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[求助]
合成高指数晶面纳米钯，怎么都没有文献里面的现象，请教大神哪里出了问题? 已有1人参与
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想合成高指数晶面的纳米Pd，参考了两篇文献，Sreedhala, S.; Sudheeshkumar, V.; Vinod, C. P., Structure sensitive chemical reactivity by palladium concave nanocubes and nanoflowers synthesised by a seed mediated procedure in aqueous medium. Nanoscale 2014, 6 (13), 7496-502.还有Sreedhala, S.; Sudheeshkumar, V.; Vinod, C. P., CO oxidation on large high-index faceted Pd nanostructures. Journal of Catalysis 2016, 337, 138-144. 按照上面的制备方法，制备Pd nanocubes，怎么都没有文献上面说的溶液逐渐变黑的现象。其中制备过程如下：About 300 mg of CTAB was dissolved in 10 mL of millipore water. To this, 125 mLof 10mMH2PdCl4 solution, 10 mL of 0.01 M NaBr, and 45 mL of 0.1 M AA were added and mixed thoroughly by gentle shaking. Around 50 mL of Pd nanospheres prepared before as the seed solution was added and kept undisturbed. The solution gradually turned to black. 按道理，作者发了两篇文章，表征都做得比较全，应该不存在做不出来的情况。有没有大神能帮帮忙。重复了N次了，溶液颜色根本就没有变化。是不是CTAB加得太多了，还是AA加少了。@dut_ameng@xiejf@nowitzki_ci@神魔流转@yswyx@wulishi8 |
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7楼2017-05-19 17:42:22
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CTAB水溶性不好，我都是加热溶解之后才开始做的，文献里面说整个合成过程是常温。我感觉CTAB浓度有点过高，是不是把钯都包裹住了，不容易形成长大的纳米钯，做电镜都是颗粒尺寸很小的纳米钯。难道文献里面的浓度过高，需要自己再调低浓度。按道理作者发了两篇文章，应该没必要在制备过程有猫腻吧。 发自小木虫IOS客户端 |
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