Thermal stability of the nanolayered Fe2AlB2 in nitrogen and argon atmospheres

The thermal stability and decomposition mechanisms of Fe₂AlB₂ powders, synthesized by reactive powder metallurgy, were studied under nitrogen (N₂) or argon (Ar) atmospheres. The effects of using different FeB precursors to synthesize the Fe₂AlB₂ and hydrochloric acid (HCl) purification treatments on the thermal stability were also investigated. When as-synthesized Fe₂AlB₂ powders are treated in dilute HCl to dissolve impurity phases, decomposition in N₂ atmospheres occurs readily above 1200 K. The decomposition reaction involves β-FeB precipitation and the liberated Al atoms reacting with the ambient N₂ to form AlN. Under Ar environments, HCl-treated Fe₂AlB₂ powders decompose and precipitate β-FeB, by the out-diffusion of Al from the nanolaminated structure. Interestingly, isothermal annealing under N₂ atmospheres revealed that Fe₂AlB₂ was more thermally stable when synthesized from lab-synthesized, instead of commercially available, FeB precursors and when the HCl treatment was avoided. The effects of the various factors on the decomposition temperature and decomposition mechanisms are discussed herein.     

One-pot foam-gelcasting/nitridation synthesis of high porosity nano-whiskers based 3D Si3N4 porous ceramics

Nano-whiskers based 3D Si₃N₄ porous ceramics (3D-NWSNPC) with high-porosity (about 91–93 %), low density (0.17–0.25 g/cm³), low thermal conductivity, and a certain degree of recoverability under cyclic compressive loading and reasonably strengths were prepared at 1423–1523 K via a one-pot foam-gelcasting/nitridation route using inexpensive commercial Si powders as starting materials and hexadecyl trimethyl ammonium bromide as foaming agent. After nitridation at 1523 K, the sample with an original solid loading of 12.5 wt% exhibited the highest compressive strength of 1.9 MPa, even though its density was lowered to 0.25 g/cm³. The sample nitrided at 1473 K had a relative density of 7.3 %. Its compressive and specific strength were respectively 1.1 MPa and 5.5 MPa·cm³ g^?1, and its thermal conductivity was as low as 0.074 W/(m K) (measured at 323 K). These outstanding properties would make the as-prepared 3D-NWSNPC a promising candidate for applications in catalysis, filtration, thermal insulation and many other important areas.     

In-situ formation of BN layers by nitriding boron powders in BN/Si3N4-based composite ceramics

Boron nitride/silicon nitride (BN/Si₃N₄) composite ceramics were fabricated via the in-situ nitridation of boron (B) and silicon (Si) powders in forming gas (95%N₂/5%H₂) at 1390?°C. The effect of the B content on the phase composition, microstructure, density/porosity, machinability as well as mechanical properties of nitridized BN/Si₃N₄ composite ceramics was investigated. The addition of B slightly increased the nitridation degree of the Si and B powders mixture, and improved the ratio of the β-Si₃N₄ phase significantly at low B contents. B powders may have acted as a nucleating agent to promote the formation of β-Si₃N₄ crystals. A core-shell Si₃N₄/BN structure was revealed by the TEM technique, and the number of BN layers increased with the increase of the B content. The in-situ BN formed by the nitridation of B played a similar role with the BN directly added in enhancing the machinability of the BN/Si₃N₄ composite ceramics. The method of the in-situ nitridation of B is also effective to prepare SiC fiber-reforced BN/Si₃N₄ ceramic matrix composites.     

