While quenching an ampoule containing Se, Ag and Bi in an electric furnace the material comes out of the ampoule from its walls, neither the ampoule gets burst nor the material is coming from the sealed neck. We also have taken care of gradual increase in temperature.
How much material is escaping? How do you determine material is escaping?
What is the composition of the ampoule?
Is the ampoule sealed prior to the heat treatment you call quenching?
What is the heat treatment temperature profile?
How have you taken care of the gradual increase in temperature?
Have you considered the furnace as a source?
You have to check two things the pressure and enough time in the furnace after being reached the right temperature gradually
Dear Dr. Joseph
We had 5 gm of sample in a quartz tube, which was sealed properly before quenching. The temperature was increased at a rate of 5-6°C per minute manually, in the increasing order of melting point of each constituent elements.
Thanks Dr. Fouad
The materials were kept about 10 hrs in an electric furnace. And can you please elaborate the role of pressure inside the furnace while giving heat treatment. Our furnace is open one.
Have a good day...
Yours,
......sksharma
Dear Dr. Suresh Sharma
How are you Dear?
Try to repeat the preparation process again and you should to use quartz ampules of high quality, adjusting their vacuum and the let them within the furnace more time (at least, let them 6 hours after you reach to the maximum temperature).
But as you described, this matter leads to the exclamation and astonishment. It is a confused matter. I have previous experience in quenching of many alloys, but I have never had such this issue. The used ampoules may be broken or explode if they are of low quality, but how does the material come out from the walls.
Good Luck
How much is outside the ampoule?
Try heating a clean, empty ampoule. Most likely the source is the furnace.
Thanks Dr. Hassanien,
I am absolutely fine and expecting the same for you.
Don't know why but things are happening the same as they are given above. Yes the quality of ampoule's material may be an issue. But earlier we have done successful quenching with the same ampoules.
yours,
.....sksharma
My dear friend Suresh Sharma,
The three factors should be adjusted simultaneously. In your last attempt may be the vacuum and the time period have been accurately adjusted. Practically, there are some personal errors which may lead to unexpected but misleading results.
I hope for you all the success.
Yours,
Ahmed S. Hassanien
Sure Dr. Hassanien,
Definitely I'll go through the vacuum profile of the ampoules.
Yours,
....sksharma
Thanks Dr. Joseph,
The material has come out in the form of droplets and the water used for quenching has been filled inside the ampoule. The water has become locked along with materials inside the ampoule. This is strange that the quenching water is permanently locked inside the ampoule.
Yours,
....sksharma
Dr. Hassnaien
The materials were kept inside the furnace for about 7 hrs after reaching the maximum required temperature.
Yours,
....sksharma
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