CN107293412A - 一种电容器用埃洛石纳米管增强的电极材料及其制备方法 - Google Patents
一种电容器用埃洛石纳米管增强的电极材料及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种电容器用埃洛石纳米管增强的电极材料的制备方法,其特征在于,将金刚石粉干燥后,加入无水乙醇、KH550,得预处理金刚石粉;向氧化石墨烯中加KH550、催化剂,油浴下搅拌反应;然后分散于丙酮中,加入凹凸棒土,超声处理,得复合增强体;将埃洛石纳米管加入盐酸中,离心分离,烘干;再加无水甲苯,超声混合后,加KH550,搅拌回流,得改性埃洛石纳米管;将改性埃洛石纳米管加入去离子水中,超声得悬浮液;将氧化石墨烯分散到去离子水中,超声得悬浮液;将悬浮液混合,离心分离、水洗,分散到去离子水中,加入水合肼,水浴中回流,离心分离,与前面所得物料混合研磨,得到电极材料。
Description
技术领域
本发明涉及电容器领域,具体涉及一种电容器用埃洛石纳米管增强的电极材料的制备方法。
背景技术
随着电子信息技术的飞速发展,对电子电路用印刷电路板(PCB)的性能也提出了更高的要求。体积轻薄且功耗较大的电子设备从诞生起就被发热问题所困扰,PCB作为每个发热器件的桥梁和载体,一直是增强设备散热的研究重点,导热性能优良的基板材料以及良好散热结构的PCB都能够将发热器件产生的热量均匀分布,增强散热效率,减少昂贵器件的热损伤。
发明内容
本发明主要解决的技术问题是提供一种电容器用埃洛石纳米管增强的电极材料的制备方法,依照该工艺制备的电极材料具有良好的电化学性能和导热性。
本发明所要解决的技术问题采用以下的技术方案来实现:
一种电容器用埃洛石纳米管增强的电极材料的制备方法,其特征在于,按以下步骤进行:
a. 金刚石粉的预处理:
将10-15重量份金刚石粉于90-100℃烘箱中干燥1-2h后,1:5-10加入无水乙醇中,超声搅拌均匀,加入0.5-1重量份KH550,于80-90℃回流3-4h,静置、过滤3-5次,放入100-110℃真空烘箱中干燥2-4h,研磨粉碎;
b. 氧化石墨烯的部分还原及修饰:
向5-10重量份氧化石墨烯中加入0.5-1重量份KH550,置于冰水浴中,用超声波细胞粉碎机超声剥离1-2h,分散均匀,加入0.5-1重量份催化剂,在70-80℃油浴下,磁力搅拌反应5-6h,过滤、醇洗3-5次,置于80-90℃鼓风烘箱中干燥完全、机械研磨粉碎;
然后1:5-10分散于丙酮中,超声振荡1-2h,加入6-9重量份凹凸棒土,继续超声处理1-2h,将混合液置于敞口容器中在70-80℃持续搅拌,蒸发掉溶剂丙酮,制得复合增强体;
c. 埃洛石纳米管的改性处理:
将10-15重量份埃洛石纳米管1:5-10加入pH为2-3的盐酸中,搅拌处理2-4h,离心分离,置于120-130℃真空烘箱中烘干;再加入20-30重量份无水甲苯,超声混合30-40min后,加入1-2重量份KH550,110-120℃下搅拌回流2-4h,离心分离,洗涤,在40-60℃的真空烘箱中烘干,得改性埃洛石纳米管;
d. 将c中所得改性埃洛石纳米管1:15-20加入去离子水中,超声1-2h得悬浮液A;将5-10重量份氧化石墨烯1:20-25分散到去离子水中,超声1-2h得悬浮液B;
