CN101636436A - 制备导电薄膜的方法和由该方法制得的制品 - Google Patents

制备导电薄膜的方法和由该方法制得的制品 Download PDF

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CN101636436A
CN101636436A CN200880006048A CN200880006048A CN101636436A CN 101636436 A CN101636436 A CN 101636436A CN 200880006048 A CN200880006048 A CN 200880006048A CN 200880006048 A CN200880006048 A CN 200880006048A CN 101636436 A CN101636436 A CN 101636436A
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array
film
freely
base layer
heat
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CN101636436B (zh
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卡尔·费尔班克
马克·费舍尔
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Dow Silicones Corp
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Abstract

一种自由立膜，包括：i.基体层，其具有相对的表面，和ii.纳米棒阵列，其中纳米棒定向的穿过基体层并从基体层的一个或两个表面伸出至少1微米的距离。一种制备自由立膜的方法，包括：(a)在基底上提供纳米棒阵列，任选的，(b)用牺牲层渗透该阵列；(c)用基体层渗透该阵列，由此产生渗透的阵列；任选的，(d)当步骤(b)存在时，除去牺牲层，保留基体层；和(e)将渗透的阵列从基底平面上移除。根据所选用纳米棒的类型和密度，自由立膜可以用于作为滤光片、ACF、或TIM。

Description

制备导电薄膜的方法和由该方法制得的制品
对相关申请的交叉引用
根据35 U.S.C.§119(e)，本申请请求享有于2007年2月22日提交的、系列号为60/902,804的美国临时申请的优先权。将系列号为60/902,804的美国临时申请合并于此作为参考。
关于联邦政府赞助研究的声明
无
技术领域
通过本文所述的方法，制备一种含纳米管的自由立膜(free standingfilm)。根据纳米管的类型，自由立膜可以用作滤光片、各向异性导电薄膜(ACF)、或者是导热界面材料(TIM)。
背景技术
电子元件，例如半导体、晶体管、集成电路(ICs)、分立器件、和其它本领域已知的元件，都被设计为在标准操作温度或在标准操作温度范围内工作。但是，电子元件的工作会产生热。如果不将足够的热量除去，电子元件就会在显著高于其标准操作温度的温度下工作。过高的温度会对电子元件的性能和其所连接装置的工作产生不利影响，并且还会对平均无故障时间产生消极影响。
为了避免这些问题，通过热传导将热从电子元件向热管理器件、如散热器传递。随后可以利用任何常规的手段对散热器进行冷却，所述的常规手段例如对流或辐射技术。在热传导期间，可以通过电子元件与散热器之间的表面接触，或者通过使电子元件与散热器与TIM接触，使热量从电子元件向散热器传递。TIM的热阻抗越低，从电子元件向散热器流出的热量就越多。
电子元件和散热器的表面，一般不是完全平滑的；因此，表面之间的充分接触是很难达到的。空气间隙的热传导性很差，其存在于表面之间，增加了热阻抗。这些间隙可以通过在表面之间插入TIM膜来充填。由于生产商们制造出了越来越小的装置，因此，业界对于TIM保持着持续性的需求，人们希望TIM很薄并且具有改善的热传导性，以有效的从电子元件向热管理器件传递热量。
