CN111995991B - Thermal interface material and preparation method thereof - Google Patents
Thermal interface material and preparation method thereof Download PDFInfo
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- CN111995991B CN111995991B CN202010730605.1A CN202010730605A CN111995991B CN 111995991 B CN111995991 B CN 111995991B CN 202010730605 A CN202010730605 A CN 202010730605A CN 111995991 B CN111995991 B CN 111995991B
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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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L23/00—Details of semiconductor or other solid state devices
- H01L23/34—Arrangements for cooling, heating, ventilating or temperature compensation ; Temperature sensing arrangements
- H01L23/36—Selection of materials, or shaping, to facilitate cooling or heating, e.g. heatsinks
- H01L23/373—Cooling facilitated by selection of materials for the device or materials for thermal expansion adaptation, e.g. carbon
- H01L23/3735—Laminates or multilayers, e.g. direct bond copper ceramic substrates
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L23/00—Details of semiconductor or other solid state devices
- H01L23/34—Arrangements for cooling, heating, ventilating or temperature compensation ; Temperature sensing arrangements
- H01L23/36—Selection of materials, or shaping, to facilitate cooling or heating, e.g. heatsinks
- H01L23/373—Cooling facilitated by selection of materials for the device or materials for thermal expansion adaptation, e.g. carbon
- H01L23/3738—Semiconductor materials
Abstract
The invention discloses a thermal interface material and a preparation method thereof, wherein the thermal interface material is used for transferring heat generated by a heat source to a radiator and comprises a base material layer, a first contact layer, a second contact layer and a doping material. The substrate material layer is made of a positive thermal expansion coefficient material or a negative thermal expansion coefficient material, and the first contact layer covers one surface of the substrate material layer and is in contact with a heat source; the second contact layer covers the other surface of the substrate material layer and is in contact with the radiator; the thermal expansion coefficient of the doping material is opposite to that of the base material layer, and the concentration of the doping material is increased in a preset gradient from the central surface of the base material layer to the first contact layer and the second contact layer respectively. According to the invention, the concentration of the doping material is increased in a preset gradient manner, so that the small difference of thermal deformation of organic matters and heat conducting particles in the thermal interface material is ensured, the reduction of heat conducting capability caused by the formation of holes due to the stripping of the organic matters and the heat conducting particles is avoided, and the stable performance of the thermal interface material is ensured.
Description
Technical Field
The invention relates to the technical field of heat dissipation materials, in particular to a thermal interface material for a radiator and a preparation method thereof.
Background
The heat-conducting silicone grease is mainly used as a heat-conducting silicone grease which is commonly called as a heat-dissipating paste, and the heat-conducting silicone grease is a heat-conducting silicone grease-like compound prepared by adding a granular material with excellent heat resistance and heat-conducting property into organic silicone grease serving as a main raw material and is used for heat conduction and heat dissipation of electronic components such as a power amplifier, a transistor, an electronic tube, a CPU and the like, so that the stability of the electrical properties of electronic instruments, instruments and the like is ensured.
However, the thermal expansion coefficient of the heat-conducting silicone grease heat-conducting particles is small, the thermal expansion coefficient of the organic matter is large, and the thermal deformation difference between the organic matter and the heat-conducting particles is large, so that a plurality of gaps or holes are formed between the organic matter and the heat-conducting particles due to stripping in the use process, and the heat conduction capability of the composite material is reduced.
Disclosure of Invention
The invention aims to provide a thermal interface material and a preparation method thereof, and aims to solve the problems that in the prior art, the thermal expansion coefficient of heat-conducting silicone grease heat-conducting particles is small, the thermal expansion coefficient of organic matters is large, and the thermal deformation difference between the organic matters and the heat-conducting particles is large, so that a plurality of gaps or holes are formed between the organic matters and the heat-conducting particles due to stripping, and the heat conduction capability of a composite material is reduced.
