I am synthesizing zirconium based ceramics via high energy ball milling.
I cannot seem to find a chemical company willing to ship zirconium powder packaged in argon. I have a positive pressure argon glovebox to handle the powders in; however, the zirconium powder offered is packaged in water.
Do you know of a way to dry the zirconium powder without compromising the glovebox or oxidizing the zirconium?
I have thought of using dense non-aqueous phase liquid extraction or solvent exchange. I do have a furnace which operates under a nitrogen atmosphere; however, transferring the dry zirconium powder will expose the powder to oxygen in the lab atmosphere.
Hi, Cody.
That is a tricky question. Could you evacuate the glove box, wait for the water to evaporate, then refill it with Ar?
Be safe.
-Jon
Olá Cody,
My suggestion (for me worked): with the powder in water, in a vacuum desiccator in the glove box, the vacuum was applied through a gas port of the glove box (caution with the gas flux). After dried the desiccator was opened in the argon atmosphere, the powder transferred to another flask and reserved in the glove box for use.
Hi Cody, I support the Tomasi's answer. Caution with risk of depression in the box would you have a leak in the vacuum line.
Rinse down with alcohol and then blow dry in the inert gas filled glove box
I have been drying Zirconium powder for years. Here is how you do it. Hook up a tee to your vacuum exhaust port. Place an argon cylinder with a flow meter and regulator teed into the port with a shut off valve.
Put the wet zirconium in a shallow stainless steel drying tray The amount you dry depends on the size of the oven. I have never had a need to dry more than 200 grams
Turn on the over and pull about 25 inches of vacuum.
Set the temperature at around 180 Deg. F.
Dry the Zirconium for 4 to 5 hours
Turn off the oven and continue to pull vacuum for another 1/2 to 1 hour.
Set the argon flow meter to around 10 scfm.
Make sure the line is purged and there is no air in it (just argon).
Slowly open the argon valve and suck the argon into the oven ( very slowly ) no more than 10 " WC pressure of argon in oven.
Allow the oven to cool to room temperature.
Slowly vent argon. Open oven door.
Remove tray place behind full body shield and use velostat or Be Cu spatula to scoop dried Zr into conductive rubber container. Use Usual Flameproof PPE and safety goggles ground everything and don't allow powder to form dust .
I have only had this stuff light off once on me in the 30 years I have handled it. .
If it does don't panic and try to put it out.. Just Put a stainless bowl or PBI blanket over the top of it and let it burn it self out Don't dry any more than you have to
Remember what you are dealing with and you will be OK . We're not talking about plutonium here, but you have to be careful with this stuff . I saw a 100 gram container of this stuff ignite and burn a hole through a stainless steel table once.
Why, you may ask ??? because it was a Tuesday !
The stuff in Question was MIL-Z-399 Cl2 type 2 Morton Ventron stock.
Just be careful
Chuck Piper
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