I'm having a hard time finding data about an experiment that I know has been done a bunch of times:

I have a sheet of single crystal rutile $\ce{TiO_{2}}$ (110) that I want to reduce to various $\ce{TiO_{2-x}}$ forms where the x is what I want to vary. I want to try to avoid conversion to the other Magnéli phases if possible $(\ce{Ti_{n}O_{2n-1}})$. To do this reduction, I have a high temp oven that I can flow with 95% $\ce{N_2}$ and 5% $\ce{H_2}$ or simply evacuate. I can set the flow rate to cubic centimeters per second. I need a chart that will tell me what temperature, flow rate, and duration I need to convert my sheets surface to a desired reduced value (i.e., I want a specific x).

I then want to reoxidize the surface by using lower temperatures in a furnace that I can fill with oxygen at different pressures. I need a chart that will tell me what temp, partial pressure of $\ce{O_2}$, and duration I need to re-Oxidize the surface.

The goal here is not to simply get the surface, but to test other properties. I was hoping this step (finding the proper charts) would have been fairly straightforward, but my literature searches haven't turned up quite what I need. I was hoping someone here can point me to a resource that has this data.


I can't post a comment, so this is not a true answer but I think can help. If I've understand what you mean you want to perform a Temperature-programmed reduction (TPR) followed by a temperature-programmed oxidation (TPO). In this case I think this old book can help: Temperature-programmed Reduction for Solid Materials Characterization. I don't know much about single crystal but I think that many things from TiO2 studies of nanomaterials can be consider valid for your case, this online book can be helpful to understand all the variables.

| improve this answer | |

Your Answer

By clicking “Post Your Answer”, you agree to our terms of service, privacy policy and cookie policy

Not the answer you're looking for? Browse other questions tagged or ask your own question.