CN106206682B - Pi膜制备的多层石墨烯量子碳基半导体材料及其制备方法 - Google Patents
Pi膜制备的多层石墨烯量子碳基半导体材料及其制备方法 Download PDFInfo
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Abstract
提供一种多层石墨烯量子碳基二维半导体材料及其制备方法,制备方法包括:S1.以PI膜为原料,在第一温度下进行高分子烧结,脱除H、O、N原子,形成碳素前驱体;S2.调整至第二温度,所述碳素前驱体进行石墨化,形成多层石墨烯量子碳基二维半导体材料;其中,至少在所述步骤S2中,进行纳米金属材料的掺杂,以在所述多层石墨烯中形成量子点。经该方法制备的多层石墨烯量子碳基二维半导体材料为六角平面网分子结构,且有序排列,具备柔性,曲折率大、面内分散度和偏差度非常小;通过纳米金属的掺杂形成带隙,且带隙可控;该制备方法能够大面积、低成本、大批量、卷到卷连续生产。
Description
技术领域
本发明涉及石墨烯半导体材料领域,特别涉及一种多层石墨烯量子碳基二维半导体材料的制备方法。
背景技术
二维纳米碳材料特别是石墨烯量子碳基半导体材料越来越受到人们关注,具有极其优异的电学、光学、磁学、热学和力学性能,是理想的纳米电子和光学电子材料。石墨烯量子碳基半导体材料具有特殊的几何结构,使得费米子面附近的电子态主要为扩展π态,由于没有表面悬挂键,表面纳米碳结构的缺陷,对扩展π态的散射几乎不影响电子在材料中的传输,常温下电子和空穴在多层石墨烯中的迁移率极高,均大于100000cm2·VS,超出最好硅基场效应晶体管的电子迁移率。1000cm2·VS的石墨烯可以通过控制其结构得到半导体性晶体管,在小偏电压的情况下,电子能量不足以激发石墨中的光学声子,但与石墨烯中的声学声子的相互作用又很弱,其平均自由程可长达数微米,使得载流子在典型的几百纳米长的石墨烯器件中呈现完美的弹道输运特征,基于石墨烯结构的电子器件可以有非常好的高频响应,对于弹道输运的晶体管中工作频率有望超过太赫兹(THz),性能优于所有硅基已知的的半导体材料。
石墨烯因其超薄结构以及优异的物理特性,在场效应晶体管(TET)应用上展现出了优异的性能和诱人的应用前景。但由于石墨烯带隙为零,意味着无法制作逻辑电路,成为石墨烯应用于晶体管等器件中的主要困难和挑战。从天然石墨矿中制备石墨烯采用外延生长法、氧化石墨还原法、CVD法剥离再嵌入扩涨法、有机合成法,据文献报道,采用上述方法能打开带隙仅为0.03eV,且面积小于1英寸根本无法进行工业化进程。
发明内容
为解决上述问题,本发明提供一种多层石墨烯量子碳基二维半导体材料的制备方法,形成带隙可控的柔性多层石墨烯量子碳基二维半导体材料,并且能够大面积、低成本、大批量、卷到卷连续生产。
本发明提供一种多层石墨烯量子碳基半导体材料的制备方法,包括如下步骤:S1.以聚酰亚胺薄膜(PI膜)为原料,在第一温度下进行高分子烧结,脱除H、O、N原子,形成微晶态的碳素前驱体;S2.调整至第二温度,所述碳素前驱体进行石墨化,形成多层石墨烯量子碳基二维半导体材料;其中,至少在所述步骤S2中,进行纳米金属材料的掺杂,以在所述多层石墨烯中形成量子点。
优选地,第一温度分为三段,脱除H原子的温度为900℃-1100℃,脱除O原子的温度为1800℃-2200℃,脱除N原子的温度为2700℃-3300℃。
进一步地优选,第一温度分为三段,脱除H原子的温度为1000℃,脱除O原子的温度为2000℃,脱除N原子的温度为3000℃。
优选地,第二温度为2000℃-3500℃。
进一步优选,第二温度分为两段,第一阶段温度为2000℃-2500℃,第二阶段温度为2500℃-3500℃。
优选地,掺杂的纳米金属材料包括钙(Ca)、锑(Sb)、铌(Nb)、钇(Y)、钼(Mo)、硅(Si)、砷(As)、铟(In)、铪(Hf)、镓(Ga)中的至少一种或至少两种的合金;纳米金属材料的粒径在2-5nm之间。
