CN109056306A - 一种NiO/Ni复合石墨烯包覆棉碳纤维材料的制备方法 - Google Patents

一种NiO/Ni复合石墨烯包覆棉碳纤维材料的制备方法 Download PDF

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CN109056306A
CN109056306A CN201811058941.5A CN201811058941A CN109056306A CN 109056306 A CN109056306 A CN 109056306A CN 201811058941 A CN201811058941 A CN 201811058941A CN 109056306 A CN109056306 A CN 109056306A
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张学谦
王依山
温广武
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Shandong University of Technology
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Abstract

本发明公开了一种NiO/Ni复合石墨烯包覆棉碳纤维材料的制备方法，包括以下步骤：（1）将无纺棉浸入氧化石墨(GO)溶液中进行超声处理；（2）冷冻后进行冷冻干燥处理，得到氧化石墨烯包覆无纺棉纤维；（3）氯化镍溶于无水乙醇溶液中，将氧化石墨烯包覆无纺棉纤维浸入上述溶液，取出后放入干燥箱中烘干；（4）放入炉中，通入保护气体，600℃～1100℃保温1～10 h；（5）停止加热，继续通入保护气体，待炉温降低至室温，取出样品，即得NiO/Ni复合石墨烯包覆棉碳纤维材料。

Description

一种NiO/Ni复合石墨烯包覆棉碳纤维材料的制备方法
技术领域
本发明涉及材料技术领域，尤其涉及的是一种NiO/Ni复合石墨烯包覆棉碳纤维材料的制备方法。
背景技术
过渡金属氧化物材料中，NiO是一种广泛应用的无机材料，具有廉价和无毒的特点，并且是一种具有前途的功能化材料，因而在陶瓷、热敏原件、催化剂、磁性材料和能源存储等领域具有广泛的应用。
与其它金属氧化物相似，单纯利用NiO作为基本材料，由于材料电导性较低，因此NiO的稳定性较差。相比与金属氧化物，金属Ni的电导性较高，金属Ni和NiO由于都含有Ni元素，因此NiO与Ni复合可以提高材料整体的电导率并且具有较好的结合性。
作为一种独特的二维单原子晶体材料，石墨烯具有优异的机械性能、较高的热导率和载流子迁移率、超宽带的光学响应谱、较大的结构稳定性和表面积，因此石墨烯适合搭载金属氧化物制备复合材料。
碳化纤维作为碳材料，具有较高的电导率和力学性能，同时碳化纤维具有大量的孔隙，可以释放材料在使用过程中产生的应力，增强材料结构稳定性。在众多碳化纤维中，利用棉纤维经过碳化制备的棉碳纤维具有成本低的特点。因此利用NiO/Ni与石墨烯和棉碳纤维进行复合，可以制备出具有优异性能的复合材料，满足一些高性能领域的需求。
因此，研究一种操作简单，工艺要求不苛刻，可实现高质量、大规模制备NiO/Ni复合石墨烯与棉碳纤维材料，具有重要的研究价值和科研意义。
发明内容
本发明的技术目的是针对上述NiO/Ni复合石墨烯与棉碳纤维材料制备技术的现状，提供了一种工艺简单的NiO/Ni复合石墨烯包覆棉碳纤维新型结构材料的方法。
本发明技术方案如下：
一种NiO/Ni复合石墨烯包覆棉碳纤维材料的制备方法，包括以下步骤：
(1) 将无纺棉浸入氧化石墨(GO)溶液中，超声处理；
(2) 冷冻后进行冷冻干燥处理，得到氧化石墨烯包覆无纺棉纤维；
(3) 氯化镍溶于无水乙醇溶液中，将氧化石墨烯包覆无纺棉纤维浸入上述溶液，取出后放入干燥箱中烘干；
(4) 放入炉中，通入保护气体，600℃～1100 ℃保温1～10 h；
(5) 停止加热，继续通入保护气体，待炉温降低至室温，取出样品，即得NiO/Ni复合石墨烯包覆棉碳纤维材料。
所述的制备方法，所述无纺棉为天然棉花制成的无纺棉。
所述的制备方法，所述步骤(1)中GO浓度为0.5~15 mg/ml。
所述的制备方法，所述步骤(1)中GO为Hummers法制备的GO。
所述的制备方法，所述步骤(1)中GO溶液为前期经过超声处理1~2 h的GO溶液。
所述的制备方法，所述步骤(1)中超声处理时间为0.5~2 h。
所述的制备方法，所述步骤(2)中冷冻处理可以为低温冰箱冷冻或液氮冷冻，温度低于-30 ℃。
所述的制备方法，所述步骤(3)中氯化镍无水乙醇溶液的密度为5~30 mg/ml。
所述的制备方法，所述步骤(4)和(5)中保护气体为氮气或氩气。
附图说明
图1是本发明实施例1中NiO/Ni复合石墨烯包覆棉碳纤维材料XRD图片。
图2是本发明实施例1中NiO/Ni复合石墨烯包覆棉碳纤维材料SEM图片。
具体实施方法
以下结合附图与实施例对本发明作进一步详细描述，需要指出的是，以下所述实施例旨在便于对本发明的理解，而对其不起任何限定作用。
实施例1：
本实施例中提供一种NiO/Ni复合石墨烯包覆棉碳纤维材料的制备方法，具体制备方法如下。
（1）将无纺棉浸入7 mg/ml的GO溶液中，超声0.5h，其中无纺棉为天然棉花制备的无纺棉，GO为Hummers法制备的GO，GO溶液为前期经过超声处理1 h的GO溶液。
（2）放入低温冰箱冷冻24 h，放入冷冻干燥机冷冻干燥48 h，得到氧化石墨烯包覆无纺棉纤维，其中低温冰箱温度为-35 ℃。
（3）制备10 mg/ml的氯化镍的无水乙醇溶液中，将氧化石墨烯包覆无纺棉纤维浸入上述溶液，浸泡24 h，取出后放入干燥箱中烘干。
（4）放入陶瓷坩埚中，放入通入氮气的保护气体的炉中，10 ℃/min升温至600 ℃，保温1 h。
（5）停止加热，继续通入氩气，待炉温降低至室温，取出样品，得到NiO/Ni复合石墨烯包覆棉碳纤维材料。
图1是上述NiO/Ni复合石墨烯包覆天然棉花纤维结构材料XRD图片。从图中可以看出：出现多个NiO和Ni峰位，同时还出现了石墨(Graphite)的峰位，石墨的峰位反应石墨烯包覆棉碳纤维，说明成功合成出NiO/Ni复合石墨烯包覆棉碳纤维材料。
图2是上述NiO/Ni复合石墨烯包覆棉碳纤维材料SEM图。从图中可以看出，石墨烯包覆着棉碳纤维，还有部分石墨烯分布在棉碳纤维周围，没有发现NiO和Ni颗粒，说明NiO/Ni以纳米形式存在，不易观察到。
实施例2：
本实施例中提供一种NiO/Ni复合石墨烯包覆棉碳纤维材料的制备方法，具体制备方法如下。
（1）将无纺棉浸入5 mg/ml的GO溶液中，超声0.5h，其中无纺棉为天然棉花制备的无纺棉，GO为Hummers法制备的GO，GO溶液为前期经过超声处理1 h的GO溶液。
（2）放入低温冰箱冷冻24 h，放入冷冻干燥机冷冻干燥48 h，得到氧化石墨烯包覆无纺棉纤维，其中低温冰箱温度为-35 ℃。
（3）制备10 mg/ml的氯化镍的无水乙醇溶液中，将氧化石墨烯包覆无纺棉纤维浸入上述溶液，浸泡24 h，取出后放入干燥箱中烘干。
（4）放入陶瓷坩埚中，放入通入氩气的保护气体的炉中，10 ℃/min升温至700 ℃，保温1 h。
（5）停止加热，继续通入氩气，待炉温降低至室温，取出样品，得到NiO/Ni复合石墨烯包覆棉碳纤维材料。
实施例3：
本实施例中提供一种NiO/Ni复合石墨烯包覆棉碳纤维材料的制备方法，具体制备方法如下。
（1）将无纺棉浸入7 mg/ml的GO溶液中，超声0.5h，其中无纺棉为天然棉花制备的无纺棉，GO为Hummers法制备的GO，GO溶液为前期经过超声处理1 h的GO溶液。
（2）放入低温冰箱冷冻24 h，放入冷冻干燥机冷冻干燥48 h，得到氧化石墨烯包覆无纺棉纤维，其中低温冰箱温度为-35 ℃。
（3）制备20 mg/ml的氯化镍的无水乙醇溶液中，将氧化石墨烯包覆无纺棉纤维浸入上述溶液，浸泡24 h，取出后放入干燥箱中烘干。
（4）放入陶瓷坩埚中，放入通入氮气的保护气体的炉中，10 ℃/min升温至700 ℃，保温5 h。
（5）停止加热，继续通入氮气，待炉温降低至室温，取出样品，得到NiO/Ni复合石墨烯包覆棉碳纤维材料。
实施例4：
本实施例中提供一种NiO/Ni复合石墨烯包覆棉碳纤维材料的制备方法，具体制备方法如下。
（1）将无纺棉浸入3 mg/ml的GO溶液中，超声0.5 h，其中无纺棉为天然棉花制备的无纺棉，GO为Hummers法制备的GO，GO溶液为前期经过超声处理1 h的GO溶液。
（2）放入低温冰箱冷冻24 h，放入冷冻干燥机冷冻干燥48 h，得到氧化石墨烯包覆无纺棉纤维，其中低温冰箱温度为-40 ℃。
（3）制备20 mg/ml的氯化镍的无水乙醇溶液中，将氧化石墨烯包覆无纺棉纤维浸入上述溶液，浸泡24 h，取出后放入干燥箱中烘干。
（4）放入陶瓷坩埚，放入通入氮气的保护气体的炉中，10 ℃/min升温至1000 ℃，保温1 h。
（5）停止加热，继续通入氮气，待炉温降低至室温，取出样品，得到NiO/Ni复合石墨烯包覆棉碳纤维材料。
实施例5：
本实施例中提供一种NiO/Ni复合石墨烯包覆棉碳纤维材料的制备方法，具体制备方法如下。
（1）将无纺棉浸入7 mg/ml的GO溶液中，超声1 h，其中无纺棉为天然棉花制备的无纺棉，GO为Hummers法制备的GO，GO溶液为前期经过超声处理2 h的GO溶液。
（2）放入低温冰箱冷冻30 h，放入冷冻干燥机冷冻干燥48 h，得到氧化石墨烯包覆无纺棉纤维，其中低温冰箱温度为-35 ℃。
（3）制备20 mg/ml的氯化镍的无水乙醇溶液中，将氧化石墨烯包覆无纺棉纤维浸入上述溶液，浸泡24 h，取出后放入干燥箱中烘干。
（4）放入陶瓷坩埚，放入通入氩气的保护气体的炉中，10 ℃/min升温至700 ℃，保温1 h。
（5）停止加热，继续通入氩气，待炉温降低至室温，取出样品，得到NiO/Ni复合石墨烯包覆棉碳纤维材料。
以上所述的实施例对本发明的技术方案进行了详细说明，应理解的是以上所述仅为本发明的具体实施例，并不用于限制本发明，凡在本发明的原则范围内所做的任何修改、补充或类似方式替代等，均应包含在本发明的保护范围之内。

Claims (9)

1.一种NiO/Ni复合石墨烯包覆棉碳纤维材料的制备方法，包括以下步骤：
（1）将无纺棉浸入氧化石墨(GO)溶液中进行超声处理；
（2）冷冻后进行冷冻干燥处理，得到氧化石墨烯包覆无纺棉纤维；
（3）氯化镍溶于无水乙醇溶液中，将氧化石墨烯包覆无纺棉纤维浸入上述溶液，取出后放入干燥箱中烘干；
（4）放入炉中，通入保护气体，600℃～1100 ℃保温1～10 h；
（5）停止加热，继续通入保护气体，待炉温降低至室温，取出样品，即得NiO/Ni复合石墨烯包覆棉碳纤维材料。
2.根据权利要求1所述的制备方法，其特征在于，所述无纺棉为天然棉花制成的无纺棉。
3.根据权利要求1所述的制备方法，其特征在于，所述步骤（1）中GO浓度为0.5~15 mg/ml。
4.根据权利要求1所述的制备方法，其特征在于，所述步骤（1）中GO为Hummers法制备的GO。
5.根据权利要求1所述的制备方法，其特征在于，所述步骤（1）中GO溶液为前期经过超声处理1~2 h的GO溶液。
6.根据权利要求1所述的制备方法，其特征在于，所述步骤（1）中超声处理时间为0.5~2h。
7.根据权利要求1所述的制备方法，其特征在于，所述步骤（2）中冷冻需要在低温冰箱或液氮中进行冷冻，温度低于-30 ℃。
8.根据权利要求1所述的制备方法，其特征在于，所述步骤（3）中氯化镍无水乙醇溶液的浓度为5~30 mg/ml。
9.根据权利要求1所述的制备方法，其特征在于，所述步骤(4)和(5)中保护气体为氮气或氩气。
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