CN107987536A - A kind of high heat conductive insulating silica gel piece and preparation method thereof - Google Patents
A kind of high heat conductive insulating silica gel piece and preparation method thereof Download PDFInfo
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- CN107987536A CN107987536A CN201810008568.6A CN201810008568A CN107987536A CN 107987536 A CN107987536 A CN 107987536A CN 201810008568 A CN201810008568 A CN 201810008568A CN 107987536 A CN107987536 A CN 107987536A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/08—Materials not undergoing a change of physical state when used
- C09K5/14—Solid materials, e.g. powdery or granular
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
Abstract
The invention discloses a kind of high heat conductive insulating silica gel piece and preparation method thereof, silica gel piece makees thermal conductivity filler by three kinds of different-grain diameter ball-aluminium oxides.The powder of the low particle diameter of two of which is mixed with high particle diameter again by surface conditioning agent is modified.Base-material is completed plus kneadings such as vinyl silicone oil, containing hydrogen silicone oil, inhibitor, catalyst, base-material is then poured into calender or hydraulic press shaped cut sheets.Such as fruit product needs, different colors, can also add color in accordance with the appropriate ratio.The heat-conducting silica gel sheet volume production, can be applied in the CPU of high cooling requirements, motor, security product etc., there is a huge market demand potential.
Description
Technical field
The present invention relates to a kind of heat conductive silica gel, the insulation of particularly a kind of high thermal conductivity by modified aluminas filling
Silica gel piece and preparation method thereof.
Background technology
With the development of science and technology the application of electronic product is more and more, height operating CPU and high performance motor, battery etc.
Requirement to heat dissipation is also higher and higher, and hot-spot can cause electronic product to crash, the serious danger that can cause to burn and explode
Danger.It is more and more but also with the demand of the material of high thermal conductivity to sealing function can be played.The kind of heat conduction product on the market
Class numerous and complicated, there is heat-conducting silicone grease, heat conductive silica gel, heat conduction mud, heat-conducting glue, conductive graphite piece etc..Heat-conducting silica gel sheet is special due to it
Different performance is come out top, and thermal conductivity factor is mainly determined by conduction powder species and loading, filling mode.High heat conduction powder
Such as aluminium nitride, boron nitride cause industrialization to be subject to serious restriction due to hydrolysis and the unstable of other performance.
The most still alundum (Al2O3) powder of industrial application at present.Since alundum (Al2O3) is subject to the shadow of loading
Ring, the heat-conducting silica gel sheet thermal conductivity factor upper limit is restricted, and the filling thermal conductivity factor of general spherical shape aluminium oxide can only accomplish 4.0W/
M.k or so.Match somebody with somebody in consideration of it, carrying out pole to diameter of particle and surface is modified to improve loading, improve and disperse, so that
The research for improving thermal conductivity factor is very necessary.
The content of the invention
It is an object of the invention to provide a kind of high heat conductive insulating silica gel piece and preparation method thereof, to solve above-mentioned background
The problem of common ball-aluminium oxide proposed in technology is by filling limit, the heat-conducting silica gel sheet thermal conductivity factor upper limit are restricted,
The filling thermal conductivity factor of general spherical shape aluminium oxide can only accomplish 4.0W/m.k or so.
To achieve the above object, the present invention provides following technical solution：
A kind of high heat conductive insulating silica gel piece, is made of the raw material of following weight fraction：Vinyl-based silicone oil 3%~10%,
Methyl Hydrogen Polysiloxane Fluid 0.1%~0.8%, inhibitor 0.01%~0.05%, platinum catalyst 0.2%~0.6%, powder table
Surface treatment agent 0.5%~3.8% (accounts for powder quality percentage), and remainder is conductive powder.
As the further scheme of the present invention：The vinyl-based silicone oil refers to end-vinyl dimethyl silicone polymer
Or end-vinyl Polymethyl methacrylate, vinyl molar content 0.8%~10%；Viscosity 200cs~3000cs.
As the further scheme of the present invention：The Methyl Hydrogen Polysiloxane Fluid refers to viscosity in 1.5-40mm2/ S, it is hydrogeneous
Measure the polysiloxanes between 0.5%~1.65%.
As the further scheme of the present invention：The inhibitor refers to propilolic alcohol, diallyl maleate, acetylene ring
One kind in hexanol.
As the further scheme of the present invention：The platinum catalyst refers to chloroplatinic acid, and concentration range is in 1500ppm
Between~3000ppm.
