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纳米级复合金属氟化物的溶胶-凝胶合成法

Sol-Gel-Synthesis of Nanoscopic Complex Metal Fluorides.

作者信息

Rehmer Alexander, Scheurell Kerstin, Scholz Gudrun, Kemnitz Erhard

机构信息

Institut für Chemie, Humboldt-Universität zu Berlin, Brook-Taylor- Str. 2, D-12489 Berlin, Germany.

Nanofluor GmbH, Rudower Chaussee 29, D-12489 Berlin, Germany.

出版信息

Nanomaterials (Basel). 2017 Nov 2;7(11):362. doi: 10.3390/nano7110362.

DOI:10.3390/nano7110362
PMID:29099086
原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC5707579/
Abstract

The fluorolytic sol-gel synthesis for binary metal fluorides (AlF₃, CaF₂, MgF₂) has been extended to ternary and quaternary alkaline earth metal fluorides (CaAlF₅, Ca₂AlF₇, LiMgAlF₆). The formation and crystallization of nanoscopic ternary CaAlF₅ and Ca₂AlF₇ sols in ethanol were studied by F liquid and solid state NMR (nuclear magnetic resonance) spectroscopy, as well as transmission electron microscopy (TEM). The crystalline phases of the annealed CaAlF₅, Ca₂AlF₇, and LiMgAlF₆ xerogels between 500 and 700 °C could be determined by X-ray powder diffraction (XRD) and F solid state NMR spectroscopy. The thermal behavior of un-annealed nanoscopic ternary and quaternary metal fluoride xerogels was ascertained by thermal analysis (TG/DTA). The obtained crystalline phases of CaAlF₅ and Ca₂AlF₇ derived from non-aqueous sol-gel process were compared to crystalline phases from the literature. The corresponding nanoscopic complex metal fluoride could provide a new approach in ceramic and luminescence applications.

摘要

用于二元金属氟化物（AlF₃、CaF₂、MgF₂）的氟解溶胶 - 凝胶合成法已扩展至三元和四元碱土金属氟化物（CaAlF₅、Ca₂AlF₇、LiMgAlF₆）。通过氟的液态和固态核磁共振（NMR）光谱以及透射电子显微镜（TEM）研究了乙醇中纳米级三元CaAlF₅和Ca₂AlF₇溶胶的形成与结晶过程。500至700°C之间退火的CaAlF₅、Ca₂AlF₇和LiMgAlF₆干凝胶的晶相可通过X射线粉末衍射（XRD）和氟的固态NMR光谱确定。通过热分析（TG/DTA）确定未退火的纳米级三元和四元金属氟化物干凝胶的热行为。将非水溶胶 - 凝胶法得到的CaAlF₅和Ca₂AlF₇的晶相与文献中的晶相进行了比较。相应的纳米级复合金属氟化物可为陶瓷和发光应用提供一种新方法。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/a12e/5707579/db127532552e/nanomaterials-07-00362-g013.jpg
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https://cdn.ncbi.nlm.nih.gov/pmc/blobs/a12e/5707579/a0895c96e3ef/nanomaterials-07-00362-g007.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/a12e/5707579/549bb30ec86b/nanomaterials-07-00362-g008.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/a12e/5707579/10634b287798/nanomaterials-07-00362-g009.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/a12e/5707579/204af61f5a17/nanomaterials-07-00362-g010.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/a12e/5707579/d2ac35510fab/nanomaterials-07-00362-g011.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/a12e/5707579/25e61711c874/nanomaterials-07-00362-g012.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/a12e/5707579/db127532552e/nanomaterials-07-00362-g013.jpg

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本文引用的文献

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The non-aqueous fluorolytic sol-gel synthesis of nanoscaled metal fluorides.纳米级金属氟化物的非水氟解溶胶-凝胶合成法。
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Mechanistic insight into formation and changes of nanoparticles in MgF2 sols evidenced by liquid and solid state NMR.通过液-固核磁共振对 MgF2 溶胶中纳米颗粒的形成和变化的机理研究。
Dalton Trans. 2012 Feb 28;41(8):2360-6. doi: 10.1039/c2dt11762b. Epub 2012 Jan 3.
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Solvothermal synthesis of well-dispersed NaMgF3 nanocrystals and their optical properties.
溶剂热法合成均匀分散的NaMgF₃纳米晶体及其光学性质
J Colloid Interface Sci. 2009 Jan 1;329(1):103-6. doi: 10.1016/j.jcis.2008.09.076. Epub 2008 Oct 7.
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Correlation between 19F environment and isotropic chemical shift in barium and calcium fluoroaluminates.钡和钙氟铝酸盐中¹⁹F环境与各向同性化学位移之间的相关性。
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Amorphous metal fluorides with extraordinary high surface areas.具有超高表面积的非晶态金属氟化物。
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