CN103333447A - Phase-change thermal interface material and preparation method thereof - Google Patents
Phase-change thermal interface material and preparation method thereof Download PDFInfo
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- CN103333447A CN103333447A CN 201310260251 CN201310260251A CN103333447A CN 103333447 A CN103333447 A CN 103333447A CN 201310260251 CN201310260251 CN 201310260251 CN 201310260251 A CN201310260251 A CN 201310260251A CN 103333447 A CN103333447 A CN 103333447A
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Abstract
The invention discloses a phase-change thermal interface material and a preparation method thereof. The phase-change thermal interface material mainly comprises phase-change resin, one or more of heat-conducting powder, a cross-linking agent, a polymerization initiator and a coupling agent. The preparation method of the phase-change thermal interface material comprises the following steps of: adding the polymerization initiator to the phase-change resin, and initially polymerizing the phase-change resin through light polymerization or thermal polymerization; then adding the coupling agent, uniformly mixing, then adding the heat-conducting powder for multiple times, and then fast stirring to promote the combination of the coupling agent and the heat-conducting powder; after mixing for certain time, adding the cross-linking agent and supplementing the polymerization initiator to obtain the phase-change thermal interface material. According to the invention, a polymer generates a certain degree of cross-linking; the phase-change thermal interface material disclosed by the invention has the advantage that a heat-conducting fin can not generate phase separation under the condition without influencing phase-change property when being increased in temperature in such a way that the cross-linking degree of the polymer is controlled.
Description
Technical field
The invention belongs to functionalized macromolecular material field, be specifically related to a kind of phase change heat interfacial material and preparation method thereof.
Background technology
Electronics can produce heat in use, die sites especially, and thermal value is big, and usually uses the heat interfacial material with high thermal conductivity to conduct heat between electro-heat equipment and heat abstractor, with the excluding air bad accumulation of heat that causes that conducts heat.
Common heat interfacial material has conducting strip, thermal grease, phase-transition material; Conducting strip is solid-state, and is easy to use, but reaches 3.0w/m.K when above when thermal conductivity, and hardness obviously raises, and is difficult to get rid of ideally the space between the interface.Thermal grease is the thickness paste, even high performance thermal grease, it still can get rid of interfacial gap more satisfactoryly, but need smear when using evenly, cause and use inconvenience, the unnecessary thermal grease that the interface is squeezed out when fitting may pollute parts on every side, and thermal grease after use for some time solid-liquid separation takes place, heat transfer property decline; Phase-transition material has the advantage of conducting strip and thermal grease concurrently, is sheet material during room temperature, and is easy to operate, becomes thickly when being heated, and can effectively get rid of the gap.
And present phase-transition material multidate changing resin adds heat conduction powder formation, in order to make it docile and obedient effect is arranged, and often needs to increase tackifying resin and realizes.The phase-transition material that colds and heat succeed each other for a long time is subjected to displacement, and when serious the same being separated of similar thermal grease may take place, and causes the decline of heat conductivility.
Summary of the invention
The purpose of this invention is to provide a kind of phase change heat interfacial material and preparation method thereof, polymkeric substance is produced to a certain degree crosslinked, crosslinking degree by the control polymkeric substance, the phase change heat interfacial material is not influenced under the situation of its phase change performance when temperature raises, had concurrently conducting strip can not be separated advantage.
Heat interfacial material of the present invention mainly is made of a kind of phase change resin, one or more heat conduction powders, a kind of linking agent, a kind of polymerization starter and a kind of coupling agent.
Wherein, described phase change resin is obtained by polymerization by chain alkyl (methyl) acrylate resin.This chain alkyl is straight chain type or the branch chain type alkyl that contains 10 carbon to 18 carbon.The straight chain type alkyl of preferred 12～15 carbon.
Described heat conduction powder can be that ceramics powder also can be metal powder.Ceramics powder has insulativity, but heat conductivility is not as having the metal powder of conductivity.Described ceramics powder can be aluminum oxide, zinc oxide, silicon-dioxide, magnesium oxide, boron nitride, silicon nitride, silicon carbide, aluminium nitride etc., and metal powder can be powders such as silver powder, copper powder, aluminium powder.
Described heat conduction powder can be spherical, needle-like, sheet, and is random.
Described a kind of linking agent is the acrylate monomer with two or more acrylic functional groups, the acrylate monomer that preferably has two acrylic functional groups, more preferably 1,6-hexylene glycol double methacrylate, two contracting propylene glycol double methacrylates, tripropylene glycol double methacrylate, most preferably 1,6-hexylene glycol double methacrylate is because it has strong dilution capacity, certain snappiness, low volatilization.
