Heat-conducting phase-change material and preparation method thereof

Abstract

The invention discloses a heat-conducting phase-change material and a preparation method thereof. The heat-conducting phase-change material is prepared from the following raw materials in parts by weight: 10-30 parts of an inorganic phase-change material, 15-80 parts of a tackifier, 5-20 parts of organopolysiloxane, 2-5 parts of an antioxidant, 0.5-3 parts of a temperature regulator, 0.1-3 parts of a silane coupling agent and 300-800 parts of heat-conducting filler, the preparation method comprises the following steps: S1, stirring 10-30 parts of an inorganic phase change material, 15-80 parts of a tackifier, 5-20 parts of organopolysiloxane, 2-5 parts of an antioxidant and 0.1-3 parts of a silane coupling agent for the first time at normal temperature to obtain a first compound; and S2, stirring the first compound, 0.5-3 parts of a temperature regulator and 300-800 parts of heat-conducting filler for the second time at high temperature and in vacuum to obtain the heat-conducting phase-change material. The heat-conducting phase-change material disclosed by the invention has relatively short performance release time and relatively good heat-conducting property.

Description

Technical Field

[0001] The present invention relates to the technical field of thermal conductive phase change materials, and in particular to a thermal conductive phase change material and a preparation method thereof. Background Art

[0002] Heat dissipation management of electronic devices is the key to ensuring their stable operation and extending their service life. As the power density of electronic products increases and their size continues to decrease, the heat density generated by electronic devices during operation is also increasing, so a more efficient heat dissipation solution is needed to meet this challenge. In parts such as the CPU (central processing unit) and GPU (graphics processing unit) that have extremely high heat dissipation requirements, the traditional interface material used is silicone grease. Due to the problems that silicone grease is easy to dry, easy to sag, has poor reliability, and thermal resistance is difficult to meet high thermal conductivity requirements, thermal conductive phase change materials with higher reliability and lower thermal resistance have begun to attract attention. At present, during the use of thermal conductive phase change, it often takes a long time to release its performance in the early stage to ensure that its performance reaches the best state. The performance release time is generally 1 hour or more. If the performance release time of thermal conductive phase change materials is too long, it will seriously affect the material usage experience and even cause damage to the device.

[0003] Patent CN201811619319.7 discloses a method for preparing a high-reliability thermally conductive phase change material using EVA resin, but this type of thermally conductive phase change material has a slow response rate and requires a long time to completely phase change to achieve optimal performance. In the case of incomplete phase change, the thermal resistance is very high, which may cause the chip to overheat and is difficult to meet existing needs. Patent CN202311070587.9 discloses a method for preparing a phase change thermal pad with a low volatility curing rate. The thermal conductivity of the prepared material is between 1-3.5W / mK. At 120-150°C, the product can be cured in 5-10 minutes, but the thermal conductivity is too low to meet existing needs; the phase change temperature can be quickly changed when it is greater than 120°C, but the temperature is too high to play a role in practical applications. Summary of the invention

[0004] The technical problem to be solved by the present invention is to provide a thermally conductive phase change material and a preparation method thereof.

[0005] The technical solution adopted by the present invention to solve its technical problem is: a thermally conductive phase change material is made of the following raw materials in parts by weight: 10 to 30 parts of inorganic phase change material, 15 to 80 parts of tackifier, 5 to 20 parts of organic polysiloxane, 2 to 5 parts of antioxidant, 0.5 to 3 parts of temperature regulator, 0.1 to 3 parts of silane coupling agent and 300 to 800 parts of thermally conductive filler.

[0006] In some embodiments, the inorganic phase change material includes at least one of paraffin wax, sodium sulfate, sodium acetate, and sodium carbonate hydrate salts.

[0007] In some embodiments, the organopolysiloxane includes vinyl silicone oil and hydrogen-terminated polydimethylsiloxane, wherein the structure of the vinyl silicone oil is Wherein, n=20-50; the structure of hydrogen-terminated polydimethylsiloxane is Wherein, m=20~50.

[0008] In some embodiments, the tackifier includes at least one of rosin, rosin derivatives, terpene resins, coumarone-indene resins, dicyclopentadiene resins, acrylic acid-modified petroleum resins, and alkylphenol-formaldehyde resins; acrylic acid-modified petroleum resins include acrylic acid-modified C 5 Petroleum resin and / or acrylic acid modified C 9 Petroleum resin.

