CN109679198B - Heat-conducting phase-change material and preparation method thereof - Google Patents
Heat-conducting phase-change material and preparation method thereof Download PDFInfo
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- CN109679198B CN109679198B CN201811619319.7A CN201811619319A CN109679198B CN 109679198 B CN109679198 B CN 109679198B CN 201811619319 A CN201811619319 A CN 201811619319A CN 109679198 B CN109679198 B CN 109679198B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/04—Homopolymers or copolymers of ethene
- C08L23/08—Copolymers of ethene
- C08L23/0846—Copolymers of ethene with unsaturated hydrocarbons containing other atoms than carbon or hydrogen atoms
- C08L23/0853—Vinylacetate
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- 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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
- C08K2003/382—Boron-containing compounds and nitrogen
- C08K2003/385—Binary compounds of nitrogen with boron
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- Engineering & Computer Science (AREA)
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- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Physics & Mathematics (AREA)
- Combustion & Propulsion (AREA)
- Thermal Sciences (AREA)
- Materials Engineering (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention relates to a heat-conducting phase-change material and a preparation method thereof, wherein the heat-conducting phase-change material comprises the following raw materials in parts by weight: 100-200 parts of EVA resin; 100-500 parts of heat-conducting filler; 10-100 parts of a flame retardant; 1-10 parts of a coupling agent; 1-100 parts of a tackifier; 1-10 parts of an antioxidant; wherein the EVA resin has a vinyl acetate content of 25-50%. According to the invention, through the formula and the proportion of the heat-conducting phase-change material, particularly, the EVA resin with specific vinyl acetate content is adopted as the phase-change component, the problem of poor stability of the phase-change material under thermal shock aging can be effectively avoided, the EVA resin is not easy to flow and crack, and a good heat dissipation effect can be realized.
Description
Technical Field
The invention belongs to the technical field of high polymer materials, and particularly relates to a heat-conducting phase-change material and a preparation method thereof.
Background
Thermal Interface Materials (TIM) is a material commonly used for IC packaging and electronic heat dissipation, and is mainly used for filling up micro-gaps and holes with uneven surfaces generated when two Materials are jointed or contacted, reducing heat transfer resistance and improving heat dissipation performance. With the rapid development of modern electronic technology, the integration degree and the assembly density of electronic components are continuously improved, and the working power consumption and the heat productivity of the electronic components are increased sharply while providing strong use functions. High temperatures can have a detrimental effect on the stability, reliability and lifetime of electronic components. Thermally conductive interface materials play a crucial role in the thermal management of electronic devices.
The heat-conducting phase-change material is a phase-change material with heat-conducting property, can be softened or changed into a liquid state from a solid state along with the temperature change, and can reduce the interface thermal resistance. The existing phase-change materials mostly use paraffin as a phase-change component, and the paraffin is generally poor in compatibility with a polymer matrix, poor in stability under the conditions of thermal shock and thermal cycle aging, easy to flow and deform and capable of influencing the heat dissipation effect.
Disclosure of Invention
The invention aims to solve the technical problem of providing a heat-conducting phase-change material with good stability under thermal shock aging and a preparation method thereof.
In order to solve the technical problems, the invention adopts the following technical scheme:
the invention aims to provide a heat-conducting phase-change material which comprises the following raw materials in parts by weight:
wherein the EVA resin has a vinyl acetate content of 25-50%.
Preferably, the melting point of the EVA resin is 30-70 ℃.
Preferably, the heat conducting filler is one or a mixture of more of aluminum oxide, zinc oxide, aluminum hydroxide, silicon micropowder, aluminum nitride, boron nitride, aluminum powder and graphite.
Preferably, the median particle size of the heat-conducting filler is 0.5-100 μm.
Preferably, the flame retardant is aluminum hydroxide, magnesium hydroxide, tetrabromobisphenol A, Sb2O3And one or more of alkyl phosphates.
Preferably, the coupling agent is one or more of a silane coupling agent, a titanate coupling agent and an aluminate coupling agent.
Preferably, the tackifier is one or more of C9 petroleum resin, C5 petroleum resin, rosin resin and terpene resin.
Preferably, the antioxidant is one or more of hindered phenol, hindered amine and phosphite antioxidant.
