CN112194898A - Low-thermal-resistance phase-change heat-conducting soft sheet and preparation method thereof - Google Patents
Low-thermal-resistance phase-change heat-conducting soft sheet and preparation method thereof Download PDFInfo
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- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
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- C08J2383/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
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- C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
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- C08J2445/00—Characterised by the use of homopolymers or copolymers of compounds having no unsaturated aliphatic radicals in side chain, and having one or more carbon-to-carbon double bonds in a carbocyclic or in a heterocyclic ring system; Derivatives of such polymers
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- C08K3/042—Graphene or derivatives, e.g. graphene oxides
Abstract
The invention relates to the technical field of heat conducting soft sheets, in particular to a phase change heat conducting soft sheet with low thermal resistance and a preparation method thereof, wherein the phase change heat conducting soft sheet with low thermal resistance comprises the following components in percentage by weight: 0.5-20% of polymer matrix, 0.1-10% of phase-change material, 60-98% of heat-conducting filler, 0.01-3% of coupling agent, 0.1-10% of diluent, 0.1-5% of tackifier and 0.1-1.0% of adjuvant, wherein when the phase-change heat-conducting film is in the working temperature range, the solid sheet is gradually changed into viscous state, so that the contact interface is fully wetted, the contact thermal resistance is reduced, the heat transfer efficiency is maximized, the temperature of the electronic element is minimized, and the service life of the electronic equipment is effectively prolonged.
Description
Technical Field
The invention relates to the technical field of heat-conducting flexible sheets, in particular to a phase-change heat-conducting flexible sheet with low thermal resistance and a preparation method thereof.
Background
An extremely fine uneven gap exists between the surface of the microelectronic material and the radiator, the actual contact area of the radiator and the surface of the material is smaller, and the rest is an air gap. Since the thermal conductivity of air is only 0.024W/(m.K), which is a poor thermal conductor, the thermal contact resistance between the electronic component and the heat sink is large, the heat conduction is seriously hindered, and finally the efficiency of the heat sink is low.
To solve the above-mentioned technical problems, a thermal interface material with high thermal conductivity is developed to fill these gaps, remove air therein, establish an effective thermal conduction channel between the electronic component and the heat sink, and make the heat sink function sufficiently with a substantially low contact thermal resistance.
Generally, a thermal interface material is made of heat-conducting silicone grease to be arranged in an air gap, but the heat-conducting silicone grease becomes dry after long-term use, thermal resistance becomes large, heat dissipation performance is reduced, and oil leakage is also accompanied, so that electronic components are polluted, and the service life of the electronic components is influenced.
Disclosure of Invention
In view of the above problems, embodiments of the present invention are proposed to provide a phase change thermal conductive film with low thermal resistance and a method for manufacturing the same, which overcome or at least partially solve the above problems.
In order to solve the above problems, the embodiment of the present invention discloses a phase change thermal conductive film with low thermal resistance, which comprises the following components by weight:
0.5-20% of polymer matrix, 0.1-10% of phase-change material, 60-98% of heat-conducting filler, 0.01-3% of coupling agent, 0.1-10% of diluent, 0.1-5% of tackifier and 0.1-1.0% of adjuvant.
Further, the polymer matrix comprises at least one of silicone rubber, epoxy, acrylic, polyurethane, neoprene, nitrile rubber, ethylene-propylene, polyethylene-butylene, polyethylene-propylene-styrene, polyethylene-butylene-styrene, hydroxyl-terminated polybutadiene, hydroxyl-terminated polyisoprene, polybutadiene, hydrogenated polyolefin, preferably hydrogenated polyolefin with elasticity or liquid silicone rubber made of silicone rubber.
Further, the phase change material comprises at least one of inorganic compounds, low-melting alloys, paraffin wax, Fischer-Tropsch wax, microcrystalline wax, polyethylene wax, polypropylene wax, oxidized polyethylene wax, hydrogenated modified wax and polyethylene-maleic anhydride copolymerized modified wax, and preferably, paraffin wax or hydrogenated modified wax is selected.
