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bagboo

捐助贵宾 (小有名气)

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[交流] 【求助】请教EDX的问题，谁还有办法，我让版主转金币

我做了一个4-6微米的ZnO小球，在上面担载的1.6at%的Ag,审稿人对我的EDX表征提出一下观点：
As to SEM and EDS analysis, there are following errors:
a.) I thiank that the EDS results (Figure 2e and 2f) （注：图２ｅ是ＥＤＸ谱峰，２ｆ是Ａｇ的elementa mapping scanl）are not trusty, because the signal of noise is much higher than that of Ag species. If the authers do the same analysis of other elements (i.g., Au) with the x-ray nenery in the range of 2-7 keV, they will get many similar pictures as shown in Figure 2f. But as we kown, there is no Au in the sample, and the signal results from noise. And I believe that it is difficult to get Ag signal at present content because the surface of Ag/ZnO microspheres is curve not flat (the diameter of microspheres is about 2 micrometers), most of signals can not be dectected due to the position of detector.
b.) EDS can not give the information about Ag nanoparticle locating on the suface or not. Because the electron beam can penetrate several micrometers of sample, which depends on the accerating voltage.
So the conclusions from these two images should be not correct. For example, the sentence of “The precise compositions of the microspheres were confirmed by employing a highly sensitive, energy-dispersive X-ray analyzer (EDX) coupled to the FESEM instrument” (page 9, line 47-48) is incorrect. And the author should also provide the Ag content calculated from EDS.

我翻译了一下
关于EDX的问题：
审稿人的问题有两点；
1. 说我们的EDX关于Ag的表征是不可靠的，由于含量太低，Ag的信号淹没在背景峰之中了，并且这个审稿人确信由于微球的表面是曲面不是平的，所以对Ag来说很难检测到EDX信号。
2. 他是不是说由于EDX表征可以穿透几个微米，所以即使有Ag的信号，也不能说明Ag是在ZnO的表面。

不知道他说的有没有道理，如果有道理，我们怎样回答？还要换作其他的表征手段吗？HAADF（高角环形暗场像）可以吗？这么大的颗粒（４-６微米）可以吗？Ａｇ和ＺｎＯ的反差够大吗？

谢谢

谢谢！

[ Last edited by bagboo on 2008-6-10 at 14:28 ]

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