CN109679198A - A kind of heat conductive phase change material and preparation method thereof - Google Patents

A kind of heat conductive phase change material and preparation method thereof Download PDF

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Publication number
CN109679198A
CN109679198A CN201811619319.7A CN201811619319A CN109679198A CN 109679198 A CN109679198 A CN 109679198A CN 201811619319 A CN201811619319 A CN 201811619319A CN 109679198 A CN109679198 A CN 109679198A
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phase change
change material
heat conductive
conductive phase
heat
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CN109679198B (en
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李明轩
邓建波
姚明乾
高畠博
陈洪野
吴小平
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Suzhou Competition Application Technology Ltd By Share Ltd
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Suzhou Competition Application Technology Ltd By Share Ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L23/00Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
    • C08L23/02Compositions 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
    • C08L23/04Homopolymers or copolymers of ethene
    • C08L23/08Copolymers of ethene
    • C08L23/0846Copolymers of ethene with unsaturated hydrocarbons containing other atoms than carbon or hydrogen atoms
    • C08L23/0853Vinylacetate
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K5/00Heat-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
    • C09K5/08Materials not undergoing a change of physical state when used
    • C09K5/14Solid materials, e.g. powdery or granular
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2227Oxides; Hydroxides of metals of aluminium
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/38Boron-containing compounds
    • C08K2003/382Boron-containing compounds and nitrogen
    • C08K2003/385Binary compounds of nitrogen with boron
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/08Stabilised against heat, light or radiation or oxydation

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Combustion & Propulsion (AREA)
  • Thermal Sciences (AREA)
  • Materials Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The present invention relates to a kind of heat conductive phase change materials and preparation method thereof, and by weight, the raw material of heat conductive phase change material includes following component: 100~200 parts of EVA resin;100~500 parts of heat filling;10~100 parts of fire retardant;1~10 part of coupling agent;1~100 part of tackifier;1~10 part of antioxidant;Wherein, the vinyl acetate content of the EVA resin is 25~50%.The present invention passes through the formula and proportion to heat conductive phase change material, EVA resin especially with specific vinyl acetate content is phase transformation component, it can effectively avoid the problem of stability difference of the phase-change material under thermal shock aging, and it is not easy trickling cracking, good heat dissipation effect can be achieved, heat-conducting interface material prepared by the present invention has good thermal conductivity, excellent wearability, ageing-resistant performance, and room temperature flexibility is more preferable, thinner, reduction interface resistance, easy to process and use can be done by solvent coating method.

