Giordano Cristina, Erpen Christian, Yao Weitang, Antonietti Markus
Max-Planck-Institute of Colloids and Interfaces, Department of Colloid Chemistry, Research Campus Golm, D-14424 Potsdam, Germany.
Nano Lett. 2008 Dec;8(12):4659-63. doi: 10.1021/nl8018593.
A simple, inexpensive, and versatile route for the synthesis of metal nitrides and carbides (such as Mo2N, Mo2C, W2N and WC) nanoparticles was set up. For the first time, metal carbides were obtained using urea as carbon-source. MoCl5 and WCl4 are in a first step contacted with alcohols and an appropriate amount of urea to form a polymer-like, glassy phase, which acts as the starting product for further conversions. Just by heating this phase it was possible to prepare either molybdenum and tungsten nitrides or carbides simply by changing the metal precursor/urea molar ratio. In this procedure, urea plays a double role as a nitrogen/carbon source and stabilizing agent (necessary for the nanoparticle dispersion). Molybdenum and tungsten nitride and carbides synthesized are almost pure and highly crystalline. Sizes estimated by WAXS range around 20 and 4 nm in diameter for Mo and W nitrides or carbides, respectively. The specific surface area was found between 10 and 80 m2/g, depending on the metal and the initial ratio of metal precursor to urea.
建立了一种简单、廉价且通用的合成金属氮化物和碳化物(如Mo₂N、Mo₂C、W₂N和WC)纳米颗粒的方法。首次使用尿素作为碳源获得了金属碳化物。第一步,将MoCl₅和WCl₄与醇类和适量尿素接触,形成类似聚合物的玻璃相,该玻璃相作为进一步转化的起始产物。仅通过加热该相,就可以通过改变金属前驱体/尿素的摩尔比简单地制备钼和钨的氮化物或碳化物。在此过程中,尿素既作为氮/碳源又作为稳定剂(这对于纳米颗粒的分散是必要的)发挥双重作用。合成的钼和钨的氮化物及碳化物几乎是纯的且高度结晶。通过广角X射线散射(WAXS)估计,Mo和W的氮化物或碳化物的尺寸分别约为直径20和4 nm。根据金属以及金属前驱体与尿素的初始比例,比表面积在10至80 m²/g之间。