CN110229367A - A kind of anisotropy insulating heat-conductive sheet material and preparation method thereof - Google Patents
A kind of anisotropy insulating heat-conductive sheet material and preparation method thereof Download PDFInfo
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- CN110229367A CN110229367A CN201910430426.3A CN201910430426A CN110229367A CN 110229367 A CN110229367 A CN 110229367A CN 201910430426 A CN201910430426 A CN 201910430426A CN 110229367 A CN110229367 A CN 110229367A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/001—Combinations of extrusion moulding with other shaping operations
- B29C48/0022—Combinations of extrusion moulding with other shaping operations combined with cutting
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
- B29C48/07—Flat, e.g. panels
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/36—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
- B29C48/50—Details of extruders
- B29C48/695—Flow dividers, e.g. breaker plates
- B29C48/70—Flow dividers, e.g. breaker plates comprising means for dividing, distributing and recombining melt flows
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
- C08J7/0427—Coating with only one layer of a composition containing a polymer binder
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29L—INDEXING SCHEME ASSOCIATED WITH SUBCLASS B29C, RELATING TO PARTICULAR ARTICLES
- B29L2007/00—Flat articles, e.g. films or sheets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2383/00—Characterised by the use 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; Derivatives of such polymers
- C08J2383/04—Polysiloxanes
- C08J2383/07—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2483/00—Characterised by the use 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; Derivatives of such polymers
- C08J2483/04—Polysiloxanes
- C08J2483/07—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
-
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
Abstract
The invention discloses a kind of anisotropy insulating heat-conductive sheet materials, including thermally-conductive sheet, the raw material for preparing the anisotropy insulating heat-conductive sheet material includes at least flexible high molecular material, carbon fiber, ball-shaped micro powder and fire retardant, and the carbon fiber is orientated in the thickness direction of heat conductive sheet.The invention also discloses the preparation methods of the anisotropy insulating heat-conductive sheet material.The invention anisotropy insulating heat-conductive sheet material has included at least flexible high molecular material, carbon fiber, ball-shaped micro powder and fire retardant, so that random heat filling is blended in thermosetting flexible high molecular material, using shearing force fibrous heat filling is orientated in the flowing direction, is the heat conductive sheet of a kind of heating conduction and excellent insulation performance.
Description
Technical field
The present invention relates to heat-conducting interface material and preparation technical fields, and in particular to a kind of insulating heat-conductive material and its system
Preparation Method.
Background technique
With the fast development of data network, electric equipment products integrates electricity to intelligent and high speed, complication development
Road densification will approach physics limit, and it is also increasing that this will lead to the heat that product facility generates in the process of running, heat
Can not express delivery transfer scatter, affect the stability in use and service life of electronic product, therefore heat problem becomes electronic product
Development primarily solves the problems, such as.
For high efficiency heat radiation, heat-conducting interface material is filled between semiconductor chip and radiator, radiator fan, in the market
Conventional Heat Conduction Material needs the high filler loading capacity of ceramic powder then to obtain preferable heating conduction, then loses the soft of material
Property and stickiness, and high filler loading capacity will lead to stability of material and the service life decline.Using heat filling in each of heating conduction
The characteristic of anisotropy can also obtain preferable heat-conducting effect in the case where loading is little.Leading with anisotropic properties
Hot filler has graphite, boron nitride, alumina whisker, ZnOw, carbon fiber etc..Thermally conductive system of the carbon fiber in machine direction
If number can achieve 1500w/m.K. and fill a small amount of carbon fiber and be orientated carbon fiber along product thickness direction, not only
Retain product flexible well, will also obtain excellent heating conduction.
There are some heat conductive sheets that super-high heat-conductive coefficient is obtained using carbon fiber orientation currently on the market, but due to
Carbon fiber itself has good electric conductivity, causes product on-insulated, in application process can be with associated circuit board by voltage
The risk of breakdown.
Summary of the invention
To solve the above problems, it is an object of the invention to mix and take with high score flexible high molecular material by carbon fiber
To obtaining that a kind of flexible, thermal coefficient is high and the anisotropic thermal conductivity sheet material of insulation.
