CN114771043B - 高结合强度金刚石碳纤维复合材料及其制备方法 - Google Patents
高结合强度金刚石碳纤维复合材料及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种高结合强度金刚石碳纤维复合材料及其制备方法,该复合材料由依次交替排列的自支撑金刚石膜片和碳纤维层叠置而成,并且其顶层和底层均为自支撑金刚石膜片;自支撑金刚石膜片与碳纤维层的接触面均进行了织构化处理。制备时,首先对自支撑金刚石膜片进行形状切割、厚度修整、表明光滑化和表面织构化;然后将浸润过粘结剂的碳纤维平铺、粘合于织构化处理的自支撑金刚石膜片之间;接着采用夹持架固定并施加法向静压力,排出碳纤维内富余粘结剂和残留气泡,再对粘结剂进行加热固化,最终获得本发明高结合强度金刚石碳纤维复合材料。本发明操作简单,易规模化、批量化生产,为新一代高导热部件工程化研制奠定基础。
Description
技术领域
本发明属于热管理材料及其制备技术领域,具体涉及一种高结合强度金刚石碳纤维复合材料及其制备方法。
背景技术
随着电子技术的迅速发展,军民领域电子设备热控***中元器件的功率越来越高,热管理变得尤为重要,甚至成为大功率电子器件发展的瓶颈。然而,目前通用的金属(Al,Cu)、陶瓷(SiC,AlN)、金属基复合材料(Cu/Mo,Al/SiC)等越来越难以满足大功率电子器件散热的需求。因此,开发新一代高导热材料来保证大功率电子设备热控***的稳定工作成为热管理材料领域的研发重点。
不同于金属依靠***电子进行传热,金刚石依靠声子传热,其室温下热导率最高可达2000 W/(m·K),是铜的5倍。同时,金刚石具有极好的绝缘性,低的热膨胀系数和密度,使得金刚石成为大功率电子设备最佳的热管理应用材料。目前,金刚石在热管理材料上的应用主要有三种形式:CVD金刚石膜单独使用;CVD金刚石膜与金属焊接形成复合散热片;金刚石粉/颗粒与铜、铝等金属形成复合材料。金刚石单独作为散热材料面临如下问题:金刚石厚膜生长周期长,深加工困难,成本高;金刚石膜硬而脆,韧性差,易断裂。金刚石膜与金属焊接存在的问题是:金刚石化学惰性高,与金属材料浸润差,很难形成良好的界面结合;金刚石与金属热膨胀系数差异大,热冲击会引起变形失调。金刚石粉/颗粒与铜、铝等金属复合则面临界面热阻高、复合热导率较小的问题。
碳纤维具有抗拉强度高、热膨胀系数小(甚至可为负值-1.5×10-6/℃)、比重轻等一系列优异性能。若将金刚石与碳纤维复合,则有望将金刚石的超高导热优点及碳纤维的高强、高韧优势综合。尽管碳纤维和金刚石同属碳材料,然而二者结构不同,复合困难,使得目前尚未研制出二者的复合材料。本发明通过材料的结构功能一体化设计,制备获得高导热、高强度、高韧性、低密度的金刚石碳纤维复合热管理材料,满足大功率电子器件的散热需求。
发明内容
本发明的目的是针对现有热管理材料无法满足大功率电子器件日益增加的散热需求,而提供了一种高结合强度金刚石碳纤维复合材料。金刚石热导率高,碳纤维抗拉强度高,韧性好,本发明将二者进行复合,可实现其性能互补,获得高导热、高强度、高韧性、低密度的热管理材料。
本发明是通过如下技术方案实现的:
一种高结合强度金刚石碳纤维复合材料,由依次交替排列的自支撑金刚石膜片和碳纤维层叠置而成,并且其顶层和底层均为自支撑金刚石膜片;顶层自支撑金刚石膜片的底面、底层自支撑金刚石膜片的顶面以及中间各层自支撑金刚石膜片的顶面及底面均进行了织构化处理,即每层自支撑金刚石膜片凡是与碳纤维层接触的面均进行了织构化处理,这样就有效的保障了金刚石与碳纤维间的结合力,其结构如图1所示。
作为优选的技术方案,自支撑金刚石膜片为采用CVD法制备得到的自支撑金刚石膜片,其热导率≥600 W/(m·K)、平行度≤0.1 mm、非织构处的平整度≤0.1 mm;自支撑金刚石膜片的厚度为0.3 mm~1 mm,碳纤维层的厚度为0.1 mm~0.3 mm。
作为优选的技术方案,自支撑金刚石膜片表面的织构图案为圆形盲孔阵列或线性凹痕阵列,织构图案的深度为自支撑金刚石膜片厚度的1%~10%,如图3和图4所示。
作为优选的技术方案,自支撑金刚石膜片的层数为2~20层,碳纤维层的层数即为自支撑金刚石膜片的层数-1层。
进一步的,本发明还提供了上述高结合强度金刚石碳纤维复合材料的制备方法,以解决金刚石难以膜形式沉积于碳纤维表面,二者连接和复合困难的问题。该制备方法首先对CVD自支撑金刚石膜片进行形状切割、厚度修整、表面光滑化和表面织构化,然后将粘结剂刷涂在自支撑金刚石膜片表面,使粘结剂填充织构化盲孔或凹痕,然后将浸润过粘结剂的碳纤维平铺、粘合于自支撑金刚石膜片上,重复平铺浸润过粘结剂的碳纤维和刷涂了粘结剂的织构化自支撑金刚石膜片,直至复合厚度达到要求,保持侧面夹持的同时在顶层自支撑金刚石膜片表面施加静压力,对粘结剂进行加热固化,最后去除加持架和静压力,即获得高结合强度金刚石碳纤维复合材料。
高结合强度金刚石碳纤维复合材料的具体制备方法包括如下步骤:
步骤1:根据高结合强度金刚石碳纤维复合材料对自支撑金刚石膜片的尺寸要求,选择合适直径及厚度的自支撑金刚石膜片,设计形状阵列并进行切割;
步骤2:采用激光修面机对切割所得的自支撑金刚石膜片进行厚度修整和表面光滑处理;
步骤3:对厚度修整和表面光滑处理后的自支撑金刚石膜片表面进行单面织构化处理或双面织构化处理;
步骤4:将粘结剂和无水乙醇按比例均匀调配,把调配液刷涂到底层自支撑金刚石膜片的织构表面,使调配液填充织构化盲孔或凹痕;把碳纤维置于调配液中浸润1-5分钟,取出后在空气中放置10-30分钟,然后平铺、粘合于底层自支撑金刚石膜片的织构表面,重复平铺浸润过粘结剂的碳纤维和刷涂了粘结剂的织构化的自支撑金刚石膜片,直至复合厚度达到要求,得到复合层结构;
步骤5:通过夹持架对复合层结构进行夹持以保证其平整度,同时在最上层自支撑金刚石膜片表面放置重物,如图2所示,依靠法向静压力排出碳纤维内富余粘结剂及弥散于粘结剂内的气泡,然后在保持侧面夹持及上表层施加压力的状态下对粘结剂进行加热固化;
步骤6:去除重物及夹持架,对复合层结构的侧面进行打磨和超声清洗,最终得到所述的高结合强度金刚石碳纤维复合材料。
作为优选的技术方案,步骤4中,粘结剂采用钡酚醛树脂、环氧树脂或改性环氧树脂。
作为优选的技术方案,步骤4中,粘结剂和无水乙醇调配比例为1:1~1:5。
作为优选的技术方案,步骤5中,加热固化时的加热温度为200~300 ℃、保温时间为3~8 h。
作为优选的技术方案,步骤5中,夹持架的材质采用疏松材质或者夹持架上加工有用于排出粘结剂的通孔。
本发明的有益效果如下:
1)本发明采用钡酚醛树脂、环氧树脂、改性环氧树脂等作为粘合剂,将CVD金刚石自支撑膜和碳纤维两种性能优异的碳材料结合起来,实现二者的性能互补,制备出高结合强度金刚石碳纤维复合材料,该材料能够兼有金刚石的高热导率和碳纤维的高抗拉强度和高韧性,可作为高导热、高强度、高韧性、低密度的热管理材料,有效抵抗机械冲击和热冲击。
2)本发明高结合强度金刚石碳纤维复合材料在水平方向存在多层自支撑金刚石膜片,可作为高效散热通道,把接触的热量快速传走,因此可保证面内水平方向的高热导率,可达金刚石材料的90%左右,尤其适合主要需要面内散热的特殊场合。
3)本发明为了有效保障金刚石碳纤维间的结合力,提出织构化处理的创新方案;由于碳纤维为编织材料,粘合剂可完全渗透,因此粘合剂可实现对碳纤维的高强度粘合,金刚石片则表面粗糙度低,加上自身的惰性,导致粘合剂对其粘合度不高,本发明对金刚石进行织构化处理,织构图案为凹坑或凹痕组成的阵列,一方面增加了金刚石和胶黏剂的结合面积,另一方面,织构化的凹坑或凹痕会作为嵌入点,增加机械锁合作用力,提升金刚石和粘合剂的结合强度,最终实现高结合强度的金刚石/碳纤维复合材料的制备。
4)高结合强度金刚石碳纤维复合材料由两种材料通过粘合剂粘和形成,两种材料的形状、厚度均可调,因此复合材料整体的形状和厚度可根据热控***空间进行灵活调整,热导率可根据成本及实际需求进行调控。
附图说明
本申请的示意性附图只是用于对本申请的进一步理解,并不构成对本申请的不当限定。
图1为本发明高结合强度金刚石碳纤维复合材料的结构示意图。
图2为本发明高结合强度金刚石碳纤维复合材料制备示意图。
图3为本发明高结合强度金刚石碳纤维复合材料中自支撑金刚石膜片及其上的织构图案示意图。
图4为图3中的A-A剖视图。
图5为实施例1制备得到的高结合强度金刚石碳纤维复合材料的结构示意图。
图6为实施例2制备得到的高结合强度金刚石碳纤维复合材料的结构示意图。
图7为实施例3制备得到的高结合强度金刚石碳纤维复合材料的结构示意图。
图中:1-自支撑金刚石膜片、2-碳纤维层、3-织构图案、4-夹持架、5-重物。
具体实施方式
下面将结合参考附图及实施例,对本发明作进一步说明,但不局限于以下实施例。本领域普通人员在没有做出创造性劳动前提下所获得的所有其他实施例,均属于本发明的保护范围。
实施例1:
一种高结合强度金刚石碳纤维复合材料及其制备方法,由依次交替排列的自支撑金刚石膜片1和碳纤维层2叠置而成,并且其顶层和底层均为自支撑金刚石膜片1;自支撑金刚石膜片1的层数为三层,每层长、宽、厚为10 mm×5 mm×1 mm,碳纤维层2的层数为两层,每层长、宽、厚为10 mm×5 mm×0.3 mm;顶层自支撑金刚石膜片1的底面、底层自支撑金刚石膜片1的顶面以及中间层自支撑金刚石膜片1的顶面及底面均进行了织构化处理,如图5所示。
上述高结合强度金刚石碳纤维复合材料的具体制备方法包括以下步骤:
步骤1:选择直径为20 mm、厚度为1.2 mm、抗拉强度为900 MPa、热导率为600 W/(m·K)的CVD自支撑金刚石膜片1,考虑切割损耗,设计10 mm×5 mm的阵列,采用激光切割机进行切割,激光功率为12 W,频率为6 Hz;
步骤2:采用激光修面机对切割所得的自支撑金刚石膜片1进行厚度修整和表面光滑处理,厚度修整时激光功率为1000 W,沿厚度方向修整速度为0.02 μm/d,表面光滑处理时激光功率为450 W,修面处理后金刚石表面平整度为0.1 mm、平行度为0.1 mm、粗糙度为0.05 mm;