The invention also aims to provide a preparation method of the heat-conducting phase change material, which is prepared by uniformly mixing the EVA resin, the heat-conducting filler, the coupling agent, the flame retardant, the tackifier and the antioxidant in a kneader in a melt blending mode, and calendering the mixture into a sheet with the required thickness by using a compression roller.
Preferably, the mixture is stirred at 60 to 70 ℃ for 20 to 30 min.
The invention also aims to provide a preparation method of the heat-conducting phase change material, which comprises the steps of dissolving EVA resin with a solvent, adding a heat-conducting filler, a coupling agent, a flame retardant, a tackifier and an antioxidant, coating the mixture into a film of 10-200 mu m in a coating mode, removing the solvent, and cooling and forming the film.
Preferably, the solvent is toluene or xylene.
Due to the implementation of the technical scheme, compared with the prior art, the invention has the following advantages:
according to the invention, through the formula and the proportion of the heat-conducting phase-change material, particularly, the EVA resin with specific vinyl acetate content is adopted as the phase-change component, the problem of poor stability of the phase-change material under thermal shock aging can be effectively avoided, the EVA resin is not easy to flow and crack, and good heat dissipation effect can be realized.
In addition, the preparation method of the invention has simple process and easy operation.
Detailed Description
The present invention will be described in further detail with reference to specific examples, but the present invention is not limited to the following examples. The implementation conditions adopted in the embodiments can be further adjusted according to different requirements of specific use, and the implementation conditions not mentioned are conventional conditions in the industry. All other embodiments obtained by a person skilled in the art without making any inventive step are within the scope of protection of the present invention.
Examples 1 to 4, comparative examples 1 to 6
The raw material components for each example are shown in Table 1, and the performance data are shown in Table 2.
The preparation methods of the heat-conducting phase-change materials of examples 1 to 3 and comparative examples 1 to 6 were as follows:
sequentially adding EVA resin, heat-conducting filler, coupling agent, flame retardant, tackifier and antioxidant into a kneader according to a certain proportion; stirring for 20-30 min at the temperature of 60-70 ℃, discharging after uniformly stirring, rolling into a sheet with a certain thickness by using a multi-roll calender, cooling, forming and cutting.
The preparation method of the heat-conducting phase-change material of embodiment 4 comprises the following steps:
solvent-based coating: dissolving EVA in toluene or xylene solvent, sequentially adding heat-conducting filler, coupling agent, flame retardant, tackifier and antioxidant, stirring uniformly, coating into a film of 10-200 um by coating, at 80-100 ℃, removing solvent, cooling, molding and cutting.
TABLE 1
TABLE 2
The thermal conductivity coefficient and thermal resistance testing method adopts an ASTM D5470 method to test the thermal resistance values of three thermal conductive materials with different thicknesses, the thermal conductivity coefficient is obtained through linear fitting, and the model of testing equipment is LW 9389.
The present invention has been described in detail in order to enable those skilled in the art to understand the invention and to practice it, and it is not intended to limit the scope of the invention, and all equivalent changes and modifications made according to the spirit of the present invention should be covered by the present invention.
Claims (9)
1. A thermally conductive phase change material, comprising: the raw material components by weight portion are as follows:
100-150 parts of EVA resin;
350-500 parts of heat-conducting filler;
10-100 parts of a flame retardant;
1-10 parts of a coupling agent;
5-10 parts of a tackifier;
1-10 parts of an antioxidant;
the EVA resin has the vinyl acetate content of 41-50%, and the melting point of the EVA resin is 30-45 ℃.
2. The thermally conductive phase change material of claim 1, wherein: the heat-conducting filler is one or a mixture of more of aluminum oxide, zinc oxide, aluminum hydroxide, silicon micropowder, aluminum nitride, boron nitride, aluminum powder and graphite.
3. The thermally conductive phase change material of claim 1, wherein: the median particle size of the heat-conducting filler is 0.5-100 mu m.
4. The thermally conductive phase change material of claim 1, wherein: the flame retardant is one or more of aluminum hydroxide, magnesium hydroxide, tetrabromobisphenol A, Sb2O3 and alkyl phosphate.
5. The thermally conductive phase change material of claim 1, wherein: the coupling agent is one or more of silane coupling agent, titanate coupling agent and aluminate coupling agent.
