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Preparation method of graphene

A graphene and graphite powder technology, applied in the field of graphene preparation, can solve the problems of complex process, difficult single-layer graphene, high production equipment, and high conditions, achieve low requirements for preparation conditions, no structural defects, and simple preparation process Effect

Inactive Publication Date: 2015-10-21
XIDIAN UNIV
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Problems solved by technology

[0004] The yield of the micromechanical exfoliation method is too low, which is only suitable for small-scale laboratory tests; the epitaxial growth method has high requirements for production equipment and conditions, and is not suitable for the current production requirements; it is difficult to obtain uniform single-layer graphene by chemical vapor deposition , and the process is complex; the reduced graphene obtained by the graphite oxide reduction method often has too many defects, which is fatal to the electrical properties of graphene

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Embodiment Construction

[0021] In order to make the technical means, creative features, goals and effects achieved by the present invention easy to understand, the present invention will be further described below in conjunction with specific illustrations.

[0022] Such as figure 1 所示,一种石墨烯的制备方法,利用含亲水基团的并苯稠环类芳烃衍生物作为插层试剂,且利用水及非水极性溶剂作为分散体系,分步超声波法制备石墨烯,包括以下步骤:

[0023] 步骤110中,将石墨粉加入到溶解有并苯稠环类芳烃衍生物的非水极性溶剂形成混合体系。取1mg至1000mg的石墨微粒(粒径在5μm至300μm之间)加入到溶解有1mg至500mg的并苯稠环类芳烃衍生物(如萘甲酸、萘甲醛、蒽甲酸、蒽甲醛、菲甲酸、菲甲醛、苊甲酸、苊甲醛、芴甲酸、芴甲醛、芘甲酸等)的10ml至1000ml非水极性溶剂中(如甲酰胺、乙腈、甲醇、乙醇、丙醇、乙酸、二恶烷、N-N二甲基甲酰胺等)。

[0024] 步骤120中,对所述混合体系进行震荡、洗涤、离心和过滤得到石墨烯溶液。

[0025] 上述过程,利用并苯稠环类芳烃衍生物其上的含稠环基团与石墨上π电子的相互作用,在非水极性溶剂中,以一定功率的超声波震荡,起到对石墨插层的效果;再加入极性很强的水做分散剂,利用超声波破坏石墨其上的化学键,此时并苯稠环类芳烃衍生物其上的亲水基团溶于水分散液,帮助石墨烯溶解,避免石墨烯堆积,得到石墨烯原始溶液。再多次利用超声波震荡、洗涤、离心的方法纯化石墨烯溶液,去除原始溶液中过量的并苯稠环类芳烃衍生物及未剥离的石墨,最终得到纯净的石墨烯溶液,产率约为1%。制备过程中可保证每一步均在常温常压下操作,无需加热,无强腐蚀性、剧毒性试剂,制备条件要求不高、制备工艺简单、所得石墨烯品质优良,几乎没有结构缺陷,且产率可观。

[0026] 在本实施例中,混合体系的震荡采用超声波震荡。

[0027] Such as figure 2 所示,在本实施例中,经过步骤110得...

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Abstract

Disclosed is a preparation method of grapheme. The preparation method of the grapheme comprises the following steps: graphite powder is added to non-water polar solvent dissolved with acene condensed nucleus arene derivative to form a mixed system; the mixed system is shocked, washed, centrifuged and filtered to obtain grapheme solution. The preparation method of the grapheme is not high in requirements for preparation conditions, simple in preparation process, good in quality of obtained grapheme, almost free of structural defects and considerable in productivity.

Description

Technical field: [0001] 本发明涉及一种碳元素的同素异形体,尤其涉及一种石墨烯的制备方法。 Background technique: [0002] 2004年Geim等人第一次从高取向热解石墨上剥离得到单原子层的纳米石墨片——石墨烯。石墨烯的出现给碳家族增添了新的成员,成为碳元素的第五种同素异形体。单层石墨烯是真正意义上的二维原子晶体,是目前世界上己知最薄的材料,20万片单层石墨烯的叠加厚度仅相当于一根头发丝的直径。石墨烯具有超高的机械强度、良好的导电导热性能以及独特的电学性质,因而具有广泛的应用前景。 [0003] 高质量石墨烯的大量生产是实现石墨烯广泛应用的前提,也一直是石墨烯研究的一个热点。目前常用的石墨烯制备方法有四种:微机械剥离法、外延生长法、化学气相沉积法和氧化石墨还原法。 [0004] 微机械剥离法产率过低,仅适用于实验室小型试验;外延生长法对于生产设备、条件均要求较高,不适应于现阶段生产要求;化学气相沉积法难于得到均匀的单层石墨烯,且工艺复杂;氧化石墨还原法得到的还原石墨烯往往有太多的缺陷,对于石墨烯的电学性质是致命的影响。 Invention content: [0005] 为了解决上述问题,本发明提供了一种产率可观、制备条件要求不高、制备工艺简单、所得产品性质优良的石墨烯生产工艺。 [0006] 一种石墨烯的制备方法,包括以下步骤: [0007] 将石墨粉加入到溶解有并苯稠环类芳烃衍生物的非水极性溶剂形成混合体系; [0008] 对所述混合体系进行震荡、洗涤、离心和过滤得到石墨烯溶液。 [0009] 在优选的实施例中,所述混合体系的震荡采用超声波震荡。 [0010] 在优选的实施例中,得到所述的混合体系后,步骤如下: [0011] 将所述混合体系以100~2500瓦的超声波震荡0.1~24小时,得到第一次震荡混合体系; [0012] 向所述第一次震荡混合体系中加入1~2000毫升的水,然后以100~2500瓦的震荡功率震荡1~200小时,得到第二次震荡混合体系; [0013] 将所述第二次震荡混合体系静置1~96小时,去除上层清液,并补水至原有体积,再用100~2500瓦的超声波震荡0.5~24小时,得第三次震荡混合体系。 [...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B31/04C01B32/184
Inventor 马中发庄弈琪肖郑操吴勇张鹏凌宇
Owner XIDIAN UNIV
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