Wednesday, November 25, 2009

Research Sucesses

So recently I actually made some pretty significant progress in my research and solved a couple of the major problems that had been hindering my progress.  This was very exciting!  Even though now I have lots and lots of work to do because I feel like I'm a bit behind after taking so long to resolve these issues, it's really good to have something new to work on.

First off: I solved my problem with my iron oxide compound.  Previously, I was having difficulties getting the synthesis product completely clean, and this was really annoying.  I now have devised a several day, multi-step process for washing away various impurities to get a clean product.  Complicated and time consuming, yes, but it works.  Here's a TEM picture!

And a close up:

(The scale bar is really small, but that dark black bar in the second picture represents 5 nm.  So, each little particle is about 10 nm across!)

See those nice lines across each particle in the second picture?  Those are actually the planes of iron and oxygen atoms, nicely arranged in the configuration I want.  These are responsible for creating the x-ray diffraction pattern below, which proves to me that this is actually the compound that I want:



Sorry it's kinda fuzzy, but basically here I'm proving to myself that I actually have about 95% magnetite, which is the iron oxide phase that I want.  The issue here is that these particles are pretty thermodynamically unstable, mostly because they are so small that they have all sorts of surface energy issues (small particles have a larger surface area/volume ratio than normal size particles, and this causes all sorts of stability problems because of strains within them).  So, they tend to transform into goethite (another iron oxide phase) if you add any small amount of heat.  You can see here that I have about 5% goethite in my sample, which is an OK level.

The other exciting research development is that I made some very nice, titanium dioxide coated, silicon dioxide spheres.  The coating procedure is really complicated, and uses a very air sensitive compound.  If the chemical is exposed to air for more than about 10 seconds at a time, it will oxidize and ruin the synthesis.  So, throughout the whole process, I am required to work with ninja-like quickness.  But, I now have these great-looking spheres:

The inner spheres are made of silicon dioxide, and the darker ring on the outside of each is titanium dioxide.  The little bits outside the spheres are rogue clumps of titanium dioxide that form when I expose the compound to air during the synthesis.  Guess my ninja skills are not perfect yet!

So now I just have to do the in-between part: coat the iron oxide with silicon dioxide.  Then, I'll just put more titanium dioxide on top of that, similar to the previous picture.  However, no one has actually done the silicon dioxide coating on iron oxide, so that part is up to me to figure out.  Should be fun!

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