CN103764733B - 导热性片材的制备方法 - Google Patents
导热性片材的制备方法 Download PDFInfo
- Publication number
- CN103764733B CN103764733B CN201380002853.2A CN201380002853A CN103764733B CN 103764733 B CN103764733 B CN 103764733B CN 201380002853 A CN201380002853 A CN 201380002853A CN 103764733 B CN103764733 B CN 103764733B
- Authority
- CN
- China
- Prior art keywords
- heat conductive
- conductive sheet
- fibrous filler
- sheet
- extruding
- 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.)
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- 230000015572 biosynthetic process Effects 0.000 claims description 31
- 238000002360 preparation method Methods 0.000 claims description 25
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- 239000003795 chemical substances by application Substances 0.000 claims description 20
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
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- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 1
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Classifications
-
- 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
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- B29C43/02—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor of articles of definite length, i.e. discrete articles
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- 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
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- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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- 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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- B29D—PRODUCING PARTICULAR ARTICLES FROM PLASTICS OR FROM SUBSTANCES IN A PLASTIC STATE
- B29D7/00—Producing flat articles, e.g. films or sheets
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F28—HEAT EXCHANGE IN GENERAL
- F28F—DETAILS OF HEAT-EXCHANGE AND HEAT-TRANSFER APPARATUS, OF GENERAL APPLICATION
- F28F21/00—Constructions of heat-exchange apparatus characterised by the selection of particular materials
