CN116265511A - Preparation method and application of inorganic fiber gasket material with high heat conductivity - Google Patents

Preparation method and application of inorganic fiber gasket material with high heat conductivity Download PDF

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CN116265511A
CN116265511A CN202310160015.3A CN202310160015A CN116265511A CN 116265511 A CN116265511 A CN 116265511A CN 202310160015 A CN202310160015 A CN 202310160015A CN 116265511 A CN116265511 A CN 116265511A
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fibers
short
gasket material
short fiber
inorganic
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杨浩然
楚盛
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Guangdong Guangti Leading New Materials Co ltd
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    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/18Manufacture of films or sheets
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    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K5/00Heat-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
    • C09K5/08Materials not undergoing a change of physical state when used
    • C09K5/14Solid materials, e.g. powdery or granular
    • 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
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2375/00Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
    • C08J2375/04Polyurethanes
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
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    • C08K2201/005Additives being defined by their particle size in general
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00Use of ingredients characterised by shape
    • C08K7/02Fibres or whiskers
    • C08K7/04Fibres or whiskers inorganic
    • C08K7/10Silicon-containing compounds

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Abstract

The invention discloses a preparation method and application of a high-heat-conductivity inorganic fiber gasket material, wherein the preparation method comprises the following steps: s1: cutting inorganic fibers into short fibers, and arranging the short fibers in parallel to obtain a short fiber bundle; s2: coating a high molecular polymer on the short fiber bundles to obtain high molecular short fiber bundles; s3: the macromolecule short fiber bundles are stacked and cut after being solidified, and a semi-finished product is obtained; s4: and (5) carrying out post-treatment on the semi-finished product to obtain the finished product. The high-heat-conductivity silicon nitride fiber gasket prepared by the method is simple in preparation method, good in heat conductivity, excellent in insulativity and tensile strength, overcomes the defects of the traditional high-heat-conductivity material, better meets the requirements of practical application, and can be applied to electronic packaging, such as a shell of a circuit built-in chip.

