CN108570726A - 一种SnO2/CuO复合石墨烯包覆棉碳纤维材料的制备方法 - Google Patents
一种SnO2/CuO复合石墨烯包覆棉碳纤维材料的制备方法 Download PDFInfo
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- 229920000742 Cotton Polymers 0.000 title claims abstract description 64
- 239000000463 material Substances 0.000 title claims abstract description 45
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 title claims abstract description 41
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 37
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 28
- 239000000835 fiber Substances 0.000 title claims abstract description 27
- 239000002131 composite material Substances 0.000 title claims abstract description 26
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 22
- 239000010439 graphite Substances 0.000 title claims abstract description 22
- -1 graphite alkene Chemical class 0.000 title claims abstract description 21
- TXUICONDJPYNPY-UHFFFAOYSA-N (1,10,13-trimethyl-3-oxo-4,5,6,7,8,9,11,12,14,15,16,17-dodecahydrocyclopenta[a]phenanthren-17-yl) heptanoate Chemical compound C1CC2CC(=O)C=C(C)C2(C)C2C1C1CCC(OC(=O)CCCCCC)C1(C)CC2 TXUICONDJPYNPY-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims abstract description 19
- 235000011150 stannous chloride Nutrition 0.000 claims abstract description 19
- 239000001119 stannous chloride Substances 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 17
- 230000001681 protective effect Effects 0.000 claims abstract description 14
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000005253 cladding Methods 0.000 claims abstract description 6
- 238000007710 freezing Methods 0.000 claims abstract description 6
- 230000008014 freezing Effects 0.000 claims abstract description 6
- 238000004321 preservation Methods 0.000 claims abstract description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 28
- 229910052757 nitrogen Inorganic materials 0.000 claims description 14
- 239000007789 gas Substances 0.000 claims description 11
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- 230000033116 oxidation-reduction process Effects 0.000 claims description 7
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 2
- 238000000527 sonication Methods 0.000 claims description 2
- 238000002604 ultrasonography Methods 0.000 claims 1
- 238000004108 freeze drying Methods 0.000 abstract description 7
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 29
- 238000001035 drying Methods 0.000 description 12
- BBGVVPLPLBJJLS-UHFFFAOYSA-N copper ethanol dinitrate Chemical compound C(C)O.[N+](=O)([O-])[O-].[Cu+2].[N+](=O)([O-])[O-] BBGVVPLPLBJJLS-UHFFFAOYSA-N 0.000 description 7
- 150000001336 alkenes Chemical class 0.000 description 6
- 239000000919 ceramic Substances 0.000 description 6
- 238000007654 immersion Methods 0.000 description 6
- 238000010792 warming Methods 0.000 description 6
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 229910001416 lithium ion Inorganic materials 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229910044991 metal oxide Inorganic materials 0.000 description 3
- 150000004706 metal oxides Chemical class 0.000 description 3
- 229920000049 Carbon (fiber) Polymers 0.000 description 2
- 239000005751 Copper oxide Substances 0.000 description 2
- 239000004917 carbon fiber Substances 0.000 description 2
- 229910000431 copper oxide Inorganic materials 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000010405 anode material Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000007770 graphite material Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
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Abstract
本发明公开了一种SnO2/CuO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0.5~10 mg/mL的氧化石墨烯(GO)溶液中；（2）放入冰箱中冷冻24‑48 h，之后进行冷冻干燥处理，得到GO包覆天然棉花纤维；（3）氯化亚锡和硝酸铜溶于无水乙醇溶液中，将氧化石墨烯包覆无纺棉纤维浸入溶液中；（4）材料放入管式炉中，通入保护气体，300℃～1400℃保温1～10h；（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SnO2/CuO复合石墨烯包覆棉碳纤维材料。
Description
技术领域
本发明涉及材料技术领域，尤其涉及的是一种SnO2/CuO复合石墨烯包覆棉碳纤维材料的制备方法。
背景技术
随着环境污染和能源危机的日益严重，新能源的开发与新能源的存储受到人们的广泛关注，在众多能源存储设备中，锂离子电池由于其高能量密度、高功率密度、使用寿命长和无记忆效应等特性，成为各国研究的热点。
锂离子电池由四部分组成：正极、负极、电解液和隔膜。在这四部分之中，负极材料的性能影响电池整体性能。目前，商业化最广泛应用的负极材料为石墨材料，然而石墨由于其理论比容量较低，无法满足新型电子器件对电池高能量密度的需求，因此需要开发和寻找新型负极材料来满足新型电子器件的需求。金属氧化物具有理论比容量高、资源广泛和生产工艺简单的优势，近些年来作为负极材料受到科研人员的广泛研究。其中SnO2和CuO由于比容量高，材料电势低的优点，得到了多家科研机构的关注。利用SnO2与CuO进行复合，可以更加有效发挥两种电极材料的优势，提高材料比容量。但作为金属氧化物，SnO2和CuO在充放电循环的过程中，由于材料体积膨胀和电导率较低的缺陷，会产生粒子聚集和材料失效的问题。通过将金属氧化物与碳材料进行有效复合，可以提高材料的整体电导率，提升循环稳定性。碳化纤维具有相互搭接的三维网状结构，这种结构有利于电解液和电子的传输。石墨烯作为近些年发现的新型碳材料，具有高的电导率和稳定性的优点。因此利用SnO2/CuO与碳化纤维和石墨烯进行有效复合，可以得到性能优异的锂离子电池负极材料。
发明内容
本发明的技术目的是针对上述锂离子电池负极材料制备技术的现状，提供了一种工艺简单的SnO2/CuO复合石墨烯包覆棉碳纤维材料的制备方法。
本发明技术方案如下：
一种SnO2/CuO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) 将天然棉花浸入氧化石墨烯(GO)溶液中，超声处理；
(2) 之后冷冻处理，再进行冷冻干燥，得到氧化石墨烯包覆棉纤维；
(3) 氯化亚锡和硝酸铜溶于无水乙醇溶液中，将氧化石墨烯包覆棉纤维浸入溶液中；
(4) 材料放入炉中，通入保护气体，300℃～1500℃保温1～10h；
(5) 停止加热，继续通入保护气体，待炉温降低至室温，得到SnO2/CuO复合石墨烯包覆棉碳纤维材料，取出样品。
所述的制备方法，所述天然棉花纤维为天然棉花或由天然棉花制成的无纺棉。
所述的制备方法，步骤(1)中GO浓度为0.5 mg/ml~15 mg/ml；
所述的制备方法，步骤(1)中GO为氧化还原法制备的GO；
所述的制备方法，步骤(1)中GO溶液前期需要超声处理1~2h。
所述的制备方法，步骤(1)中超声处理时间为0.5~2 h；
所述的制备方法，步骤(2)中冷冻处理可以为低温冰箱冷冻或液氮冷冻；
所述的制备方法，步骤(3)中氯化亚锡与硝酸铜无水乙醇溶液的密度为5 mg/mL~100mg/ml；
所述的制备方法，步骤(3)中氯化亚锡与硝酸铜的摩尔比为20:1~1:10；
所述的制备方法，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实施后SnO2/CuO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实施后SnO2/CuO复合石墨烯包覆棉碳纤维材料SEM图片。
具体实施方式
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SnO2/CuO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）将天然棉花制成的无纺棉浸入4 mg/ml的GO溶液中，超声0.5h，GO为氧化还原法制备的GO，GO溶液前期经过1 h超声处理。
（2）将浸泡过GO溶液的棉花放入低温冰箱冷冻24 h，放入冷冻干燥机冷冻干燥48h。
（3）将干燥后的浸泡过GO的棉花浸入40 mg/ml的氯化亚锡和硝酸铜无水乙醇溶液中，氯化亚锡与硝酸铜的摩尔比为5:1，浸泡24 h，之后放入干燥箱中干燥12 h。
（4）将材料放入陶瓷坩埚，放入通入氮气的保护气氛的炉中，10 ℃/min升温至600℃，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SnO2/CuO复合石墨烯包覆棉碳纤维材料。
图1是上述SnO2/CuO复合石墨烯包覆棉碳纤维材料XRD图片。从图中可以看出：出现很多二氧化锡和氧化铜峰位，说明成功合成了二氧化锡和氧化铜。
图2是上述SnO2/CuO复合石墨烯包覆棉碳纤维材料SEM图。从图中可以看出，石墨烯包裹于棉碳纤维，还有部分石墨烯分布在棉花纤维周围，没有看见SnO2和CuO颗粒，说明SnO2和CuO以很小的纳米粒子形式存在。
实施例2：
本实施例中提供一种SnO2/CuO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）将天然棉花浸入7 mg/ml的GO溶液中，超声0.5h，GO为氧化还原法制备的GO，GO溶液前期经过1 h超声处理。
（2）将浸泡过GO溶液的棉花放入低温冰箱冷冻24 h，放入冷冻干燥机冷冻干燥48h。
（3）将干燥后的浸泡过GO的棉花浸入40 mg/ml的氯化亚锡与硝酸铜无水乙醇溶液中，氯化亚锡与硝酸铜的摩尔比为5:1，浸泡24 h，之后放入干燥箱中干燥12 h，得到复合物。
（4）将材料放入陶瓷坩埚，放入通入氮气的保护气氛的炉中，10 ℃/min升温至600℃，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SnO2/CuO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SnO2/CuO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）将天然棉花浸入7 mg/ml的GO溶液中，超声0.5h，GO为氧化还原法制备的GO，GO溶液前期经过1 h超声处理。
（2）将浸泡过GO溶液的棉花放入低温冰箱冷冻24 h，放入冷冻干燥机冷冻干燥48h。
（3）将干燥后的浸泡过GO的棉花浸入70 mg/ml的氯化亚锡和硝酸铜无水乙醇溶液中，氯化亚锡与硝酸铜摩尔比5:1，为浸泡24 h，之后放入干燥箱中干燥12 h。
（4）将材料放入陶瓷坩埚，放入通入氮气的保护气氛的炉中，10 ℃/min升温至600℃，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SnO2/CuO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SnO2/CuO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）将天然棉花浸入7 mg/ml的GO溶液中，超声0.5h，GO为氧化还原法制备的GO，GO溶液前期经过1 h超声处理。
（2）将浸泡过GO溶液的棉花放入低温冰箱冷冻24 h，放入冷冻干燥机冷冻干燥48h。
（3）将干燥后的浸泡过GO的棉花浸入70 mg/ml的氯化亚锡和硝酸铜无水乙醇溶液中，氯化亚锡与硝酸铜摩尔比1:2，为浸泡24 h，之后放入干燥箱中干燥12 h。
（4）将材料放入陶瓷坩埚，放入通入氮气的保护气氛的炉中，10 ℃/min升温至600℃，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SnO2/CuO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SnO2/CuO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）将天然棉花浸入7 mg/ml的GO溶液中，超声0.5h，GO为氧化还原法制备的GO，GO溶液前期经过1 h超声处理。
（2）将浸泡过GO溶液的棉花放入低温冰箱冷冻24 h，放入冷冻干燥机冷冻干燥48h。
（3）将干燥后的浸泡过GO的棉花浸入70 mg/ml的氯化亚锡和硝酸铜无水乙醇溶液中，氯化亚锡与硝酸铜摩尔比1:2，为浸泡24 h，之后放入干燥箱中干燥12 h。
（4）将材料放入陶瓷坩埚，放入通入氮气的保护气氛的炉中，10 ℃/min升温至800℃，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SnO2/CuO复合石墨烯包覆棉碳纤维材料。
实施例6：
本实施例中提供一种SnO2/CuO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）将天然棉花浸入7 mg/ml的GO溶液中，超声0.5h，GO为氧化还原法制备的GO，GO溶液前期经过1 h超声处理。
（2）将浸泡过GO溶液的棉花放入低温冰箱冷冻24 h，放入冷冻干燥机冷冻干燥48h。
（3）将干燥后的浸泡过GO的棉花浸入70 mg/ml的氯化亚锡和硝酸铜无水乙醇溶液中，氯化亚锡与硝酸铜摩尔比1:2，为浸泡24 h，之后放入干燥箱中干燥12 h。
（4）将材料放入陶瓷坩埚，放入通入氩气的保护气氛的炉中，10 ℃/min升温至800℃，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SnO2/CuO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 (10)
1.一种SnO2/CuO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) 将天然棉花浸入氧化石墨烯(GO)溶液中；
(2) 之后冷冻干燥，得到氧化石墨烯包覆棉纤维；
(3) 氯化亚锡和硝酸铜溶于无水乙醇溶液中，将氧化石墨烯包覆棉纤维浸入溶液中；
(4) 放入炉中，通入保护气体，300℃～1500℃保温1～10h；
(5) 停止加热，继续通入保护气体，待炉温降低至室温，得到SnO2/CuO复合石墨烯包覆棉碳纤维材料，取出样品。
2.根据权利要求1所述的制备方法，其特征在于，所述步骤(1)中天然棉花纤维为天然棉花或由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 mg/ml~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为氧化还原法制备的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溶液前期需要超声处理1~2h。
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)中冷冻处理可以为低温冰箱冷冻或液氮冷冻。
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)中氯化亚锡与硝酸铜无水乙醇溶液的密度为5 mg/mL~100 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(3)中氯化亚锡与硝酸铜的摩尔比为20:1~1:10。
10.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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