- F28F21/02—Constructions of heat-exchange apparatus characterised by the selection of particular materials of carbon, e.g. graphite
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/48—Manufacture or treatment of parts, e.g. containers, prior to assembly of the devices, using processes not provided for in a single one of the subgroups H01L21/06 - H01L21/326
- H01L21/4814—Conductive parts
- H01L21/4871—Bases, plates or heatsinks
- H01L21/4878—Mechanical treatment, e.g. deforming
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L23/00—Details of semiconductor or other solid state devices
- H01L23/34—Arrangements for cooling, heating, ventilating or temperature compensation ; Temperature sensing arrangements
- H01L23/36—Selection of materials, or shaping, to facilitate cooling or heating, e.g. heatsinks
- H01L23/373—Cooling facilitated by selection of materials for the device or materials for thermal expansion adaptation, e.g. carbon
- H01L23/3737—Organic materials with or without a thermoconductive filler
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K7/00—Constructional details common to different types of electric apparatus
- H05K7/20—Modifications to facilitate cooling, ventilating, or heating
- H05K7/2039—Modifications to facilitate cooling, ventilating, or heating characterised by the heat transfer by conduction from the heat generating element to a dissipating body
- H05K7/20436—Inner thermal coupling elements in heat dissipating housings, e.g. protrusions or depressions integrally formed in the housing
- H05K7/20445—Inner thermal coupling elements in heat dissipating housings, e.g. protrusions or depressions integrally formed in the housing the coupling element being an additional piece, e.g. thermal standoff
- H05K7/20472—Sheet interfaces
- H05K7/20481—Sheet interfaces characterised by the material composition exhibiting specific thermal properties
-
- 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
- B29C2793/00—Shaping techniques involving a cutting or machining operation
- B29C2793/0027—Cutting off
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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
