Author Topic: Issues for Low kV Analyses that need to be addressed by PfE  (Read 7049 times)

Dan R

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Issues for Low kV Analyses that need to be addressed by PfE
« on: October 18, 2013, 01:08:02 PM »
Hello-
   We have a JEOL 8530F Field emission microprobe specifically designed for low kV analyses. We purchased PfE for this instrument, but so far our software is limited. I have two outstanding issues that need to be resolved by PfE in order to free us from using the vendor-supplied software (and limitations that come along with that) for low kV analyses:

1) Probe tracking. For small phases, the ability to use probe tracking is essential unless you want to sit and acquire each point manually (i.e., acquiring an image during digitization, storing this image, and then comparing the before image with a second image acquired during automated acquisition in order to account for slop in the stage).

2) Spot analyses. Currently we see the beam raster over a small area at 300,000X instead of using a true spot. The raster area corresponds to ~500 um2... This is considerably larger than the analytical volumes we are trying to achieve using low kV.

Are solutions for these limitations by PfE on the horizon? Until then, we are stuck using vendor-supplied software...

-Dan
« Last Edit: October 20, 2013, 02:08:12 PM by John Donovan »

John Donovan

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Re: Issues for Low kV Analyses that need to be addressed by PfE
« Reply #1 on: October 18, 2013, 01:51:46 PM »
1) Probe tracking. For small phases, the ability to use probe tracking is essential unless you want to sit and acquire each point manually (i.e., acquiring an image during digitization, storing this image, and then comparing the before image with a second image acquired during automated acquisition in order to account for slop in the stage).

Hi Dan,
The probe tracking feature *is* "on the horizon". It will be pretty cool because it will use the image that you acquired for the Digitize Image feature and then use that as a reference for image shift. I'm hoping to implement it around the end of the year- that will be my Christmas vacation!  :)

However, this assumes that JEOL provides the image shift commands for the 8530 relatively soon, which they have not as yet. I do have the image shift commands for the Cameca Sx100/SXFive so I will start testing this feature on the Cameca instrument for now. Philippe Pinard, Mike Meyers (both with 8530 instruments) and I have already requested these image shift commands from JEOL but if you'd like to add your voice to the chorus that might help...  :)

Quote from: Dan Ruscitto
2) Spot analyses. Currently we see the beam raster over a small area at 300,000X instead of using a true spot. The raster area corresponds to ~500 um2... This is considerably larger than the analytical volumes we are trying to achieve using low kV.

This sounds like you do not have the EIKSVersionNumber keyword properly set in the Probewin.ini file [hardware] section.  It should be set as follows:

[hardware]
JEOLEIKSVersionNumber = 5

This is because JEOL did not originally provide the spot mode commands for the 8530, but they have earlier this year. Assuming you have the proper PC-SEM version on your JEOL computer, this change will provide an actual spot mode for you!

Basically this is what you should see for the spot, scan and beam deflection modes on your JEOL screen:

 Analog spot (green cross hairs)
 Analog scan (blank screen)
 Digital spot (yellow cross hairs with circle)
« Last Edit: October 20, 2013, 02:08:26 PM by John Donovan »
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Dan R

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Re: Issues for Low kV Analyses that need to be addressed by PfE
« Reply #2 on: October 19, 2013, 12:20:05 PM »
John-
 My Probewin.ini file is correct, the EIKS version is set to 5. As for the versions of the PC-SEM software I have, they are:
PC-SEM V3.0.1.6
EIK Driver 2.0.0.8
PC-EPMA 1.9.0.3

The same found on the 8530F at ASU (see quoted message below).
Are these versions correct? I am not getting a true spot mode.
-Dan

Can someone please explain how one determines which version of Jeol PC-SEM one has, as here at ASU, where the Jeol engineer reinstalled the system software after there was a major software crash. So I look at the engineer's record of the software and see the following
PC-EPMA Software Ver. 1.9.0.3
PC-SEM Software Ver. 3. 0.1.6 (so is this version 3? or version 16? or v 6? I don't see any way to think is is at least version 8)
EOS-Firm Software  (JXA-8530F) Ver. 1.7.4.0
Stage Software Ver. 2. 85
EDS Software Ver.1.11
« Last Edit: October 20, 2013, 02:08:42 PM by John Donovan »

John Donovan

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Re: Issues for Low kV Analyses that need to be addressed by PfE
« Reply #3 on: October 19, 2013, 01:41:42 PM »
My Probewin.ini file is correct, the EIKS version is set to 5. As for the versions of the PC-SEM software I have, they are:
PC-SEM V3.0.1.6
EIK Driver 2.0.0.8
PC-EPMA 1.9.0.3

The same found on the 8530F at ASU (see quoted message below).
Are these versions correct? I am not getting a true spot mode.

