CN108656676A - 一种多层导热复合材料及其制备方法 - Google Patents

一种多层导热复合材料及其制备方法 Download PDF

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CN108656676A
CN108656676A CN201810179677.4A CN201810179677A CN108656676A CN 108656676 A CN108656676 A CN 108656676A CN 201810179677 A CN201810179677 A CN 201810179677A CN 108656676 A CN108656676 A CN 108656676A
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heat
composite material
conductive composite
mass parts
thermal insulation
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祝渊
孙琪
付婷婷
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Southwest University of Science and Technology
Southern University of Science and Technology
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Abstract

本发明涉及导热材料领域，具体涉及一种多层导热复合材料及其制备方法。所述多层导热复合材料包括依次层叠的绝缘导热层一、碳材料导热层和绝缘导热层二，所述碳材料导热层包括聚合物和碳材料，所述绝缘导热层一和绝缘导热层二均包括聚合物和导热填料。本发明的多层导热复合材料利用碳材料良好的导热性能，同时，加入绝缘导热层，进一步增强材料的绝缘性能，保证复合材料在绝缘性和导热性两个方面的平衡，本发明所述的多层导热复合材料在对精密电子设备领域具有广泛的应用前景。

Description

一种多层导热复合材料及其制备方法
技术领域
本发明涉及导热材料领域，具体涉及一种多层导热复合材料及其制备方法。
背景技术
导热材料是一种新型工业材料。这些材料是近年来针对设备的热传导要求而设计的，性能优异、可靠。它们适合各种环境和要求，对可能出现的导热问题都有妥善的对策，对设备的高度集成，以及超小超薄提供了有力的帮助，导热材料已经越来越多的应用到许多产品中，提高了产品的可靠性。
众所周知，评价导热材料需要从两个方面进行，即绝缘性和导热性。传统的导热材料，如金属、碳材料等，虽具有较好的导热性能，但同时存在导电问题，对于电气元件的正常运行极为不利，在手机等通讯设备上，若导热材料导电，会极大影响通讯信号的传输能力和质量。因此，需要制造具有绝缘性的导热材料，这种导热材料主要为金属氧化物、氮化物及其他非金属材料制成，但是，绝缘性导热材料由于采用上述材料，其本身的导热性能低于金属、碳材料制成的导热材料，需要很高的填充量才能获得较高的热导率。因此，人们急需一种兼顾绝缘性和导热性，即在提高材料绝缘性的前提下，同时可提高材料的导热性能，以克服现有的导热材料绝缘性和导热性难以兼顾的缺陷。
发明内容
本发明所要解决的技术问题是：提供一种多层导热复合材料及其制备方法，其可克服现有的导热材料绝缘性和导热性难以兼顾的缺陷，在提高材料绝缘性的前提下，同时可提高材料的导热性能。
为解决上述技术问题所采用的技术方案是：
一种多层导热复合材料，包括依次层叠的绝缘导热层一、碳材料导热层和绝缘导热层二，所述碳材料导热层包括56-90质量份的聚合物、10-40质量份的碳材料和0-4质量份的偶联剂，所述绝缘导热层一和绝缘导热层二均分别包括16-50 质量份的聚合物、50-80质量份的导热填料和0-4质量份的偶联剂。
在一种优选的实施方式中，所述偶联剂包括硅烷偶联剂、钛酸酯偶联剂KB-44、KR-38S、KR-TTS中的至少一种。