Description

A kind of heat conductive phase change material and preparation method thereof
Technical field
The invention belongs to technical field of polymer materials, and in particular to a kind of heat conductive phase change material and preparation method thereof.
Background technique
Heat-conducting interface material (Thermal Interface Materials, TIM), be one kind be commonly used to IC package and The material of electronic radiation is mainly used for filling up the hole of the microvoid and surface irregularity that generate when two kinds of material engagements or contact Heat transfer resistance is reduced in hole, improves heat dissipation performance.As contemporary electronic technology rapidly develops, the degree of integration of electronic component It is continuously improved with packing density, while providing powerful use function, also results in its operating power consumption and calorific value It increased dramatically.High temperature will generate harmful influence in stability, reliability and service life on electronic component.Heat-conducting interface material Vital effect is played in electronic device heat management.
Heat conductive phase change material is a kind of phase-change material with heating conduction, can vary with temperature softened by solid state or It is changed into liquid, and a kind of composite material of interface resistance can be reduced.Existing phase-change material is mostly by paraffin as phase transformation Component, paraffin is generally poor with polymer matrix compatability, poor in thermal shock, thermal cycling ageing condition stability inferior, Yi Liu Deformation is dropped down, heat dissipation effect is influenced.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of thermally conductive phase transformation materials good in thermal shock aging stability inferior Material and preparation method thereof.
In order to solve the above technical problems, the present invention adopts the following technical scheme that:
It is an object of the present invention to provide a kind of heat conductive phase change materials, and by weight, raw material includes following component:
Wherein, the vinyl acetate content of the EVA resin is 25~50%.
Preferably, the fusing point of the EVA resin is 30~70 DEG C.
Preferably, the heat filling is aluminium oxide, zinc oxide, aluminium hydroxide, silicon powder, aluminium nitride, boron nitride, aluminium The mixture of one or more of powder, graphite.
Preferably, the median of the heat filling is 0.5~100 μm.
Preferably, the fire retardant is aluminium hydroxide, magnesium hydroxide, tetrabromobisphenol A, Sb2O3, in alkyl acid phosphate esters One or more.
Preferably, the coupling agent is one of silane coupling agent, titanate coupling agent, aluminate coupling agent or several Kind.
Preferably, the tackifier are one of C9 Petropols, C5 Petropols, rosin resin, terpene resin Or it is several.
Preferably, the antioxidant is one of Hinered phenols, hindered amines, phosphite ester antioxidant or several Kind.
It is a further object to provide the preparation methods of the heat conductive phase change material described in one kind, pass through melt blending Mode EVA resin, heat filling, coupling agent, fire retardant, tackifier, antioxidant are uniformly mixed in kneader, then pass through The sheet material that mixture is rolled into required thickness is made pressure roller.
Preferably, 20~30min is stirred at 60~70 DEG C to be mixed.
It is also another object of the present invention to provide the preparation methods of the heat conductive phase change material described in one kind, first by EVA resin It is dissolved with solvent, adds heat filling, coupling agent, fire retardant, tackifier, antioxidant, then painted by way of coating The film of 10~200um is cooled and shaped after solvent removal and is made.
Preferably, the solvent is toluene or dimethylbenzene.
Due to the implementation of above technical scheme, the invention has the following advantages over the prior art:
The present invention is by the formula and proportion to heat conductive phase change material, especially with the EVA of specific vinyl acetate content Resin is phase transformation component, can effectively avoid the problem of stability difference of the phase-change material under thermal shock aging, and is not easy trickling and opens It splits, it can be achieved that good heat dissipation effect, heat-conducting interface material prepared by the present invention have good thermal conductivity, excellent is wear-resisting Property, ageing-resistant performance, and room temperature flexibility is more preferable, thinner (web-like) that can be done by solvent coating method, reduces interface Thermal resistance, easy to process and use.
In addition, preparation method process of the invention is simple, it is easy to operate.
Specific embodiment
The present invention will be further described in detail combined with specific embodiments below, but the present invention is not limited to following implementations Example.Implementation condition used in the examples can do further adjustment according to specifically used different requirements, the implementation being not specified Condition is the normal condition in the industry.It is obtained by those of ordinary skill in the art without making creative efforts All other embodiment, shall fall within the protection scope of the present invention.
Embodiment 1 to 4, comparative example 1 to 6
The raw material components of each embodiment are shown in Table 1, and performance data is shown in Table 2.
Embodiment 1 to 3, the heat conductive phase change material of comparative example 1 to 6 the preparation method comprises the following steps:
It is sequentially placed into EVA resin, heat filling, coupling agent, fire retardant, tackifier, antioxygen in proportion in kneader machine Agent;60~70 DEG C of temperature, 20~30min is stirred, is discharged after mixing evenly, then is pressed into multi-rolling mill certain thickness thin Piece is cut after rear cooling and shaping.
The heat conductive phase change material of embodiment 4 the preparation method comprises the following steps:
Solvent type coating: first EVA toluene or xylene solvent are dissolved, sequentially add heat filling, coupling agent, resistance Agent, tackifier, antioxidant are fired, stirs evenly, the film of 10~200um, temperature 80-100 is then painted by way of coating DEG C, it is cooled and shaped and cuts after solvent removal.
Table 1
Table 2
Above-mentioned thermal coefficient and thermo-resistance measurement method are tested using ASTM D5470 method, test leading for three different-thickness The thermal resistance value of hot material, linear fitting obtain thermal coefficient, test equipment model LW9389.
The present invention is described in detail above, its object is to allow the personage for being familiar with this field technology that can understand this The content of invention is simultaneously implemented, and it is not intended to limit the scope of the present invention, all Spirit Essence institutes according to the present invention The equivalent change or modification of work, should be covered by the scope of protection of the present invention.