在本领域中，将含自由分散在基体中的纳米管的复合材料用作TIM是公知的。但是，当纳米管定向排列而不再自由分布时，这种排列会展示出改善的性能，例如热传导性。制造含有这种排列的TIM是十分困难的。
发明内容
一种用于制造自由立膜的方法，所述薄膜具有从基体层中伸出的纳米棒。该方法包括以下步骤：
(a)在基底上提供纳米棒阵列；
任选的(b)用牺牲层渗透该阵列；
(c)用基体层渗透该阵列，由此产生渗透的阵列；
当步骤(b)存在时，任选的(d)除去牺牲层，保留基体层；和
(e)将渗透的阵列从基底上移除，这样就形成了自由立膜，此时基体层具有相对的表面，纳米管定向的穿过基体层，并从基体层的一个或正反两个相对的表面上伸出至少1微米的距离。
附图说明
图1a示出了MWNT在硅片上的排列。这种排列用于实施例1中。
图1b和1c示出了不同放大率下，实施例1中制备的自由立膜的横截面。该薄膜包括基体层，且在基体层的表面上伸出了MWNT阵列。
图1d示出了实施例2中制备的自由立膜的横截面。
图2示出了电子装置的一部分的横截面，所述电子装置中包括本文所述的自由立膜。
具体实施方式
术语的定义和使用
除非另有说明，否则所有的数量、比率、和百分比都是基于重量的。对本申请来说，冠词″a″、″an″、和″the″都分别指代一个和多个。在本文的通式中，″Et″代表乙基，″Me″代表甲基，″Ph″代表苯基，″Vi″代表乙烯基。″MWNT″的意思是，多层碳纳米管(multi-walled carbon nanotube)。″SWNT″的意思是单层碳纳米管(single-walled carbon nanotubes)。″TEOS″的意思是四乙氧基甲硅烷(tetraethoxysilane)。
“纳米棒”(nanorod)的意思是宽度不大于0.5微米且长宽比大于10、或者大于100的导热结构。纳米棒可以是中空的纳米管。纳米棒可以是圆柱形的，此时其宽度(直径)不大于0.5微米。或者，纳米棒可以具有不同的形状。术语纳米棒包括但不局限于：单层碳纳米管、MWNT、和氮化硼纳米管。
“纳米棒的阵列”的意思是，存在多个对齐纳米棒，这些纳米棒大多数都彼此平行并按着与基底平面相交成一定角度的方向排列。图1a中示例性的示出了MWNT阵列。
“牺牲层”的意思是，在不去除基体层并不去除基体层中的纳米棒的前提下，可以被选择性去除的任意成膜材料。
方法
一种用于制造自由立膜的方法，所述薄膜具有从基体层中伸出的纳米棒。该方法包括以下步骤：
(a)在基底平面上提供纳米棒阵列；
任选的(b)用牺牲层渗透该阵列；
(c)用基体层渗透该阵列，由此产生渗透的阵列；
任选的，(d)当步骤(b)存在时，除去牺牲层，保留基体层；和
(e)将渗透的阵列从基底平面上移除，以形成自由立膜，其中基体层具有相对的表面，纳米管定向排列，穿过基体层，并从基体层的一个或正反两个相对的表面上伸出至少1微米的距离。
基体层可以处于和不处于纳米棒的中心。在该方法中，可以渗透一层和多层基体层。第二基体层可以在该方法中的不同时刻加入。例如，当步骤(d)存在时，该方法可以任选的在步骤(d)之前、之间、或之后，进一步包括用第二基体层渗透阵列。去除牺牲层所引起的空隙，可以用第二基体层来渗透。
纳米棒的阵列，通过等离子体增强的化学气相沉积生成方法来提供。在步骤(a)之前，可以任选的使纳米棒阵列经受石墨化步骤。在不希望被理论所束缚的前提下，人们认为，当碳纳米管用来形成阵列时，石墨化步骤可以增强本文所述方法制得的自由立膜的导热性。纳米棒阵列是本领域公知的，可以由纳米实验室，55礼拜街，牛顿(NanoLab，55 Chapel Street，Newton)，MA 02458处购得。
在该方法中可以包括步骤(b)和(d)，来提供纳米管伸出至基体层正反两个相对的表面之外的自由立膜。步骤(b)中使用的牺牲层可以是热塑性的，例如高粘度非硫化硅酮油或硅橡胶、氟硅氧烷、光定义硅酮(photodefinable silicone)、二氧化硅、或蜡。步骤(b)可以通过任何方便的手段来实施，而精确的方法依赖于所选择的牺牲层类型。例如，当牺牲层是二氧化硅时，可以通过由溶胶凝胶溶液中涂覆一层二氧化硅的方式，来形成牺牲层。