-
- 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
- B29C48/267—Intermediate treatments, e.g. relaxation, annealing or decompression step for the melt
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
- B29K2083/00—Use of polymers having silicon, with or without sulfur, nitrogen, oxygen, or carbon only, in the main chain, as moulding material
- B29K2083/005—LSR, i.e. liquid silicone rubbers, or derivatives thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
- B29K2505/00—Use of metals, their alloys or their compounds, as filler
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
- B29K2507/00—Use of elements other than metals as filler
- B29K2507/04—Carbon
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
- B29K2509/00—Use of inorganic materials not provided for in groups B29K2503/00 - B29K2507/00, as filler
- B29K2509/02—Ceramics
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
- B29K2509/00—Use of inorganic materials not provided for in groups B29K2503/00 - B29K2507/00, as filler
- B29K2509/08—Glass
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
- B29K2995/00—Properties of moulding materials, reinforcements, fillers, preformed parts or moulds
- B29K2995/0012—Properties of moulding materials, reinforcements, fillers, preformed parts or moulds having particular thermal properties
- B29K2995/0013—Conductive
-
- 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
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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
- C08J2383/05—Polysiloxanes containing silicon bound to hydrogen
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Abstract
本发明提供导热性片材的制备方法,所述制备方法具有以下工序:工序(A)通过使纤维状填充剂和球状填充剂分散于粘合剂树脂中来制备导热性片材形成用组合物的工序;工序(B)由所制备的导热性片材形成用组合物形成成形体块料的工序;工序(C)将所形成的成形体块料切削成所希望的厚度形成片材的工序;和工序(D)挤压所形成的片材的切削面的工序,所述工序进行挤压以使得挤压后的片材的热阻值与挤压前的片材的热阻值相比降低。
Description
技术领域
本发明涉及导热性片材的制备方法。
背景技术
为防止在驱动时伴有发热的IC芯片等发热体的故障,将发热体介助导热性片材粘附于散热片等散热体。近年来,作为提高这样的导热性片材的导热性的努力,提出以下方案:在使用磁场发生装置使纤维状填充剂分散于热固化性树脂中而得的层状热固化性树脂组合物中的该纤维状填充剂在层的厚度方向上取向后,使热固化性树脂固化制备导热性片材(专利文献1)。此导热性片材为纤维状填充剂的端部在片材表面露出,在应用于发热体与散热体之间时,纤维状填充剂露出的端部没入导热性片材内的结构。
现有技术文献
