CN103975429A - Thermally conductive sheet and method for manufacturing thermally conductive sheet - Google Patents

Thermally conductive sheet and method for manufacturing thermally conductive sheet Download PDF

Info

Publication number
CN103975429A
CN103975429A CN201280061296.7A CN201280061296A CN103975429A CN 103975429 A CN103975429 A CN 103975429A CN 201280061296 A CN201280061296 A CN 201280061296A CN 103975429 A CN103975429 A CN 103975429A
Authority
CN
China
Prior art keywords
thermal conductivity
sheet
conductivity sheet
filler
composition
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN201280061296.7A
Other languages
Chinese (zh)
Other versions
CN103975429B (en
Inventor
荒卷庆辅
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Dexerials Corp
Original Assignee
Dexerials Corp
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Dexerials Corp filed Critical Dexerials Corp
Priority to CN201810153894.6A priority Critical patent/CN108384248B/en
Publication of CN103975429A publication Critical patent/CN103975429A/en
Application granted granted Critical
Publication of CN103975429B publication Critical patent/CN103975429B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L23/00Details of semiconductor or other solid state devices
    • H01L23/34Arrangements for cooling, heating, ventilating or temperature compensation ; Temperature sensing arrangements
    • H01L23/36Selection of materials, or shaping, to facilitate cooling or heating, e.g. heatsinks
    • H01L23/373Cooling facilitated by selection of materials for the device or materials for thermal expansion adaptation, e.g. carbon
    • H01L23/3737Organic materials with or without a thermoconductive filler
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/28Nitrogen-containing compounds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00Use of ingredients characterised by shape
    • C08K7/02Fibres or whiskers
    • C08K7/04Fibres or whiskers inorganic
    • C08K7/06Elements
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L101/00Compositions of unspecified macromolecular compounds
    • HELECTRICITY
    • H05ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05KPRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K7/00Constructional details common to different types of electric apparatus
    • H05K7/20Modifications to facilitate cooling, ventilating, or heating
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2924/00Indexing scheme for arrangements or methods for connecting or disconnecting semiconductor or solid-state bodies as covered by H01L24/00
    • H01L2924/0001Technical content checked by a classifier
    • H01L2924/0002Not covered by any one of groups H01L24/00, H01L24/00 and H01L2224/00

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Medicinal Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Materials Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Power Engineering (AREA)
  • Computer Hardware Design (AREA)
  • General Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Cooling Or The Like Of Semiconductors Or Solid State Devices (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Cooling Or The Like Of Electrical Apparatus (AREA)
  • Manufacture Of Macromolecular Shaped Articles (AREA)

Abstract

Provided is a thermally conductive sheet having good thermal conductivity in the thickness direction thereof. A thermally conductive sheet includes a thermally conductive composite containing a silicone resin, thermally conductive fillers, and a filling material for aligning the thermally conductive fillers in a predetermined direction, the thermally conductive fillers are oriented along the thickness direction of the thermally conductive sheet, and at least aluminum nitride is contained as the filling material. Further, the lightness (L*) represented by the ''L*'' value in the L*a*b color system prescribed in ''JIS Z 8729'' and ''JIS Z 8730'' when the surface of the thermally conductive sheet is measured is 32.5 or more.