Description

Preparation method and application of inorganic fiber gasket material with high heat conductivity
Technical Field
The invention relates to the technical field of heat conducting strips, and specifically relates to a preparation method and application of a high-heat-conductivity inorganic fiber gasket material, wherein the classification number of the material is C08J 5/18.
Background
With the rapid development of two electronic products, people put higher demands on the performance and service life of the electronic products, and thermal management becomes one of the great problems in the development of the electronic product industry. If the heat conducting and radiating material is not good, the performance of the electronic product is greatly reduced, and the service life of the electronic product is shortened. In most high power electronics, heat is dissipated by the heat sink, but the rigidity of the chip and the heat sink both prevent full contact and create a large number of wavy, concave-convex air gaps between the interfaces. These gaps greatly impede heat transfer between the mating surfaces. There is therefore a need for efficient heat dissipation using a thermally conductive interface material (TIM) to efficiently transfer a heat source to a heat sink.
In the prior art, in order to improve the heat conducting performance of the silicone rubber/gel gasket, a composite material is generally formed by using a plurality of heat conducting fillers such as metal, ceramic, carbon nano tube, graphene, boron nitride and the like, but the following problems occur, because of the high interface thermal resistance between the gel and the heat conducting filler, the heat conducting performance is reduced to a certain extent, and in addition, if the filler content is further increased, the mechanical performance of the heat conducting gasket is reduced.
Silicon nitride fiber has advantages such as insulating nature is good, mechanical strength is high, the wearability is good, coefficient of thermal expansion is low, thermal conductivity is good, is widely used as the raw and other materials of TIMs, but under the general circumstances, the fibre can not vertically arrange along the horizontal direction to the arrangement between fibre and the fibre is inseparable, and fibre heat conduction gasket surface is uneven, and then makes heat conductivility greatly reduced.
Patent CN112409798A discloses a high thermal conductivity gasket and a preparation method thereof, and after aluminum oxide and liquid silicone rubber are solidified and formed by a vacuum resin transfer process, the overall thermal conductivity of the material is improved, but the problem of mechanical properties of the thermal conductivity gasket is not solved.
Disclosure of Invention
In order to solve the above problems, the first aspect of the present invention provides a method for preparing an inorganic fiber gasket material with high heat conductivity, comprising the following steps:
s1: cutting inorganic fibers into short fibers, bundling the short fibers into a bundle, and simultaneously arranging the fibers in parallel to obtain a short fiber bundle with the thickness of 0.1-0.5 mm;
s2: coating a high molecular polymer on the short fiber bundles to fully infiltrate each short fiber, and naturally solidifying for 1-1.5h to obtain the high molecular short fiber bundles;
s3: and (3) bonding the polymer short fiber bundles and the other polymer short fiber bundles in parallel, sequentially repeating the steps, stacking the polymer short fiber bundles layer by layer, naturally curing for 0.5-1h, and longitudinally cutting to obtain a semi-finished product.
S4: soaking the semi-finished product with 15-20mL of sol for 5-10min, ultrasonically washing with deionized water for 10-20min, naturally drying, and polishing the surface to be smooth.
Preferably, the mass ratio between the inorganic fiber and the high molecular polymer is (3-6): (4-6).
Further preferably, the mass ratio between the inorganic fiber and the high molecular polymer is (3-5): (4-6).
Further preferably, the mass ratio between the inorganic fiber and the high molecular polymer is 4:5.
preferably, the inorganic fibers include at least one of glass fibers, ceramic fibers, boron fibers, and carbon fibers.
Further preferably, the inorganic fibers are ceramic fibers including at least one of quartz fibers, silicon carbide fibers, zirconia fibers, alumina fibers, and silicon nitride fibers.
Further preferably, the ceramic fiber is a silicon nitride fiber.
Preferably, the inorganic fibers have a diameter of 1 to 5 μm.
Further preferably, the inorganic fibers have a diameter of 2 to 4. Mu.m.
Further preferably, the inorganic fiber has a diameter of 3 μm.
Preferably, the high molecular polymer comprises at least one of epoxy resin, phenolic resin, furfural resin, polyurethane, acrylic resin, polybutene and organic silica gel.
Further preferably, the high molecular polymer is polyurethane.
Preferably, the length of the short fiber in the step S1 is 5-10cm.
Further preferably, the length of the short fibers in the step S1 is 6-8cm.
Further preferably, the length of the short fiber in the step S1 is 7cm.
Preferably, the number of the short fibers in the short fiber bundles in the step S1 is 20-35.
Further preferably, the number of the short fibers in the short fiber bundles in the step S1 is 25 to 35.
Further preferably, the number of the short fibers in the short fiber bundles in the step S1 is 30.
Preferably, the thickness of the polymer staple fiber bundles in the step S2 is 0.1-0.5mm.
Further preferably, the thickness of the polymer staple fiber bundles in the step S2 is 0.2-0.4mm.
Further preferably, the thickness of the polymer staple fiber bundles in the step S2 is 0.3mm.
Preferably, the thickness of the semi-finished product in the step S3 is 0.5-1.5mm.
Further preferably, the thickness of the semi-finished product in the step S3 is 0.8-1.2mm.
Further preferably, the thickness of the semi-finished product in the step S3 is 1mm.
The invention provides an application of a preparation method of a high-heat-conductivity silicon nitride fiber gasket material in electronic products.
The applicant found that when the mass ratio between the silicon nitride fiber and the polyurethane is (3-6): (4-6) improving the heat conduction property of the gasket material, and supposing that: when the amount of the silicon nitride fibers is small, the silicon nitride fibers are in discrete distribution in the high polymer, the silicon nitride fibers are distributed in the high polymer in an isolated manner, the mutual effect is not generated, the heat conducting performance is reduced, the silicon nitride fibers are in synergistic effect along with the increase of the filling amount, and overlap joint to form a heat conducting passage, at the moment, the heat conducting performance of the heat conducting gasket is obviously improved, but if the content of the silicon nitride fibers is too high, the cross-linking density among the high molecules is reduced, so that the tensile strength is reduced to a certain extent, and in order to obtain more heat conducting performance, the applicant further limits the thickness of the high polymer fiber bundles to be 0.2-0.4mm, the number of the short fibers to be 25-35, the heat conducting performance is ensured, meanwhile, the tensile strength is improved, and presumably, polyurethane and the silicon nitride fibers form a three-dimensional reticular elastomer structure after solidification, the fibers are tightly arranged, and meanwhile, the tensile strength is improved.