步骤3:采用激光打标机对切割、修整后的自支撑金刚石膜片1的碳纤维接触面进行织构化处理,形成织构图案3,织构图案3深度为0.1 mm;
步骤4:选用钡酚醛树脂和无水乙醇按1:5比例进行均匀调配,将抗拉强度为5000MPa、弹性模量为230 GPa的12 K碳纤维束置于上述溶液中浸润5分钟,取出后在空气中放置30分钟,然后平铺、粘合于有织构图案3的底层自支撑金刚石膜片1上,然后再在碳纤维束上铺设中层自支撑金刚石膜片1,交替平铺浸润过钡酚醛树脂的碳纤维和自支撑金刚石膜片1的过程,直至复合厚度达到要求,为提高复合强度,相邻两层碳纤维层2正交平铺,得到复合层结构;
步骤5:采用夹持架4对复合层结构的四个侧面施加5 N的夹持力使其平整,同时在顶层自支撑金刚石膜片1表面放置一质量为0.5 Kg的重物5,依靠其法向静压力排出碳纤维内富余树脂及弥散于树脂内的少量气泡;在保持侧面夹持及上表层施加压力的状态下对钡酚醛树脂进行加热固化,缓慢加热到200 ℃,保温3小时;
步骤6:移走夹持架4及重物5,对复合层结构的四个侧面进行打磨和超声清洗,去除侧面固化的钡酚醛树脂及碳纤维外漏的端部,打磨采用320#~800#的SiC金刚砂纸,超声清洗选用丙酮,清洗时间为15分钟,最终制备获得高结合强度金刚石碳纤维复合材料,如图5所示。
通过上述步骤制备的高结合强度金刚石碳纤维复合材料面内热导率约为500 W/(m·K),抗拉强度约为2000 MPa,同金刚石抗拉强度相比提高了约2.2倍。
实施例2:
一种高结合强度金刚石碳纤维复合材料及其制备方法,由依次交替排列的自支撑金刚石膜片1和碳纤维层2叠置而成,并且其顶层和底层均为自支撑金刚石膜片1;自支撑金刚石膜片1的层数为六层,每层长、宽、厚为15 mm×15 mm×0.6 mm,碳纤维层2的层数为五层,每层长、宽、厚为15 mm×15 mm×0.15 mm;顶层自支撑金刚石膜片1的底面、底层自支撑金刚石膜片1的顶面以及中间各层自支撑金刚石膜片1的顶面及底面均进行了织构化处理,如图6所示。
上述高结合强度金刚石碳纤维复合材料的具体制备方法包括以下步骤:
步骤1:选择直径为55 mm、厚度为0.8 mm、抗拉强度为600 MPa、热导率为1200 W/(m·K)的CVD自支撑金刚石膜片1,考虑切割损耗,设计15 mm×15 mm的阵列,采用激光切割机进行切割,激光功率为11 W,频率为7 Hz;
步骤2:采用激光修面机对切割所得的自支撑金刚石膜片1进行厚度修整和表面光滑处理,厚度修整时激光功率为900 W,沿厚度方向修整速度为0.02 μm/d,表面光滑处理时激光功率为400 W,修面处理后金刚石表面平整度为0.08 mm、平行度为0.08 mm、粗糙度为0.03 mm;
步骤3:采用激光打标机对切割、修整后的自支撑金刚石膜片1的碳纤维接触面进行织构化处理,形成织构图案3,织构图案3深度为0.08 mm;
步骤4:选用环氧树脂和无水乙醇按1:3比例进行均匀调配,将抗拉强度为4500MPa、弹性模量为220 GPa的12 K碳纤维束置于上述溶液中浸润3分钟,取出后在空气中放置20分钟,然后平铺、粘合于有织构图案3的底层自支撑金刚石膜片1上,然后再在碳纤维束上铺设中层自支撑金刚石膜片1,交替平铺浸润过环氧树脂的碳纤维和自支撑金刚石膜片1的过程,直至复合厚度达到要求,为提高复合强度,相邻碳纤维层2正交平铺,得到复合层结构;