将悬浮液A、B混合,边搅拌边缓慢加盐酸调pH为2-3,离心分离、水洗3-5次,1:5-10分散到去离子水中,加入1-2重量份水合肼,置于85-95℃水浴中回流2-3h,离心分离,用去离子水、乙醇各洗涤3-5次,产物于60-70℃真空烘箱中烘干,与a、b中所得物料混合研磨,得到电极材料。
其中,步骤b中所述催化剂为N,N,-二环己基碳二亚胺。步骤c中所述洗涤是用甲苯、乙醇各洗涤3-5次。步骤d中所述盐酸浓度为5-10%,水合肼浓度为30-35%。
本发明的反应机理及有益效果如下:
先用酸对埃洛石纳米管进行处理,再用KH550对其外表面进行有机化修饰;改性后的埃洛石纳米管分子末端存在氨基短链,在酸性条件下可转化为正电;与带负电的氧化石墨烯以静电相互作用自组装,得到复合物;用水合肼还原复合物,使氧化石墨烯转化为石墨烯,所得材料具有良好的电化学性能,可用作超级电容器的电极材料,在能源存储方面有应用价值。
用硅烷偶联剂KH550对金刚石粉进行表面处理后,颗粒表面更光滑,不会产生团聚,降低了颗粒表面极性,提高其在复合物中的分散性,金刚石颗粒之间相互接触,形成导热链条,提高了复合材料的导热系数;用KH550对氧化石墨烯进行部分还原及功能化修饰,得到改性石墨烯,偶联剂的氨基与氧化石墨烯表面的环氧基团发生了亲核取代反应;再通过溶液法,使凹凸棒土颗粒以氢键结合的方式吸附在氧化石墨烯片层表面,得到复合增强体,提高了复合材料的力学性能、断裂韧性及热稳定性。
具体实施方式
为了使本发明实现的技术手段、创作特征、达成目的与功效易于明白了解,下面结合具体实施例,进一步阐述本发明。
实施例
一种电容器用埃洛石纳米管增强的电极材料的制备方法,其特征在于,按以下步骤进行:
a. 金刚石粉的预处理:
将10kg金刚石粉于90-100℃烘箱中干燥1h后,1:5加入无水乙醇中,超声搅拌均匀,加入0.5kg KH550,于80-90℃回流3h,静置、过滤3次,放入100-110℃真空烘箱中干燥2h,研磨粉碎;
b. 氧化石墨烯的部分还原及修饰:
向5kg氧化石墨烯中加入0.5kg KH550,置于冰水浴中,用超声波细胞粉碎机超声剥离1h,分散均匀,加入0.5kg催化剂,在70-80℃油浴下,磁力搅拌反应5h,过滤、醇洗3次,置于80-90℃鼓风烘箱中干燥完全、机械研磨粉碎;
然后1:10分散于丙酮中,超声振荡1h,加入6kg凹凸棒土,继续超声处理1h,将混合液置于敞口容器中在70-80℃持续搅拌,蒸发掉溶剂丙酮,制得复合增强体。
c. 埃洛石纳米管的改性处理:
将10kg埃洛石纳米管1:10加入pH为2-3的盐酸中,搅拌处理2h,离心分离,置于120-130℃真空烘箱中烘干;再加入20kg无水甲苯,超声混合35min后,加入1kg KH550,110-120℃下搅拌回流2h,离心分离,洗涤,在40-60℃的真空烘箱中烘干,得改性埃洛石纳米管;
d. 将c中所得改性埃洛石纳米管1:15加入去离子水中,超声1h得悬浮液A;将5kg氧化石墨烯1:20分散到去离子水中,超声1h得悬浮液B;
将悬浮液A、B混合,边搅拌边缓慢加盐酸调pH为2-3,离心分离、水洗3次,1:10分散到去离子水中,加入1kg水合肼,置于85-95℃水浴中回流2h,离心分离,用去离子水、乙醇各洗涤3次,产物于60-70℃真空烘箱中烘干,与a、b中所得物料混合研磨,得到电极材料。
