Dong Yongkwan, Chai Ping, Beekman Matt, Zeng Xiaoyu, Tritt Terry M, Nolas George S
†Department of Physics, University of South Florida, Tampa, Florida 33620, United States.
‡Department of Natural Sciences, Oregon Institute of Technology, Klamath Falls, Oregon 97601, United States.
Inorg Chem. 2015 Jun 1;54(11):5316-21. doi: 10.1021/acs.inorgchem.5b00348. Epub 2015 May 18.
Single crystals of the ternary clathrate-I Na8Al8Si38 were synthesized by kinetically controlled thermal decomposition (KCTD), and microcrystalline Na8Al8Si38 was synthesized by spark plasma sintering (SPS) using a NaSi + NaAlSi mixture as the precursor. Na8AlxSi46-x compositions with x ≤ 8 were also synthesized by SPS from precursor mixtures of different ratios. The crystal structure of Na8Al8Si38 was investigated using both Rietveld and single-crystal refinements. Temperature-dependent transport and UV/vis measurements were employed in the characterization of Na8Al8Si38, with diffuse-reflectance measurement indicating an indirect optical gap of 0.64 eV. Our results indicate that, when more than one precursor is used, both SPS and KCTD are effective methods for the synthesis of multinary inorganic phases that are not easily accessible by traditional solid-state synthesis or crystal growth techniques.
通过动力学控制热分解（KCTD）合成了三元笼型 - I化合物Na8Al8Si38的单晶，并使用NaSi + NaAlSi混合物作为前驱体通过放电等离子烧结（SPS）合成了微晶Na8Al8Si38。还通过SPS从不同比例的前驱体混合物中合成了x≤8的Na8AlxSi46 - x组成。使用Rietveld精修和单晶精修对Na8Al8Si38的晶体结构进行了研究。在Na8Al8Si38的表征中采用了温度依赖的输运和紫外/可见光谱测量，漫反射测量表明其间接光学带隙为0.64 eV。我们的结果表明，当使用不止一种前驱体时，SPS和KCTD都是合成传统固态合成或晶体生长技术难以获得的多元无机相的有效方法。
