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混合溶剂分散法制备耐高温、高导热六方氮化硼/半芳香聚酰胺12T复合材料及其性能研究

陈晓杰 马舸 孟慧迪 崔喆 付鹏 赵蔚 庞新厂 赵清香 刘民英 张晓朦

陈晓杰, 马舸, 孟慧迪, 等. 混合溶剂分散法制备耐高温、高导热六方氮化硼/半芳香聚酰胺12T复合材料及其性能研究[J]. 复合材料学报, 2022, 40(0): 1-11
引用本文: 陈晓杰, 马舸, 孟慧迪, 等. 混合溶剂分散法制备耐高温、高导热六方氮化硼/半芳香聚酰胺12T复合材料及其性能研究[J]. 复合材料学报, 2022, 40(0): 1-11
Xiaojie CHEN, Ge MA, Huidi MENG, Zhe CUI, Peng FU, Wei ZHAO, Xinchang PANG, Qingxiang ZHAO, Minying LIU, Xiaomeng ZHANG. Study on preparation and properties of hexagonal boron nitride/semi-aromatic polyamide 12T composites with high-temperature resistance and high thermal conductivity prepared by mixed solvent dispersion method[J]. Acta Materiae Compositae Sinica.
Citation: Xiaojie CHEN, Ge MA, Huidi MENG, Zhe CUI, Peng FU, Wei ZHAO, Xinchang PANG, Qingxiang ZHAO, Minying LIU, Xiaomeng ZHANG. Study on preparation and properties of hexagonal boron nitride/semi-aromatic polyamide 12T composites with high-temperature resistance and high thermal conductivity prepared by mixed solvent dispersion method[J]. Acta Materiae Compositae Sinica.

混合溶剂分散法制备耐高温、高导热六方氮化硼/半芳香聚酰胺12T复合材料及其性能研究

基金项目: 国家重点研发计划(2017YFB0307600);中国博士后科学基金(2020M682317);河南省博士后基金(202002018);高分子材料工程国家重点实验室开放课题(sklpme2021-05-10);河南省高等学校重点科研项目(22A430037)
详细信息
    通讯作者:

    刘民英,博士,教授,博士生导师,研究方向为聚酰胺的结构设计与聚合方法 E-mail: lmy@zzu.edu.cn

    张晓朦,博士,副教授,硕士生导师,研究方向为聚酰胺基复合材料的结构设计与性能研究 E-mail: zhangxm@zzu.edu.cn

  • 中图分类号: TB332

Study on preparation and properties of hexagonal boron nitride/semi-aromatic polyamide 12T composites with high-temperature resistance and high thermal conductivity prepared by mixed solvent dispersion method

  • 摘要: 制备兼具优异耐高温性能和导热性能的聚合物基复合材料对于电子元器件的封装保护、高效散热和稳定成型至关重要。本文通过混合溶剂分散法(MSD)制备了六方氮化硼(BN)/半芳香聚酰胺12T(PA12T)复合材料,并对复合材料的微观结构、导热、耐高温、介电和力学性能进行了表征。结果表明,混合溶剂分散法可以有效实现BN和PA12T粉末的均匀悬浮,并可协同真空辅助自组装法与真空热压法构筑具有均一分散和取向结构的复合材料。研究表明,当BN/PA12T复合材料中的BN含量为40wt%时,混合溶剂分散法制备的样品的平面导热率可以达到2.73 W/(m·K),是机械混合法(MM)制备的样品(1.59 W/(m·K))的1.72倍,同时其具有优异的力学性能、低介电常数(3.6)、介电损耗(0.016)和显著的耐高温性能(维卡软化点超过250°C且初始分解温度可达445°C)。综上所述,混合溶剂分散法制备的BN/PA12T复合材料在电子封装及热管理领域中具有广阔的应用前景。

     

  • 图  1  六方氮化硼(BN)和半芳香聚酰胺12T(PA12T)粉末悬浮于不同溶剂和混合溶剂 (a) 及不同静置时间的40wt% BN/PA12T混合粉末悬浮于混合溶剂 (b) 的光学图

    Figure  1.  Images of hexagonal boron nitride (BN) and semi-aromatic polyamide 12T (PA12T) powder suspended in different solvents and mixed solvent (a) and 40wt% BN/PA12T mixed powder suspended in mixed solvent with different resting time (b)

    图  2  BN (a)、PA12T (b) 及机械混合法 (c, e, g, i) 和混合溶剂分散法 (d, f, h, j) 制备的BN/PA12T复合材料的扫描电镜图

    Figure  2.  SEM images of BN powder (a) and pure PA12T (b), the composites prepared by mechanical mixing (MM) method (c, e, g, i) and mixed solvent dispersion (MSD) method (d, f, h, j)

    图  3  不同方法制备的BN/PA12T复合材料的XRD谱图

    Figure  3.  XRD patterns of the BN/PA12T composites prepared by different methods with various content of BN

    图  4  不同方法制备的BN/PA12T复合材料沿平面方向和厚度方向的导热率 (a) 以及各项异性指数 (b)

    Figure  4.  Thermal conductivities (a) along the in-plane and through-plane directions and anisotropy index (b) of the BN/PA12T composites prepared by different methods with various content of BN