专利文献
专利文献1:日本专利第4814550号。
发明内容
发明所要解决的课题
但是,专利文献1的技术存在为使纤维状填充剂如期望地取向而必须使用高成本的磁发生装置的问题。另外,为通过磁发生装置使纤维状填充剂取向,必须降低热固化性树脂组合物的粘度,因此无法大幅增加纤维状填充剂的含量,存在导热性片材的导热性不足的问题。此外,由于导热性片材在发热体与散热体之间的应用条件,亦存在露出的纤维状填充剂的端部未没入导热性片材内的问题。反之,亦存在以下问题:由于使露出的纤维状填充剂的端部完全没入导热性片材内,在配置于发热体与散热体之间时,存在必须对它们施加妨碍它们的正常工作的负荷的情况。
本发明的目的在于,解决以上现有技术的问题,使得在制备导热性片材时无需使用高成本的磁发生装置,可在热固化性树脂组合物中掺混大量的纤维状填充剂,使得可制备在配置于发热体与散热体之间时,即使对它们不施加妨碍它们的正常工作的负荷,仍示出良好的导热性的导热性片材。
解决课题的手段
当本发明人在使纤维状填充剂在导热性片材的厚度方向上取向并不是引起现有技术的问题的主要原因的假设下对纤维状填充剂的取向状态进行研究时发现,通过使粘合剂树脂中含有较大量的纤维状填充剂制备导热性片材形成用组合物,并且不使用磁发生装置以有意地使纤维状填充剂取向,而仅由导热性片材形成用组合物通过公知的成形法(优选挤出成形法或模具成形法)形成成形体块料,将其切削,进而对所形成的片材进行挤压处理,可制备能够达成上述目的的导热性片材,从而完成本发明。
即,本发明提供导热性片材的制备方法,所述制备方法具有以下工序(A)~(D):
工序(A)
通过使纤维状填充剂和球状填充剂分散于粘合剂树脂中来制备导热性片材形成用组合物的工序,
工序(B)
由所制备的导热性片材形成用组合物形成成形体块料的工序,
工序(C)
将所形成的成形体块料切削成所希望的厚度形成片材的工序,和
工序(D)
挤压所形成的片材的切削面的工序,其中,进行挤压以使得挤压后的片材的热阻值与挤压前的片材的热阻值相比降低,
上述工序(A)的纤维状填充剂为具有8~12μm的平均直径和2~50的长宽比的碳纤维,
上述导热性片材形成用组合物中的纤维状填充剂和球状填充剂的掺混量分别为16~40体积%和30~60体积%,
将在上述工序(C)中形成的片材的挤压前的热阻值(K·cm2/W)调整为0.31~1.00。
另外,本发明提供通过上述制备方法得到的导热性片材和将此导热性片材配置于发热体与散热体之间而得的过热保护设备(サーマルデバイスthermal device)。
此外,本发明提供导热性片材,在将通过包含导热性片材形成用组合物的成形体块料形成的片材挤压而成的导热性片材中,
上述导热性片材形成用组合物使纤维状填充剂和球状填充剂分散于粘合剂树脂中而成,纤维状填充剂为具有8~12μm的平均直径和2~50的长宽比的碳纤维,在上述导热性片材形成用组合物中分别以16~40体积%和30~60体积%掺混纤维状填充剂和球状填充剂,
将成形体块料中的纤维状填充剂的取向无规则率调整为55~95%的范围,由此使由成形体块料形成的片材的挤压前热阻值(K·cm2/W)为0.31~1.00的范围。
发明的效果
根据本发明的制备方法,使得作为纤维状填充剂的碳纤维以及球状填充剂这二者一起以较大量包含于粘合剂树脂中,制备导热性片材形成用组合物,另一方面优选以纤维状填充剂的取向无规则的方式形成成形体块料,将切削此成形体块料而得的片材热阻值(K·cm2/W)的范围在此片材的挤压处理前有意地设定为0.31~1.00的范围之类的高的范围。
在这样的成形体块料和将其切削而得的片材中,由于纤维状填充剂未在特定方向上取向(换言之无规则取向),所以通过以下各工序的工序(D)时的挤压可促进纤维状填充剂相互的接触。这是,若纤维状填充剂在特定方向、特别是与挤压的方向水平或垂直取向,则无法通过挤压期待纤维状填充剂相互接触,但如本发明所示,由于若有意地使纤维状填充剂无规则取向,则随着粘合剂树脂的流动或变形,纤维状填充剂在片材内部相互接触,所以可制备事后改善片材内部的导热性的导热性片材。并且由于可使片材的表面平滑,所以与发热体或散热体的密合性良好,可制备在配置于发热体与散热体之间时,即使不对它们施加妨碍它们的正常工作的负荷,也示出良好的导热性的导热性片材。
实施发明的最佳方式
本发明的导热性片材的制备方法具有以下工序(A)~(D)。对每个工序进行详细说明。
<工序(A)>
首先,通过使纤维状填充剂分散于粘合剂树脂中来制备导热性片材形成用组合物。
构成导热性片材形成用组合物的纤维状填充剂用以将来自于发热体的热有效传导至散热体。作为这样的纤维状填充剂,由于若平均直径过小则其比表面积过大,担心导热性片材形成用组合物的粘度过度升高,若过大则导热性片材的表面凹凸增大,担心与发热体或散热体的密合性降低,所以优选为8~12μm。另外,其长宽比(长度/直径)由于若过小则有导热性片材形成用组合物的粘度过高的趋势,若过大则有抑制导热性片材的压缩的趋势,所以优选为2~50,更优选为3~30。