在一种优选的实施方式中，所述碳材料导热层为聚合物和碳材料形成的三维编织物。
在一种优选的实施方式中，所述碳材料导热层和绝缘导热层一的厚度比为 1:10-10:1，所述碳材料导热层和绝缘导热层二的厚度比为1:10-10:1。
在一种优选的实施方式中，所述碳材料包括碳纤维、石墨纤维、碳纳米管纤维、石墨烯纤维中的至少一种。
在一种优选的实施方式中，所述导热填料包括氮化硼、氮化硅、氮化铝、碳化硅、氧化铝、氧化硅、氧化镁中的至少一种。
在一种优选的实施方式中，所述聚合物包括聚酰亚胺、环氧树脂、酚醛树脂、聚酯树脂中的至少一种。
上述任一项所述的多层导热复合材料的制备方法，包括以下步骤：
(1)取碳材料和聚合物混合均匀形成碳材料导热层原料；
(2)取导热填料和聚合物混合均匀形成绝缘导热层原料；
(3)取所述碳材料导热层原料置于模具中层，取所述绝缘导热层原料置于模具的上下层，利用热压成型工艺制备得到多层导热复合材料。
(4)还包括在步骤(1)和(2)的至少一项中加入偶联剂进行改性处理的任选步骤。
在一种优选的实施方式中，还包括将制得的碳材料导热层原料进行静电纺丝得到纤维，并对所述纤维进行三维编织，得到相互旋转或正交交织的具有整体结构的织物。
本发明的有益效果是：
本发明所述复合材料利用碳材料良好的导热性能，同时，加入绝缘导热层，进一步增强材料的绝缘性能，所述复合材料具有优异的导热性能和绝缘性，解决了现有技术中导热性能和绝缘性不能兼顾的问题。
具体实施方式
为使本领域技术人员更好的理解本发明的技术方案，以下对本发明所述多层导热复合材料及其制备方法做详细说明。
实施例1
(1)取40质量份的碳纤维与60质量份的环氧树脂搅拌混合均匀后，在模具中，100℃条件热压固化1h，冷却后脱模得到半固化碳纤维导热层；
(2)将60质量份的氮化硼与30质量份的环氧树脂搅拌混合均匀后填充在模具上下层，步骤(1)中制得的碳纤维导热层置于模具中层，在120℃条件下热压固化2h，得到多层导热复合材料。
所述多层导热复合材料具有绝缘导热层一和绝缘导热层二，一层碳材料导热层位于绝缘导热层一和绝缘导热层二之间。
实施例2
(1)取40质量份的碳纤维与60质量份的聚酰亚胺搅拌混合均匀后，在模具中，100℃条件热压固化1h，冷却后脱模得到半固化碳纤维导热层；
(2)将60质量份的氮化硼与30质量份的聚酰亚胺搅拌混合均匀后填充在模具上下层，步骤(1)中制得的碳纤维导热层置于模具中层，在120℃条件下热压固化2h，得到多层导热复合材料。
实施例3
(1)分别用1质量份的KH560对40质量份的碳纤维和60质量份的氮化硼进行改性处理；
(2)将改性后的碳纤维与60质量份的环氧树脂搅拌混合均匀后，在模具中， 100℃条件热压固化1h，冷却后脱模得到半固化碳纤维导热层；
(3)将改性后的氮化硼与30质量份的环氧树脂搅拌混合均匀后填充在模具上下层，步骤(2)中制得的碳纤维导热层置于模具中层，在150℃条件下热压固化2h，得到多层导热复合材料。
本实施例中加入KH560作为偶联剂对碳材料和导热填料进行改性，可使碳材料和导热填料分散于聚合物中，从而提高复合材料的导热性能和绝缘性能。
实施例4
(1)分别用1质量份的KH560对40质量份的碳纤维和60质量份的氮化硼进行改性处理；
(2)将改性后的碳纤维与60质量份的环氧树脂搅拌混合均匀后形成溶胶，对溶胶进行静电纺丝，得到碳纤维-环氧树脂纤维；
(3)步骤(2)中制得的碳纤维-环氧树脂纤维进行三维编织，得到碳纤维导热层预制体；
(4)将改性后的氮化硼与30质量份的环氧树脂搅拌混合均匀后填充在模具上下层，步骤(3)中制得的碳纤维导热层预制体置于模具中层，在150℃条件下热压固化2h，得到多层导热复合材料。
本实施例中对改性后的碳材料和聚合物溶胶进行纺丝并进行三维编织，促进了碳材料的取向性，提高了材料的热导率。
实施例5：导热性能和绝缘性能测试
对比例1
(1)用1质量份的KH560对60质量份的氮化硼陶瓷粉末进行改性处理；
(2)将改性后的氮化硼与30质量份的环氧树脂搅拌混合均匀后填充在模具中，在150℃条件下热压固化2h，得到导热复合材料。
对比例2
(1)用1质量份的KH560对10质量份的碳纤维进行改性处理；
(2)将改性后的碳纤维与60质量份的环氧树脂混合均匀后填充在模具中，在150℃条件下热压固化2h，得到导热复合材料。
