--- tags: Sb, XPS, Mg, Antimony, Magnesium --- Mg insertion into Sb layers =========================== ## Sb depostion in literature ![](https://i.imgur.com/BLUt6Jk.png) ### XPS The 3d XP spectra of Sb is undergoing plasmon loss features that were already described in literature [pollak1974]: ![](https://i.imgur.com/QLBQDVD.png) ## My results * To deposit Sb on the Au Crystall of the UHV holder, I found out that the deposition is only working if the Au surface is prior to the experiment roughend. * Discussion with Mr. B: suprising result, since it looks as if the deposition is diffusion limited. Hypothises of faster diffusion o a surface then in the bulk, that was also reported some time ago by Hubbard et al. * My results are not in agrrement with the bulk Sb depostion of Da an Zan (on a single crystall). **Typical CV (19.07.2019):** ![](https://i.imgur.com/811yZl9.png) ### XPS analysis of the deposited Sb layers * Sb depostion for $t=90$ min to get a Sb layer with a neglegible Au signal in spectra. * a series of spectra is recordes after sputtering **Survey spectra:** ![](https://i.imgur.com/Ex4sGjd.png) * 50 eV resolution * spectra only shows the Au, Sb, C and O contribution * After 90 min sputtering in total, the AU surface becomes clearly visble. **high resolution Sb/O region (15 eV CAE):** ![](https://i.imgur.com/UVNZ0OQ.png) ![](https://i.imgur.com/9gycPZ4.png) ![](https://i.imgur.com/8u5w6eZ.png) ![](https://i.imgur.com/ufj8Y7j.png) * deconvolution of the spectra is chellenging due to: * X-ray satelittes of the non monochomatic Mg source ($\alpha_3$, displacement 8.4 eV I=8% and $\alpha_4$ , displacement 10.1 eV I=4.1%) * humb after the peaks -> plasmon loss see [pollak1974] * the following was considerered for the deconvolution of the Sb/O region: * 3d intensity ratios of the Sb peaks (3:2) * Area of O to fulfill chemcial structure of Sb2O3 * Same G : L ratio for all peaks * Same FWHM for same chemical nature * Duiring sputtering the Sb(0) amount is increasing and the Sb(+III) ratio decreasing. * After 90 min sputtering there is still some Sb(+III) left * This could also be an artfact out of diffrent sputtering rates for the diffent materials * Sb(+III) is likley to be formed duiring air contact. Da Xings old measurements show, that the m.p.e. value of Sb formation. * general idea: QMB experiment in which the m.p.e. value for the dissolution is measured after a certain time of air contact of the deposited Sb film. **Atomic percenteges:** | sputter time / min | Sb(0) | Sb(III) | | -------- | -------- | -------- | | 0 | 37.32 | 62.68 | | 15 | 49.47 | 50.26 | | 60 | 53.88 | 46.12 | | 90 | 74.65 | 25.35 | **Maybe the spectra need a new analysis due to the peak postion of the O1s signal. My evalutation: 530 eV, Literature: 531.5 eV** ### Measuring the amount of formed Sb(+III) in Potential step experiments **General idea:** Sb(+III) will not contibute to the charge duiring the Sb desolution. The ratio between deposition and desolution charge is investigated after different electrode treatments: ![](https://i.imgur.com/7TXVLRs.png) **Results of the desolution process (normalized to the deposition charge):** ![](https://i.imgur.com/4DsnzMf.png) **Results in a table:** ![](https://i.imgur.com/JwUe1mR.png) ### XPS analysis of the Mg deposition into Sb layers #### CV in glovebox ![](https://i.imgur.com/h2IzfbM.png) - Potential jump after two cycles ![](https://i.imgur.com/s48qVLv.png) #### XP Spectra ![survey](https://i.imgur.com/43JHpKY.jpg) ![Mg](https://i.imgur.com/KKf8ObL.jpg) ![Al](https://i.imgur.com/q1iOUJW.jpg) ![Cl](https://i.imgur.com/0PZc5ws.jpg) ![C](https://i.imgur.com/Jt5yrlZ.jpg) ![Sb_O](https://i.imgur.com/A702hpc.jpg) # Open questions * diffrence between single crystall bulk deposition and my deposition. Why do I need a rough surface? * Where is the Sb(+III) coming from? Can we show in an QMB measurement, that it is formed duiring air contact? * Another way to show, that Sb(+III) is formed after Air contact colud be, just to measure the depostion/desolution current after air contact. * O1s peak position in the deconvolution ### Literature [pollak1974] Journal of ELectron Spectroscopy and Related Phenomena, 3 (1974) 381-398!