CN110157389A - A kind of high intensity heat conductive silica gel gasket and preparation method thereof - Google Patents

A kind of high intensity heat conductive silica gel gasket and preparation method thereof Download PDF

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Publication number
CN110157389A
CN110157389A CN201910222687.6A CN201910222687A CN110157389A CN 110157389 A CN110157389 A CN 110157389A CN 201910222687 A CN201910222687 A CN 201910222687A CN 110157389 A CN110157389 A CN 110157389A
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carbon fiber
weight
parts
gasket
coupling agent
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CN110157389B (en
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刘斌
淮秀兰
周敬之
李勋锋
胡玄烨
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Zhongke Heat Technology Jiangsu Co ltd
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Institute of Engineering Thermophysics of CAS
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B60VEHICLES IN GENERAL
    • B60LPROPULSION OF ELECTRICALLY-PROPELLED VEHICLES; SUPPLYING ELECTRIC POWER FOR AUXILIARY EQUIPMENT OF ELECTRICALLY-PROPELLED VEHICLES; ELECTRODYNAMIC BRAKE SYSTEMS FOR VEHICLES IN GENERAL; MAGNETIC SUSPENSION OR LEVITATION FOR VEHICLES; MONITORING OPERATING VARIABLES OF ELECTRICALLY-PROPELLED VEHICLES; ELECTRIC SAFETY DEVICES FOR ELECTRICALLY-PROPELLED VEHICLES
    • B60L58/00Methods or circuit arrangements for monitoring or controlling batteries or fuel cells, specially adapted for electric vehicles
    • B60L58/10Methods or circuit arrangements for monitoring or controlling batteries or fuel cells, specially adapted for electric vehicles for monitoring or controlling batteries
    • B60L58/24Methods or circuit arrangements for monitoring or controlling batteries or fuel cells, specially adapted for electric vehicles for monitoring or controlling batteries for controlling the temperature of batteries
    • B60L58/26Methods or circuit arrangements for monitoring or controlling batteries or fuel cells, specially adapted for electric vehicles for monitoring or controlling batteries for controlling the temperature of batteries by cooling
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
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    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/006Combinations of treatments provided for in groups C09C3/04 - C09C3/12
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    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/06Treatment with inorganic compounds
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/10Treatment with macromolecular organic compounds
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/12Treatment with organosilicon compounds
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • 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
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00Secondary cells; Manufacture thereof
    • H01M10/05Accumulators with non-aqueous electrolyte
    • H01M10/052Li-accumulators
    • H01M10/0525Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00Secondary cells; Manufacture thereof
    • H01M10/60Heating or cooling; Temperature control
    • H01M10/61Types of temperature control
    • H01M10/613Cooling or keeping cold
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00Secondary cells; Manufacture thereof
    • H01M10/60Heating or cooling; Temperature control
    • H01M10/62Heating or cooling; Temperature control specially adapted for specific applications
    • H01M10/625Vehicles
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    • 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
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage using batteries
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02TCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO TRANSPORTATION
    • Y02T10/00Road transport of goods or passengers
    • Y02T10/60Other road transportation technologies with climate change mitigation effect
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Abstract

The invention discloses a kind of high-intensitive heat conductive silica gel gaskets and preparation method thereof, suitable for fields such as new energy heat dissipation of lithium batteries, it is realized by using the volatilizable retarder thinner of organic and coupling agent modified to the infiltration dispersion of carbon fiber powder body material and surface, carbon fiber dispersion liquid is brushed in substrate carrier upper surface, with the volatilization of organic retarder thinner, the arrangement for being parallel to heat-conducting pad plane can be presented in carbon fiber, the carbon fibre material high thermal conductivity upward along fiber axis is played, makes gasket that there is good soakage function on gasket in-plane.The carbon fibre material of oriented alignment can play similar skeleton invigoration effect, greatly improve the mechanical performances such as stretching and the tearing of gasket.During high temperature vulcanized, carbon fiber surface can generate cross-linking reaction with containing hydrogen silicone oil and gasket surface vinyl with the coupling agent containing unsaturated group of chemical bonds, to realize the secured connection of layer of carbon fiber material and gasket, process convenient for subsequent calendering.

