CN107409480B - 热扩散片 - Google Patents
热扩散片 Download PDFInfo
- Publication number
- CN107409480B CN107409480B CN201680015565.4A CN201680015565A CN107409480B CN 107409480 B CN107409480 B CN 107409480B CN 201680015565 A CN201680015565 A CN 201680015565A CN 107409480 B CN107409480 B CN 107409480B
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- CN
- China
- Prior art keywords
- agent layer
- adhering agent
- thickness
- graphite flake
- film
- 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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- 238000009792 diffusion process Methods 0.000 title claims abstract description 45
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 91
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 84
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 82
- 239000010439 graphite Substances 0.000 claims abstract description 82
- 229920006267 polyester film Polymers 0.000 claims abstract description 41
- NIXOWILDQLNWCW-UHFFFAOYSA-N Acrylic acid Chemical class OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000004020 conductor Substances 0.000 claims abstract description 12
- 150000001875 compounds Chemical class 0.000 claims description 34
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- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 2
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- LLLVZDVNHNWSDS-UHFFFAOYSA-N 4-methylidene-3,5-dioxabicyclo[5.2.2]undeca-1(9),7,10-triene-2,6-dione Chemical compound C1(C2=CC=C(C(=O)OC(=C)O1)C=C2)=O LLLVZDVNHNWSDS-UHFFFAOYSA-N 0.000 description 1
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- MKYBYDHXWVHEJW-UHFFFAOYSA-N N-[1-oxo-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propan-2-yl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(C(C)NC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 MKYBYDHXWVHEJW-UHFFFAOYSA-N 0.000 description 1
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