In order to solve the above problems, the present invention provides a thermal interface material for a heat sink, the thermal interface material comprising:
the substrate material layer is made of a positive thermal expansion coefficient material or a negative thermal expansion coefficient material;
the first contact layer covers one surface of the substrate material layer and is in contact with the heat source;
the second contact layer covers the other surface of the substrate material layer and is in contact with the radiator;
and the doping material is mixed in the base material layer, the thermal expansion coefficient of the doping material is opposite to that of the base material layer in value, and the concentration of the doping material is increased in a preset gradient from the central surface of the base material layer to the first contact layer and the second contact layer respectively.
As a further improvement of the invention, the base material layer is made of organic materials and comprises one or more of silane, polymethyl methacrylate and epoxy resin.
As a further improvement of the invention, the doping material comprises one or more of manganese three-phase alloy, anti-perovskite, silicate, tungstate, molybdate, eucryptite, zirconium vanadate and zirconium tungstate.
As a further development of the invention, the concentration of the doping material increases in the interval (0%, 50%).
As a further improvement of the present invention, the thickness of the first contact layer and the second contact layer each range from 0.1 micrometers to 4.0 micrometers.
As a further improvement of the invention, the thickness of the base material layer ranges from 1.0 micrometer to 200.0 micrometers.
As a further improvement of the present invention, the thermal interface material further comprises a heat conducting material uniformly mixed in the base material layer, and the heat conducting material comprises one or more of aluminum nitride, silicon nitride and silicon carbide.
As a further improvement of the invention, a curing agent is further added into the base material layer, and the mass ratio of the curing agent to the base material layer is 1: 1.1-1: 1.4.
As a further improvement of the invention, a surface tension regulator is also added into the base material layer, and the mass percentage of the surface tension regulator is 0.5-6%.
In order to solve the above problems, the present invention also provides a method for preparing a thermal interface material, comprising the following steps:
equally dividing the substrate material into preset parts;
adding a doping material into each part of the substrate material according to a preset gradient concentration;
respectively adding heat conduction materials with equal mass into each part of base material to form a mixed material;
respectively carrying out tape casting on each part of mixed material to form a tape casting film with a preset thickness;
sequentially superposing and attaching each cast film according to the preset gradient concentration to form a semi-finished product;
attaching the surfaces with the lowest concentration of the two semi-finished products to each other, and forming a thermal interface material body after curing;
and respectively coating or pasting low-melting-point alloy on two surfaces of the thermal interface material body to be used as a first contact layer and a second contact layer, and forming the thermal interface material after solidification.
According to the invention, the doping materials are mixed in the substrate material, and the concentrations of the doping materials are respectively increased from the central surface of the substrate material layer to the first contact layer and the second contact layer in a preset gradient mode, so that the thermal deformation difference of organic matters and heat conducting particles is small when the temperature of a heat source of the thermal interface material is high, the phenomenon that the heat conducting capacity is reduced due to the fact that the organic matters and the heat conducting particles are stripped to form internal holes is avoided, the performance of the thermal interface material is stable, and the service life is long.
Drawings
FIG. 1 is a schematic structural diagram of one embodiment of a thermal interface material for a heat spreader according to the present invention;
FIG. 2 is a schematic flow chart illustrating a method for preparing a thermal interface material for a heat spreader according to one embodiment of the present invention;
FIG. 3 is a schematic flow chart illustrating a method for preparing a thermal interface material for a heat spreader according to one embodiment of the present invention;
FIG. 4 is a graph showing the results of testing the thermal interface contact resistance of an embodiment of the method for preparing a thermal interface material for a heat spreader of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Fig. 1 shows an embodiment of the thermal interface material for a heat spreader of the present invention, and referring to fig. 1, in the present embodiment, the thermal interface material includes a base material layer 1, a first contact layer 2, a second contact layer 3, and a doping material 4.
The substrate material layer 1 is made of a positive thermal expansion coefficient material or a negative thermal expansion coefficient material, and the first contact layer 2 covers one surface of the substrate material layer 1 and is in contact with a heat source; the second contact layer 3 covers the other surface of the substrate material layer 1 and is in contact with the radiator; the doping material 4 is mixed in the base material layer 1, the thermal expansion coefficient of the doping material 4 is opposite to the thermal expansion coefficient of the base material layer 1, and the concentration of the doping material 4 is increased in a preset gradient from the central surface of the base material layer 1 to the first contact layer 2 and the second contact layer 3 respectively.
