Reduction and re-oxidation of TiO₂

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)](http://en.wikipedia.org/wiki/Temperature-programmed_reduction) followed by a temperature-programmed oxidation (TPO). In this case I think this old book can help: [Temperature-programmed Reduction for Solid Materials Characterization](http://books.google.it/books?id=n03ZL1U0BbQC&dq=TPR+Temperature-programmable+reduction&hl=it&source=gbs_book_similarbooks). 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](http://etd.fcla.edu/CF/CFE0001432/QIU_SHIPENG_200612_MS.pdf) can be helpful to understand all the variables.


 1