Description

The manufacture method of thermal conductivity sheet and thermal conductivity sheet
Technical field
The present invention relates to promote the thermal conductivity sheet of the heat radiations such as heat generation electronic unit and the manufacture method of thermal conductivity sheet.
The application is to advocate preference in the Japanese patent application No. Patent 2011-278788 of application on December 20th, 2011 as basis in Japan, and by reference, these applications are quoted in the application.
Background technology
Be accompanied by the further high performance of electronic instrument, densification, the mounting of height of semiconductor element are developed.Accompany therewith, the heat that the electronic unit that forms electronic instrument is generated heat further dispels the heat and becomes a very important ring expeditiously.For high efficiency heat radiation, semiconductor is installed in the heat abstractor such as heat emission fan, heating panel (heat sink) via thermal conductivity sheet.Thermal conductivity sheet is widely used the sheet that the packing materials such as inorganic filler is disperseed and are contained in gained in organosilicon.Such radiating component is required to the further raising of thermal conductivity, conventionally taking high-termal conductivity as object, the filling rate that is matched with the inorganic filler in matrix by raising is dealt with.But if improve the filling rate of inorganic filler, flexibility is impaired, or the filling rate of inorganic filler is high causes occurring powder falling, and therefore, the filling rate that improves inorganic filler is limited.
Inorganic filler for example can be enumerated aluminium oxide, aluminium nitride, aluminium hydroxide etc.Taking high thermal conductivity as object, also the flake shaped particle such as boron nitride, graphite, carbon fiber etc. can be filled in matrix.This is that the anisotropy of the thermal conductivity that has according to flake shaped particle etc. is established.For example known carbon fiber has the thermal conductivity of about 600-1200W/mK in machine direction.Boron nitride has about 110W/mK in face direction, has the thermal conductivity of about 2W/mK left and right in the direction vertical with face direction, has anisotropy.
Conventionally known, if thermal conductivity sheet is increased to the loading of thermal conductivity filler, thermal conductivity improves.But fibrous thermal conductivity filler, compared with ball filler, cannot increase loading.Therefore independent fibrous thermal conductivity filler cannot obtain high thermal conductivity.Here by making the face direction of fibrous thermal conductivity filler identical with the thickness direction of the thermal conductivity sheet as direction of heat transfer, that is, by making the thickness direction orientation of fibrous thermal conductivity filler along thermal conductivity sheet, can make thermal conductivity improve, tremendously.
In patent documentation 1, record the heat conductivity composition that coating contains carbon fiber and applied magnetic field and make the method for carbon fiber orientation.But, when carbon fiber orientation, must there is mobility, in the method for therefore recording at patent documentation 1, cannot make the loading of thermal conductivity filler increase.People wish to obtain thermal conductivity filler along thermal conductivity sheet thickness direction orientation, the good thermal conductivity sheet of thermal conductivity of thickness direction for this reason.
Prior art document
Patent documentation
Patent documentation 1: TOHKEMY 2006-335957 communique.
Summary of the invention
The problem that invention will solve
The present invention is directed to above-mentioned situation and propose, its object is to provide the good thermal conductivity sheet of the thermal conductivity of thickness direction and the manufacture method of thermal conductivity sheet.
Solve the scheme of problem
The inventor conducts in-depth research, found that: in the L*a*b* color specification system that " the JIS Z 8729 " and " JIS Z 8730 " in the time measuring thermal conductivity sheet surperficial records, to there is height correlation relation between the brightness L* of " L* " value representation and thermal conductivity, thereby complete the present invention.
The present invention relates to a kind of thermal conductivity sheet that contains heat conductivity composition, the packing material that described heat conductivity composition contains hardening resin composition and thermal conductivity filler is arranged along prescribed direction, wherein, thermal conductivity filler is along the thickness direction orientation of thermal conductivity sheet, at least contain aluminium nitride as packing material, in the L*a*b* color specification system that " JIS Z 8729 " and " JIS Z 8730 " in the time measuring thermal conductivity sheet surperficial records, taking the brightness L* of " L* " value representation as more than 32.5.
The manufacture method of thermal conductivity sheet of the present invention has following operation: heat conductivity composition production process, wherein, make heat conductivity composition, the packing material that this heat conductivity composition contains hardening resin composition, thermal conductivity filler and thermal conductivity filler is arranged along prescribed direction; Orientation procedure, wherein, is formed as column by the heat conductivity composition of making in heat conductivity composition production process, makes the length direction orientation of thermal conductivity filler along column simultaneously; Cut off operation, wherein, by ultrasonic wave cutting machine, the heat conductivity composition of column is cut into the size of regulation along the direction intersecting vertically with length direction, obtain thermal conductivity sheet; In thermal conductivity sheet, thermal conductivity filler is along the thickness direction orientation of thermal conductivity sheet, at least contain aluminium nitride as packing material, the L*a*b* that " JIS Z 8729 " and " JIS Z 8730 " in the time measuring thermal conductivity sheet surperficial records shows in look mode, taking the brightness L* of " L* " value representation as more than 32.5.
Thermal conductivity evaluation method of the present invention is: in the L*a*b* color specification system that " the JIS Z 8729 " and " JIS Z 8730 " in the time measuring thermal conductivity sheet surperficial records, use the brightness L* with " L* " value representation, evaluate the thermal conductivity of thermal conductivity sheet, described thermal conductivity sheet contains heat conductivity composition, the packing material that described heat conductivity composition contains hardening resin composition, thermal conductivity filler and thermal conductivity filler is arranged along prescribed direction; In thermal conductivity sheet, thermal conductivity filler, along the thickness direction orientation of thermal conductivity sheet, at least contains aluminium nitride as packing material.
Invention effect
According to the present invention, by at least contain aluminium nitride in thermal conductivity sheet, in the L*a*b* color specification system that " JIS Z 8729 " and " JIS Z 8730 " in the time measuring thermal conductivity sheet surperficial records, make brightness L* taking " L* " value representation as more than 32.5, thermal conductivity filler can be along the thickness direction orientation of thermal conductivity sheet, can make the thermal conductivity of thickness direction of thermal conductivity sheet good.
Brief description of the drawings
[Fig. 1] Fig. 1 is the flow chart of an example of the manufacture method for thermal conductivity sheet of the present invention is described.
[Fig. 2] Fig. 2 is the outside drawing of an example of the ultrasonic wave cutting machine that uses in the cut-out operation being illustrated in the manufacture method of thermal conductivity sheet of the present invention.
[Fig. 3] Fig. 3 is the outside drawing that represents an example of slicing device.
[Fig. 4] Fig. 4 is for the flow chart at an example of the alignment process of the manufacture method of other thermal conductivity sheet of the present invention is described.
[Fig. 5] Fig. 5 is the schematic diagram of an example of interim molding procedure, alignment process and the formal molding procedure of the manufacture method for thermal conductivity sheet of the present invention is described.
[Fig. 6] Fig. 6 is the oblique view of an example of the lamilated body that obtains in the alignment process representing in the manufacture method of thermal conductivity sheet of the present invention.
[Fig. 7] Fig. 7 (A) is the oblique view that represents an example of the formal formed body of not implementing pressurization, and Fig. 7 (B) is the oblique view that represents an example implementing the formal formed body after pressurization.
Embodiment
Referring to accompanying drawing, in the following order embodiment of the present invention (hereinafter referred to as the present embodiment) are elaborated.
1. thermal conductivity sheet
2. the manufacture method of thermal conductivity sheet
3. the manufacture method of other thermal conductivity sheet
4. thermal conductivity evaluation method.
<1. thermal conductivity sheet >
The thermal conductivity sheet 1 of the present embodiment contains heat conductivity composition, the packing material that this heat conductivity composition contains hardening resin composition, thermal conductivity filler and thermal conductivity filler is arranged along prescribed direction, thermal conductivity filler is along the thickness direction orientation of thermal conductivity sheet.In the thermal conductivity sheet of the present embodiment, in thermal conductivity sheet, at least contain aluminium nitride, in the L*a*b* color specification system that " the JIS Z 8729 " and " JIS Z 8730 " while measuring thermal conductivity sheet surperficial records, taking the brightness L* of " L* " value representation as more than 32.5.Brightness L* when making to measure thermal conductivity sheet surperficial is more than 32.5, makes the thickness direction orientation of thermal conductivity filler along thermal conductivity sheet, can make the thermal conductivity of thickness direction of thermal conductivity sheet good.
(dependency relation between brightness L* and thermal conductivity in L*a*b* color specification system)
The color of object is made up of brightness (lightness), form and aspect (tone) and 3 key elements of chroma (color saturation) conventionally.At Accurate Determining and while showing these key elements, need they to be quantized to the color specification system showing objectively.Such color specification system for example can be enumerated L*a*b* color specification system.L*a*b* color specification system for example can easily be measured by analyzers such as commercially available spectral photometric colour measuring meters.
L*a*b* color specification system is the color specification system that for example " JIS Z 8729 " and " JIS Z 8730 " record, and wherein each color configuration is represented in the spherical color space.In L*a*b* color specification system, brightness is with the positional representation of the longitudinal axis (z axle) direction, and form and aspect are with the positional representation of peripheral direction, and chroma represents with the distance apart from central shaft.
The position that represents the longitudinal axis (z axle) direction of brightness represents with L*.The value of brightness L* is positive number, and the less brightness of this numeral is lower, has dimmed tendency.Specifically, the value of L* be equivalent to black 0 to be equivalent to white 100 between change.
In the sectional view that the spherical color space is cut off along level in the position of L*=50, the positive direction of x axle is red direction, and the positive direction of y axle is yellow direction, and the negative direction of x axle is green direction, and the negative direction of y axle is blue direction.The position of X-direction represents by the a* that gets-60 to+60 value.The axial position of y represents by the b* that gets-60 to+60 value.Like this, a* and b* are the positive and negative numerals that represents colourity, more approach 0 more black.Form and aspect and chroma are by their a* value and b* value representation.
In L*a*b* color specification system, brightness L* more than 32 turns white, and brightness L* is lower than 32 blackouts.In L*a*b* color specification system, a* is lower than-1 greening, and a* is more than-1 rubescent.B* turns blue lower than-1, exceed+1 jaundice of b*.
For example using L*a*b* color specification system to containing carbon fiber as thermal conductivity filler, while containing aluminium nitride and aluminium oxide as the cross-section determination degree of blackness of the thermal conductivity sheet of packing material, brightness L* more than 32.5 turns white.Its reason is, brightness L* is more than 32.5, and while observing thermal conductivity sheet from the direction vertical with cross section, the area of the thermal conductivity filler in thermal conductivity sheet reduces, the surface that the aluminium oxide of white and aluminium nitride expose thermal conductivity sheet in addition.That is, brightness L* is more than 32.5, means the thickness direction orientation of thermal conductivity filler along thermal conductivity sheet.