The beneficial effects are that: the preparation method of the high-heat-conductivity silicon nitride fiber gasket is simple, the silicon nitride fibers in the prepared heat-conductivity gasket have high directionality, the silicon nitride fibers are closely arranged, the heat conducting performance of the high-heat-conductivity silicon nitride fiber gasket is improved, in addition, the high-heat-conductivity silicon nitride fiber gasket conducts heat longitudinally, so that transverse heat accumulation is avoided, the high-heat-conductivity silicon nitride fiber gasket also has excellent insulativity and tensile strength, the defects of the traditional high-heat-conductivity material are overcome, the requirements of practical application are better met, and the high-heat-conductivity silicon nitride fiber gasket can be applied to electronic packaging such as a shell of a circuit built-in chip.
Examples
Example 1
A preparation method of a high-heat-conductivity inorganic fiber gasket material comprises the following steps:
s1: cutting inorganic fibers into short fibers with the length of 7cm, bundling 30 short fibers into a bundle, and arranging the fibers in parallel to obtain a short fiber bundle;
s2: coating a high polymer on the short fiber bundles, wherein the coating thickness is 50 mu m, so that each short fiber is fully soaked, and naturally solidifying for 1h to obtain the high polymer short fiber bundles with the thickness of 0.3 mm;
s3: and (3) bonding the polymer short fiber bundles and the other polymer short fiber bundles in parallel, sequentially repeating the steps, stacking the polymer short fiber bundles layer by layer, naturally curing for 1h, and longitudinally cutting to obtain a semi-finished product with the thickness of 1mm.
S4: soaking the semi-finished product with 20mL of sol for 8min, ultrasonically washing with deionized water for 15min, naturally drying, and polishing the surface to be smooth.
The inorganic fiber is silicon nitride fiber with the diameter of 3 mu m, and is purchased from Fu-established new material Co., ltd, and the model is 03.
The high polymer is polyurethane, and is purchased from Dongli (Dongguan) new material technology Co., ltd, and the model is JL-6039.
The mass ratio of the silicon nitride fiber to the polyurethane is 4:5.
example 2
A preparation method of a high-heat-conductivity inorganic fiber gasket material comprises the following steps:
s1: cutting inorganic fibers into short fibers with the length of 7cm, bundling 30 short fibers into a bundle, and arranging the fibers in parallel to obtain a short fiber bundle;
s2: coating a high polymer on the short fiber bundles, wherein the coating thickness is 50 mu m, so that each short fiber is fully soaked, and naturally solidifying for 1h to obtain the high polymer short fiber bundles with the thickness of 0.3 mm;
s3: and (3) bonding the polymer short fiber bundles and the other polymer short fiber bundles in parallel, sequentially repeating the steps, stacking the polymer short fiber bundles layer by layer, naturally curing for 1h, and longitudinally cutting to obtain a semi-finished product with the thickness of 1mm.
S4: soaking the semi-finished product with 20mL of sol for 8min, ultrasonically washing with deionized water for 15min, naturally drying, and polishing the surface to be smooth.
The inorganic fiber is silicon nitride fiber with the diameter of 3 mu m, and is purchased from Fu-established new material Co., ltd, and the model is 03.
The high polymer is polyurethane, and is purchased from Dongli (Dongguan) new material technology Co., ltd, and the model is JL-6039.
The mass ratio of the silicon nitride fiber to the polyurethane is 3:4.
example 3
A preparation method of a high-heat-conductivity inorganic fiber gasket material comprises the following steps:
s1: cutting inorganic fibers into short fibers with the length of 7cm, bundling 25 short fibers into a bundle, and arranging the fibers in parallel to obtain a short fiber bundle;
s2: coating a high polymer on the short fiber bundles, wherein the coating thickness is 50 mu m, so that each short fiber is fully soaked, and naturally solidifying for 1h to obtain the high polymer short fiber bundles with the thickness of 0.4 mm;
s3: and (3) bonding the polymer short fiber bundles and the other polymer short fiber bundles in parallel, sequentially repeating the steps, stacking the polymer short fiber bundles layer by layer, naturally curing for 1h, and longitudinally cutting to obtain a semi-finished product with the thickness of 1mm.
S4: soaking the semi-finished product with 20mL of sol for 8min, ultrasonically washing with deionized water for 15min, naturally drying, and polishing the surface to be smooth.
The inorganic fiber is silicon nitride fiber with the diameter of 3 mu m, and is purchased from Fu-established new material Co., ltd, and the model is 03.
The high polymer is polyurethane, and is purchased from Dongli (Dongguan) new material technology Co., ltd, and the model is JL-6039.
The mass ratio of the silicon nitride fiber to the polyurethane is 4:5.
example 4
A preparation method of a high-heat-conductivity inorganic fiber gasket material comprises the following steps:
s1: cutting inorganic fibers into short fibers with the length of 7cm, bundling 30 short fibers into a bundle, and arranging the fibers in parallel to obtain a short fiber bundle;
s2: coating a high polymer on the short fiber bundles, wherein the coating thickness is 50 mu m, so that each short fiber is fully soaked, and naturally solidifying for 1h to obtain the high polymer short fiber bundles with the thickness of 0.2 mm;
s3: and (3) bonding the polymer short fiber bundles and the other polymer short fiber bundles in parallel, sequentially repeating the steps, stacking the polymer short fiber bundles layer by layer, naturally curing for 1h, and longitudinally cutting to obtain a semi-finished product with the thickness of 1mm.
S4: soaking the semi-finished product with 20mL of sol for 8min, ultrasonically washing with deionized water for 15min, naturally drying, and polishing the surface to be smooth.
The inorganic fiber is silicon nitride fiber with the diameter of 3 mu m, and is purchased from Fu-established new material Co., ltd, and the model is 03.
The high polymer is polyurethane, and is purchased from Dongli (Dongguan) new material technology Co., ltd, and the model is JL-6039.
The mass ratio of the silicon nitride fiber to the polyurethane is 6:6.
comparative example 1
The mass ratio between the silicon nitride fiber and polyurethane is changed to 4:2, the thickness of the polymer short fiber bundles was changed to 0.1mm, and the procedure of example 1 was repeated.
Comparative example 2
The procedure of example 1 was repeated except that the thickness of the polymer staple fiber bundles was changed to 0.6mm, the number of the staple fibers was changed to 15.
Comparative example 3
The mass ratio between the silicon nitride fiber and polyurethane is changed to 1:5, the number of short fibers was changed to 40, and the rest was the same as in example 1.
Evaluation of Performance
(1) Measurement of thermal conductivity: the thermal conductivity measurements were performed for examples 1-4 and comparative examples 1-3 using a TIM Tester 1400 material thermal resistance thermal conductivity Tester from ANALYSIS TECH, U.S. A.A., with test standard ASTM D5470, and the test data are given in Table 1 below.
(2) Determination of tensile Strength: examples 1-4 and comparative examples 1-3 were tested according to the methods described in standard ASTM D638-2010, with test data as in table 1 below.
TABLE 1
Figure BDA0004093781150000061
Figure BDA0004093781150000071