Description

A kind of high intensity heat conductive silica gel gasket and preparation method thereof
Technical field
The invention belongs to thermal interfacial material fields, are related to a kind of heat conductive silica gel gasket, and in particular to one kind has high intensity Heat conductive silica gel gasket and preparation method thereof, can be widely applied to the fields such as heat dissipation of lithium battery.
Background technique
In new-energy automobile field, lithium battery group can generate a large amount of waste heat when working, will if cannot distribute in time It is light then cause the lithium battery group service life decline, explosion or burning are even resulted in when serious, therefore the heat management of power battery pack is just shown It obtains of crucial importance.Heat conductive silica gel gasket has played key effect in new-energy automobile heat dissipation of lithium battery technology, battery can be produced Raw heat is effectively conducted to liquid cooling plate, while guaranteeing the consistency of battery pack temperature.In addition, heat conductive silica gel gasket can also buffer The impact force that battery pack is subject to plays the role of antidetonation shock attenuation, protects battery cell.Therefore, for lithium battery group thermal conductive silicon Glue gasket will also have certain mechanical strength other than needing good thermally conductive and soaking performance, avoid using a period of time Afterwards, phenomena such as softening, creep and stress relaxation occurs.
Discovery is investigated and furtherd investigate extensively by inventor, and thermal conductive silicon rubber mat is mainly by organosilicon high score at present A large amount of spherical or irregular shape conduction powder fillers are added in son to hand over to form effective thermal conducting path using high temperature The characteristics of connection is solidified to form, and heating conduction shows isotropism is not well positioned to meet lithium battery under high heat flux density The temperature uniformity requirement of group, while when powder is under high filler loading capacity, the stretching of heat-conducting pad and tearing strength are decreased obviously, and are made With being easy to produce breakage in the process.
Carbon fiber is a kind of new fiber materials of phosphorus content 95% or more, it is by organic fibre such as flake graphite Dimension is piled up along fiber axial direction, through microcrystalline graphite material obtained from carbonization and graphitization processing, therefore in fiber axis There is extraordinary heat-conductive characteristic to direction, thermal coefficient may be up to 900W/mK.Carbon fiber guiding hot property and direction are direct Correlation, therefore how to realize that its oriented alignment in heat-conducting pad becomes difficult point.It is existing to be added using the method being commonly blended The thermal conductivity of heat-conducting pad can be improved in carbon fibre material, but since carbon fibre material arranges disorderly and unsystematic, thermal conductivity and pad Piece strength character is promoted limited.It is existing to use woven in advance carbon cloth or carbon fiber layer as sandwich material and heat conductive pad Piece combines, and there are carbon cloth or carbon fiber layer and gasket organosilicon macromolecule thermal contact resistance are big, adhesive strength deficiency, finished product is not The high disadvantage of yield.
Summary of the invention
In view of the above problems in the prior art, the present invention provides a kind of high-intensitive heat conductive silica gel gasket product and its preparation side Method can be widely applied to the fields such as heat dissipation of lithium battery, using carbon fibre material oriented alignment and with silicagel pad composite forming technology, Infiltration dispersion good to carbon fiber powder body material and surface are realized by using the volatilizable retarder thinner of organic and coupling agent It is modified.Gained carbon fiber dispersion liquid is brushed in substrate carrier upper surface, and with the volatilization of organic retarder thinner, carbon fiber can be in It is now parallel to the arrangement of heat-conducting pad plane, the carbon fibre material high thermal conductivity upward along fiber axis is played, gasket is made to exist There is good soakage function on gasket in-plane.Meanwhile can to play similar skeleton strong for the carbon fibre material of oriented alignment Change effect, greatly improves the mechanical performances such as stretching and the tearing of gasket.During high temperature vulcanized, carbon fiber surface is with chemistry Cross-linking reaction can be generated with containing hydrogen silicone oil and gasket surface vinyl by being bonded the coupling agent containing unsaturated group closed, thus It realizes the secured connection of layer of carbon fiber material and gasket, is processed convenient for subsequent calendering, this method is easy to operate, is suitble to extensive work Industry metaplasia produces.
