CN115216277A - Heat conduction material and preparation method thereof - Google Patents
Heat conduction material and preparation method thereof Download PDFInfo
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- CN115216277A CN115216277A CN202210892765.5A CN202210892765A CN115216277A CN 115216277 A CN115216277 A CN 115216277A CN 202210892765 A CN202210892765 A CN 202210892765A CN 115216277 A CN115216277 A CN 115216277A
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- heat conduction
- conduction material
- aqueous solution
- aluminum hydroxide
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- 239000000463 material Substances 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title abstract description 15
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 28
- 239000011701 zinc Substances 0.000 claims abstract description 28
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000001354 calcination Methods 0.000 claims abstract description 14
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 8
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 8
- 239000002131 composite material Substances 0.000 claims abstract description 6
- 239000002243 precursor Substances 0.000 claims abstract description 4
- 239000007864 aqueous solution Substances 0.000 claims description 37
- 239000007787 solid Substances 0.000 claims description 36
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 28
- 238000003756 stirring Methods 0.000 claims description 21
- 239000011259 mixed solution Substances 0.000 claims description 20
- -1 zinc aluminate Chemical class 0.000 claims description 20
- 238000001035 drying Methods 0.000 claims description 18
- 239000000126 substance Substances 0.000 claims description 18
- 239000004020 conductor Substances 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 10
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 10
- 239000008213 purified water Substances 0.000 claims description 10
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- 239000012670 alkaline solution Substances 0.000 claims description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 2
- 239000000843 powder Substances 0.000 abstract description 5
- 239000002245 particle Substances 0.000 abstract description 3
- 230000002349 favourable effect Effects 0.000 abstract 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 16
- 229910021529 ammonia Inorganic materials 0.000 description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 239000003054 catalyst Substances 0.000 description 5
- 239000000741 silica gel Substances 0.000 description 5
- 229910002027 silica gel Inorganic materials 0.000 description 5
- 229920002545 silicone oil Polymers 0.000 description 5
- 239000003431 cross linking reagent Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 239000000945 filler Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 2
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical group CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 description 2
- 238000000748 compression moulding Methods 0.000 description 2
- 239000012975 dibutyltin dilaurate Substances 0.000 description 2
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 2
- HIHIPCDUFKZOSL-UHFFFAOYSA-N ethenyl(methyl)silicon Chemical compound C[Si]C=C HIHIPCDUFKZOSL-UHFFFAOYSA-N 0.000 description 2
- 229920000620 organic polymer Polymers 0.000 description 2
- 229910000077 silane Inorganic materials 0.000 description 2
- 229920002379 silicone rubber Polymers 0.000 description 2
- 239000004945 silicone rubber Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 2
- 229920002554 vinyl polymer Polymers 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000008119 colloidal silica Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000000499 gel Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/08—Materials not undergoing a change of physical state when used
- C09K5/14—Solid materials, e.g. powdery or granular
Abstract
The invention relates to a heat conduction material and a preparation method thereof, wherein the heat conduction material is an inorganic composite oxide formed by calcining and crushing a precursor containing a zinc source and an aluminum source. The heat conduction material is an inorganic composite oxide formed by calcining and crushing a precursor containing a zinc source and an aluminum source, and compared with spherical alumina, the heat conduction material has larger contact area and stronger heat conduction capability due to the non-spherical characteristic of powder particles, and is favorable for improving the heat conduction coefficient of the heat conduction material.
Description
Technical Field
The invention relates to the technical field of heat conduction materials, in particular to a heat conduction material and a preparation method thereof.
Background
Heat conducting materials such as heat conducting rubber are one of the hot points of research in the field of new materials in the last decade, and in order to meet the development requirements of high integration and lightness and thinness of electronic and electric products, manufacturers continuously push out products with better heat conducting performance so as to meet the heat dissipation requirements of electronic and electric products. The heat-conducting insulating material is prepared by filling inorganic heat-conducting powder filler in an organic polymer, and the heat-conducting property of the composite material is improved by dispersing the inorganic heat-conducting powder filler in the organic polymer and conducting the inorganic heat-conducting powder filler in a point contact manner.
For example, "a high thermal conductivity insulating and thermal conductivity silica gel gasket and a preparation method thereof" disclosed in chinese invention patent application with patent No. CN201310372003.3 (publication No. CN 103436019A), wherein the thermal conductivity silica gel gasket is prepared from the following raw materials in parts by weight: 600-1000 parts of spherical alumina, 5-15 parts of methyl vinyl silicone rubber, 30-70 parts of dimethyl silicone oil, 2-15 parts of hydrogen-containing silicone oil and 0.5-1.5 parts of catalyst, and the heat-conducting silica gel gasket is prepared by the steps of screening and sintering alumina particles, grinding the methyl vinyl silicone rubber and the dimethyl silicone oil, stirring, vacuumizing, vulcanizing and forming and the like.
