CN113388769A - Slurry alloy heat conduction material - Google Patents
Slurry alloy heat conduction material Download PDFInfo
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- CN113388769A CN113388769A CN202110652466.XA CN202110652466A CN113388769A CN 113388769 A CN113388769 A CN 113388769A CN 202110652466 A CN202110652466 A CN 202110652466A CN 113388769 A CN113388769 A CN 113388769A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C28/00—Alloys based on a metal not provided for in groups C22C5/00 - C22C27/00
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/08—Materials not undergoing a change of physical state when used
- C09K5/10—Liquid materials
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/08—Materials not undergoing a change of physical state when used
- C09K5/14—Solid materials, e.g. powdery or granular
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C13/00—Alloys based on tin
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C30/00—Alloys containing less than 50% by weight of each constituent
Abstract
The invention provides a slurry alloy heat conduction material, which consists of liquid alloy and alloy particles; the liquid alloy comprises, by mass, 10-15 wt% of tin, 60-70 wt% of gallium and 20-30 wt% of indium; the alloy particles comprise 33.3-46.4 wt% of tin, 13.0-25.9 wt% of gallium and 34.8-47.8 wt% of indium in percentage by mass; the heat conduction material effectively avoids the water drop phenomenon generated during coating by matching the liquid alloy with the same components but different component contents with the alloy particles, greatly improves the heat conduction effect, reduces the production cost and has better industrial application prospect.
Description
Technical Field
The invention belongs to the technical field of heat conduction materials, and particularly relates to a slurry alloy heat conduction material.
Background
The heat conducting material is a heat conducting medium specially made for heat management. With the improvement of the performance of electronic products, the wide application of high-power electric and electronic products puts higher requirements on the heat management under high-integration-level assembly.
Generally, in the operation of the electronic device, the heat generated from the main body portion is balanced thermally by heat conduction and heat dissipation. The heat conducting material is arranged between the heat source and the heat radiator to form a good heat conducting path. In many cases, the thermally conductive portion must be thermally conductive and electrically insulating, while at the same time having certain requirements for specific gravity, coefficient of thermal expansion, chemical stability, physical form and appearance.
At present, the existing heat conduction materials are mainly prepared by mixing liquid organic materials and inorganic materials to prepare colloidal state or slurry state materials, wherein the organic materials mainly comprise organic silicon resin, epoxy resin, acrylic resin and the like, and the inorganic materials mainly comprise metal oxides, nitride and other ceramic materials or metal silver and the like. Among them, nitrides have high thermal conductivity, but have disadvantages of high price, unstable properties, etc., and increase of viscosity of the system during a large amount of filling, thereby limiting the application field of the product. In the use process of the metal oxide, a layer of resin material with very low thermal conductivity needs to be coated on the periphery of the metal oxide, the fluidity and the shaking property of the metal oxide are adjusted, and the resin material can reduce the thermal conductivity of the final heat conduction material. The liquid metal is an amorphous metal, and generally includes mercury, low melting point metals such as indium and gallium, and alloys thereof. The liquid metal has high thermal conductivity, and besides the function of phase change heat dissipation, the liquid metal can rapidly conduct heat in the heat conducting channel due to the high thermal conductivity of the metal or the alloy when in the liquid state, which is an advantage that other heat conducting materials cannot compare with. However, the surface tension, high cohesion and affinity of the conventional pure liquid metal sometimes cause a lotus effect when the pure liquid metal is coated on a heating/heat dissipation material, so that the surface is wet, the pure liquid metal exists on the surface of a workpiece in a droplet shape, and is not easy to be uniformly dispersed on the workpiece, and the use trouble is caused.
CN108997980A discloses a phase change heat conduction material for an optical fiber laser, a preparation method and an application method thereof, wherein the phase change heat conduction material is prepared from the following components in percentage by mass: 55-58 wt% of indium, 17-20 wt% of tin, 20-25 wt% of bismuth, 1-2 wt% of aluminum, 0.5-5 wt% of gallium and 1-2 wt% of paraffin; the heat conduction material uses metal bismuth which is not dissolved with gallium, and the phenomenon of phase separation is easy to generate in the use process, so that the heat conduction performance is influenced.
