Preparation of Multicomponent Nitrides and their Crystal Chemstry

多元氮化物的制备及其晶体化学

• 批准号: 09650726
• 负责人: YAMANE Hisanori
• 金额: $ 2.05万
• 依托单位: Tohoku University
• 依托单位国家: 日本
• 项目类别: Grant-in-Aid for Scientific Research (C)
• 财政年份: 1997
• 资助国家: 日本
• 起止时间: 1997 至 1998
• 项目状态: 已结题
• 来源: https://kaken.nii.ac.jp/grant/KAKENHI-PROJECT-09650726/
• 关键词: Nitrides; Na metal; Single Crystals; Crystal Structure Analysis; Sodium Azide; Powder X-Ray Diffraction; アルカリ金属アジ化物; アルカリ土類亜鉛窒化物; 窒化亜鉛基

Preparation of multi-component nitrides was attempted by using sodium azide (NaN3) as anitrogen source and sodium metal (Na) as a flux. Metal sources were sealed with NaN3 and Na in a stainless-steel tube container in which the inner wall was covered with a niobium sheet. This tube was placed in an electric furnace with argon gas and heated at 750ﾟC.After the heating, the tube was cooled to room temperature. The Na flux was washed with liquid ammonia. An H-shape cell was designed for this process. By using the present method, single crystals of strontium gallium nitride, Sr_3Ga_2N_4 were prepared. The crystals were below 1 mm in size, thin platelet, yellow, and transparent. X-ray single crystal structure analysis revealed that this compound has an orthorhombic symmetry (lattice parameters : alpha= 5.9579(12) , b = 10.285(2) , c = 9.557(2) A, space group P nna). Sr_3Ga_2N_4 is isostructural with Sr_3Al_2N_4 and Ba_3Ga_2N_4. Ga atoms were coordinated by four nitrogen atoms and form tetrahedra. The tetrahedra share two edges and make a one-dimensional chain. Strontium atoms are surrounded by six nitrogen atoms. Red color transparent single crystals were also obtained in the system of Ba-Ti-N, but not in the Sr-Ti N.Mixture of binary nitrides were obtained and multi-component nitrides could not be synthesized in the systems including rare-earth elements.

尝试使用叠氮化钠（NaN3）作为氮源和金属钠（Na）作为助熔剂来制备多组分氮化物。将金属源与NaN3和Na密封在不锈钢管容器中，其中内壁被覆盖。将该管放入装有氩气的电炉中并在750℃下加热。加热后，将管冷却至室温。采用该方法制备了H型氮化镓单晶Sr_3Ga_2N_4，晶体尺寸小于1mm，呈薄片状，呈黄色、透明。 X射线单晶结构分析表明该化合物具有斜方对称性（晶格参数： alpha= 5.9579(12) , b = 10.285(2) , c = 9.557(2) A, Sr_3Ga_2N_4 与Sr_3Al_2N_4 和Ba_3Ga_2N_4 原子配位形成四面体，四面体共享两个边并形成一维。锶原子被六个氮原子包围，还获得了红色透明单晶。在Ba-Ti-N体系中，但在Sr-Ti N体系中则不然。在含有稀土元素的体系中，得到了二元氮化物的混合物，并且不能合成多元氮化物。

项目成果

Hisanori Yamane: "The Crystal Structure of Sr_6Cu_3N_5 with isolated,bent(Cu^1_2N_3)^<7-> anions and the single Crystal Structural Determination of SrCuN" J.Alloys Comp. 255. 122-129 (1997)

Hisanori Yamane：“具有孤立弯曲(Cu^1_2N_3)^<7->阴离子的Sr_6Cu_3N_5的晶体结构和SrCuN的单晶结构测定”J.Alloys Comp。