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- 125000005375 organosiloxane group Chemical group 0.000 description 1
- 230000001151 other effect Effects 0.000 description 1
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- 239000012286 potassium permanganate Substances 0.000 description 1
- PNXMTCDJUBJHQJ-UHFFFAOYSA-N propyl prop-2-enoate Chemical compound CCCOC(=O)C=C PNXMTCDJUBJHQJ-UHFFFAOYSA-N 0.000 description 1
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- 238000010792 warming Methods 0.000 description 1
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Classifications
-
- 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
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- B32B9/005—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising one layer of ceramic material, e.g. porcelain, ceramic tile
- B32B9/007—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising one layer of ceramic material, e.g. porcelain, ceramic tile comprising carbon, e.g. graphite, composite carbon
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- B32B9/04—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising such particular substance as the main or only constituent of a layer, which is next to another layer of the same or of a different material
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- B32B9/045—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising such particular substance as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
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- 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
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- 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
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- 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
- H01L23/3735—Laminates or multilayers, e.g. direct bond copper ceramic substrates
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K50/00—Organic light-emitting devices
- H10K50/80—Constructional details
- H10K50/87—Arrangements for heating or cooling
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K85/00—Organic materials used in the body or electrodes of devices covered by this subclass
- H10K85/10—Organic polymers or oligomers
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K85/00—Organic materials used in the body or electrodes of devices covered by this subclass
- H10K85/10—Organic polymers or oligomers
- H10K85/141—Organic polymers or oligomers comprising aliphatic or olefinic chains, e.g. poly N-vinylcarbazol, PVC or PTFE
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Abstract
本发明提供扩展方向的导热率高且从粘附体剥离后仍可再使用的热扩散片。提供热扩散片(2),由从石墨片(10)开始依次层叠丙烯酸系粘着剂层(21)、聚酯膜(22)和有机硅粘着剂层(23)形成,其中,石墨片(10)的厚度为20μm以上且小于80μm,上述丙烯酸系粘着剂层(21)的厚度为5μm以上且15μm以下的范围且不含有导热性材料,上述聚酯膜(22)的厚度为5μm以上且30μm以下的范围,上述有机硅粘着剂层(23)比上述聚酯膜(22)薄,厚度为2μm以上且25μm以下的范围、不含有导热性材料且剥离强度为0.005N/cm以上且1.0N/cm以下。贴附了有机硅粘着剂层(23)的粘附体的发热易于传输至石墨片(10),此外,剥离后易于再利用。
Description
技术领域
本发明涉及散热中使用的热扩散片,尤其是涉及使热在热扩散片的扩展方向扩散的热扩散片。
背景技术
近年来,个人计算机、手机、PDA等电子设备的性能显著提高,这得益于CPU的性能的显著提升。伴随着这样的CPU的性能提升,CPU的发热量也明显增加,如何进行电子设备中的散热就成为重要的课题。
作为热对策,有通过风扇进行空冷、使用热管、水的水冷等方法,但任何一种方法都需要用于散热的新装置,存在不仅导致设备重量的增加、还导致噪音、使用电量的增加等的缺点。
另一方面,将CPU所产生的热尽可能迅速地大面积地扩散的方法是以提高冷却效率为目的的方法,因此作为手机、个人计算机等电子设备中的冷却方法是最现实的。
然而,在以有机EL元件为代表的显示装置中,近年来在推进大型化,装置的精度、尤其是均匀性受到重视。尤其是有机EL元件中,元件自身由有机物构成,因此已知因热而导致的劣化会对元件的寿命、特别是发光特性和色度变化产生影响,由于构成装置的驱动电路等的发热,有时会伴随地发生经时变化。
作为在这样的散热目的中所使用的导热片,近年来,大多集中关注于片状的石墨。
其理由是,优质的石墨片具有100W/(m·K)以上1000W/(m·K)以下的非常高的导热性,与其他的凝胶状散热材料、片状的散热材料的导热度的特性相比是显著的高性能,最适合用于使热扩散。
专利文献1中,记载了用于将来自发热体的热直接传导至散热部件的导热性片,专利文献2、专利文献3中记载了使来自发热体的热在平面方向上扩散的热扩散性的导热性片。
作为导热性片,受到关注的不是专利文献1中的导热性片,而是专利文献2、专利文献3中记载的导热性片,尤其是将石墨进行片状化而成的所谓石墨片受到关注。
即,石墨片在平面方向上具有100W/(m·K)以上1000W/(m·K)以下的高导热性,通过使来自发热体的热扩散而使电子设备内的温度均匀化,防止设备内被配置的部件的机能下降。