CN112457821A discloses a diamond and liquid metal containing heat conducting gel, its preparation and application, the heat conducting gel is composed of silicone oil matrix, platinum catalyst and composite heat conducting filler; the weight ratio of the composite heat-conducting filler to the silicone oil matrix is (40-90): 10; the composite heat-conducting filler consists of diamond, liquid metal and conventional heat-conducting filler, and the diamond, the liquid metal and the conventional heat-conducting filler are uniformly dispersed in a mixture of a silicone oil matrix and a platinum catalyst; the mass percentage of the diamond in the composite heat-conducting filler is 10-40%; the liquid metal accounts for 5-15% of the composite heat-conducting filler by mass percent; the platinum catalyst accounts for 0.15 to 1.5 percent of the mass of the silicone oil matrix; the heat-conducting gel has complex components, uses platinum and diamond components with higher cost, and has poor economy.
In summary, it is an urgent need to provide a heat conductive material with high thermal conductivity, which can avoid the water drop phenomenon and reduce the production cost.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a slurry alloy heat conduction material, which effectively avoids the water drop phenomenon generated during coating by matching liquid alloy and alloy particles, greatly improves the heat conduction effect, reduces the production cost and has better industrial application prospect.
In order to achieve the purpose, the invention adopts the following technical scheme:
in one aspect, the invention provides a slurry alloy heat conducting material, which consists of liquid alloy and alloy particles;
the liquid alloy comprises 10-15 wt% of tin, such as 10 wt%, 11 wt%, 12 wt%, 13 wt%, 14 wt% or 15 wt% in percentage by mass; gallium 60-70 wt%, such as 60 wt%, 62 wt%, 64 wt%, 66 wt%, 68 wt%, or 70 wt%, and the like; 20 to 30 wt% of indium, for example, 20 wt%, 22 wt%, 24 wt%, 26 wt%, 28 wt%, or 30 wt%, and the selection of the above numerical values is not limited to the recited numerical values, and other numerical values not recited in the respective numerical values are also applicable.
The alloy particles comprise 33.3-46.4 wt% of tin, such as 33.3 wt%, 35.0 wt%, 37.0 wt%, 39.0 wt%, 41.0 wt%, 43.0 wt% or 46.4 wt% by mass percentage; gallium 13.0-25.9 wt%, e.g., 13.0 wt%, 14.0 wt%, 17.0 wt%, 19.0 wt%, 21.0 wt%, 23.0 wt%, or 25.9 wt%, etc.; 34.8 to 47.8 wt% of indium, for example, 34.8 wt%, 36.0 wt%, 38.0 wt%, 41.0 wt%, 44.0 wt%, or 47.8 wt%, and the selection of the above numerical values is not limited to the enumerated values, and other non-enumerated values within the respective numerical values are also applicable.
In the invention, the components of the liquid alloy and the alloy particles in the heat conduction material are the same, so that the compatibility of the liquid alloy and the alloy particles is improved, and meanwhile, the heat conduction coefficient of the heat conduction material is effectively improved by the matching use of the liquid alloy and the alloy particles; in addition, the melting point of the prepared liquid alloy is 5-12 ℃, which is far lower than the room temperature, and the liquid alloy has larger supercooling degree, so that the liquid alloy can still keep liquid state without crystallization at the temperature of below 15 ℃ below zero, the application range of the heat conducting material is expanded, and the crystallization generated at the lower temperature in winter is avoided, and the use is prevented from being interfered; the melting point of the prepared alloy particles is 60-100 ℃, the alloy particles enter a heating temperature range of a common electronic chip, and the alloy particles are added into the liquid alloy to change the surface tension of the pure liquid alloy and reduce the cohesion and affinity, so that the prepared alloy particles are not simple low-viscosity liquid metal but slurry materials with higher viscosity, the generation of a water drop phenomenon can be avoided, and the using amount is easier to control; the heat conduction material has simple components and lower cost than metal silver, can effectively improve the heat conduction performance and is beneficial to industrial application.
In the present invention, the addition of a metal immiscible with gallium, such as bismuth metal, is avoided to avoid the occurrence of phase separation.
In the present invention, the ratio of tin, gallium and indium in the liquid alloy is controlled. If the content of tin is too low, the cost is too high; if the content of tin is too high, the melting point of the liquid alloy can be increased and even be higher than the room temperature; if the content of gallium is too low, the melting point of the liquid alloy is too high, even higher than room temperature; if the content of gallium is excessive, the gallium is easy to react with alloy particles to form metal compounds, so that the original alloy particles are liquefied; if the content of indium is too low, the surface tension and the melting point of the liquid alloy cannot be controlled, and the main low-melting-point characteristic needs the matching of gallium and indium; if the content of indium is too large, cost is not favorable.
