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Preparation of γ-Gd_2 S_3 via thermolysis of Gd[S_2 CN(C_4 H_8)]_3 ·phen coordination

Preparation of γ-Gd_2 S_3 via thermolysis of Gd[S_2 CN(C_4 H_8)]_3 ·phen coordination
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摘要 Pure γ-Gd2S3 was synthesized by the thermolysis of a single Gd[S2CN(C4H8)]3 phen complex precursor in a flow of argon carrier gas containing sulfur vapor. The complex precursor was decomposed into amorphous Gd2S3 and carbon at about 350 ℃. Crystalline y-Gd2S3 could be achieved at temperature exceeding 600 ℃, and the obtained γ-Gd2S3 presented a very high degree of crystallinity at 800 ℃. Carbon prevented the formation of Gd2O2S impurity in the preparation of y-Gd2S3. However, the carbon blackened the product. At temperature ≥ 1000 ℃, the residual carbon impurity could be efficiently removed by introducing sulfur into the system for the volatile CS2 could be formed in situ via the reaction of sulfur with the deposited carbon. In the meantime, S also promoted the crystallization of γ-Gd2S3 remarkablely. Pure γ-Gd2S3 was synthesized by the thermolysis of a single Gd[S2CN(C4H8)]3 phen complex precursor in a flow of argon carrier gas containing sulfur vapor. The complex precursor was decomposed into amorphous Gd2S3 and carbon at about 350 ℃. Crystalline y-Gd2S3 could be achieved at temperature exceeding 600 ℃, and the obtained γ-Gd2S3 presented a very high degree of crystallinity at 800 ℃. Carbon prevented the formation of Gd2O2S impurity in the preparation of y-Gd2S3. However, the carbon blackened the product. At temperature ≥ 1000 ℃, the residual carbon impurity could be efficiently removed by introducing sulfur into the system for the volatile CS2 could be formed in situ via the reaction of sulfur with the deposited carbon. In the meantime, S also promoted the crystallization of γ-Gd2S3 remarkablely.
出处 《Journal of Rare Earths》 SCIE EI CAS CSCD 2012年第8期802-806,共5页 稀土学报(英文版)
基金 Project supported by National Natural Science Foundation of China(60979003) New Century Educational Talents Plan of Chinese EducationMinistry,China(NCET-10-0171) Fundamental Research Funds for the Central Universities(2011QN153,2012QN065,2012QN068,2012TD018) Scientific Research Fund of Zhejiang Provincial Education Department(Y201121038)
关键词 THERMOLYSIS rare earth sesquisulfides γ-Gd2S3 single source precursor thermolysis rare earth sesquisulfides γ-Gd2S3 single source precursor
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参考文献12

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