The present invention is to solve its technical problem, used technical solution are as follows:
A kind of preparation method of high intensity heat conductive silica gel gasket, which is characterized in that the preparation method includes following sequence Step:
SS1. by conduction powder filler, heat drying, removing excessive moisture obtain dry conduction powder under vacuum conditions Filler;
SS2. by the drying conduction powder filler prepared in step SS1 and methyl vinyl silicon oil, containing hydrogen silicone oil, coupling Agent, inhibitor and catalyst are according to 50~800 parts by weight: 12~35 parts by weight: 2~6 parts by weight: 0.5~6 parts by weight: 0.5~ 3 parts by weight: room temperature stirs at low speed uniformly mixed, obtained mixing paste base-material to the ratio of 0.3~2 parts by weight under vacuum conditions;
SS3. by a part of calendering formation of the mixing paste base-material prepared in step SS2, the gasket after calendering formation is thick Degree is the 1/5~4/5 of target heat conductive silica gel gasket products thickness, and molding by high temperature vulcanization is to get basic gasket;
SS4. by carbon fiber powder, containing hydrogen silicone oil, organic is volatilizable retarder thinner, catalyst, inhibitor and coupling agent According to 50~100 parts by weight: 3~5 parts by weight: 50~300 parts by weight: 0.2~1 parts by weight: 0.5~2 parts by weight: 0.5~4 weight High-speed stirred is uniformly mixed the ratio of amount part at normal temperature, is completely dispersed uniformly to carbon fiber powder, is obtained carbon fiber dispersion liquid;
SS5. substrate is used as using basic gasket prepared by step SS3, carbon fiber dispersion liquid brushing prepared by step SS4 in The upper surface of substrate carrier is heated to the volatilizable retarder thinner volatilization of organic completely, so that carbon fiber is on substrate carrier surface It is upper to arrange (being parallel to x/y plane) in rules orientation, while being adsorbed on the coupling agent containing vinyl groups of carbon fiber surface It crosslinks and reacts with unsaturated group in substrate carrier and containing hydrogen silicone oil, carbon fiber layer is made to be firmly attached to substrate carrier table Face, it is preferable that in order to increase soaking and the reinforcing effect of carbon fiber, SS5 step can be repeated several times, to increase carbon fiber arrangement layer Thickness;
SS6. the heat-conducting pad of oriented alignment carbon fiber layer will be attached with obtained by step SS5 as substrate, it will be in step SS2 Remaining mixing paste base-material of preparation presses on substrate, and molding by high temperature vulcanization, obtains having both with high mechanical strength and lead The target heat conductive silica gel gasket product of heat and soaking performance.The heat conductive silica gel gasket product is in addition in a z-direction (perpendicular to thermally conductive Gasket plane) have except heating conduction, the direction xy (being parallel to heat-conducting pad plane) since there are oriented alignment carbon fibers Layer, therefore there is splendid soaking performance.And since carbon fiber aligns the reinforcing character of similar skeleton, gained gasket is drawn Mind, tearing strength can significantly improve.
Preferably, in step SS1, the heating temperature of conduction powder filler is 120 DEG C, Shi Changwei 1~2 hour.
Preferably, in step SS1, conduction powder filler can be spherical or irregular shape metal, metal oxide or Mixture between them, it is further preferred that conduction powder filler is aluminium oxide or Zinc oxide powder, partial size is 1~100 μm, when filling out Material granularity be lower than preferred value, cause base-material thixotropy increase, can not calendering formation, when filler particle size be higher than preferred value, gained pad Piece thermal resistance is excessively high.
Preferably, it in step SS2, is stirred at low speed using planetary mixer, 500~1000 revs/min of mixing speed, Mixing time 30~80 minutes.
Preferably, in step SS2, the range of viscosities of methyl vinyl silicon oil is 30~2000mPas, works as silicon oil viscosity Gained gasket hardness is too big when lower than preferred scope, will lead to the sticky mistake of lotion base-material when silicon oil viscosity is higher than preferred scope It is difficult to calendering formation greatly.
Preferably, in step SS2, containing hydrogen silicone oil plays crosslinking curing, hydrogeneous mass fraction in heat conductive silica gel gasket Range is 0.05%~0.3%, when hydrogeneous mass fraction is higher than preferred scope, gained gasket toughness decline, when hydrogeneous quality point Number is lower than preferred scope, and base-material can not vulcanize.
Preferably, step SS2, in SS4, coupling agent is silane coupling agent, silane coupling agent type be containing vinyl groups, Such as vinyltrimethoxysilane, vinyl triethoxyl, vinyl silane triisopropoxide coupling agent, γ-methacryl Oxygroup propyl trimethoxy silicane and γ-(the third oxygen of 2,3- epoxy) propyl trimethoxy silicane etc. have the coupling of unsaturated group Agent.