Further, the heat conducting filler comprises at least one of aluminum, copper, silver, zinc, nickel, silver-plated aluminum, aluminum-plated carbon fiber, nickel-plated fiber, carbon black, graphite, carbon nanotubes, carbon fiber, graphene, diamond, glass, silica, silicon nitride, aluminum oxide, magnesium oxide, aluminum nitride, boron nitride, zinc oxide and tin oxide, preferably, a granular aluminum material is used as the heat conducting filler, more preferably, at least two aluminum granules with different grain sizes are mixed to be used as the heat conducting filler, and if two aluminum granules are used, the grain size ratio is 1: (0.1-10).
Further, the coupling agent comprises at least one of titanate coupling agent, silane coupling agent, aluminate coupling agent, zirconate coupling agent and aluminum zirconate coupling agent, preferably, silane coupling agent is selected.
Further, the diluent comprises at least one of benzene, toluene, xylene, naphtha, paraffin oil, pentane, hexane, isohexane, heptane, petroleum ether, mineral oil, kerosene, silicone oil, isobutylbenzene, methylnaphthalene, ethyltoluene and tetrahydrofuran, and preferably, the silicone oil or the mineral oil with lower viscosity is selected.
Further, the tackifier comprises at least one of C9 petroleum resin, C5 petroleum resin, terpene resin, rosin resin, epoxy, polyurethane and acrylic acid, and preferably, the terpene resin is selected.
Further, the auxiliary agent comprises at least one of an antioxidant, a flame retardant and a reinforcing agent;
the antioxidant comprises at least one of phenolic antioxidants and amine antioxidants;
the flame retardant comprises at least one of aluminum hydroxide, magnesium hydroxide, halogen flame retardants and nitrogen and phosphorus flame retardants;
the reinforcing agent comprises at least one of active whisker silicon, fumed silica, graphene and carbon fiber.
Further, the phase-change heat-conducting soft sheet comprises the following components in percentage by weight:
3.5% of a polymer matrix, 1.0% of a phase-change material, 92% of a heat-conducting filler, 0.5% of a coupling agent, 1.5% of a diluent, 0.5% of a tackifier and 1.0% of an auxiliary agent, wherein the auxiliary agent comprises a reinforcing agent accounting for 0.5% of the phase-change heat-conducting film by weight.
Also provides a preparation method of the phase change heat conducting film with low thermal resistance, which comprises the following steps:
s1, heating and stirring the polymer matrix, the tackifier and the diluent until the polymer matrix is fully melted to obtain a carrier material;
s2, adding the phase-change material, the reinforcing agent, the heat-conducting filler and the auxiliary agent, heating to 80-120 ℃ in a vacuum environment, and stirring for 0.5-1 hour to obtain a mixed and dispersed phase-change material;
and S3, performing tabletting treatment by a calender to obtain the phase change heat conducting soft sheet.
The embodiment of the invention has the following advantages:
the hydrogenated polymer matrix and the hydrogenated modified wax are used in the invention, so that the thermal stability is better; secondly, the reinforcing material endows the material with better mechanical strength, and the larger sheet-to-diameter ratio and the larger length-to-diameter ratio of the reinforcing material enable the reinforcing material and the heat-conducting filler to form a heat-conducting network chain more easily; the silane coupling agent is selected, so that the viscosity of a polymer matrix is effectively reduced, a bridge bond is formed between the powder and the polymer, the wettability of the powder and the polymer is increased, the melting point of the phase-change material is 40-55 ℃, the temperature is basically consistent with the working temperature of general electronic equipment, when the phase-change heat-conducting film is in the working temperature range, the solid sheet is gradually changed into a viscous state, a contact interface is fully wetted, the contact thermal resistance is reduced, the heat transfer efficiency is maximized, the temperature of an electronic element is reduced to the minimum, and the service life of the electronic equipment is effectively prolonged.