当步骤(b)存在时，步骤(d)就可以存在。步骤(d)可以通过任何方便的手段来实施，而具体的方法依赖于所选牺牲层的类型。例如，当牺牲层是蜡时，可以通过加热来除去。当牺牲层是二氧化硅且牺牲层是通过由溶胶凝胶溶液中涂覆一层二氧化硅的方式形成时，步骤(d)通过浸入含HF的溶液中来实施。步骤(d)和(e)可以依次进行，也可以同时进行。例如，当牺牲层是二氧化硅且步骤(d)是通过浸入含HF的溶液中实施时，就同时进行步骤(d)和(e)。该方法可以任选的进一步包括步骤(f)：在步骤(e)之后清洗自由立膜。步骤(f)可以用于除去残留的HF和/或牺牲层的残留部分。
任选的，方法中可以存在步骤(b)而不存在步骤(d)。例如，该方法可以用于制备这样的自由立膜——该薄膜在步骤(b)中渗透了蜡。当不存在步骤(d)时，蜡就可以作为自由立膜中的相变层。
步骤(c)可以通过任何方便的手段来实施，而具体的方法依赖于所选基体层的类型。例如，步骤(c)可以通过选自以下的方法来实施：旋涂、浸涂、喷涂、和溶剂浇注。基体层可以包括热固性聚合物。合适的热固性聚合物的实例包括：环氧树脂、氰酸酯树脂、双马来酰亚胺树脂、酚醛树脂、聚酯树脂、硅酮弹性体、聚氨酯弹性体、丙烯酸弹性体、和它们的组合。当使用硅酮弹性体作为基体层时，硅酮弹性体可以通过以下方法制备：在步骤(d)或步骤(e)之前，通过用包括下述成分的组合物来渗透阵列，并使组合物固化形成硅酮弹性体；所述的组合物包括：A)在每个分子中平均具有至少两个脂肪族不饱和有机基团的聚硅氧烷，B)每个分子中平均具有至少两个与氢原子键合的硅的交联剂，和C)氢化硅烷化催化剂。
或者，基体层可以包括热塑性聚合物。合适的热塑性聚合物实例包括：聚酰胺、聚酰亚胺、聚苯撑、聚碳酸酯、聚缩醛、聚丙烯、聚乙二醇、聚氧化甲烯、聚甲醛、硅酮酰胺共聚物、硅酮聚醚、硅酮聚醚酰亚胺共聚物、硅酮氨基甲酸乙酯共聚物、硅酮脲、和它们的组合。
基体层可以任选的包括填料，此时纳米棒的阵列具有相对较低的密度。填料必须具有足够小的粒径，以免抑制基体中纳米棒阵列中的渗透。填料可以是导热填料。合适的导热填料的实例包括：铜、氮化硼、氧化铝、氮化铝、氧化锌、银、铝、和它们的组合。
自由立膜
上文所述的方法得到的产品是一种自由立膜，包括：
具有正反相对表面的基体层，和
纳米棒阵列，其中纳米棒定向的穿过基体层并从基体层的一个或两个表面伸出至少1微米的距离。
阵列中纳米棒的密度处于0.5体积(vol)％-50vol％的范围。精确的密度依赖于提供阵列所用的方法和自由立膜的最终用途。例如，ACF的纳米棒密度较低，例如为0.1vol％-10vol％。为了提高导热性，使用导热纳米棒时，其密度的范围为5vol％-50vol％。
本发明所用的纳米棒可以是纳米管。所选用的纳米棒可以是导热性的并且是电绝缘的。合适的纳米棒实例包括MWNT和单层碳纳米管。或者，所选用的纳米棒可以是既导电又导热的。合适的纳米棒的实例包括氮化硼纳米管。
纳米棒的平均高度范围为5-500微米。纳米棒定向穿过基体层并从基体层的一个或正反两个相对的表面伸出至少1微米的距离。或者，纳米棒可以从基体层的一个或正反两个相对的表面伸出范围在1微米-0.8毫米的距离。
自由立膜的用途
自由立膜可以用在各种不同的用途中。根据纳米管的类型，自由立膜可以用作滤光片、ACF、或TIM。当将自由立膜用作TIM时，自由立膜可以用在以下装置中，所述装置包括：
a)发热元件，
b)导热界面材料，和
c)热管理器件；
其中导热界面材料被插入在发热元件和热管理器件之间，沿着导热路径从发热元件表面向着热管理器件表面延伸，导热界面材料包括上述自由立膜和纳米棒，所述的纳米棒与发热元件表面和热管理器件表面接触。
