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[交流]
求教上转换NaGdF4纳米棒的合成细节已有3人参与
最近一直在做NaGdF4纳米棒,但是拍出的TEM形貌非常不好,成型不好,不均一。不知道自己的方法是不是有问题。
反应环境就是 1.2gNaOH+8ml乙醇+20ml油酸
反应物是 1mmol稀土硝酸化物+8mmolNaF
我做的是Gd:Yb:Tm= 70:30:0.5
我的添加顺序是NaOH,乙醇,油酸在大力搅拌下,依次加到烧杯中。
油酸加入的时候,皂化特别严重,但是搅拌个二十分钟,基本溶液就澄清了,但是是淡黄色的。
再下来,先添加稀土硝酸化物的水溶液,每添加进烧杯一些,溶液就会出现乳白色的浑浊装,搅拌下整体过一会儿会变乳白色。
加入NaF时,溶液会变得更加的白。长久搅拌后,溶液会非常浓稠,像浓稠的洗衣液,不过没有那么多气泡。
搅拌完后,放入50ml反应釜中,190度下加热24h。
总觉得自己的反应情况很奇怪,不知道有没有做过这个方法的童鞋,帮忙指点一下。
我主要是想问,是不是由于稀土硝酸化物和NaF溶液中的水太多,导致反应状态变化,有没有可能用别的溶剂来溶解这两种物质。
原文方法
In a typical synthesis, 1.2 g of
NaOH was dissolved in 2 mL of deionized water and then 8 mL
of ethanol and 20 mL of oleic acid were added under vigorously
stirring to form a transparent homogeneous solution. After
stirring for 20 min, 1 mmol (total amounts) of Ln(NO3)3
(Ln = Gd, Yb, Er, Tm, and Ho) with designed compositions was
added to the solution under vigorous stirring. An 8 mL portion of
NaF (1.0 M) aqueous solution was then added, and the resulting
mixture was stirred for another 30 min. Finally, the resulting
solution was transferred into a 50 mL stainless Teflon-lined
autoclave, sealed, and kept at 190 C for 24 h. After reaction, the
system was cooled to room temperature naturally and the
products were deposited at the bottom of the vessel. The asprepared
samples were separated by centrifugation and washed
with ethanol and deionized water several times to remove oleic
acid and other remnants and then dried in air at 60 C for 12 h.
Undoped NaGdF4 nanocrystals were synthesized by using the
same method at 190 C for 24 h.
这是我的产物的TEM图
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这是原文的TEM图
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