CN108788134A - 一种石墨烯-纳米锌铜合金核壳结构导电材料的制备方法 - Google Patents

一种石墨烯-纳米锌铜合金核壳结构导电材料的制备方法 Download PDF

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CN108788134A
CN108788134A CN201810569538.2A CN201810569538A CN108788134A CN 108788134 A CN108788134 A CN 108788134A CN 201810569538 A CN201810569538 A CN 201810569538A CN 108788134 A CN108788134 A CN 108788134A
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张燕萍
赵志国
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Shanghai Co Ltd Of Li Wusheng Enterprise Group
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Abstract

本发明公开了一种石墨烯‑纳米锌铜核壳结构导电薄膜材料的制备方法。该方法利用直流磁控溅射系统制备锌薄膜和铜薄膜，并先后经过高温退火处理，使得铜包覆锌并形成纳米合金颗粒。再采用等离子体增强化学气相沉积方法，将石墨烯生长并包覆于铜锌合金颗粒表面，形成核壳结构薄膜材料。该材料中石墨烯不仅有效地保护铜锌核不受空气氧化和腐蚀，还协同两者优异的导电性，结合集流体与导电膜于一体，可广泛应用于导电及电发热基材。

Description

一种石墨烯-纳米锌铜合金核壳结构导电材料的制备方法
技术领域
本发明涉及一种石墨烯-纳米锌铜核壳结构导电薄膜材料的制备方法，属于导电石墨烯基复合材料制备及应用技术领域。
背景技术
对于核壳结构纳米二元合金材料，常见的化学制备方法有：连续还原法和共还原法。该两种方法都涉及到液相化学还原，反应体系中众多因素，如温度、pH值、金属前驱体、还原剂、络合剂、杂质离子等，任何因素的变化都对产物造成一定程度影响，如粒子的平均尺寸、形貌、分散度等，工艺实施的可控性较差。此外，常见的物理制备方法有：共蒸发法。真空蒸发法生长样品时操作步骤复杂，设备也非常昂贵，不利于大规模工业化生产。
发明内容
本发明公开了一种石墨烯-纳米锌铜核壳结构导电薄膜材料的制备方法。该制备方法可调制石墨烯和纳米合金的结构及形貌，大幅改善电子在石墨烯中的传输具有方向差异性的缺点，可促进石墨烯协同纳米锌铜合金材料优异的导电性，形成巨大的技术潜力，对现有导电、存储、储能、催化、光学等领域技术将有很大提升。
本发明技术方案是这样实现的：
一种石墨烯-纳米锌铜合金核壳结构导电材料的制备方法，其特征在于：具体步骤如下：
步骤一、采用直流磁控溅射系统在衬底上制备锌薄膜；
步骤二、将锌薄膜进行高温退火处理，过程中锌薄膜形成球状锌颗粒；
步骤三、采用直流磁控溅射系统，在经退火处理的锌颗粒表面沉积铜薄膜；
步骤四、将附有铜薄膜的复合材料进行高温退火处理，过程中准液态的铜薄膜发生迁移，并包覆于纳米锌颗粒表面；
步骤五、采用等离子体增强化学气相沉积系统，在含衬底的纳米锌铜颗粒表面沉积石墨烯，并包覆于纳米锌铜颗粒表面，制备得到石墨烯-纳米锌铜核壳结构导电薄膜材料。
进一步的，步骤一中所述衬底为铜或铝或镍或铁或钛或锌中的一种或两种以上合金片材料的组合。
进一步的，步骤一中所制备的锌薄膜厚度为100nm-500nm。
进一步的，步骤二中所设定的退火温度为700-900℃，退火时间为10-60分钟，锌颗粒粒径为5-30nm。
进一步的，步骤三中所制备的铜薄膜厚度为400nm-1μm。
进一步的，步骤四中所设定的退火温度为700-900℃，退火时间为10-60分钟，所形成的纳米锌铜颗粒粒径为10-50nm。
进一步的，步骤五中所制备的石墨烯-纳米锌铜核壳结构导电薄膜材料粒径为60-100nm。
本发明的有益效果是：本发明公开的纳米合金材料制备方法采用物理合成，利用直流磁控溅射系统制备合金材料，能有效大幅提高其粒径和纯度的可控性。且相对于射频溅射，直流溅射气氛的离化率比较低，也就是化学反应活性较低，因此采用直流反应溅射时，所制备的纳米合金材料对溅射气氛的敏感性相对来说要低许多。而且，其制备工艺简单，能够对接产线，极大地降低了生产成本。