6. The thermally conductive phase change material of claim 1, wherein: the tackifier is one or more of C9 petroleum resin, C5 petroleum resin, rosin resin and terpene resin.
7. The thermally conductive phase change material of claim 1, wherein: the antioxidant is one or more of hindered phenol, hindered amine and phosphite antioxidant.
8. A method for preparing a thermally conductive phase change material as claimed in any one of claims 1 to 7, wherein: the EVA resin, the heat-conducting filler, the coupling agent, the flame retardant, the tackifier and the antioxidant are uniformly mixed in a kneader by a melt blending mode, and the mixture is calendered into a sheet with required thickness by a compression roller to prepare the heat-conducting heat-insulating sheet.
9. A method for preparing a thermally conductive phase change material as claimed in any one of claims 1 to 7, wherein: dissolving EVA resin with a solvent, adding a heat-conducting filler, a coupling agent, a flame retardant, a tackifier and an antioxidant, coating the mixture into a film of 10-200 mu m in a coating mode, removing the solvent, and cooling and forming to obtain the EVA heat-conducting.
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| CN201811619319.7A CN109679198B (en) | 2018-12-28 | 2018-12-28 | Heat-conducting phase-change material and preparation method thereof |
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| CN109679198B true CN109679198B (en) | 2022-03-08 |
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| CN1880399A (en) * | 2005-06-16 | 2006-12-20 | 鸿富锦精密工业（深圳）有限公司 | Thermally conductive glue and method of manufacturing same |
| CN1990818A (en) * | 2005-12-28 | 2007-07-04 | 财团法人工业技术研究院 | Composition for heat interfacial material |
| CN1990816A (en) * | 2005-12-28 | 2007-07-04 | 财团法人工业技术研究院 | Composition for heat interfacial material |
| CN106479030A (en) * | 2016-10-20 | 2017-03-08 | 东莞市兆科电子材料科技有限公司 | A kind of heat conduction phase change composite and preparation method thereof |
| CN107163182A (en) * | 2017-07-06 | 2017-09-15 | 昆山市中迪新材料技术有限公司 | A kind of phase-change heat conductive material and preparation method thereof and the composition for preparing phase-change heat conductive material |
| CN108003406A (en) * | 2017-12-20 | 2018-05-08 | 深圳德邦界面材料有限公司 | A kind of heatproof heat conduction phase-change material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US6483707B1 (en) * | 2001-06-07 | 2002-11-19 | Loctite Corporation | Heat sink and thermal interface having shielding to attenuate electromagnetic interference |
| TWI291480B (en) * | 2005-12-20 | 2007-12-21 | Ind Tech Res Inst | Composition for thermal interface materials |
| JP6266116B2 (en) * | 2013-09-11 | 2018-01-24 | ダウ グローバル テクノロジーズ エルエルシー | Multiphase elastic heat conductive material |
| CN106753263B (en) * | 2016-12-27 | 2021-03-05 | 深圳德邦界面材料有限公司 | Heat-conducting phase-change material and preparation method thereof |
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- 2018-12-28 CN CN201811619319.7A patent/CN109679198B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1880399A (en) * | 2005-06-16 | 2006-12-20 | 鸿富锦精密工业（深圳）有限公司 | Thermally conductive glue and method of manufacturing same |
| CN1990818A (en) * | 2005-12-28 | 2007-07-04 | 财团法人工业技术研究院 | Composition for heat interfacial material |
| CN1990816A (en) * | 2005-12-28 | 2007-07-04 | 财团法人工业技术研究院 | Composition for heat interfacial material |
| CN106479030A (en) * | 2016-10-20 | 2017-03-08 | 东莞市兆科电子材料科技有限公司 | A kind of heat conduction phase change composite and preparation method thereof |
| CN107163182A (en) * | 2017-07-06 | 2017-09-15 | 昆山市中迪新材料技术有限公司 | A kind of phase-change heat conductive material and preparation method thereof and the composition for preparing phase-change heat conductive material |
| CN108003406A (en) * | 2017-12-20 | 2018-05-08 | 深圳德邦界面材料有限公司 | A kind of heatproof heat conduction phase-change material and preparation method thereof |
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