To achieve the above object, the present invention uses following scheme:
Anisotropy insulating heat-conductive sheet material, including thermally-conductive sheet prepare the original of the anisotropy insulating heat-conductive sheet material
Material includes at least flexible high molecular material, carbon fiber, ball-shaped micro powder and fire retardant, thickness of the carbon fiber in heat conductive sheet
Direction orientation.
As further embodiment, it is flexible high that raw material of the present invention includes at least 150-300 part in parts by weight
Molecular material, 500-800 part carbon fiber, 1200-1800 parts of ball-shaped micro powders and 150-200 parts of fire retardants.
As further embodiment, flexible high molecular material of the present invention be liquid acrylic, epoxy resin,
The mixing of one or more of polyurethane resin, unsaturated polyester resin, organic siliconresin.
As further embodiment, raw material of the present invention also includes 100-150 parts by weight of ethylene base silicone oil, the ethylene
The viscosity of base silicone oil is 500-100000mpa.s.
As further embodiment, raw material of the present invention also includes 80-120 parts by weight dimethicone, 0.05-
The delay inhibitor of 0.2 parts by weight, 3-6 parts by weight silicone oil containing H, 1-3 parts by weight platinum water catalyst.
As further embodiment, ball-shaped micro powder of the present invention is the compounding powder comprising aluminium oxide and silicate powder
End, the average grain diameter of the ball-shaped micro powder powder are 0.1-5 μm.Preferably, the ball-shaped micro powder also includes a small amount of nitridation
Boron, aluminium nitride, one or two kinds of above mixing in silicon carbide.
As further embodiment, carbon fiber of the present invention be surface insulation cladding polyacrylonitrile-based carbon fibre,
One of asphalt base carbon fiber, viscose-based carbon fiber, phenolic aldehyde base carbon fibre, gas-phase growth of carbon fibre, the carbon fiber are put down
Equal diameter is 2-30 μm, and length is 50-300 μm.
As further embodiment, thermally-conductive sheet surface of the present invention forms macromolecule by coating high-molecular coating
Coating, it includes 80-120 parts of vinyl silicone oils, 40-65 parts of dimethicones, 0.05- that the high-molecular coating calculates by weight
The delay inhibitor of 0.2 parts by weight, 2-5 parts of silicone oil containing H, 1-3 parts of platinum water catalyst, 150-200 parts of chain alkyl siloxanes.
Preferably, thickness≤50 μm of polymeric coating layer of the present invention.In the present invention, the polymeric coating layer tool in thermally-conductive sheet
Toughness, convenient for the assembly between heat-conducting pad and other component.
The present invention also provides a kind of preparation methods of anisotropy insulating heat-conductive sheet material to be made using shearing force
It obtains fibrous heat filling to be orientated in the flowing direction, obtains a kind of anisotropy insulating heat-conductive sheet material haveing excellent performance.
A kind of preparation method of anisotropy insulating heat-conductive sheet material, including
The step of preparing thermal conductivity pre-feed: carbon fiber, ball-shaped micro powder and fire retardant are evenly mixed in flexible macromolecule
In material, thermal conductivity pre-feed is prepared;
Flow velocity shears orientation step: above-mentioned thermal conductivity pre-feed is squeezed out by extruder and takes carbon fiber on flow velocity direction
To, and be heating and curing in the slot that moves moulds that can be molded, form formed body;
Ultrasonic cutting step: above-mentioned formed body ultrasonic cutting mode is obtained along the flow velocity direction cutting that intersects vertically
Obtain the heat conductive sheet that carbon fiber is orientated along thickness direction.
Further embodiment, preparation method of the present invention further include heat conductive sheet surface treatment step, thermal conductivity
Sheet surface processing is by way of in thermally-conductive sheet surface coating high-molecular coating formation polymeric coating layer or by polishing
Thermally-conductive sheet surface is polished smooth.
As further embodiment, in preparation method of the present invention after preparing thermal conductivity pre-feed step, flow velocity
Before shearing orientation step, further includes the steps that the thermal conductivity pre-feed that will be uniformly mixed is placed and vacuumized in vacuum tank, vacuum tank
Vacuum degree be≤- 0.09Mpa, the pumpdown time >=8min.
As further embodiment, the surrounding of die device of the present invention posts release film.Preferably, described release
Film can choose but be not limited to one of PET film, PI film, oiliness paper, dripping film, that paper of day, antiadhesion barrier, skidding film.