石墨烯是由单层碳原子紧密排列而成的二维原子晶体材料，具有优异的电学性能，其室温下的载流子迁移率可达15000cm2/(V·s)，在柔性电子器件、传感器、复合材料、储能、储氢等领域具有广泛的应用前景。纳米合金材料由于其粒径尺寸及结构不同于块状合金材料，因而在电学性能等方面表现出独特的性质。通过石墨烯包覆在纳米锌铜外部，调制了其沿着衬底呈现的平坦形貌，大幅改善了电子在石墨烯中的传输具有方向差异性的缺点，其电导率可达62.1MS/m，高于标准退火纯铜6.6％。此外，纳米合金通过结构的调控，可实现尺寸效应、表面效应及组分效应的组合，并产生广泛的新功能。本发明提供的制备技术，可促进石墨烯协同纳米锌铜合金材料优异的导电性，形成巨大的技术潜力，对现有导电、存储、储能、催化、光学等领域技术将有很大提升。
具体实施方式
以下结合实施例对本发明进行详细说明，但本实施例不能用于限制本发明，凡是采用本发明的相似方法及其相似变化，均应列入本发明的保护范围。
实施例1
采用直流磁控溅射系统在铜衬底上制备厚度为100nm锌薄膜，将锌薄膜进行700℃高温退火处理，退火时间为30分钟，锌颗粒粒径为30nm。继续采用直流磁控溅射系统，在经退火处理的锌颗粒表面沉积厚度为1μm铜薄膜，将附有铜薄膜的复合材料进行700℃高温退火处理，退火时间为10分钟过程中准液态的铜薄膜发生迁移，并包覆于纳米锌颗粒表面，所形成的纳米锌铜颗粒粒径为50nm。最后采用等离子体增强化学气相沉积系统，制备得到粒径为100nm石墨烯-纳米锌铜核壳材料。
实施例2
采用直流磁控溅射系统在铜铁镍合金衬底上制备厚度为500nm锌薄膜，将锌薄膜进行900℃高温退火处理，退火时间为60分钟，锌颗粒粒径为20nm。继续采用直流磁控溅射系统，在经退火处理的锌颗粒表面沉积厚度为800nm铜薄膜，将附有铜薄膜的复合材料进行900℃高温退火处理，退火时间为60分钟过程中准液态的铜薄膜发生迁移，并包覆于纳米锌颗粒表面，所形成的的纳米锌铜颗粒粒径为40nm。最后采用等离子体增强化学气相沉积系统，制备得到粒径为90nm石墨烯-纳米锌铜核壳材料。
实施例3
采用直流磁控溅射系统在铜铁镍合金衬底上制备厚度为300nm锌薄膜，将锌薄膜进行800℃高温退火处理，退火时间为30分钟，锌颗粒粒径为30nm。继续采用直流磁控溅射系统，在经退火处理的锌颗粒表面沉积厚度为900nm铜薄膜，将附有铜薄膜的复合材料进行800℃高温退火处理，退火时间为30分钟过程中准液态的铜薄膜发生迁移，并包覆于纳米锌颗粒表面，所形成的的纳米锌铜颗粒粒径为30nm。最后采用等离子体增强化学气相沉积系统，制备得到粒径为80nm石墨烯-纳米锌铜核壳材料。
实施例4
采用直流磁控溅射系统在钛铝合金衬底上制备厚度为150nm锌薄膜，将锌薄膜进行800℃高温退火处理，退火时间为15分钟，锌颗粒粒径为20nm。继续采用直流磁控溅射系统，在经退火处理的锌颗粒表面沉积厚度为300nm铜薄膜，将附有铜薄膜的复合材料进行800℃高温退火处理，退火时间为30分钟过程中准液态的铜薄膜发生迁移，并包覆于纳米锌颗粒表面，所形成的的纳米锌铜颗粒粒径为30nm。最后采用等离子体增强化学气相沉积系统，制备得到粒径为70nm石墨烯-纳米锌铜核壳材料。
实施例5
采用直流磁控溅射系统在铜铝合金衬底上制备厚度为200nm锌薄膜，将锌薄膜进行800℃高温退火处理，退火时间为30分钟，锌颗粒粒径为15nm。继续采用直流磁控溅射系统，在经退火处理的锌颗粒表面沉积厚度为500nm铜薄膜，将附有铜薄膜的复合材料进行800℃高温退火处理，退火时间为30分钟过程中准液态的铜薄膜发生迁移，并包覆于纳米锌颗粒表面，所形成的的纳米锌铜颗粒粒径为25nm。最后采用等离子体增强化学气相沉积系统，制备得到粒径为60nm石墨烯-纳米锌铜核壳材料。
下表为5个实施例所制备的石墨烯-纳米锌铜核壳材料采用四端法测试电性能的结果：
电阻率(10-8Ω·m) 电导率(MS/m)
标准退火纯铜 1.72 58
实施例1 1.70 58.8
实施例2 1.62 61.7
实施例3 1.67 59.9
实施例4 1.65 60.6
实施例5 1.61 62.1
从表中可以看出，实施例所制备的复合材料有着优异的电性能，其电导率与标准退火纯铜的电导率相比均有明显提升，其中实施例5在对比组中具有最优异的电性能，电导率提升了6.6％。将来可通过工艺优化提高材料的致密度、结晶性，有效降低材料内部产生的点缺陷，导电性能有望能进一步提升。