图2示出了电子装置200的部分横截面。装置200包括发热元件(图中示为集成电路芯片)203、第一导热界面材料(TIM1)206、和热管理器件(图中示为金属罩)207，其中所述的TIM1 206是自由立膜，其具有如上文所述的从基体层中伸出的MWNT。TIM1 206被插入在发热元件203和热管理器件207之间，沿着由箭头208表示的导热路径从发热元件203的表面向热管理器件207的表面延伸。纳米管与发热元件203的表面和热管理器件207的表面接触，从而可以在装置200运转的时候促进热传导。发热元件203借助芯片粘合剂209安装在基底204上。基底204上具有焊球205，该焊球205通过焊点210附着于基底上。第二界面材料(TIM2)202被插入于热管理器件207和散热器201之间。当装置运转的时候，热量沿着由箭头208表示的导热路径传导。
自由立膜可以用在生产电子装置的方法中。该方法包括将导热界面材料插入于发热元件和热管理器件之间。导热界面材料沿着导热路径从发热元件的表面向热管理器件的表面延伸。导热界面材料包括上文所述的自由立膜，纳米管与发射元件的表面和热管理器件的表面接触。发热元件可以包括半导体芯片，热管理器件可以包括散热器或放热器。
可以制备出带有上述自由立膜的装置。例如，上文所述的自由立膜可以在某些装置中作为导热界面材料，或者用在导热界面材料中，所述的装置例如在美国专利5,912,805和6,054,198中所公开的，用来代替上述装置中的界面材料，或者与之一起使用。
实施例
这些实施例用于向本领域技术人员示例性的说明本发明，其不应被解释为对本发明在权利要求中所阐明范围的限制。
实施例1：制备无牺牲层的自由立膜
将充分量的溶液(0.5-1毫升)分配在2×2厘米的硅片上，所述硅片上具有MWNT阵列，所述的溶液是20重量％的可固化硅酮弹性体组合物(道康宁(DOW CORNING)Sylgard 184，由美国密歇根州米德兰德市的道康宁公司(Dow Corning Corporation of Midland，Michigan，U.S.A.)处购得)溶解于氯仿中形成的。如图1a所示，MWNT的平均高度为18微米±2微米，平均直径为0.1微米，其密度为覆盖硅片表面积的6-10％。纳米管阵列适合于通过温和的机械力从硅片表面上释放。
接着，利用凯美特匀胶机(Chemat Spin Coater)KW-4A，以1000转数/分(rpm)的速度对硅片和溶液进行30秒的旋转。在旋转之后，将硅片放置15分钟，随后在150℃的烘箱中加热1小时，使硅酮弹性体进行固化。冷却之后，将硅片浸入35vol％的HF溶液和去离子水中，10分钟后，自由立膜从硅片漂离。在图1b和1c中示出了不同放大率下的自由立膜。将自由立膜取出，并进行清洗，以除去残留的HF溶液。
实施例2：制备带有牺牲层的自由立膜
将充分量的溶液分配在2×2厘米的硅片基底上，所述硅片基底上覆盖有MWNT，所述的溶液含有5％的硅溶胶凝胶溶液(TEOS/HCl/Ethanol/H2O)。利用Chemat Spin Coater KW-4A，以2000转数/分(rpm)的速度对溶液和基底进行30秒的旋转。在环境条件(20℃，35％RH)下，将硅片放置30分钟，随后在50℃下加热30分钟，在150℃下加热15分钟。接着，将充分量的浓度为11wt％的硅酮聚醚酰亚胺共聚物(Gelest SSP-085)的甲苯溶液置于MWNT阵列上，并使溶液和硅片在1000转数/分(rpm)下旋转30分钟。将硅片在室温下放置15分钟，随后在100℃下放置15分钟以除去甲苯。冷却之后，将硅片浸入35vol％的HF溶液和去离子水中，约20分钟后，自由立膜由硅片漂离，如图1d所示。将自由立膜取出，并进行清洗，以除去残留的HF溶液。
工业适用性
通过本发明所述的方法制得的自由立膜，可以作为滤光片、ACF、或TIM。在不受理论制约的前提下，我们认为，当使用碳纳米管、特别是MWNT阵列时，可以使导热性能进一步提高。

Claims (35)

1.一种方法，包括：
(a)在基底上提供纳米棒阵列，
任选的，(b)用牺牲层渗透该阵列；
(c)用基体层渗透该阵列，由此产生渗透的阵列；
任选的，(d)当步骤(b)存在时，除去牺牲层，保留基体层；和
(e)将渗透的阵列从基底平面上移除，以形成自由立膜，其中基体层具有正反相对的表面，纳米管定向排列，穿过基体层，并从基体层的一个或正反两个相对的表面上伸出至少1微米的距离。
2.根据权利要求1所述的方法，当步骤(d)存在时，该方法进一步包括在步骤(d)之前、期间、或之后，用第二基体层渗透阵列。