As further embodiment, extruder of the present invention is screw-type extruder, and the nozzle of extruder is bee
Nest nozzle;Sectional area≤81mm of single hole in the honeycomb nozzle2, wall thickness≤0.1mm, honeycomb nozzle length >=
5cm.Further, the honeycomb cross section of fluid channel size of the honeycomb nozzle is at least 30mm × 30mm, the shape of single hole
It does not limit, can be circle, ellipse, rectangle, square, other polygons etc., wherein more preferably with equilateral symmetrical more
Side shape or circle or ellipse.
As further embodiment, the extrusion channel of extruder of the present invention is tapered runner, the tapered runner
One part flow arrangement, honeycomb nozzle end and the mobile mould molded are at least installed with honeycomb nozzle joint
Has slot connection, the end of the slot that moves moulds is equipped with the limiter that control mold slots move back distance.Specifically, removable dynamic model
Tool slot one end is nested honeycomb nozzle end.In this scenario, using honeycomb nozzle, carbon fiber can be increased in runner
It is orientated possibility, removable mold slots one end is connected to honeycomb nozzle end, so that pre-feed extruded velocity and moving back speed
Unanimously, reduce interference of the air in die cavity, mold the molding that is heating and curing in removable mold slots.
As further embodiment, in flow velocity shearing orientation step of the present invention, it is heating and curing roasting using blowing-type
Case, the temperature setting of oven are 80-120 DEG C, baking time 4-8H.
The beneficial effects of the present invention are:
1. anisotropy insulating heat-conductive sheet material of the present invention has included at least flexible high molecular material, carbon fiber,
Ball-shaped micro powder and fire retardant, so that random heat filling is blended in thermosetting flexible high molecular material, threadiness is thermally conductive to be filled out
Material is orientated in the flowing direction, is the heat conductive sheet of a kind of heating conduction and excellent insulation performance;
2. preparation method of the present invention utilizes shearing force, so that fibrous heat filling takes in the flowing direction
To obtaining good heating conduction in flow velocity direction after so that thermally conductive prepared material is heating and curing, obtain a kind of carbon fiber by slice
Tie up the insulating heat-conductive sheet material being orientated in thickness direction.
Specific embodiment
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described implementation
Example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common
Technical staff's all other embodiment obtained without creative efforts belongs to the model that the present invention protects
It encloses.
Anisotropy insulating heat-conductive sheet material, including thermally-conductive sheet prepare the original of the anisotropy insulating heat-conductive sheet material
Material includes at least flexible high molecular material, carbon fiber, ball-shaped micro powder and fire retardant, thickness of the carbon fiber in heat conductive sheet
Direction orientation.
As further embodiment, it is flexible high that raw material of the present invention includes at least 150-300 part in parts by weight
Molecular material, 500-800 part carbon fiber, 1200-1800 parts of ball-shaped micro powders and 150-200 parts of fire retardants.
As further embodiment, flexible high molecular material of the present invention can choose but be not limited to liquid propene
The mixing of one or more of acid resin, epoxy resin, polyurethane resin, unsaturated polyester resin, organic siliconresin.It is excellent
Choosing, select organic siliconresin.The fire retardant is aluminium hydroxide, magnesium hydroxide, phosphoric acid flame retardant, a kind of in antimony oxide
Or two or more mixing, preferred aluminium hydroxide, the average grain diameter of aluminium hydroxide are 0.1-5 μm in the present invention.
As further embodiment, raw material of the present invention also includes 100-150 parts by weight of ethylene base silicone oil, the ethylene
The viscosity of base silicone oil is 500-100000mpa.s.
As further embodiment, raw material of the present invention also includes 80-120 parts by weight dimethicone, 0.05-
0.2 parts by weight postpone inhibitor, 3-6 parts by weight silicone oil containing H, 1-3 parts by weight platinum water catalyst.
As further embodiment, ball-shaped micro powder of the present invention is the compounding powder comprising aluminium oxide and silicate powder
End, the average grain diameter of the ball-shaped micro powder powder are 0.1-5 μm.Preferably, the ball-shaped micro powder also includes a small amount of nitridation
Boron, aluminium nitride, one or two kinds of above mixing in silicon carbide.