作为纤维状填充剂的具体例,可优选列举出例如碳纤维、金属纤维(例如镍、铁等)、玻璃纤维、陶瓷纤维(例如氧化物(例如氧化铝、二氧化硅等)、氮化物(例如氮化硼、氮化铝等)、硼化物(例如硼化铝等)、碳化物(例如碳化硅等)等非金属类无机纤维)。
纤维状填充剂可根据导热性片材所要求的机械性质、热学性质、电学性质等特性选择,可特别优选使用碳纤维。其中,从示出高弹性模量、良好的导热性、高导电性、电磁波屏蔽性、低热膨胀性等的方面出发可优选使用沥青类碳纤维。需说明的是,在以后的段落中,只要无预先说明,“纤维状填充剂”的术语指碳纤维。
由于若纤维状填充剂在导热性片材形成用组合物中的含量过少则导热率降低,若过多则有粘度升高的趋势,所以通过调整各种材料的添加量,纤维状填充剂在导热性片材中的含量优选为16~40vol%,相对于构成导热片材形成用组合物的下述粘合剂树脂100质量份,优选为120~300质量份,更优选为130~250质量份。
需说明的是,除纤维状填充剂外,在不损害本发明的效果的范围内,可合用板状填充剂、鳞片状填充剂、球状填充剂等。特别是从抑制纤维状填充剂在导热性片材形成用组合物中的二次凝集的观点出发,直径为0.1~5μm的球状填充剂(优选球状氧化铝或球状氮化铝)的优选范围为30~60体积%,更优选为35~50体积%,相对于纤维状填充剂100质量份,优选合用100~900质量份。
粘合剂树脂将纤维状填充剂保持在导热性片材内,可根据导热性片材所要求的机械强度、耐热性、电学性质等特性选择。作为这样的粘合剂树脂,可从热塑性树脂、热塑性弹性体、热固化性树脂中选择。
作为热塑性树脂,可列举出聚乙烯、聚丙烯、乙烯-丙烯共聚物等乙烯-α链烯烃共聚物、聚甲基戊烯、聚氯乙烯、聚偏氯乙烯、聚醋酸乙烯酯、乙烯-醋酸乙烯酯共聚物、聚乙烯醇、聚乙烯醇缩醛、聚偏氟乙烯和聚四氟乙烯等氟类聚合物、聚对苯二甲酸乙二醇酯、聚对苯二甲酸丁二醇酯、聚萘二甲酸乙二醇酯、聚苯乙烯、聚丙烯腈、苯乙烯-丙烯腈共聚物、丙烯腈-丁二烯-苯乙烯共聚物(ABS)树脂、聚苯撑-醚共聚物(PPE)树脂、改性PPE树脂、脂肪族聚酰胺类、芳族聚酰胺类、聚酰亚胺、聚酰胺酰亚胺、聚甲基丙烯酸、聚甲基丙烯酸甲酯等聚甲基丙烯酸酯类、聚丙烯酸、聚碳酸酯、聚苯硫醚、聚砜、聚醚砜、聚醚腈、聚醚酮、聚酮、液晶聚合物、有机硅树脂、离聚物等。
作为热塑性弹性体,可列举出苯乙烯-丁二烯嵌段共聚物或其氢化物、苯乙烯-异戊二烯嵌段共聚物或其氢化物、苯乙烯类热塑性弹性体、链烯烃类热塑性弹性体、氯乙烯类热塑性弹性体、聚酯类热塑性弹性体、聚氨酯类热塑性弹性体、聚酰胺类热塑性弹性体等。
作为热固化性树脂,可列举出交联橡胶、环氧树脂、酚树脂、聚酰亚胺树脂、不饱和聚酯树脂、邻苯二甲酸二烯丙基酯树脂等。作为交联橡胶的具体例,可列举出天然橡胶、丙烯酸橡胶、丁二烯橡胶、异戊二烯橡胶、苯乙烯-丁二烯共聚橡胶、丁腈橡胶、氢化丁腈橡胶、氯丁橡胶、乙烯-丙烯共聚橡胶、氯化聚乙烯橡胶、氯磺化聚乙烯橡胶、丁基橡胶、卤化丁基橡胶、氟橡胶、氨基甲酸酯橡胶和有机硅橡胶。
导热性片材形成用组合物可通过将纤维状填充剂、粘合剂树脂和根据需要掺混的各种添加剂或挥发性溶剂通过公知的技术均匀混合来制备。
<工序(B)>
接着,由所制备的导热性片材形成用组合物,通过公知的成形方法形成成形体块料。此时,优选采用不使纤维状填充剂在特定方向上取向的成形方法。特别优选通过挤出成形法或模具成形法形成成形体块料。
作为挤出成形法、模具成形法,无特别限制,可从公知的各种挤出成形法、模具成形法中根据导热性片材形成用组合物的粘度或导热性片材所要求的特性等适宜采用。
在挤出成形法中,在将导热性片材形成用组合物由模具挤出时,或者在模具成形法中,在将导热性片材形成用组合物压入模具时,粘合剂树脂流动,一部分纤维状填充剂沿其流动方向取向,但多数的取向无规则。此时,在全部纤维状填充剂中取向无规则的纤维状填充剂的比例(纤维状填充剂的取向无规则率)由于若过低,则在下述工序(D)的挤压后相互接触的纤维状填充剂的比例低,有导热性片材的导热性不足的趋势,若过多则担心片材的厚度方向的导热性不足,所以优选为55~95%,更优选为60~90%。纤维状填充剂的取向无规则率可通过电子显微镜观察来计算。
需说明的是,取向无规则率为0%的状态指单位立方体(例如0.5mm四边形)所包含的纤维状填充剂全部在某个特定方向上(例如片材厚度方向)取向的状态。无规则率为100%的状态指在单位立方体(例如0.5mm四边形)所包含的纤维状填充剂中在某个特定方向上(例如片材厚度方向)取向的集合不存在的状态。取向无规则率为50%的状态指在单位立方体(例如0.5mm四边形)所包含的纤维状填充剂中属于在某个特定方向上(例如片材厚度方向)取向的集合的纤维状填充剂的比例为50%的状态。因此,取向无规则率为55%的状态指在单位立方体(例如0.5mm四边形)所包含的纤维状填充剂中属于在某个特定方向上(例如片材厚度方向)取向的集合的纤维状填充剂的比例为45%的状态,取向无规则率为95%的状态指在单位立方体(例如0.5mm四边形)所包含的纤维状填充剂中属于在某个特定方向上(例如片材厚度方向)取向的集合的纤维状填充剂的比例为5%的状态。
