Out of Mortar, Into the Furnace

Hello,


The past few days have been fairly warm across my area of the UK. And, as a typical British person, I must complain about its timing. Just when I have to share a lab with a furnace.

On Tuesday, it was decided that it would be a good opportunity for me to get to know the tube furnace I'll be baking the superconductor in. As previous readers know, this experienced a minor set-back last week when my previous attempt at YBCO sort of... well... micro-exploded in there. Thus, when I came to having a go at practical trials after reading the instruction booklet, I found that the inside was covered in black, partially burnt nitrate mix. Eww...

Luckily, my beamline manager gave me a hand at clearing it out, using towels and solvents. Being nitrates, we also got to use dust masks... and I realised I've never had to use one before. Yes, I tried to put it on sideways first attempt.

The solvents needed time to dry though, so I came back to it in the afternoon and set it on a quick heating cycle. Just up to 250 degrees Celsius at 5 degrees a minutes and then hold for half an hour. This seems trivial, especially when you think some ovens can do that, but simple practice allowed me to monitor the cooldown rate too.

While this was heating, I was also able to prepare miniature glass vials of Yttrium Oxide, ready for synthesis. We're still waiting on the copper oxide.

The outside of Diamond. The large canister is filled with Liquid Nitrogen... though I don't think I'll be using all of that!

This had arrived by Wednesday, so that morning I was able to start grinding up all the salts together to create my first batch of superconductor using the Oxides. And it didn't turn to paste. Instead, it was a dusty, clay-coloured substance, which I was able to press into a mini pellets of superconductor and stick in the oven.

I was also able to make a second boat of mixture, but this one without pressing. Why? Because we're still experimenting with the process of making the superconductor; we're trying several techniques to see which works best. Science can sometimes be trial and error.

While it was cooking, I prepared two boats of salts to cook tomorrow. I also tried to make a capillary of the nitrate mix... and I tried again... well, maybe another day. *sigh* Before the end of the day, I took out the second boat of unpressed salts, reground, pelleted and replaced it. Just to see what happens.

To the left, you can see the bridge that allows access to Diamond. It is slightly like entering a spaceship, I won't lie.

I came in on Thursday to find the furnace hadn't cut out after ten hours like I thought I'd set it. I blame it on fiddling about with the settings after it had started. Never mind, I let the superconductor cool and was able to load the new boats in and set them off, this time under a flow of oxygen. And yes, I got to make pretty warning signs. I then mixed up two new boats for Friday's firing. 

Once cool, I ground up a little of the second superconductor to place in a capillary... Second attempt lucky. In between this, I was able to sneak into the beamline to watch a new experiment being set up. And I hope to learn more.

My final task was to withdraw one of the boats to regrind and pelleted before replacing. Every angle covered. Now I must hope the furnace switches off over night. Not least, because it makes the lab pretty warm. Well, I am setting it to 930 degrees C.

Type soon.