Sort of Synthesising

Hello,

On Thursday, the view of my day was mainly this:

This is the view from my desk in Diamond. As you can see, I'm actually in the Synchrotron building itself, with the walkway outside. From there, you can look down onto the beamline control and hutches or across at the slabs of concrete that provide the shielding around the main beam circuit (see below). Some days, you can even watch the built-in crane lift the slabs as engineers get underneath.
 
I was mainly researching Thursday, checking phase patterns and the absorption of my superconductor if it was put in the beamline - too absorbing and there's little point in placing it in the beamline as there wouldn't be a diffraction pattern. However, I also had two training sessions so I can use all types of fire extinguishers and the library at Harwell campus. So, all pretty useful skills.

Friday, though, I was back in the lab, actually synthesising superconductor. Or at least trying too.

Using the balance was a skill in itself, especially since I'm trying to measure quantities to three decimal places. The gusts in the fume cabinet have a large effect at this level of precision. The scales have their own doors to exclude the draught.

I then grind the salts together into a powder... which is where it started to go a bit wrong. I mentioned that Yttrium Nitrate and Copper Nitrate absorbs water in the air. Well, soon I had a paste instead of a powder. Trying to make this into an even colour is more challenging and so it took more mixing than expected. But at least it was a very nice blue.

It then went in the tube furnace at 850 degrees Celsius with the oxygen cylinder hooked up. And it stayed there for almost a whole minute.

By then, it was bubbling and spitting everywhere. It was quickly pulled out before any real damage was down. Disappointing, but part of science; things rarely go to plan, but that's how things are discovered.

In light of this, we've (my supervisor and I) have decided to change the starting materials. I'm now going to try Yttrium Oxide, Barium Carbonate and Copper Oxide. 

Above the beamline. Everything yellow contains lead shielding.

The Oxides hadn't arrived by Monday, but that didn't mean the day went to waste. I spent the morning filling two 0.3 mm capillaries with Barium Nitrate and Barium Carbonate. Because I'm now in a place which has a lot of Barium Carbonate sitting around. As can happen. This is purely for interest's sake, but obtaining results from anything I've made on the beamline would be pretty awesome. And now...

Capillary 4  Ros 4

It would appear practice does make... a draw at least.

The afternoon I decided to get a head-start on the new synthesis process by measuring out all the Barium Carbonate. At the end of the day, I left 11 glass vials of BaCO3 sitting on the side, ready and waiting. And the scales only played up once! (they autocalibrated).

Type soon!