Preferably, step SS2, in SS4, inhibitor is ethynylcyclohexanol.
Preferably, step SS2, in SS4, catalyst is the platinum catalyst of concentration 2000ppm.
Preferably, in step SS3, when high temperature vulcanized molding, curing temperature is 110~150 DEG C, 30~50 points of vulcanization time Clock.
Preferably, in step SS4, using planetary mixer carry out high-speed stirred, 3000~10000 revs/min of mixing speed Clock, mixing time 60~100 minutes.
Preferably, in step SS4, containing hydrogen silicone oil plays viscous in the combination of oriented alignment carbon fiber and heat conductive silica gel gasket Knot effect, hydrogeneous mass fraction range are 0.5%~2.5%, when hydrogeneous mass fraction is higher than preferred scope, the adhesive layer of formation Excessive high hardness influences gasket flexibility, and when hydrogeneous mass fraction is lower than preferred scope, adhesion strength is inadequate.
Preferably, in step SS4, organic is volatilizable decentralized medium of the retarder thinner as carbon fiber powder is and hydrogeneous Silicone oil has excellent compatibility, and boiling point is 50~80 DEG C of ranges, is not particularly limited, such as: methyl ethyl ketone, n-hexane, tetrachloro Change carbon, isohexane etc., when the volatilizable retarder thinner boiling point of organic is lower than 50 DEG C, because of volatilization in mechanical stirring dispersion process Too fast carbon fiber powder surface modification and dispersion are insufficient.When the volatilizable retarder thinner boiling point of machine class is higher than 80 DEG C, because of volatilization Required temperature is excessively high, influences the adhesion strength of carbon fiber Yu thermal conductive silicon rubber mat.
Preferably, in step SS4, carbon fiber powder, 5~20 μm of filament diameter, length is 50~1000 μm, works as carbon fiber Diameter is less than preferred value, and fiber is limited to the reinforcing effect of gasket, and when fibre diameter is greater than preferred value, axial direction thermal conductivity goes out Now it is decreased obviously.When carbon fiber length is less than preferred value, specific surface area increases sharply, dispersion effect decline, while axial thermal conductivity Thermal resistance increases, and the equal thermal effect decline of gained gasket, when fibre length is greater than preferred value, fiber is easy to appear curved in process Phenomena such as complications are disconnected, influences the equal thermal effect of gasket and mechanical strength.
Preferably, in step SS5, heating temperature is 100~130 DEG C, heating time 20~50 minutes.
Preferably, in step SS6, when high temperature vulcanized molding, curing temperature is 110~150 DEG C, 30~50 points of vulcanization time Clock.
Another technical purpose of the invention is to provide a kind of high-intensitive thermal conductive silicon obtained using above-mentioned preparation method Rubber mat sheet articles, which is characterized in that the component utilized in preparation process is as follows:
(A) 12~35 parts by weight of methyl vinyl silicon oil;
(B) 5~8 parts by weight of containing hydrogen silicone oil;
(C) 1~10 parts by weight of coupling agent;
(D) 0.5~3 parts by weight of catalyst;
(E) 50~800 parts by weight of conduction powder filler;
(F) volatilizable 50~300 parts by weight of retarder thinner of organic;
(G) 50~100 parts by weight of carbon fiber powder;
(H) 1~5 parts by weight of inhibitor.
High-intensitive heat conductive silica gel gasket product of the invention and preparation method thereof, the beneficial effect is that:
Compared with prior art, high-intensitive heat conductive silica gel gasket product and preparation method thereof of the invention, by using having Machine class is volatilizable retarder thinner and coupling agent realization infiltration dispersion good to carbon fiber powder body material and surface are modified.Gained carbon The construction of brushing can be used in substrate carrier upper surface in fiber dispersion, and with the volatilization of organic retarder thinner, carbon fiber can Presentation is parallel to the arrangement in heat-conducting pad plane (direction xy), plays the carbon fibre material high-termal conductivity upward along fiber axis Can, make gasket that there is good soakage function on gasket in-plane.Meanwhile the carbon fibre material of oriented alignment can play Similar skeleton invigoration effect, greatly improves the mechanical performances such as stretching and the tearing of gasket.During high temperature vulcanized, carbon fiber Surface can generate friendship with containing hydrogen silicone oil and gasket surface vinyl with the coupling agent containing unsaturated group of chemical bonds Connection reaction is processed to realize the secured connection of layer of carbon fiber material and gasket convenient for subsequent calendering, and this method is easy to operate, It is suitble to large-scale industrial production.
