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Science Forum Index » Materials Forum » HELP-Synthesis Issue
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| MSMaxwell |
 Posted: Thu Aug 21, 2003 12:47 am |
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I need to learn how to make Tb oxide. I have metallic Tb that I have
been firing @ ~(1000-1100)°C for a while to oxidze it. This is working
well, but the question is which oxide(s) I may be forming. References
say that TbO2 and Tb2O3 form. So how do I get to one or the other
(high quality) so I can use this material for massing other complex
oxides? I have a TGA and can synthesize via TGA if necessary, but if
you are familiar with this instrument you are aware that this method
is a bit time consuming. I can also do powder XRD to check relative
sample purity. However, I don't have a reference pattern/paper handy
so any help there would save me some time as well. |
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| Uncle Al |
| Posted: Thu Aug 21, 2003 8:07 am |
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MSMaxwell wrote:
Quote:
I need to learn how to make Tb oxide. I have metallic Tb that I have
been firing @ ~(1000-1100)°C for a while to oxidze it. This is working
well, but the question is which oxide(s) I may be forming. References
say that TbO2 and Tb2O3 form. So how do I get to one or the other
(high quality) so I can use this material for massing other complex
oxides? I have a TGA and can synthesize via TGA if necessary, but if
you are familiar with this instrument you are aware that this method
is a bit time consuming. I can also do powder XRD to check relative
sample purity. However, I don't have a reference pattern/paper handy
so any help there would save me some time as well.
You could look it up! I suspect the synthesis is something closer to
1) Dissolve the metal in (dilute) nitric acid.
2) Either evaporate or precipitate as the oxalate.
3) Calcine the isolated nitrate or oxalate.
The nitrate is probably a hydrated mush. Tb2O3 is most likely the
product unless you go to a forcing oxygen atmosphere. TGA will tell
you how to proceed, then you do it in bulk. Calcining the oxalate in
an oxidizing atmoshere might get you a colored mixed oxide like Tb4O7.
Inner transition elements are rather toxic, but their +3 ions are not
well absorbed orally. Don't breathe the dust.
--
Uncle Al
http://www.mazepath.com/uncleal/
(Toxic URL! Unsafe for children and most mammals)
"Quis custodiet ipsos custodes?" The Net! |
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| MSMaxwell |
| Posted: Thu Aug 21, 2003 9:39 pm |
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Guest
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<snip>
You could look it up!
<snip>
Wow. Wonder why I hadn't thought of that? It's as if my original
statement contained no clues that I had done just that. Let me
clarify. From the time I made the post, until maybe friday or
saturday, I will not have access to the literature necessary to answer
my question. I had spent hours looking for the answer via websites.
However, terbium oxide synthesis isn't exactly a popular web page
topic. Insightful journal articles are on secured sites that I do not
have access to unless I use the PC in my lab. I cannot go in to my lab
until the friday or saturday mentioned. Thus, I made my post in the
hope that someone with some experience in the matter might be able to
lend me a friendly hand, and save me some time. I will, otherwise, be
committing myself to becoming educated on the matter on my own at that
time. Though I would prefer spending that time actually DOING THE
SYNTHESIS.
<snip>
I suspect the synthesis is something closer to
1) Dissolve the metal in (dilute) nitric acid.
2) Either evaporate or precipitate as the oxalate.
3) Calcine the isolated nitrate or oxalate.
The nitrate is probably a hydrated mush. Tb2O3 is most likely the
product unless you go to a forcing oxygen atmosphere. TGA will tell
you how to proceed, then you do it in bulk. Calcining the oxalate in
an oxidizing atmosphere might get you a colored mixed oxide like
Tb4O7.
<snip>
I anticipated a route such as this was possible myself. We have done
combustion reactions using citric as a solvent before for synthesis.
Rather quick and clean. (Faster than TGA or mortar & pestle
mixing/firings anyway) Your remarks here seem rather on the mark.
However, many metals can be quickly oxidized in air at high
temperature as I am attempting now.
It is apparent that you do have meaningful contributions to share. The
kind of tone you employ would have earned you a confrontation at the
bike rack around here though. Anyway, it's unfortunate that you so
frequently choose to somehow insert some kind of an insult when you
post replies. It really makes it difficult to appreciate a thing you
have to say. |
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