[0009] In some embodiments, the antioxidant includes at least one of tris(2,4-di-tert-butylphenyl)phosphite, pentaerythritol tetrakis[methyl-β-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate], 2,6-di-tert-butyl-4-methylphenol, 1,1,3-tris(2-methyl-4-hydroxy-5-tert-butylphenyl)butane, and 4,4'-methylenebis(2,6-di-tert-butylphenol).

[0010] In some embodiments, the temperature regulator includes at least one of potassium chloride, ammonium chloride, and sodium chloride.

[0011] In some embodiments, the silane coupling agent includes at least one of 3-aminopropylethoxysiloxane, γ-glycidyloxypropyltrimethoxysilane, γ-(methacryloxy)propyltrimethoxysilane, dodecyltrimethoxysilane, vinyltriethoxysilane, titanate coupling agent and aluminate coupling agent; and / or,

[0012] The thermally conductive filler includes at least one of aluminum oxide, magnesium oxide, zinc oxide, aluminum nitride, boron nitride, silicon nitride, silicon carbide, carbon fiber and graphene.

[0013] The present invention also provides a method for preparing any of the above thermally conductive phase change materials, comprising the following steps, where the raw materials are measured in parts by weight:

[0014] S1, stirring 10 to 30 parts of an inorganic phase change material, 15 to 80 parts of a tackifier, 5 to 20 parts of an organopolysiloxane, 2 to 5 parts of an antioxidant, and 0.1 to 3 parts of a silane coupling agent for the first time at room temperature to obtain a first composite;

[0015] S2. Stirring the first composite, 0.5 to 3 parts of a temperature regulator and 300 to 800 parts of a thermally conductive filler for a second time under high temperature and vacuum to obtain a thermally conductive phase change material.

[0016] In some embodiments, in step S1, the rotation speed of the first stirring is 1000-5000 rpm, and the stirring time is 0.5-1.5 h.

[0017] In some embodiments, in step S2, the stirring temperature of the second stirring is 80-125° C., the vacuum degree is ≤0.1 MPa, the rotation speed is 1000-5000 rpm, and the stirring time is 1.5-2.5 h.

[0018] Beneficial effects of the present invention:

[0019] In the thermally conductive phase change material of the present invention, the inorganic phase change material gives the thermally conductive phase change material phase change performance; the organic polysiloxane can fix the thermally conductive filler inside to ensure that the thermally conductive filler will not precipitate when the thermally conductive phase change material is heated; the tackifier can improve the gap filling ability and rapid response ability of the thermally conductive phase change material; the temperature regulator reduces the phase change temperature of the thermally conductive phase change material, so that the material has the gap filling ability at a lower temperature and improves the response rate; the thermally conductive filler improves the thermal conductivity of the thermally conductive phase change material, and at the same time, the thermally conductive filler is treated with a silane coupling agent to maintain the high phase change latent heat of the thermally conductive phase change material. The performance release time of the thermally conductive phase change material of the present invention is shortened to within five minutes, and a rapid response can be achieved, thereby greatly improving the use efficiency and experience of the thermally conductive phase change material, and avoiding the problem of overheating of electronic devices when the material is not completely phase-changed.

[0020] The preparation method of the thermally conductive phase change material of the present invention is simple and feasible to operate, and is suitable for large-scale production. The prepared thermally conductive phase change material has a shorter performance release time and better thermal conductivity. DETAILED DESCRIPTION

[0021] In order to have a clearer understanding of the technical features, purposes and effects of the present invention, the present invention will be further described in detail below in conjunction with embodiments. The embodiments are only used to explain the present invention and do not constitute a limitation on the protection scope of the present invention.