此取向无规则率可在观察片材的一个截面时通过除去配置于厚度方向且可确认规定长度的纤维状填充剂来算出。另外,通过增加观察的截面数,取得到的取向无规则率的平均值,可提高其数值精度。
成形体块料的大小/形状可根据需要的导热性片材的大小决定。例如,可列举出截面的纵向大小为0.5~15cm、横向大小为0.5~15cm的长方体。长方体的长度只要根据需要决定即可。
<工序(C)>
接着,切削所形成的成形体块料形成片材。此成形体块料与将其切削而得的片材中的纤维填充剂的取向程度可视为基本相同。另外,纤维状填充剂在通过切削得到的片材的表面(切削面)露出。作为切削的方法,无特别限制,可根据成形体块料的大小或机械强度由公知的切削装置(优选超声切削刀)中适宜选择。作为成形体块料的切削方向,当成形方法为挤出成形法时,为了有在挤出方向上取向的纤维状填充剂,相对于挤出方向为60~120度,更优选为70~100度的方向。特别优选为90度(垂直)的方向。
如上所述,在切削成形体块料而得的片材中,在维持成形体块料的取向无规则率,并且将使用的纤维状填充剂指定为碳纤维,亦规定其形状和掺混量时,可将片材的挤压前的热阻值限定于规定的范围。具体而言,通过将纤维状填充剂设为具有8~12μm的平均直径和2~50的平面形状的碳纤维,将该纤维状填充剂和球状填充剂的含量分别设为16~40体积%和30~60体积%,可使进行下述工序(D)的挤压前(挤压前)的热阻值为超过0.31且不足1.00。需说明的是,在测定热阻值时,对片材施加1kg/cm2的负荷。
对于切削成形体块料的宽度(形成的片材的厚度)无特别限制,可根据导热性片材的使用目的等适宜选择。在这里,对于与热阻值的关系,当切削成形体块料使工序(C)的成形体块料的切削宽度(形成的片材的片材厚度)为不足0.65mm时,片材的热阻值(K·cm2/W)优选超过0.31且不足0.47的范围。当切削成形体块料使得为0.65mm以上且3mm以下时,片材的热阻值(K·cm2/W)优选超过0.47且不足1.00的范围。
<工序(D)>
接着,挤压所得到的片材的切削面。由此得到导热性片材。作为挤压的方法,可使用由平板和表面平坦的压头构成的成对的挤压装置。另外,亦可通过夹送辊进行挤压。
作为挤压时的压力,通常若过低则有不进行挤压的情况和热阻不变的趋势,若过高则有片材伸长的趋势。另外,在挤压时为防止伸长而插入垫片(スペーサーspacer)时,可设定高的挤压压力。通常,施加至片材的压力为1~100kgf/cm2,但当不使用垫片时,优选为2~8kgf/cm2,更优选为3~7kgf/cm2,当使用垫片时,挤压时的设定压力为0.1~30MPa,优选为0.5~20MPa。
在本发明中,作为垫片,可使用由与希望制备的片材厚度相同厚度的硬质材料构成的框架或平板。例如,作为垫片,可示例出在与希望制备的片材厚度相同厚度的正方形(例如25cm四边形)不锈钢板上设置4个正方形(例如10cm四边形)的孔穴,制成如汉字“田”形状的框架的垫片,但并不限定于此。
为进一步提高挤压的效果,缩短挤压时间,这样的挤压优选在粘合剂树脂的玻璃化转变温度以上进行。通常在0~180℃的温度范围内、优选室温(约25℃)~100℃的温度范围内、更优选30~100℃的温度范围内进行挤压。
在本发明中,虽然挤压后的片材厚度因压缩而变薄,但由于若片材的压缩率[{(挤压前的片材厚度-挤压后的片材厚度)/挤压前的片材厚度}×100]过小则有热阻不减小的趋势,若过大则有片材伸长的趋势,所以进行挤压以使得压缩率为2~15%。
另外,可通过挤压时片材的表面平滑。平滑的程度可通过表面光泽度(光泽值)评价。由于若表面光泽度过低则导热性降低,所以优选进行挤压以使得在60度的入射角、60度的反射角下用光泽计测定的表面光泽度(光泽值)为0.2以上。
通过以上说明的导热性片材的制备方法得到的该导热性片材亦为本发明的一个实施方式,其优选的实施方式为纤维状填充剂的取向无规则率为55~95%、厚度为0.1~50mm、通过光泽计得到的表面光泽度(光泽值)为0.2以上的导热性片材。
这样的导热性片材可提供用于将由发热体产生的热驱散至散热体而配置于它们之间的结构的过热保护设备。作为发热体,可列举出IC芯片、IC模块等,作为散热体,可列举出由不锈钢等金属材料形成的散热片等。
如以上说明所示,虽然导热性片材的热学特性大大依赖于所含有的纤维状填充剂的取向无规则率,但其热学性质亦可通过纤维状填充剂以何种角度的偏差排列于片材的厚度方向来进行评价。具体而言,只要用50~300倍的光学显微镜拍摄导热性片材的一个截面,将片材的表面方向计为90度时,采集拍摄图像,求得纤维状填充剂的角度分布,进而求得其标准偏差即可。标准偏差优选为10°以上。
需说明的是,通过本发明的制备方法得到的导热性片材本身是本发明的一个实施方式,可作为“物品”如下表述。
