG C, is finally heated up with the speed of 4 DEG C/min and carries out high temperature sintering, be warming up to 1000 DEG C, keep the temperature 3h,
Porous silica ceramic monolith is obtained after cooling；
Step 4,2 parts of trimesic acids are mixed with 25 parts of the ethanol solution that mass fraction is 95%, are stirred evenly, are obtained organic match
Liquid solution takes 5 parts of porous silica ceramic monoliths to be put into organic ligand solution obtained above, impregnates 12h, filters, will
Gained sample is put into the ethanol solution that 25 parts of mass fractions are 95% after filtering, is added in 4.8 parts of nitrate trihydrate copper, is stirred evenly,
It is reacted at 80 DEG C, filters, cleans, and the drying and processing at 100 DEG C, obtain porous silica ceramic load Cu-MOF, i.e.,
Nano material Cu-BTC-SiO2。
Embodiment 2
Step 2, again by 35 parts of Cu-BTC-SiO2Nano material, 100 parts of zirconium oxides and 3 parts of fluxing agent silica are added to ball
In grinding jar, pre-mixing liquor ball milling mixing is then added in 30 hours, obtain slurry；
Remaining is prepared and embodiment 1 is identical.
Embodiment 3
Step 2, again by 25 parts of Cu-BTC-SiO2Nano material, 100 parts of zirconium oxides and 3 parts of fluxing agent silica are added to ball
In grinding jar, pre-mixing liquor ball milling mixing is then added in 30 hours, obtain slurry；
Remaining is prepared and embodiment 1 is identical.
Embodiment 4
Step 2, again by 15 parts of Cu-BTC-SiO2Nano material, 100 parts of zirconium oxides and 3 parts of fluxing agent silica are added to ball
In grinding jar, pre-mixing liquor ball milling mixing is then added in 30 hours, obtain slurry；
Remaining is prepared and embodiment 1 is identical.
Embodiment 5
Step 2, again by 5 parts of Cu-BTC-SiO2Nano material, 100 parts of zirconium oxides and 3 parts of fluxing agent silica are added to ball milling
In tank, pre-mixing liquor ball milling mixing is then added in 30 hours, obtain slurry；
Remaining is prepared and embodiment 1 is identical.
Embodiment 6
Step 2, again by 45 parts of Cu-BTC-SiO2Nano material, 80 parts of zirconium oxides and 3 parts of fluxing agent silica are added to ball milling
In tank, pre-mixing liquor ball milling mixing is then added in 30 hours, obtain slurry；
Remaining is prepared and embodiment 1 is identical.
Embodiment 7
Step 2, again by 45 parts of Cu-BTC-SiO2Nano material, 60 parts of zirconium oxides and 3 parts of fluxing agent silica are added to ball milling
In tank, pre-mixing liquor ball milling mixing is then added in 30 hours, obtain slurry；
Remaining is prepared and embodiment 1 is identical.
Embodiment 8
Step 2, again by 45 parts of Cu-BTC-SiO2Nano material, 40 parts of zirconium oxides and 3 parts of fluxing agent silica are added to ball milling
In tank, pre-mixing liquor ball milling mixing is then added in 30 hours, obtain slurry；
Remaining is prepared and embodiment 1 is identical.
Embodiment 9
Step 2, again by 45 parts of Cu-BTC-SiO2Nano material, 20 parts of Fe3O4Magnetic particle, 100 parts of zirconium oxides and 3 parts of fluxing agents
Silica is added in ball grinder, then adds in pre-mixing liquor ball milling mixing 30 hours, obtains slurry；
Remaining is prepared and embodiment 1 is identical.
The Fe3O4Magnetic particle preparation method is as follows：
2.6g Iron(III) chloride hexahydrates, 7.6g acetate and 0.8g citrates are dissolved in 70ml ethylene glycol, at 160 DEG C
Mechanical agitation 1h is subsequently placed in the stainless steel autoclave containing polytetrafluoroethyllining lining, reaction kettle is positioned over
16h in 200 DEG C of baking oven takes out, is water-cooled to room temperature；Product is isolated, and washed with absolute ethyl alcohol and deionization with magnet
Unreacted raw material is washed away, finally obtains Fe3O4Magnetic particle.
Embodiment 10
Step 2, again by 45 parts of Cu-BTC-SiO2Nano material, 10 parts of zirconium oxides and 3 parts of fluxing agent silica are added to ball milling
In tank, pre-mixing liquor ball milling mixing is then added in 30 hours, obtain slurry；
Remaining is prepared and embodiment 1 is identical.