专利文献2的实施方式3(0048段)中公开了如下的技术:将在PET膜等基材的两面形成有粘着剂层的双面胶带预先贴附到石墨片的一个面上,通过该粘着剂层贴附到电子设备的贴附对象表面(以下,称为粘附面);但通常粘着剂层不具有导热性,片整体的热扩散效果有下降的倾向。此外,就通常作为粘着剂层而使用的丙烯酸系粘着剂层而言,难以为了重新贴附而进行剥离。
因此,在专利文献3中,尝试了通过提供在石墨片的单面上在有机硅橡胶等弹性层(相当于粘着剂层)中含有导热性材料而成的石墨片(权利要求1),来防止导热率的下降,并且容易进行用于重新贴附的剥离。
但是,像图像面板、尤其是OLED面板(有机EL面板)这样的图像显示面板,构成该面板的表面为玻璃并且非常平滑,如果粘着剂层中含有导热性材料,则会在粘着剂层表面形成凹凸,因此会产生初期的密合性下降的不良状况。虽然这样的密合性的下降对剥离的容易性会有帮助,但相对而言使构成粘着剂层的树脂成分的比例下降,因而无法避免粘接可靠性的下降(课题1)。
此外,在石墨片的厚度为300μm以下时,不会有这样的问题,但如果石墨片的厚度比这厚,则整个片的刚性提高,其结果是,剥离时难以使片弯曲。因此,在将石墨片从石墨片所贴附的表面剥离时,要在使石墨片与表面所形成的角度不变大的同时,从上方侧进行拉伸,这种情况下,有机硅粘着剂层易于发生凝聚破坏,其结果是,成为容易残留于粘附面的结果(课题2)。
现有技术文献
专利文献
专利文献1:日本特开2007-180281号公报
专利文献2:日本特开2008-060527号公报
专利文献3:日本特开2007-012913号公报
发明内容
发明要解决的课题
为了克服上述的问题点,本发明的目的在于,提供能够在充分确保优异的导热率的同时有效地传播元件、装置所产生的热的可再剥离的热扩散片。
此外,本发明的目的在于,提供粘接可靠性高的热扩散片。
此外,本发明的目的在于,在不使有机硅粘着剂层凝聚破坏的情况下可剥离的热扩散片。
解决课题的方法
为了实现上述目的的本发明涉及的发明是一种热扩散片,是具有石墨片和在上述石墨片的表面配置的复合粘着剂膜的热扩散片,其特征在于,上述石墨片的厚度为20μm以上且小于80μm,上述复合粘着剂膜的厚度为5μm以上且15μm以下的范围,上述复合粘着剂膜具有:配置于上述石墨片上且不含有导热性材料的丙烯酸系粘着剂层,配置于上述丙烯酸系粘着剂层上且厚度为5μm以上且30μm以下的范围的聚酯膜,配置于上述聚酯膜上配置且比上述聚酯膜更薄、厚度为2μm以上且25μm以下的范围、不含有导热性材料且剥离强度为0.005N/cm以上且1.0N/cm以下的有机硅粘着剂层。
发明效果
如上所述,本发明是对石墨片使用了复合化的具有粘着剂层的复合粘着剂膜而成的热扩散片。这样的热扩散片中,首先,通过石墨片的使用,在扩展方向上具有优异的导热率,由发热元件产生的热在热扩散片的扩展方向上传输,使热扩散片达到均匀的温度,即使热扩散片所贴附的粘附体部分地发热,也能实现温度均匀上升的效果。
此外,有机硅粘着剂层的一个面牢固地粘着于聚酯膜,另一个面具有能够从玻璃板等粘附体剥离的粘着力,因此,在从粘附体剥离后,能够再利用。
复合粘着剂膜的导热率低,但由于形成为厚度薄,减小复合粘着剂膜在膜厚方向的热阻,因此,由粘附体所产生的热易于传输至石墨片。
附图说明
图1是用于对本发明的热扩散片进行说明的图。
具体实施方式
按照以下项目来描述本发明的实施方式。
1.本发明的热扩散片(带有粘着剂的石墨片)
2.石墨片
3.复合粘着剂膜
4.丙烯酸系粘着剂层
5.聚酯膜
6.有机硅粘着剂层
7.聚酯膜与有机硅粘着剂层的关系
8.带有粘着剂的石墨片的制造方法
<1.本发明的带有粘着剂的石墨片>
图1的符号2是本发明的热扩散片,具有石墨片10和复合粘着剂膜11。
该热扩散片2贴附于以有机EL元件为代表的显示装置这样的设备内和部位上,起到使由该热源产生的热扩散的作用。
<2.石墨片>
本发明中所使用的石墨片10主要由天然石墨制造,具有高导热性,且具有能调整至数十微米~数千微米的任意厚度的特性。
本发明中所使用的石墨片10因其晶体性而在导热方面具有各向异性,在厚度方向的导热率低,难以传输热,而在扩展方向(与片的表面平行的方向)上的导热率高,易于传输热。在扩展方向上的导热率具有铜、铝的数倍的大小,此外,石墨片10与金属片相比要轻。
石墨片的厚度通常在50μm以上且2000μm以下的范围内,但本发明的热扩散片2所使用的石墨片10的情况中,为了以在OLED的图像面板这样的要求薄型化的设备中使用为目的、为了应对片自身柔软性受损、容易产生起皱这样的不良状况,优选为小于80μm。而且,本发明的复合粘着剂膜11,如后所述,当石墨片10的厚度为20μm以上时,尤其是30μm以上时,适合于薄型化,防止起皱的产生。
