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liu355

金虫 (小有名气)

[求助] 纳米合金的合成

按照文献Low-temperature solution synthesis of the non-equilibrium ordered intermetallic compounds Au3Fe, Au3Co, and Au3Ni as nanocrystals做Au3Ni纳米合金,详细步骤是The synthesis was modified from a procedure published by Zhou
et al. 8 In a typical reaction, HAuCl 4 · 3H 2 O (10.0 mg), oleylamine
(50 μL), and the appropriate amount of Fe(acac) 3 , Co(acac) 2 , or
Ni(acac) 2 to yield a 3:1 molar ratio were added to 5 mL of octyl
ether and heated to 80 °C under Ar. Then, 0.7 mL of 2.81 M
n-butyllithium was added quickly via syringe to 10 mL of octyl
ether, also at 80 °C and under Ar. Finally, the 5-mL octyl ether
metal salt solution at 80 °C was added quickly via syringe. The
reaction mixture was heated to 250 °C, the heat was turned off,
and the sample was cooled to room temperature. The product was
isolated by adding 10 mL of ethanol, centrifuging at 13 krpm, then
extracting into the toluene layer of a toluene/water mixture.
药品的量是按照Au:Ni=3:1的量加的,但是做出来Ni的量不够,差不多是Au:Ni=9:1了,请问这个问题要怎么解决。我用的时间是2h,250度。
元素        线类型        表观浓度        k 比值        wt%        wt% Sigma        标准样品标签        厂家标准        标准样品标定日期
Ni        L线系        5.12        0.05119        2.10        0.96        Ni        是       
Au        M线系        206.42        2.06422        97.90        0.96        Au        是       
总量:                                100.00
纳米合金的合成
clip_image002.jpg
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gxytju2008

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【答案】应助回帖

引用回帖:
5楼: Originally posted by liu355 at 2013-10-25 08:54:45
粉末的纳米粒子会不会团聚呀?我一般做出来都分散在甲苯溶剂里面。还有就是我的样做出来达不到比例怎么办呀它要么就Ni少了,要么就是没有Ni,全是金。...

团聚不团聚对元素分析也没影响的,测的是宏观含量

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6楼2013-10-25 09:44:04
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gxytju2008

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【答案】应助回帖

感谢参与,应助指数 +1
你用EDS算的比例么
2楼2013-10-24 20:51:16
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liu355

金虫 (小有名气)

引用回帖:
2楼: Originally posted by gxytju2008 at 2013-10-24 20:51:16
你用EDS算的比例么

嗯,用重量比换算成摩尔比,是不是有问题呀?
3楼2013-10-24 21:21:01
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gxytju2008

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引用回帖:
3楼: Originally posted by liu355 at 2013-10-24 21:21:01
嗯,用重量比换算成摩尔比,是不是有问题呀?...

这个定量很不准的,如果你做的是粉末建议你测下XRF元素分析,或者XPS都比这个准
4楼2013-10-24 22:00:26
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