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文献中合成Bi2Te3时原料BiCl3和Te的摩尔比4:8,这是为什么啊?
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| 按照分子式,摩尔配比不应该是4:6吗?文献上为什么是4:8啊(他们几篇文章都是这个配比,也没说明原因)?而且最后XRD表征是单相的Bi2Te3,请问该如何解释?谢谢! |
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2楼2013-04-22 15:34:38
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7楼2013-04-23 21:21:58
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文献在此哈: http://www.nature.com/nmat/journal/v11/n3/full/nmat3213.html 文中描述如下: Thioglycolic acid (CH2COOHSH, 95%), anhydrous bismuth chloride (BiCl3), antimony chloride (SbCl3), 1,5-pentanediol (95%), technical grade trioctylphosphine (TOP), 200-mesh tellurium shots and 100-mesh selenium shots obtained from Sigma Aldrich were used without further purification. In a typical small-scale synthesis, we added ~0.08 mmol of tellurium or selenium to 2 – 5 mL TOP and heated in the multimode 1250 W domestic microwave oven for 90 – 120 s to obtain a faint yellow TOPchalcogen complex. We added ~0.04 mmol of BiCl3 or SbCl3 to 2.5 – 10 ml of 1-5 pentanediol followed by sonication for 5 min to obtain a bismuth chloride or antimony chloride solution. The bismuth chloride solution turns yellow upon addition of 100 – 350 µL of thioglycolic acid (TGA) due to thioligated bismuth complex formation. The solutions with TOP-chalcogen and thioligated bismuth (or antimony) were mixed and exposed to microwaves for ~30-60 s in a multi-mode domestic microwave oven or a single-mode variable power 300 W CEM microwave oven equipped with the IR sensor for temperature control. 谢谢! |
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