The following technical solutions are preferred technical solutions of the present invention, but not limited to the technical solutions provided by the present invention, and technical objects and advantageous effects of the present invention can be better achieved and achieved by the following technical solutions.
As a preferred embodiment of the present invention, the alloy liquid further includes zinc.
In the present invention, the addition of zinc can further assist in lowering the melting point of the alloy.
As a preferred embodiment of the present invention, the liquid alloy includes, by mass, 10 to 15 wt% of tin, for example, 10 wt%, 11 wt%, 12 wt%, 13 wt%, 14 wt%, or 15 wt%; gallium 60-70 wt%, such as 60 wt%, 62 wt%, 64 wt%, 66 wt%, 68 wt%, or 70 wt%, and the like; 20-30 wt% of indium, such as 20 wt%, 22 wt%, 24 wt%, 26 wt%, 28 wt%, or 30 wt%, etc.; 1 wt.% or less, for example, 0.1 wt.%, 0.2 wt.%, 0.4 wt.%, 0.6 wt.%, 0.8 wt.%, or 1 wt.%, and the above-mentioned values are not limited to the values listed, and other values not listed in the respective numerical ranges are also applicable.
In a preferred embodiment of the present invention, the alloy particles have a particle size of 0.5 to 100. mu.m, for example, 0.5. mu.m, 1. mu.m, 10. mu.m, 20. mu.m, 30. mu.m, 40. mu.m, 50. mu.m, 60. mu.m, 70. mu.m, 80. mu.m, 90. mu.m or 100. mu.m, but the invention is not limited to the above-mentioned values, and other values not shown in the above-mentioned numerical range are also applicable.
In the invention, the particle size of the alloy particles has certain influence on the final heat conduction effect. If the particle size is too large, the gap of the heat-conducting interface layer is influenced, so that the thermal resistance is increased; if the particle size is too small, the specific surface area increases, which increases the oil absorption, and more liquid metal is required to fill the gaps between the metal particles, which increases the viscosity and affects the handling and coating properties.
In a preferred embodiment of the present invention, the mass ratio of the liquid alloy to the alloy particles is 1 (2-9), for example, 1:2, 1:3, 1:4, 1:5, 1:6, 1:7, 1:8, or 1:9, but the present invention is not limited to the above-mentioned values, and other values not listed in the above-mentioned range of values are also applicable.
In the invention, the mass ratio of the liquid alloy to the alloy particles needs to be controlled. If too many alloy particles are added, the appearance is sand-grained, and the coating is not facilitated; if too few alloy particles are added, the overall viscosity is too low, and the phenomenon of fluid escape is easy to occur during use.
In another aspect, the present invention provides a preparation method of the above thermal conductive material, including the following steps:
(1) mixing tin, gallium and indium to obtain liquid alloy;
(2) mixing tin and indium, adding gallium, and performing spray granulation or rapid condensation to obtain alloy particles;
(3) and mixing the obtained liquid alloy and alloy particles to obtain the slurry alloy heat conduction material.
In the preparation method, the required slurry-like alloy heat conduction material can be obtained by respectively preparing the liquid alloy and the alloy particles and then mixing the liquid alloy and the alloy particles, and the preparation method has the advantages of simple process flow, lower equipment cost and better industrial application prospect.
As a preferable technical scheme of the invention, the raw material of the liquid alloy in the step (1) also comprises zinc.
Preferably, the tin, gallium, indium and zinc, in mass percent, are 10-15 wt% of tin, such as 10 wt%, 11 wt%, 12 wt%, 13 wt%, 14 wt% or 15 wt%, etc., respectively; gallium 60-70 wt%, such as 60 wt%, 62 wt%, 64 wt%, 66 wt%, 68 wt%, or 70 wt%, and the like; 20-30 wt% of indium, such as 20 wt%, 22 wt%, 24 wt%, 26 wt%, 28 wt%, or 30 wt%, etc.; 1 wt.% or less, for example, 0.1 wt.%, 0.2 wt.%, 0.4 wt.%, 0.6 wt.%, 0.8 wt.%, or 1 wt.%, and the above-mentioned values are not limited to the values listed, and other values not listed in the respective numerical ranges are also applicable.
Preferably, the temperature of the mixing in step (1) is 100-.
