Preparation of fiber-like complex nickel oxalate by precipitation-transformation method
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摘要: 以六水合硫酸镍为原料、两水合草酸为沉淀剂制备了草酸镍沉淀，再以乙二胺为配位剂配位转化草酸镍，合成了纤维状复杂草酸镍盐前驱体粉末。利用X射线衍射分析、扫描电子显微镜观察、傅里叶变换红外光谱分析及热重‒差热分析表征了前驱体物相组成及显微形貌，讨论了制备工艺参数对前驱体尺寸及形貌的影响，并得出了最佳工艺参数。结果表明，沉淀-转化法制备的镍盐前驱体结构中含有乙二胺成分，其晶体形貌呈纤维状，组成分布均匀。最佳工艺参数为正加料方式，初始pH 7.5，Ni2+浓度0.6 mol·L‒1，反应温度65 ℃，表面活性剂（PVP）0.4 g，在此条件下可制得分散性良好的纤维状复杂草酸镍盐前驱体，其最高长径比可达55。Abstract: The fiber-like complex nickel oxalate precursor powders were prepared by precipitation-transformation method using nickel sulfate hexahydrate as the raw materials, oxalic acid dihydrate as the precipitants, and ethylenediamine as the complexants in this paper. The composition and morphology of the precursors were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), and thermogravimetric‒differential thermal analysis (TG‒DTA). The effects of preparation process parameters on the size and morphology of the precursors were studied. The results show that, the nickel salt precursors prepared by the precipitation-transformation method contain ethylenediamine, and the crystal morphology are fibrous and dispersed uniformly. The optimum conditions are as follows: the positive feeding mode, initial pH 7.5, Ni2+ concentration 0.6 mol·L‒1, reaction temperature 65 ℃, and surfactant 0.4 g. Under these conditions, the desire fiber-like complex nickel oxalate precursors with good dispersibility can be prepared, and the maximum aspect ratio can reach 55.
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Key words:
- precipitation-transformation /
- fibrous /
- nickel powders /
- ethylenediamine /
- precursors
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图 4 不同加料方式制备的复杂镍盐前驱体显微形貌：（a）正加料；（b）反加料
Figure 4. SEM images of the complex nickel salt precursors prepared by the different feeding methods: (a) positive feeding; (b) negative feeding
图 5 不同pH条件下制备的复杂镍盐前驱体显微形貌：（a）pH=4.8；（b）pH=6.7；（c）pH=7.0；（d）pH=7.5；（e）pH=8.0
Figure 5. SEM images of the complex nickel salt precursors prepared at the different pH: (a) pH=4.8; (b) pH=6.7; (c) pH=7.0; (d) pH=7.5; (e) pH=8.0
图 6 不同Ni2+浓度下制备复杂镍盐前驱体显微形貌：（a）0.2 mol·L‒1；（b）0.4 mol·L‒1；（c）0.6 mol·L‒1；（d）0.8 mol·L‒1
Figure 6. SEM images of the complex nickel salt precursors prepared under the different Ni2+ concentrations: (a) 0.2 mol·L‒1; (b) 0.4 mol·L‒1; (c) 0.6 mol·L‒1; (d) 0.8 mol·L‒1
图 7 不同温度下制备复杂镍盐前驱体显微形貌：（a）55 ℃；（b）65 ℃；（c）75 ℃
Figure 7. SEM images of the complex nickel salt precursors prepared at the different temperature: (a) 55 ℃; (b) 65 ℃; (c) 75 ℃
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