二乙醇胺控制水热合成亚微米球形 CoAl<sub>2</sub>O<sub>4</sub>色料

doi:10.11901/1005.3093.2014.532

材料研究学报

2015, Vol. 29

Issue (7): 542-548 DOI: 10.11901/1005.3093.2014.532

本期目录 | 过刊浏览

二乙醇胺控制水热合成亚微米球形 CoAl₂O₄色料

钟幸福子¹,卢希龙¹,曹春娥¹(

),陈云霞^1,²,沈华荣¹

1. 景德镇陶瓷学院材料科学与工程学院景德镇 333403
2. 江西省先进陶瓷材料重点实验室景德镇 333001

Diethanolamine Controlled Hydrothermal Synthesis of Submicron Spherical CoAl₂O₄ Pigments

Xingfuzi ZHONG¹,Xilong LU¹,Chun'e CAO^1,^**(

),Yunxia CHEN^1,²,Huarong SHEN¹

1. School of Material Science and Engineering, Jingdezhen Ceramic Institute, Jingdezhen 333403, China
2. Jiangxi Key Laboratory of Advanced Ceramic Materials, Jingdezhen 333000, China

引用本文:

钟幸福子,卢希龙,曹春娥,陈云霞,沈华荣. 二乙醇胺控制水热合成亚微米球形 CoAl₂O₄色料[J]. 材料研究学报, 2015, 29(7): 542-548.
Xingfuzi ZHONG, Xilong LU, Chun'e CAO, Yunxia CHEN, Huarong SHEN. Diethanolamine Controlled Hydrothermal Synthesis of Submicron Spherical CoAl₂O₄ Pigments[J]. Chinese Journal of Materials Research, 2015, 29(7): 542-548.

全文: PDF(2367 KB) HTML

摘要:

以CoCl₂6H₂O和AlCl₃为起始原料, 以NaOH为沉淀剂, 以二乙醇胺为包覆剂, 用水热法合成亚微米球形CoAl₂O₄色料, 使用XRD、TEM和色度分析等手段研究了反应物浓度、n_Co/n_Al和二乙醇胺加入量对合成色料的物相组成、颗粒形貌及大小和呈色的影响, 并从晶体生长动力学角度分析了二乙醇胺包覆控制下球形颗粒形成的原因。结果表明: 当Co²⁺浓度为0.05 mol/L、n_Co/n_Al为1∶2、二乙醇胺添加量为12%(V/V)时, 可制得亚微米级球形CoAl₂O₄颗粒, 粒径大多为100-230 nm。加入的二乙醇胺能在晶粒成核和生长过程中定向吸附于顶点和边棱处产生空间位阻作用, 使颗粒发育成球形。

关键词 ：无机非金属材料, 球形CoAl₂O₄, 水热法, 二乙醇胺, 包覆剂

Abstract：

Submicron spherical CoAl₂O₄pigments were hydrothermal synthesized using CoCl₂·6H₂O and AlCl₃ as raw materials, NaOH as the precipitant and diethanolamine (DEA) as capping agent, respectively. The effect of the concentration of raw materials, the ratio of n_Co/n_Al and the amount of DEA on the phase composition, particle size and morphology as well as the chroma of the as-prepared pigments was investigated by means of XRD, TEM and calorimetric analysis. The results show that submicron spherical CoAl₂O₄pigments with size in a range of 100-230 nm could be synthesized under the conditions of n_Co/n_Al=1: 2, Co²⁺concentration 0.05 mol/L and DEA 12%(V/V). The formation of spherical particles was analyzed from the point of view of kinetically controlled crystal growth in the presence of DEA. It follows that during the nucleation and growth process of the crystalline particles, DEA molecules can be adsorbed onto the edges and vertices of the particles in a highly oriented manner thus causing steric hindrance, which enable the spherical growth of the crystalline particles to be possible.

Key words： inorganic non-metallic materials spherical CoAl₂O₄ hydrothermal method diethanolamine capping agent

收稿日期: 2014-09-26

基金资助:* 国家自然科学基金51162016和景德镇陶瓷学院研究生创新基金JYC1105资助项目。2014年9月26日收到初稿; 2015年 1月 12日收到修改稿。本文联系人: 曹春娥, 教授

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https://www.cjmr.org/CN/10.11901/1005.3093.2014.532 或 https://www.cjmr.org/CN/Y2015/V29/I7/542

表1 实验安排表

图1 不同Co2+浓度样品的XRD图谱

图2 不同Co2+浓度样品的TEM照片

表2

图3 不同nCo/nAl样品的XRD图谱

表3 不同nCo/nAl样品的色度测试结果

图4 二乙醇胺加入量不同的样品XRD图谱

图5 二乙醇胺加入量不同的样品TEM照片

表4 不同二乙醇胺加入量样品的色度测试结果

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