需说明的是,石墨片10的导热率为200W/(m·K)以上且2000W/(m·K)以下,其导热率因石墨的取向、分子量、压延密度等而受到影响。
<3.复合粘着剂膜>
本发明的复合粘着剂膜11形成于上述石墨片10的一个面,起到将石墨片10贴附于贴附对象物的表面的作用。
此外,如后所述,复合粘着剂膜11不含有导热性材料,因此,复合粘着剂膜11的整体的导热率为0.05W/(m·K)以上且0.5W/(m·K)以下的范围。
因此,为了不损害石墨片10的导热性,也为了不对本发明的其他效果产生影响,复合粘着剂膜11的总厚度设为20μm以上且100μm以下的范围,尤其优选设为22μm以上且55μm以下的范围。
复合粘着剂膜11构成为,在聚酯膜22的一个面上设置有丙烯酸系粘着剂层21,且在该一个面的相反侧的面上设置有有机硅粘着剂层23,热扩散片2为,丙烯酸系粘着剂层21的表面与石墨片10的表面接触,将石墨片10与复合粘着剂膜11粘接的片。
<4.丙烯酸系粘着剂层>
构成丙烯酸系粘着剂层21的材料含有作为基质聚合物的丙烯酸共聚物(a)、与基质聚合物相溶且呈现粘着性的增粘剂(b)和调整丙烯酸共聚物(a)的凝聚力的固化剂(c),在使丙烯酸系粘着剂层21接触石墨片10之前,丙烯酸共聚物(a)与固化剂(c)的反应虽不完全但结束反应。
作为丙烯酸共聚物(a),可以使用作为具有甲基丙烯酰基、羟基、羧基、羟甲基或酰胺基等官能基的单体而从除了甲基丙烯酸2-羟乙酯之外、还包括丙烯酸、甲基丙烯酸、丙烯酸2-羟乙酯或丙烯酸丙酯、甲基丙烯酸2-羟丙酯、N-羟甲基丙烯酰胺、N-羟甲基甲基丙烯酰胺、丙烯酰胺或甲基丙烯酰胺等的单体中选择的丙烯酸共聚物。此外,作为增粘剂(b),可以使用包括酚醛系树脂、萜烯系树脂、松香系树脂、氢化松香树脂、二甲苯树脂、丙烯酸树脂的低分子聚合物。
作为固化剂(c),当含有具有羟基等的单体等作为丙烯酸共聚物(a)的成分时,可以使用异氰酸酯型固化剂等,另一方面,当含有具有环氧等官能基的单体等时,可以使用乙烯亚胺型固化剂等。
丙烯酸系粘着剂层21的厚度为5μm以上且15μm以下,特别是10μm以下。在比5μm薄时,会有与粘附体的粘接力不足的不良状况,另一方面,在比15μm厚时,虽然与聚酯膜22的厚度也有关,但会有热阻上升而得不到良好的导热的不良状况。厚度为10μm以下时,热阻变得更小。
需说明的是,在不含有导热性材料方面,与后述的有机硅粘着剂层23相同。
<5.聚酯膜>
聚酯膜22可以产生复合粘着剂膜11整体的强度,基于与后述的有机硅粘着剂层23的厚度之间的关系,起到容易剥离的效果。
此外,还起到防止在将丙烯酸系粘着剂层21与有机硅粘着剂层23直接层叠时两层被混合的效果。
聚酯膜22优选使用聚对苯二甲酸乙二醇酯(PET),其厚度可以为5μm以上且30μm以下的范围,特别是可以为10μm以上,此外,可以为25μm以下的范围。在使用双轴延伸加工的PET膜时,关于拉伸强度,在纵向延伸方向上可以为100MPa以上且300MPa以下的范围,在横向延伸方向上可以为10MPa以上且50MPa以下的范围。
而且,关于储能模量,可以为1000Pa以上且10000MPa以下的范围。
<6.有机硅粘着剂层>
有机硅粘着剂层23由加成反应型有机硅树脂形成,从对OLED等图像面板(玻璃)的附着力(剥离强度)为0.005N/cm以上且1.0N/cm以下的观点来选择。具体而言,可以使用二甲基硅氧烷等有机硅氧烷。
需说明的是,如上所述,复合粘着剂膜11通过聚酯膜22来提高强度,因此,本发明中,有机硅粘着剂层23不必形成较厚,具体而言,有机硅粘着剂层23的厚度从需要粘接性的观点考虑为2μm以上的厚度,特别优选为5μm以上,从使剥离性良好的观点考虑为25μm以下,特别优选为20μm以下的厚度。
此外,有机硅粘着剂层23与上述的丙烯酸系粘着剂层21同样,不含有导热性材料。
<7.聚酯膜与有机硅粘着剂层的关系>
聚酯膜22和有机硅粘着剂层23,与丙烯酸系粘着剂层21不同,左右着剥离性,优选随着石墨片10的厚度、所需面积来改变其厚度关系。
例如,当石墨片10的厚度为50μm以上且小于80μm且其面积较小、为25cm2以上且300cm2以下(例如,12cm×6.7cm)时,聚酯膜22的厚度设为10μm以上且20μm以下的范围,有机硅粘着剂层23的厚度设为比聚酯膜22厚度薄、优选设为5μm以上且10μm以下。