进一步地优选,掺杂的纳米金属材料为InAs,形成具有InAs量子点的多层石墨烯量子碳基二维半导体材料。
本发明还提供一种多层石墨烯量子碳基二维半导体材料,采用如上所述的制备方法制备得到。
本发明的有益效果包括:通过PI膜碳化和石墨化,制备具有六角平面网分子结构且有序排列的柔性石墨烯形态结构,该结构曲率大、面内分散和偏差度非常小。通过纳米金属材料的掺杂,形成量子点,实现带隙的开启与调控。该制备方法还能满足大面积、低成本、大批量、卷到卷连续生产。
通过该方法制备的多层石墨烯量子碳基二维半导体材料,能够应用于制备高性能场效应晶体管、量子计算芯片半导体等材料。
具体实施方式
以下对本发明的实施方式作详细说明。应该强调的是,下述说明仅仅是示例性的,而不是为了限制本发明的范围及其应用。
在一种实施例中,一种多层石墨烯量子碳基二维半导体材料的制备方法,包括如下步骤:S1.以PI膜为原料,在第一温度下进行高分子烧结,脱除H、O、N原子,形成微晶态的碳素前驱体;S2.调整至第二温度,所述碳素前驱体进行石墨化,形成多层石墨烯量子碳基二维半导体材料;其中,至少在所述步骤S2中,进行纳米金属材料的掺杂,以在所述多层石墨烯中形成量子点。
在优选的实施例中,PI膜采用的是现有技术CN103289402A中制备的新型透明聚酰亚胺薄膜。该PI膜通过芳香族二元胺和芳香族多酸酐进行相互杂化,并导入甲基制得聚酰亚胺,再进行环化脱水、缩聚、酰亚胺化得到。该薄膜取向性优良,并有着双折射高的特性,在碳化、石墨化时面向的厚度膨胀变小,面方向长度变化量也小,因此趋向性紊乱减少,线取向性提高,强度也提高,不易产生破裂,可以任意加热、加压而无破损。
PI膜经高分子烧结碳化,脱除H、O、N原子,使高分子热处理接近于单结晶石墨的温度,C原子得到重新排列,形成连续区大的芳杂环化合物微晶态,最终形成具有优良人造异源石墨结构的微晶态碳素前驱体,该碳素前躯体实现平面特性。碳素前躯体经石墨化,碳结构重组,微晶态边缘的碳原子经高温加速加剧运动,微晶态互相键合生成大分子,开始六角网眼构造结合并进行结晶配向,六角碳网层面形成并逐渐生长,从一轴转变为二轴,生成曲折率大、面内分散度和偏差度非常小,并可以弯曲的柔性石墨烯形态结构。
在优选的实施例中,高分子烧结碳化,脱除H原子的温度为900℃-1100℃,脱除O原子的温度为1800℃-2200℃,脱除N原子的温度为2700℃-3300℃。
在另一优选的实施例中,高分子烧结碳化,脱除H原子的温度为1000℃,脱除O原子的温度为2000℃,脱除N原子的温度为3000℃。
在优选的实施例中,进行石墨化的温度为2000℃-3500℃。
在另一优选的实施例中,进行石墨化分两阶段,第一阶段反应温度为2000℃-2500℃,第二阶段反应温度为2500℃-3500℃。
在进一步优选的实施例中,石墨化是在1.4×10-8-1.8×10-8mm Hg,更优的是在1.6×10-8mm Hg下进行。
PI膜经碳化和石墨化后组成的晶体结构最高峰G峰位于1582.6cm-1右侧;次高峰为2D双峰结构,位于2719.8cm-1;G峰右侧的D峰1363cm-1很小,结构缺陷少。多层石墨烯形态是二维结晶,其中,原子遵循六角形构造的规则有秩序进行配置的平面状六角形格子形态,各碳素原子是3个碳原子接合起来,化学结合中4个外壳电子中有一个电子是自由移动的状态,自由电子可以沿结晶格子移动,因此,石墨烯在面方向具有很高的导电率。
在碳化和石墨化的过程中,同时掺杂纳米金属材料,形成量子点,制备二维多层石墨烯量子碳基,实现石墨烯带隙的开启与调控。纳米过渡性金属与石墨烯以共价键连接,电子云重叠时,具有共轭体系(离域π键),两个原子之间共用电子对数,电子越过纳米势垒,形成费米电子海,电子从一个量子阱穿越量子势垒进入另一个量子阱,形成量子隧道效应,结构效应,量子限域效应。