It should be noted that the central plane of the base material layer is a virtual plane passing through the midpoint of the base material layer and parallel to both the upper surface and the lower surface of the base material, and the virtual plane does not necessarily exist actually, and is used to describe that the concentration of the doping material 4 increases in a gradient manner.
Specifically, if the base material layer is made of a positive expansion coefficient material, the doping material is made of a negative expansion coefficient material; if the base material layer is made of a material with a negative expansion coefficient, the doped material is made of a material with a positive expansion coefficient.
Preferably, the sum of the value of the coefficient of expansion of the base material and the value of the coefficient of expansion of the dopant material is about zero to ensure that the thermal interface material does not expand or contract significantly when heated.
Preferably, the concentration of the doping material 4 comprises a first gradient 41(5 wt%), a second gradient 42(10 wt%), a third gradient 43(15 wt%), a fourth gradient 44(20 wt%), a fifth gradient 45(25 wt%).
Specifically, the base material layer 1 is an organic material including one or more of silane, polymethyl methacrylate, and epoxy resin.
Further, the doping material 4 includes one or more of manganese three-phase alloy, anti-perovskite, silicate, tungstate, molybdate, eucryptite, zirconium vanadate, and zirconium tungstate.
Further, the increasing interval of the concentration of the doping material 4 is (0% to 50%).
Further, the thickness of the first contact layer 2 and the second contact layer 3 are both in the range of 0.1 micrometers to 4.0 micrometers.
Further, the thickness of the base material layer 1 ranges from 1.0 micrometer to 200.0 micrometers.
Further, the thermal interface material further comprises a heat conducting material uniformly mixed in the base material layer 1, and the heat conducting material comprises one or more of aluminum nitride, silicon nitride and silicon carbide.
Further, a curing agent is added into the base material layer 1, and the mass ratio of the curing agent to the base material layer 1 is 1: 1.1-1: 1.4.
Further, a surface tension regulator is added into the base material layer 1, and the mass percentage range of the surface tension regulator is 0.5-6%.
This embodiment is through mixing doping material 4 in substrate material layer 1, and the concentration of doping material 4 by substrate material layer 1's central plane respectively to first contact layer 2 second contact layer 3 is and predetermines the gradient and increases progressively, has guaranteed that thermal interface material when the heat source temperature is higher, and the thermal deformation difference of organic matter and heat conduction particle is little, has avoided organic matter and heat conduction particle to take place to peel off and forms inside hole and lead to the heat conduction ability to descend for thermal interface material's stable performance, long service life.
Fig. 2 and 3 show an embodiment of a method for preparing a thermal interface material for a heat spreader according to the present invention, and referring to fig. 2, in this embodiment, the method comprises the following steps:
step S1, respectively adding a curing agent with a first preset mass ratio, a surface tension regulator with a second preset mass ratio and a viscosity regulator with a third preset mass ratio into epoxy resin to form a substrate material.
Step S2, equally dividing the base material into preset parts.
And step S3, adding doping materials into each part of the base material according to the preset gradient concentration.
And step S4, adding heat conduction materials with equal mass into each part of the base material respectively to form a mixed material.
Step S5, casting each part of the mixed material into a casting film with a preset thickness.
And step S6, sequentially superposing and attaching each cast film according to the preset gradient concentration to form a semi-finished product.
And step S7, attaching the surfaces with the lowest concentration of the two semi-finished products to each other, and forming a thermal interface material body after curing.
And step S8, coating low-melting-point alloys as a first contact layer and a second contact layer on the two surfaces of the thermal interface material body respectively, and forming the thermal interface material after solidification.
Specifically, referring to fig. 3, the specific embodiment of the preparation method of the thermal interface material of this embodiment is as follows:
in step S101, the E51 epoxy resin is preferably used as a matrix to ensure that the epoxy resin has substantially better curing performance and better mechanical properties.
And step S102, adding a curing agent MHHPA, and controlling the ratio of the epoxy resin to the curing agent to be 1.1: 1-1.4: 1.
Step S103, adding a surface tension regulator which accounts for 0.5 wt% to 6 wt% of the total mass of the matrix, wherein the surface tension regulator comprises one or more of a cosolvent, a surfactant and a small molecule compound for regulating surface tension. Wherein the small molecular compound for adjusting the surface tension comprises imidazole and derivatives thereof, phenol and hydroquinone.
And step S104, adding a viscosity regulator with the mass fraction content ranging from 0.1% to 5%, wherein the viscosity regulator comprises one or more of alcohol, ether, ester, phenol and amine.
And S105, adding 0.2 to 0.6 weight percent of accelerator 2E4MZ-CN in the total mass of the base to accelerate curing to form the treated epoxy resin.
And step S106, dividing the treated epoxy resin into 5 equal parts.
Step S107, adding 5 wt%, 10 wt%, 15 wt%, 20 wt% and 25 wt% of doping material MnNiGe alloy in the total mass of each part of treated epoxy resin, wherein the doping material also comprises eucryptite (LiAlSiO SiO)4)、ZrV2O7Zirconium vanadate, zirconium tungstate (ZrW)2O8) One or more of (a).
Specifically, the MnNiGe alloy adopts high-purity Mn, Ni and Ge as raw materials, manganese powder, nickel powder and germanium powder are weighed according to a stoichiometric ratio, fully ground and then put into a self-made mold, and a hydraulic press is used for keeping the pressure for 2min under the pressure of 10t to be pressed into tablets. And then placing the sample in a vacuum sintering furnace for sintering under the protection of argon, heating to 800 ℃ at a heating rate of 10 ℃/min, keeping the temperature for 5h, cooling along with the furnace, taking out the sample, placing the sample in a mortar for grinding, tabletting and sintering again, heating to 1000 ℃ at a heating rate of 10 ℃/min, keeping the temperature for 5h, and cooling along with the furnace.
After sintering, the martensite phase transformation causes a large lattice contraction, and the formed MnNiGe is naturally crushed into a powder sample with a large size after being cooled to room temperature.
Further, the obtained powder is placed in a stainless steel ball milling tank (inert protective gas argon is filled in the ball milling tank to prevent the powder from being oxidized), ball milling treatment is carried out, zirconia balls are used as grinding balls (the material ball ratio is 1: 2), absolute ethyl alcohol is used as a ball milling medium, the rotating speed of the ball milling tank is 400 r/min, the ball milling time is 1h, after the ball milling is finished, the material in the ball milling tank is dried in vacuum to remove the absolute ethyl alcohol, the drying condition is-0.1 MPa and 40 ℃, the drying time is 8h, and the dried powder is sieved through a 400-mesh sieve, so that the MnNiGe alloy with a large negative thermal expansion coefficient is obtained.
In addition, LiAlSiO4、ZrV2O7、ZrW2O8Has a negative thermal expansion coefficient, but is higher than that of MnNiGe alloy, and a larger amount is needed to make the mixed material have a thermal expansion coefficient close to 0, but in practical application, a smaller amount is beneficial to maintain the excellent performance of the epoxy resin.
And step S108, adding the doping material and heat conduction material particles SiC accounting for 10 wt% of the total mass at the same time, and mixing in a mixer under a vacuum condition to a completely uniform state.
Preferably, a vacuum state is maintained in the mixing state to allow air bubbles formed during the mixing of the slurry to be discharged.
Step S109, five casting films with the thickness of 10-200 microns are respectively prepared by adopting casting molding: casting film No. 1 with doping material of 5 wt%, casting film No. 2 with doping material of 10 wt%, casting film No. 3 with doping material of 15 wt%, casting film No. 4 with doping material of 20 wt%, and casting film No. 5 with doping material of 25 wt%.
Step S110, superposing each casting film in two opposite directions from low to high according to the mass percent of the doping materials, namely, the concentration of the doping materials is gradually increased towards two sides by taking the extremely low material as the center.
