I am not sure what you intend to measure at the Boron K-edge. X-ray absorption? If yes, with what detection scheme? XPS?

I don't know the material properties well, but if the material is still a good insulator, then electron yield may fail badly. It is fairly surface sensitive anyway and you will not be able to determine a depth profile.

Transmission might also be very difficult, due to the small absorption length of quasi all materials at such small energies (check Henke tables at CXRO). Again, no depth profiling, since the whole film would be measured.

XPS might give you some results, but this is a highly nontrivial task. Depth sensitivity is also small compared to your film thickness. Possible experiments include taking various measurements at different electron takeoff angles, but recovering the (correct) depth profile is numerically not well conditioned and needs extremely good handling of spectroscopic data (consult articles of S. Tougaard, for example). This is particularly true with insulators.

Using very high photon energies (several keV, available at synchrotron radiation sources) increases the probing depth, but will yield very small cross section for the light elements, unfortunately. Also, correct handling of spectroscopic data is still required.

Finally, you could go with destructive methods, such as doing series of spectroscopic measurements and sputtering off fractions of the film in between. You will need to understand the sensitivity of the film to preferential sputtering in order to understand what you'll be getting.

Alternative methods might therefore be more adequate. Examples include Rutherford backscattering (nondestructive) and mass spectroscopy techniques [e.g. SIMS] (destructive).

@ Kai Fauth

Sir,

Sorry for  not providing adequate information. The film that I am working on is conducting (~10 mohms-cm at RT). I have done some XPS measurement recently, what I observe is the following,

1. Even though B content is sufficiently high (4 at %) I did not find any signal of XPS at 189 eV. Whereas Raman measurement, resistivity measurement and Hall effect measurement supports the effective doping of B into the diamond film.

2. We observed oxygen peak 532 eV , which is not expected for the boron doped diamond films.

3 We observed the carbon peak at 284 eV.

The film that I am working on has diamond (sp3 carbon) grain size of 400 nm  surrounded by1 nm width grain boundaries (sp2 carbon).

Can you please help me know how I can rectify the above inconsistencies in my measurements?

Sincerely,

Dinesh

I would consider the transport properties to provide quite indirect evidence for the kind of doping you have produced. But aus you probably reckon, these measurements essentially probe the volume of the sample, while XPS is surface specific.

The probing depth of Raman scattering will depend on the material properties. If specific vibrational modes involving Boron are well-known and documented, it may well serve as a finger print. if on the other hand, you "only" evaluate Carbon sp2 and sp3 contribs to the Raman data, then this might again be quite indirect.

In order to find out *whether* you can detect the boron in your sample with the XPS instrument accessible to you, I'd do some simple tests along the lines I mentioned in my previous post:

a) scraping with a diamond or TiN tool to remove surface layers. Now, since your film material is actually diamond, and since you have, after all, thin film samples, I do not know, whether this simple approach is adequate.

b) Systematically sputtering off surface layers and see whether the binding energies and stoichiometry change. Do check the pertinent literature for estimates of the sputtering yield of the elements in your material and design your experiment accordingly (choice of ion energy and ion dose per step).

@ Kai

Dear Sir,

I will once again carry out the measurement, this time I'll be more careful to do the literature survey.

Sincerely,

Dinesh