Polymerization initiator of the present invention can be that light trigger also can be the superoxide thermal initiator.The preferred TPO of available light trigger and 819, the preferred lauroyl peroxide of superoxide thermal initiator.
Coupling agent of the present invention can be that titanate coupling agent also can be silane coupling agent.Titanate coupling agent is preferably with commercial three hard ester acid isopropyl titanates, silane coupling agent is the preferred and similar chain alkyl silicone resin of phase change resin structure then, the chain alkyl siloxanes that more preferably contains 8 carbon to 16 carbon most preferably contains the chain alkyl siloxanes of 12～15 carbon.
The effect of coupling agent mainly is that powder surface is handled, and strengthens the consistency of powder and resin, improves the addition of powder.
The present invention also provides the preparation method of this phase change heat interfacial material: will add polymerization starter in the phase change resin, by photopolymerization or thermopolymerization the phase change resin is carried out preliminary polymerization, then add coupling agent, add the heat conduction powder after mixing several times, then stir fast, promote the combination of coupling agent and heat conduction powder.Behind the certain hour to be mixed, add linking agent and add polymerization starter, can obtain the phase change heat interfacial material.
By the rolling press calendering, sulfuration produces partial cross-linked, cuts or rolling, namely gets sheet material or the coiled material of phase change heat interfacial material then.
Beneficial effect of the present invention is:
Polymkeric substance is produced to a certain degree crosslinked, and the crosslinking degree by the control polymkeric substance does not influence under the situation of its phase change performance the phase change heat interfacial material when temperature raises, had concurrently conducting strip can not be separated advantage.
Specific embodiment
A certain amount of polymerization starter will be added in the phase change resin, by photopolymerization or thermopolymerization with the phase change resin polymerization to certain viscosity, then add coupling agent, add the heat conduction powder after mixing several times, then stir fast, promote the combination of coupling agent and heat conduction powder.Behind the certain hour to be mixed, drip a certain amount of linking agent and add polymerization starter.
The above-mentioned material that mixes is rolled by rolling press, and sulfuration produces partial cross-linked, cuts or rolling, namely gets sheet material or the coiled material of phase change heat interfacial material.
Embodiment 1
Get 100 parts of decyl methacrylic esters, after light trigger TPO0.25 part mixes, polyase 13 is 0 minute under the ultraviolet lamp of 100W, obtain the poly-decyl methacrylic ester of viscosity 1000～1300cps, then add 1.2 part of three hard ester acid isopropyl titanate, stir in planetary mixer that to divide the particle diameter that adds 600 parts for three times after 30 minutes be 3 microns ball aluminum powder, stir after 2 hours, drip 0.12 part of 1,6-hexylene glycol double methacrylate, light trigger TPO0.25 part.Vacuumize, continue to stir 30 minutes.Through preheating, calendering, curing, obtain the partial cross-linked phase change heat interfacial material of 42～45 ℃ of thermal conductivity 5.2W/m.K, transformation temperature.
Phase change heat interfacial material with 0.25mm thickness at room temperature is attached on the aluminium sheet of vertical placement, puts into-50～60 ℃ high-low temperature test chamber, and through round-robin test in 1000 hours, the phase change heat interfacial material trickling did not take place and is separated.
Embodiment 2
Remove 100 parts of pentadecyl acrylate, 0.5 part of thermal initiator lauroyl peroxide, mix post-heating to 120 ℃, obtain the poly-pentadecyl acrylate of viscosity 1500cps～1800cps after 30 minutes, then be down to room temperature, add 2 parts of octyl group Trimethoxy silanes, in planetary mixer, stir after 30 minutes the aluminium nitride of 2 microns of particle diameters that add 500 parts for three times, stir after 3 hours, drip 0.5 part of 1,6-hexylene glycol double methacrylate, 0.5 part of lauroyl peroxide, vacuumize, continue to stir 30 minutes.Through preheating, calendering, curing, obtain thermal conductivity 4.0W/m.K, the partial cross-linked phase-change thermal interface material that transformation temperature is 47～51 ℃.
With the phase change heat interfacial material of thickness with 0.25mm thickness, at room temperature be attached on the aluminium sheet of vertical placement, put into-50～60 ℃ high-low temperature test chamber, through round-robin test in 1000 hours, trickling did not take place and is separated in the phase change heat interfacial material.