As further preferred scheme, carbon fiber of the present invention is the polyacrylonitrile-radical carbon fiber of surface insulation cladding
One of dimension, asphalt base carbon fiber, viscose-based carbon fiber, phenolic aldehyde base carbon fibre, gas-phase growth of carbon fibre, the carbon fiber
Average diameter is 2-30 μm, and length is 50-300 μm.
Carbon fiber surface insulating wrapped technique employed in the present invention is as follows:
Carbon fiber surface activation step: being heat-treated carbon fiber base material surface using Muffle furnace, 500-1000 DEG C, place
Selection of time 10h is managed, the activity on carbon fiber base material surface, the carbon fiber activated are enhanced;
Formed insulating coating the step of: by after above-mentioned activation carbon fiber and ethyl orthosilicate, ethyl alcohol and catalyst according to
30~100g of carbon fiber, 5~200ml of ethyl orthosilicate, 100~500ml of ethyl alcohol, 10% 10~100ml of Ammonia,
It is heated to 50 DEG C on warm table, is uniformly mixed, so that carbon fiber surface gradually forms one layer of uniform and stable SiO2Absolutely
Edge coating obtains SiO after suction filtration2The carbon fiber of insulating wrapped;
Baking procedure: the carbon fiber of above-mentioned insulating wrapped is gone in oven and is toasted.
It in above-mentioned baking procedure, is toasted using segmented, 50~120 DEG C of first stage baking temperature, the time is 1~3h,
Preferred temperature is 100 DEG C;Second stage baking temperature is 200~300 DEG C, toasts 2~4h, and preferred temperature is 250 DEG C.
As further embodiment, thermally-conductive sheet surface of the present invention forms macromolecule by coating high-molecular coating
Coating, the high-molecular coating calculate by weight including 80-120 parts of vinyl silicone oils, 40-65 parts of dimethicones,
0.05-0.2 parts by weight postpone inhibitor, 2-5 parts of silicone oil containing H, 1-3 parts of platinum water catalyst, 150-200 parts of chain alkyl silicon oxygen
Alkane.The chain alkyl siloxanes added in high-molecular coating has the effect of heated volatilization, is conducive to increase polymeric coating layer
Viscosity.Further, in order to obtain better heat-conducting effect, it is micro- that a small amount of spherical shape can also be added in the high-molecular coating
Powder, specific additive amount are that calculating is 200-450 parts by weight, and the average grain diameter of the ball-shaped micro powder is 0.1-5 μm.
As further embodiment, thickness≤50 μm of polymeric coating layer of the present invention.
The present invention also provides a kind of preparation methods of anisotropy insulating heat-conductive sheet material to be made using shearing force
It obtains fibrous heat filling to be upwardly oriented in flow velocity side, obtains a kind of anisotropy insulating heat-conductive sheet material haveing excellent performance.
A kind of preparation method of anisotropy insulating heat-conductive sheet material, including
The step of preparing thermal conductivity pre-feed: carbon fiber, ball-shaped micro powder and fire retardant are evenly mixed in flexible macromolecule
In material, thermal conductivity pre-feed is prepared;
Flow velocity shears orientation step: above-mentioned thermal conductivity pre-feed is squeezed out by extruder and takes carbon fiber on flow velocity direction
To, and be heating and curing in the slot that moves moulds that can be molded, form formed body;
Ultrasonic cutting step: above-mentioned formed body ultrasonic cutting mode is obtained along the flow velocity direction cutting that intersects vertically
Obtain the heat conductive sheet that carbon fiber is orientated along thickness direction.
Further embodiment, preparation method of the present invention further include heat conductive sheet surface treatment step, thermal conductivity
Sheet surface processing is by way of in thermally-conductive sheet surface coating high-molecular coating formation polymeric coating layer or by polishing
Thermally-conductive sheet surface is polished smooth.
As further embodiment, in preparation method of the present invention after preparing thermal conductivity pre-feed step, flow velocity
Before shearing orientation step, further includes the steps that the thermal conductivity pre-feed that will be uniformly mixed is placed and vacuumized in vacuum tank, vacuum tank
Vacuum degree be≤- 0.09Mpa, the pumpdown time >=8min.
As further embodiment, the surrounding of die device of the present invention posts release film.