As a preferred technical scheme of the invention, in the mixing process in the step (2), the tin and the indium respectively account for 45-53 wt% of tin, such as 45 wt%, 47 wt%, 48 wt%, 49 wt%, 51 wt% or 53 wt% in percentage by mass; 47 to 55 wt% of indium, for example, 47 wt%, 49 wt%, 50 wt%, 51 wt%, 52 wt%, 54 wt%, or 55 wt%, and the selection of the above numerical values is not limited to the recited numerical values, and other numerical values not recited in the respective numerical values are also applicable.
Preferably, the gallium is added in step (2) in an amount of 15-35%, for example 15%, 17%, 20%, 22%, 25%, 28%, 30%, 33% or 35% by weight of the total mass of tin and indium, but not limited to the recited values, and other values not recited in this range are also applicable.
In the invention, in the process of preparing the alloy particles, the tin and the indium are mixed to reach the eutectic point, and then the gallium with the mass sum of the two is taken as the reference, 15-35 percent of gallium is added, so that the melting point of the tin-indium alloy can be reduced to 120 ℃ of the eutectic point, and when the gallium is added, the gallium is not required to be easily oxidized in order to melt the tin with higher melting point (the melting point is 234 ℃).
In the present invention, the sum of the mass fractions of tin and indium in the mixing in step (2) is "100 wt%".
In the invention, the addition amount of gallium has an important influence on the melting point of the alloy when preparing the alloy particles. If the addition amount of gallium is too much, the melting point of the alloy is low; if the amount of gallium added is too small, the melting point of the alloy will be too high.
Preferably, the temperature of the mixing in step (2) is 100-.
As a preferred embodiment of the present invention, the temperature of the spray granulation in the step (2) is 150-200 ℃, for example, 150 ℃, 160 ℃, 170 ℃, 180 ℃, 190 ℃ or 200 ℃, but the temperature is not limited to the values listed, and other values not listed in the numerical range are also applicable.
Preferably, the temperature of said flash condensation of step (2) is from-15 to 10 ℃, such as-15 ℃, -10 ℃, -5 ℃, 0 ℃, 5 ℃ or 10 ℃ and the like, but is not limited to the recited values, and other values not recited in this range of values are equally applicable.
In a preferred embodiment of the present invention, the liquid alloy and the alloy particles in step (3) are mixed at a mass ratio of 1 (2 to 9), for example, 1:2, 1:3, 1:4, 1:5, 1:6, 1:7, 1:8, or 1:9, but the present invention is not limited to the above-mentioned values, and other values not shown in the above-mentioned range are also applicable.
Compared with the prior art, the invention has the following beneficial effects:
(1) according to the heat conduction material, the tin, the gallium and the indium are used as main components, and the liquid alloy and the alloy particles which are the same in components but different in component content are matched for use, so that the heat conduction coefficient of the heat conduction material is effectively improved, and the heat conduction coefficient of the heat conduction material can reach 60.9W/(m)2K) or more, and the thermal resistance is reduced to be below 0.34K/W; meanwhile, the particle size of the alloy particles and the proportion of the liquid alloy to the alloy particles are further controlled, so that the heat conduction effect is remarkably improved, the thermal resistances are all below 0.13K/W, the heat is transferred out quickly, and the electronic component is protected from being influenced by heat;
(2) the heat conduction material has simple composition, easily obtained raw materials, lower cost and high economic benefit; the preparation method has simple process flow and better industrial application prospect.
Detailed Description
In order to better illustrate the present invention and facilitate the understanding of the technical solutions of the present invention, the present invention is further described in detail below. However, the following examples are only simple examples of the present invention and do not represent or limit the scope of the present invention, which is defined by the claims.
The following are typical but non-limiting examples of the invention:
example 1:
the embodiment provides a slurry alloy heat conduction material and a preparation method thereof, wherein the heat conduction material consists of liquid alloy and alloy particles;
the liquid alloy comprises, by mass, 10 wt% of tin, 60 wt% of gallium and 30 wt% of indium;
the alloy particles comprise 33.3 wt% of tin, 25.9 wt% of gallium and 40.8 wt% of indium in percentage by mass.
The preparation method of the heat conduction material comprises the following steps:
(1) mixing 10 wt% of tin, 60 wt% of gallium and 30 wt% of indium at the temperature of 100 ℃ to obtain a liquid alloy;
(2) mixing 45 wt% of tin and 55 wt% of indium at 100 ℃, adding 35% of gallium based on the total mass of the tin and the indium, and performing spray granulation at 150 ℃ to obtain alloy particles with the particle size of 100 microns;
(3) and mixing the obtained liquid alloy and alloy particles according to the mass ratio of 1:2 to obtain the slurry alloy heat conduction material.
Example 2:
the embodiment provides a slurry alloy heat conduction material and a preparation method thereof, wherein the heat conduction material consists of liquid alloy and alloy particles;
the liquid alloy comprises 15 wt% of tin, 70 wt% of gallium and 15 wt% of indium in percentage by mass;
the alloy particles comprise 46.1 wt% of tin, 13.0 wt% of gallium and 40.9 wt% of indium in percentage by mass.
The preparation method of the heat conduction material comprises the following steps:
(1) mixing 15 wt% of tin, 70 wt% of gallium and 15 wt% of indium at the temperature of 200 ℃ to obtain a liquid alloy;
(2) mixing 53 wt% of tin and 47 wt% of indium at 200 ℃, adding 15% of gallium based on the total mass of the tin and the indium, and performing spray granulation at 200 ℃ to obtain alloy particles with the particle size of 5 microns;
(3) and mixing the obtained liquid alloy and alloy particles according to the mass ratio of 1:9 to obtain the slurry alloy heat conduction material.
Example 3:
the embodiment provides a slurry alloy heat conduction material and a preparation method thereof, wherein the heat conduction material consists of liquid alloy and alloy particles;
the liquid alloy comprises, by mass, 10 wt% of tin, 70 wt% of gallium and 20 wt% of indium;
the alloy particles comprise, by mass, 41.7 wt% of tin, 16.6 wt% of gallium and 41.7 wt% of indium.
The preparation method of the heat conduction material comprises the following steps:
(1) mixing 10 wt% of tin, 70 wt% of gallium and 20 wt% of indium at the temperature of 150 ℃ to obtain a liquid alloy;
(2) mixing 50 wt% of tin and 50 wt% of indium at 130 ℃, adding 20% of gallium based on the total mass of the tin and the indium, and performing spray granulation at 170 ℃ to obtain alloy particles with the particle size of 20 microns;
(3) and mixing the obtained liquid alloy and alloy particles according to the mass ratio of 1:5 to obtain the slurry alloy heat conduction material.
Example 4:
the embodiment provides a slurry alloy heat conduction material and a preparation method thereof, wherein the heat conduction material consists of liquid alloy and alloy particles;
the liquid alloy comprises 12 wt% of tin, 65 wt% of gallium, 22.5 wt% of indium and 0.5 wt% of zinc in percentage by mass;
the alloy particles comprise 39.2 wt% of tin, 20 wt% of gallium and 40.8 wt% of indium in percentage by mass.
The preparation method of the heat conduction material comprises the following steps:
(1) mixing 12 wt% of tin, 65 wt% of gallium, 22.5 wt% of indium and 0.5 wt% of zinc at 140 ℃ to obtain a liquid alloy;
(2) mixing 49 wt% of tin and 51 wt% of indium at 180 ℃, adding 25% of gallium based on the total mass of the tin and the indium, and performing spray granulation at 160 ℃ to obtain alloy particles with the particle size of 10 microns;
(3) and mixing the obtained liquid alloy and alloy particles according to the mass ratio of 1:3 to obtain the slurry alloy heat conduction material.
Example 5:
the embodiment provides a slurry alloy heat conduction material and a preparation method thereof, wherein the heat conduction material consists of liquid alloy and alloy particles;
the liquid alloy comprises 14 wt% of tin, 62 wt% of gallium, 23 wt% of indium and 1 wt% of zinc in percentage by mass;
the alloy particles comprise, by mass, 38.5 wt% of tin, 23.0 wt% of gallium and 38.5 wt% of indium.
The preparation method of the heat conduction material comprises the following steps:
(1) mixing 14 wt% of tin, 62 wt% of gallium, 23 wt% of indium and 1 wt% of zinc at 150 ℃ to obtain a liquid alloy;
(2) mixing 50 wt% of tin and 50 wt% of indium at 130 ℃, adding 30% of gallium based on the total mass of the tin and the indium, and rapidly condensing at-15 ℃ to obtain alloy particles with the particle size of 0.5 mu m;
(3) and mixing the obtained liquid alloy and alloy particles according to the mass ratio of 1:7 to obtain the slurry alloy heat conduction material.
Example 6:
the present embodiment provides a slurry alloy heat conductive material and a method for preparing the same, which is referred to the heat conductive material of embodiment 1.
The preparation method of the heat conductive material is as described in example 1, except that: and (3) preparing alloy particles with the particle size of 110 microns in the step (2).
Example 7:
the present embodiment provides a slurry alloy heat conductive material and a method for preparing the same, which is referred to the heat conductive material of embodiment 5.
The preparation method of the heat conductive material is as described in example 5, except that: and (3) preparing alloy particles with the particle size of 0.1 mu m in the step (2).
Example 8:
the present embodiment provides a slurry alloy heat conductive material and a method for preparing the same, which is referred to the heat conductive material of embodiment 1.
The preparation method of the heat conductive material is as described in example 1, except that: and (4) mixing the obtained liquid alloy and alloy particles according to the mass ratio of 1:1 in the step (3).
Example 9:
the present embodiment provides a slurry alloy heat conductive material and a method for preparing the same, which is referred to the heat conductive material of embodiment 2.
The preparation method of the heat conductive material is as described in example 2, except that: and (4) mixing the obtained liquid alloy and alloy particles according to the mass ratio of 1:10 in the step (3).
Comparative example 1:
this comparative example provides a slurry alloy heat conductive material and a method of making the same, the heat conductive material being as described in example 1 with the only difference being: the liquid alloy comprises 5 wt% of tin, 63.3 wt% of gallium and 31.7 wt% of indium in percentage by mass, namely the addition amount of tin is reduced, and the reduced part is proportionally increased to other components.
The preparation method of the heat conductive material is as described in example 1, except that: in step (1), 5 wt% of tin, 63.3 wt% of gallium and 31.7 wt% of indium were mixed.
Comparative example 2:
this comparative example provides a slurry alloy heat conductive material and a method of making the same, the heat conductive material being as described in example 2 with the only difference that: the liquid alloy comprises 20 wt% of tin, 65.9 wt% of gallium and 14.1 wt% of indium in percentage by mass, namely the addition amount of tin is increased, and the increased part is proportionally subtracted from other components.
The preparation method of the heat conductive material is as described in example 2, except that: in step (1), 20 wt% of tin, 65.9 wt% of gallium and 14.1 wt% of indium are mixed.
Comparative example 3:
this comparative example provides a slurry alloy heat conductive material and a method of making the same, the heat conductive material being as described in example 1 with the only difference being: the liquid alloy comprises 11.25 wt% of tin, 55 wt% of gallium and 33.75 wt% of indium in percentage by mass, namely the addition amount of gallium is reduced, and the reduced part is proportionally increased to other components.
The preparation method of the heat conductive material is as described in example 1, except that: in step (1), 11.25 wt% tin, 55 wt% gallium and 33.75 wt% indium were mixed.
Comparative example 4:
this comparative example provides a slurry alloy heat conductive material and a method of making the same, the heat conductive material being as described in example 2 with the only difference that: the liquid alloy comprises 12.5 wt% of tin, 75 wt% of gallium and 12.5 wt% of indium in percentage by mass, namely the addition amount of gallium is increased, and the increased part is proportionally subtracted from other components.
The preparation method of the heat conductive material is as described in example 2, except that: 12.5 wt% tin, 75 wt% gallium and 12.5 wt% indium were mixed in step (1).
Comparative example 5:
this comparative example provides a slurry alloy heat conductive material and a method of making the same, the heat conductive material being as described in example 1 with the only difference being: the liquid alloy comprises 9.3 wt% of tin, 55.7 wt% of gallium and 35 wt% of indium in percentage by mass, namely the addition amount of the indium is increased, and the increased part is proportionally subtracted from other components.
The preparation method of the heat conductive material is as described in example 1, except that: in step (1), 9.3 wt% tin, 55.7 wt% gallium and 35 wt% indium were mixed.
Comparative example 6:
this comparative example provides a slurry alloy heat conductive material and a method of making the same, the heat conductive material being as described in example 3 with the only difference that: the liquid alloy comprises 10.6 wt% of tin, 74.4 wt% of gallium and 15 wt% of indium in percentage by mass, namely the addition amount of indium is reduced, and the reduced part is proportionally increased to other components.
The preparation method of the heat conductive material is as described in example 3, except that: in step (1), 10.6 wt% of tin, 74.4 wt% of gallium and 15 wt% of indium are mixed.
Comparative example 7:
this comparative example provides a slurry alloy heat conductive material and a method of making the same, the heat conductive material being as described in example 1 with the only difference being: the alloy particles comprise 32.1 wt% of tin, 28.6 wt% of gallium and 39.3 wt% of indium in percentage by mass.
The preparation method of the heat conductive material is as described in example 1, except that: in the step (2), 45 wt% of tin and 55 wt% of indium are mixed, and then 40% of gallium is added based on the total mass of the tin and the indium.
Comparative example 8:
this comparative example provides a slurry alloy heat conductive material and a method of making the same, the heat conductive material being as described in example 2 with the only difference that: the alloy particles comprise 48.2 wt% of tin, 9.1 wt% of gallium and 42.7 wt% of indium in percentage by mass.
The preparation method of the heat conductive material is as described in example 2, except that: in the step (2), 53 wt% of tin and 47 wt% of indium are mixed, and then 10% of gallium is added based on the total mass of the tin and the indium.
Comparative example 9:
this comparative example provides a paste-like heat conductive material, which is different from the heat conductive material of example 1 only in that: the heat conductive material consists of only liquid alloy and does not include alloy particles.
Comparative example 10:
this comparative example provides a paste-like heat conductive material comprising 20 wt% of dimethyl siloxane and 80 wt% of alumina.
The thermal conductivity and thermal resistance of the slurry alloy heat conductive materials obtained in examples 1 to 9 and comparative examples 1 to 10 were measured and coated on a copper block, and the coating results were observed, and all the results are shown in table 1.
TABLE 1
The heat conduction materials obtained in the embodiments 1 to 5 effectively avoid the water drop phenomenon generated during coating by matching the liquid alloy with the alloy particles, which have the same components but different component contents, and greatly improve the heat conduction effect, so that the heat conduction coefficients are increased to 60.9W/(m) m2K) above, the thermal resistance is below 0.13K/W, and the viscosity is adjustable; example 6 increases the particle size of the alloy particles, so that the viscosity is reduced and the thermal resistance is increased; example 7 reduces the particle size of the alloy particles, so that the viscosity is increased and the thermal resistance is increased; example 8 the amount of alloy particles added was reduced, the phenomenon of water drops occurred during coating, and the thermal resistance was increased; example 9 increased the amount of alloy particles added, resulting in increased viscosity and a sandy appearance, which makes coating impossible.
Comparative examples 1 to 6 in the preparation of the liquid alloy, the contents of the components were adjusted so that the contents of one of the components were excessively large or small, which resulted in the decrease of the thermal conductivity and the generation of the water drop phenomenon; comparative example 7 the amount of added gallium was increased in the process of preparing alloy particles, resulting in a decrease in the heat transfer coefficient; while comparative example 8 reduced the amount of added gallium during the preparation of the alloy particles, resulting in an increase in the melting point of the alloy particles; the heat conductive material obtained in comparative example 9 does not contain alloy particles, resulting in a drop-like shape when coated; the comparative example 10 is a conventional thermal conductive adhesive material, and has a low thermal conductivity coefficient and a poor thermal conductive effect during use.
As can be seen from a combination of the above examples and comparative examples, the thermally conductive material of the present invention is obtained by mixing tin,Gallium and indium are used as main components, and liquid alloy and alloy particles which have the same components but different component contents are used in a matching way, so that the heat conductivity coefficient of the heat conduction material is effectively improved, and the heat conduction coefficient of the heat conduction material reaches 60.9W/(m)2K) or more, and the thermal resistance is reduced to be below 0.34K/W; meanwhile, by further controlling the grain diameter of the alloy particles and the proportion of the liquid alloy and the alloy particles, the heat conduction effect is remarkably improved, the thermal resistance is enabled to be below 0.13K/W, and the operability is improved; the heat conduction material has simple composition, easily obtained raw materials, lower cost and high economic benefit; the preparation method has simple process flow and better industrial application prospect.
The applicant states that the present invention is illustrated by the above examples to show the products and detailed methods of the present invention, but the present invention is not limited to the above products and detailed methods, i.e. it is not meant that the present invention must rely on the above products and detailed methods to be carried out. It will be apparent to those skilled in the art that any modifications to the present invention, equivalents thereof, additions of additional operations, selection of specific ways, etc., are within the scope and disclosure of the present invention.