Drawings
FIG. 1 is a flowchart illustrating steps of an embodiment of a method for manufacturing a phase-change thermal conductive film with low thermal resistance according to the present invention.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in further detail below.
The invention provides a phase change heat conducting soft sheet with low thermal resistance, which comprises the following preparation raw materials in percentage by weight:
0.5-20% of polymer matrix, 0.1-10% of phase-change material, 60-98% of heat-conducting filler, 0.01-3% of coupling agent, 0.1-10% of diluent, 0.1-5% of tackifier and 0.1-1.0% of adjuvant.
In the above, the polymer matrix comprises at least one of silicone rubber, epoxy, acrylic, polyurethane, neoprene, nitrile rubber, ethylene-propylene, polyethylene-butylene, polyethylene-propylene-styrene, polyethylene-butylene-styrene, hydroxyl-terminated polybutadiene, hydroxyl-terminated polyisoprene, polybutadiene, and hydrogenated polyolefin;
the phase-change material comprises at least one of inorganic compounds, low-melting alloy, paraffin, Fischer-Tropsch wax, microcrystalline wax, polyethylene wax, polypropylene wax, oxidized polyethylene wax, hydrogenated modified wax and polyethylene-maleic anhydride copolymerized modified wax;
the heat conducting filler comprises at least one of aluminum, copper, silver, zinc, nickel, silver-plated aluminum, aluminum-plated carbon fiber, nickel-plated fiber, carbon black, graphite, carbon nanotubes, carbon fiber, graphene, diamond, glass, silica, silicon nitride, aluminum oxide, magnesium oxide, aluminum nitride, boron nitride, zinc oxide and tin oxide;
the coupling agent comprises at least one of titanate coupling agent, silane coupling agent, aluminate coupling agent, zirconate coupling agent and aluminum zirconate coupling agent;
the diluent comprises at least one of benzene, toluene, xylene, naphtha, paraffin oil, pentane, hexane, isohexane, heptane, petroleum ether, mineral oil, kerosene, silicone oil, isobutyl benzene, methylnaphthalene, ethyltoluene and tetrahydrofuran;
the tackifier comprises at least one of C9 petroleum resin, C5 petroleum resin, terpene resin, rosin resin, epoxy, polyurethane and acrylic acid;
the auxiliary agent comprises at least one of an antioxidant, a flame retardant and a reinforcing agent;
the antioxidant comprises at least one of phenolic antioxidants and amine antioxidants;
the flame retardant comprises at least one of aluminum hydroxide, magnesium hydroxide, halogen flame retardants and nitrogen and phosphorus flame retardants;
the reinforcing agent comprises at least one of active whisker silicon, fumed silica, graphene and carbon fiber.
Referring to fig. 1, the invention also provides a preparation method of the phase-change heat-conducting film with low thermal resistance, which comprises the following steps:
s1, heating and stirring the polymer matrix, the tackifier and the diluent until the polymer matrix is fully melted to obtain a carrier material;
s2, adding the phase-change material, the reinforcing agent, the heat-conducting filler and the auxiliary agent, heating to 80-120 ℃ in a vacuum environment, and stirring for 0.5-1 hour to obtain a mixed and dispersed phase-change material;
and S3, performing tabletting treatment by a calender to obtain the phase change heat conducting soft sheet.
The following embodiments are further described with reference to the raw materials and the preparation method of the phase-change thermal conductive film.
Example 1:
the phase change heat conducting film in the embodiment is prepared from the following raw materials in percentage by weight: 6.5% of liquid silicone rubber, 1.0% of terpene resin, 4% of paraffin with the melting point of 40-55 ℃, 85% of aluminum particles, 2% of silicone oil, 0.5% of silane and 1.0% of auxiliary agent;
wherein, three aluminum particles with different particle sizes are selected and mixed as the heat conducting filler, and the particle sizes are respectively 15 microns, 6 microns and 1 micron;
wherein, the auxiliary agent contains graphene which accounts for 0.5 percent of the weight of the phase-change heat-conducting soft sheet and is used as a reinforcing agent.
