Empathy List Archives

BB

Barry Bickmore

Wed, Apr 3, 2024 10:30 PM

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

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

CW

Cornell, Winton

Thu, Apr 4, 2024 5:22 PM

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

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

DZ

Dongzhou Zhang

Fri, Apr 5, 2024 3:20 PM

Hi Barry,

I did some high temperature diffraction with fused silica glass capillary (Hampton HR6-128), and my experience is that the fused silica would re-crystallize slightly above the alpha-beta quartz transition temperature (573 C). It seems that for your temperature range it is OK.

Dongzhou

From: Cornell, Winton via MSA-talk msa-talk@minlists.org
Sent: Thursday, April 4, 2024 12:22 PM
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

Hi Barry, I did some high temperature diffraction with fused silica glass capillary (Hampton HR6-128), and my experience is that the fused silica would re-crystallize slightly above the alpha-beta quartz transition temperature (573 C). It seems that for your temperature range it is OK. Dongzhou ________________________________ From: Cornell, Winton via MSA-talk <msa-talk@minlists.org> Sent: Thursday, April 4, 2024 12:22 PM 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

BB

Barry Bickmore

Wed, Apr 10, 2024 1:12 AM

Thanks for all the advice and information from everyone. If anyone is interested, here is my first attempt (which I haven’t tried in the oven, yet). I have a mini-kiln in my lab that I can put a slow heat ramp on, but I can’t control the cooling ramp, so I’ll see how it goes and post a follow-up with the results.

I’m using quartz disks from MTI, which a couple of people recommended. The ones I bought https://www.mtixtl.com/zero-SiO2-25D25C2.aspx are 25 mm diameter and 2.5 mm thick.
I designed and 3D printed PETG plastic holders where I can easily pop the quartz disk in (and the sample surface is at the correct height), but the fit is snug enough that it doesn’t shift around when it is tilted. It’s also easy to pop the disk out with a fingernail. I’ve designed similar holders for random mounts, and they work just fine on the 6-sample changer in the Rigaku MiniFlex 600 diffractometer.
There are holes on the bottom of the holder so I could pop in tiny 3 mm diameter neodymium magnets and superglue them there.

Let me know if anyone wants the STL or OpenSCAD files for the holders. Here are a few pictures.

Barry

On Apr 3, 2024, at 4:30 PM, Barry Bickmore bbickmore1970@gmail.com wrote:

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

Thanks for all the advice and information from everyone. If anyone is interested, here is my first attempt (which I haven’t tried in the oven, yet). I have a mini-kiln in my lab that I can put a slow heat ramp on, but I can’t control the cooling ramp, so I’ll see how it goes and post a follow-up with the results. 1. I’m using quartz disks from MTI, which a couple of people recommended. The ones I bought <https://www.mtixtl.com/zero-SiO2-25D25C2.aspx> are 25 mm diameter and 2.5 mm thick. 2. I designed and 3D printed PETG plastic holders where I can easily pop the quartz disk in (and the sample surface is at the correct height), but the fit is snug enough that it doesn’t shift around when it is tilted. It’s also easy to pop the disk out with a fingernail. I’ve designed similar holders for random mounts, and they work just fine on the 6-sample changer in the Rigaku MiniFlex 600 diffractometer. 3. There are holes on the bottom of the holder so I could pop in tiny 3 mm diameter neodymium magnets and superglue them there. Let me know if anyone wants the STL or OpenSCAD files for the holders. Here are a few pictures. Barry > On Apr 3, 2024, at 4:30 PM, Barry Bickmore <bbickmore1970@gmail.com> wrote: > > 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 >