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一种新方法用于合成纳米晶态钴硼化物,该方法是在热分解钴配合物[Co(DMF)]与硼簇阴离子的过程中实现的。

A New Approach to the Synthesis of Nanocrystalline Cobalt Boride in the Course of the Thermal Decomposition of Cobalt Complexes [Co(DMF)] with Boron Cluster Anions.

机构信息

Kurnakov Institute of General and Inorganic Chemistry, Russian Academy of Sciences, Moscow 119991, Russia.

出版信息

Molecules. 2023 Jan 3;28(1):453. doi: 10.3390/molecules28010453.

DOI:10.3390/molecules28010453
PMID:36615646
原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC9823307/
Abstract

In the course of the study, nanocrystalline cobalt monoboride was prepared by thermal decomposition of precursors [Co(DMF)][An], where [An] = [BH] (), [-BH] () or [BCl] () in an argon atmosphere. Three new salt-like compounds - were prepared when Co(NO) was allowed to react with (EtNH)[An]. Compound is new; the structures of compounds and have been previously reported. Samples - were annealed at 900 °C in argon to form samples -, which were characterized by single crystal XRD for and powder XRD for . Powder XRD on the products showed the formation of BN and CoB for in a 1:1 ratio; gave a higher CoB:BN ratio but an overall decreased crystallinity. For , only CoB was found. IR spectra of samples - as well as X-ray spectral fluorescence analysis for 3a confirmed these results. The nanoparticular character of the decomposition products - was shown using TEM; quite small particle sizes of about 10-15 nm and a quite normal size distribution were found for and a, while the decomposition of gave large particles with 200-350 nm and a broad distribution.

摘要

在研究过程中,通过在氩气气氛中热分解前驱物 [Co(DMF)][An](其中 [An] = [BH] ()、[-BH] () 或 [BCl] ())来制备纳米晶钴单硼化物。当 Co(NO) 与 (EtNH)[An] 反应时,制备了三种新的类似盐的化合物 -。化合物 是新的;化合物 和 的结构以前已有报道。将样品 - 在氩气中于 900°C 退火以形成样品 -,通过单晶 XRD 对 和粉末 XRD 对 进行了表征。产物的粉末 XRD 显示 BN 和 CoB 以 1:1 的比例形成;但结晶度总体降低。对于 ,仅发现了 CoB。样品 - 的 IR 光谱以及 3a 的 X 射线光谱荧光分析证实了这些结果。通过 TEM 显示了分解产物 - 的纳米颗粒特征;和 发现粒径约为 10-15nm,分布相当正常,而 的分解则产生了粒径为 200-350nm 且分布较宽的大颗粒。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/da38/9823307/817ad6981d83/molecules-28-00453-sch002.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/da38/9823307/c65c03cb2ec6/molecules-28-00453-g010.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/da38/9823307/58170754284c/molecules-28-00453-g011.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/da38/9823307/817ad6981d83/molecules-28-00453-sch002.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/da38/9823307/c65c03cb2ec6/molecules-28-00453-g010.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/da38/9823307/58170754284c/molecules-28-00453-g011.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/da38/9823307/817ad6981d83/molecules-28-00453-sch002.jpg

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