And S111, placing the superposed cast film into a mold, placing the mold into a drying oven at 160 ℃ for curing for 3 hours, and demolding after curing to obtain the thermal interface material body.
Step S112, coating a first contact layer and a second contact layer on two surfaces of the thermal interface material body respectively, wherein the first contact layer and the second contact layer are both low-melting-point materials.
Preferably, the low melting point material is: 52In +48Sn (52 parts indium +48 parts tin-indium-tin alloy, the same applies hereinafter), 80Sn +10Bi +5Zn, 63Sn +37Pb, 91.2Sn +8.8 Zn.
Preferably, the contact layer can be formed by coating, or the alloy can be formed into a sheet and adhered to the mixed material to form the thermal interface material.
Further, in this embodiment, the thermal conductivity of the prepared thermal interface material is tested by using a thermal conductivity tester:
the prepared mixed material is processed into square slices with the size of 25.4 multiplied by 25.4mm, the upper surface and the lower surface are evenly coated with heat conducting paste, then the square slices are placed on a test platform to be pressurized for testing, and the computer automatically captures data of test results. Test 5 samples with an average of 0.83Wm-1K-1And the thermal conductivity of the epoxy resin doped with the same amount of heat conduction material particles SiC at room temperature is only 0.42Wm-1K-1Therefore, the thermal conductivity of the thermal interface material prepared by the scheme is improved by 1 time.
Further, this example also uses a tensile tester to test the shear strength of the prepared thermal interface material:
the thermal interface material for curing is uniformly coated between two steel plates for curing and overlapping, and the overlapping length, the overlapping width and the glue line thickness of the mixed material between the steel plates are respectively kept at 12.5 mm, 25 mm and (0.1-0.5) mm. The average value of 5 samples is 29.63MPa, the shear strength of the epoxy resin doped with the same amount of heat conduction material particles SiC at room temperature is only 7.26MPa, and the shear strength of the thermal interface material prepared by the scheme is improved by nearly 4 times.
Further, in this embodiment, the interface contact thermal resistance of the prepared thermal interface material is also tested by using a steady state method:
respectively simulating a heat source and a heat sink material by using a copper hot plate and a copper cold plate, respectively setting the temperature of temperature sensors at different thickness positions of the copper hot plate and the copper cold plate, and respectively measuring the total heat quantity of a sample passing through an interface heat conduction material and the copper hot plateAnd calculating the interface contact thermal resistance according to the surface temperature of the copper cold plate. The measurement conditions were set as: the thickness of the sample is 0.2mm, the pressure is 0.4MPa, the temperature is 80 ℃, 100 ℃ and 120 ℃, and the test results are respectively as follows: 0.1562K cm2/W、0.1424K·cm2/W、0.1398K·cm2and/W. Under the same conditions, the test results of the epoxy resin doped with the same amount of the heat conducting material particles SiC are as follows: 0.2312K cm2/W、0.2114K·cm2/W、0.2074K·cm2/W。
In order to verify the application reliability of the interface material, an interface contact thermal resistance aging test of 240 hours is carried out on the interface material at a constant temperature of 120 ℃ at a hot end, a sample with the thickness of 0.4mm is adopted for the test, and the pressure of the sample is set to be 0.4 MPa. The test results are shown in FIG. 4.
As shown in FIG. 4, the interface contact resistance of the thermal interface material is stable in 0.225-0.235 Kcm2between/W. Therefore, the thermal interface material of the embodiment has stable and reliable interface contact resistance within a period of 240h at 120 ℃.
The embodiments of the present invention have been described in detail, but the present invention is only exemplary and is not limited to the embodiments described above. It will be apparent to those skilled in the art that any equivalent modifications or substitutions can be made within the scope of the present invention, and thus, equivalent changes and modifications, improvements, etc. made without departing from the spirit and scope of the present invention should be included in the scope of the present invention.
