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Synthetic Routes And Formation Mechanisms Of Spherical Boron Nitride Nanoparticles

机译：球形氮化硼纳米粒子的合成途径和形成机理

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摘要

A new concept is proposed to explain the formation of spherical boron nitride (BN) nanoparticles synthesized by the chemical vapor deposition (CVD) reaction of trimethoxyborane (B(OMe)_3) with ammonia. The intermediate phases formed during the CVD under differeat reaction conditions are analyzed by X-ray diffraction, electron microscopy, thermogravimetry, and spectroscopy techniques. The transition mechanism from an intermediate B(OMe)_(3-x)H_(3-x)N (x < 2) phase having single B-N bonds to the BN nanoparticles is elucidated. This particularly emphasizes the CVD temperature effect governing the conversion of the N-H...O-B hydrogen bonds in (OMe)_3B · NH_3 into the N-B bonds in B(OMe)_(3-x)H_(3-x)N. The spherical morphology strongly depends on the remnant impurity oxygen formed upon Me_2O group elimination in the intermediate. Two types of spherical BN nanoparticles primarily attractive for immediate commercialization (with C and H impurities at a level less than 1 wt %) are synthesized by the adjustment of experimental parameters: high oxygen-containing (～6.3 wt %) BN spheres with a diameter of ～90 nm and a specific surface area of 26.8 m~2 g~(-1); and low oxygen-containing (< 1 wt %) BN spheres with a diameter of ～30nm and a surface area of 52.7 m~2 g~(-1). Finally, the regarded synthetic techniques are fully optimized in the present work.
机译：提出了一种新的概念来解释通过三甲氧基硼烷（B（OMe）_3）与氨的化学气相沉积（CVD）反应合成的球形氮化硼（BN）纳米颗粒的形成。通过X射线衍射，电子显微镜，热重分析和光谱技术分析在不同反应条件下在CVD期间形成的中间相。阐明了从具有单B-N键的中间B（OMe）_（3-x）H_（3-x）N（x <2）相过渡到BN纳米粒子的机制。这特别强调了控制（OMe）_3B·NH_3中的N-H ... O-B氢键到B（OMe）_（3-x）H_（3-x）N中的N-B键的转换的CVD温度效应。球形形态很大程度上取决于在中间体中消除Me_2O基后形成的残留杂质氧。通过调整实验参数，合成了两种主要对立即商业化具有吸引力的球形BN纳米颗粒（C和H杂质含量均小于1 wt％）：高含氧（〜6.3 wt％）直径的BN球形〜90nm，比表面积26.8m〜2g〜（-1）；直径约30nm，表面积52.7 m〜2 g〜（-1）的低氧BN球（<1 wt％）。最后，在目前的工作中对所考虑的合成技术进​​行了充分优化。

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