Claims (10)

1. The preparation method of the inorganic fiber gasket material with high heat conductivity is characterized by comprising the following steps:
s1: cutting inorganic fibers into short fibers, and arranging the short fibers in parallel to obtain a short fiber bundle;
s2: coating a high molecular polymer on the short fiber bundles to obtain high molecular short fiber bundles;
s3: stacking and cutting the macromolecule short fiber bundles to obtain a semi-finished product;
s4: and (5) carrying out post-treatment on the semi-finished product to obtain the finished product.
2. The method for preparing a high thermal conductivity inorganic fiber gasket material according to claim 1, wherein the mass ratio between the inorganic fiber and the high molecular polymer is (3-6): (4-6).
3. The method of making a highly thermally conductive inorganic fibrous gasket material of claim 1 wherein said inorganic fibers comprise at least one of glass fibers, ceramic fibers, boron fibers and carbon fibers.
4. The method for preparing a high thermal conductivity inorganic fiber gasket material according to claim 1, wherein the diameter of the inorganic fiber is 1-5 μm.
5. The method for preparing a high thermal conductivity inorganic fiber gasket material according to claim 1, wherein said high molecular polymer comprises at least one of epoxy resin, phenolic resin, furfural resin, polyurethane, acrylic resin, polybutene and silicone.
6. The method for preparing a high thermal conductivity inorganic fiber gasket material according to claim 1, wherein the length of the short fiber in the step S1 is 5-10cm.
7. The method for preparing a high thermal conductivity inorganic fiber gasket material according to claim 1, wherein the number of short fibers in the short fiber bundles in the step S1 is 20-35.
8. The method for preparing a high thermal conductivity inorganic fiber gasket material according to claim 1, wherein the thickness of the polymer short fiber bundles in the step S2 is 0.1-0.5mm.
9. The method for preparing a high thermal conductivity inorganic fiber gasket material according to claim 1, wherein the thickness of the semi-finished product in the step S3 is 0.5-1.5mm.
10. Use of a method for the preparation of a highly thermally conductive inorganic fibrous gasket material according to any one of claims 1 to 9 in an electronic product.
CN202310160015.3A 2023-02-24 2023-02-24 Preparation method and application of inorganic fiber gasket material with high heat conductivity Pending CN116265511A (en)

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