Claims (10)
1. A thermal interface material for transferring heat generated by a heat source to a heat sink, the thermal interface material comprising:
the substrate material layer is made of a positive thermal expansion coefficient material or a negative thermal expansion coefficient material;
the first contact layer covers one surface of the substrate material layer and is in contact with the heat source;
the second contact layer covers the other surface of the substrate material layer and is in contact with the radiator;
the doping material is mixed in the base material layer, the thermal expansion coefficient of the doping material is opposite to that of the base material layer, and the concentration of the doping material is gradually increased from the center face of the base material layer to the first contact layer and the second contact layer in a first gradient of 5 wt%, a second gradient of 10 wt%, a third gradient of 15 wt%, a fourth gradient of 20 wt% and a fifth gradient of 25 wt%; the material of the first contact layer and the second contact layer is one of 52In +48Sn, 80Sn +10Bi +5Zn, 63Sn +37Pb and 91.2Sn +8.8 Zn.
2. A thermal interface material as defined in claim 1, wherein said base material layer is made of an organic material including one or more of silane, polymethylmethacrylate, and epoxy.
3. A thermal interface material as defined in claim 1, wherein the dopant material comprises one or more of a manganese three-phase alloy, an anti-perovskite, a silicate, a tungstate, a molybdate, eucryptite, zirconium vanadate, zirconium tungstate.
4. A thermal interface material as defined in claim 1, wherein the dopant material has an increasing concentration interval of (0%, 50% ].
5. A thermal interface material as defined in claim 1, wherein the first contact layer and the second contact layer each have a thickness in the range of 0.1 microns to 4.0 microns.
6. A thermal interface material as defined in claim 1, wherein said base material layer has a thickness in the range of 1.0 to 200.0 microns.
7. The thermal interface material as claimed in claim 1, further comprising a thermally conductive material uniformly mixed in the base material layer, the thermally conductive material comprising one or more of aluminum nitride, silicon nitride, and silicon carbide.
8. The thermal interface material as claimed in claim 1, wherein a curing agent is further added to the base material layer, and the mass ratio of the curing agent to the base material layer is in the range of 1:1.1 to 1: 1.4.
9. The thermal interface material as claimed in claim 1, wherein a surface tension modifier is further added to the base material layer, and the surface tension modifier is present in an amount ranging from 0.5% to 6% by mass.
10. A preparation method of a thermal interface material is characterized by comprising the following steps:
equally dividing the substrate material into preset parts;
adding a doping material into each part of the substrate material according to a preset gradient concentration;
respectively adding heat conduction materials with equal mass into each part of base material to form a mixed material;
respectively carrying out tape casting on each part of mixed material to form a tape casting film with a preset thickness;
sequentially superposing and attaching each cast film according to the preset gradient concentration to form a semi-finished product;
attaching the surfaces with the lowest concentration of the two semi-finished products to each other, and forming a thermal interface material body after curing;
and respectively coating or pasting low-melting-point alloy on two surfaces of the thermal interface material body to be used as a first contact layer and a second contact layer, and forming the thermal interface material after solidification.
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| CN103548123A (en) * | 2011-05-19 | 2014-01-29 | 莱尔德技术股份有限公司 | Thermal interface materials and methods for processing the same |
| CN106810877A (en) * | 2015-12-02 | 2017-06-09 | 中国科学院金属研究所 | A kind of heat-conducting interface material and its application |
| CN206188727U (en) * | 2016-08-09 | 2017-05-24 | 天津莱尔德电子材料有限公司 | System for thermal interface material subassembly and controllable its surface viscosity that changes |
| CN107722942A (en) * | 2017-11-10 | 2018-02-23 | 苏州环明电子科技有限公司 | Phase transformation high heat conduction boundary material and preparation method thereof |
| CN108336247A (en) * | 2018-01-30 | 2018-07-27 | 武汉华星光电半导体显示技术有限公司 | A kind of OLED encapsulation method and encapsulating structure |
| CN109054302A (en) * | 2018-08-02 | 2018-12-21 | 中国科学院深圳先进技术研究院 | Thermal interfacial material and preparation method thereof |
| CN110776745A (en) * | 2019-10-09 | 2020-02-11 | 苏州欣天新精密机械有限公司 | Preparation method of thermal interface material |
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