Specific embodiment
To make the objectives, technical solutions, and advantages of the present invention more comprehensible, following example 1~2 and reference examples 1~ 3 for being described in more detail the present invention:
Embodiment 1
The component that high-intensitive heat conductive silica gel gasket product of the invention utilizes during the preparation process is as follows: (A) ethylene methacrylic 20 parts by weight of base silicone oil, viscosity 400mPas;(B) 6 parts by weight of containing hydrogen silicone oil, hydrogen content 0.1%;(C) γ-(2,3- epoxy Third oxygen) 4 parts by weight of propyl trimethoxy silicane coupling agent;(D) 1.5 parts by weight of platinum catalyst;(E) spherical thermally conductive alumina powder 300 parts by weight of body filler, 50 μm of partial size, irregular 200 parts by weight of Zinc oxide powder, 4 μm of partial size;(F) 200 weight of n-hexane Part;(G) 80 parts by weight of carbon fibre material, 6 μm of filament diameter, length is 70 μm;(H) 3 parts by weight of ethynylcyclohexanol.Prepare work Skill includes the following steps: that (1) by described in (E) 120 degree heat drying 1~2 hour, heating remove superfluous water under vacuum conditions Point;(2) (A)~(E) by described in, (H) are uniformly mixed using planetary mixer normal-temperature vacuum, and 600 revs/min of mixing speed Clock, mixing time 80 minutes obtained mixing paste base-materials, wherein (B) dosage is 3 parts by weight, (C) dosage is 2 parts by weight, (D) dosage is 1 parts by weight, and (H) dosage is 2 parts by weight;(3) by mixing paste base-material by calendering formation, with a thickness of required production Product thickness 1/2,120 DEG C of curing temperature, vulcanization time 60 minutes to get heat-conducting pad;(4) will described in (B), (C) (D), (F), (G), (H) sequentially adds planetary mixer and is uniformly mixed, wherein (B) dosage is 3 parts by weight, (C) dosage is 2 parts by weight, and (D) is used Amount is 0.5 parts by weight, and (H) dosage is 1 parts by weight, room temperature high-speed stirred, 3000~10000 revs/min of mixing speed, when stirring Between 80 minutes, be completely dispersed uniformly to carbon fiber, obtain carbon fiber dispersion liquid;(5) heat-conducting pad obtained by step (3) is as lining Carbon fiber dispersion liquid obtained by step (4) is brushed in heat-conducting pad upper surface of substrate, is then heated 30 minutes at 120 DEG C by bottom, The carbon fiber layer (6) with oriented alignment is obtained to make the heat-conducting pad for being attached with oriented alignment carbon fiber layer obtained by step (5) For substrate, remaining lotion base-material pressure is pressed together in substrate carrier using calender, and molding by high temperature vulcanization, curing temperature 120 DEG C, vulcanization time 50 minutes to get to have it is high draw mind and tearing strength, and leading with excellent heat conducting and soaking performance Hot silica gel pad.