As the further scheme of the present invention：The surface treatment agent for powder refers to gamma-aminopropyl-triethoxy-silane
(KH-550), vinyl three ('beta '-methoxy ethyoxyl) silane (A-172), hexamethyldisilazane (MMN), three second of vinyl
One kind in oxysilane (A-151).
As the further scheme of the present invention：The conduction powder be particle diameter be 1~10um, 40~50um, 70~
The mixed powder of the full spherical alundum (Al2O3) of 100um.
A kind of production method of high heat conductive insulating silica gel piece, includes the following steps：
(1), it is 1~10um by particle diameter, 40~50um, it is small that 70~100um powders are positioned over baking 24 in 120 DEG C of baking ovens
When；
(2), it is 1~10um powders and 40~50um powders according to 2.0~3.0 by particle diameter:1 ratio premix, with wet method
1~4h is stirred under vacuum after adding surface conditioning agent, surface conditioning agent accounts for powder quality percentage as 0.5%~3.8%.Wherein,
Under vacuum, surface conditioning agent is sufficiently mixed with liquid spray-type with powder；
(3), it is 4%~10% that mass fraction is added in step (2) powder；Vacuum kneading 30 divides after vinyl silicone oil
Clock, the vinyl silicone oil refer to end-vinyl dimethyl silicone polymer or end-vinyl Polymethyl methacrylate or
The mixture of person between the two；Vinyl molar content 0.8%~10%；Viscosity 200cs~3000cs；
(4), the containing hydrogen silicone oil and 0.01% that mass fraction is 0.3%~0.8% is added in mixture in step (3)
Vacuum kneading 10~20 minutes after~0.05% inhibitor, the Methyl Hydrogen Polysiloxane Fluid refer to viscosity in 1.5-40mm2/S,
Polysiloxanes of the hydrogen content between 0.5%~1.65%；
(5), the alundum (Al2O3) powder that particle diameter is 70~100um in step (1) is added in step (4), and vacuum is pinched again
Close 20~30 minutes；
(6), the platinum catalyst vacuum kneading 15~30 that mass fraction is 0.2%~0.6% is added in step (5)
Minute；
(7), the base-material completed will be mediated in step (6) and pours on calender or hydraulic press 110 DEG C~140 DEG C, 10~
20 minutes sulfidization moldings.
Compared with prior art, the beneficial effects of the invention are as follows：
The high heat conductive insulating silica gel for the ball-aluminium oxide filling that the reasonable pole of a kind of particle diameter is matched somebody with somebody and surface was modified
Piece, thermal conductivity factor can bring up to 6.0~8.0W/m.k, breakdown voltage resistant to reach more than 6KV/mm, and tearing strength reaches
0.5KN/m, heat-conducting silica gel sheet volume production, can be applied in the CPU of high cooling requirements, motor, security product etc., and market needs
Ask and have a high potential.
Embodiment
Below in conjunction with the embodiment of the present invention, the technical solution in the embodiment of the present invention is clearly and completely retouched
State, it is clear that described embodiment is only part of the embodiment of the present invention, instead of all the embodiments.Based on the present invention
In embodiment, the every other implementation that those of ordinary skill in the art are obtained without making creative work
Example, belongs to the scope of protection of the invention.
The present embodiment is the preferred embodiment for the present invention, other its all principle and basic structure, color etc. and the present embodiment
It is identical or approximate, within the scope of the present invention.With reference to specific embodiment to high-performance heat conductive insulating silica gel piece
The person that is not specified actual conditions and production method further describes in detail, in embodiment, suggests according to normal condition or manufacturer
Condition carry out.Reagents or instruments used without specified manufacturer, is the conventional production that can be obtained by commercially available purchase
Product.