On the other hand, using L*a*b* color specification system to containing carbon fiber as thermal conductivity filler, while containing aluminium nitride and aluminium oxide as the cross-section determination degree of blackness of the thermal conductivity sheet of packing material, brightness L* is lower than 32.5 blackouts.Its reason is, brightness L* is lower than 32.5, and while observing thermal conductivity sheet from the direction vertical with cross section, the area of the thermal conductivity filler in thermal conductivity sheet increases, and aluminium oxide and the aluminium nitride of white are difficult to expose from the surface of thermal conductivity sheet in addition.That is, brightness L* is lower than 32.5, means that with brightness L* be 32.5 comparisons when above, and thermal conductivity filler is not along the thickness direction orientation of thermal conductivity sheet.
Conventionally thermal conductivity filler high thermal conductivity is filled in thermal conductivity sheet, the thermal conductivity of thermal conductivity sheet improves.Originally think, for example a large amount of filled bitumen base carbon fibres are as thermal conductivity filler, and thermal conductivity improves.Think, the brightness L* on thermal conductivity sheet surface reduces, and thermal conductivity improves.But obtain high thermal conductivity, be not the content that merely increases thermal conductivity filler, but, not only to add packing material and keep shape, and reduce heat conductivity composition while extruding viscosity, to make thermal conductivity filler be also very important along the thickness direction orientation of thermal conductivity sheet.
The inventor conducts in-depth research, found that, in the L*a*b* color specification system that " JIS Z 8729 " and " JIS Z 8730 " in the time measuring thermal conductivity sheet surperficial records, to there is dependency relation highly between the brightness L* of " L* " value representation and thermal conductivity.Also find, in order to make the thickness direction orientation of thermal conductivity filler along thermal conductivity sheet, compared with the use level of thermal conductivity filler, the use level of the aluminium nitride that thermal conductivity ratio thermal conductivity filler is low has a significant impact.That is, by making at least to contain aluminium nitride in thermal conductivity sheet, and brightness L* while making to measure thermal conductivity sheet surperficial is more than 32.5, makes the thickness direction orientation of thermal conductivity filler along thermal conductivity sheet, can make the thermal conductivity of thickness direction of thermal conductivity sheet good.
(hardening resin composition)
Hardening resin composition contained in thermal conductivity sheet is not particularly limited, for example, can use silicone based bonding agent, acrylate class bonding agent etc.Silicone based bonding agent can use the bonding agent of condensation cured type or addition curable.The content of hardening resin composition is not particularly limited, for example, can be 25-45 volume %.
(thermal conductivity filler)
Thermal conductivity filler for example can use carbon fiber, particularly preferably uses the carbon fiber of asphaltic base.The carbon fiber of asphaltic base is taking pitch as main material, at melt spinning, do not melt and each treatment process such as carbonization after, with 2000-3000 DEG C or exceed the high temperature of 3000 DEG C and heat-treat and graphited carbon fiber.Material asphalt is divided into the isotropic pitch that optics is out of order, do not show deflection, becomes liquid crystal shape, the anisotropic anisotropy pitch of display optical (mesophase pitch) with formation molecules align.The carbon fiber of being manufactured by anisotropy pitch is than the mechanical property excellence of the carbon fiber of being manufactured by isotropic pitch, and electricity and thermal conductivity improve.Therefore preferably use the graphitized carbon fibre of intermediate phase pitch-based.
More than the average fiber length of thermal conductivity filler is preferably 100 μ m.Be more than 100 μ m by making the average fiber length of thermal conductivity filler, thermal conductivity filler is easily arranged in the same direction, therefore can make thermal conductivity sheet more good in the thermal conductivity of thickness direction.
Thermal conductivity filer content in thermal conductivity sheet is preferably 15-25 volume %.Be more than 15 volume % by making the content of thermal conductivity filler, can more effectively reduce thermal resistance value, therefore can make thermal conductivity sheet more good in the thermal conductivity of thickness direction.Be below 25 volume % by making the content of thermal conductivity filler, for example, in the time extruding heat conductivity composition by extruder, can prevent from extruding difficulty.
(packing material)
Packing material be according to heat conductivity composition in the flow velocity difference of thermal conductivity filler, for thermal conductivity filler is easily arranged along prescribed direction, that is, for making thermal conductivity filler easily along extruding direction orientation.Packing material is also for working as thermally conductive materials.
Packing material for example can use aluminium oxide, aluminium nitride, boron nitride, zinc oxide, Si powder, metal dust, at least uses aluminium nitride.Aluminium nitride has nitrogen in its molecule, and this nitrogen hinders the reaction of hardening resin composition, suppresses the rising of heat conductivity composition viscosity.Therefore, by least using aluminium nitride as packing material, when only using alumina particle as packing material compared with, can more effectively make thermal conductivity filler along prescribed direction along the thickness direction orientation of thermal conductivity sheet.Therefore, by least using aluminium nitride as packing material, can make thermal conductivity filler more effectively along the thickness direction orientation of thermal conductivity sheet, therefore, can make the thermal conductivity of thermal conductivity sheet thickness direction good.
In addition, by using the different spherical particle of more than two kinds of particle diameter as packing material, can more effectively make thermal conductivity filler easily be orientated along the thickness direction of thermal conductivity sheet.As a result, in the L*a*b* color specification system that " the JIS Z 8729 " and " JIS Z 8730 " in the time measuring thermal conductivity sheet surperficial records, can be more positively as more than 32.5 taking the brightness L* of " L* " value representation.Like this, by using the different spherical particle of more than two kinds of particle diameter as packing material, make the thickness direction orientation of thermal conductivity filler along thermal conductivity sheet, therefore can make thermal conductivity sheet more good in the thermal conductivity of thickness direction.
The content of the packing material in thermal conductivity sheet is preferably 40-50 volume %.In addition, more than preferably aluminium nitride contains 5.1 volume % in thermal conductivity sheet.Be more than 5.1 volume % by making the content of the aluminium nitride in thermal conductivity sheet, the viscosity that can effectively suppress heat conductivity composition raises, and more effectively makes the thickness direction orientation of thermal conductivity filler along thermal conductivity sheet.As a result, in the L*a*b* color specification system that " the JIS Z 8729 " and " JIS Z 8730 " in the time measuring thermal conductivity sheet surperficial records, can be more effectively as more than 32.5 taking the brightness L* of " L* " value representation.Like this, be more than 5.1 volume % by making the content of aluminium nitride in thermal conductivity sheet, can make thermal conductivity sheet more good in the thermal conductivity of thickness direction.
The average grain diameter of packing material is preferably 0.5-5 μ m.Be below the above 5 μ m of 0.5 μ m by making the average grain diameter of packing material, can be used as thermally conductive materials and fully work, and, in heat conductivity composition, the orientation of thermal conductivity filler is difficult to upset, and therefore can make thermal conductivity sheet 1 more good in the thermal conductivity of thickness direction.
In addition, as mentioned above, while using the different spherical particle of more than two kinds of particle diameter as packing material, preferably making large spherical particle is 2-5 μ m, little spherical particle is 0.3-2 μ m, can more effectively make thus thermal conductivity filler easily be orientated along the thickness direction of thermal conductivity sheet.As a result, in the L*a*b* color specification system that " the JIS Z 8729 " and " JIS Z 8730 " in the time measuring thermal conductivity sheet surperficial records, can be more positively as more than 32.5 taking the brightness L* of " L* " value representation.
It should be noted that, in above-mentioned explanation, with L*a*b* color specification system example, but the selection mode of color specification system is not particularly limited, as long as being scaled the color specification system of L*a*b* color specification system.Can be for example XYZ color specification system, L*C*h color specification system.
<2. the manufacture method > of thermal conductivity sheet
Above-mentioned thermal conductivity sheet 1 for example can be according to following manufacture method manufacture.The manufacture method of the thermal conductivity sheet of the present embodiment as shown in Figure 1, has heat conductivity composition production process S1, orientation procedure S2 and cuts off operation S3.
(heat conductivity composition production process S1)
In heat conductivity composition production process S1, make above-mentioned heat conductivity composition.For example preferred thermal conductivity filler of use level in heat conductivity composition is 15-25 volume %, and packing material is 40-50 volume %.In addition, in heat conductivity composition, preferably contain the above aluminium nitride of 5.1 volume % as packing material.
(orientation procedure S2)
In orientation procedure S2, the heat conductivity composition of making in heat conductivity composition production process S1 is formed as to column, make the length direction orientation of thermal conductivity filler along column simultaneously.In orientation procedure S2, for example, by being expressed in the mould that has been coated with release materials, as shown in Figure 2, can form the column heat conductivity composition 2 of thermal conductivity filler along the length direction L orientation of column.Or, in orientation procedure S2, for example, also the heat conductivity composition of making in heat conductivity composition production process S1 can be coated on the polyester film that has been coated with release materials, form the column heat conductivity composition 2 shown in Fig. 2.
(cutting off operation S3)
Cutting off in operation S3, by ultrasonic wave cutting machine, the direction that the heat conductivity composition of the column forming in orientation procedure S2 2 edges and length direction are intersected vertically cuts into the size of regulation, obtains thermal conductivity sheet 1.
In cut-out operation S3, for example as shown in Figures 2 and 3, by using ultrasonic wave cutting machine 3, with ultrasonic cutter 4 by the heat conductivity composition of column 2 along the direction V section intersecting vertically with the length direction L of the heat conductivity composition 2 of column, can under the state of orientation that keeps thermal conductivity filler, form thermal conductivity sheet 1.Therefore, the orientation of thermal conductivity filler remains on thickness direction, can obtain the thermal conductivity sheet 1 that thermal conduction characteristic is good.
Ultrasonic wave cutting machine 3 as shown in Figure 3, possess the workbench 5 of the heat conductivity composition 2 of placing column, and limit applies the ultrasonic cutter 4 of being cut into slices in ultrasonic vibration limit by the heat conductivity composition of the column on workbench 52.
In workbench 5, on metal travelling carriage 6, be equipped with silicon rubber 7.Travelling carriage 6 can move along prescribed direction by travel mechanism 8, and the bottom of the heat conductivity composition of column 2 being sent to successively to ultrasonic cutter 4 operates.Silicon rubber 7 has the thickness that is enough to the point of a knife that bears ultrasonic cutter 4.In workbench 5, on silicon rubber 7, place the heat conductivity composition 2 of column, coordinate the sectioning of ultrasonic cutter 4, travelling carriage 6 is moved to prescribed direction, the heat conductivity composition of column 2 is delivered to successively to the bottom of ultrasonic cutter 4.