Reference examples 1
It is with 1 difference of embodiment：In step 1 prepared by nano ceramic material, by 2 parts of acrylamides, 15 parts of methylene third
Acrylamide and 1 part of ammonium polyacrylate add water to mix, and regulated value obtains pre-mixing liquor, remaining step and 1 complete phase of embodiment to 9
Together.
Reference examples 2
It is with 1 difference of embodiment：In step 1 prepared by nano ceramic material, by 20 parts of acrylamides, 1 part of methylene third
Acrylamide and 1 part of ammonium polyacrylate add water to mix, and regulated value obtains pre-mixing liquor, remaining step and 1 complete phase of embodiment to 9
Together.
Reference examples 3
It is with 1 difference of embodiment：In step 2 prepared by nano ceramic material, zirconium oxide is not added, remaining step and reality
It is identical to apply example 1.
Reference examples 4
It is with 1 difference of embodiment：In step 2 prepared by nano ceramic material, replace zirconium oxide with 100 parts of titanium oxide,
Remaining step is identical with embodiment 1.
Reference examples 5
It is with 1 difference of embodiment：Cu-BTC-SiO2In step 1 prepared by nano material, by 5 parts of silicon dioxide powders, 0.1
Part Sodium Polyacrylate, 10.4 parts of camphenes, 2.9 parts of tert-butyl alcohols and 0.5 part of yttrium oxide mixing are put into flask, are uniformly stirred at 75 DEG C
It mixes, obtains slurry, remaining step is identical with embodiment 1.
Reference examples 6
It is with 1 difference of embodiment：Cu-BTC-SiO2In step 1 prepared by nano material, by 15 parts of silicon dioxide powders, 10
Part Sodium Polyacrylate, 1.4 parts of camphenes, 9 parts of tert-butyl alcohols and 5 parts of yttrium oxides mixing are put into flask, and the uniform stirring at 75 DEG C obtains
To slurry, remaining step is identical with embodiment 1.
Reference examples 7
It is with 1 difference of embodiment：Cu-BTC-SiO2In step 1 prepared by nano material, by 12 parts of silicon dioxide powders, 21
Part Sodium Polyacrylate, 0.4 part of camphene, 2.9 parts of tert-butyl alcohols and 0.5 part of yttrium oxide mixing are put into flask, are uniformly stirred at 75 DEG C
It mixes, obtains slurry, remaining step is identical with embodiment 1.
Reference examples 8
It is with 1 difference of embodiment：：Cu-BTC-SiO2Nano material prepare step 1 in, by 35 parts of silicon dioxide powders,
0.1 part of Sodium Polyacrylate, 2.4 parts of camphenes, 9.7 parts of tert-butyl alcohols and 0.1 part of yttrium oxide mixing are put into flask, at 75 DEG C uniformly
Stirring, obtains slurry, remaining step is identical with embodiment 1.
Reference examples 9
It is with 1 difference of embodiment：Cu-BTC-SiO2In step 4 prepared by nano material, 20 parts of trimesic acids and quality
25 parts of mixing of ethanol solution that score is 95%, stir evenly, obtain organic ligand solution, remaining step and 1 complete phase of embodiment
Together.
Reference examples 10
It is with 1 difference of embodiment：Cu-BTC-SiO2In step 4 prepared by nano material, 0.1 part of trimesic acid and matter
25 parts of mixing of ethanol solution that score is 95% are measured, stirs evenly, obtains organic ligand solution, remaining step is complete with embodiment 1
It is identical.