As further embodiment, extruder of the present invention is screw-type extruder, and the nozzle of extruder is bee
Nest nozzle;Sectional area≤81mm of single hole in the honeycomb nozzle2, wall thickness≤0.1mm, honeycomb nozzle length >=
5cm。
As further embodiment, the extrusion channel of extruder of the present invention is tapered runner, the tapered runner
One part flow arrangement, honeycomb nozzle end and the mobile mould molded are at least installed with honeycomb nozzle joint
Has slot connection, the end of the slot that moves moulds is equipped with the limiter that control mold slots move back distance.
As further embodiment, in flow velocity shearing orientation step of the present invention, it is heating and curing roasting using blowing-type
Case, the temperature setting of oven are 80-120 DEG C, baking time 4-8H.
Further, in ultrasonic cutting step, the vibration frequency > 20KHz of the ultrasonic cutting machine, knife rest is downward
Movement speed < 10mm/min.
It is specific embodiment of the present invention below, in the following embodiments, used raw material, equipment etc. come from the present invention
Outside particular determination, it can be obtained by buying pattern.
In the following embodiments, carbon fiber of the present invention is prepared by the following:
Carbon fiber surface activation step: being heat-treated carbon fiber base material surface using Muffle furnace, 500 DEG C, when processing
Between select 12h, enhance the activity on carbon fiber base material surface, the carbon fiber activated;
The step of forming insulating coating: weighing the above-mentioned carbon fiber of 50g and be placed in beaker, measure 80ml ethyl orthosilicate,
400ml dehydrated alcohol is poured into ethyl orthosilicate and dehydrated alcohol in beaker by the drainage of glass bar, with agitating paddle into
Row stirring, whipping process are heated on warm table, and heating platen temperature is set as 50 DEG C, mixing speed 1500rpm, stirring
Time is 4h, when carbon fiber is evenly mixed in solution, uses rubber head dropper that ammonium hydroxide is added dropwise as catalyst, the additive amount of ammonium hydroxide
For 100ml, time for adding is controlled in 40min, and in whipping process, solution ph maintains 10 or so, when pH value is greater than 10
When, acetic acid is added dropwise and is adjusted, after stirring terminates, carbon fiber mixed solution is filtered with Vacuum filtration device, takes out
During filter, the continuous ethanol solution that is added cleans carbon fiber, until the solution after filtering obtains SiO at neutrality2
The carbon fiber of insulating wrapped;
Baking procedure: by above-mentioned SiO2The carbon fiber of insulating wrapped, which is gone in oven, to be toasted, and is toasted using segmented,
First stage is in the oven for placing it in temperature setting and being 50 DEG C, and baking time 3h is removed and is attached on carbon fiber
Ethyl alcohol and moisture evaporate, second stage is to place it in Muffle furnace to be calcined, temperature setting be 300 DEG C, forge
The burning time is 2h, forms one layer of fine and close, stable SiO in carbon fiber surface2Insulating coating.
