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亞微米球形鎳粉的兩步法可控制備與表征
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中南大學(xué)粉末冶金研究院,中南大學(xué)粉末冶金研究院,中南大學(xué)粉末冶金研究院

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國家自然科學(xué)基金項目(面上項目,重點項目,重大項目)


Controllable preparation and characterization of sub-micron spherical Ni powder with two step method
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The National Natural Science Foundation of China (General Program, Key Program, Major Research Plan)

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    摘要:

    以H2C2O4?2H2O為沉淀劑,NiSO4?6H2O為鎳源,第一步通過共沉淀法制得NiC2O4前驅(qū)體粉末;然后在H2氣氛、中溫條件下(250-500℃)煅燒還原,第二步制得高規(guī)則度的亞微米球形鎳粉。采用掃描電子顯微鏡、X 射線衍射、激光粒度分析等檢測手段對所制備的樣品形貌、顯微結(jié)構(gòu)進(jìn)行表征。結(jié)果表明:亞微米球形鎳粉純度高,二次顆粒粒徑約為40μm左右,由大量大小均勻、分散性好的粒徑0.5μm左右的一次顆粒團(tuán)聚而成,這種結(jié)構(gòu)保證了鎳粉具有良好的成形性和燒結(jié)活性。隨煅燒溫度的升高,結(jié)晶度逐漸升高;亞微米球形鎳粉的最佳制備工藝參數(shù)為:鎳離子濃度0.7mol.L-1,反應(yīng)溫度40℃和煅燒溫度500℃。鎳粉的晶粒長大活化能為26.9 kJ?mol-1,其晶粒長大機(jī)制為界面擴(kuò)散控制機(jī)制。

    Abstract:

    With H2C2O4?2H2O as precipitant and NiSO4?6H2O as Ni source, NiCO4 precursor was prepared through coprecipitation method in the first step. Afterwards, highly regular sub-micron spherical Ni powders were calcined and reduced under H2 atmosphere at middle temperature in the second step. Scanning electronic microscopy, X-ray diffraction and laser particle size analyzer were used to characterize the morphology and microstructure of Ni powder. The results show that the purity of Ni powder is very well. The secondary particle of Ni powder is about 40μm agglomerated with a lot of 0.5μm dispersed and uniform primary particles, which guarantees the excellent forming property and sintering activity. The crystallinity of Ni powder increases with the sintering temperature. The optimal preparing parameters are 0.7mol.L-1 Ni2+ concentration, 40℃ reactive temperature and 500℃ sintering temparature. Grain growth activation energy of Ni powder can be calculated as 26.9 kJ?mol-1 according to the relationship between grain size and sintering temperature and Ni powder’s growing mechanism is interfacial diffusion controlling mechanism.

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鄒儉鵬,楊洪志,劉如鐵.亞微米球形鎳粉的兩步法可控制備與表征[J].稀有金屬材料與工程,2018,47(9):2847~2851.[zoujianpeng, yang hongzhi, liu rutie. Controllable preparation and characterization of sub-micron spherical Ni powder with two step method[J]. Rare Metal Materials and Engineering,2018,47(9):2847~2851.]
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  • 收稿日期:2016-11-08
  • 最后修改日期:2017-03-10
  • 錄用日期:2017-03-16
  • 在線發(fā)布日期: 2018-11-01
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