The preparation method of the phase change heat conducting film in the embodiment comprises the following steps:
s1, quantitatively selecting a polymer matrix, a tackifier and a diluent, heating and stirring until the polymer matrix is fully melted;
s2, quantitatively selecting the phase-change material, the reinforcing agent, the heat-conducting filler and the auxiliary agent, adding the materials into the molten polymer matrix, heating the mixture to 80-120 ℃ in a vacuum environment, and stirring the mixture for 0.5-1 hour to obtain the mixed and dispersed phase-change material;
and S3, performing tabletting treatment by a calender to obtain the phase change heat conducting soft sheet.
Example 2:
the phase change heat conducting film in the embodiment is prepared from the following raw materials in percentage by weight: 3.5% of thermoplastic polyolefin, 1.0% of terpene resin, 4% of hydrogenated modified wax with the melting point of 40-55 ℃, 88% of aluminum particles, 2% of silicone oil, 0.5% of silane and 1.0% of auxiliary agent;
wherein, three aluminum particles with different particle sizes are selected and mixed as the heat conducting filler, and the particle sizes are respectively 15 microns, 6 microns and 1 micron;
wherein, the auxiliary agent contains graphene which accounts for 0.5 percent of the weight of the phase-change heat-conducting soft sheet and is used as a reinforcing agent.
The preparation method of the phase change heat conducting film described in this embodiment is the same as that of embodiment 1.
Example 3:
the phase change heat conducting film in the embodiment is prepared from the following raw materials in percentage by weight: 3.5% of hydrogenated polyolefin, 1.0% of terpene resin, 2% of hydrogenated modified wax with the melting point of 40-55 degrees, 90% of aluminum particles, 2% of mineral oil, 0.5% of silane and 1.0% of auxiliary agent;
wherein, three aluminum particles with different particle sizes are selected and mixed as the heat conducting filler, and the particle sizes are respectively 15 microns, 6 microns and 1 micron;
wherein, the auxiliary agent contains graphene which accounts for 0.5 percent of the weight of the phase-change heat-conducting soft sheet and is used as a reinforcing agent.
The preparation method of the phase change heat conducting film described in this embodiment is the same as that of embodiment 1.
Example 4:
the phase change heat conducting film in the embodiment is prepared from the following raw materials in percentage by weight: 3.5% of hydrogenated polyolefin, 0.5% of terpene resin, 1% of hydrogenated modified wax with the melting point of 40-55 ℃, 92% of aluminum particles, 1.5% of mineral oil, 0.5% of silane and 1.0% of auxiliary agent;
wherein, three aluminum particles with different particle sizes are selected and mixed as the heat conducting filler, and the particle sizes are respectively 15 microns, 6 microns and 1 micron;
wherein, the auxiliary agent contains graphene which accounts for 0.5 percent of the weight of the phase-change heat-conducting soft sheet and is used as a reinforcing agent.
The preparation method of the phase change heat conducting film described in this embodiment is the same as that of embodiment 1.
Example 5:
the phase change heat conducting film in the embodiment is prepared from the following raw materials in percentage by weight: 2.5% of thermoplastic polyolefin, 0.2% of terpene resin, 0.5% of paraffin with the melting point of 40-55 ℃, 94.5% of aluminum particles, 1.5% of mineral oil, 0.5% of silane and 0.3% of auxiliary agent;
wherein, three aluminum particles with different particle sizes are selected and mixed as the heat conducting filler, and the particle sizes are respectively 15 microns, 6 microns and 1 micron;
wherein, the auxiliary agent contains graphene which accounts for 0.2 percent of the weight of the phase-change heat-conducting soft sheet and is used as a reinforcing agent.
The preparation method of the phase change heat conducting film described in this embodiment is the same as that of embodiment 1.