Ultrasonic cutter 4 has: the cutter 9 that the heat conductivity composition of column 2 is cut into slices, the ultrasonic wave Fa Zhen mechanism 10 that tool setting 9 gives ultrasonic vibration, make cutter 9 carry out the elevating mechanism 11 of descending operation.
Cutter 9 be point of a knife towards workbench 5, carry out descending operation by elevating mechanism 11, thus the heat conductivity composition 2 that is positioned over the column on workbench 5 is cut into slices.Size, the material of cutter 9 are determined according to size, the composition etc. of the heat conductivity composition 2 of column.For example cutter 9 is formed by the steel of 10 ° of wide 40mm, thickness 1.5mm, point of a knife angles.
Ultrasonic wave Fa Zhen mechanism 10 gives ultrasonic vibration along the slice direction tool setting 9 of the heat conductivity composition 2 of column, and for example transmission frequency is 20.5kHz, and amplitude is adjustable as 50 μ m, 60 μ m, these 3 stages of 70 μ m.
Such ultrasonic wave cutting machine 3 gives ultrasonic vibration limit by limit to ultrasonic cutter 4 heat conductivity composition 2 of column is cut into slices, and can make the orientation of the thermal conductivity filler of conducting strip 1 remain on the thickness direction of thermal conductivity sheet 1.
On one side give by ultrasonic wave cutting machine 3 the thermal conductivity sheet 1 that ultrasonic vibration is cut into slices on one side, compared with the thermal conductivity sheet of cutting into slices with not giving ultrasonic vibration, thermal resistance is suppressed for lower.Its reason is, ultrasonic wave cutting machine 3 gives ultrasonic vibration along slice direction to ultrasonic cutter 4, and therefore interface resistance is low, is difficult to because of cutter 9 overturnings along the thermal conductivity filler of the thickness direction orientation of thermal conductivity sheet 1.And in the thermal conductivity sheet of cutting into slices not giving ultrasonic vibration, because the frictional resistance of cutter makes the orientation confusion of thermal conductivity filler, reducing being exposed to tangent plane, thermal resistance raises thus.Therefore,, by using ultrasonic wave cutting machine 3, can obtain the thermal conductivity sheet 1 of thermal conduction characteristic excellence.
According to the manufacture method of thermal conductivity sheet as above, can obtain thermal conductivity sheet 1, wherein, thermal conductivity filler is along the thickness direction orientation of thermal conductivity sheet 1, the L*a*b* that " JIS Z 8729 " and " JIS Z 8730 " in the time measuring thermal conductivity sheet 1 surperficial records shows in look mode, taking the brightness L* of " L* " value representation as more than 32.5.
<3. the manufacture method > of other thermal conductivity sheet
Thermal conductivity sheet 1 can be according to manufacture method manufacture as described below., as shown in Figure 4, in the orientation procedure S2 of the manufacture method of above-mentioned thermal conductivity sheet, can there is interim molding procedure S21, alignment process S22 and formal molding procedure S23.According to the manufacture method of such thermal conductivity sheet, can more positively obtain thermal conductivity sheet 1, wherein, in the L*a*b* color specification system that " the JIS Z 8729 " and " JIS Z 8730 " in the time measuring thermal conductivity sheet 1 surperficial records taking the brightness L* of " L* " value representation as more than 32.5.That is, can more positively make the thermal conductivity filler in thermal conductivity sheet 1 arrange in the same direction, can make thermal conductivity sheet 1 more good in the thermal conductivity of thickness direction.It should be noted that, in the following description, for above-mentioned heat conductivity composition production process S1, description is omitted.
(interim molding procedure S21)
In interim molding procedure S21, as shown in Fig. 5 (A), the heat conductivity composition of making in heat conductivity composition production process S1 12 use extruders 13 are extruded, be shaped to thermal conductivity filler wherein along the interim formed body 14 (hereinafter referred to as interim formed body 14) of elongate column of extruding direction orientation.
Extruder 13 for example, as shown in Fig. 5 (A), is configured to the cartridge type of elongate, preferably discharges diameter reduction compared with the bore W2 of peristome 12B of heat conductivity composition 12 1 sides and the internal diameter W1 of body 12A.In extruder 13, the internal diameter W1 of body 12A is to be coniform by the assigned position of length direction to extruding direction diameter reduction, and the bore W2 of peristome 12B can diameter reduction compared with the internal diameter W1 of body 12A.By extruder 13 such heat conductivity composition 12 use is extruded, in extruder 13, heat conductivity composition 12 is passed through towards the part of diameter reduction compared with the internal diameter W1 of body 12A, thus, thermal conductivity filler is easily along extruding direction.Can more positively make thus the length direction orientation of thermal conductivity filler along interim formed body 14.
For example, when the thermal conductivity filer content in heat conductivity composition 12 is 15-25 volume %, preferably the bore W2 of the peristome 12B of extruder 13 is 1.5-9.5mm left and right.In this case, be more than 1.5mm by making the bore W2 of peristome 12B, in the time that heat conductivity composition 12 use extruders 13 are extruded, can prevent from extruding difficulty.Be below 9.5mm by making the bore W2 of peristome 12B, the orientation of thermal conductivity filler is difficult to confusion, therefore can make thermal conductivity sheet 1 more good in the thermal conductivity of thickness direction.
In extruder 13, the cross sectional shape of peristome 12B for example can be set as round shape, triangular shape, rectangular-shaped, square shape, is preferably set as rectangular-shaped or square shape.Be rectangular-shaped or square shape by making the cross sectional shape of peristome 12B, interim formed body 14 can be prism-shaped.Therefore, in alignment process S22, in the direction vertical with length direction, arrange in the mode of adjoining making multiple interim formed bodys 14, and the multiple interim formed body 14 of arranging is disposed in to the direction approximately intersecting vertically with orientation, while obtaining lamilated body 14A (hereinafter referred to as lamilated body 14A), between lamilated body 14A, be difficult to produce gap.Thus, in lamilated body 14A, be difficult to contain bubble, therefore, in formal molding procedure S23, can obtain the formal formed body 16 that anti-flammability is more excellent.
Interim formed body 14 makes thermal conductivity filler along extruding direction orientation by extruder 13, is the shape of elongate column, for example elongated quadrangular shape, elongated triangular prism shape, elongated cylindric.
(alignment process S22)
In alignment process S22, for example, as shown in Fig. 5 (B), Fig. 5 (C), Fig. 6, the multiple interim formed body 14 of moulding in interim molding procedure S21 is arranged in the mode of adjoining in the direction intersecting vertically with length direction, obtained lamilated body 14A.For example, in alignment process S22, interim formed body 14 is arranged in the frame 15 of regulation, interim formed body 14 is arranged to rectangular-shaped or cubic, obtain lamilated body 14A.In formal molding procedure S23, in the time making formal formed body 16 moulding, frame 15 uses as the fixture of the fit 14A of fixed bed, and moderate finite deformation occurs the fit 14A of preventing layer.Frame 15 is for example formed by metal.
(formal molding procedure S23)
In formal molding procedure S23, for example, as shown in Fig. 5 (D), solidify by the lamilated body 14A that makes to obtain in alignment process S22, as shown in Fig. 5 (E) and Fig. 7 (A), (B), be shaped to the wherein interim formed body 14 integrated formal formed body 16 each other of the fit 14A of constituting layer.The curing method of lamilated body 14A for example can be enumerated: method lamilated body 14A being heated by heater, or by heating pressue device, lamilated body 14A is heated the method for pressurization.Using acrylate when forming the hardening resin composition of heat conductivity composition 12, for example, by contain isocyanate compound in heat conductivity composition 12, can make lamilated body 14A solidify at normal temperatures.
Make the curing method of these lamilated bodies 14A preferably heat the method for pressurization to lamilated body 14A by heating pressue device,, in the time that lamilated body 14A is solidified, in the upper pressurization of direction (vertical direction) (press) intersecting vertically with the length direction of the multiple interim formed body 14 of the fit 14A of constituting layer.Like this, by lamilated body 14A pressurization, can positively bubble be got rid of from lamilated body 14A, therefore, in formal molding procedure S23, can obtain the formal formed body 16 that anti-flammability is more excellent.
Cutting off in operation S4, by ultrasonic wave cutting machine 3, the formal formed body 16 of moulding in formal molding procedure S23 is cut into the size of regulation along the direction intersecting vertically with the length direction of interim formed body 14.In order to obtain thermal conductivity sheet 1, formal formed body 16 is sliced into each thermal conductivity sheet 1 by ultrasonic wave cutting machine 3.Use ultrasonic wave cutting machine 3, with ultrasonic cutter 4, formal formed body 16, along the direction of arrow section intersecting vertically with the length direction of interim formed body 14, can be formed to thermal conductivity sheet 1 thus under the state of orientation that keeps thermal conductivity filler.The orientation that therefore can obtain thermal conductivity filler remains on thickness direction, the thermal conductivity sheet 1 that thermal conduction characteristic is good.
<4. the evaluation method > of color
The evaluation method of the color of the present embodiment is: in the L*a*b* color specification system that " the JIS Z 8729 " and " JIS Z 8730 " in the time measuring above-mentioned thermal conductivity sheet 1 surperficial records, the thermal conductivity of thermal conductivity sheet 1 is evaluated in use with the brightness L* of " L* " value representation.For example, the brightness L* while measuring thermal conductivity sheet 1 surperficial is 32.5 when above, and thermal conductivity filler is orientated along the thickness direction of thermal conductivity sheet 1, and therefore thermal conductivity sheet 1 can be evaluated as well in the thermal conductivity of thickness direction.Brightness L* while measuring thermal conductivity sheet 1 surperficial was lower than 32.5 o'clock, and thermal conductivity filler is not along the thickness direction orientation of thermal conductivity sheet 1, and therefore thermal conductivity sheet 1 can be evaluated as bad in the thermal conductivity of thickness direction.
Embodiment
Below embodiments of the invention are described.It should be noted that, the present invention is not limited to these embodiment.In the present embodiment, for the thermal conductivity sheet of embodiment 1-6 and comparative example 1-3 gained, orientation, thermal conductivity and outward appearance to its asphalt base carbon fiber are evaluated.
(embodiment 1)
In embodiment 1, in the aqueous organic siliconresin of addition reaction-type of two component, disperse alumina particle (packing material) (Deuki Kagaku Kogyo Co., Ltd's manufacture of 24 volume % average grain diameter 3 μ m, ProductName: DAW-03), the aluminum nitride particle (manufacture of the Tokuyama of Co., Ltd. (ト Network ヤ マ) company) of 18.3 volume % average grain diameter 1 μ m, 24.1 volume % average major axis length 150 μ m, (Teijin Ltd manufactures the asphalt base carbon fiber (thermal conductivity filler) of average minor axis length 8 μ m, trade name: ラ ヒ ー マ R-A301), prepare organosilicon resin composition (heat conductivity composition).The aqueous organic siliconresin of two component addition reaction-type is that 16.8 volume % organosilicon A liquid (having the organopolysiloxane of vinyl) and 18.8 volume % organosilicon B liquid (having the organopolysiloxane of H-Si base) are mixed.Gained organosilicon resin composition is extruded in the mould that has been coated with release materials (20mm × 20mm), be shaped to organosilicon formed body.Gained organosilicon formed body is solidified 1 hour with 100 DEG C in baking oven, make organosilicon solidfied material.Gained organosilicon solidfied material is cut into thickness 2.0mm with ultrasonic cutter, obtain the thermal conductivity sheet of thickness 2.0mm.The section speed of ultrasonic cutter is 50mm per second.The ultrasonic vibration that gives ultrasonic cutter is: send out vibration frequency 20.5kHz, amplitude 60 μ m.
(embodiment 2)
