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[求助]
合成高指數(shù)晶面納米鈀,怎么都沒有文獻里面的現(xiàn)象,請教大神哪里出了問題? 已有1人參與
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想合成高指數(shù)晶面的納米Pd,參考了兩篇文獻,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.還有Sreedhala, S.; Sudheeshkumar, V.; Vinod, C. P., CO oxidation on large high-index faceted Pd nanostructures. Journal of Catalysis 2016, 337, 138-144. 按照上面的制備方法,制備Pd nanocubes,怎么都沒有文獻上面說的溶液逐漸變黑的現(xiàn)象。其中制備過程如下: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,作者發(fā)了兩篇文章,表征都做得比較全,應(yīng)該不存在做不出來的情況。有沒有大神能幫幫忙。重復(fù)了N次了,溶液顏色根本就沒有變化。是不是CTAB加得太多了,還是AA加少了。@dut_ameng@xiejf@nowitzki_ci@神魔流轉(zhuǎn)@yswyx@wulishi8 |
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CTAB水溶性不好,我都是加熱溶解之后才開始做的,文獻里面說整個合成過程是常溫。我感覺CTAB濃度有點過高,是不是把鈀都包裹住了,不容易形成長大的納米鈀,做電鏡都是顆粒尺寸很小的納米鈀。難道文獻里面的濃度過高,需要自己再調(diào)低濃度。按道理作者發(fā)了兩篇文章,應(yīng)該沒必要在制備過程有貓膩吧。 發(fā)自小木蟲IOS客戶端 |
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