Example 6:
the phase change heat conducting film in the embodiment is prepared from the following raw materials in percentage by weight: 1.9% of thermoplastic polyolefin, 0.2% of terpene resin, 0.2% of paraffin with the melting point of 40-55 ℃, 96% of aluminum particles, 0.9% of mineral oil, 0.5% of silane and 0.3% of auxiliary agent;
wherein, three aluminum particles with different particle sizes are selected and mixed as the heat conducting filler, and the particle sizes are respectively 15 microns, 6 microns and 1 micron;
wherein, the auxiliary agent contains graphene which accounts for 0.1 percent of the weight of the phase-change heat-conducting soft sheet and is used as a reinforcing agent.
The preparation method of the phase change heat conducting film described in this embodiment is the same as that of embodiment 1.
Six phase-change thermal conductive films with a thickness of 0.25mm and a length and width of 26mm × 26mm were prepared according to the first to sixth embodiments, and the six phase-change thermal conductive films were subjected to thermal resistance tests using a thermal conductivity tester (model LW9389), and the results are recorded in table 1.
Table 1:
as shown in table 1, the filling of the heat conductive filler has a large influence on the thermal resistance, the filling is too little, a large number of heat conductive networks cannot be formed in the polymer matrix, and more heat conductive particles are isolated by the polymer matrix or air, resulting in an increase in the interface thermal resistance; the phase change heat conducting film prepared by the moderate mixture ratio in the embodiment 4 has smaller thermal resistance and better heat dissipation performance.
And (3) respectively assembling specific tools for the six phase-change heat-conducting films, placing the six phase-change heat-conducting films into a thermostat with the temperature of 125 ℃ for baking for 1000 hours, testing the thermal resistance before and after aging, and recording the results in a table 2.
Table 2:
as shown in table 2, the phase change thermal conductive sheets prepared by examples 1 to 6 have good thermal aging resistance and good stability in long-term operation.
While preferred embodiments of the present invention have been described, additional variations and modifications of these embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. Therefore, it is intended that the appended claims be interpreted as including preferred embodiments and all such alterations and modifications as fall within the scope of the embodiments of the invention.
Finally, it should also be noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or terminal that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or terminal. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other like elements in a process, method, article, or terminal that comprises the element.
The phase-change heat-conducting soft sheet with low thermal resistance and the preparation method thereof provided by the invention are described in detail, the principle and the implementation mode of the invention are explained by applying specific examples, and the description of the examples is only used for helping to understand the method and the core idea of the invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, there may be variations in the specific embodiments and the application scope, and in summary, the content of the present specification should not be construed as a limitation to the present invention.
Claims (10)
1. A phase change heat conducting soft sheet with low thermal resistance is characterized by comprising the following components in percentage by weight:
0.5-20% of polymer matrix, 0.1-10% of phase-change material, 60-98% of heat-conducting filler, 0.01-3% of coupling agent, 0.1-10% of diluent, 0.1-5% of tackifier and 0.1-1.0% of adjuvant.
2. The phase change thermally conductive film of claim 1, wherein the polymer matrix comprises at least one of silicone rubber, epoxy, acrylic, polyurethane, neoprene, nitrile rubber, ethylene-propylene, polyethylene-butylene, polyethylene-propylene-styrene, polyethylene-butylene-styrene, hydroxyl terminated polybutadiene, hydroxyl terminated polyisoprene, polybutadiene, hydrogenated polyolefin.
3. The phase-change thermal film according to claim 1, wherein the phase-change material comprises at least one of an inorganic compound, a low-melting alloy, paraffin wax, fischer-tropsch wax, microcrystalline wax, polyethylene wax, polypropylene wax, oxidized polyethylene wax, hydrogenated modified wax, and polyethylene-maleic anhydride copolymerized modified wax.