In embodiment 2, in the aqueous organic siliconresin of two component addition reaction-type that 16.8 volume % organosilicon A liquid and 18.8 volume % organosilicon B liquid form, disperse the alumina particle of 11.7 volume % average grain diameter 3 μ m (Deuki Kagaku Kogyo Co., Ltd manufactures mixing, ProductName: DAW-03), the aluminum nitride particle (manufacture of Tokuyama company of Co., Ltd.) of 31.2 volume % average grain diameter 1 μ m, 23.5 volume % average major axis length 150 μ m, (Teijin Ltd manufactures the asphalt base carbon fiber of average minor axis length 8 μ m, trade name: ラ ヒ ー マ R-A301), prepare organosilicon resin composition, in addition similarly to Example 1, obtain thermal conductivity sheet.
(embodiment 3)
In embodiment 3, mixing 18.8 volume % organosilicon A liquid, in the aqueous organic siliconresin of two component addition reaction-type that 18.8 volume % organosilicon B liquid form, disperse alumina particle (Deuki Kagaku Kogyo Co., Ltd's manufacture of 20.2 volume % average grain diameter 3 μ m, ProductName: DAW-03), the aluminum nitride particle (manufacture of Tokuyama company of Co., Ltd.) of 20.1 volume % average grain diameter 1 μ m, 24.1 volume % average major axis length 150 μ m, (Teijin Ltd manufactures the asphalt base carbon fiber of average minor axis length 8 μ m, trade name: ラ ヒ ー マ R-A301), prepare organosilicon resin composition, in addition similarly to Example 1, obtain thermal conductivity sheet.
(embodiment 4)
In embodiment 4, mixing 18.8 volume % organosilicon A liquid, in the aqueous organic siliconresin of two component addition reaction-type that 18.8 volume % organosilicon B liquid form, disperse alumina particle (Deuki Kagaku Kogyo Co., Ltd's manufacture of 28 volume % average grain diameter 3 μ m, ProductName: DAW-03), the aluminum nitride particle (manufacture of Tokuyama company of Co., Ltd.) of 14.3 volume % average grain diameter 1 μ m, 20.1 volume % average major axis length 150 μ m, (Teijin Ltd manufactures the asphalt base carbon fiber of average minor axis length 8 μ m, trade name: ラ ヒ ー マ R-A301), prepare organosilicon resin composition.Gained organosilicon resin composition is coated on the polyester film (stacked coating) that has been coated with release materials, manufactures organosilicon formed body.Gained organosilicon formed body is heated 1 hour with 100 DEG C in baking oven, make organosilicon solidfied material.Gained organosilicon solidfied material is cut into thickness 2.0mm with ultrasonic cutter, obtain the thermal conductivity sheet of thickness 2.0mm.The section speed of ultrasonic cutter is 50mm per second.The ultrasonic vibration that gives ultrasonic cutter is: send out vibration frequency 20.5kHz, amplitude 60 μ m.
(embodiment 5)
In embodiment 5, mixing 18.8 volume % organosilicon A liquid, in the aqueous organic siliconresin of two component addition reaction-type that 18.8 volume % organosilicon B liquid form, disperse alumina particle (Deuki Kagaku Kogyo Co., Ltd's manufacture of 37.2 volume % average grain diameter 3 μ m, ProductName: DAW-03), the aluminum nitride particle (manufacture of Tokuyama company of Co., Ltd.) of 5.1 volume % average grain diameter 1 μ m, 20.1 volume % average major axis length 150 μ m, (Teijin Ltd manufactures the asphalt base carbon fiber of average minor axis length 8 μ m, trade name: ラ ヒ ー マ R-A301), prepare organosilicon resin composition, in addition similarly to Example 1, obtain thermal conductivity sheet.
(embodiment 6)
In embodiment 6, in the aqueous organic siliconresin of two component addition reaction-type forming at mixing 17.1 volume % organosilicon A liquid, 17.1 volume % organosilicon B liquid, disperse the aluminum nitride particle (manufacture of Tokuyama company of Co., Ltd.) of 42.6 volume % average grain diameter 1 μ m, asphalt base carbon fiber (Teijin Ltd's manufacture of 23.2 volume % average major axis length 150 μ m, average minor axis length 8 μ m, trade name: ラ ヒ ー マ R-A301), prepare organosilicon resin composition, in addition similarly to Example 1, obtain thermal conductivity sheet.
(comparative example 1)
In comparative example 1, in the aqueous organic siliconresin of two component addition reaction-type forming at mixing 18.8 volume % organosilicon A liquid, 18.8 volume % organosilicon B liquid, disperse alumina particle (Deuki Kagaku Kogyo Co., Ltd's manufacture of 42.3 volume % average grain diameter 3 μ m, ProductName: DAW-03), (Teijin Ltd manufactures for the asphalt base carbon fiber of 24.1 volume % average major axis length 150 μ m, average minor axis length 8 μ m, trade name: ラ ヒ ー マ R-A301), prepare organosilicon resin composition, in addition similarly to Example 1, obtain thermal conductivity sheet.
(comparative example 2)
In comparative example 2, in the aqueous organic siliconresin of two component addition reaction-type forming at mixing 18.8 volume % organosilicon A liquid, 18.8 volume % organosilicon B liquid, disperse alumina particle (Deuki Kagaku Kogyo Co., Ltd's manufacture of 41.3 volume % average grain diameter 3 μ m, ProductName: DAW-03), (Teijin Ltd manufactures for the asphalt base carbon fiber of 20.1 volume % average major axis length 150 μ m, average minor axis length 8 μ m, trade name: ラ ヒ ー マ R-A301), prepare organosilicon resin composition, in addition similarly to Example 4, obtain thermal conductivity sheet.
(comparative example 3)
In comparative example 3, in the aqueous organic siliconresin of two component addition reaction-type forming at mixing 18 volume % organosilicon A liquid, 18 volume % organosilicon B liquid, disperse alumina particle (Deuki Kagaku Kogyo Co., Ltd's manufacture of 44.8 volume % average grain diameter 3 μ m, ProductName: DAW-03), (Teijin Ltd manufactures for the asphalt base carbon fiber of 19.2 volume % average major axis length 150 μ m, average minor axis length 8 μ m, trade name: ラ ヒ ー マ R-A301), prepare organosilicon resin composition, in addition similarly to Example 1, obtain thermal conductivity sheet.
The summary sheets such as the condition of embodiment 1-embodiment 6, comparative example 1-comparative example 3 are shown in Table 1.
[table 1]
(about the orientation of asphalt base carbon fiber)
The orientation of asphalt base carbon fiber is observed the cross section of thermal conductivity sheet by SEM and is measured to evaluate with the degree of blackness of L*a*b* color specification system.
Observe the cross section of the thermal conductivity sheet of gained in embodiment 1-embodiment 6 by SEM, found that the thickness direction orientation of asphalt base carbon fiber to thermal conductivity sheet.The particularly thermal conductivity sheet of embodiment 1-embodiment 3, embodiment 5 and embodiment 6 gained, with the thermal conductivity sheet comparison of embodiment 4 gained, asphalt base carbon fiber is orientated along the thickness direction of thermal conductivity sheet better.Think that its reason is due in embodiment 1-embodiment 3, embodiment 5 and embodiment 6, is expressed in the mould that has been coated with release materials and is shaped to organosilicon formed body.
On the other hand, the cross section of the thermal conductivity sheet by SEC observation and comparison example 1-comparative example 3 gained, found that, with the thermal conductivity sheet comparison of embodiment 1-embodiment 6 gained, asphalt base carbon fiber is the thickness direction orientation to thermal conductivity sheet not.
For the cross section of thermal conductivity sheet, also use L*a*b* color specification system to measure degree of blackness.Adopt the color showing method representing using the L*a*b* color specification system of " JIS Z 8729 " defined as degree of blackness index.Adopt the mensuration of the degree of blackness of L*a*b* color specification system to use spectrophotometer (ProductName: CM-700d, Konica Minolta Sensing Co., Ltd manufactures).
The thermal conductivity sheet of gained in embodiment 1-embodiment 6, in the L*a*b* color specification system that " the JIS Z 8729 " in the time measuring thermal conductivity sheet surperficial records, taking the brightness L* of " L* " value representation as more than 32.5.And in the thermal conductivity sheet of comparative example 1-comparative example 3 gained, in the L*a*b* color specification system that " the JIS Z 8729 " in the time measuring thermal conductivity sheet surperficial records, with the brightness L* of " L* " value representation lower than 32.5.By this result, think the thermal conductivity sheet of embodiment 1-embodiment 6 gained, with the thermal conductivity sheet comparison of comparative example 1-comparative example 3 gained, asphalt base carbon fiber is more effectively along the thickness direction orientation of thermal conductivity sheet.
From these results, in thermal conductivity sheet, contain aluminium nitride, and in the L*a*b* color specification system in the time measuring thermal conductivity sheet surperficial, taking the brightness L* of " L* " value representation as more than 32.5, thus, make the thickness direction orientation of asphalt base carbon fiber along thermal conductivity sheet, can make thermal conductivity sheet good in the thermal conductivity of thickness direction.
(about the evaluation of thermal conductivity)
The thermal conductivity measurement result of the thermal conductivity sheet of embodiment 1-embodiment 6, comparative example 1-comparative example 3 gained is as shown in table 1.The evaluation of thermal conductivity is carried out according to the assay method of ASTM-D5470.
In the thermal conductivity sheet of embodiment 1-embodiment 6 gained, in thermal conductivity sheet cross section entirety, thermal conductivity sheet is 22.3-33.1W/mK in the thermal conductivity of thickness direction, and the thermal conductivity of known thickness direction is good.Think that its reason is, in the thermal conductivity sheet of embodiment 1-embodiment 6 gained, in L*a*b* color specification system in the time measuring thermal conductivity sheet surperficial, taking the brightness L* of " L* " value representation as more than 32.5, therefore, asphalt base carbon fiber, along the thickness direction orientation of thermal conductivity sheet, can make thermal conductivity sheet good in the thermal conductivity of thickness direction.
On the other hand, the thermal conductivity of the thermal conductivity sheet of comparative example 1-comparative example 3 gained is below 20.2W/mK, thermal conductivity sheet comparison with embodiment 1-embodiment 6 gained, the thermal conductivity of known thickness direction is bad, thinks that its reason is, in the thermal conductivity sheet of comparative example 1-comparative example 3 gained, in thermal conductivity sheet, do not contain aluminium nitride, in addition, in the L*a*b* color specification system adopting in the time measuring thermal conductivity sheet surface, do not reach more than 32.5 with the brightness L* of " L* " value representation.
(about ocular estimate)
The evaluation of fraction defective is, in the time being sliced into thermal conductivity sheet by organosilicon solidfied material, being involved in the number in bubble or thermal conductivity sheet with the sheet of through hole carrying out according to the surface of thermal conductivity sheet.Have or not in bubble and sheet and have or not through hole, judge by the cross section of visual thermal conductivity sheet.
In the thermal conductivity sheet of embodiment 1-embodiment 6 gained, the surface of thermal conductivity sheet is not involved in bubble, does not have through hole in thermal conductivity sheet yet, and therefore fraction defective is lower than 5%, lower.
And in the thermal conductivity sheet of comparative example 1 gained, surface is involved in bubble, in sheet, there is through hole in addition, therefore fraction defective is 28%, higher.This can think owing to not containing aluminium nitride, the therefore bad dispersibility of organosilicon resin composition in thermal conductivity sheet.
The thermal conductivity sheet of comparative example 2 gained is to manufacture by stacked coating, therefore compares with comparative example 1, and the amount of bubble reduces, and compared with comparative example 1, can reduce fraction defective in addition, but the orientation confusion of asphalt base carbon fiber, and the deviation of thermal conductivity is large.This can think owing to not containing aluminium nitride in thermal conductivity sheet, and cause by stacked coating making organosilicon formed body.
In the thermal conductivity sheet of comparative example 3 gained, the surface of thermal conductivity sheet is not involved in bubble, and does not have through hole in thermal conductivity sheet, and therefore fraction defective is lower than 5%, lower.But compare with embodiment 1-embodiment 6, thermal conductivity is bad.This thinks not contain aluminium nitride in the thermal conductivity sheet due to comparative example 3 gained, and the use level of aluminium oxide too much causes.
Symbol description
1 thermal conductivity sheet, 2 column heat conductivity compositions, 3 ultrasonic wave cutting machines, 4 ultrasonic cutters, 5 workbench, 6 travelling carriages, 7 silicon rubber, 8 travel mechanisms, 9 cuttves, 10 ultrasonic wave Fa Zhen mechanisms, 11 elevating mechanisms, 12 heat conductivity compositions, 13 extruders, 14 interim formed bodys, 14A lamilated body, 15 frames, 16 formal formed bodys.