步骤5:采用夹持架4对复合层结构的四个侧面施加5 N的夹持力使其平整,同时在顶层自支撑金刚石膜片1表面放置一质量为0.6 Kg的重物5,依靠其法向静压力排出碳纤维内富余树脂及弥散于树脂内的少量气泡;在保持侧面夹持及上表层施加压力的状态下对钡酚醛树脂进行加热固化,缓慢加热到260 ℃,保温6小时;
步骤6:移走夹持架4及重物5,对复合层结构的四个侧面进行打磨和超声清洗,去除侧面固化的钡酚醛树脂及碳纤维外漏的端部,打磨采用320#~800#的SiC金刚砂纸,超声清洗选用丙酮,清洗时间为15分钟,最终制备获得高结合强度金刚石碳纤维复合材料,如图6所示。
通过上述步骤制备的高结合强度金刚石碳纤维复合材料面内热导率约为1100 W/(m·K),抗拉强度约为1600 MPa,同金刚石抗拉强度相比提高了约2.7倍。
实施例3:
一种高结合强度金刚石碳纤维复合材料及其制备方法,由依次交替排列的自支撑金刚石膜片1和碳纤维层2叠置而成,并且其顶层和底层均为自支撑金刚石膜片1;自支撑金刚石膜片1的层数为十层,每层长、宽、厚为20 mm×15 mm×0.3 mm,碳纤维层2的层数为九层,每层长、宽、厚为20 mm×15 mm×0.1 mm;顶层自支撑金刚石膜片1的底面、底层自支撑金刚石膜片1的顶面以及中间各层自支撑金刚石膜片1的顶面及底面均进行了织构化处理,如图7所示。
上述高结合强度金刚石碳纤维复合材料的具体制备方法包括以下步骤:
步骤1:选择直径为75 mm、厚度为0.5 mm、抗拉强度为450 MPa、热导率为2000 W/(m·K)的CVD自支撑金刚石膜片1,考虑切割损耗,设计20 mm×15 mm的阵列,采用激光切割机进行切割,激光功率为10 W,频率为8 Hz;
步骤2:采用激光修面机对切割所得的自支撑金刚石膜片1进行厚度修整和表面光滑处理,厚度修整时激光功率为850 W,沿厚度方向修整速度为0.02 μm/d,表面光滑处理时激光功率为350 W,修面处理后金刚石表面平整度为0.05 mm、平行度为0.05 mm、粗糙度为0.01 mm;
步骤3:采用激光打标机对切割、修整后的自支撑金刚石膜片1的碳纤维接触面进行织构化处理,形成织构图案3,织构图案3深度为0.04 mm;
步骤4:选用环氧树脂和无水乙醇按1:1比例进行均匀调配,将抗拉强度为4000MPa、弹性模量为200 GPa的12 K碳纤维束置于上述溶液中浸润1分钟,取出后在空气中放置10分钟,然后平铺、粘合于有织构图案3的底层自支撑金刚石膜片1上,然后再在碳纤维束上铺设中层自支撑金刚石膜片1,交替平铺浸润过环氧树脂的碳纤维和自支撑金刚石膜片1的过程,直至复合厚度达到要求,为提高复合强度,相邻碳纤维层2正交平铺,得到复合层结构;
步骤5:采用夹持架4对复合层结构的四个侧面施加5 N的夹持力使其平整,同时在顶层自支撑金刚石膜片1表面放置一质量为0.7 Kg的重物5,依靠其法向静压力排出碳纤维内富余树脂及弥散于树脂内的少量气泡;在保持侧面夹持及上表层施加压力的状态下对钡酚醛树脂进行加热固化,缓慢加热到300 ℃,保温8小时;
步骤6:移走夹持架4及重物5,对复合层结构的四个侧面进行打磨和超声清洗,去除侧面固化的钡酚醛树脂及碳纤维外漏的端部,打磨采用320#~800#的SiC金刚砂纸,超声清洗选用丙酮,清洗时间为15分钟,最终制备获得高结合强度金刚石碳纤维复合材料,如图7所示。