A kind of high heat conductive insulating silica gel piece, is made of the raw material of following weight fraction：Vinyl-based silicone oil 3%~10%,
The vinyl-based silicone oil refers to end-vinyl dimethyl silicone polymer or end-vinyl Polymethyl methacrylate, second
Alkenyl molar content 0.8%~10%；Viscosity 200cs~3000cs, Methyl Hydrogen Polysiloxane Fluid 0.1%~0.8%, inhibitor
0.01%~0.05%, platinum catalyst 0.2%~0.6%, surface treatment agent for powder 0.5%~3.8% (accounts for powder quality
Fraction), remainder is conductive powder, and the vinyl-based silicone oil refers to end-vinyl dimethyl silicone polymer or end ethene
Base Polymethyl methacrylate, vinyl molar content 0.8%~10%；Viscosity 200cs~3000cs, the methyl
Containing hydrogen silicone oil refers to viscosity in 1.5-40mm2/ S, polysiloxanes of the hydrogen content between 0.5%~1.65%, the suppression
Agent refers to one kind in propilolic alcohol, diallyl maleate, acetylene cyclohexanol, and the platinum catalyst refers to chloroplatinic acid, dense
Scope is spent between 1500ppm~3000ppm, and the surface treatment agent for powder refers to gamma-aminopropyl-triethoxy-silane
(KH-550), vinyl three ('beta '-methoxy ethyoxyl) silane (A-172), hexamethyldisilazane (MMN), three second of vinyl
One kind in oxysilane (A-151), the conduction powder are that particle diameter is 1~10um, and 40~50um's, 70~100um is complete
The mixed powder of global type alundum (Al2O3).
A kind of production method of high heat conductive insulating silica gel piece, includes the following steps：
(1), it is 1~10um by particle diameter, 40~50um, it is small that 70~100um powders are positioned over baking 24 in 120 DEG C of baking ovens
When；
(2), it is 1~10um powders and 40~50um powders according to 2.0~3.0 by particle diameter:1 ratio premix, with wet method
1~4h is stirred under vacuum after adding surface conditioning agent, surface conditioning agent accounts for powder quality percentage as 100.5~3.8%.Wherein,
Under vacuum, surface conditioning agent is sufficiently mixed with liquid spray-type with powder；The specific purposes of step (2) are to match somebody with somebody pole
Powder surface cladding layer of surface inorganic agent afterwards, makes dispersiveness and associativity of the powder in silicone oil more preferably.
(3), it is 4%~10% that mass fraction is added in step (2) powder；Vacuum kneading 30 divides after vinyl silicone oil
Clock, the vinyl silicone oil refer to end-vinyl dimethyl silicone polymer or end-vinyl Polymethyl methacrylate or
The mixture of person between the two；Vinyl molar content 0.8%~10%；Viscosity 200cs~3000cs；
(4), the containing hydrogen silicone oil and 0.01% that mass fraction is 0.3%~0.8% is added in mixture in step (3)
Vacuum kneading 10~20 minutes after~0.05% inhibitor, the Methyl Hydrogen Polysiloxane Fluid refer to viscosity in 1.5-40mm2/S,
Polysiloxanes of the hydrogen content between 0.5%~1.65%；
(5), the alundum (Al2O3) powder that particle diameter is 70~100um in step (1) is added in step (4), and vacuum is pinched again
Close 20~30 minutes；The purpose of high particle diameter powder is not involved in the cladding of surface conditioning agent in step (5) is improved between powder and powder
The reasonability of filling and prevent mucous membrane.
(6), the platinum catalyst vacuum kneading 15~30 that mass fraction is 0.2%~0.6% is added in step (5)
Minute；
(7), the base-material completed will be mediated in step (6) and pours on calender or hydraulic press 110 DEG C~140 DEG C, 10~
20 minutes sulfidization moldings.
Embodiment 1
1. be 5um by particle diameter, 40um, when 80um powders are positioned over that baking 24 is small in 120 DEG C of baking ovens, to remove vapor
With other low boiling impurities；
2. prepare 2kg surface modified powders：
(1), it is that the ball-aluminium oxide that 5um ball-types aluminium oxide is 40um with 606g particle diameters carries out by 1334g particle diameters after drying
Premixing 20 minutes, equipment is micro-powder mixer.
(2), the powder mixed in (1) is taken out to be put into in liquid ejection outlet vacuum kneader.When mediating by second
('beta '-methoxy ethyoxyl) silane of alkenyl three (A-172) 60g is mixed into powder with even spraying formula, when kneading 3 is small.
3. kneader continues to add the vinyl-terminated silicone fluid 106g of 400cs in 2, hydrogen content is 0.5% methyl hydrogen
Silicone oil 10.6g, inhibitor propilolic alcohol 5.3g.Vacuum kneading 20 minutes.
4. kneader continues to add the ball-aluminium oxide 1406g of 80um in 3, continue vacuum kneading 30 and divide 20 clocks.
5. continue to add platinum catalyst 7.1g, vacuum kneading 30 minutes in mixture in 4.Base in order to prevent at this time
Vulcanization is done sth. in advance in material stirring fever to be caused extremely to expect, kneader must take logical cooling water to mediate, and reduce base temperature.
6. base-material in 5 is taken out and pours into five roll calendars the semi-finished product performance to be detected for making thickness 2mm.
Embodiment 2
1. be 10um by particle diameter, 45um, when 100um powders are positioned over that baking 24 is small in 120 DEG C of baking ovens, to remove water steaming
Gas and other low boiling impurities；
2. prepare 2kg surface modified powders：
(1), by 1416g particle diameters after drying be 10um ball-types aluminium oxide with the ball-aluminium oxide that 524g particle diameters are 45um into
Row premixing 20 minutes, equipment is micro-powder mixer.
(2), the powder mixed in (1) is taken out to be put into in liquid ejection outlet vacuum kneader.While mediate while incite somebody to action
Gamma-aminopropyl-triethoxy-silane (KH-550) 60g is mixed into powder with even spraying formula, when kneading 3 is small.
3. kneader continues to add the vinyl-terminated silicone fluid 144g of 400cs in 2, hydrogen content is 0.5% methyl hydrogen
Silicone oil 10.8g, inhibitor propilolic alcohol 5.40g.Vacuum kneading 20 minutes.
4. kneader continues to add the ball-aluminium oxide 1487g of 100um in 3, continue vacuum kneading 15 minutes.
5. continue to add platinum catalyst 7.5g, vacuum kneading 30 minutes in mixture in 4.Base in order to prevent at this time
Vulcanization is done sth. in advance in material stirring fever to be caused extremely to expect, kneader must take logical cooling water to mediate, and reduce base temperature.
6. base-material in 5 is taken out and pours into five roll calendars the semi-finished product performance to be detected for making thickness 2mm.
Performance test
In order to verify the performance of product, following test has been done：
(1) Determination of conductive coefficients
By high heat conductive insulating silica gel piece is on the testing stand of Hotdisk testers made from embodiment 1~2, thickness
Control measures thermal conductivity factor, the results are shown in Table 1, shows there is leading for superelevation between 0.5~3.0mm
Hot coefficient, suitable for the occasion higher to cooling requirements.
(2) burn-in test
1st, degradation 1：It is small in 150 DEG C of bakings 1000 that high heat conductive insulating silica gel piece made from embodiment 1~2 will be prepared
When.
2nd, degradation 2：Will prepare embodiment 1~2 made from high heat conductive insulating silica gel piece at 85 DEG C, 85% humidity bar
Under part, when experiment 1000 is small.
(3) thermal shock is tested
High heat conductive insulating silica gel piece made from embodiment 1~2 is circulated 600 times at -55 DEG C~125 DEG C.
(4) breakdown voltage resistant test
High heat conductive insulating silica gel piece made from embodiment 1~2 is tested into breakdown voltage on resistance to breakdown tester.
(5) tearing strength test
High heat conductive insulating silica gel piece made from embodiment 1~2 is tested on semi-automatic tearing strength test instrument.
Table 1
| Embodiment 1 | Embodiment 2 | |
| Thermal conductivity factor (W/m.k) | 7.19 | 6.81 |
| Thermal resistance (m2.k/w) | 0.000285 | 0.000301 |
| Breakdown voltage (KV) | >6 | >6 |
| Tearing strength (KN/m) | 0.51 | 0.61 |
| Thermal resistance (m after degradation 12.k/w) | 0.000288 | 0.000306 |
| Thermal resistance (m after degradation 22.k/w) | 0.000286 | 0.000304 |
| Thermal resistance (m after thermal shock2.k/w) | 0.000284 | 0.000302 |
It is obvious to a person skilled in the art that the invention is not restricted to the details of above-mentioned one exemplary embodiment, Er Qie
In the case of without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, nothing
By from the point of view of which point, the present embodiments are to be considered as illustrative and not restrictive, and the scope of the present invention is by institute
Attached claim rather than described above limit, it is intended that will fall in the implication and scope of the equivalency of claim
All changes include in the present invention.
Moreover, it will be appreciated that although the present specification is described in terms of embodiments, not each embodiment is only
Comprising an independent technical solution, this narrating mode of specification is only that for clarity, those skilled in the art should
When using specification as an entirety, the technical solutions in the various embodiments may also be suitably combined, forms people in the art
In the other embodiment that member is appreciated that.