Claims (8)

1. a thermal conductivity sheet, this thermal conductivity sheet contains heat conductivity composition, the packing material that this heat conductivity composition contains hardening resin composition, thermal conductivity filler and described thermal conductivity filler is arranged along prescribed direction, wherein,
Described thermal conductivity filler is orientated along the thickness direction of this thermal conductivity sheet,
At least contain aluminium nitride as described packing material,
In the L*a*b* color specification system that " JIS Z 8729 " and " JIS Z 8730 " in the time measuring this thermal conductivity sheet surperficial records, taking the brightness L* of " L* " value representation as more than 32.5.
2. the thermal conductivity sheet of claim 1, wherein, this thermal conductivity sheet contains described aluminium nitride more than 5.1 volume %.
3. the thermal conductivity sheet of claim 2, wherein, this thermal conductivity sheet contains the spherical particle different from the particle diameter of described aluminium nitride as described packing material.
4. the thermal conductivity sheet of claim 3, wherein, described spherical particle is alumina particle.
5. the thermal conductivity sheet of any one in claim 1-4, wherein, described thermal conductivity filler is carbon fiber, average fiber length is more than 100 μ m.
6. a manufacture method for thermal conductivity sheet, it has following operation:
Heat conductivity composition production process, wherein, makes heat conductivity composition, the packing material that this heat conductivity composition contains hardening resin composition, thermal conductivity filler and described thermal conductivity filler is arranged along prescribed direction;
Orientation procedure, wherein, is formed as column by the heat conductivity composition of making in described heat conductivity composition production process, makes the length direction orientation of described thermal conductivity filler along described column simultaneously; With
Cut off operation, wherein, by ultrasonic wave cutting machine, the heat conductivity composition of described column is cut into the size of regulation along the direction intersecting vertically with length direction, obtain thermal conductivity sheet;
In described thermal conductivity sheet, described thermal conductivity filler is along the thickness direction orientation of described thermal conductivity sheet, at least contain aluminium nitride as described packing material, the L*a*b* that " JIS Z 8729 " and " JIS Z 8730 " in the time measuring described thermal conductivity sheet surperficial records shows in look mode, taking the brightness L* of " L* " value representation as more than 32.5.
7. the manufacture method of the thermal conductivity sheet of claim 6, wherein,
Described orientation procedure comprises following operation:
Interim molding procedure, wherein, extrudes the heat conductivity composition extruder of making in described heat conductivity composition production process, is shaped to wherein said thermal conductivity filler along the interim formed body of elongate column of extruding direction orientation;
Alignment process, wherein, arranges in the direction intersecting vertically with length direction multiple interim formed bodys, and the multiple interim formed body of arranging is disposed in and the substantially vertical crossing direction of described orientation in the mode of adjoining, obtain lamilated body; With
Formal molding procedure, wherein, by described lamilated body is solidified, is shaped to the wherein multiple interim formed body integrated formal formed body each other of constituting layer zoarium;
In described cut-out operation, by ultrasonic wave cutting machine, cut into given size along the direction intersecting vertically with the length direction of described formal formed body, obtain described thermal conductivity sheet.
8. a thermal conductivity evaluation method, wherein, in the L*a*b* color specification system that " JIS Z 8729 " and " JIS Z 8730 " in the time measuring the surface color of thermal conductivity sheet records, use the brightness L with " L* " value representation, evaluate the thermal conductivity of described thermal conductivity sheet, wherein said thermal conductivity sheet contains heat conductivity composition, the packing material that this heat conductivity composition contains hardening resin composition, thermal conductivity filler and described thermal conductivity filler is arranged along prescribed direction;
In described thermal conductivity sheet, described thermal conductivity filler, along the thickness direction orientation of this thermal conductivity sheet, at least contains aluminium nitride as described packing material.
CN201280061296.7A 2011-12-20 2012-12-18 The manufacture method of thermal conductivity piece and thermal conductivity piece Active CN103975429B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201810153894.6A CN108384248B (en) 2011-12-20 2012-12-18 Thermally conductive sheet and method for producing thermally conductive sheet