其中,步骤b中所述催化剂为N,N,-二环己基碳二亚胺。步骤c中所述洗涤是用甲苯、乙醇各洗涤3次。步骤d中所述盐酸浓度为8%,水合肼浓度为30%。
Claims (5)
1.一种电容器用埃洛石纳米管增强的电极材料,其特征在于:
将金刚石粉干燥后,加入无水乙醇、KH550,得预处理金刚石粉;向氧化石墨烯中加KH550、催化剂,油浴下搅拌反应;然后分散于丙酮中,加入凹凸棒土,超声处理,得复合增强体;将埃洛石纳米管加入盐酸中,离心分离,烘干;再加无水甲苯,超声混合后,加KH550,搅拌回流,得改性埃洛石纳米管;将改性埃洛石纳米管加入去离子水中,超声得悬浮液;将氧化石墨烯分散到去离子水中,超声得悬浮液;将悬浮液混合,离心分离、水洗,分散到去离子水中,加入水合肼,水浴中回流,离心分离,与前面所得物料混合研磨,得到电极材料。
2.一种电容器用埃洛石纳米管增强的电极材料的制备方法,其特征在于:
a. 金刚石粉的预处理:
将10-15重量份金刚石粉于90-100℃烘箱中干燥1-2h后,1:5-10加入无水乙醇中,超声搅拌均匀,加入0.5-1重量份KH550,于80-90℃回流3-4h,静置、过滤3-5次,放入100-110℃真空烘箱中干燥2-4h,研磨粉碎;
b. 氧化石墨烯的部分还原及修饰:
向5-10重量份氧化石墨烯中加入0.5-1重量份KH550,置于冰水浴中,用超声波细胞粉碎机超声剥离1-2h,分散均匀,加入0.5-1重量份催化剂,在70-80℃油浴下,磁力搅拌反应5-6h,过滤、醇洗3-5次,置于80-90℃鼓风烘箱中干燥完全、机械研磨粉碎;
然后1:5-10分散于丙酮中,超声振荡1-2h,加入6-9重量份凹凸棒土,继续超声处理1-2h,将混合液置于敞口容器中在70-80℃持续搅拌,蒸发掉溶剂丙酮,制得复合增强体;
c. 埃洛石纳米管的改性处理:
将10-15重量份埃洛石纳米管1:5-10加入pH为2-3的盐酸中,搅拌处理2-4h,离心分离,置于120-130℃真空烘箱中烘干;再加入20-30重量份无水甲苯,超声混合30-40min后,加入1-2重量份KH550,110-120℃下搅拌回流2-4h,离心分离,洗涤,在40-60℃的真空烘箱中烘干,得改性埃洛石纳米管;
d. 将c中所得改性埃洛石纳米管1:15-20加入去离子水中,超声1-2h得悬浮液A;将5-10重量份氧化石墨烯1:20-25分散到去离子水中,超声1-2h得悬浮液B;
将悬浮液A、B混合,边搅拌边缓慢加盐酸调pH为2-3,离心分离、水洗3-5次,1:5-10分散到去离子水中,加入1-2重量份水合肼,置于85-95℃水浴中回流2-3h,离心分离,用去离子水、乙醇各洗涤3-5次,产物于60-70℃真空烘箱中烘干,与a、b中所得物料混合研磨,得到电极材料。
3.根据权利要求2所述的一种电容器用埃洛石纳米管增强的电极材料的制备方法,其特征在于,步骤b中所述催化剂为N,N,-二环己基碳二亚胺。
4.根据权利要求2所述的一种电容器用埃洛石纳米管增强的电极材料的制备方法,其特征在于,步骤c中所述洗涤是用甲苯、乙醇各洗涤3-5次。
5.根据权利要求2所述的一种电容器用埃洛石纳米管增强的电极材料的制备方法,其特征在于,步骤d中所述盐酸浓度为5-10%,水合肼浓度为30-35%。
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