取实施例1-4制得的多层导热复合材料和对比例1-2制得的复合材料，进行导热性能和绝缘性能测试。遵照ASTM E1461，用闪光法测定所述导热复合材料的热扩散系数，差示扫描量热仪测定比热容，密度天平测定密度，按照热导率＝热扩散系数×比热容×密度可计算出所述导热复合材料的导热系数。按照GB/T 1410-2006测定所述导热复合材料的体积电阻率。上述各实施例和对比例中所制备的多层导热复合材料的热导率和体积电阻率如下表所示：
由上表可知，实施例3制备的复合材料热导率为21.45W/m·K，体积电阻率为5.32×1015Ω·cm，对比例1中只使用了绝缘导热层，其绝缘性能较实施例3 更好，体积电阻率达到3.81×1016Ω·cm，而热导率为18.64W/m·K。表明绝缘导热层虽然提供了材料较好的绝缘性能，但由于采用了金属氧化物或金属氮化物等，其本身的导热性能不佳；对比例2中只使用了碳材料导热层，其导热率可达到 27.02W/m·K，但是体积电阻率仅为4.67×1010Ω·cm，远远低于实施例3中的体积电阻率，碳材料导热层在保证良好导热率的前提下，由于本身导电的特性，体积电阻率极低，不能保证复合材料的绝缘特性。因此，实施例3中将碳材料导热层置于两层绝缘导热层之间，使复合材料利用碳材料良好的导热性能，同时，加入绝缘导热层，进一步增强材料的绝缘性能，保证复合材料在绝缘性和导热性两个方面的平衡。
另外，实施例4中，复合材料的热导率为30.14W/m·K，体积电阻率为2.64 ×1015Ω·cm，相对于实施例3，其热导率有较大提升，且体积电阻率保持在一个数量级上。可见，利用静电纺丝制成碳纤维-聚合物纤维，再利用三维编织成为相互旋转或正交交织形成的具有整体结构的织物，促进了碳材料的取向性，提高了材料的热导率，同时也可保持材料较好的绝缘性。
实施例6
(1)分别用1质量份的KR-38S对10质量份的碳纤维和50质量份的氮化硼进行改性处理；
(2)将改性后的碳纤维与56质量份的环氧树脂搅拌混合均匀后，在模具中， 100℃条件热压固化1h，冷却后脱模得到半固化碳纤维导热层；
(3)将改性后的氮化硼与16质量份的环氧树脂搅拌混合均匀后填充在模具上下层，步骤(2)中制得的碳纤维导热层置于模具中层，在120℃条件下热压固化2h，得到多层导热复合材料。
实施例7
本实施例与实施例6基本相同，不同之处在于：步骤(1)中，分别用1质量份的KR-38S对10质量份的石墨纤维和50质量份的氮化硅进行改性处理。
实施例8
本实施例与实施例6基本相同，不同之处在于：步骤(1)中，分别用1质量份的KR-38S对10质量份的碳纳米管纤维和50质量份的氮化铝进行改性处理。
实施例9
本实施例与实施例6基本相同，不同之处在于：步骤(1)中，分别用1质量份的KR-38S对10质量份的石墨烯纤维和50质量份的碳化硅进行改性处理。
实施例10
(1)分别用1质量份的KR-TTS对40质量份的碳纤维和80质量份的氮化硼进行改性处理；
(2)将改性后的碳纤维与90质量份的环氧树脂搅拌混合均匀后形成溶胶，对溶胶进行静电纺丝，得到碳纤维-环氧树脂纤维；
(3)步骤(2)中制得的碳纤维-环氧树脂纤维进行三维编织，得到碳纤维导热层预制体；
(4)将改性后的氮化硼与50质量份的环氧树脂搅拌混合均匀后填充在模具上下层，步骤(3)中制得的碳纤维导热层预制体置于模具中层，在150℃条件下热压固化2h，得到多层导热复合材料。
实施例11
本实施例与实施例10基本相同，不同之处在于：步骤(1)中，分别用4 质量份的KR-TTS对40质量份的石墨纤维和80质量份的氮化硅进行改性处理。
实施例12
本实施例与实施例10基本相同，不同之处在于：步骤(1)中，分别用4 质量份的KR-TTS对40质量份的碳纳米管纤维和80质量份的氮化铝进行改性处理。
实施例13
本实施例与实施例10基本相同，不同之处在于：步骤(1)中，分别用4 质量份的KR-TTS对40质量份的石墨烯纤维和80质量份的碳化硅进行改性处理。
以上对本发明的较佳实施方式进行了具体说明，但本发明并不限于所述实施例，熟悉本领域的技术人员在不违背本发明精神的前提下还可作出种种的等同变型或替换，这些等同的变型或替换均包含在本申请权利要求所限定的范围内。