通过上述步骤制备的高结合强度金刚石碳纤维复合材料面内热导率约为1800 W/(m·K),抗拉强度约为1500 MPa,同金刚石抗拉强度相比提高了3倍。
Claims (8)
1.一种高结合强度金刚石碳纤维复合材料,其特征在于:由依次交替排列的自支撑金刚石膜片和碳纤维层叠置而成,并且其顶层和底层均为自支撑金刚石膜片;顶层自支撑金刚石膜片的底面、底层自支撑金刚石膜片的顶面以及中间各层自支撑金刚石膜片的顶面及底面均进行了织构化处理;
上述高结合强度金刚石碳纤维复合材料的制备方法,包括如下步骤:
步骤1:根据高结合强度金刚石碳纤维复合材料对自支撑金刚石膜片的尺寸要求,选择合适直径及厚度的自支撑金刚石膜片,设计形状阵列并进行切割;
步骤2:采用激光修面机对切割所得的自支撑金刚石膜片进行厚度修整和表面光滑处理;
步骤3:对厚度修整和表面光滑处理后的自支撑金刚石膜片表面进行单面织构化处理或双面织构化处理;
步骤4:将粘结剂和无水乙醇按比例均匀调配,把调配液刷涂到底层自支撑金刚石膜片的织构表面,使调配液填充织构化盲孔或凹痕;把碳纤维置于调配液中浸润1-5分钟,取出后在空气中放置10-30分钟,然后平铺、粘合于底层自支撑金刚石膜片的织构表面,重复平铺浸润过粘结剂的碳纤维和刷涂了粘结剂的织构化的自支撑金刚石膜片,直至复合厚度达到要求,得到复合层结构;
步骤5:通过夹持架对复合层结构进行夹持以保证其平整度,同时在最上层自支撑金刚石膜片表面放置重物,依靠法向静压力排出碳纤维内富余粘结剂及弥散于粘结剂内的气泡,然后在保持侧面夹持及上表层施加压力的状态下对粘结剂进行加热固化;
步骤6:去除重物及夹持架,对复合层结构的侧面进行打磨和超声清洗,最终得到所述的高结合强度金刚石碳纤维复合材料。
2.根据权利要求1所述的高结合强度金刚石碳纤维复合材料,其特征在于:自支撑金刚石膜片为采用CVD法制备得到的自支撑金刚石膜片,其热导率≥600 W/(m·K)、平行度≤0.1 mm、非织构处的平整度≤0.1 mm;自支撑金刚石膜片的厚度为0.3 mm~1 mm,碳纤维层的厚度为0.1 mm~0.3 mm。
3.根据权利要求1或2所述的高结合强度金刚石碳纤维复合材料,其特征在于:自支撑金刚石膜片表面的织构图案为圆形盲孔阵列或线性凹痕阵列,织构图案的深度为自支撑金刚石膜片厚度的1%~10%。
4.根据权利要求1或2所述的高结合强度金刚石碳纤维复合材料,其特征在于:自支撑金刚石膜片的层数为2~20层。
5.根据权利要求1所述的高结合强度金刚石碳纤维复合材料,其特征在于:步骤4中,粘结剂采用钡酚醛树脂、环氧树脂或改性环氧树脂。
6.根据权利要求1所述的高结合强度金刚石碳纤维复合材料,其特征在于:步骤4中,粘结剂和无水乙醇调配比例为1:1~1:5。
7.根据权利要求1所述的高结合强度金刚石碳纤维复合材料,其特征在于:步骤5中,加热固化时的加热温度为200~300 ℃、保温时间为3~8 h。
8.根据权利要求1所述的高结合强度金刚石碳纤维复合材料,其特征在于:步骤5中,夹持架的材质采用疏松材质或者夹持架上加工有用于排出粘结剂的通孔。
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