Embodiment 1
A kind of anisotropy insulating heat-conductive sheet material, including thermally-conductive sheet, the thermally-conductive sheet surface pass through coating high score
Sub- coating forms polymeric coating layer, and the raw material for preparing the anisotropy insulating heat-conductive sheet material includes at least flexible macromolecule material
Material, carbon fiber, ball-shaped micro powder and fire retardant, the carbon fiber are orientated in the thickness direction of heat conductive sheet;
Preparation method is as follows:
The step of preparing thermal conductivity pre-feed: will be respectively by 15 parts by weight methyl vinyl silicone rubbers, 100 parts by weight viscosity
For the vinyl silicone oil of 800mpa.s, 80 parts by weight dimethicones, 3 parts by weight silicone oil containing H, 1 parts by weight platinum water catalyst,
1200 parts by weight ball-shaped micro powders, 150 parts by weight aluminium hydroxides, 500 parts by weight of carbon fibers are uniformly mixed by way of mill, are obtained
To thermal conductivity pre-feed;
Flow velocity shears orientation step: it is -0.09Mpa that uniformly mixed thermal conductivity pre-feed, which is placed on vacuum degree, it is true
Pumpdown time 10min in empty van is squeezed out by extruder and is upwardly oriented carbon fiber in flow velocity side, and extruded velocity is less than
20rpm/min, and 80 DEG C of solidifications are heated in the slot that moves moulds that can be molded, formed body is formed, wherein the extruder is
Screw-type extruder, the nozzle of extruder are honeycomb nozzle;The single aperture of honeycomb nozzle in the honeycomb nozzle
Area is 10mm2, length 10cm, wall thickness 0.1mm;
Ultrasonic cutting step: above-mentioned formed body ultrasonic cutting mode is obtained along the flow velocity direction cutting that intersects vertically
The heat conductive sheet that be orientated along thickness direction of carbon fiber, wherein the vibration frequency of ultrasonic cutting machine is 25KHz, knife rest to
Lower movement speed 8mm/min;
Coat polymeric coating layer step: by 80 parts by weight of ethylene base silicone oil, 40 parts by weight dimethicones, 0.05 parts by weight
Postpone inhibitor, 2 parts by weight silicone oil containing H, 1 parts by weight platinum water catalyst, the stirring of 150 parts by weight chain alkyl siloxanes are equal
It is even, obtain high-molecular coating, uniformly coated high-molecular coating in thermally-conductive sheet with coating machine, coating layer thickness less than 50 μm,
Then it puts into 150 DEG C of oven, heating 10min solidification obtains surface and has sticking heat conductive sheet.
Embodiment 2
A kind of anisotropy insulating heat-conductive sheet material, including thermally-conductive sheet, the thermally-conductive sheet surface pass through coating high score
Sub- coating forms polymeric coating layer, and the raw material for preparing the anisotropy insulating heat-conductive sheet material includes at least flexible macromolecule material
Material, carbon fiber, ball-shaped micro powder and fire retardant, the carbon fiber are orientated in the thickness direction of heat conductive sheet;
Preparation method is as follows:
The step of preparing thermal conductivity pre-feed: will be respectively by 15 parts by weight methyl vinyl silicone rubbers, 150 parts by weight viscosity
Postpone inhibitor, 4.0 parts by weight for the vinyl silicone oil, 120 parts by weight dimethicones, 0.08 parts by weight of 100000mpa.s
Silicone oil containing H, 3 parts by weight platinum water catalyst, 1200 parts by weight ball-shaped micro powders, 150 parts by weight aluminium hydroxides, 850 parts by weight carbon
Fiber is uniformly mixed by way of mill, obtains thermal conductivity pre-feed;
Flow velocity shears orientation step: it is -0.09Mpa that uniformly mixed thermal conductivity pre-feed, which is placed on vacuum degree, it is true
Pumpdown time 10min in empty van is squeezed out by extruder and is upwardly oriented carbon fiber in flow velocity side, and extruded velocity is less than
20rpm/min, and 80 DEG C of solidifications are heated in the slot that moves moulds that can be molded, formed body is formed, wherein the extruder is
Screw-type extruder, the nozzle of extruder are honeycomb nozzle;The single aperture of honeycomb nozzle in the honeycomb nozzle
Area is 10mm2, length 10cm, wall thickness 0.1mm;
Ultrasonic cutting step: above-mentioned formed body ultrasonic cutting mode is obtained along the flow velocity direction cutting that intersects vertically
The heat conductive sheet that be orientated along thickness direction of carbon fiber, wherein the vibration frequency of ultrasonic cutting machine is 25KHz, knife rest to
Lower movement speed 8mm/min;
Coat polymeric coating layer step: by 120 parts by weight of ethylene base silicone oil, 65 parts by weight dimethicones, 0.05 weight
Part delay inhibitor, 5 parts by weight silicone oil containing H, 3 parts by weight platinum water catalyst, the stirring of 200 parts by weight chain alkyl siloxanes are equal
It is even, obtain high-molecular coating, uniformly coated high-molecular coating in thermally-conductive sheet with coating machine, coating layer thickness less than 50 μm,
Then it puts into 150 DEG C of oven, heating 10min solidification obtains surface and has sticking heat conductive sheet.
Embodiment 3
On the basis of embodiment 1, coating polymeric coating layer step is changed into and polishing light is carried out to heat conductive sheet surface
Sliding, the mode of surface polishing is not limited to sand polishing, sander polishing, brown paper polishing, silicon carbide ceramics porous grinding wheel
Deng.