即,相对于有机硅粘着剂层23的厚度,聚酯膜22的厚度优选设为大于1.0倍且4.0倍以下的范围。
此外,当石墨片10的面积较大、为4000cm2以上且15000cm2以下(例如121.7cm×68.5cm)时,聚酯膜22的厚度设为20μm以上且30μm以下,有机硅粘着剂层23的厚度在比聚酯膜22的厚度薄的条件下,优选设为大于10μm且25μm以下。即,相对于有机硅粘着剂层23的厚度,聚酯膜22的厚度优选设为大于1.0倍且3.0倍以下。
<8.带有粘着剂的石墨片的制造方法>
本发明的带有粘着剂的石墨片的制造方法可以是,准备上述中说明的石墨片10;准备复合粘着剂膜11,关于该复合粘着剂膜11,可以对该石墨片10依次形成丙烯酸系粘着剂层21、聚酯膜22和有机硅粘着剂层23,此外,在聚酯膜22的一个面上形成了与聚酯膜22接触的丙烯酸系粘着剂层21、在另一面上形成了与聚酯膜22接触的有机硅粘着剂层23的双面粘着片;将该复合粘着剂膜11的丙烯酸系粘着剂层21侧与石墨片10接触,将复合粘着剂膜11贴附于石墨片10,从而制造本发明的热扩散片(带有粘着剂的石墨片)2。
此外还可以是,形成在聚酯膜22上形成了有机硅粘着剂层23的中间片A,另外,形成在剥离膜上形成了丙烯酸系粘着剂层21的中间片B,使上述中间片A的聚酯膜22的表面与上述中间片B的丙烯酸系粘着剂层21的表面接触,贴附中间片A和中间片B,制成作为双面粘着片的复合粘着剂膜11,将该丙烯酸系粘着剂层21侧的剥离膜除去,使露出的丙烯酸系粘着剂层21的表面与石墨片10的表面接触,将复合粘着剂膜11贴附于石墨片10,制造本发明的热扩散片2。
此外还可以是,准备在聚酯膜22上设置有机硅粘着剂层23的中间片A、以及在石墨片10上通过涂布丙烯酸系粘着剂层21的材料来设置丙烯酸系粘着剂层21的中间片C,使中间片A的聚酯膜22的表面露出,使上述中间片C的丙烯酸系粘着剂层21的表面接触该露出的表面,从而制成本发明的热扩散片2。
实施例
以下,通过实施例更具体地说明本发明。
<膨胀石墨片的调整方法>
对约15重量份的将高锰酸钾溶解于浓硫酸而成的混合溶液浸渍天然石墨100重量份,将得到的鳞片状石墨加热至约900℃,对膨胀至容积比约150cm3/g的膨胀石墨进行加压成形,得到密度约1.5g/cm3的膨胀石墨。从上述的膨胀石墨中进一步去除杂质,得到密度约1.7g/cm3的膨胀石墨。对其进一步进行压延处理,得到厚度0.127mm、0.106mm、0.076mm、0.051mm、0.040mm的膜状的膨胀石墨压延片。通过能测定平面方向的热扩散率的热波分析仪对其进行测定,其结果为,热扩散率分别为4×10-4m2/s、4×10-4m2/s、4×10-4m2/s、3×10- 4m2/s、3×10-4m2/s。
<碳化石墨片的调整方法>
将市售的聚酰亚胺膜((株)KANEKA制,APICAL AH的厚度为25、50、75、125、225μm)夹于石墨板中,使用电炉在氮气氛下升温至1000℃,然后在1000℃热处理1小时,进行碳化处理(炭素化処理),将得到的碳化膜用板状的平滑石墨从上方夹持,在该状态下保持于长方体状的石墨容器内,用以焦炭为主成分的碳粉末覆盖容器,不进行气氛加热,而是通过对容器和碳粉末整体通入直流电压而加热至3000℃,制作厚度0.040mm、0.025mm的石墨膜。通过能测定平面方向的热扩散率的热波分析仪对其进行测定,其结果为,热扩散率均为1×10-3m2/s。
<有机硅粘着剂层的制作方法>
在由具有乙烯基作为烯基的有机二甲基聚硅氧烷和有机氢聚硅氧烷构成的加成型有机聚硅氧烷(信越化学(株)制:商品名“KS-847H”;固体成分30质量%)10质量部中,添加甲苯和甲基乙基酮的混合溶剂(质量比6:4)15质量部、铂催化剂(信越化学(株)制:商品名“PL-50T”)0.1质量部,调制成涂覆液(固体成分12质量%),使用迈耶棒(マイヤーバー)#3将该涂覆液分别涂布于厚度12μm和厚度20μm的两种聚酯膜22(帝人杜邦膜(株)制的聚对苯二甲酸乙二醇酯膜:商品名“G2”),在160℃干燥60秒,在聚酯膜22上形成由有机硅弹性体构成的具有微粘着性的有机硅粘着剂层23。
关于涂覆液,以涂布量1.0g/m2涂布,形成厚度20μm的有机硅粘着剂层23,此外,以其1/4的涂布量涂布,形成厚度5μm的有机硅粘着剂层23。
<丙烯酸系粘着剂层的制作方法>