Spherical alumina is largely used in heat conduction materials due to the advantages of price and heat conduction performance, but spherical alumina has limited contact area with other materials due to the spherical reason, so the heat conduction rate is limited, and in order to improve the heat conduction rate of the heat conduction materials, a large amount of spherical alumina is needed, so the cost is high.
Disclosure of Invention
The first technical problem to be solved by the present invention is to provide a thermal conductive material with high thermal conductivity in view of the current state of the prior art.
The second technical problem to be solved by the present invention is to provide a method for preparing the above thermal conductive material, aiming at the current situation of the prior art.
The technical scheme adopted by the invention for solving the first technical problem is as follows: a thermally conductive material, characterized by: the heat conduction material is an inorganic composite oxide formed by calcining and crushing a precursor containing a zinc source and an aluminum source.
Preferably, the heat conducting material is composed of aluminum oxide and zinc aluminate, wherein the mass percentage of the zinc aluminate is 19% -75%.
The technical scheme adopted by the invention for solving the second technical problem is as follows: a preparation method of a heat conduction material is characterized by comprising the following steps: the method comprises the following steps:
(1) Adding an aluminum source into purified water, and uniformly stirring to obtain an aluminum source water solution;
(2) Adding an alkaline solution and a zinc source aqueous solution into an aluminum source aqueous solution, and stirring for 100-150 min to prepare a mixed solution, wherein the pH value of the alkaline solution is 8.5-9;
(3) Centrifugally separating the mixed solution obtained in the step (2), and drying the separated solid substances;
(4) Calcining the solid matter dried in the step (3) at 1280-1320 ℃ for 6-10 h, and crushing to obtain the heat conduction material.
In the above scheme, preferably, the alkaline solution is ammonia water or sodium hydroxide or potassium hydroxide or sodium carbonate.
In the above scheme, preferably, the zinc source is ZnCl 2 。
In the above scheme, preferably, the aluminum source is aluminum hydroxide.
Compared with the prior art, the invention has the advantages that: compared with spherical alumina, the heat conduction material has the advantages that the non-spherical characteristic of powder particles enables the heat conduction material to have larger contact area and stronger heat conduction capability, and is beneficial to improving the heat conduction coefficient of the heat conduction material.
Detailed Description
The present invention will be described in further detail with reference to specific examples.
Example 1
The preparation method of the heat conduction material of the embodiment comprises the following steps:
(1) Adding 1 liter of purified water and 500 g of aluminum hydroxide into a 5 liter beaker, and stirring for 30 minutes to prepare an aluminum hydroxide aqueous solution;
(2) ZnCl was prepared in an amount of 0.5 kg and a concentration of 100 g/l 2 Aqueous solution and ammonia with concentration of 10% and pH value of 9, then ZnCl is added 2 Adding the aqueous solution and ammonia water into the aqueous solution of aluminum hydroxide at the same time, and stirring for 100min to obtain a mixed solution;
(3) Centrifuging the mixed solution obtained in the step (2) by a roller centrifuge, and drying the separated solid substance in a drying oven at 120 ℃ for 10h until the solid substance is in a state of no moisture basically;
(4) And (4) calcining the solid matter dried in the step (3) in a muffle furnace at the temperature of 1280 ℃ for 6 hours, and then crushing the solid matter by using a ball mill to obtain the heat conduction material.
The heat conducting material prepared in this example is composed of alumina and zinc aluminate, wherein the mass percentage of zinc aluminate is 19%.
Example 2
The preparation method of the heat conduction material of the embodiment comprises the following steps:
(1) Adding 1 liter of purified water and 500 g of aluminum hydroxide into a 5 liter beaker, and stirring for 30 minutes to prepare an aluminum hydroxide aqueous solution;
(2) ZnCl was prepared in an amount of 0.75 kg and a concentration of 100 g/l 2 Aqueous solution and ammonia with concentration of 10% and pH value of 9, then ZnCl is added 2 Adding the aqueous solution and ammonia water into the aluminum hydroxide aqueous solution at the same time, and stirring for 120min to obtain a mixed solution;
(3) Centrifuging the mixed solution obtained in the step (2) by a roller centrifuge, and drying the separated solid substance in a drying oven at 120 ℃ for 10h until the solid substance is in a state of no moisture basically;
(4) And (4) calcining the solid matter dried in the step (3) in a muffle furnace at 1300 ℃ for 10h, and then crushing the solid matter by using a ball mill to obtain the heat conduction material.
The heat conducting material prepared in this example is composed of alumina and zinc aluminate, wherein the mass percentage of zinc aluminate is 27%.
