CN116801595A - Heat conducting material and preparation method and application thereof - Google Patents

Heat conducting material and preparation method and application thereof Download PDF

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Publication number
CN116801595A
CN116801595A CN202310968501.8A CN202310968501A CN116801595A CN 116801595 A CN116801595 A CN 116801595A CN 202310968501 A CN202310968501 A CN 202310968501A CN 116801595 A CN116801595 A CN 116801595A
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China
Prior art keywords
liquid metal
metal layer
sheet
layer
indium
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Chinese (zh)
Inventor
张嘉楠
曹勇
孙爱祥
杨健虹
窦兰月
周晓燕
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Shenzhen Hongfucheng New Material Co ltd
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Shenzhen Hongfucheng New Material Co ltd
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Priority to CN202310968501.8A priority Critical patent/CN116801595A/en
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    • HELECTRICITY
    • H05ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05KPRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K7/00Constructional details common to different types of electric apparatus
    • H05K7/20Modifications to facilitate cooling, ventilating, or heating
    • H05K7/2039Modifications to facilitate cooling, ventilating, or heating characterised by the heat transfer by conduction from the heat generating element to a dissipating body
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B15/00Layered products comprising a layer of metal
    • B32B15/01Layered products comprising a layer of metal all layers being exclusively metallic
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B33/00Layered products characterised by particular properties or particular surface features, e.g. particular surface coatings; Layered products designed for particular purposes not covered by another single class
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/06Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the heating method
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/10Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the pressing technique, e.g. using action of vacuum or fluid pressure
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B38/00Ancillary operations in connection with laminating processes
    • B32B38/10Removing layers, or parts of layers, mechanically or chemically
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00Properties of the layers or laminate
    • B32B2307/30Properties of the layers or laminate having particular thermal properties
    • B32B2307/302Conductive
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2457/00Electrical equipment

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  • Physics & Mathematics (AREA)
  • Engineering & Computer Science (AREA)
  • Thermal Sciences (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Fluid Mechanics (AREA)
  • Mechanical Engineering (AREA)
  • Cooling Or The Like Of Semiconductors Or Solid State Devices (AREA)

Abstract

The application discloses a heat conduction material, a preparation method and application thereof, and belongs to the technical field of materials. The heat conduction material comprises an indium sheet layer, a first liquid metal layer and a second liquid metal layer, wherein the first liquid metal layer and the second liquid metal layer are arranged on the upper surface and the lower surface of the indium sheet layer; the melting points of the two liquid metal layers are not more than 30 ℃, or the melting points of the two liquid metal layers are not less than 30 ℃; the connection areas of the indium sheet layer and the two liquid metal layers are both formed with a solid indium-rich alloy. The heat conduction material has low heat resistance, good heat conductivity and heat performance equivalent to that of pure liquid metal, and is in a solid form in use and after use, no observable liquid component exists, and the problems of short circuit and burnout of devices and the like caused by leakage or flow of the liquid metal when the liquid metal is singly used in the prior art are avoided.