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
JP2011-278788 2011-12-20
JP2011278788A JP6034562B2 (en) 2011-12-20 2011-12-20 Thermally conductive sheet and method for producing the thermally conductive sheet
PCT/JP2012/082817 WO2013094613A1 (en) 2011-12-20 2012-12-18 Thermally conductive sheet and method for manufacturing thermally conductive sheet

Related Child Applications (1)

Application Number Title Priority Date Filing Date
CN201810153894.6A Division CN108384248B (en) 2011-12-20 2012-12-18 Thermally conductive sheet and method for producing thermally conductive sheet

Publications (2)

Publication Number Publication Date
CN103975429A true CN103975429A (en) 2014-08-06
CN103975429B CN103975429B (en) 2018-03-30

Family

ID=48668500

Family Applications (2)

Application Number Title Priority Date Filing Date
CN201810153894.6A Active CN108384248B (en) 2011-12-20 2012-12-18 Thermally conductive sheet and method for producing thermally conductive sheet
CN201280061296.7A Active CN103975429B (en) 2011-12-20 2012-12-18 The manufacture method of thermal conductivity piece and thermal conductivity piece

Family Applications Before (1)

Application Number Title Priority Date Filing Date
CN201810153894.6A Active CN108384248B (en) 2011-12-20 2012-12-18 Thermally conductive sheet and method for producing thermally conductive sheet

Country Status (4)

Country Link
JP (1) JP6034562B2 (en)
CN (2) CN108384248B (en)
TW (1) TWI611013B (en)
WO (1) WO2013094613A1 (en)

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105308740A (en) * 2013-06-19 2016-02-03 迪睿合株式会社 Thermally conductive sheet and process for manufacturing thermally conductive sheet
CN107004651A (en) * 2014-12-25 2017-08-01 迪睿合株式会社 Manufacture method, thermally conductive sheet and the semiconductor device of thermally conductive sheet
CN107022196A (en) * 2016-02-02 2017-08-08 中兴通讯股份有限公司 Heat Conduction Material, its preparation method and heat-conducting piece
CN108495897A (en) * 2016-02-01 2018-09-04 阪东化学株式会社 Heat conductivity synthetic resin
CN110191925A (en) * 2017-01-19 2019-08-30 国立大学法人福井大学 High conductivity material and its manufacturing method
CN110625877A (en) * 2019-09-05 2019-12-31 上海阿莱德实业股份有限公司 Preparation method of heat-conducting interface material
CN112041411A (en) * 2018-12-25 2020-12-04 富士高分子工业株式会社 Thermally conductive composition and thermally conductive sheet using same
CN112712944A (en) * 2020-12-24 2021-04-27 武汉肯达科讯科技有限公司 High-thermal-conductivity insulating gasket and preparation method thereof
CN114106564A (en) * 2021-11-17 2022-03-01 深圳市鸿富诚屏蔽材料有限公司 Oriented heat-conducting gel, preparation method and application thereof
CN114746486A (en) * 2020-02-21 2022-07-12 积水保力马科技株式会社 Thermally conductive sheet and method for producing same