Embodiment 2
The component that high-intensitive heat conductive silica gel gasket product of the invention utilizes during the preparation process is as follows: (A) ethylene methacrylic 25 parts by weight of base silicone oil, viscosity 1000mPas;(B) 4 parts by weight of containing hydrogen silicone oil, hydrogen content 0.15%;(C) vinyl front three 4 parts by weight of oxysilane coupling agent;(D) 1.5 parts by weight of catalyst;(E) spherical thermally conductive 350 parts by weight of alumina powder filler, 70 μm of partial size, 150 parts of irregular Zinc oxide powder, 5 μm of partial size;(F) 230 parts by weight of n-hexane;(G) 80 weight of carbon fibre material Part, 15 μm of filament diameter, length is 500 μm;(H) 3 parts by weight of ethynylcyclohexanol.Preparation process includes the following steps: that (1) will (E) 120 degree heat drying 1~2 hour, heating remove excessive moisture under vacuum conditions;(A)~(E) described in (2) inciting somebody to action, (H) it is uniformly mixed, 800 revs/min of mixing speed, is made within mixing time 80 minutes mixed using planetary mixer normal-temperature vacuum Lotion base-material is closed, wherein (B) dosage is 2 parts by weight, (C) dosage is 2.5 parts by weight, and (D) dosage is 1 parts by weight, and (H) is used Amount is 2 parts by weight;(3) mixing paste base-material is rolled into curing temperature by calendering formation with a thickness of required product thickness 1/2 120 DEG C, vulcanization time 60 minutes to get heat-conducting pad;(4) (B), (C) (D), (F), (G), (H) by described in sequentially add planet Blender is uniformly mixed, wherein (B) dosage is 1 parts by weight, (C) dosage is 1.5 parts by weight, and (D) dosage is 0.5 parts by weight, (H) Dosage be 1 parts by weight, room temperature high-speed stirred, 3000~10000 revs/min of mixing speed, mixing time 80 minutes, to carbon fiber It is completely dispersed uniformly, obtains carbon fiber dispersion liquid;(5) heat-conducting pad obtained by step (3) is as substrate, by carbon obtained by step (4) Fiber dispersion is constructed by the way of brushing in heat-conducting pad upper surface of substrate, is then heated 30 minutes, is obtained at 120 DEG C Carbon fiber layer with oriented alignment;(6) heat-conducting pad of oriented alignment carbon fiber layer will be attached with obtained by step (5) as lining Remaining lotion base-material pressure is pressed together in substrate carrier by bottom using calender, and molding by high temperature vulcanization, and 120 DEG C of curing temperature, Mind and tearing strength, and the heat conductive silica gel with excellent heat conducting and soaking performance are drawn to get to high within vulcanization time 50 minutes Gasket.
Reference examples 1
(A) 20 parts by weight of methyl vinyl silicon oil, viscosity 400mPas;(B) 2 parts by weight of containing hydrogen silicone oil, hydrogen content 0.1%;(C) 2 parts by weight of γ-(the third oxygen of 2,3- epoxy) propyl trimethoxy silicane coupling agent;(D) 1 parts by weight of catalyst;(E) Spherical thermally conductive 300 parts by weight of alumina powder filler of dry method modification, 50 μm of partial size, irregular 200 parts by weight of Zinc oxide powder, grain 4 μm of diameter;(F) 2 parts by weight of ethynylcyclohexanol.Preparation process: (1) (A)~(F) raw material by described in uses planetary mixer low speed It is stirred under vacuum and mixes, 800 revs/min of mixing speed, mixing time 60 minutes obtained mixing paste base-materials;(2) mixing paste base Material is formed using calender, and 120 DEG C of curing temperature, vulcanization time 50 minutes to get heat conductive silica gel gasket.
Reference examples 2
Basic recipe is consistent with technique and embodiment 1, only change carbon fibre material specification, and 5 μm of filament diameter, length It is 500 μm.
Reference examples 3
Basic recipe is consistent with technique and embodiment 1, only changes carbon fibre material specification, 30 μm of filament diameter, long Degree is 500 μm.
Reference examples 4
Basic recipe is consistent with technique and embodiment 1, only changes carbon fibre material specification, 15 μm of filament diameter, long Degree is 30 μm.
Reference examples 5
Basic recipe is consistent with technique and embodiment 1, only changes carbon fibre material specification, 15 μm of filament diameter, long Degree is 1500 μm.
Performance detection:
The thermal conductivity for the heat conductive silica gel gasket that each embodiment, reference examples are prepared uses resistance to LFA427 laser heat conducting instrument of speeding The measurement of thermal conductivity instrument.Heat-conducting pad test result of the present invention sees table 1:
1 heat-conducting pad test result of table
Particular embodiments described above has carried out further in detail the purpose of the present invention, technical scheme and beneficial effects It describes in detail bright.It should be understood that the above is only a specific embodiment of the present invention, it is not intended to restrict the invention, it is all Within the spirit and principles in the present invention, any modification, equivalent substitution, improvement and etc. done should be included in guarantor of the invention Within the scope of shield.