Embodiment 4
On the basis of example 1, using the vinyl silicone oil of viscosity 10000mpa.s, the entirety of thermal conductivity pre-feed is adjusted
Viscosity carries out operation by the identical step with example 1 and obtains heat conductive sheet.
Embodiment 5-8
On the basis of example 1, the single aperture area of honeycomb nozzle is adjusted, is walked according to the identical operation of embodiment 1
Rapid to obtain heat conductive sheet, the single aperture area for the honeycomb nozzle that embodiment 5-8 is respectively adopted is 4mm2、8mm2、30mm2、
60mm2。
Embodiment 9-12
On the basis of embodiment 1, the thickness for adjusting surface polymeric coating layer, according to the identical operating procedure of embodiment 1
Heat conductive sheet is obtained, the thickness of polymeric coating layer is respectively 20 μm, 30 μm, 80 μm, 110 μm in embodiment 9-12.
The performance of the thermally-conductive sheet of above-described embodiment 1-12 is detected respectively, the project of detection include thermal coefficient,
Hardness, breakdown voltage, surface viscosity.Concrete outcome is referring to table 1.
Table 1: the performance comparison of the thermally-conductive sheet of embodiment 1-12
From the result of table 1 it can be concluded that draw a conclusion
1) viscosity of pre-feed is smaller known to finally obtained heat conductive sheet thermal coefficient result, more advantageous carbon fiber
It is upwardly oriented in flow velocity side, so that higher thermal coefficient is obtained, and when the vinyl silicone oil of use 10000mpa.s, thermally conductive system
Number is influenced by viscosity number and is declined.
2) dosage of carbon fiber will affect the orientation of heat conductive sheet, when the promotion of carbon fiber packing ratio, also result in preparation
The overall viscosity of material is also promoted, and hinders orientation effect of the carbon fiber in honeycomb nozzle instead.
3) the single aperture area of honeycomb nozzle will affect the thermal coefficient of heat conductive sheet, specific manifestation are as follows: work as bee
The single aperture area < 10mm of nest nozzle2, observed in 2.5 dimension image instruments, the whole sequence of carbon fiber is good, thermally conductive system
Number influences little;As the single aperture area > 50mm of honeycomb nozzle2When, it is observed in 2.5 dimension image instruments, it is only adherent
Position carbon fiber sorts more chaotic, thermal coefficient is different along flow velocity direction marshalling closer to centre carbon fiber
Degree decline.
4) thickness of the polymeric coating layer on heat conductive sheet surface also has an impact to thermal coefficient, specific manifestation are as follows: works as table
Finishing coat thickness influences thermal coefficient little less than 50 μm;When 100 μm of coating layer thickness >, the thermally conductive system of heat conductive sheet
Number rapid drawdown.
A kind of anisotropy insulating heat-conductive sheet material is provided for the embodiments of the invention above to be described in detail, this
Apply that a specific example illustrates the principle and implementation of the invention in text, the explanation of above example is only intended to
Help understands core of the invention thought;At the same time, for those skilled in the art, it is according to the thought of the present invention and square
Method, there will be changes in the specific implementation manner and application range, in conclusion the content of the present specification should not be construed as pair
Limitation of the invention.
Claims (16)
1. anisotropy insulating heat-conductive sheet material, including thermally-conductive sheet, which is characterized in that prepare the anisotropy insulating heat-conductive
The raw material of sheet material includes at least flexible high molecular material, carbon fiber, ball-shaped micro powder and fire retardant, and the carbon fiber is in thermal conductivity piece
The thickness direction of material is orientated.
2. anisotropy insulating heat-conductive sheet material according to claim 1, which is characterized in that the raw material include at least with
150-300 part flexible high molecular material, 500-800 parts of carbon fibers, 1200-1800 parts of ball-shaped micro powders and the 150- of parts by weight meter
200 parts of fire retardants.
3. anisotropy insulating heat-conductive sheet material according to claim 1, which is characterized in that the flexible high molecular material
For one or both of liquid acrylic, epoxy resin, polyurethane resin, unsaturated polyester resin, organic siliconresin
The above mixing.