在优选的实施例中,掺杂的纳米金属材料包括Ca、Sb、Nb、Y、Mo、Si、As、In、Hf、Ga中的至少一种或至少两种的合金。
在另一优选的实施例中,掺杂的纳米金属材料为InAs,形成的具有InAs量子点的多层石墨烯量子碳基二维半导体材料。
实施例1
在惰性气体中,PI膜经高分子烧结碳化,分别在1000℃、2000℃和3000℃,脱除H、O、N原子,C原子重排,形成碳素前驱体;碳素前驱体在惰性气体保护下,在2800℃进行石墨化,开始六角网眼构造,生成高纯度单晶石墨烯构造,二维碳层为六方密堆积,具有平面网状分子有序排列。在碳化和石墨化过程中,掺杂InAs纳米金属材料,形成量子点,制得多层石墨烯量子碳基二维半导体材料,量子点密度为1×1010~3×1010cm-2,带隙宽度为1.3-1.4ev。
实施例2
与实施例1的区别在于,掺杂的纳米金属材料为InAs和Sb的混合物,形成的量子点密度为1.2×1012cm-2。通过量子隧道效应,调控在InAs中加入Sb元素,形成InSbxAs1-x量子点,调整含量x时,可调控带隙宽度。
对比实施例1
与实施例一或实施例二的区别在于:PI膜经高分子烧结碳化,分别在500℃、600℃和800℃进行H、O、N原子的脱除,无法形成多层石墨烯量子碳基二维半导体材料。
以上内容是结合具体/优选的实施方式对本发明所作的进一步详细说明,不能认定本发明的具体实施只局限于这些说明。对于本发明所属技术领域的普通技术人员来说,在不脱离本发明构思的前提下,其还可以对这些已描述的实施方式做出若干替代或变型,而这些替代或变型方式都应当视为属于本发明的保护范围。
Claims (9)
1.一种多层石墨烯量子碳基二维半导体材料的制备方法,其特征在于,包括如下步骤:
S1.以PI膜为原料,在第一温度下进行高分子烧结,脱除H、O、N原子,形成微晶态的碳素前驱体;所述PI是膜通过芳香族二元胺和芳香族多酸酐进行相互杂化,并导入甲基制得聚酰亚胺,再进行环化脱水、缩聚、酰亚胺化得到的;所述PI膜经所述高分子烧结后碳化,形成连续区大的芳杂环化合物微晶态,最终形成具有优良人造异源石墨结构的微晶态碳素前驱体;
S2.调整至第二温度,所述碳素前驱体进行石墨化,形成多层石墨烯量子碳基二维半导体材料;经所述石墨化后,生成可以弯曲的柔性石墨烯形态结构;其中,至少在所述步骤S2中,进行纳米金属材料的掺杂,以在所述多层石墨烯中形成量子点。
2.如权利要求1所述的制备方法,其特征在于,所述第一温度分为三段,脱除H原子的温度为900℃-1100℃,脱除O原子的温度为1800℃-2200℃,脱除N原子的温度为2700℃-3300℃。
3.如权利要求2所述的制备方法,其特征在于,所述第一温度分为三段,脱除H原子的温度为1000℃,脱除O原子的温度为2000℃,脱除N原子的温度为3000℃。
4.如权利要求1所述的制备方法,其特征在于,所述第二温度为2000℃-3500℃。
5.如权利要求4所述的制备方法,其特征在于,所述第二温度分为两段,第一阶段温度为2000℃-2500℃,第二阶段温度为2500℃-3500℃。
6.如权利要求1所述的制备方法,其特征在于,所述纳米金属材料包括:Ca、Sb、Nb、Y、Mo、As、In、Hf、Ga中的至少一种或至少两种的合金;纳米金属材料的粒径在2-5nm之间。
7.如权利要求6所述的制备方法,其特征在于,所述纳米金属材料为InAs,形成的具有InAs量子点的多层石墨烯量子碳基二维半导体材料。
8.如权利要求1所述的制备方法,其特征在于,所述多层石墨烯量子碳基二维半导体材料的层数为2-50层。
9.一种多层石墨烯量子碳基二维半导体材料,其特征在于,通过权利要求1-8任一所述的制备方法制备得到。
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