即,本发明的导热性片材为“导热性片材,在将通过包含导热性片材形成用组合物的成形体块料形成的片材挤压而成的导热性片材中,
上述导热性片材形成用组合物使纤维状填充剂和球状填充剂分散于粘合剂树脂中而成,纤维状填充剂为具有8~12μm的平均直径和2~50的长宽比的碳纤维,在上述导热性片材形成用组合物中分别以16~40体积%和30~60体积%掺混纤维状填充剂和球状填充剂,
将成形体块料中的纤维状填充剂的取向无规则率调整为55~95%的范围,由此使由成形体块料形成的片材的挤压前热阻值(K·cm2/W)为0.31~1.00的范围。”。
此导热性片材中的发明的组成具有与在本发明的制备方法中说明内容相同的意义,另外发明的效果亦与通过本发明的制备方法制备的导热性片材的效果相同。
实施例
实施例1
通过将17体积%的有机硅A液(具有乙烯基的有机聚硅氧烷)、16体积%的有机硅B液(具有氢甲硅烷基的有机聚硅氧烷)、22体积%的氧化铝粒子(平均粒径为3μm)、22体积%的球状氮化铝(平均粒径为1μm)和23体积%的沥青类碳纤维(平均长轴长度为150μm,平均轴径为8μm)均匀混合来制备导热性片材形成用有机硅树脂组合物。若以质量份换算,则相对于有机硅树脂100质量份,混合153质量份的沥青类碳纤维制备导热性片材形成用有机硅树脂组合物。
将此导热性片材形成用有机硅树脂组合物浇铸于具有长方体状内部空间的模具中,通过在100℃的烘箱中加热固化6小时来制备成形体块料。需说明的是,事先在模具的里面粘贴剥离聚对苯二甲酸乙二醇酯薄膜,使剥离处理面为内侧。
用超声切削刀将得到的成形体块料切削成0.2mm厚,得到片材。在此片材的表面,纤维状填充剂的一部分因切削时的剪切力而在表面露出,在片材表面形成微小凹凸。在对此片材施加1kgf/cm2的负荷的同时,使用符合ASTM-D5470的热阻测定装置测定热阻[(K/W)和(K·cm2/W)]。将得到的结果示出于表1中。其热阻值为0.41K·cm2/W。
将这样得到的片材放置于不锈钢平板上,通过于常温(25℃)用表面为镜面抛光的平坦的不锈钢压头以对片材施加2kgf/cm2的负荷的方式挤压30分钟,从而得到表面平滑的导热性片材。将挤压前、挤压后的片材厚度和压缩率示出于表1中。
需说明的是,用100倍的光学显微镜拍摄导热性片材的平面,将片材的表面方向计为90度时,采集拍摄图像,求得纤维状填充剂的角度分布,进而求得其标准偏差。角度分布的平均值为-12.9°,标准偏差为15.6°。
实施例2~45、比较例1
除如表1所示地变更实施例的成形体块料的切削厚度、挤压条件(压力、温度)以外,通过与实施例1相同的操作得到导热性片材。另外,将挤压前、挤压后的片材厚度和压缩率示出于表1中。
比较例1
除不进行挤压以外,通过与实施例1相同的操作得到导热性片材。
实施例46~51
如表1所示地变更实施例的成形体块料的切削厚度、挤压条件(压力、温度)、沥青类碳纤维的平均长轴长度(μm)和平均轴径(μm),另外在挤压时使用垫片(在具有与希望制备的片材厚度相同厚度的25cm四边形不锈钢板上设置4个10cm四边形孔穴而得的垫片),此外实施例46、47在100质量份的有机硅树脂中混合240质量份的碳纤维,实施例48~51在100质量份的有机硅树脂中混合150质量份的碳纤维,除此之外通过与实施例1相同的操作得到导热性片材。将挤压前后的片材厚度和压缩率示出于表1中。
<评价>
对于得到的导热性片材,在施加1kgf/cm2的负荷的同时,使用符合ASTM-D5470的热阻测定装置测定各自的热阻[(K/W)和(K·cm2/W)]。将得到的结果示出于表1中。在实际使用中,就热阻而言,当挤压前的片材厚度为0.1mm以上且不足0.2mm时希望为0.4K/W (1.256 (K·cm2/W))以下,当片材厚度为0.2mm以上且不足0.6mm时希望为0.130K/W (0.41 (K·cm2/W))以下,当片材厚度为0.6mm以上且不足1.0mm时希望为0.140K/W (0.44 (K·cm2/W))以下,当片材厚度为1.0mm以上且不足3.0mm时希望为0.5K/W (1.57 (K·cm2/W))以下。
需说明的是,挤压前的片材厚度为0.1mm以上且不足0.2mm时的实际使用上希望的热阻上限设定高于片材厚度为0.2mm以上且不足0.6mm时的实际使用上希望的热阻上限。其原因在于,若片材厚度过薄,则存在于片材中的填充剂对片材表面的影响变大,从而易破坏片材表面的平滑性。
另外,对于实施例6、10、21、25、46~51和比较例1,使用光泽计(入射角为60度,反射角为60度)测定表面光泽度(光泽值)。将得到的结果示出于表1中。
[表1]
。
表1的实施例1~45的导热性片材在挤压后在各种片材厚度下分别示出良好的低热阻。另外,测定表面光泽度的实施例6、10、21、25的导热性片材的表面光泽度(光泽值)为0.2以上。
另外,可知随着挤压压力升高热阻有降低的趋势,随着挤压温度升高热阻有升高的趋势,随着片材厚度变厚热阻有升高的趋势。
另一方面,在未实施挤压的比较例1的导热性片材的情况下,热阻超过0.41K·cm2/W,并且光泽值为0.1,表面光泽度低。