Description

Heat conducting material and preparation method and application thereof
Technical Field
The application relates to the technical field of materials, in particular to a heat conduction material, a preparation method and application thereof.
Background
Along with the continuous progress of technology, electronic components and electronic devices are miniaturized and miniaturized, but negative effects caused by heat dissipation problems are increasingly serious, heat dissipation design becomes an important component of the modern electronic and electric industry, at this time, heat generated by heat conduction is dissipated by an insulating material, and heat dissipation methods using heat dissipation fins to conduct heat are more common.
The liquid metal is a novel heat conduction interface material developed in the last ten years, and has the characteristics of low heat resistance and high heat conductivity. The most critical problem with current liquid metals arises from their fluidity as liquid metal, which, if flowed or splashed onto the energized nodes on the surrounding circuit, can cause shorting and burning of the device, with significant losses. In order to prevent this, manufacturers using liquid metal heat conducting materials often make a layer of protective material, usually a ring of foam, around the device (e.g. chip) to be cooled, so that the liquid metal can be effectively blocked from leaking. But this adds additional cost and takes up considerable volume, making the otherwise crowded space around the main chip more intense.
Although the method for blocking and protecting can prevent the short circuit risk of liquid metal overflow, the liquid metal still leaks to the outside of the chip in the blocking material, and the liquid metal still has great influence on the heat conduction performance although the liquid metal does not leak to the outside of the blocking material. Since it is envisaged that the surface of the CPU would be coated with a uniform layer of liquid metal material and then some of the liquid metal would leak out and flow to the side during use. The enclosing material cannot be closely attached to the edge of the CPU chip, and a gap space is necessarily formed between the enclosing material and the CPU chip, so that liquid metal can flow. Then the liquid metal on the surface of the CPU may not be sufficient, and voids may even occur in some places, which obviously greatly affect the overall heat conducting performance. This situation is more pronounced after the machine has been placed vertically.
In view of this, the present application has been made.
Disclosure of Invention
The application aims to provide a heat conduction material, a preparation method and application thereof, so as to solve the technical problems.
The application can be realized as follows:
in a first aspect, the present application provides a thermally conductive material, including an indium sheet layer, a first liquid metal layer and a second liquid metal layer disposed on an upper surface and a lower surface of the indium sheet layer, respectively;
wherein the melting points of the first liquid metal layer and the second liquid metal layer are not more than 30 ℃ or are not lower than 30 ℃;
the connecting area of the indium sheet layer and the first liquid metal layer and the connecting area of the indium sheet layer and the first liquid metal layer are both formed with solid indium-rich alloy.
In an alternative embodiment, when the melting point of the first liquid metal layer and the second liquid metal layer is not more than 30 ℃, the starting materials for the preparation of the first liquid metal layer and the second liquid metal layer are both metals or metal alloys having a melting point of not more than 30 ℃.
In an alternative embodiment, the metal is Ga.
In an alternative embodiment, the metal alloy is formed from Ga, in, and Sn; more preferably, the metal alloy consists of Ga, in and Sn In a mass ratio of 68.5:21:10.5.
In an alternative embodiment, when the melting point of the first liquid metal layer and the second liquid metal layer is not lower than 30 ℃, the raw materials for preparing the first liquid metal layer and the second liquid metal layer each contain In, bi and Sn at the same time.
In an alternative embodiment, the first liquid metal layer and the second liquid metal layer are each made up of In, bi and Sn In a mass ratio of 51.3:32.3:16.4 or 51:32.5:16.5.
In an alternative embodiment, the first liquid metal layer and the second liquid metal layer each have a thickness of 10 to 50 μm and the indium platelet layer has a thickness of 0.05 to 0.5mm when the melting point of the first liquid metal layer and the second liquid metal layer is not more than 30 ℃.