4. The phase-change thermal film according to claim 1, wherein the thermal conductive filler comprises at least one of aluminum, copper, silver, zinc, nickel, silver-plated aluminum, aluminum-plated carbon fiber, nickel-plated fiber, carbon black, graphite, carbon nanotube, carbon fiber, graphene, diamond, glass, silica, silicon nitride, aluminum oxide, magnesium oxide, aluminum nitride, boron nitride, zinc oxide, and tin oxide.
5. The phase-change thermal film according to claim 1, wherein the coupling agent comprises at least one of a titanate coupling agent, a silane coupling agent, an aluminate coupling agent, a zirconate coupling agent, and an aluminum zirconate coupling agent.
6. The phase-change thermal film according to claim 1, wherein the diluent comprises at least one of benzene, toluene, xylene, naphtha, paraffin oil, pentane, hexane, isohexane, heptane, petroleum ether, mineral oil, kerosene, silicone oil, isobutylbenzene, methylnaphthalene, ethyltoluene, tetrahydrofuran.
7. The phase change thermally conductive film as claimed in claim 1, wherein the tackifier comprises at least one of C9 petroleum resin, C5 petroleum resin, terpene resin, rosin resin, epoxy, polyurethane, and acrylic.
8. The phase change thermal film according to claim 1, wherein the adjuvant comprises at least one of an antioxidant, a flame retardant, and a reinforcing agent;
the antioxidant comprises at least one of phenolic antioxidants and amine antioxidants;
the flame retardant comprises at least one of aluminum hydroxide, magnesium hydroxide, halogen flame retardants and nitrogen and phosphorus flame retardants;
the reinforcing agent comprises at least one of active whisker silicon, fumed silica, graphene and carbon fiber.
9. The phase-change thermal film according to claim 1, comprising in weight percent:
3.5% of polymer matrix, 1.0% of phase-change material, 92% of heat-conducting filler, 0.5% of coupling agent, 1.5% of diluent, 0.5% of tackifier and 1.0% of auxiliary agent.
10. A method for preparing a phase-change thermal conductive film with low thermal resistance according to any one of claims 1 to 9, comprising the steps of:
s1, heating and stirring the polymer matrix, the tackifier and the diluent until the polymer matrix is fully melted to obtain a carrier material;
s2, adding the phase-change material, the reinforcing agent, the heat-conducting filler and the auxiliary agent, heating to 80-120 ℃ in a vacuum environment, and stirring for 0.5-1 hour to obtain a mixed and dispersed phase-change material;
and S3, performing tabletting treatment by a calender to obtain the phase change heat conducting soft sheet.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011061526.2A CN112194898A (en) | 2020-09-30 | 2020-09-30 | Low-thermal-resistance phase-change heat-conducting soft sheet and preparation method thereof |
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| CN113248923A (en) * | 2021-02-10 | 2021-08-13 | 天瀚材料科技(深圳)有限公司 | High-elasticity heat-conducting silica gel sheet |
| CN113698754A (en) * | 2021-07-16 | 2021-11-26 | 中国科学院宁波材料技术与工程研究所 | Heat-conducting gasket and preparation method and application thereof |
| CN114163705A (en) * | 2021-12-31 | 2022-03-11 | 深圳先进电子材料国际创新研究院 | Polyolefin-based flame-retardant heat conduction material and preparation method and application thereof |
| CN114479257A (en) * | 2022-02-23 | 2022-05-13 | 深圳市飞荣达科技股份有限公司 | Non-wax phase-change heat conducting fin and preparation method thereof |
| WO2022163192A1 (en) * | 2021-01-29 | 2022-08-04 | 積水ポリマテック株式会社 | Heat-conductive sheet, method for installing same, and method for manufacturing same |
| CN115181551A (en) * | 2022-07-07 | 2022-10-14 | 深圳市鸿富诚新材料股份有限公司 | Anisotropic heat conduction phase change material and preparation method thereof |
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| CN115181551A (en) * | 2022-07-07 | 2022-10-14 | 深圳市鸿富诚新材料股份有限公司 | Anisotropic heat conduction phase change material and preparation method thereof |
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Application publication date: 20210108 |