I did my thesis about nanoparticle and I synthesized my work. My XRD shows that I have copper in my product but there still is some noise that I am sure about. How can I check this with a simple method?
Did you try XPS? The chemical shift is sensitive to the state of oxidation.
X-ray absorption spectroscopy may tell you whether there is something else apart from Cu(0) in your sample. You have to look at the Cu-K edge for that.
You can also try EDX analysis which gives elemental composition of your product.
Go for XPS to check that. I agree with Sir. Banhegyi as you can confirm from the oxidation state. You can also do UV-vis. absorption spectrum analysis and see if you find any peak corresponding to CuO/Cu2O to strengthen your claim. FTIR might also be suitable to find some peaks corresponding to metal or metal oxides.
Good luck!
I also agree with Sir Nagapradeep about EDS to give the compositional analysis but I"m afraid it won't help you that much in finding whether you have Cu(0) or some oxides of it in particular.
first you should notice that from the appearance of Cupric Oxide more darker to black than reddish-brown color of pure copper, then the EDS or XRF will do the job
Hi Nana
If you have enough powder quantity, you can measure the powder density using Helium Picnometry. It is a very simple technique and gives you density typically better than 1/1000.
Density value can give you a good hint of what you have.
TEM can also help, since you can try to determine cell parameters.
I understand from your question formation of Cu / CuO is in trace level. Chemical methods will not help as the conc. is very less. PXRD is the right tool; use the characteristic peak to identify the compound. You can also try with XRF.
If you have peaks in XRD that you are not able to index to any phase, you can try the following things to try to find the correct assignment to them:
1) use a software for phase identification, if possible with an 'complete' database, pdf, cod, icsd
2) try to select only the peak you are missing and run the search on the peaks, using chemical limits defined either by the products used in your synthesis process, or from a chemical analysis.
4) if your peaks are too low to clearly distinguish them from the background noise, you can increase acquisition time, and limit the scan range to the locations of the peaks.
In general with XRD, one can identify phases which are present at a level of a few percents and bellow.
If then you have some potentially identified phases but still some doubts, Rietveld refinement of the spectrum can help you confirm which phase you have.
One thing that can sometimes happen, depending on how you prepare your sample and setup the scan is that you get some peaks from the sample holder, if it is a possibility you can perform another scan without powder to check if it can be the case. Another issue can be sample misalignment from the diffraction plane, this will shift the peaks and often bug the phase identification process.
UV-Vis reflectance spectroscopy is simple and will tell you is you have an oxide on the surface and which oxide has been formed.
Article Differential Reflectance Spectroscopy in Analysis of Surfaces
Yes UV/Vis spectroscopy can be used for detecting the oxide on the surface of Cu. UV/Vis will also be able to tell you whether you also have free copper. See: http://physics.nist.gov/PhysRefData/ASD/lines_form.html
for atomic lines of copper. Do not use XRF, it will only give you the total amount of copper.
EDS and XPS (X-ray Photoelectron Spectroscopy) analysis can help you.
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