3.根据权利要求1所述的方法，其中纳米棒从一个或正反两个相对的表面伸出1微米-0.8毫米的距离。
4.根据权利要求1所述的方法，其中该阵列的密度为0.1体积％-50体积％。
5.根据权利要求1所述的方法，其中纳米棒的平均高度为5-500微米。
6.根据权利要求1所述的方法，其中纳米棒是导热的和电绝缘的。
7.根据权利要求1所述的方法，其中纳米棒是导电和导热的。
8.根据权利要求1所述的方法，其中纳米棒是氮化硼纳米管。
9.根据权利要求1所述的方法，其中纳米棒选自多层碳纳米管和单层碳纳米管。
10.根据权利要求9所述的方法，其中纳米棒阵列是通过等离子体增强的化学汽相沉积生成方法提供的。
11.根据权利要求10所述的方法，其中纳米管的阵列在步骤(a)之前经受了石墨化步骤。
12.根据权利要求1所述的方法，其中当步骤(b)存在时，牺牲层选自：氟硅氧烷、光定义硅酮、二氧化硅、和蜡。
13.根据权利要求12所述的方法，其中牺牲层是蜡。
14.根据权利要求13所述的方法，其中当步骤(d)存在时，牺牲层通过加热除去。
15.根据权利要求12所述的方法，其中牺牲层是二氧化硅，且通过从溶胶凝胶溶液中涂覆一层二氧化硅来形成牺牲层。
16.根据权利要求15所述的方法，其中当步骤(d)存在时，步骤(d)和(e)通过暴露于HF溶液中来实施。
17.根据权利要求16所述的方法，进一步包括步骤(f)：在步骤(e)之后清洗步骤(f)。
18.根据权利要求1所述的方法，其中基体包括热固性聚合物。
19.根据权利要求18所述的方法，其中热固性聚合物选自：环氧树脂、氰酸铵树脂、双马来酰亚胺树脂、酚醛树脂、聚酯树脂、硅酮弹性体、聚氨酯弹性体、丙烯酸弹性体、和它们的组合。
20.根据权利要求18所述的方法，其中热固性聚合物包括含下列物质的组合物：
A)每个分子中平均含有至少两个脂肪族不饱和有机基的聚硅氧烷，
B)平均每个分子中含有至少两个与氢原子相连的硅的交联剂，和
C)氢化硅烷化催化剂。
21.根据权利要求1所述的方法，其中基体包括热塑性聚合物。
22.根据权利要求21所述的方法，其中热塑性聚合物选自：聚酰胺、聚酰亚胺、聚苯撑、聚碳酸酯、聚缩醛、聚丙烯、聚乙二醇、聚氧化甲烯、聚甲醛、硅酮酰胺共聚物、硅酮聚醚、硅酮聚醚酰亚胺共聚物、硅酮氨基甲酸乙酯共聚物、硅酮脲、和它们的组合。
23.根据权利要求18到22中任一所述的方法，其中基体进一步包括填料。
24.根据权利要求23所述的方法，其中填料是导热的。
24.根据权利要求1所述的方法，其中步骤(c)通过选自以下的方法来实施：旋涂、浸涂、喷涂、和溶剂浇注。
25.通过权利要求1到23中任一所述的方法制得的自由立膜。
26.一种自由立膜，包括：
i基体层，其具有相对的表面，和
ii纳米棒阵列，其中纳米棒定向的穿过基体层并从基体层的一个或两个表面伸出至少1微米的距离。
27.根据权利要求26所述的自由立膜，其中阵列的平均密度为0.5体积％-50体积％。
28.根据权利要求26所述的自由立膜，其中纳米棒的平均高度为5-500微米。
29.权利要求26到28中任一所述的自由立膜作为滤光片的用途。
30.权利要求26到28中任一所述的自由立膜作为各向异性导电薄膜的用途。
31.权利要求26到28中任一所述的自由立膜作为导热界面材料的用途。
32.一种装置，包括：
a)发热元件，
b)导热界面材料，和
c)热管理器件；
其中导热界面材料插入在发热元件和热管理器件之间，沿着导热路径从发热元件的表面向热管理器件的表面延伸，导热界面材料包括如权利要求26到28中任一所述的自由立膜，且纳米棒与发热元件的表面和热管理器件的表面接触。
33.一种方法，包括将导热界面材料插入到发热元件和热管理器件之间，其中导热界面材料沿着导热路径从发热元件表面向热管理器件表面延伸，导热界面材料包括如权利要求26到28中任一所述的自由立膜，且纳米棒与发热元件的表面和热管理器件的表面接触。
34.根据权利要求33所述的方法，其中发热元件包括半导体芯片，热管理器件包括散热器或放热器。
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