Claims (8)
1. a kind of high heat conductive insulating silica gel piece, it is characterised in that be made of the raw material of following weight fraction：Vinyl-based silicone oil 3%
~10%, Methyl Hydrogen Polysiloxane Fluid 0.1%~0.8%, inhibitor 0.01%~0.05%, platinum catalyst 0.2%~0.6%, powder surface
Inorganic agent 0.5%~3.8%（Account for powder quality percentage）, remainder is conductive powder.
2. a kind of high heat conductive insulating silica gel piece according to claim 1, it is characterised in that the vinyl-based silicone oil is
Finger tip vinyldimethicone or end-vinyl Polymethyl methacrylate, vinyl molar content 0.8%~10%；
Viscosity 200cs~3000cs.
3. a kind of high heat conductive insulating silica gel piece according to claim 1, it is characterised in that the Methyl Hydrogen Polysiloxane Fluid is
Refer to viscosity in 1.5-40mm2/ S, polysiloxanes of the hydrogen content between 0.5%~1.65%.
4. a kind of high heat conductive insulating silica gel piece according to claim 1, it is characterised in that the Methyl Hydrogen Polysiloxane Fluid is
Refer to viscosity in 1.5-40mm2/ S, polysiloxanes of the hydrogen content between 0.5%~1.65%.
5. a kind of high heat conductive insulating silica gel piece according to claim 1, it is characterised in that the platinum catalyst refers to
Chloroplatinic acid, concentration range is between 1500ppm~3000ppm.
6. a kind of high heat conductive insulating silica gel piece according to claim 1, it is characterised in that the surface treatment agent for powder is
Refer to gamma-aminopropyl-triethoxy-silane（KH-550）, vinyl three（'beta '-methoxy ethyoxyl）Silane (A-172), hexamethyl two
Silazane（MMN）, vinyltriethoxysilane（A-151）In one kind.
7. a kind of high heat conductive insulating silica gel piece according to claim 1, it is characterised in that the conduction powder is particle diameter
For 1~10um, the mixed powder of the full spherical alundum (Al2O3) of 40~50um, 70~100um.
8. a kind of production method of high heat conductive insulating silica gel piece as claimed in claim 1, it is characterised in that including following step
Suddenly：
（1）, be 1~10um by particle diameter, 40~50um, when 70~100um powders are positioned over that baking 24 is small in 120 DEG C of baking ovens；
（2）, by particle diameter be 1~10um powders and 40~50um powders according to 1.0~5.0:1 ratio premix, is added with wet method
Be stirred under vacuum after surface treatment agent for powder as described in claim 6, surface conditioning agent account for powder quality percentage for 0.5~
3.8%, wherein, under vacuum, surface conditioning agent is sufficiently mixed with liquid spray-type with powder；
（3）, in step（2）Add vacuum kneading after vinyl silicone oil as described in claim 2 in powder, addition according to
Mass fraction addition in claim 1；
（4）, in step（3）Containing hydrogen silicone oil as described in claim 3 is added in middle mixture and such as institute in claim 4
Vacuum kneading after inhibitor is stated, additive amount is added according to the mass fraction in claim 1；
（5）, in step（4）Middle addition step（1）The alundum (Al2O3) powder vacuum kneading again that middle particle diameter is 70~100um；
（6）, in step（5）It is middle to add platinum catalyst vacuum kneading as described in claim 5；
（7）, by step（6）The middle base-material completed of mediating pours into 110 DEG C~140 DEG C shapings on calender or hydraulic press.
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| CN109233287A (en) * | 2018-08-09 | 2019-01-18 | 张剑 | A kind of heat-conducting type electrically insulating silicone rubber gasket |
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| CN111073612A (en) * | 2019-12-31 | 2020-04-28 | 深圳德邦界面材料有限公司 | Resin-free low-permeability oil heat conduction mud and preparation method thereof |
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| CN114573988A (en) * | 2022-04-18 | 2022-06-03 | 闽都创新实验室 | Interface heat management material and preparation method thereof |
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| CN111944498A (en) * | 2020-08-20 | 2020-11-17 | 广东鼎泰新材料科技有限公司 | Heat-conducting gel with ultralow oil extraction amount and high flow rate performance and preparation method thereof |
| CN112552882A (en) * | 2020-12-02 | 2021-03-26 | 上海阿莱德实业股份有限公司 | Single-component muddy interface heat conduction material and application thereof |
| CN114573988A (en) * | 2022-04-18 | 2022-06-03 | 闽都创新实验室 | Interface heat management material and preparation method thereof |
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