主题：【讨论】xps谱图

You cannot judge just by this narrow-spectrum. On the Nd3d peak there should be a double of 3d5 and 3d3.

If it is a metal Nd, Nd3d5 should be near 202eV BE and 3d3 at 205.2eV BE. But the peaks you have seems to be near 204eV indicating even Nd is existed it maybe in an Oxide form.
***There looks like a peak near 198eV BE too but it is almost no way for the Nd3d peak to shift to lower binding energy in Chemical form. Or unless you have some sample charging effect on your sample?

Going to next step if you want to "believe" the peak near 204eV is really  Nd3d and looking at your spectrum this "peak" have an intensity of 0.05e+4 (peak to background). Then if you want to prove what you "believe" then you can look at Nd3p which is around 360eV BE. From standard spectra checking, if Nd is really presence, then Nd3p should have an intensity about half to Nd3d. So if you can see a peak at ~360eV BE and intensity is roughly like 0.025e+4 (peak to BG) then you can double confirm it is indeed the Nd being presence.

The peaks in your spectrum are really quite small, so it is indeed difficult to judge if such an element really presence or not. But with another small peaks in what so-called the same family peaks to come up, it can be a good proof for a presence of an element.

Hope you enjoy XPS~

谢谢，我的样品是含有Nb的，我不太明白是为什么这种峰并不光滑，好像是噪音一样。

Maybe the concentration of Nb is really low. What atomic concentration % do you expect?

Usually we say XPS detection limit is 0.01 to 0.1AC%, but it also highly depending on the interested element. So we better use the higher limit meaning 0.1AC% as the line. So do you expect Nb concentration is >0.1AC%?

Like mentioned, please confirm with Nb3p peaks too. Many other factors can also affect you to really detect Nb or not, such as surface contamination on sample.

Your same is in powder or big piece of solid?
If it is powder, how do you prepare your sample?

Thank you for reply.
AC%=at.%?
我这个样品室片状的，Nb含量是0.85wt.%（0.83at%)。
我想说一下，表面污染对谱峰的影响应该是导致峰的漂移吧，但是我主要的目的并不乎这个结合能在什么，我主要关注的是我的表面是否含有这个元素，至于是什么化合价，我在其次，本来可用俄歇来测，但是学校没有俄歇，所以就把XPS当俄歇用。

yes, AC% = at.%

0.83at% should be able to detect by XPS or AES (Auger) both no problem. So still the idea is you try to confirm the Nb3p peak is there then you can confirm.

关于Nb的谱峰的位置我倒不是很关心，因为我不太注重化合价的信息，主要是想得到在表面是否有这个元素存在，我的疑问是，为什么这个谱峰的形状怪怪的，不容其他元素峰那么整齐（如图所示），而这样的一个峰到底算算峰，并且我要进行峰面积的计算，哪里才是基底？

From O1s spectra, its difficult to see if seeing Metal-Oxide. Can you look at the survey spectrum at ~361eV Binding Energy because this is where Nb3p3 peak is. And from standard spectra I just check, its intensity maybe about half of Nb3d peak.

If you can see "some" peaks there you can have more proof if Nb really detect in your sample or not.

Thank you for your reply.
我的疑问是：铌峰是肯定有的，但是我不明白为什么会以这样的峰形显示，看来是实验员操作的问题，是不是有这种可能？感觉这个铌峰右边好像不全一样，横坐标取的不够似得。

You said the presence of Nb is "CONFIRMED".

I think you said that because you 'think' your sample surely have Nb. But for me as only looking at the XPS spectra, the presence of Nb seems uncertain to me. Like you said, the peaks acquired for Nb3d seems too small. Acquiring in bigger range for Nb3d like you said can be useful, because the right-hand-side peak is in doubt what exact is it. But after all, I still would try to look at the Nb3p peaks and if I can see it, then I will say it is "CONFIRMED".

Good luck~