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November 2015

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Subject:
From:
Julien Allaz <[log in to unmask]>
Reply To:
JEOL-Focused Probe Users List <[log in to unmask]>
Date:
Tue, 24 Nov 2015 22:11:43 +0000
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Thanks Joe,

Replacing the BSE is a good idea (I’ve seen it last year, and effectively it is as bad as you would expect it after 27 years of service [!]…), but since our current instrument will be replace in early 2016, this is not an option…

Regarding the Ti Ll interference on N Ka, I’m well aware of this, and I do correct for this. Still, some phases suggest up to 1.8% N after correction for Ti Ll. Again, N is not really important for this customer (they know the strong limitation / huge error associated to this). What was surprising to them was the oxygen content. It is true that the k-ratio is already indicative, but it is important for the customer to know what are the atomic proportion (hence the “as accurate as possible” weight-% element).

Best,

Julien


> On Nov 24, 2015, at 14:49, Joe Geller <[log in to unmask]> wrote:
> 
> Julien:
> 	I'd recommend you replace the backscattered detector as they do get contaminated over the years.
> 	We did our recently and it made a huge difference.
> 	As far as N and Ti goes there is a pretty complete overlap with the Ti Lα and N Kα. At low concentration forget about it.
> 	The same K-ratios go into the different ZAF corrections so you will see the same relative differences in concentrations but the absolute levels will change.
> 
> -Joe
> 
> Joe Geller
> Geller MicroAnalytical Laboratory, Inc.
> 426e Boston St.
> Topsfield, Ma 01983 (USA)
> 978 887-7000, fax 978 887-6671
> www.GellerMicro.com
> 
> 
> -----Original Message-----
> From: JEOL-Focused Probe Users List [mailto:[log in to unmask]] On Behalf Of Julien Allaz
> Sent: Tuesday, November 24, 2015 3:09 PM
> To: [log in to unmask]
> Subject: [PROBEUSERS] Pt-Ti alloy
> 
> Dear microprobers,
> 
> A customer recently asked me to analyze several alloys of Pt-Ti (in various mixture), and quantify the different Ti-Pt phases within each. In addition, they asked me if it was possible to analyze also O (and N). First importance for this job is the Ti - Pt ratio, and this light element work is just an “extra” if possible. So… I gave it a try... Beside the “usual” light element problem, I have two specific questions for you.
> 
> (1) With my vintage instrument (JEOL-8600), it is very hard if not impossible to work on these samples at low keV (<10 keV), as I loose the necessary BSE contrast despite cranking up the BSE gain and adjusting for the contrast - and some phases in a single sample can be ~1-2 µm in size, they are already just barely distinguishable from the mass. Therefore I opt for 15 keV, a level at which the contrast is sufficient. I know… This is definitely not great for light element. The results can vary quite dramatically, notably for O, depending on the matrix correction procedure used (e.g., in one domain, it can vary from 0.7 to 1.2 wt-%, so not negligible (Calculated DetLim for O is around 320 ppm; 1sigma counting precision at 3% relative). Do you have any recommendation for the appropriate ZAF correction procedure (currently I’m using Armstrong ZAF and FFAST MAC table). Is it possible to have oxygen “contamination” during the analyses at high current (100-200 nA).
> 
> (2) Results show high O-content from a few hundred ppm to above 1 wt-%. These measurement are repeatable within a single phase in a specific sample (5 analyses each, each with similar wt-% O), and in the same sample, one phase might have 0.9% O and the other almost nothing (100 to 1000 ppm). The customer has actually prepared these sample in a neutral-atmosphere (argon) furnace ~1 year ago. I have yet to double check if the problem could come from Pt Mz (3rd order! - so probably not so important, but we are speaking here of ~0.1-0.4 cps/nA on O Ka in the unknown [Std O Ka at 118 cps/nA]) lines around O Ka, but I don’t see a correlation between O wt-% and Pt wt-%. The samples were re-polished, but I recently learnt that the customer only did a single 0.02 µm fine polishing, which may not have been enough to remove this oxidized layer?!? If you have ever worked with such alloy, do you think it is possible the samples have been oxidized (i.e., do Pt-Ti alloys oxidize easily)?
> 
> About the setting: I’m using an LDE1 crystal (60 Å) for O Ka and apply an exponential background correction (curvature determined using WDS scan in a representative TiPt phase), and high current (100 - 200 nA - this further help my BSE detector to “see” the different phases). I opt for Ti Ka on LiF (lower count rate, but with high current / ~60 sec counting, the precision is enough) and Pt La on PET. If I drop the voltage, I would probably have to opt for Pt Ma (and maybe even Ti La) which raises other problems...
> 
> Your help will be greatly appreciated! Thanks, and Happy Thanksgiving!!!
> 
> Julien
> 
> 
> P.S. Let’s not worry about N, another beast… In most (90%) of the phase, the N-level is probably a few hundreds of ppm and with (a) the low count rate (3 cps/nA on BN at 15 keV… I know… way to high absorption in every component and low efficiency in the P-10 gas), and (b) a strong correction from Ti Ll (up to 100% of the signal received).
> 
> 
> =============================
> Dr. Julien Allaz
> Electron microprobe manager
> University of Colorado Boulder
> Dept. of Geological Sciences
> UCB 399
> 2200 Colorado Av.
> Boulder, CO 80309-0399
> 
> Phone: (303) 735 2413
> Cell: (413) 210 0917
> Lab: (303) 492 5251
> Fax: (303) 492 2606
> 
> Personal website: http://geoloweb.ch
> Lab website: http://geode.colorado.edu/~jallaz/
> =============================
> 
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