Claims (9)

1.一种多层导热复合材料，其特征在于，包括依次层叠的绝缘导热层一、碳材料导热层和绝缘导热层二，所述碳材料导热层包括56-90质量份的聚合物、10-40质量份的碳材料和0-4质量份的偶联剂，所述绝缘导热层一和绝缘导热层二均分别包括16-50质量份的聚合物、50-80质量份的导热填料和0-4质量份的偶联剂。
2.如权利要求1所述的多层导热复合材料，其特征在于，所述偶联剂包括硅烷偶联剂、钛酸酯偶联剂中的至少一种。
3.如权利要求1或2所述的多层导热复合材料，其特征在于，所述碳材料导热层为聚合物和碳材料形成的三维编织物。
4.如权利要求1所述的多层导热复合材料，其特征在于，所述碳材料导热层和绝缘导热层一的厚度比为1:10-10:1，所述碳材料导热层和绝缘导热层二的厚度比为1:10-10:1。
5.如权利要求1所述的多层导热复合材料，其特征在于，所述碳材料包括碳纤维、石墨纤维、碳纳米管纤维、石墨烯纤维中的至少一种。
6.如权利要求1所述的多层导热复合材料，其特征在于，所述导热填料包括氮化硼、氮化硅、氮化铝、碳化硅、氧化铝、氧化硅、氧化镁中的至少一种。
7.如权利要求1所述的多层导热复合材料，其特征在于，所述聚合物包括聚酰亚胺、环氧树脂、酚醛树脂、聚酯树脂中的至少一种。
8.权利要求1-7任一项所述的多层导热复合材料的制备方法，其特征在于，包括以下步骤：
(1)取碳材料和聚合物混合均匀形成碳材料导热层原料；
(2)取导热填料和聚合物混合均匀形成绝缘导热层原料；
(3)取所述碳材料导热层原料置于模具中层，取所述绝缘导热层原料置于模具的上下层，利用热压成型工艺制备得到多层导热复合材料。
(4)还包括在步骤(1)和(2)的至少一项中加入偶联剂进行改性处理的任选步骤。
9.如权利要求9所述的多层导热复合材料的制备方法，其特征在于，还包括将制得的碳材料导热层原料进行静电纺丝得到纤维，并对所述纤维进行三维编织，得到相互旋转或正交交织的具有整体结构的织物。
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