Above-mentioned example only is explanation technical conceive of the present invention and characteristics, and its purpose is to allow the people who is familiar with this technology can understand content of the present invention and enforcement according to this, can not limit protection scope of the present invention with this.All equivalent transformations that spirit is done according to the present invention or modification all should be encompassed within protection scope of the present invention.
Claims (6)
1. phase change heat interfacial material and preparation method thereof.It is characterized in that being constituted by a kind of phase change resin, one or more heat conduction powders, a kind of linking agent, a kind of polymerization starter and a kind of coupling agent.
2. phase change heat interfacial material according to claim 1 is characterized in that:
Described phase change resin is obtained by polymerization by (methyl) acrylate resin of chain alkyl;
Described heat conduction powder is ceramics powder or metal powder;
Described linking agent is the acrylate monomer with two or more acrylic functional groups;
Described polymerization initiator is light trigger or superoxide thermal initiator;
Described coupling agent is titanate coupling agent or silane coupling agent.
3. phase change heat interfacial material according to claim 2 is characterized in that:
Described chain alkyl is straight chain type or the branch chain type alkyl that contains 10 carbon to 18 carbon;
Described ceramics powder heat conduction powder can be in aluminum oxide, zinc oxide, silicon-dioxide, magnesium oxide, boron nitride, silicon nitride, silicon carbide, the aluminium nitride one or more with any than mixing; Described metal powder ceramics powder heat conduction powder can be one or more of silver powder, copper powder, aluminium powder with any than mixing;
Described linking agent is a kind of in 1,6-hexylene glycol double methacrylate, two contracting propylene glycol double methacrylates, the tripropylene glycol double methacrylate;
Described polymkeric substance light trigger is TPO or 819, and the polymer peroxide thermal initiator is lauroyl peroxide;
Described titanate coupling agent is three hard ester acid isopropyl titanates, and silane coupling agent is and the similar chain alkyl silicone resin of phase change resin structure.
4. phase change heat interfacial material according to claim 2 is characterized in that:
Described chain alkyl is straight chain type or the branch chain type alkyl that contains 10 carbon to 15 carbon;
Described conductive powder shape is spherical, needle-like, sheet or random;
Described linking agent is 1,6-hexylene glycol double methacrylate;
Described silane coupling agent is the chain alkyl siloxanes that contains 8 carbon to 16 carbon.
5. phase change heat interfacial material according to claim 2 is characterized in that described silane coupling agent is the chain alkyl siloxanes that contains 12 carbon to 15 carbon.
6. the preparation method of phase change heat interfacial material according to claim 1, it is characterized in that comprising following steps: will add polymerization starter in the phase change resin, by photopolymerization or thermopolymerization the phase change resin is carried out preliminary polymerization, then add coupling agent, add the heat conduction powder after mixing several times, then stir fast and make its combination, add linking agent and polymerization starter again, mixing gets final product.
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Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105315414A (en) * | 2015-10-28 | 2016-02-10 | 苏州天脉导热科技有限公司 | Preparation method for phase-change heat conduction silicon sheet |
| TWI576414B (en) * | 2015-11-20 | 2017-04-01 | 財團法人工業技術研究院 | Packaging composition and packing structure employing the same |
| 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 |
| CN107312130A (en) * | 2017-07-06 | 2017-11-03 | 昆山市中迪新材料技术有限公司 | A kind of Heat Conduction Material and preparation method thereof and the composition for preparing Heat Conduction Material |
| US10068830B2 (en) | 2014-02-13 | 2018-09-04 | Honeywell International Inc. | Compressible thermal interface materials |
| US10155894B2 (en) | 2014-07-07 | 2018-12-18 | Honeywell International Inc. | Thermal interface material with ion scavenger |
| US10174433B2 (en) | 2013-12-05 | 2019-01-08 | Honeywell International Inc. | Stannous methanesulfonate solution with adjusted pH |