    图  5  机械混合法 (A) 和混合溶剂分散法 (B) 制备的40wt% BN/PA12T复合材料在LED热管理应用过程中的热成像图

    Figure  5.  Optical and thermal images of the 40wt% BN/PA12T composites prepared by the mechanical mixing method (A) and the mixed solvent dispersion method (B) for the thermal management of LED

    图  6  不同方法制备的BN/PA12T复合材料的储能模量

    Figure  6.  Storage modulus of BN/PA12T composites prepared by different methods with various content of BN

    图  7  不同方法制备的BN/PA12T复合材料的拉伸 (a) 和弯曲 (b) 性能

    Figure  7.  Tensile (a) and flexural (b) properties of composites prepared by different methods with various content of BN

    图  8  混合溶剂分散法制备的BN/PA12T复合材料在氮气气氛下的TG (a) 和DTG (b) 曲线

    Figure  8.  The TG (a) and DTG (b) curves of BN/PA12T composites prepared by mixed solvent dispersion method under N2 atmosphere with various content of BN

    图  9  混合溶剂分散法制备的BN/PA12T复合材料的维卡软化温度

    Figure  9.  The Vicat softening temperatures of BN/PA12T composites prepared by mixed solvent dispersion method with various content of BN

    图  10  混合溶剂分散法制备的BN/PA12T复合材料的介电常数

    Figure  10.  The dielectric constant of the BN/PA12T composites prepared by mixed solvent dispersion method with various BN content

    表  1  BN的取向度分析

    Table  1.   Analysis on the orientation degree of BN

    BN content/
    wt%
    Preparation methodsI(002)I(100)I(002)/I(100)
    10Mixed solvent dispersion63324236927
    10Mechanical mixing2287941336
    20Mixed solvent dispersion93765361026
    20Mechanical mixing5000558389
    30Mixed solvent dispersion89145606915
    30Mechanical mixing6512772859
    40Mixed solvent dispersion106008741614
    40Mechanical mixing97303815112
    下载: 导出CSV

    表  2  热塑性耐高温聚合物基导热复合材料的导热率

    Table  2.   Thermal conductivities of thermoplastic heat-resistance polymer-based composites

    MatrixFillerContentTC/
    (W·(m·K)−1)
    Preparation method/
    Testing method
    Year
    Liquid crystral polymer (LCP) BN (~60 μm) 33vol% 3.29 Clamped-air-cooling/Heat Flow 2013[31]
    Poly(ether ether ketone)
    (PEEK)
    BN nanopowders (~70 nm) 30wt% 1.04 Casting/LFA 2021[32]
    Poly(ether ether ketone)
    (PEEK)
    BN (4-10 μm) 30wt% 1.01 Hot pressing/LFA 2020[33]
    Polyetherimide (PEI) Non-covalent modified BN 30wt% 0.82 Hot pressing/LFA 2021[34]
    Polyetherimide (PEI) Polyimide-coated BN 60wt% 2.55 Injection molding/LFA 2014[35]
    Polyphenylene sulfide (PPS) Micrometer BN/nanometer BN 60wt% 2.64 Hot pressing /Hot Disk 2017[36]
    Polyphenylene sulfide (PPS) Siloxane modified BN 50wt% 1.60 Injection molding/LFA 2018[37]
    Polyphenylene sulfide (PPS) Siloxane modified nanometer BN 60wt% 1.12 Hot pressing/ Hot Disk 2017[38]
    Theromplastic polyimide (TPI) Silver nanowires-decorated multi-walled carbon nanotubes 3wt% 0.44 Casting/Transient Hot-wire 2022[39]
    Polyamide 46 (PA46) Carbon fiber (diameter=7.2μm, aspect ratio=7) 40wt% 1.49 Injection molding/LFA 2017[40]
    PA12T BN (2-4μm) 40wt% 2.73 Mixed solvent dispersion /LFA This work
    下载: 导出CSV

    表  3  混合溶剂分散法制备的BN/PA12T复合材料的热失重性能

    Table  3.   The thermogravimetic analysis of BN/PA12T composites prepared by mixed solvent dispersion method

    BN content /wt%T5%/℃Tmax/℃Vmax/(%·℃−1)ω/% (600℃)
    0439.37476.483.0181.353
    10441.79473.492.65410.375
    20441.48473.912.42621.261
    30443.92472.652.14630.852
    40445.85472.311.89639.622
    Notes: T5% is decomposition temperature in 5wt% mass loss fraction; Tmax is the temperature corresponding to the maximum decomposition rate; -Vmax is the maximum decomposition rate; ω is the mass residual rate in 600℃.
    下载: 导出CSV

    表  4  混合溶剂分散法制备的BN/PA12T复合材料的介电损耗

    Table  4.   The dielectric loss of BN/PA12T composites prepared by mixed solvent dispersion method with various content of BN

    BN content/wt%Dielectric loss (106 Hz)
    00.050
    100.041
    200.033
    300.025
    下载: 导出CSV
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    CAI Delong, CHEN Fei, HE Fengmei, et al. Recent progress and prospestion on high-temperature wave-transparent ceramic materials[J]. Advanced Ceramics,2019,40(Z1):4-120(in Chinese).
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出版历程
  • 收稿日期:  2022-01-10
  • 录用日期:  2022-03-13
  • 修回日期:  2022-03-04
  • 网络出版日期:  2022-03-30

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