Claims (10)

1. a kind of preparation method of high intensity heat conductive silica gel gasket, which is characterized in that the preparation method includes following sequence step It is rapid:
SS1. by conduction powder filler, heat drying, removing excessive moisture obtain dry conduction powder filler under vacuum conditions;
SS2. by the drying conduction powder filler prepared in step SS1 and methyl vinyl silicon oil, containing hydrogen silicone oil, coupling agent, suppression Preparation and catalyst are according to 50~800 parts by weight: 12~35 parts by weight: 2~6 parts by weight: 0.5~6 parts by weight: 0.5~3 weight Part: room temperature stirs at low speed uniformly mixed, obtained mixing paste base-material to the ratio of 0.3~2 parts by weight under vacuum conditions;
SS3. by a part of calendering formation of the mixing paste base-material prepared in step SS2, the spacer thickness after calendering formation is The 1/5~4/5 of target heat conductive silica gel gasket products thickness, and molding by high temperature vulcanization is to get basic gasket;
SS4. by carbon fiber powder, containing hydrogen silicone oil, organic is volatilizable retarder thinner, catalyst, inhibitor and coupling agent according to 50~100 parts by weight: 3~5 parts by weight: 50~300 parts by weight: 0.2~1 parts by weight: 0.5~2 parts by weight: 0.5~4 parts by weight Ratio at normal temperature high-speed stirred be uniformly mixed, be completely dispersed uniformly to carbon fiber powder, obtain carbon fiber dispersion liquid;
SS5. using basic gasket prepared by step SS3 as substrate, carbon fiber dispersion liquid prepared by step SS4 is brushed in substrate The upper surface of gasket is heated to the volatilizable retarder thinner volatilization of organic completely, so that carbon fiber is on substrate carrier surface Rules orientation is arranged (being parallel to x/y plane), while being adsorbed on the coupling agent and lining containing vinyl groups of carbon fiber surface Unsaturated group and containing hydrogen silicone oil crosslink reaction in bottom spacer, and carbon fiber layer is made to be firmly attached to substrate carrier surface, excellent SS5 step can be repeated several times in order to increase soaking and the reinforcing effect of carbon fiber in selection of land, to increase carbon fiber row's ply gage;
SS6. it using the heat-conducting pad for being attached with oriented alignment carbon fiber layer obtained by step SS5 as substrate, will be prepared in step SS2 The pressing of remaining mixing paste base-material on substrate, and molding by high temperature vulcanization, obtain having both with high mechanical strength it is thermally conductive and The target heat conductive silica gel gasket product of soaking performance.
2. the method according to the claims, which is characterized in that in step SS1, the heating temperature of conduction powder filler It is 120 DEG C, Shi Changwei 1~2 hour.
3. the method according to the claims, which is characterized in that in step SS1, conduction powder filler can be spherical shape Or irregular shape metal, metal oxide or the mixture between them, it is further preferred that conduction powder filler is aluminium oxide or oxygen Change zinc powder body, partial size is 1~100 μm.
4. the method according to the claims, which is characterized in that in step SS2, carry out low speed using planetary mixer Stirring, 500~1000 revs/min of mixing speed, mixing time 30~80 minutes.
5. the method according to the claims, which is characterized in that in step SS2, the viscosity model of methyl vinyl silicon oil It encloses for 30~2000mPas.
6. the method according to the claims, which is characterized in that in step SS2, containing hydrogen silicone oil is in heat conductive silica gel gasket In play crosslinking curing, hydrogeneous mass fraction range is 0.05%~0.3%.
7. the method according to the claims, which is characterized in that step SS2, in SS4, coupling agent is silane coupling agent, Silane coupling agent type is containing vinyl groups.
8. the method according to the claims, which is characterized in that step SS2, in SS4, inhibitor is acetenyl hexamethylene Alcohol.
9. the method according to the claims, which is characterized in that step SS2, in SS4, catalyst is concentration 2000ppm Platinum catalyst.
10. the method according to the claims, which is characterized in that in step SS3, when high temperature vulcanized molding, vulcanization temperature Degree is 110~150 DEG C, vulcanization time 30~50 minutes.
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CN117603660A (en) * 2024-01-24 2024-02-27 北京泰派斯特电子技术有限公司 Ultrathin breakdown voltage-resistant heat-conducting insulating gasket and preparation method thereof
CN117603660B (en) * 2024-01-24 2024-04-26 北京泰派斯特电子技术有限公司 Ultrathin breakdown voltage-resistant heat-conducting insulating gasket and preparation method thereof

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