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以硅藻土为前驱体制备白榴石的合成与表征

Synthesis and Characterization of Leucite Using a Diatomite Precursor.

作者信息

Novembre Daniela, Gimeno Domingo, Poe Brent

机构信息

Dipartimento di Ingegneria e Geologia, Università degli Studi "G.D'Annunzio", Via dei Vestini 30, 66013, Chieti, Italy.

Department Mineralogia, Petrologia i Geologia Aplicada, Universitat de Barcelona, 08028, Barcelona, Spain.

出版信息

Sci Rep. 2019 Jul 11;9(1):10051. doi: 10.1038/s41598-019-46569-y.

Abstract

Leucite is nowadays an important component in ceramic restoration systems with particular suitability to dental porcelains. The leucite synthesis from a hydrothermally-derived precursor is here presented. A silicate solution was prepared by mixing a naturally derived amorphous silica (diatomitic rock from Crotone, southern Italy) with potassium hydroxide and an aluminate solution was obtained by mixing aluminium hydroxide and potassium hydroxide. Three mixtures of varying ratios of aluminate and silicate solutions were prepared and submitted to hydrothermal treatment at 150 °C for one hour. Subsequently these hydrothermal precursors were subjected to calcination at the temperature of 1000 °C for variable time intervals, thus resulting in 3 series of syntheses. The synthesis run 3 turned out to be the best from the point of view of temporal yield showing the crystallization of the leucite after only 15 hours of heat treatment. The products of synthesis run 3 were fully characterised by Powder X-Ray Diffraction, Inductively Coupled Plasma Optical Emission Spectrometry, Infrared Spectroscopy and Thermal Analysis. The amorphous phase in the synthesis powders was estimated by quantitative phase analysis using the combined Rietveld and reference intensity ratio methods. Density of leucite was also achieved by He-pycnometry. The use of a cost effective starting material such as a diatomite in the experimental route makes the process highly attractive for expansion to an industrial scale especially considering that both the chemical and physical characterizations of our leucite product are highly satisfactory. Last but not least we explain some inferences that can be obtained from this process of synthesis in order to a better understanding of some natural occurrences of leucite in geologic systems related to basaltic magmas.

摘要

如今,白榴石是陶瓷修复系统中的重要成分,特别适用于牙科瓷器。本文介绍了由水热衍生前驱体制备白榴石的方法。通过将天然衍生的无定形二氧化硅(来自意大利南部克罗托内的硅藻土)与氢氧化钾混合制备硅酸盐溶液,并通过将氢氧化铝与氢氧化钾混合获得铝酸盐溶液。制备了三种不同比例的铝酸盐和硅酸盐溶液混合物,并在150℃下进行水热处理1小时。随后,将这些水热前驱体在1000℃的温度下进行不同时间间隔的煅烧,从而得到3系列合成产物。从时间产率的角度来看,合成批次3是最好的,仅在热处理15小时后就显示出白榴石的结晶。通过粉末X射线衍射、电感耦合等离子体发射光谱、红外光谱和热分析对合成批次3的产物进行了全面表征。使用Rietveld方法和参考强度比方法相结合的定量相分析来估计合成粉末中的非晶相。还通过氦比重瓶法测定了白榴石的密度。在实验路线中使用硅藻土等具有成本效益的起始原料,使得该工艺对于扩大到工业规模极具吸引力,特别是考虑到我们白榴石产品的化学和物理特性都非常令人满意。最后但同样重要的是,我们解释了从这个合成过程中可以得到的一些推断,以便更好地理解与玄武岩浆相关的地质系统中白榴石的一些自然成因。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/f0b5/6624203/7619a2ec5ccc/41598_2019_46569_Fig1_HTML.jpg

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