Example 3
The preparation method of the heat conduction material of the embodiment comprises the following steps:
(1) Adding 1L of purified water and 500 g of aluminum hydroxide into a 5L beaker, and stirring for 30 minutes to prepare an aluminum hydroxide aqueous solution;
(2) ZnCl was prepared in an amount of 1.0 kg and a concentration of 100 g/l 2 Aqueous solution and ammonia with concentration of 10% and pH value of 9, then ZnCl is added 2 Adding the aqueous solution and ammonia water into the aluminum hydroxide aqueous solution at the same time, and stirring for 120min to obtain a mixed solution;
(3) Centrifuging the mixed solution obtained in the step (2) by a roller centrifuge, and drying the separated solid substance in a drying oven at 120 ℃ for 10h until the solid substance is in a state of no moisture basically;
(4) And (4) calcining the solid matter dried in the step (3) in a muffle furnace at 1300 ℃ for 6h, and then crushing the solid matter by using a ball mill to obtain the heat conduction material.
The heat conducting material prepared in this example is composed of alumina and zinc aluminate, wherein the mass percentage of zinc aluminate is 35%.
Example 4
The preparation method of the heat conduction material of the embodiment comprises the following steps:
(1) Adding 1 liter of purified water and 500 g of aluminum hydroxide into a 5 liter beaker, and stirring for 30 minutes to prepare an aluminum hydroxide aqueous solution;
(2) Separately, 1.25 kg of ZnCl was prepared at a concentration of 100 g/l 2 Aqueous solution and ammonia with concentration of 10% and pH value of 9, then ZnCl is added 2 Adding the aqueous solution and ammonia water into the aluminum hydroxide aqueous solution at the same time, and stirring for 120min to obtain a mixed solution;
(3) Centrifuging the mixed solution obtained in the step (2) by a roller centrifuge, and drying the separated solid substance in a drying oven at 120 ℃ for 10h until the solid substance is in a state of no moisture basically;
(4) And (4) calcining the solid matter dried in the step (3) in a muffle furnace at the temperature of 1320 ℃ for 6h, and then crushing the solid matter by using a ball mill to obtain the heat conduction material.
The heat conductive material prepared in this example was composed of alumina and zinc aluminate, wherein the mass percentage of zinc aluminate was 42%.
Example 5
The preparation method of the heat conduction material of the embodiment comprises the following steps:
(1) Adding 1 liter of purified water and 500 g of aluminum hydroxide into a 5 liter beaker, and stirring for 30 minutes to prepare an aluminum hydroxide aqueous solution;
(2) Separately, 1.5 kg of ZnCl was prepared at a concentration of 100 g/l 2 Aqueous solution and ammonia with the concentration of 10% and the PH value of 9, and then ZnCl 2 Adding the aqueous solution and ammonia water into the aluminum hydroxide aqueous solution at the same time, and stirring for 120min to obtain a mixed solution;
(3) Centrifugally separating the mixed solution obtained in the step (2) by a roller centrifuge, and drying the separated solid substances in a drying oven at 120 ℃ for 10 hours until the solid substances are basically in a moisture-free state;
(4) And (4) calcining the solid matter dried in the step (3) in a muffle furnace at 1300 ℃ for 10h, and then crushing the solid matter by using a ball mill to obtain the heat conduction material.
The heat conducting material prepared in this example is composed of alumina and zinc aluminate, wherein the mass percentage of the zinc aluminate is 48%.
Example 6
The preparation method of the heat conduction material of the embodiment comprises the following steps:
(1) Adding 1 liter of purified water and 500 g of aluminum hydroxide into a 5 liter beaker, and stirring for 30 minutes to prepare an aluminum hydroxide aqueous solution;
(2) ZnCl was prepared in an amount of 1.75 kg and a concentration of 100 g/l 2 Aqueous solution and ammonia with the concentration of 10% and the PH value of 9, and then ZnCl 2 Adding the aqueous solution and ammonia water into the aluminum hydroxide aqueous solution at the same time, and stirring for 120min to obtain a mixed solution;
(3) Centrifuging the mixed solution obtained in the step (2) by a roller centrifuge, and drying the separated solid substance in a drying oven at 120 ℃ for 10h until the solid substance is in a state of no moisture basically;
(4) And (4) calcining the solid matter dried in the step (3) in a muffle furnace at the temperature of 1300 ℃ for 10 hours, and then crushing the solid matter by using a ball mill to obtain the heat conduction material.
The heat conducting material prepared in this example is composed of alumina and zinc aluminate, wherein the mass percentage of zinc aluminate is 55%.