内凝胶工艺结合碳热氮化法制备ZrN纳米粉体

采用内凝胶工艺制得无定形的氧化锆凝胶与炭黑均匀混合的前驱体粉末,获得的前驱体在氮气条件下进行碳热氮化处理后得到氮化锆(ZrN)纳米粉体。结合热重/差式扫描量热分析(TGA/DSC)、X射线衍射(XRD)、扫描电子显微镜(SEM)和透射电子显微镜(TEM)等手段,对内凝胶前驱体的热处理行为、所得产物的物相组成、微观形貌及显微结构等进行了表征。研究结果表明,氮化温度的升高有利于氮化程度的提高,1400℃氮化温度下可得到纯相纳米ZrN粉体;此外,碳的引入在热处理过程中起到了必要的还原作用,且碳的加入量需要适当,C/Zr摩尔比接近2是获得纯相ZrN粉体产物较为合适的条件。     

外延GaN基薄膜表面晶体结构RHEED图像研究

论述了反射高能电子衍射(RHEED)作为外延薄膜进行原位监测的一个重要手段以及RHEED图像与外延薄膜的表面形貌的关系,提出了以RHEED图像分析外延GaN基薄膜晶格结构的演变情况,并从衬底α-Al2O3的等离子体清洗、氮化进行了具体的分析和演算.结论指出,RHEED不仅是进行外延薄膜原位监测,而且还可以作为分析外延薄膜晶体结构演变的一个有力手段.     

Study on rapid nitridation process of molten silicon by thermogravimetry and in situ Raman spectroscopy

The melt of silicon, hindering nitridation for its agglomeration, should be avoided in the direct nitridation of silicon to synthesize silicon nitride powders, although liquid phase facilitates nitridation. Therefore, we proposed a method to nitride molten silicon without agglomeration. Thermogravimetric and in situ Raman studies on the nitridation process of molten silicon were performed. The as-prepared silicon nitride samples were found to be micron clusters composed of submicron grains with high α-Si₃N₄ content. The nitridation of molten silicon at 1500°C was completed after 500 s and 109 times faster than the nitridation of solid silicon at 1350°C. β-Si₃N₄ is produced dominantly by α–β-phase transition. Less nitridation time and low temperature can decrease the β-Si₃N₄ content. The rapid nitridation was owning to core–shell structure Si@Si₃N₄, which was formed after the initial nitridation of silicon particles and hindered the agglomeration of molten silicon.     

溶胶-凝胶法辅助碳热还原氮化反应制备CeN粉末

以柠檬酸（CA）为螯合剂,即以有机物为碳源,通过溶胶-凝胶法辅助碳热还原氮化反应制备了CeN粉末。整个反应过程分为水相过程和热处理过程。水相过程主要是Ce³⁺和CA的螯合和聚酯,形成稳定的Ce³⁺-CA螯合物前驱体。通过水相过程实现Ce源与C源在分子水平上的均匀混合。热处理过程包括原位碳化和碳热还原氮化反应两部分。原位碳化过程形成的CeO₂/C粉末促进了CeO₂和C之间的紧密接触,从而减少Ce源和C源原子的扩散距离,以促进碳热还原氮化过程。     

Fast,Scalable Synthesis of Micronized Ge3N4@C with a High Tap Density for Excellent Lithium Storage

Nanostructuring has significantly contributed to alleviating the huge volume expansion problem of the Ge anodes. However, the practical use of nanostructured Ge anodes has been hindered due to several problems including a low tap density, poor scalability, and severe side reactions. Therefore, micrometer-sized Ge is desirable for practical use of Ge-based anode materials. Here, micronized Ge₃N₄ with a high tap density of 1.1 mg cm⁻² has been successfully developed via a scalable wet oxidation and a subsequent nitridation process of commercially available micrometer-sized Ge as the starting material. The micronized Ge₃N₄ shows much-suppressed volume expansion compared to micrometer-sized Ge. After the carbon coating process, a thin carbon layer (≈3 nm) is uniformly coated on the micronized Ge₃N₄, which significantly improves electrical conductivity. As a result, micronized Ge₃N₄@C shows high reversible capacity of 924 mAh g⁻¹ (2.1 mAh cm⁻²) with high mass loading of 3.5 mg cm⁻² and retains 91% of initial capacity after 300 cycles at a rate of 0.5 C. Additionally, the effectiveness of Ge₃N₄@C as practical anodes is comprehensively demonstrated for the full cell, showing stable cycle retention and especially excellent rate capability, retaining 47% of its initial capacity at 0.2 C for 12 min discharge/charge condition.