It chooses the insulated type ceramic heat emission material being prepared and carries out performance detection respectively, resistivity uses GB/T10064-2006
《Measure the test method of solid insulating material insulation resistance》；GB/T5598-2015 thermal conductivity factors（Thermal conductivity）Assay method；
Test result
The experimental results showed that insulating radiation type nano ceramic material prepared by the present invention has good heat dissipation effect, material is in state
Under family's standard test condition, mechanical strength is certain, and thermal conductivity is higher, illustrates that heat dissipation effect is better, conversely, effect is poorer；Implement
Example 2 arrives embodiment 10, and volume resistivity reaches insulating materials standard, and thermal conductivity more than 150W/ (mk), changes ceramics respectively
The proportioning of each raw material composition, has different degrees of influence, in Cu- to the heat dissipation performance of material in radiation nano composite material
BTC-SiO2Nano material, zirconium oxide quality proportioning are 9：20, when other dispensing dosages are fixed, heat dissipation effect is best；It is worth note
Meaning is that embodiment 9 adds in Fe3O4Magnetic particle, insulation and heat dissipation effect significantly improve, and illustrate Fe3O4Magnetic particle is to ceramics
The heat dissipation performance of filling-material structure has better optimization function；Reference examples 1 to reference examples 2 change pre-mixing liquor acrylamide, methylene
The proportioning of acrylamide and ammonium polyacrylate, heat dissipation effect are decreased obviously, and illustrate that pre-mixing liquor generates weight to the modified of composite material
It influences；Reference examples 3 do not add zirconium oxide to reference examples 4 and are replaced with titanium oxide, and insulating properties and thermal diffusivity are substantially reduced；It is right
5 change Cu-BTC-SiO to reference examples 8 as usual2The dosage and proportioning of nano material primary raw material, effect is also bad, illustrates to form
Ingredient is to Cu-BTC-SiO2Nano material synthesis plays an important role；Reference examples 9 change the dosage of trimesic acid to example 10,
The SOLUTION PROPERTIES of organic ligand changes, and heat dissipation effect is substantially reduced, and illustrates how many pairs of ceramic packing structures of organic ligand
Composite modified influence it is very big；Therefore using the insulating radiation type nano ceramic material for preparing of the present invention have excellent insulation and
Heat dissipation effect.
Claims (2)
1. a kind of preparation method of insulating radiation type nano ceramic material, it is characterised in that this method includes the following steps：
2 parts of acrylamides, 5 parts of methylene acrylamides and 10 parts of ammonium polyacrylates are added water to mix, and regulated value is extremely by step 1
9, obtain pre-mixing liquor；
Step 2, again by 45 parts of Cu-BTC-SiO2Nano material, 100 parts of zirconium oxides and 3 parts of fluxing agent silica are added to ball milling
In tank, pre-mixing liquor ball milling mixing is then added in about 30 hours, obtain slurry；
Step 3 adds in 2 parts of tetramethylammonium hydroxide and 3 parts of ammonium persulfates into above-mentioned slurry, by pulp gel injection moulding,
Again with the heating rate of 3 DEG C/min from room temperature to 1450 DEG C, and heat preservation sintering 2 hours at 1450 DEG C；
Above-mentioned sintered product from normal temperature and pressure increasing temperature and pressure 4 hours to 1450 DEG C of pressure of temperature is 120MPa by step 4, and
1450 DEG C, hip treatment is carried out under conditions of 120MPa 4 hours, then decrease temperature and pressure 3 hours is normal to room temperature
Pressure obtains insulating radiation type ceramics.
A kind of 2. preparation method of insulated type ceramic heat-dissipating nanocomposite according to claim 1, it is characterised in that institute
It states,
The Cu-BTC-SiO2Preparation method of nano material is as follows：
Step 1 aoxidizes 10 parts of silicon dioxide powders, 0.3 part of Sodium Polyacrylate, 19.4 parts of camphenes, 2.9 parts of tert-butyl alcohols and 0.5 part
Yttrium mixing is put into flask, and the uniform stirring at 75 DEG C obtains slurry；
Step 2 pours into slurry in mold, is placed at -16 DEG C, obtains being shaped to columnar SiO 2-ceramic particle modeling
Base；
SiO 2-ceramic particle preform is first placed 12h by step 3 at -16 DEG C, is then put it into freeze drier
The dry 6h under the conditions of -60 DEG C, is finally heated up with the speed of 4 DEG C/min and carries out high temperature sintering, be warming up to 1000 DEG C, keep the temperature 3h,
Porous silica ceramic monolith is obtained after cooling；
Step 4,2 parts of trimesic acids are mixed with 25 parts of the ethanol solution that mass fraction is 95%, are stirred evenly, are obtained organic match
Liquid solution takes 5 parts of porous silica ceramic monoliths to be put into organic ligand solution obtained above, impregnates 12h, filters, will
Gained sample is put into the ethanol solution that 25 parts of mass fractions are 95% after filtering, is added in 4.8 parts of nitrate trihydrate copper, is stirred evenly,
It is reacted at 80 DEG C, filters, cleans, and the drying and processing at 100 DEG C, obtain porous silica ceramic load Cu-MOF, i.e.,
Nano material Cu-BTC-SiO2。
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| CN110698187A (en) * | 2019-11-26 | 2020-01-17 | 衡阳阳光陶瓷有限公司 | Ceramic processing technology for avoiding high-temperature adhesion of powder |
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