在混合了丙烯酸单体和丙烯酸聚合物的树脂液55重量份中,添加作为增粘剂的氢化松香(荒川化学工业(株)社制,商品名“KE311”)5重量份并进行混合,进而加入甲苯40重量份并混合至均匀。在其中加入TDI系异氰酸酯改性交联剂(日本聚氨酯工业(株)社制:商品名“CORONATE L”)2重量份,进一步混合至均匀。使用迈耶棒#3以涂布量10g/m2在厚度38μm的脱模膜上涂布该涂覆液,在130℃干燥120秒,在脱模膜上形成厚度10μm的丙烯酸系粘着剂层21。此外,以一半的涂布量在脱模膜上形成厚度5μm的丙烯酸系粘着剂层21。
<复合粘着剂膜>
将所得到的上述组合物以1kg/cm的线压在能够加热的装置中进行层叠,制成在聚酯膜22的一个面上配置有机硅粘着剂层23、且在其相反侧的面上配置丙烯酸系粘着剂层21而成的结构的复合粘着剂膜11。
<实施例1~5>
通过将上述工序中制造的石墨片10(该石墨片10中含有膨胀石墨压延片和碳化石墨片这二者)与复合粘着剂膜11进行真空加热加压,得到将丙烯酸系粘着剂层21与石墨片10接触并被固定的热扩散片2。
关于该热扩散片2,制成作为层叠体的、聚酯膜为25μm的热扩散片2(实施例1、4)和聚酯膜为12μm的热扩散片2(实施例2、3、5)。
<比较例1、2>
替代在本发明中所使用的复合粘着剂膜11,将不含有导热性材料且两面形成有丙烯酸系粘着剂层的双面粘着片(“市售品1”)作为复合粘着剂膜贴附到石墨片10的一个面上,制成热扩散片。关于该双面粘着片,比较例1中,在石墨片侧和粘附体侧形成10μm的丙烯酸系粘着剂层,比较例2中,在石墨片侧和粘附体侧形成30μm的丙烯酸系粘着剂层,石墨片层的厚度为106μm和127μm。
由于在粘附体上贴附丙烯酸系粘着剂层,因而剥离性差。
<比较例3>
在厚度12μm的聚酯膜上,形成厚度10μm的丙烯酸系粘着剂层和厚度20μm的有机硅粘着剂层,将丙烯酸系粘着剂层贴附到厚度127μm的石墨片上。有机硅粘着剂层中,使用迪睿合(株)制的有机硅粘着剂片(商品名T4082S)。
有机硅粘着剂层的厚度比聚酯膜厚,有时剥离困难、或者聚酯膜变形,操作性差。
<比较例4>
在由上述工序制造的石墨片上,涂布上述有机硅粘着剂层用的涂覆液并干燥,形成有机硅粘着剂层23,得到热扩散片。不使用复合粘着剂膜。
<测定试验>
对各实施例1~5和比较例1~4的热扩散片,进行下述试验。
○热扩散率试验
用冲床切出热扩散片15mm×15mm,使用热扩散率测定装置(热波分析仪TA3:(株)Bethel制),算出在25℃温度下达到平衡状态时的热扩散率。热扩散率的数值越高越优选,希望为10-4m2/s以上。
○剥离性试验
在玻璃板(碱石灰玻璃)上以1kg/cm的线压层叠热扩散片,常温下经过7天后,确认复合粘着剂片能否从玻璃板剥离。进一步,确认在玻璃板的表面上是否残留剥离后的剥离残渣。
○粘接可靠性试验
在玻璃板(碱石灰玻璃)上以1kg/cm的线压层叠热扩散片,放入调整至60℃、75%RH的大气恒温恒湿烘箱中,确认经过1000Hr后的外观。
<试验结果>
○测定值
各试验的结果示于以下表1、表2。
[表1]
表1 实施例1-5的热扩散片的测定结果
[表2]
表2 比较例1-4的热扩散片的测定结果
(“-”表示没有设置)
○剥离性的评价
表1、表2中的剥离性一栏中,显示如下的评价。
A良好:能以较小的力从玻璃板剥离,从玻璃板剥离后的面上没有残留残渣。
B可能:能从玻璃板一次性剥离。从玻璃板剥离后的面上虽没有残留残渣,但聚酯膜产生变形。
C不良:从玻璃板剥离需要相当的力。从玻璃板剥离后的面上残留残渣。
○粘接可靠性的评价
表1、表2中,在粘接可靠性一栏中,显示如下评价。
A良好:完全没有发生浮起,端部也完整粘接。
B可能:几乎没有发生浮起,部分端部上翘。
C不良:发生浮起,端部上翘。
符号说明
2……热扩散片
10……石墨片
11……复合粘着剂膜
21……丙烯酸系粘着剂层
22……聚酯膜
23……有机硅粘着剂层
Claims (1)
1.一种热扩散片,其特征在于,是具有石墨片和在所述石墨片的表面上配置的复合粘着剂膜的热扩散片,
所述石墨片的厚度为20μm以上且小于80μm,
所述复合粘着剂膜的厚度为20μm以上且100μm以下的范围,
所述复合粘着剂膜具有:
配置于所述石墨片上且不含有导热性材料的丙烯酸系粘着剂层、
配置于所述丙烯酸系粘着剂层上且厚度为5μm以上且12μm以下的范围的聚酯膜、和
配置于所述聚酯膜上、比所述聚酯膜薄、厚度为2μm以上且25μm以下的范围、不含有导热性材料且剥离强度为0.005N/cm以上且1.0N/cm以下的有机硅粘着剂层。
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