[0022] The present invention provides a thermally conductive phase change material, which is made of the following raw materials in parts by weight: 10 to 30 parts of inorganic phase change material, 15 to 80 parts of tackifier, 5 to 20 parts of organic polysiloxane, 2 to 5 parts of antioxidant, 0.5 to 3 parts of temperature regulator, 0.1 to 3 parts of silane coupling agent and 300 to 800 parts of thermally conductive filler. For example, the inorganic phase change material can be selected at 10 parts, 15 parts, 20 parts, 25 parts, 30 parts, etc., the thickener can be selected at 15 parts, 30 parts, 50 parts, 65 parts, 80 parts, etc., the organopolysiloxane can be selected at 5 parts, 10 parts, 15 parts, 18 parts, 20 parts, etc., the antioxidant can be selected at 2 parts, 3 parts, 4 parts, 5 parts, etc., the temperature regulator can be selected at 0.5 parts, 1 parts, 1.5 parts, 2 parts, 3 parts, etc., the silane coupling agent can be selected at 0.1 parts, 0.5 parts, 1 parts, 2 parts, 3 parts, etc., and the thermal conductive filler can be selected at 300 parts, 400 parts, 500 parts, 600 parts, 800 parts, etc.

[0023] The inorganic phase change material includes at least one of paraffin, sodium sulfate, sodium acetate and sodium carbonate hydrate salts. The inorganic phase change material gives the thermal conductive phase change material phase change properties.

[0024] Organic polysiloxanes include vinyl silicone oil and hydrogen-terminated polydimethylsiloxane. The structure of vinyl silicone oil is Wherein, n=20-50; the structure of hydrogen-terminated polydimethylsiloxane is In the formula, m=20 to 50. The cross-linked network is formed by the reaction of vinyl silicone oil and hydrogen-terminated polydimethylsiloxane, and the thermal conductive filler can be fixed inside to ensure that the thermal conductive filler will not precipitate when the organic silicone thermal conductive phase change material is heated.

[0025] The tackifier includes at least one of rosin, rosin derivatives, terpene resin, coumarone-indene resin, dicyclopentadiene resin, acrylic acid-modified petroleum resin and alkylphenol-formaldehyde resin, wherein the acrylic acid-modified petroleum resin preferably includes acrylic acid-modified C 5 Petroleum resin and / or acrylic acid modified C 9 Petroleum resin. The introduction of tackifier can increase the bonding force between the thermal conductive phase change material and the surface of the attached device, thereby improving the gap filling ability and rapid response ability of the thermal conductive phase change material.

[0026] The antioxidant includes at least one of tris(2,4-di-tert-butylphenyl)phosphite, pentaerythritol tetrakis[methyl-β-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate], 2,6-di-tert-butyl-4-methylphenol, 1,1,3-tris(2-methyl-4-hydroxy-5-tert-butylphenyl)butane and 4,4'-methylenebis(2,6-di-tert-butylphenol).

[0027] The temperature regulator includes at least one of potassium chloride, ammonium chloride and sodium chloride. The introduction of the temperature regulator allows the hydrolyzed cations to be distributed between water molecules and inorganic phase change material molecules, increasing the binding resistance between inorganic phase change material molecules and water molecules, thereby reducing the phase change temperature of the thermal conductive phase change material, so that the material has the ability to fill gaps at a lower temperature, thereby improving the response rate.

[0028] The silane coupling agent includes at least one of 3-aminopropylethoxysiloxane, γ-glycidyloxypropyltrimethoxysilane, γ-(methacryloxy)propyltrimethoxysilane, dodecyltrimethoxysilane, vinyltriethoxysilane, titanate coupling agent and aluminate coupling agent.

[0029] The thermal conductive filler includes at least one of aluminum oxide, magnesium oxide, zinc oxide, aluminum nitride, boron nitride, silicon nitride, silicon carbide, carbon fiber and graphene. The introduction of the thermal conductive filler can improve the thermal conductivity of the thermal conductive phase change material. At the same time, the thermal conductive filler can increase the compatibility with the matrix after being treated with a silane coupling agent, improve the cycle stability of the thermal conductive phase change material, and provide heterogeneous nucleation sites, reduce the crystallization energy barrier and promote crystallization, thereby maintaining the high phase change latent heat of the thermal conductive phase change material.

[0030] The above raw materials include inorganic phase change material, tackifier, organopolysiloxane, antioxidant, temperature regulator, silane coupling agent and thermal conductive filler, all of which can be commercially available or obtained by existing preparation methods, which will not be described in detail here.

[0031] The present invention also provides a method for preparing any of the above thermally conductive phase change materials, which comprises the following steps, wherein the raw materials are calculated by weight:

[0032] S1. Stir 10-30 parts of inorganic phase change material, 15-80 parts of thickener, 5-20 parts of organopolysiloxane, 2-5 parts of antioxidant and 0.1-3 parts of silane coupling agent for the first time at room temperature to obtain a first composite. The components of inorganic phase change material, thickener, organopolysiloxane, antioxidant and silane coupling agent are the same as the raw material components of the aforementioned thermal conductive phase change material, which will not be repeated here. Normal temperature refers to 20-25°C, and the first stirring temperature can be within 20-25°C without limitation.

[0033] In some embodiments, the first stirring speed is 1000-5000 rpm, and the stirring time is 0.5-1.5 h. For example, the speed can be 1000 rpm, 2000 rpm, 3000 rpm, 4000 rpm, 5000 rpm, etc., and the stirring time can be 0.5 h, 0.8 h, 1.0 h, 1.2 h, 1.5 h, etc. The stirring can be performed in a stirrer, such as a planetary stirrer.

[0034] S2, stirring the first composite, 0.5-3 parts of the temperature regulator and 300-800 parts of the thermal conductive filler for a second time under high temperature and vacuum to obtain a thermal conductive phase change material. The components of the temperature regulator and the thermal conductive filler are the same as the raw material components of the thermal conductive phase change material, which will not be repeated here.

[0035] In some embodiments, the stirring temperature (high temperature) of the second stirring is 80-125°C, the vacuum degree is ≤0.1MPa, the rotation speed is 1000-5000rpm, and the stirring time is 1.5-2.5h. For example, the stirring temperature can be 80°C, 90°C, 100°C, 110°C, 125°C, etc.; the vacuum degree refers to the reading of the vacuum gauge, and the vacuum degree is ≤0.1MPa, which is not limited here; the rotation speed can be 1000rpm, 2000rpm, 3000rpm, 4000rpm, 5000rpm, etc., and the stirring time can be 1.5h, 1.8h, 2h, 2.3h, 2.5h, etc.

[0036] Thermally conductive phase change materials need to release their performance during use. This process includes stabilization treatment and cyclic activation. Stabilization treatment is to place the thermally conductive phase change material in a stable temperature environment, usually within the range of its designed operating temperature, to ensure that the thermally conductive phase change material reaches a stable state and eliminates any possible initial instability. Cyclic activation is to perform multiple phase change cycles within a certain temperature range to ensure the performance stability and reliability of the thermally conductive phase change material. This helps to eliminate any potential initial non-uniformity and ensure that the thermally conductive phase change material can work reliably in practical applications. The performance release time of existing thermally conductive phase change materials is relatively long, generally 1 hour or more, but the performance release time of the thermally conductive phase change material of the present invention is within five minutes, which can achieve a rapid response, greatly improving the efficiency and experience of the material, and avoiding the problem of overheating of electronic devices when the material is not completely phase changed.

[0037] The following is described by specific examples:

[0038] Example 1

[0039] A thermally conductive phase change material is made of the following raw materials in parts by weight: 30 parts of inorganic phase change material (paraffin), 15 parts of tackifier (dicyclopentadiene resin), 20 parts of organic polysiloxane (10 parts of vinyl silicone oil, 10 parts of hydrogen-terminated polydimethylsiloxane), 2 parts of antioxidant (2,6-di-tert-butyl-4-methylphenol), 0.5 parts of temperature regulator (potassium chloride), 0.1 parts of silane coupling agent (dodecyltrimethoxysilane) and 700 parts of thermally conductive filler (alumina) with a particle size of 10 μm. Among them, the structure of vinyl silicone oil is The structure of hydrogen-terminated polydimethylsiloxane is

[0040]

[0041] The preparation method of the thermal conductive phase change material of this embodiment comprises the following steps, where the raw materials are calculated by weight:

[0042] S1. Add 30 parts of inorganic phase change material (paraffin), 15 parts of tackifier (dicyclopentadiene resin), 20 parts of organopolysiloxane (10 parts of vinyl silicone oil, 10 parts of hydrogen-terminated polydimethylsiloxane), 2 parts of antioxidant (2,6-di-tert-butyl-4-methylphenol) and 0.1 parts of silane coupling agent (dodecyltrimethoxysilane) into a planetary mixer, and perform the first stirring at room temperature to obtain a first composite. The first stirring speed is 2000 rpm and the stirring time is 0.5 h.

[0043] S2, the first composite, 0.5 parts of the temperature regulator (potassium chloride) and 700 parts of the thermal conductive filler (aluminum oxide) with a particle size of 10 μm are stirred for a second time under high temperature and vacuum to obtain a thermal conductive phase change material. The stirring temperature of the second stirring is 100° C., the vacuum degree is -0.1 MPa, the rotation speed is 1500 rpm, and the stirring time is 2 hours.

[0044] Example 2

[0045] A thermally conductive phase change material is made of the following raw materials in parts by weight: 30 parts of inorganic phase change material (paraffin), 15 parts of tackifier (rosin), 20 parts of organic polysiloxane (10 parts of vinyl silicone oil, 10 parts of hydrogen-terminated polydimethylsiloxane), 2 parts of antioxidant (2,6-di-tert-butyl-4-methylphenol), 0.5 parts of temperature regulator (ammonium chloride), 0.1 parts of silane coupling agent (dodecyltrimethoxysilane) and 700 parts of thermally conductive filler (alumina) with a particle size of 10 μm. Among them, the structure of vinyl silicone oil is The structure of hydrogen-terminated polydimethylsiloxane is

[0047] The preparation method of the thermal conductive phase change material of this embodiment comprises the following steps, where the raw materials are calculated by weight:

[0048] S1. Add 30 parts of inorganic phase change material (paraffin), 15 parts of tackifier (rosin), 20 parts of organopolysiloxane (10 parts of vinyl silicone oil, 10 parts of hydrogen-terminated polydimethylsiloxane), 2 parts of antioxidant (2,6-di-tert-butyl-4-methylphenol) and 0.1 parts of silane coupling agent (dodecyltrimethoxysilane) into a planetary mixer, and perform the first stirring at room temperature to obtain a first composite. The first stirring speed is 2000 rpm and the stirring time is 0.5 h.

[0049] S2, the first composite, 0.5 parts of the temperature regulator (ammonium chloride) and 700 parts of the thermal conductive filler (aluminum oxide) with a particle size of 10 μm are stirred for a second time under high temperature and vacuum to obtain a thermal conductive phase change material. The stirring temperature of the second stirring is 100° C., the vacuum degree is -0.1 MPa, the rotation speed is 1500 rpm, and the stirring time is 2 hours.

[0050] Example 3

[0051] A thermally conductive phase change material is made of the following raw materials in parts by weight: 20 parts of inorganic phase change material (paraffin), 10 parts of tackifier (dicyclopentadiene resin), 20 parts of organic polysiloxane (10 parts of vinyl silicone oil, 10 parts of hydrogen-terminated polydimethylsiloxane), 2 parts of antioxidant (2,6-di-tert-butyl-4-methylphenol), 0.5 parts of temperature regulator (potassium chloride), 0.1 parts of silane coupling agent (dodecyltrimethoxysilane) and 700 parts of thermally conductive filler (aluminum oxide) with a particle size of 10 μm. Among them, the structure of vinyl silicone oil is The structure of hydrogen-terminated polydimethylsiloxane is

[0053] The preparation method of the thermal conductive phase change material of this embodiment comprises the following steps, where the raw materials are calculated by weight:

[0054] S1. Add 20 parts of inorganic phase change material (paraffin), 10 parts of tackifier (dicyclopentadiene resin), 20 parts of organopolysiloxane (10 parts of vinyl silicone oil, 10 parts of hydrogen-terminated polydimethylsiloxane), 2 parts of antioxidant (2,6-di-tert-butyl-4-methylphenol) and 0.1 parts of silane coupling agent (dodecyltrimethoxysilane) into a planetary mixer, and perform the first stirring at room temperature to obtain a first composite. The first stirring speed is 2000 rpm and the stirring time is 0.5 h.

[0055] S2, the first composite, 0.5 parts of the temperature regulator (potassium chloride) and 700 parts of the thermal conductive filler (aluminum oxide) with a particle size of 10 μm are stirred for a second time under high temperature and vacuum to obtain a thermal conductive phase change material. The stirring temperature of the second stirring is 100° C., the vacuum degree is -0.1 MPa, the rotation speed is 1500 rpm, and the stirring time is 2 hours.

[0056] Example 4

[0057] A thermally conductive phase change material is made of the following raw materials in parts by weight: 30 parts of inorganic phase change material (paraffin), 15 parts of tackifier (rosin), 20 parts of organic polysiloxane (10 parts of vinyl silicone oil, 10 parts of hydrogen-terminated polydimethylsiloxane), 2 parts of antioxidant (2,6-di-tert-butyl-4-methylphenol), 2 parts of temperature regulator (potassium chloride), 0.1 parts of silane coupling agent (dodecyltrimethoxysilane) and 700 parts of thermally conductive filler (aluminum oxide) with a particle size of 10 μm. Among them, the structure of vinyl silicone oil is The structure of hydrogen-terminated polydimethylsiloxane is

[0059] The preparation method of the thermal conductive phase change material of this embodiment comprises the following steps, where the raw materials are calculated by weight:

[0060] S1. Add 30 parts of inorganic phase change material (paraffin), 15 parts of tackifier (rosin), 20 parts of organopolysiloxane (10 parts of vinyl silicone oil, 10 parts of hydrogen-terminated polydimethylsiloxane), 2 parts of antioxidant (2,6-di-tert-butyl-4-methylphenol) and 0.1 parts of silane coupling agent (dodecyltrimethoxysilane) into a planetary mixer, and perform the first stirring at room temperature to obtain a first composite. The first stirring speed is 2000 rpm and the stirring time is 0.5 h.

[0061] S2, the first composite, 2 parts of the temperature regulator (potassium chloride) and 700 parts of the thermal conductive filler (aluminum oxide) with a particle size of 10 μm are stirred for a second time under high temperature and vacuum to obtain a thermal conductive phase change material. The stirring temperature of the second stirring is 100° C., the vacuum degree is -0.1 MPa, the rotation speed is 1500 rpm, and the stirring time is 2 hours.

[0062] Example 5

[0063] A thermally conductive phase change material is made of the following raw materials in parts by weight: 30 parts of inorganic phase change material (15 parts of paraffin wax, 15 parts of sodium sulfate), 80 parts of tackifier (40 parts of terpene resin, 40 parts of alkylphenol resin), 20 parts of organic polysiloxane (10 parts of vinyl silicone oil, 10 parts of hydrogen-terminated polydimethylsiloxane), 5 parts of antioxidant (2 parts of tris (2,4-di-tert-butylphenyl) phosphite, 3 parts of 2,6-di-tert-butyl-4-methylphenol), 3 parts of temperature regulator (1 part of potassium chloride, 2 parts of sodium chloride), 3 parts of silane coupling agent (2 parts of 3-aminopropylethoxysiloxane, 1 part of titanate coupling agent) and 800 parts of thermally conductive filler with a particle size of 15 μm (400 parts of magnesium oxide, 400 parts of boron nitride). Among them, the structure of vinyl silicone oil is The structure of hydrogen-terminated polydimethylsiloxane is

[0065] The preparation method of the thermal conductive phase change material of this embodiment comprises the following steps, where the raw materials are calculated by weight:

[0066] S1. Add 30 parts of inorganic phase change material (15 parts of paraffin wax, 15 parts of sodium sulfate), 80 parts of tackifier (40 parts of terpene resin, 40 parts of alkylphenol resin), 20 parts of organopolysiloxane (10 parts of vinyl silicone oil, 10 parts of hydrogen-terminated polydimethylsiloxane), 5 parts of antioxidant (2 parts of tris(2,4-di-tert-butylphenyl)phosphite, 3 parts of 2,6-di-tert-butyl-4-methylphenol) and 3 parts of silane coupling agent (2 parts of 3-aminopropylethoxysiloxane, 1 part of titanate coupling agent) into a planetary mixer, and perform the first stirring at room temperature to obtain a first composite. The speed of the first stirring is 5000 rpm, and the stirring time is 0.5 h.

[0067] S2, the first composite, 3 parts of the temperature regulator (1 part of potassium chloride, 2 parts of sodium chloride) and 800 parts of the thermal conductive filler (400 parts of magnesium oxide, 400 parts of boron nitride) with a particle size of 15 μm are stirred for the second time under high temperature and vacuum to obtain a thermal conductive phase change material. The stirring temperature of the second stirring is 125° C., the vacuum degree is -0.1 MPa, the rotation speed is 5000 rpm, and the stirring time is 1.5 hours.

