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湿化学法制备锗材料的研究

发布时间:2018-07-22 21:22
【摘要】: 金属Ge材料的制备研究近年来在国内外受到广泛关注,其中包括纳微尺度Ge粒子、纤维和薄膜材料。本论文通过研究六方晶型GeO2粉末与氨水的化学反应,合成出了高浓度、高稳定性的锗酸根离子前驱液。使用还原剂。NaBH4,在室温下还原此锗酸根离子前驱液,合成出了纳微尺度Ge纳米材料,并对各类材料的微观形貌、结构和生长机制进行了研究。 通过改变NaBH4与GeO2的比例在相同条件下进行反应,在比例为4-6时获得了结晶性较好的Ge材料。通过不同反应时间和烘干温度条件下的实验发现制得结晶性较好Ge材料的反应时间为12小时以上,烘干温度为120℃。研究发现制备Ge纳米材料的最佳工艺条件为:前驱液中Ge02的浓度为3%。NaBH4/GeO2摩尔比为5,还原时间24小时,120℃烘干。NaBH4还原锗酸根离子前驱液12小时得到的Ge粒子为球型(20-50 nm),24小时为蠕虫状。粒子此形状的变化符合奥斯瓦尔德熟化机制。 以NaBI-14还原锗氨溶液所得氢化的Ge溶胶为原料,通过干燥和蒸镀可以得到致密Ge薄膜材料。薄膜由直径在100纳米左右的粒子组成。随着蒸发温度的升高,致密Ge薄膜中粒子的结晶性随之提高,薄膜厚度增加。Ge薄膜的拉曼光谱在300 cm-1左右有一个尖锐的峰,对应着晶态Ge的,在265-270 cm-1左右有一个强度较弱的峰,对应着非晶态的Ge,随着蒸镀温度的升高非晶峰逐渐消失,与XRD结果相一致。Ge薄膜材料由325nm波长激发产生的发光峰主要集中在693nm到835 nm之间,峰的最高点位于753 nm左右。Ge薄膜的拉曼和荧光性质与纯Ge单晶不同,是由Ge薄膜生长时形成的缺陷和晶格内应力效应引起的。我们所制备的Ge薄膜为p型半导体,空穴浓度的数量级为1023cm-3,迁移率为60cm2.V-1.s-1。
[Abstract]:In recent years, the preparation of metallic GE materials has attracted extensive attention at home and abroad, including nanoscale GE particles, fibers and thin film materials. In this paper, a high concentration and high stability precursor solution of germanate ion was synthesized by studying the chemical reaction between hexagonal GeO2 powder and ammonia water. Nanoscale GE nanomaterials were synthesized by reducing this germanate ion precursor at room temperature using reductant. NaBH4. The microstructure, microstructure and growth mechanism of various materials were studied. By changing the ratio of NaBH4 to GeO2 under the same conditions, a good crystallinity GE material was obtained when the ratio of NaBH4 to GeO2 was 4-6. Through the experiments under different reaction time and drying temperature, it was found that the crystallization time of GE was more than 12 hours and the drying temperature was 120 鈩,

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