另外,在实施例46的导热性片材的情况下,由于在挤压时使用垫片,所以设定高的挤压温度,达到100℃,并且由于碳纤维的平均长轴长度较短,为100μm,所以片材的压缩率非常高,达到67%。因此,在挤压前0.10mm的片材厚度下示出良好的低热阻。另外,表面光泽度(光泽值)为0.1以上。
在实施例47的导热性片材的情况下,除将挤压温度设为70℃以外,重复与实施例46相同的操作。因此,压缩率约为43%,与实施例46的情况相比降低,但在挤压前0.10mm的片材厚度下示出良好的低热阻。另外,表面光泽度(光泽值)为0.1以上。
在实施例48~51的导热性片材的情况下,在挤压时使用垫片。并且片材厚度较厚,但由于设定较高的挤压压力,达到1.2~20MPa,所以在挤压前1.55~2.54mm的片材厚度下示出良好的低热阻。另外,表面光泽度(光泽值)为0.2以上。
需说明的是,在这样示出良好的导热性的导热性片材中,挤压前的热阻值示出为0.1~0.32。
产业上的可利用性
根据本发明的制备方法,虽然纤维状填充剂多数在成形时取向无规则,但通过切削后的挤压将片材压缩,可制备因纤维状填充剂在片材内部相互接触而改善片材内部的导热性的导热性片材。并且由于可使片材的表面平滑,所以与发热体或散热体的密合性良好,可制备在配置于发热体与散热体之间时,即使不对它们施加妨碍它们的正常工作的负荷,也示出良好的导热性的导热性片材。因此,本发明对用以配置于IC芯片或IC模块等发热体与散热体之间的导热性片材的制备有用。
Claims (14)
1.导热性片材的制备方法,所述制备方法具有以下工序(A)~(D):
工序(A)
使纤维状填充剂和球状填充剂分散于粘合剂树脂中来制备导热性片材形成用组合物的工序,
工序(B)
由所制备的导热性片材形成用组合物形成成形体块料的工序,
工序(C)
将所形成的成形体块料切削成所希望的厚度形成片材的工序,和
工序(D)
挤压所形成的片材的切削面的工序,其中,进行挤压以使得挤压后的片材的热阻值与挤压前的片材的热阻值相比降低,
上述工序(A)的纤维状填充剂为具有8~12μm的平均直径和2~50的长宽比的碳纤维,
上述导热性片材形成用组合物中的纤维状填充剂和球状填充剂的掺混量分别为16~40体积%和30~60体积%,
将在上述工序(C)中形成的片材的挤压前的热阻值调整为0.31~1.00K·cm2/W。
2.权利要求1的制备方法,其中,在工序(B)中,通过挤出成形法或模具成形法形成成形体块料。
3.权利要求1或2的制备方法,其中,工序(A)的粘合剂树脂为有机硅树脂。
4.权利要求1~3中任一项的制备方法,其中,当在工序(C)中形成的片材的厚度不足0.65mm时,将所述片材的挤压前的热阻值调整为超过0.31K·cm2/W且不足0.47K·cm2/W的范围。
5.权利要求1~3中任一项的制备方法,其中,当在工序(C)中形成的片材的厚度为0.65mm以上且3mm以下时,将所述片材的挤压前的热阻值调整为超过0.47K·cm2/W且不足1.00K·cm2/W的范围。
6.权利要求1~5中任一项的制备方法,其中,在工序(D)中,在对片材施加的压力为1~8kgf/cm2的压力下进行挤压。
7.权利要求1~5中任一项的制备方法,其中,在工序(D)中,当使用垫片时,在0.1~30MPa的设定压力下进行挤压。
8.权利要求1~7中任一项的制备方法,其中,在工序(D)中,在加热至粘合剂树脂的玻璃化转变温度以上的同时进行挤压。
9.权利要求1~8中任一项的制备方法,其中,在工序(D)中,进行挤压以使得片材的压缩率为2~15%。
10.权利要求1~9中任一项的制备方法,其中,在工序(D)中,进行挤压以使得在挤压后片材的表面光泽度为0.1以上。
11.导热性片材,所述导热性片材通过权利要求1~10中任一项的制备方法得到。
12.权利要求11的导热性片材,其中,在工序(B)中成形的成形体块料中的纤维状填充剂的取向无规则率为55~95%,其中所述取向无规则率是在全部纤维状填充剂中取向无规则的纤维状填充剂的比例。
13.过热保护设备,所述过热保护设备包含发热体和散热体以及配置于它们之间的权利要求11或12的导热性片材。
14.导热性片材,在将通过包含导热性片材形成用组合物的成形体块料形成的片材挤压而成的导热性片材中,
上述导热性片材形成用组合物使纤维状填充剂和球状填充剂分散于粘合剂树脂中而成,纤维状填充剂为具有8~12μm的平均直径和2~50的长宽比的碳纤维,在上述导热性片材形成用组合物中分别以16~40体积%和30~60体积%掺混纤维状填充剂和球状填充剂,
将成形体块料中的纤维状填充剂的取向无规则率调整为55~95%的范围,由此使由成形体块料形成的片材的挤压前的热阻值为0.31~1.00K·cm2/W的范围,其中所述取向无规则率是在全部纤维状填充剂中取向无规则的纤维状填充剂的比例。
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