In an alternative embodiment, when the melting point of the first liquid metal layer and the second liquid metal layer is not lower than 30 ℃, the thickness of the first liquid metal layer and the second liquid metal layer is 0.025-0.1mm, the thickness of the indium sheet layer is 0.05-0.5mm, and the thickness of the whole heat conducting material is 0.05-0.5mm.
In a second aspect, the present application provides a method for preparing a thermally conductive material according to any one of the preceding embodiments, comprising the steps of: and preparing a first liquid metal layer and a second liquid metal layer on the upper surface and the lower surface of the indium sheet layer respectively.
In an alternative embodiment, the first liquid metal layer and the second liquid metal layer are coated on the upper surface and the lower surface of the indium sheet, respectively, when the melting point of the first liquid metal layer and the second liquid metal layer is not more than 30 ℃.
In an alternative embodiment, the coating is performed at 60-90 ℃.
In an alternative embodiment, when the melting points of the first liquid metal layer and the second liquid metal layer are not lower than 30 ℃, the preparation raw materials of the first liquid metal layer and the preparation raw materials of the second liquid metal layer are respectively rolled into a first liquid metal sheet and a second liquid metal sheet, and the first liquid metal sheet, the indium sheet and the second liquid metal sheet are stacked according to preset positions and then rolled into the heat conducting material.
In an alternative embodiment, the first liquid metal sheet, the indium sheet and the second liquid metal sheet are stacked and then rolled to a temperature of 65-70 ℃.
In an alternative embodiment, after the first liquid metal sheet, the indium sheet and the second liquid metal sheet are stacked, a PET film is attached to the surface of the first liquid metal sheet facing away from the indium sheet and the surface of the second liquid metal sheet facing away from the indium sheet, then rolling is performed, and after rolling is finished, the PET film is removed.
In a third aspect, the present application provides a use of a thermally conductive material as in any of the preceding embodiments, for example for heat dissipation of electronic components.
The beneficial effects of the application include:
the heat conduction material provided by the application has low heat resistance, good heat conductivity and heat performance equivalent to that of pure liquid metal, and is in a solid form in use and after use, no observable liquid component exists, so that the problems of short circuit and burnout of devices and the like caused by leakage or flow of the liquid metal which are easy to occur when the liquid metal is singly used in the prior art are avoided.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings that are needed in the embodiments will be briefly described below, it being understood that the following drawings only illustrate some embodiments of the present application and therefore should not be considered as limiting the scope, and other related drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic illustration of the fusion of liquid metal and indium flakes into a new solid indium-rich alloy in accordance with the present application;
FIG. 2 is a schematic illustration of the surface of a liquid metal layer beginning to melt and infiltrate and wet a thermally conductive interface in accordance with the present application;
fig. 3 is a physical diagram of a heat conductive material provided in embodiment 1 of the present application;
FIG. 4 is a state diagram of the notebook computer before use in the test example;
FIG. 5 is a state diagram of the notebook computer in the test example after use;
FIG. 6 is a state diagram of the heat conductive material before entering the oven in the test example;
fig. 7 is a view showing a state after the heat conductive material is put into the oven in the test example.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present application more clear, the technical solutions of the embodiments of the present application will be clearly and completely described below. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
The heat conducting material, the preparation method and the application thereof provided by the application are specifically described below.
The application provides a heat conduction material which comprises an indium sheet layer, and a first liquid metal layer and a second liquid metal layer which are respectively arranged on the upper surface and the lower surface of the indium sheet layer. The connecting area of the indium sheet layer and the first liquid metal layer and the connecting area of the indium sheet layer and the first liquid metal layer are both formed with solid indium-rich alloy.
In some embodiments, the melting point of both the first liquid metal layer and the second liquid metal layer does not exceed 30 ℃ (e.g., 5 ℃, 6 ℃, 7 ℃, 8 ℃, 9 ℃, 10 ℃, 15 ℃,20 ℃, 25 ℃, 30 ℃, etc.). For reference, under this condition, the first liquid metal layer and the second liquid metal layer may each be prepared from a metal or a metal alloy having a melting point of not more than 30 ℃. The metal may be, for example but not limited to, ga. The metal alloy may be formed of Ga, in, and Sn by way of example and not limitation, and may be composed of Ga, in, and Sn In a mass ratio of 68.5:21:10.5, and may be composed of Ga, in, and Sn In other mass ratios as long as the melting point of the metal alloy of the composition does not exceed 30 ℃.
Accordingly, the thickness of the first and second liquid metal layers may be in the range of 10-50 μm, such as 10 μm, 15 μm, 20 μm, 25 μm, 30 μm, 35 μm, 40 μm, 45 μm, 50 μm, etc., under conditions where the melting point of the first and second liquid metal layers is not more than 30 ℃. The thickness of the indium sheet layer may be 0.05-0.5mm, such as 0.05mm, 0.1mm, 0.15mm, 0.2mm, 0.25mm, 0.3mm, 0.35mm, 0.4mm, 0.45mm, 0.5mm, etc. In some embodiments, the first and second liquid metal layers have a thickness of no more than 10% of the indium sheet layer thickness.
The above-mentioned preparation raw materials of the first liquid metal layer and the second liquid metal layer with melting points not exceeding 30 ℃ are in liquid state at normal temperature, and in the prior art, the liquid metal with melting points is generally directly smeared on the surface of a device (such as a chip or a radiator) to be cooled to play a role of heat dissipation. However, because the liquid metal is in a liquid form and has fluidity, the liquid metal is easy to flow or splash to an electrified node on a surrounding circuit, short circuits and device burnout are caused, and even if a blocking protection mode is adopted, the liquid metal smeared on the surface of the device with heat dissipation is difficult to completely avoid flowing and leakage to other spaces.
According to the application, the heat conducting material is provided with the structure that the middle part is the indium sheet layer and the two sides are the liquid metal layers, so that the indium sheet layer can play a role in framework and support. In addition, the indium sheet can be used as a heat conduction interface material, has good softness, is nontoxic and non-dangerous, can generate certain deformation and play a certain gap filling capability at a heat interface, and has lower thermal resistance (about 0.15cm at 50 psi) 2 ·K/W)。
On the basis, as the thickness of the first liquid metal layer and the second liquid metal layer is thinner, most of the liquid metal preparation raw materials can react and fuse with the indium sheet covered by the liquid metal to form new alloy In the preparation process, a series of eutectic alloys (such as InBiSn alloy or GaInSn alloy) are partially formed, and unbalanced alloys (namely non-eutectic alloys) are partially formed, wherein the series of eutectic alloys and the unbalanced alloys are solid, and the content of In is smaller at the position close to the surface of the heat conducting material. When the heat conductive material is heated (e.g., 50-70 ℃) and used, the whole of the series of eutectic alloy and unbalanced alloy formed above will undergo a brief (about 10 s) phase change melting, and the phase change process occurs in a brief period of time, but the brief period of time is enough for the melted part to move to the position where the gap is needed to be filled in the heat conductive material (i.e., to fill the gap of the thermal interface, such as the micro-relief and gap between the chip and the heat dissipation module, and bring about extremely low thermal resistance) to function as a "thermal interface material". In other words, most of the liquid metal and the surface indium sheet covered by the liquid metal react and fuse to form a new alloy, the middle indium sheet plays a supporting role, the original ductility and toughness of the middle indium sheet are maintained, and a small part of the liquid metal fills the gap of the contact surface. The formed new solid alloy is a metastable non-eutectic alloy, the melting point of the new solid alloy is not fixed and is about 130-150 ℃, and then, in the conventional operation of a device to be radiated, the whole heat conducting material is in a solid state (no liquid state), so that important key defects such as liquid metal flow, vertical flow and the like are effectively solved.
In other embodiments, the melting point of both the first liquid metal layer and the second liquid metal layer is not less than 30 ℃, such as 40 ℃, 50 ℃, 55 ℃, 60 ℃, 65 ℃, or 70 ℃, etc., preferably 50-70 ℃. For reference, in this case, the raw materials for preparing the first liquid metal layer and the second liquid metal layer may include In, bi, and Sn, for example, and may be composed of In, bi, and Sn In a mass ratio of 51.3:32.3:16.4 or 51:32.5:16.5. In addition, the metal alloy may be composed of In, bi and Sn In other mass ratios as long as the melting point of the metal alloy of the composition is not lower than 30 ℃.
Accordingly, when the melting point of the first liquid metal layer and the second liquid metal layer is not lower than 30 ℃, the thickness of the first liquid metal layer and the second liquid metal layer may be 0.025-0.1mm, such as 0.025mm, 0.05mm, 0.08mm, or 0.1 mm. The thickness of the indium sheet layer may be 0.05-0.5mm, such as 0.05mm, 0.1mm, 0.15mm, 0.2mm, 0.25mm, 0.3mm, 0.35mm, 0.4mm, 0.45mm, 0.5mm, etc. In some embodiments, the thickness of the whole heat conducting material is 0.05-0.5mm, that is, the stacked first liquid metal layer, indium sheet layer and second liquid metal layer are pressed together to the preset thickness of the heat conducting material in a calendaring mode.
The first liquid metal layer and the second liquid metal layer with melting points not lower than 30 ℃ are solid at normal temperature, the first liquid metal layer and the second liquid metal layer are usually placed on the surface of a device to be cooled, however, when the temperature of the device to be cooled exceeds 60 ℃, the liquid metal in the metal layers can be melted into liquid, and the liquid metal has fluidity and flows or splashes to the electrified nodes on a surrounding circuit easily, so that short circuits and device burning are caused, and even if a blocking protection mode is adopted, the liquid metal smeared on the surface of the device with the cooling is difficult to completely avoid flowing and leakage to other spaces.
According to the application, the heat conducting material is provided with the structure that the middle part is the indium sheet layer and the two sides are the liquid metal layers, so that the indium sheet layer can play a role in framework and support. In addition, the indium sheet can be used as a heat conduction interface material, has good softness, is nontoxic and non-dangerous, can generate certain deformation and play a certain gap filling capability at a heat interface, and has lower thermal resistance (about 0.15cm at 50 psi) 2 ·K/W)。
Under the calendaring temperature (65-70 ℃) in the preparation process, the liquid metal layer is in a solid-liquid mixed melting state, the flaky shape of the liquid metal layer is maintained, but the surface of the liquid metal layer is melted, the surface contacted with the indium flake can be infiltrated into indium metal, and the surface of the indium metal is fused into a whole to form a new solid indium-rich alloy (shown in figure 1), and after the temperature is reduced to room temperature, the whole heat conducting material is in a solid form. When the heat source is placed in a device to be cooled, if the heat source generates heat at a temperature exceeding 60 ℃, the surface of the liquid metal layer of the heat conducting material begins to melt, infiltrate and wet a heat conducting interface (shown in figure 2), and is quickly absorbed by the indium sheet layer at the same time, so that solidification and joint filling are completed, a new solid alloy layer formed by the middle indium sheet layer and two sides plays a role in supporting a framework, the heat conducting material cannot be melted, and the integrity and the stability of the heat conducting material can be ensured. In the conventional operation of the device to be cooled, the whole heat conducting material is solid (in a non-liquid state), so that important key defects such as liquid metal flow and vertical flow are effectively overcome.
As a result, the heat conduction material provided by the application has very low heat resistance, and the heat conduction material is about 0.04cm under 20psi 2 K/W is superior to silicone grease or phase-change silicone grease on the market, and in the practical computer CPU operation test, the heat performance is equivalent to that of pure liquid metal, but the heat conduction material has no observable liquid component in use and after use, so the risk that the liquid metal needs to be blocked and leaked is avoided.
Correspondingly, the application also provides a preparation method of the heat conducting material, which comprises the following steps: and preparing a first liquid metal layer and a second liquid metal layer on the upper surface and the lower surface of the indium sheet layer respectively.
When the melting points of the first liquid metal layer and the second liquid metal layer are not more than 30 ℃, the preparation raw materials of the first liquid metal layer and the preparation raw materials of the second liquid metal layer are respectively coated on the upper surface and the lower surface of the indium sheet.
The coating is carried out at 60-90deg.C (such as 60deg.C, 65deg.C, 70deg.C, 75deg.C, 80deg.C, 85deg.C or 90deg.C, etc.). For reference, the coating may be performed by spraying or knife coating, by way of example and not limitation. The liquid metal is alloyed with indium by heating while coating.
When the melting points of the first liquid metal layer and the second liquid metal layer are not lower than 30 ℃, respectively rolling the preparation raw materials of the first liquid metal layer and the preparation raw materials of the second liquid metal layer into a first liquid metal sheet and a second liquid metal sheet, stacking the first liquid metal sheet, the indium sheet and the second liquid metal sheet according to preset positions, and then rolling the stacked first liquid metal sheet, the indium sheet and the second liquid metal sheet into a heat conducting material.
For reference, the rolling temperature after the first liquid metal sheet, the indium sheet and the second liquid metal sheet are stacked may be 65 to 70 ℃, such as 65 ℃, 66 ℃, 67 ℃, 68 ℃, 69 ℃, 70 ℃, or the like.
In some embodiments, after stacking the first liquid metal sheet, the indium sheet and the second liquid metal sheet, attaching a PET film to a surface of the first liquid metal sheet facing away from the indium sheet and a surface of the second liquid metal sheet facing away from the indium sheet, then rolling, and removing the PET film after rolling is finished. In the calendaring process, the contact area of the liquid metal and the PET film can not be fused with each other, and only the contact area of the liquid metal and the indium sheet can be fused into a whole to form a new solid indium-rich alloy, and after the temperature is reduced to the room temperature, the PET film is peeled off to form the heat conducting material with the preset structure.
In addition, the application also provides application of the heat conduction material, for example, the heat conduction material can be used for heat dissipation of electronic components. The electronic device may be, for example but not limited to, a chip or a heat sink, etc.
The features and capabilities of the present application are described in further detail below in connection with the examples.
Example 1
The embodiment provides a heat conduction material, which is prepared by the following method:
the liquid metal raw material is sprayed on the upper surface and the lower surface of the indium sheet at 70 ℃ to form a first liquid metal layer with the thickness of 10 mu m and a second liquid metal layer with the thickness of 10 mu m.
Wherein the thickness of the indium sheet is 0.15mm. The first liquid metal layer and the second liquid metal layer are prepared from Ga, in and Sn In a mass ratio of 68.5:21:10.5. The melting point of the liquid metal feedstock in the first liquid metal layer and the second liquid metal layer is about 10 ℃.
A physical diagram of the thermally conductive material is shown in fig. 3.
Example 2
The embodiment provides a heat conduction material, which is prepared by the following method:
the liquid metal raw material was blade coated on the upper and lower surfaces of the indium sheet at 60 c to form a first liquid metal layer having a thickness of 10 μm and a second liquid metal layer having a thickness of 10 μm.
Wherein the thickness of the indium sheet is 0.15mm. The first liquid metal layer and the second liquid metal layer are each prepared from metal Ga having a melting point of about 29.5 ℃.
The eutectic alloy formed after the mutual diffusion and fusion of Ga and In is In75Ga25.
Example 3
The embodiment discloses a heat conduction material, which is prepared by the following method:
pure indium particles, bismuth particles and tin particles with purity more than 99.99% are used as raw materials, the mass ratio of indium to bismuth to tin is 51:32.5:16.5 in sequence, the raw materials with equal proportion are placed into a vacuum intermediate frequency smelting furnace, and the raw materials are vacuumized and heated to 400 ℃ for 2 hours.
After smelting, the mixture is placed into a vacuum heating stirrer, the temperature is kept at 80 ℃, and the mixture is stirred for 30min at 400rpm, so that liquid metal (the melting point is about 60 ℃) is uniformly mixed, and the mixture is poured into a mould for cooling for standby.
Pure indium ingots with purity of more than 99.99% are pressed to 0.2mm by a calender.
The above liquid metal was rolled into a sheet having a thickness of 50. Mu.m.
And stacking the indium sheet and the two liquid metal sheets together according to the positions of which the middle is the indium sheet and the two sides are the liquid metal sheets, and then attaching PET films to the surfaces of the two liquid metal sheets, which are away from the indium sheet, to obtain an intermediate product to be calendered.
The intermediate to be rolled was rolled by heating the roll to 65℃to give a total thickness of 0.15mm, followed by cooling to remove the PET film.
Example 4
The embodiment discloses a heat conduction material, which is prepared by the following method:
pure indium particles, bismuth particles and tin particles with purity more than 99.99% are used as raw materials, the mass ratio of indium to bismuth to tin is 51.3:32.3:16.4 in sequence, the raw materials with equal proportion are placed into a vacuum intermediate frequency smelting furnace, and the raw materials are vacuumized and heated to 400 ℃ for 2 hours.
After smelting, the mixture is placed into a vacuum heating stirrer, the temperature is kept at 80 ℃, and the mixture is stirred for 30min at 400rpm, so that liquid metal (the melting point is about 60 ℃) is uniformly mixed, and the mixture is poured into a mould for cooling for standby.
Pure indium ingots with purity of more than 99.99% are pressed to 0.5mm by a calender.
The liquid metal was rolled into a sheet having a thickness of 25. Mu.m.
And stacking the indium sheet and the two liquid metal sheets together according to the positions of which the middle is the indium sheet and the two sides are the liquid metal sheets, and then attaching PET films to the surfaces of the two liquid metal sheets, which are away from the indium sheet, to obtain an intermediate product to be calendered.
The intermediate to be rolled was rolled by heating the roll to 70℃to give a total thickness of 0.5mm, followed by cooling to remove the PET film.
Example 5
The embodiment provides a heat conduction material, which is prepared by the following method:
the liquid metal raw material is sprayed on the upper surface and the lower surface of the indium sheet at 60 ℃ to form a first liquid metal layer with the thickness of 30 mu m and a second liquid metal layer with the thickness of 30 mu m.
Wherein the thickness of the indium sheet is 0.05mm. The first liquid metal layer and the second liquid metal layer are prepared from Ga, in and Sn In a mass ratio of 55:32:13. The melting point of the liquid metal feedstock in the first liquid metal layer and the second liquid metal layer is about 25 ℃.
Example 6
The embodiment provides a heat conduction material, which is prepared by the following method:
the liquid metal raw material is sprayed on the upper surface and the lower surface of the indium sheet at 90 ℃ to form a first liquid metal layer with the thickness of 50 mu m and a second liquid metal layer with the thickness of 50 mu m.
Wherein the thickness of the indium sheet is 0.5mm. The first liquid metal layer and the second liquid metal layer are prepared from Ga, in and Sn In a mass ratio of 60:19.5:20.5. The melting point of the liquid metal feedstock in the first liquid metal layer and the second liquid metal layer is about 18 ℃.
Test examples
The heat conductive material (liquid metal heat conductive sheet) prepared in example 1 was placed on a certain high performance notebook computer CPU chip, and the results were shown in fig. 4 (before the baking machine) and fig. 5 (after the baking machine) after 24 hours of comparison of the products before the baking machine. As can be seen from fig. 4 and 5, the heat conducting material is in a solid form after being used, has no observable liquid component, and avoids the problems of short circuit and burning of devices caused by leakage or flow of the liquid metal in the prior art when the liquid metal is singly used.
In addition, the heat conductive material (liquid metal heat conductive sheet) prepared in example 1 was subjected to vertical standing vertical flow test at 125℃in an oven, and the results before and after baking are shown in FIGS. 6 and 7, respectively. As can be seen from a comparison of fig. 6 and 7: after baking at 125 ℃ for 1000 hours, the product has no vertical flow, no deformation and no overflow.
In summary, the heat conducting material provided by the application is in a solid state form in the use process, so that the problems of short circuit and burnout of devices and the like caused by leakage or flow of liquid metal which are easy to occur when the liquid metal is singly used in the prior art are avoided.
The above is only a preferred embodiment of the present application, and is not intended to limit the present application, but various modifications and variations can be made to the present application by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application should be included in the protection scope of the present application.

Claims (10)

1. The heat conducting material is characterized by comprising an indium sheet layer, and a first liquid metal layer and a second liquid metal layer which are respectively arranged on the upper surface and the lower surface of the indium sheet layer;
wherein the melting points of the first liquid metal layer and the second liquid metal layer are not more than 30 ℃ or are not lower than 30 ℃;
and a solid indium-rich alloy is formed in the connecting area of the indium sheet layer and the first liquid metal layer and the connecting area of the indium sheet layer and the first liquid metal layer.
2. The heat conducting material according to claim 1, wherein when the melting point of the first liquid metal layer and the second liquid metal layer is not more than 30 ℃, the preparation raw materials of the first liquid metal layer and the second liquid metal layer are metals or metal alloys with the melting point of not more than 30 ℃;
preferably, the metal is Ga;
preferably, the metal alloy is formed of Ga, in, and Sn; more preferably, the metal alloy consists of Ga, in and Sn In a mass ratio of 68.5:21:10.5.
3. The heat conductive material according to claim 1, wherein when the melting point of each of the first liquid metal layer and the second liquid metal layer is not lower than 30 ℃, in, bi and Sn are contained In the raw materials for preparing the first liquid metal layer and the second liquid metal layer;
preferably, the preparation raw materials of the first liquid metal layer and the second liquid metal layer are composed of In, bi and Sn according to the mass ratio of 51.3:32.3:16.4 or 51:32.5:16.5.
4. The heat conductive material according to claim 1 or 2, wherein the thickness of the first liquid metal layer and the second liquid metal layer is 10-50 μm and the thickness of the indium sheet layer is 0.05-0.5mm when the melting point of the first liquid metal layer and the second liquid metal layer is not more than 30 ℃.
5. A heat conductive material according to claim 1 or 3, wherein when the melting point of the first liquid metal layer and the second liquid metal layer is not lower than 30 ℃, the thickness of the first liquid metal layer and the second liquid metal layer is 0.025-0.1mm, the thickness of the indium sheet layer is 0.05-0.5mm, and the thickness of the entire heat conductive material is 0.05-0.5mm.
6. A method of preparing a thermally conductive material as claimed in any one of claims 1 to 5, comprising the steps of: and preparing a first liquid metal layer and a second liquid metal layer on the upper surface and the lower surface of the indium sheet layer respectively.
7. The method according to claim 6, wherein when the melting point of each of the first liquid metal layer and the second liquid metal layer is not more than 30 ℃, the raw materials for preparing the first liquid metal layer and the raw materials for preparing the second liquid metal layer are coated on the upper surface and the lower surface of the indium sheet, respectively;
preferably, the coating is carried out at 60-90 ℃.
8. The method according to claim 6, wherein when the melting points of the first liquid metal layer and the second liquid metal layer are not lower than 30 ℃, the raw materials for preparing the first liquid metal layer and the raw materials for preparing the second liquid metal layer are rolled into a first liquid metal sheet and a second liquid metal sheet, respectively, and the first liquid metal sheet, the indium sheet and the second liquid metal sheet are stacked in a predetermined position and then rolled into a heat conductive material;
preferably, the calendering temperature after stacking the first liquid metal sheet, the indium sheet and the second liquid metal sheet is 65-70 ℃.
9. The method according to claim 8, wherein after the first liquid metal sheet, the indium sheet and the second liquid metal sheet are stacked, a PET film is attached to a surface of the first liquid metal sheet facing away from the indium sheet and a surface of the second liquid metal sheet facing away from the indium sheet, and then the first liquid metal sheet, the indium sheet and the second liquid metal sheet are rolled, and after the rolling is finished, the PET film is removed.
10. Use of a thermally conductive material as claimed in any of claims 1-5 for heat dissipation of electronic components.
CN202310968501.8A 2023-08-02 2023-08-02 Heat conducting material and preparation method and application thereof Pending CN116801595A (en)

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CN117316776A (en) * 2023-09-27 2023-12-29 深圳市鸿富诚新材料股份有限公司 Preparation method of heat dissipation device

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CN104218010A (en) * 2014-09-10 2014-12-17 北京依米康科技发展有限公司 Metal thermal interface material
CN107658551A (en) * 2017-10-30 2018-02-02 南京信息工程大学 A kind of frequency reconfigurable antenna based on gallium indium tin liquid metal
US20220375817A1 (en) * 2021-05-19 2022-11-24 Indium Corporation Liquid metal thermal interface

Patent Citations (3)

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Publication number Priority date Publication date Assignee Title
CN104218010A (en) * 2014-09-10 2014-12-17 北京依米康科技发展有限公司 Metal thermal interface material
CN107658551A (en) * 2017-10-30 2018-02-02 南京信息工程大学 A kind of frequency reconfigurable antenna based on gallium indium tin liquid metal
US20220375817A1 (en) * 2021-05-19 2022-11-24 Indium Corporation Liquid metal thermal interface

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* Cited by examiner, † Cited by third party
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CN117316776A (en) * 2023-09-27 2023-12-29 深圳市鸿富诚新材料股份有限公司 Preparation method of heat dissipation device

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