Synthesis and thermal stability of Zr(BH4)4 and Zr(BD4)4 produced by mechanochemical processing

被引：26

作者：

Gennari, F. C. ^{[1
,2
,3
]}

Fernandez Albanesi, L. ^{[4
]}

Rios, I. J. ^{[1
,2
]}

机构：

[1] Ctr Atom Bariloche CNEA, San Carlos De Bariloche, Argentina

[2] Univ Nacl Cuyo, Inst Balseiro, San Carlos De Bariloche, Rio Negro, Argentina

[3] Consejo Nacl Invest Cient & Tecn, RA-1033 Buenos Aires, DF, Argentina

[4] INVAP SE, San Carlos De Bariloche, Rio Negro, Argentina

来源：

INORGANICA CHIMICA ACTA | 2009年 / 362卷 / 10期

关键词：

Mechanochemistry; Complex hydrides; Tetrahydroborates; Diborane; TRANSITION-METAL; HYDRIDES; TETRAHYDROBORATE; MAGNESIUM; SCALE;

D O I：

10.1016/j.ica.2009.04.031

中图分类号：

O61 [无机化学];

学科分类号：

070301 ; 081704 ;

摘要：

Zirconium tetrahydroborate Zr(BH4)(4) and its deuteride compound Zr(BD4)(4) were successfully synthesized by mechanochemical reaction between NaBH4 or NaBD4 and ZrCl4, reaching yields of 55% and 46%, respectively. The influence of the synthesis parameters on the yield of Zr(BH4)(4) was analyzed. The composition of the ZrCl4: NaBH4 starting mixture and the use of LiBH4 instead of NaBH4 as reactive show a clear effect on the Zr(BH4)(4) yield. Instead, milling atmosphere does not affect the amount of the obtained product. FTIR analysis of atmosphere inside of milling vial allows to determine the formation of diborane during milling from Zr(BH4)(4) decomposition. Thermal stability of pure Zr(BH4)(4) and its deuterated compound was studied by combined gas-phase FTIR and DSC measurements under. owing Ar. We found that Zr(BH4)(4)/Zr(BD4)(4) melt at about 305/303 K, decompose at about 430 K from the gas-phase and show evolution of B2H6/B2D6 under heating. (C) 2009 Elsevier B. V. All rights reserved.

引用

页码：3731 / 3737

页数：7

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