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参水猿

铜虫 (初入文坛)

[求助] 上转换合成求助。求大神帮助!

参考的是清华张勇08年的文章:氯化钇、氯化镱,氯化铒将稀土金属氯化物在160度溶于3ml油酸和17ml十八烯溶液,搅拌半小时,然后静置到室温,获得澄清溶液,逐滴加入0.1gNaOH和0.148gNH4F的混合溶液10ml,溶液变浑浊。缓慢加热到100度,抽真空10分钟除去低沸点溶剂和水,加热到300度(升温速度每分15-20度),反应1小时。冷却至室温,乙醇沉淀后离心。
试了几次,XRD对不上;电镜照出来是单个球形,尺寸也不均匀。求大神帮忙看下步骤,有什么错误吗?谢谢!
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zhshcheng

木虫 (著名写手)

【答案】应助回帖

感谢参与,应助指数 +1
Wang F., Han Y., Lim C. S., et al. Simultaneous phase and size control of upconversion nanocrystals through lanthanide doping. Nature. 2010, 463(7284): 1061-1065.
2楼2013-09-05 08:22:31
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grurper

铜虫 (小有名气)

【答案】应助回帖

The nanoparticles synthesis developed via a modified wet chemical procedure (1). In a typical procedure to the synthesis of NaYbF4:Nd nanoparticles, 2-mL water solution of Ln(CH3CO2)3 (0.2 M, Ln = Y,Yb,Er) was added to a 50-mL flask containing 4 mL of oleic acid and 6 mL of 1-octadecene. The mixture was heated at 160 oC for 40 min to form the lanthanide-oleate complexes and then cooled down to 50 oC naturally. Thereafter, 5 mL of methanol solution containing NH4F (1.5 mmol) and NaOH (1 mmol) was added and the resultant solution was stirred for 30 min.
After the methanol was evaporated, the solution was heated to 290 oC under argon for 1 h and then cooled down to room temperature. The resulting nanoparticles were precipitated by
addition of ethanol, collected by centrifugation at 6000 rpm for 5 min, washed with ethanol several times, and re-dispersed in 4 mL of cyclohexane.
3楼2013-10-22 20:24:02
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