[0068] Example 6

[0069] A thermally conductive phase change material, which is made of the following raw materials in parts by weight: 10 parts of an inorganic phase change material (sodium acetate), a tackifier (acrylic acid modified C 5 Petroleum resin) 15 parts, organic polysiloxane (2 parts vinyl silicone oil, 3 parts hydrogen-terminated polydimethylsiloxane) 5 parts, antioxidant (tetrakis [methyl-β-(3,5-di-tert-butyl-4-hydroxyphenyl) propionate] pentaerythritol ester) 2 parts, temperature regulator (sodium chloride) 0.5 parts, silane coupling agent (γ-glycidyl ether oxypropyl trimethoxy silane) 0.1 parts and thermal conductive filler (silicon carbide) with a particle size of 8μm 300 parts. Among them, the structure of vinyl silicone oil is The structure of hydrogen-terminated polydimethylsiloxane is

[0071] The preparation method of the thermal conductive phase change material of this embodiment comprises the following steps, where the raw materials are calculated by weight:

[0072] S1, 10 parts of inorganic phase change material (sodium acetate), tackifier (acrylic acid modified C 515 parts of petroleum resin), 5 parts of organopolysiloxane (2 parts of vinyl silicone oil, 3 parts of hydrogen-terminated polydimethylsiloxane), 2 parts of antioxidant (tetrakis[methyl-β-(3,5-di-tert-butyl-4-hydroxyphenyl) propionate] pentaerythritol ester) and 0.1 parts of silane coupling agent (γ-glycidyloxypropyltrimethoxysilane) were added to a planetary stirrer and stirred for the first time at room temperature to obtain a first composite. The first stirring speed was 1000 rpm and the stirring time was 1.5 hours.

[0073] S2, the first composite, 0.5 parts of the temperature regulator (sodium chloride) and 300 parts of the thermal conductive filler (silicon carbide) with a particle size of 8 μm are stirred for a second time under high temperature and vacuum to obtain a thermal conductive phase change material. The stirring temperature of the second stirring is 80° C., the vacuum degree is -0.1 MPa, the rotation speed is 1000 rpm, and the stirring time is 2.5 hours.

[0074] Comparative Example 1

[0075] The difference between the thermal conductive phase change material and the preparation method thereof of this comparative example and that of Example 1 is that no tackifier is added to this comparative example, and the rest is the same as that of Example 1, which will not be described again.

[0076] Comparative Example 2

[0077] The difference between the thermal conductive phase change material and the preparation method thereof in this comparative example and that in Example 1 is that no temperature regulator is added in this comparative example, and the rest is the same as in Example 1, which will not be described again.

[0078] Comparative Example 3

[0079] The difference between the thermal conductive phase change material and the preparation method thereof of this comparative example and Example 1 is that no viscosity enhancer and temperature regulator are added to this comparative example, and the rest are the same as Example 1, which will not be described again.

[0080] Performance Test:

[0081] The thermal conductivity, thermal resistance, response time on the CPU, and response time on the GPU of the thermally conductive phase change materials prepared in Examples 1 to 4 and Comparative Examples 1 to 3 were tested. The test equipment for thermal conductivity and thermal resistance is a Ruiling thermal resistance meter, and the test conditions are a pressure of 40 psi and a temperature of 80°C. The response time is measured by a baking machine. When using a thermally conductive phase change material, the time required for the baking machine temperature to stabilize is the response time. The CPU chip is an Intel 14th generation chip, and the GPU chip is an NVIDIA 4090. The test results are shown in Table 1.

[0082] Table 1 Performance test results of Examples 1 to 4 and Comparative Examples 1 to 3

[0083]

[0084] From the data in Table 1, it can be seen that the thermally conductive phase change materials of Examples 1 to 4 of the present invention have higher thermal conductivity, lower thermal resistance and shorter response time (performance release time), while the thermally conductive phase change materials of Comparative Examples 1 to 3 all have longer response times, among which Comparative Example 3 without adding a thickener and a temperature regulator has the longest response time. It can be seen that the addition of a thickener and a temperature regulator can effectively improve the response rate of the thermally conductive phase change material, shortening the response time of up to one hour to within five minutes, and the effect of adding both the thickener and the temperature regulator at the same time is better than the effect of adding them separately.