Claims (7)

1.一种石墨烯-纳米锌铜合金核壳结构导电材料的制备方法，其特征在于：具体步骤如下：
步骤一、采用直流磁控溅射系统在衬底上制备锌薄膜；
步骤二、将锌薄膜进行高温退火处理，过程中锌薄膜形成球状锌颗粒；
步骤三、采用直流磁控溅射系统，在经退火处理的锌颗粒表面沉积铜薄膜；
步骤四、将附有铜薄膜的复合材料进行高温退火处理，过程中准液态的铜薄膜发生迁移，并包覆于纳米锌颗粒表面；
步骤五、采用等离子体增强化学气相沉积系统，在含衬底的纳米锌铜颗粒表面沉积石墨烯，并包覆于纳米锌铜颗粒表面，制备得到石墨烯-纳米锌铜核壳结构导电薄膜材料。
2.根据权利要求1所述的一种石墨烯-纳米锌铜合金核壳结构导电材料的制备方法，其特征在于：步骤一中所述衬底为铜或铝或镍或铁或钛或锌中的一种或两种以上合金片材料的组合。
3.根据权利要求1所述的一种石墨烯-纳米锌铜合金核壳结构导电材料的制备方法，其特征在于：步骤一中所制备的锌薄膜厚度为100nm-500nm。
4.根据权利要求1所述的一种石墨烯-纳米锌铜合金核壳结构导电材料的制备方法，其特征在于：步骤二中所设定的退火温度为700-900℃，退火时间为10-60分钟，锌颗粒粒径为5-30nm。
5.根据权利要求1所述的一种石墨烯-纳米锌铜合金核壳结构导电材料的制备方法，其特征在于：步骤三中所制备的铜薄膜厚度为400nm-1μm。
6.根据权利要求1所述的一种石墨烯-纳米锌铜合金核壳结构导电材料的制备方法，其特征在于：步骤四中所设定的退火温度为700-900℃，退火时间为10-60分钟，所形成的纳米锌铜颗粒粒径为10-50nm。
7.根据权利要求1所述的一种石墨烯-纳米锌铜合金核壳结构导电材料的制备方法，其特征在于：步骤五中所制备的石墨烯-纳米锌铜核壳结构导电薄膜材料粒径为60-100nm。
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