4. anisotropy insulating heat-conductive sheet material according to claim 2, which is characterized in that the raw material also includes 100-
150 parts by weight of ethylene base silicone oil, the viscosity of the vinyl silicone oil are 500-100000mpa.s.
5. anisotropy insulating heat-conductive sheet material according to claim 3, which is characterized in that the raw material also includes 80-
The delay inhibitor of 120 parts by weight dimethicones, 0.05-0.2 parts by weight, 3-6 parts by weight silicone oil containing H, 1-3 parts by weight platinum
Water catalyst.
6. according to the described in any item anisotropy insulating heat-conductive sheet materials of claim 2-5, which is characterized in that the spherical shape is micro-
Powder is the compounding powder comprising aluminium oxide and silicate powder, and the average grain diameter of the ball-shaped micro powder powder is 0.1-5 μm.
7. anisotropy insulating heat-conductive sheet material according to claim 1-5, which is characterized in that the carbon fiber
Polyacrylonitrile-based carbon fibre, asphalt base carbon fiber, viscose-based carbon fiber, phenolic aldehyde base carbon fibre, gas phase for surface insulation cladding
One of grown carbon fiber, the average diameter of the carbon fiber are 2-30 μm, and length is 50-300 μm.
8. anisotropy insulating heat-conductive sheet material according to claim 1-5, which is characterized in that the thermally conductive sheet
Material surface forms polymeric coating layer by coating high-molecular coating, and it includes 80-120 parts that the high-molecular coating calculates by weight
The delay inhibitor of vinyl silicone oil, 40-65 part dimethicone, 0.05-0.2 parts by weight, 2-5 parts of silicone oil containing H, 1-3 parts of platinum
Jinsui River catalyst, 150-200 parts of chain alkyl siloxanes.
9. anisotropy insulating heat-conductive sheet material according to claim 8, which is characterized in that the thickness of the polymeric coating layer
≤ 50 μm of degree.
10. a kind of preparation method of anisotropy insulating heat-conductive sheet material as described in claim 1, which is characterized in that including
The step of preparing thermal conductivity pre-feed: carbon fiber, ball-shaped micro powder and fire retardant are evenly mixed in flexible high molecular material
In, prepare thermal conductivity pre-feed;
Flow velocity shears orientation step: above-mentioned thermal conductivity pre-feed is squeezed out by extruder and is upwardly oriented carbon fiber in flow velocity side,
And be heating and curing in the slot that moves moulds that can be molded, form formed body;
Ultrasonic cutting step: by above-mentioned formed body ultrasonic cutting mode, carbon is obtained along the flow velocity direction cutting that intersects vertically
The heat conductive sheet that fiber is orientated along thickness direction.
11. preparation method according to claim 10, which is characterized in that after preparing thermal conductivity pre-feed step, flow velocity
Before shearing orientation step, further includes the steps that the thermal conductivity pre-feed that will be uniformly mixed is placed and vacuumized in vacuum tank, vacuum tank
Vacuum degree be≤- 0.09Mpa, the pumpdown time >=8min.
12. preparation method according to claim 10, which is characterized in that the surrounding of the die device posts release film.
13. preparation method according to claim 10, which is characterized in that the extruder is screw-type extruder, is squeezed out
The nozzle of machine is honeycomb nozzle;Sectional area≤81mm of single hole in the honeycomb nozzle2, wall thickness≤0.1mm, bee
Nest nozzle length >=5cm.
14. preparation method according to claim 13, which is characterized in that the extrusion channel of the extruder is taper flow
A part flow arrangement, honeycomb nozzle end and institute are at least installed in road, the tapered runner and honeycomb nozzle joint
The slot connection that moves moulds that can be molded is stated, the end of the slot that moves moulds is equipped with the limit that control mold slots move back distance
Device.
15. preparation method according to claim 10, which is characterized in that flow velocity is sheared in orientation step, is heating and curing and is adopted
With blowing-type oven, the temperature setting of oven is 80-120 DEG C, baking time 4-8H.
16. the described in any item preparation methods of 0-15 according to claim 1, which is characterized in that further include heat conductive sheet surface
Processing step, heat conductive sheet surface treatment by thermally-conductive sheet surface coat high-molecular coating formed polymeric coating layer or
It is to be polished smooth thermally-conductive sheet surface by polishing mode.
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