Of course I meant Dean K. Smith, not Smyth. Apologies for my senior moment.
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From: Kurt Leinenweber KURTL@asu.edu
Sent: Friday, April 5, 2024 10:16:02 AM
To: Cornell, Winton winton-cornell@utulsa.edu; MSA public List serve msa-talk@minlists.org; Barry Bickmore bbickmore1970@gmail.com
Subject: Re: [MSA-talk] Re: high temperature zero-background XRD holders
Hi, I have not tried high T but I do remember some advice from Dean Smyth about mounting quartz plates in homemade aluminum holders. He told me to put double sided Scotch tape on one side and lay the quartz plate and holder over a glass plate with the sticky tape facing down. Then epoxy from the back.
The quartz plate winds up 50 microns below the holder surface and if you make your sample about 100 microns thick then you get a very small sample displacement, which you can verify by refinement.
I am sorry that I don’t know about the high temperature part which was your main question. But it was an excuse to share a little tip from Dean Smyth and Gem Dugout from long ago.
Kurt
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From: Cornell, Winton via MSA-talk msa-talk@minlists.org
Sent: Thursday, April 4, 2024 10:22:32 AM
To: MSA public List serve msa-talk@minlists.org; Barry Bickmore bbickmore1970@gmail.com
Subject: [MSA-talk] Re: high temperature zero-background XRD holders
Barry:
How about one of the MiniFlex's 'Removable Glass Insert Sample Holders' where you could do your prep on the glass slides ('glass insert, no indent flush'), they are likely very heat tolerant.
Thus, prep the slide, X-ray, remove, heat, reinsert, X-ray, etc.
We use these glass inserts in the 'ROUND top-loading sample holders', where they also give the flush surface. (Petrographic 'rounds' do not fit)
Winton
P.S. 'names' from the MiniFlex parts' catalog, available from them (file name = 'RAC Sample Catalog w PN').....I'll send it separately
From: Barry Bickmore via MSA-talk msa-talk@minlists.org
Sent: Wednesday, April 3, 2024 5:30 PM
To: MSA public List serve msa-talk@minlists.org
Subject: [MSA-talk] high temperature zero-background XRD holders
Hi everyone,
I am doing some XRD work with oriented clay films that I put through various treatments. Sometimes it’s hard to do those without the clay film peeling, unless you reduce the thickness of the film, so I like to do them with zero background holders. The problem with the ones I have (which are made for a 6-sample changer on a Rigaku MiniFlex 600) is that they have the zero-BG material (a Si wafer) mounted in an aluminum holder using some kind of glue that I don’t think will survive heat treatments up to 500 °C. There are also a couple little magnets in the holder to keep it from falling off the stage when it tilts. Anyway, it cuts the prep time way down if you can just take the mounted clay and subject it to the next treatment I could get a big quartz crystal, cut it 6° off axis, and make some zero-BG wafers myself, but I’m wondering if heat treatment would crack the quartz. I can find glue that will withstand that kind of temperature, so that’s not a problem. Back in graduate school we used porous ceramic wafers that we suctioned a clay suspension onto, and these could be subjected to heat treatment, but I haven’t found any ceramic tiles that are both the right porosity and resistant to breakage.
So, does anyone have any ideas or experience about this? Will quartz wafers withstand the temperature? (Maybe I could just ramp the temperature slowly?) Any insight or crazy ideas are welcome.
Thanks!
Barry Bickmore
Professor of Geological Sciences
Brigham Young University
Of course I meant Dean K. Smith, not Smyth. Apologies for my senior moment.
Get Outlook for iOS<https://aka.ms/o0ukef>
________________________________
From: Kurt Leinenweber <KURTL@asu.edu>
Sent: Friday, April 5, 2024 10:16:02 AM
To: Cornell, Winton <winton-cornell@utulsa.edu>; MSA public List serve <msa-talk@minlists.org>; Barry Bickmore <bbickmore1970@gmail.com>
Subject: Re: [MSA-talk] Re: high temperature zero-background XRD holders
Hi, I have not tried high T but I do remember some advice from Dean Smyth about mounting quartz plates in homemade aluminum holders. He told me to put double sided Scotch tape on one side and lay the quartz plate and holder over a glass plate with the sticky tape facing down. Then epoxy from the back.
The quartz plate winds up 50 microns below the holder surface and if you make your sample about 100 microns thick then you get a very small sample displacement, which you can verify by refinement.
I am sorry that I don’t know about the high temperature part which was your main question. But it was an excuse to share a little tip from Dean Smyth and Gem Dugout from long ago.
Kurt
Get Outlook for iOS<https://aka.ms/o0ukef>
________________________________
From: Cornell, Winton via MSA-talk <msa-talk@minlists.org>
Sent: Thursday, April 4, 2024 10:22:32 AM
To: MSA public List serve <msa-talk@minlists.org>; Barry Bickmore <bbickmore1970@gmail.com>
Subject: [MSA-talk] Re: high temperature zero-background XRD holders
Barry:
How about one of the MiniFlex's 'Removable Glass Insert Sample Holders' where you could do your prep on the glass slides ('glass insert, no indent flush'), they are likely very heat tolerant.
Thus, prep the slide, X-ray, remove, heat, reinsert, X-ray, etc.
We use these glass inserts in the 'ROUND top-loading sample holders', where they also give the flush surface. (Petrographic 'rounds' do not fit)
Winton
P.S. 'names' from the MiniFlex parts' catalog, available from them (file name = 'RAC Sample Catalog w PN').....I'll send it separately
________________________________
From: Barry Bickmore via MSA-talk <msa-talk@minlists.org>
Sent: Wednesday, April 3, 2024 5:30 PM
To: MSA public List serve <msa-talk@minlists.org>
Subject: [MSA-talk] high temperature zero-background XRD holders
Hi everyone,
I am doing some XRD work with oriented clay films that I put through various treatments. Sometimes it’s hard to do those without the clay film peeling, unless you reduce the thickness of the film, so I like to do them with zero background holders. The problem with the ones I have (which are made for a 6-sample changer on a Rigaku MiniFlex 600) is that they have the zero-BG material (a Si wafer) mounted in an aluminum holder using some kind of glue that I don’t think will survive heat treatments up to 500 °C. There are also a couple little magnets in the holder to keep it from falling off the stage when it tilts. Anyway, it cuts the prep time way down if you can just take the mounted clay and subject it to the next treatment I could get a big quartz crystal, cut it 6° off axis, and make some zero-BG wafers myself, but I’m wondering if heat treatment would crack the quartz. I can find glue that will withstand that kind of temperature, so that’s not a problem. Back in graduate school we used porous ceramic wafers that we suctioned a clay suspension onto, and these could be subjected to heat treatment, but I haven’t found any ceramic tiles that are both the right porosity and resistant to breakage.
So, does anyone have any ideas or experience about this? Will quartz wafers withstand the temperature? (Maybe I could just ramp the temperature slowly?) Any insight or crazy ideas are welcome.
Thanks!
Barry Bickmore
Professor of Geological Sciences
Brigham Young University