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lkzmaster

木虫 (著名写手)

教授

[交流] 【求助】XPS 高手请忙帮

我的论文审稿意见中有这么一条In the Experimental Section, procedure for preparation of samples for XPS studies is to be described in more details. It seems that authors supported powders on double -sided scotch, which precludes any pretreatment of samples before spectra recording. In this case, the surface of samples is known to be hydroxylated, covered by carbonates and adsorbed CHx species trapped from air. Carbonates are also well known to be trapped in the bulk of high-surface-area ceria samples. Organic species trapped from air could reduce the surface even at room temperature especially during sample evacuation before measurements or under effect of the electron flood gun. All this makes difficult (if possible at all) reliable interpretation of XPS spectra in both O1s and Ce 3d ranges. Moreover, for sample studied after redox cycles, its inevitable transfer from reactor into the spectrometer through the air also affects its surface state even if it was reoxidized in the reactor before discharging (not mentioned, by the way). Hence, XPS data interpretation is certainly to be supported by experiments with sample supported on a metal holder which allows pretreatment in controlled conditions providing reproducible state of the surface.  If it is not possible for authors, I would advise just to remove this part of research from the article.
好像是说样品没有预处理,我是送样做的,对XPS的预处理知道的不多,看了半天还是不太明白这个审稿意见的意思,请XPS有经验的朋友帮忙看看。谢谢了!
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murt

木虫 (小有名气)

不是预处理的问题.
4楼2010-10-15 17:12:01
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wwy0233

铜虫 (小有名气)

lkzmaster(金币+3):非常感谢,我的样品真空常温脱气处理是做了的,这个应该不存在问题啊,我做的是含铈的复合氧化物,不知道您有没有这方面的经验? 2010-10-15 15:06:39
在XPS之前,样品首先高真空常温脱气处理。审稿人意见的意思我理解为可能是样品没处理好,表征的结果存在一定的问题,不知你这是什么类型的样品,因为有些金属或金属离子在X射线照射下,可能会发生转变之类的。
2楼2010-10-15 11:14:30
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murt

木虫 (小有名气)

lkzmaster(金币+3):谢谢,确实不是原位的XPS,审稿人这个说的太绝了吧,大多数论文中的XPS都不是原位的啊,难道都不能用吗?能不能指点一下怎么回答这个问题呢?谢谢了! 2010-10-15 20:59:01
因为你做的是非原位的XPS测试,所以审稿人会怀疑样品暴露空气会吸附OH基和有机物物的杂质并可能会对样品的状态造成影响.所以审稿人建议你去掉那部分内容,或者你有原位XPS.
3楼2010-10-15 17:10:05
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lkzmaster

木虫 (著名写手)

教授

如果审稿人的意思真如2楼朋友所说,那么非原位的XPS还有什么意义呢?
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5楼2010-10-15 21:00:13
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