[0085] It should be noted that, in the absence of conflict, the embodiments of the present invention and the features in the embodiments may be combined with each other.

[0086] It can be understood that the above embodiments only express the preferred implementation modes of the present invention, and the description thereof is relatively specific and detailed, but it cannot be understood as limiting the patent scope of the present invention. It should be pointed out that, for ordinary technicians in this field, without departing from the concept of the present invention, the above technical features can be freely combined, and several deformations and improvements can be made, which all belong to the protection scope of the present invention. Therefore, all equivalent changes and modifications made to the scope of the claims of the present invention should belong to the scope covered by the claims of the present invention.

Claims

1. A thermally conductive phase change material, characterized in that: The invention is prepared from the following raw materials in parts by weight: 10 to 30 parts of inorganic phase change material, 15 to 80 parts of tackifier, 5 to 20 parts of organic polysiloxane, 2 to 5 parts of antioxidant, 0.5 to 3 parts of temperature regulator, 0.1 to 3 parts of silane coupling agent and 300 to 800 parts of thermal conductive filler.

2. The thermally conductive phase change material according to claim 1, characterized in that: The inorganic phase change material includes at least one of paraffin, sodium sulfate, sodium acetate and sodium carbonate hydrate salt.

3. The thermally conductive phase change material according to claim 1, characterized in that: The organopolysiloxane comprises vinyl silicone oil and hydrogen-terminated polydimethylsiloxane. The structure of the vinyl silicone oil is: Wherein, n=20-50; the structure of hydrogen-terminated polydimethylsiloxane is Wherein, m=20~50.

4. The thermally conductive phase change material according to claim 1, characterized in that: The tackifier includes at least one of rosin, rosin derivatives, terpene resin, coumarone-indene resin, dicyclopentadiene resin, acrylic acid-modified petroleum resin and alkylphenol-formaldehyde resin; the acrylic acid-modified petroleum resin includes acrylic acid-modified C5 petroleum resin and / or acrylic acid-modified C9 petroleum resin.

5. The thermally conductive phase change material according to claim 1, characterized in that: The antioxidant includes at least one of tris(2,4-di-tert-butylphenyl)phosphite, pentaerythritol tetrakis[methyl-β-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate], 2,6-di-tert-butyl-4-methylphenol, 1,1,3-tris(2-methyl-4-hydroxy-5-tert-butylphenyl)butane and 4,4'-methylenebis(2,6-di-tert-butylphenol).

6. The thermally conductive phase change material according to claim 1, characterized in that: The temperature regulator includes at least one of potassium chloride, ammonium chloride and sodium chloride.

7. The thermally conductive phase change material according to claim 1, characterized in that: The silane coupling agent includes at least one of 3-aminopropylethoxysiloxane, γ-glycidyloxypropyltrimethoxysilane, γ-(methacryloxy)propyltrimethoxysilane, dodecyltrimethoxysilane, vinyltriethoxysilane, titanate coupling agent and aluminate coupling agent; and / or, The thermally conductive filler includes at least one of aluminum oxide, magnesium oxide, zinc oxide, aluminum nitride, boron nitride, silicon nitride, silicon carbide, carbon fiber and graphene.

8. A method for preparing the thermally conductive phase change material according to any one of claims 1 to 7, characterized in that: The method comprises the following steps, wherein the raw materials are measured by weight: S1, stirring 10 to 30 parts of an inorganic phase change material, 15 to 80 parts of a tackifier, 5 to 20 parts of an organopolysiloxane, 2 to 5 parts of an antioxidant, and 0.1 to 3 parts of a silane coupling agent for the first time at room temperature to obtain a first composite; S2. Stirring the first composite, 0.5 to 3 parts of a temperature regulator and 300 to 800 parts of a thermally conductive filler for a second time under high temperature and vacuum to obtain the thermally conductive phase change material.

9. The method for preparing a thermally conductive phase change material according to claim 8, characterized in that: In the step S1, the rotation speed of the first stirring is 1000-5000 rpm, and the stirring time is 0.5-1.5 h.

10. The method for preparing a thermally conductive phase change material according to claim 8, characterized in that: In the step S2, the stirring temperature of the second stirring is 80-125°C, the vacuum degree is ≤0.1MPa, the rotation speed is 1000-5000rpm, and the stirring time is 1.5-2.5h.

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