Example 7
The preparation method of the heat conduction material of the embodiment comprises the following steps:
(1) Adding 1 liter of purified water and 500 g of aluminum hydroxide into a 5 liter beaker, and stirring for 30 minutes to prepare an aluminum hydroxide aqueous solution;
(2) ZnCl was prepared in an amount of 2.0 kg and a concentration of 100 g/l 2 Aqueous solution and ammonia with concentration of 10% and pH value of 9, then ZnCl is added 2 Adding the aqueous solution and ammonia water into the aluminum hydroxide aqueous solution at the same time, and stirring for 120min to obtain a mixed solution;
(3) Centrifuging the mixed solution obtained in the step (2) by a roller centrifuge, and drying the separated solid substance in a drying oven at 120 ℃ for 10h until the solid substance is in a state of no moisture basically;
(4) And (4) calcining the solid matter dried in the step (3) in a muffle furnace at 1300 ℃ for 10h, and then crushing the solid matter by using a ball mill to obtain the heat conduction material.
The heat conducting material prepared in this example is composed of alumina and zinc aluminate, wherein the mass percentage of zinc aluminate is 60%.
Example 8
The preparation method of the heat conduction material of the embodiment comprises the following steps:
(1) Adding 1L of purified water and 500 g of aluminum hydroxide into a 5L beaker, and stirring for 30 minutes to prepare an aluminum hydroxide aqueous solution;
(2) ZnCl was prepared in an amount of 2.25 kg and a concentration of 100 g/l 2 Aqueous solution and ammonia with the concentration of 10% and the PH value of 9, and then ZnCl 2 Adding the aqueous solution and ammonia water into the aqueous solution of aluminum hydroxide at the same time, and stirring for 150min to obtain a mixed solution;
(3) Centrifuging the mixed solution obtained in the step (2) by a roller centrifuge, and drying the separated solid substance in a drying oven at 120 ℃ for 10h until the solid substance is in a state of no moisture basically;
(4) And (4) calcining the solid matter dried in the step (3) in a muffle furnace at the temperature of 1320 ℃ for 10 hours, and then crushing the solid matter by using a ball mill to obtain the heat conduction material.
The heat conducting material prepared in this example is composed of alumina and zinc aluminate, wherein the mass percentage of zinc aluminate is 75%.
The heat-conducting silica gel is prepared in the following steps:
and mixing 500 parts of the prepared heat conduction material with 100 parts of vinyl silicone oil, 2 parts of cross-linking agent and 2 parts of catalyst, and carrying out compression molding by using a molding device to obtain the heat conduction colloidal silica.
Wherein the crosslinking agent is tributylketoxime silane, and the catalyst is dibutyltin dilaurate.
Comparative example 1
The preparation method of the heat-conducting silica gel of the comparative example is as follows:
500 parts of spherical alumina with the grain diameter of 7 microns, 100 parts of vinyl silicone oil, 2 parts of cross-linking agent and 2 parts of catalyst are added into a mixing device for mixing treatment, and the composite material is prepared by compression molding.
Wherein the cross-linking agent is tributylketoxime silane, and the catalyst is dibutyltin dilaurate.
The thermal conductivity test data of the thermally conductive silicone gels of the above examples and comparative examples are as follows:
the above thermal conductivity test was carried out in accordance with ASTM D5470.
Claims (5)
1. A thermally conductive material, characterized by: the heat conduction material is an inorganic composite oxide formed by calcining and crushing a precursor containing a zinc source and an aluminum source.
2. The thermally conductive material of claim 1, wherein: the heat conduction material consists of alumina and zinc aluminate, wherein the mass percent of the zinc aluminate is 19-75%.
3. A method of preparing a heat conductive material according to claim 1 or 2, characterized in that: the method comprises the following steps:
(1) Adding aluminum hydroxide into purified water, and uniformly stirring to obtain an aluminum hydroxide aqueous solution;
(2) Adding an alkaline solution and an aqueous solution of a zinc source into an aqueous solution of aluminum hydroxide, and stirring for 100-150 min to prepare a mixed solution, wherein the pH value of the alkaline solution is 8.5-9;
(3) Centrifugally separating the mixed solution obtained in the step (2), and drying the separated solid substances;
(4) Calcining the solid matter dried in the step (3) at 1280-1320 ℃ for 6-10 h, and crushing to obtain the heat conduction material.
4. The production method according to claim 3, characterized in that: the alkaline solution is ammonia water or sodium hydroxide or potassium hydroxide or sodium carbonate.
5. The production method according to claim 3, characterized in that: the zinc source is ZnCl 2 。
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| CN202210892765.5A CN115216277A (en) | 2022-07-27 | 2022-07-27 | Heat conduction material and preparation method thereof |
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Application publication date: 20221021 |