| CN109269179A (en) * | 2018-09-10 | 2019-01-25 | 苏州卓睿特新材料科技有限公司 | Phase-change material accumulation of energy insulating tube for zero energy consumption insulated container of passive type |
| US10287471B2 (en) | 2014-12-05 | 2019-05-14 | Honeywell International Inc. | High performance thermal interface materials with low thermal impedance |
| US10312177B2 (en) | 2015-11-17 | 2019-06-04 | Honeywell International Inc. | Thermal interface materials including a coloring agent |
| US10428256B2 (en) | 2017-10-23 | 2019-10-01 | Honeywell International Inc. | Releasable thermal gel |
| US10501671B2 (en) | 2016-07-26 | 2019-12-10 | Honeywell International Inc. | Gel-type thermal interface material |
| US10781349B2 (en) | 2016-03-08 | 2020-09-22 | Honeywell International Inc. | Thermal interface material including crosslinker and multiple fillers |
| US11041103B2 (en) | 2017-09-08 | 2021-06-22 | Honeywell International Inc. | Silicone-free thermal gel |
| US11072706B2 (en) | 2018-02-15 | 2021-07-27 | Honeywell International Inc. | Gel-type thermal interface material |
| US11373921B2 (en) | 2019-04-23 | 2022-06-28 | Honeywell International Inc. | Gel-type thermal interface material with low pre-curing viscosity and elastic properties post-curing |
| CN115368878A (en) * | 2022-08-24 | 2022-11-22 | 苏州天脉导热科技股份有限公司 | Flexible flame-retardant silicon-free heat-conducting gasket and preparation method thereof |
| CN115505264A (en) * | 2022-08-12 | 2022-12-23 | 超聚变数字技术有限公司 | Paste-like thermal interface material, preparation method thereof and electronic equipment |
-
2013
- 2013-06-26 CN CN 201310260251 patent/CN103333447A/en active Pending
Cited By (20)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10174433B2 (en) | 2013-12-05 | 2019-01-08 | Honeywell International Inc. | Stannous methanesulfonate solution with adjusted pH |
| US10068830B2 (en) | 2014-02-13 | 2018-09-04 | Honeywell International Inc. | Compressible thermal interface materials |
| US10155894B2 (en) | 2014-07-07 | 2018-12-18 | Honeywell International Inc. | Thermal interface material with ion scavenger |
| US10428257B2 (en) | 2014-07-07 | 2019-10-01 | Honeywell International Inc. | Thermal interface material with ion scavenger |
| US10287471B2 (en) | 2014-12-05 | 2019-05-14 | Honeywell International Inc. | High performance thermal interface materials with low thermal impedance |
| CN105315414A (en) * | 2015-10-28 | 2016-02-10 | 苏州天脉导热科技有限公司 | Preparation method for phase-change heat conduction silicon sheet |
| US10312177B2 (en) | 2015-11-17 | 2019-06-04 | Honeywell International Inc. | Thermal interface materials including a coloring agent |
| TWI576414B (en) * | 2015-11-20 | 2017-04-01 | 財團法人工業技術研究院 | Packaging composition and packing structure employing the same |
| US10781349B2 (en) | 2016-03-08 | 2020-09-22 | Honeywell International Inc. | Thermal interface material including crosslinker and multiple fillers |
| US10501671B2 (en) | 2016-07-26 | 2019-12-10 | Honeywell International Inc. | Gel-type thermal interface material |
| CN107163182B (en) * | 2017-07-06 | 2019-08-02 | 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 being used to prepare phase-change heat conductive material |
| CN107312130A (en) * | 2017-07-06 | 2017-11-03 | 昆山市中迪新材料技术有限公司 | A kind of Heat Conduction Material and preparation method thereof and the composition for preparing Heat Conduction Material |
| 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 |
| US11041103B2 (en) | 2017-09-08 | 2021-06-22 | Honeywell International Inc. | Silicone-free thermal gel |
| US10428256B2 (en) | 2017-10-23 | 2019-10-01 | Honeywell International Inc. | Releasable thermal gel |
| US11072706B2 (en) | 2018-02-15 | 2021-07-27 | Honeywell International Inc. | Gel-type thermal interface material |
| CN109269179A (en) * | 2018-09-10 | 2019-01-25 | 苏州卓睿特新材料科技有限公司 | Phase-change material accumulation of energy insulating tube for zero energy consumption insulated container of passive type |
| US11373921B2 (en) | 2019-04-23 | 2022-06-28 | Honeywell International Inc. | Gel-type thermal interface material with low pre-curing viscosity and elastic properties post-curing |
| CN115505264A (en) * | 2022-08-12 | 2022-12-23 | 超聚变数字技术有限公司 | Paste-like thermal interface material, preparation method thereof and electronic equipment |
| CN115368878A (en) * | 2022-08-24 | 2022-11-22 | 苏州天脉导热科技股份有限公司 | Flexible flame-retardant silicon-free heat-conducting gasket and preparation method thereof |
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Application publication date: 20131002 |