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Native oxide and hydroxides and their implications for bulk AlN crystal growth

机译:天然氧化物和氢氧化物及其对整体AlN晶体生长的影响

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Oxygen degrades the properties of AlN, thus producing bulk single crystals with low oxygen concentrations is an important goal. Most of the oxygen in bulk AlN single crystals grown by the sublimation-recondensation method originates from the hydroxides and oxides that spontaneously form on the surfaces of the AlN source powder. For a typical AlN powder with an average particle size of 1-2 μm, a l-3 nm thick oxide and/or hydroxide can account for most of its oxygen (generally in the order of 1.0 wt%) and hydrogen (200-300 ppm). Heating the AlN powder source at 1950 ℃ for 10 h in a nitrogen atmosphere reduced its surface area by a factor of 160 (due to sintering), the oxygen concentration by 16 and the hydrogen concentration by 67. The difference in these reduction factors suggests some of the oxygen is dissolved into the bulk AlN with this heat treatment. Firstly annealing the AlN powder at a low temperature (950-1000 ℃) for several hours before sintering at 1950 ℃, the oxygen and hydrogen concentrations were reduced to lower levels. The low-temperature treatment is effective in eliminating oxygen and hydrogen from the surface of the powder, while high-temperature sintering reduces the specific surface area of the source. The combination of heat treatments produced a source with oxygen and hydrogen concentrations as low as 0.015 wt% O (1.9 × 10~(19) atoms O cm~(-3)) and 1.7 ppm H (3.4 × 10~(18) atoms H cm~(-3)). Annealing becomes less effective at removing oxygen and hydrogen with longer heat treatments, suggesting there is a minimum oxygen concentration that can be produced by this method.
机译:氧气会降低AlN的性能,因此生产具有低氧气浓度的块状单晶是一个重要的目标。通过升华-再凝结法生长的块状AlN单晶中的大多数氧气源自自发形成在AlN源粉末表面的氢氧化物和氧化物。对于平均粒径为1-2μm的典型AlN粉末,厚度为1-3 nm的氧化物和/或氢氧化物可占其大部分氧气(通常为1.0 wt%)和氢气(200-300) ppm)。在氮气气氛中将AlN粉末源在1950℃加热10小时,其表面积减少了160倍(由于烧结),氧气浓度减少了16倍,氢气浓度减少了67倍。通过该热处理,氧的一部分溶解到本体AlN中。首先在950-1000℃的低温(950-1000℃)下退火AlN粉末数小时,然后在1950℃进行烧结,氧和氢的浓度降低到较低的水平。低温处理有效地消除了粉末表面的氧气和氢气,而高温烧结则减少了光源的比表面积。热处理的组合产生的氧和氢浓度低至0.015 wt%O(1.9×10〜(19)原子O cm〜(-3))和1.7 ppm H(3.4×10〜(18)原子) H cm〜(-3))。退火在较长时间的热处理中去除氧气和氢气的效率降低,这表明通过此方法可以产生的氧气浓度最低。

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