Crystal Structure and Phase Transitions of Gd(CO3)OH Studied by Synchrotron Powder Diffraction

被引：10

作者：

Sheu, Hwo-Shuenn ^{[1
]}

Shih, Wei-Ju ^{[1
]}

Chuang, Wei-Tsung ^{[1
]}

Li, I-Fang ^{[2
]}

Yeh, Chen-Sheng ^{[2
]}

机构：

[1] Natl Synchrotron Radiat Res Ctr, Hsinchu 300, Taiwan

[2] Natl Cheng Kung Univ, Dept Chem, Tainan 701, Taiwan

来源：

JOURNAL OF THE CHINESE CHEMICAL SOCIETY | 2010年 / 57卷 / 4B期

关键词：

Rare-earth compound; Crystal structure; In-situ powder diffraction; Phase transition; NANOPARTICLES; HYDROXYCARBONATES; OXIDES;

D O I：

10.1002/jccs.201000130

中图分类号：

O6 [化学];

学科分类号：

0703 ;

摘要：

The crystal structure of Gd(CO3)OH was solved using synchrotron powder X-ray diffraction. Gd(CO3)OH was known to exist in a form Gd2O(CO3)(2)center dot H2O and its powder pattern has been listed in JCPDF (#430604) for decades, but the crystal structure has not yet been elucidated. The crystal structure is solved with simulated annealing and the DASH program. The final Rietveld refinement converged to R-wp = 6.28%, R-p = 4.47% and x(2) = 1.348, using the GSAS program. Gd(CO3)OH crystallizes in orthorhombic system with lattice parameters a = 7.08109(9), b = 4.88436(7), c = 8.45010(13)angstrom and space group P nma. Gd(CO3)OH forms a three-dimensional framework with an eight-membered ring, a one-dimensional channel and OH- in the cavity. XANES of Gd L-III-edge indicates that the oxidation state of Gd is 3+. Two phase transitions of Gd(CO3)OH were found at 500 and 650 degrees C to yield Gd2O2CO3 and Gd2O3 respectively.

引用

页码：938 / 945

页数：8

共 32 条

[1] STRUCTURE DETERMINATIONS OF LA2O2CO3-II AND THE UNUSUAL DISORDERED PHASE LA2O2.52(CO3)0.74LI0.52 USING POWDER DIFFRACTION [J].

ATTFIELD, JP ;

FEREY, G .

JOURNAL OF SOLID STATE CHEMISTRY, 1989, 82 (01) :132-138

[2] Powder and single-crystal X-ray diffraction study of the structure of [Y(H2O)]2(C2O4)(CO3)2 [J].

Bataille, T ;

Louër, D .

ACTA CRYSTALLOGRAPHICA SECTION B-STRUCTURAL SCIENCE, 2000, 56 (06) :998-1002

[3] HYDROTHERMAL PREPARATION OF NEODYMIUM OXIDE CARBONATE - LOCATION OF CARBONATE ION IN STRUCTURE OF ND2O2CO3 [J].

CHRISTEN.AN .

ACTA CHEMICA SCANDINAVICA, 1970, 24 (07) :2440-&

[4] DASH:: a program for crystal structure determination from powder diffraction data [J].

David, William I. F. ;

Shankland, Kenneth ;

van de Streek, Jacco ;

Pidcock, Elna ;

Motherwell, W. D. Samuel ;

Cole, Jason C. .

JOURNAL OF APPLIED CRYSTALLOGRAPHY, 2006, 39 :910-915

[5] DETERMINATION OF CRYSTAL-STRUCTURE OF VARIETY OF HYDROXYCARBONATES OF RARE-EARTHS LNOHCO3 (LN=NA) [J].

DEXPERT, H ;

CARO, P .

MATERIALS RESEARCH BULLETIN, 1974, 9 (11) :1577-1585

[6]

DEXPERT H, 1982, J CHEM CRYSTALLOGR, P129

[7] Bis(2-amino-6-methylpyridinium)di-μ-chlorido-μ-oxido-bis[dichlorido-antimonate(III)] [J].

Feng, Wen-Jie ;

Wang, Hai-Bin ;

Ma, Xin-Ju ;

Li, Hai-Yan ;

Jin, Zhi-Min .

ACTA CRYSTALLOGRAPHICA SECTION E-CRYSTALLOGRAPHIC COMMUNICATIONS, 2007, 63 :M1786-U201

[8] Hydroxide carbonates and oxide carbonate hydrate of rare earths grown on glass via a hydrothermal route [J].

Han, ZH ;

Xu, P ;

Ratinac, KR ;

Lu, GQ .

JOURNAL OF CRYSTAL GROWTH, 2004, 273 (1-2) :248-257

[9] Crystalline lanthanum hydroxycarbonates with controlled phases and varied morphologies prepared on non-crystalline substrates [J].

Han, ZH ;

Yang, Q ;

Lu, GQ .

JOURNAL OF SOLID STATE CHEMISTRY, 2004, 177 (10) :3709-3714

[10] X-ray structure determination of the rare earth oxides (Er1-uGdu)2O3 applying the Rietveld method [J].

Heiba, Z ;

Okuyucu, H ;

Hascicek, YS .

JOURNAL OF APPLIED CRYSTALLOGRAPHY, 2002, 35 :577-580

← 1 2 3 4 →