Claims (10)
1. The slurry alloy heat conduction material is characterized in that the heat conduction material is composed of liquid alloy and alloy particles;
the liquid alloy comprises, by mass, 10-15 wt% of tin, 60-70 wt% of gallium and 20-30 wt% of indium;
the alloy particles comprise, by mass, 33.3-46.4 wt% of tin, 13.0-25.9 wt% of gallium and 34.8-47.8 wt% of indium.
2. The thermally conductive material of claim 1, wherein the alloying liquid further comprises zinc.
3. The heat conductive material of claim 2, wherein the liquid alloy comprises, in mass percent, 10-15 wt% tin, 60-70 wt% gallium, 20-30 wt% indium, and 1 wt% or less zinc.
4. A heat conductive material according to any of claims 1 to 3, wherein the alloy particles have a particle size of 0.5 to 100 μm.
5. The heat conductive material according to any one of claims 1 to 4, wherein the mass ratio of the liquid alloy to the alloy particles is 1 (2-9).
6. A method of preparing a heat conductive material according to any of claims 1 to 5, comprising the steps of:
(1) mixing tin, gallium and indium to obtain liquid alloy;
(2) mixing tin and indium, adding gallium, and performing spray granulation or rapid condensation to obtain alloy particles;
(3) and mixing the obtained liquid alloy and alloy particles to obtain the slurry alloy heat conduction material.
7. The method according to claim 6, wherein the raw material of the liquid alloy of step (1) further includes zinc;
preferably, the tin, the gallium, the indium and the zinc respectively account for 10-15 wt% of tin, 60-70 wt% of gallium, 20-30 wt% of indium and less than or equal to 1 wt% of zinc in percentage by mass;
preferably, the temperature of the mixing in step (1) is 100-200 ℃.
8. The production method according to claim 6 or 7, wherein in the mixing process in the step (2), the tin and the indium are 45-53 wt% of tin and 47-55 wt% of indium respectively in terms of mass percentage;
preferably, the addition amount of the gallium in the step (2) accounts for 15-35% of the total mass of the tin and the indium;
preferably, the temperature of the mixing in the step (2) is 100-200 ℃.
9. The method according to any one of claims 6 to 8, wherein the temperature for the spray granulation in step (2) is 150 ℃ to 200 ℃;
preferably, the temperature of the rapid condensation in step (2) is-15 to 10 ℃.
10. The production method according to any one of claims 6 to 9, wherein the liquid alloy and the alloy particles in the step (3) are mixed at a mass ratio of 1 (2) to 9.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0411286A1 (en) * | 1989-08-03 | 1991-02-06 | International Business Machines Corporation | Liquid metal matrix thermal paste |
| JP2012111823A (en) * | 2010-11-24 | 2012-06-14 | Toyota Motor Corp | Heat dissipating grease composition |
| CN103642465A (en) * | 2013-11-08 | 2014-03-19 | 北京依米康科技发展有限公司 | Liquid metal heat conductive cream, and preparation method and applications thereof |
| CN110387217A (en) * | 2019-07-26 | 2019-10-29 | 云南中宣液态金属科技有限公司 | A kind of high-performance compound thermal interfacial material and preparation method thereof |
| CN111112632A (en) * | 2019-12-30 | 2020-05-08 | 浙江大学 | Preparation method of low-melting-point high-electric-conductivity high-heat-conductivity metal nanoparticles |
-
2021
- 2021-06-11 CN CN202110652466.XA patent/CN113388769B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0411286A1 (en) * | 1989-08-03 | 1991-02-06 | International Business Machines Corporation | Liquid metal matrix thermal paste |
| JP2012111823A (en) * | 2010-11-24 | 2012-06-14 | Toyota Motor Corp | Heat dissipating grease composition |
| CN103642465A (en) * | 2013-11-08 | 2014-03-19 | 北京依米康科技发展有限公司 | Liquid metal heat conductive cream, and preparation method and applications thereof |
| CN110387217A (en) * | 2019-07-26 | 2019-10-29 | 云南中宣液态金属科技有限公司 | A kind of high-performance compound thermal interfacial material and preparation method thereof |
| CN111112632A (en) * | 2019-12-30 | 2020-05-08 | 浙江大学 | Preparation method of low-melting-point high-electric-conductivity high-heat-conductivity metal nanoparticles |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113956853A (en) * | 2021-10-29 | 2022-01-21 | 上海交通大学 | Method for regulating and controlling thermal performance of liquid metal composite material and liquid metal composite material |
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