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稳定非晶态CaCO3在乙二醇无水体系中的制备及形成机理

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采用醇钙法在乙二醇钙无水体系中制备了纯净且稳定的非晶态 CaCO3(ACC),即利用 K2CO3 和 CaCl2 在乙二醇溶液中的反应制备ACC,并研究了溶液浓度、陈化温度和时间对产物相类型和颗粒形貌的影响.X射线衍射(XRD)结果表明,当溶液混合后立即有ACC生成;在 0℃和 20℃的反应温度下,当陈化时间延长至 4 个月时,产物依然保持非晶态,说明生成的ACC非常稳定;20℃下不同浓度溶液反应得到的产物也为纯净ACC.产物的红外光谱(IR)、透射电镜(TEM)以及选区电子衍射(SAED)结果验证了产物CaCO3 为非晶态.扫描电镜(SEM)观察结果表明,反应时间越短、反应温度越低、溶液越稀,ACC 越容易呈现疏松多孔状;随着陈化时间的延长,ACC 由疏松多孔的无定形态逐渐变成不规则颗粒状(0℃)和较规则的椭球状或球状颗粒(20℃).最后,从CaCl2 和K2CO3 在乙二醇中电离的角度探讨了ACC的形成机理.该研究为稳定的纯净ACC的制备提供了全新的途径,有助于进一步加深对ACC调控制备的理解.
Synthesis and Formation Mechanism of Amorphous CaCO3 in Anhydrous Ethylene Glycol
Pure and stable amorphous calcium carbonate(ACC)was synthesized by using alcohol-calcium method in anhydrous ethylene glycol,i.e.the reaction between CaCl2 and K2CO3 ethylene glycol solutions.The effect of solution concentration,aging temperature and time on polymorphs and morphologies of CaCO3 was studied.XRD results indicate that ACC is formed upon the mixing of the two solutions.At the reaction temperatures of 0℃ and 20℃,the product maintains amorphous even prolonging aging time to 4 months.ACC is the only polymorph in product obtained from different solution concentrations at 20℃.IR spectra,TEM images and SAED patterns verify the formation of ACC.SEM images reveal that the shorter aging time,the lower reaction temperature and the more diluted solution,the more readily for the formation of porous loose ACC.With prolonging aging time to 4 months,porous loose ACC becomes irregular particle at 0℃ and relative regular ellipsoidal or near-spherical particle at 20℃.The formation mechanism of ACC was discussed from the viewpoint of the ionization of CaCl2 and K2CO3 in ethylene glycol.This research extends the route to prepare stable pure ACC and provides new insights into its controllable synthesis.

amorphous calcium carbonatealcohol-calcium methodethylene glycol systemformation mechanism

喻欢、肖浩东、郭韬、曹孟洋、阮泓渊、蒋久信

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湖北工业大学 绿色轻工材料湖北省重点实验室,湖北 武汉 430068

湖北工业大学 新材料与绿色制造湖北省引智创新示范基地,湖北 武汉 430068

非晶态CaCO3 醇钙法 乙二醇无水体系 反应机理

湖北省大学生创新创业训练计划项目湖北省大学生创新创业训练计划项目

S202010500027S202210500067

2024

陶瓷学报
景德镇陶瓷学院

陶瓷学报

CSTPCD北大核心
影响因子:0.7
ISSN:1000-2278
年,卷(期):2024.45(2)
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