Claims (10)

1. a kind of heat conductive phase change material, it is characterised in that: by weight, raw material includes following component:
Wherein, the vinyl acetate content of the EVA resin is 25~50%.
2. heat conductive phase change material according to claim 1, it is characterised in that: the fusing point of the EVA resin is 30~70 ℃。
3. heat conductive phase change material according to claim 1, it is characterised in that: the heat filling is aluminium oxide, oxidation The mixture of one or more of zinc, aluminium hydroxide, silicon powder, aluminium nitride, boron nitride, aluminium powder, graphite.
4. heat conductive phase change material according to claim 1, it is characterised in that: the median of the heat filling is 0.5~100 μm.
5. heat conductive phase change material according to claim 1, it is characterised in that: the fire retardant is aluminium hydroxide, hydrogen-oxygen Change magnesium, tetrabromobisphenol A, Sb2O3, one or more of alkyl acid phosphate esters.
6. heat conductive phase change material according to claim 1, it is characterised in that: the coupling agent is silane coupling agent, titanium One or more of acid esters coupling agent, aluminate coupling agent.
7. heat conductive phase change material according to claim 1, it is characterised in that: the tackifier are C9 Petropols, C5 One or more of Petropols, rosin resin, terpene resin.
8. heat conductive phase change material according to claim 1, it is characterised in that: the antioxidant is Hinered phenols, is obstructed One or more of amine, phosphite ester antioxidant.
9. a kind of preparation method of such as heat conductive phase change material described in any item of the claim 1 to 8, it is characterised in that: pass through The mode of melt blending mixes EVA resin, heat filling, coupling agent, fire retardant, tackifier, antioxidant in kneader It is even, then the sheet material that mixture is rolled into required thickness is made by pressure roller.
10. a kind of preparation method of such as heat conductive phase change material described in any item of the claim 1 to 8, it is characterised in that: first will EVA resin is dissolved with solvent, adds heat filling, coupling agent, fire retardant, tackifier, antioxidant, then passes through the side of coating Formula paints the film of 10~200um, is cooled and shaped and is made after solvent removal.
CN201811619319.7A 2018-12-28 2018-12-28 Heat-conducting phase-change material and preparation method thereof Active CN109679198B (en)

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Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20020186537A1 (en) * 2001-06-07 2002-12-12 Freuler Raymond G. Heat sink and thermal interface having shielding to attenuate electromagnetic interference
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
TW200724596A (en) * 2005-12-20 2007-07-01 Ind Tech Res Inst Composition for thermal interface materials
CN1990816A (en) * 2005-12-28 2007-07-04 财团法人工业技术研究院 Composition for heat interfacial material
CN1990818A (en) * 2005-12-28 2007-07-04 财团法人工业技术研究院 Composition for heat interfacial material
US20160177159A1 (en) * 2013-09-11 2016-06-23 Dow Global Technologies Llc Multi-phase elastomeric thermally conductive materials
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
CN106753263A (en) * 2016-12-27 2017-05-31 深圳德邦界面材料有限公司 Heat conduction phase-change material 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

Patent Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20020186537A1 (en) * 2001-06-07 2002-12-12 Freuler Raymond G. Heat sink and thermal interface having shielding to attenuate electromagnetic interference
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
TW200724596A (en) * 2005-12-20 2007-07-01 Ind Tech Res Inst Composition for thermal interface materials
CN1990816A (en) * 2005-12-28 2007-07-04 财团法人工业技术研究院 Composition for heat interfacial material
CN1990818A (en) * 2005-12-28 2007-07-04 财团法人工业技术研究院 Composition for heat interfacial material
US20160177159A1 (en) * 2013-09-11 2016-06-23 Dow Global Technologies Llc Multi-phase elastomeric thermally conductive materials
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
CN106753263A (en) * 2016-12-27 2017-05-31 深圳德邦界面材料有限公司 Heat conduction phase-change material 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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