Families Citing this family (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2015073067A (en) * 2013-09-06 2015-04-16 バンドー化学株式会社 Thermally conductive resin molded product
CN106573779B (en) * 2014-12-02 2021-06-18 积水化学工业株式会社 Heat conductive sheet and method for manufacturing same
CN106810876B (en) * 2015-12-02 2020-11-10 中国科学院金属研究所 Composite material with directionally arranged fillers and preparation method thereof
JP6963100B2 (en) * 2018-11-16 2021-11-05 富士高分子工業株式会社 Thermally conductive sheet and its manufacturing method
KR102509813B1 (en) * 2018-12-25 2023-03-14 후지고분시고오교오가부시끼가이샤 Thermally conductive composition and thermally conductive sheet using the same
JP7458775B2 (en) * 2019-12-24 2024-04-01 デクセリアルズ株式会社 Method for manufacturing thermally conductive molded body
CN115141460B (en) * 2021-03-30 2023-09-01 太阳油墨(苏州)有限公司 Thermosetting resin composition, cured product, and electronic component
JP2023120623A (en) * 2022-02-18 2023-08-30 信越化学工業株式会社 Heat-conductive sheet and manufacturing method of heat-conductive sheet
JP2023179989A (en) * 2022-06-08 2023-12-20 デクセリアルズ株式会社 Laminate and method for manufacturing the same
JP2023179996A (en) * 2022-06-08 2023-12-20 デクセリアルズ株式会社 Laminate and method for manufacturing the same
JP2023179992A (en) * 2022-06-08 2023-12-20 デクセリアルズ株式会社 Laminate and method for manufacturing the same

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2000345040A (en) * 1999-06-02 2000-12-12 Denki Kagaku Kogyo Kk Manufacture of heat-conductive silicone molding
JP2001294676A (en) * 2000-04-13 2001-10-23 Jsr Corp Heat-conductive sheet, method for producing heat- conductive sheet and radiating structure using heat- conductive sheet
CN101087511A (en) * 2006-06-08 2007-12-12 保力马科技株式会社 Thermally conductive forming body and method of manufacturing the same
WO2008085999A1 (en) * 2007-01-10 2008-07-17 Momentive Performance Materials Inc. Thermal interface materials and methods for making thereof
CN101275035A (en) * 2007-03-27 2008-10-01 丰田合成株式会社 Low electric conductivity high heat radiation polymeric composition and molded body

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2006124206A (en) * 2004-10-27 2006-05-18 Sumitomo Electric Ind Ltd Degreased intermediate for aluminum nitride and sintered compact

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2000345040A (en) * 1999-06-02 2000-12-12 Denki Kagaku Kogyo Kk Manufacture of heat-conductive silicone molding
JP2001294676A (en) * 2000-04-13 2001-10-23 Jsr Corp Heat-conductive sheet, method for producing heat- conductive sheet and radiating structure using heat- conductive sheet
CN101087511A (en) * 2006-06-08 2007-12-12 保力马科技株式会社 Thermally conductive forming body and method of manufacturing the same
WO2008085999A1 (en) * 2007-01-10 2008-07-17 Momentive Performance Materials Inc. Thermal interface materials and methods for making thereof
CN101275035A (en) * 2007-03-27 2008-10-01 丰田合成株式会社 Low electric conductivity high heat radiation polymeric composition and molded body

Cited By (20)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105308740A (en) * 2013-06-19 2016-02-03 迪睿合株式会社 Thermally conductive sheet and process for manufacturing thermally conductive sheet
US10012453B2 (en) 2013-06-19 2018-07-03 Dexerials Corporation Thermally conductive sheet and method for producing thermally conductive sheet
CN105308740B (en) * 2013-06-19 2018-09-21 迪睿合株式会社 The preparation method of heat conductive sheet and heat conductive sheet
CN107004651A (en) * 2014-12-25 2017-08-01 迪睿合株式会社 Manufacture method, thermally conductive sheet and the semiconductor device of thermally conductive sheet
CN107004651B (en) * 2014-12-25 2019-07-12 迪睿合株式会社 Manufacturing method, thermally conductive sheet and the semiconductor device of thermally conductive sheet
CN108495897A (en) * 2016-02-01 2018-09-04 阪东化学株式会社 Heat conductivity synthetic resin
CN108495897B (en) * 2016-02-01 2021-09-14 阪东化学株式会社 Heat conductive resin molded article
CN107022196A (en) * 2016-02-02 2017-08-08 中兴通讯股份有限公司 Heat Conduction Material, its preparation method and heat-conducting piece
CN110191925A (en) * 2017-01-19 2019-08-30 国立大学法人福井大学 High conductivity material and its manufacturing method
CN112041411A (en) * 2018-12-25 2020-12-04 富士高分子工业株式会社 Thermally conductive composition and thermally conductive sheet using same
WO2021043052A1 (en) * 2019-09-05 2021-03-11 上海阿莱德实业股份有限公司 Method for preparing thermally conductive interface material
CN110625877B (en) * 2019-09-05 2021-06-08 上海阿莱德实业股份有限公司 Preparation method of heat-conducting interface material
CN110625877A (en) * 2019-09-05 2019-12-31 上海阿莱德实业股份有限公司 Preparation method of heat-conducting interface material
US20220184861A1 (en) * 2019-09-05 2022-06-16 Shanghai Allied Industrial Co., Ltd. Preparation Method of Heat-Conducting Interface Material
EP4026679A4 (en) * 2019-09-05 2022-10-26 Shanghai Allied Industrial Co., Ltd. Method for preparing thermally conductive interface material
CN114746486A (en) * 2020-02-21 2022-07-12 积水保力马科技株式会社 Thermally conductive sheet and method for producing same
CN114746486B (en) * 2020-02-21 2023-11-07 积水保力马科技株式会社 Thermally conductive sheet and method for producing same
CN112712944A (en) * 2020-12-24 2021-04-27 武汉肯达科讯科技有限公司 High-thermal-conductivity insulating gasket and preparation method thereof
CN114106564A (en) * 2021-11-17 2022-03-01 深圳市鸿富诚屏蔽材料有限公司 Oriented heat-conducting gel, preparation method and application thereof
CN114106564B (en) * 2021-11-17 2023-08-29 深圳市鸿富诚新材料股份有限公司 Oriented heat conduction gel, preparation method and application thereof

Also Published As

Publication number Publication date
CN103975429B (en) 2018-03-30
CN108384248A (en) 2018-08-10
JP2013131563A (en) 2013-07-04
TW201341519A (en) 2013-10-16
CN108384248B (en) 2021-10-19
TWI611013B (en) 2018-01-11
WO2013094613A1 (en) 2013-06-27
JP6034562B2 (en) 2016-11-30

Similar Documents

Publication Publication Date Title
CN103975429A (en) Thermally conductive sheet and method for manufacturing thermally conductive sheet
US10012453B2 (en) Thermally conductive sheet and method for producing thermally conductive sheet
CN106810877B (en) Heat-conducting interface material and application thereof
US9156700B2 (en) Process for producing unitary graphene materials
CN103713009B (en) The assay method of thermal expansivity
CN101275035A (en) Low electric conductivity high heat radiation polymeric composition and molded body
CN105283952A (en) Thermally conductive sheet, method for producing same, and semiconductor device
US20220289932A1 (en) Thermally conductive sheet and method for producing same
US20090251864A1 (en) Method for integrating heat transfer members,and an led device
CN106810876B (en) Composite material with directionally arranged fillers and preparation method thereof
CN108495897A (en) Heat conductivity synthetic resin
CN103897241A (en) Heat conductive plastics and manufacturing method thereof
CN109943075A (en) A kind of preparation method of the graphene thermally conductive silicone rubber composite material of magnetic aligning
KR20200075513A (en) Method for manufacturing multiple structure and high-heat radiation parts by controling packing density of carbon material, and multiple structure and high-heat radiation parts by manufactured thereof
KR101899854B1 (en) Heat-dissipating filler, sheet and production method for same
JP2013131564A (en) Heat conductive sheet, semiconductor device using the heat conductive sheet, and method of manufacturing semiconductor device
CN109553908A (en) Heat-conducting interface material for electronic equipment dissipating heat
CN114096619B (en) Heat conductive sheet and method for manufacturing the same
CN206960817U (en) A kind of display panel
JP7076871B1 (en) Thermal conductivity sheet
KR20120130866A (en) Composition of film for dissipating heat, and manufacturing method of film for dissipating heat using thereof
CN107953628B (en) Three-dimensional high-thermal-conductivity gasket and preparation method thereof
Fang et al. Enhancing thermal conductivity of spherical boron nitride/silicone rubber composites by matching interfacial modulus
KR101619631B1 (en) Manufacturing method of thermal interface pad
KR101611513B1 (en) The processing method of thermally conductive adhesive tape and the tape using the same

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant