用CuCl2为铜源高效制备形貌可控CuGeO3的研究

doi:10.15541/jim20200180

无机材料学报 ›› 2021, Vol. 36 ›› Issue (1): 69-74.DOI: 10.15541/jim20200180

用CuCl₂为铜源高效制备形貌可控CuGeO₃的研究

肖昱旻¹,李彬¹,覃礼钊¹(),林华¹,李庆¹,廖斌²

^1. 西南大学材料与能源学院, 重庆 400715
^2. 北京师范大学核科学与技术学院, 北京 100875

收稿日期:2020-04-03 修回日期:2020-05-04 出版日期:2021-01-20 网络出版日期:2020-06-09
作者简介:肖昱旻(1995-), 女, 硕士研究生. E-mail: x20172504@email.swu.edu.cn
基金资助:
中央高校基础研究经费(XDJK2019D004);广东省重点领域研发计划(2019B090909002);国家自然科学基金联合基金重点项目(U1865206);国防科技重点实验室基金(614220207011802)

Efficient Preparation of CuGeO₃ with Controllable Morphology Using CuCl₂ as Copper Source

XIAO Yumin¹,Li Bin¹,QIN Lizhao¹(),LIN Hua¹,LI Qing¹,LIAO Bin²

^1. Faculty of Materials & Energy, Southwest University, Chongqing 400715, China;
^2. College of Nuclear Science and Technology, Beijing Normal University, Beijing 100875, China

Received:2020-04-03 Revised:2020-05-04 Published:2021-01-20 Online:2020-06-09
About author:XIAO Yumin(1995-), female, Master candidate. E-mail: x20172504@email.swu.edu.cn
Supported by:
Fundamental Research Funds for the Central Universities(XDJK2019D004);Guangdong Province Key Area R&D Program(2019B090909002);National Natural Science Foundation Joint Fund Key Project(U1865206);National Defense Science and Technology Key Laboratory Fund(614220207011802)

摘要/Abstract

摘要：

锗酸铜因具有自旋佩尔斯效应以及优异的储锂性能而受到广泛关注, 普遍采用水热法制备锗酸铜。在制备过程中, 利用Cu(CH₃COO)₂等弱酸盐促进水的电离来获取CuGeO₃生长所需的OH ^-, 这种操作方法虽然简单, 但制备时间长、效率低。本研究采用强酸盐CuCl₂取代弱酸盐Cu(CH₃COO)₂为铜源, 调节前驱体溶液的pH, 控制各晶面吸附能力及溶液过饱和度, 实现高效制备CuGeO₃纳米棒和CuGeO₃六边形纳米片, 将制备时间缩短至8 h。并在此基础上, 添加一维结构导向剂乙二胺, 在加速反应过程的同时限制CuGeO₃的二维平面生长, 高效制备了100 nm、200~300 nm、350~500 nm、400~700 nm、1~2 μm和 1~3 μm六种不同尺寸、形貌均一的CuGeO₃纳米线。

关键词: CuGeO₃纳米线, CuCl₂, 水热法, 形貌控制

Abstract:

Copper germanate has attracted wide attention because of its spin-Peierls transition and excellent lithium storage performance. Typical hydrothermal method uses weak acid salts such as Cu(CH₃COO)₂ to promote the ionization of water to obtain OH ^- required for the growth of CuGeO₃. Although the operation is facile, the reaction time is long and the efficiency is low. In this work, CuCl₂ was used as the copper source instead of Cu(CH₃COO)₂ and the pH of precursor solution was adjusted to control the adsorption capacity of each crystal plane and the supersaturation of the solution, so as to achieve efficient preparation of CuGeO₃ nanorods and CuGeO₃ hexagonal nanosheets, effectively shortening the reaction time to 8 h. Based on this, one-dimensional structure-directing agent ethylenediamine was added to accelerate the reaction process while limiting the two-dimensional planar growth of CuGeO₃, and six different sizes ( 100 nm, 200-300 nm, 350-500 nm, 400-700 nm, 1-2 μm and 1-3 μm) of uniform CuGeO₃ nanowires were efficiently prepared.

Key words: CuGeO₃nanowires, CuCl₂, hydrothermal method, morphology controlled

中图分类号:

TB34

肖昱旻, 李彬, 覃礼钊, 林华, 李庆, 廖斌. 用CuCl₂为铜源高效制备形貌可控CuGeO₃的研究[J]. 无机材料学报, 2021, 36(1): 69-74.

XIAO Yumin, Li Bin, QIN Lizhao, LIN Hua, LI Qing, LIAO Bin. Efficient Preparation of CuGeO₃ with Controllable Morphology Using CuCl₂ as Copper Source[J]. Journal of Inorganic Materials, 2021, 36(1): 69-74.

图/表 6

图1 CGO-pH系列样品的XRD图谱

Fig. 1 XRD patterns of CGO-pH series samples

图2 CGO-pH5的XPS能谱图

Fig. 2 XPS spectra of CGO-pH5 (a) Cu2p; (b) Ge2p; (c) O1s

图3 CGO-pH系列样品的FESEM照片

Fig. 3 FESEM patterns of CGO-pH series samples

图4 CGO-En系列样品的XRD图谱

Fig. 4 XRD patterns of CGO-En series samples

图5 CGO-En 系列样品的FESEM照片

Fig. 5 FESEM images of CGO-En series samples

图6 (a) CGO-pH系列样品和(b) CGO-En系列样品的反应机理示意图

Fig. 6 Mechanism illustrations of (a) CGO-pH series samples and (b) CGO-En series samples

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用CuCl₂为铜源高效制备形貌可控CuGeO₃的研究

Efficient Preparation of CuGeO₃ with Controllable Morphology Using CuCl₂ as Copper Source

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