Hi Dan,
So when you start an analysis in "spot" mode you do not get the green cross hairs on the JEOL screen?  You might check that there is not a duplicate line in your Probewin.ini file. Also the spelling is important because it defaults to 4 if not found:

[hardware]
JEOLEIKSVersionNumber=5

I will have Philippe Pinard double check on his instrument, but if you get a chance, please put the software in "debugmode" using the Output menu and capture a spot mode acquisition output to the log window and send it to me so I can check it.
john
« Last Edit: October 20, 2013, 02:09:03 PM by John Donovan »
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pgopon

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Re: Issues for Low kV Analyses that need to be addressed by PfE
« Reply #4 on: October 20, 2013, 05:12:49 PM »
I think PfEPMA is about the only software that can handle low keV analysis right now.  Despite the shortcomings of PfEPMA (namely the inability to use non-standard X-ray lines), they are less than those of the the vendors (especially JEOL, whose inability to use exponential backgrounds makes it a non-starter). 

I would suggest the using automation for small phases (say under 2 um) would be ill advised for a few reasons.  Both vendors have problems with stage reproducibility, where they can't get back the spot withing a micron or so, and that is with tracking.  Also, large spectrometer motion can cause sample drift (Philippe Pinard has a great video of this from his 8530). 

John Fournelle, Xavier Llovett, Peter Sobol, and I have a paper coming out in M&M shortly about the problems (and some solutions for low keV analysis), and I direct you to it for some explanations of the difficulties especially for the transition metals.  There is a special conference at RWTH Aachen coming up specifically on low keV analysis, and I am curious to see that new problems come to light from it. 

I think it would be great if the low keV community in North America could organize such a meeting (hopefully with John Donovan present) to discuss what we need to do to make this type of analysis routinely possible.

phil

Dan R

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Re: Issues for Low kV Analyses that need to be addressed by PfE
« Reply #5 on: October 20, 2013, 06:18:24 PM »
Thank you for the information Phillip. I look forward to reading your paper... The vendor software definitely cannot handle the backgrounds and the limited matrix corrections available leave much to be desired. I hope to use PfE more for my work, but right now I'm very limited by the lack of probe tracking... I've actually been very happy with the probe tracking mode available with the vendor software.
-Dan
« Last Edit: October 20, 2013, 06:24:59 PM by John Donovan »

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Re: Issues for Low kV Analyses that need to be addressed by PfE
« Reply #6 on: October 21, 2013, 09:05:53 AM »
The goal of both methods (low keV analysis and low overvoltage analysis) is a small interaction volume, so it would be interesting to compare, say, Ni Ka at 10 keV with say, Ni La at 5 keV. One can model these scenarios with the Run | Model Xray and Electron ranges window in CalcZAF. For accurate modeling we would of course use Monte-Carlo, but this will give us some rough numbers to play with.

In this screen shot, we model Ni Ka in the NIST NiFE alloy at 15 keV. The 99% electron range is 0.94 um, but the 99% Ni Ka production range is only 0.59 um because once the incident electron energies drop below the Ni ka K edge (8.33 kV), they cannot generate inner shell ionizations thus limiting the interaction volume.



Note also the Ni ka transmission at the 99% electron depth (0.59 um) is ~90%. This will be an important number to check when we model Ni La.

The disadvantage of low overvoltage is that you might need several voltages if the various emission energies are quite different (e.g., Ni Ka vs. Si Ka). But the advantage is that one can use K lines for transition element quant, which behave better than the L lines. One the other hand, low overvoltage analysis can be problematic because the analysis can be quite affected by native oxide layers, carbon coating thickness and the physics of low overvoltage modeling.

Let's try the same analysis, now at 10 keV... We'll continue with further discussion in a moment.
« Last Edit: October 21, 2013, 09:09:01 AM by John Donovan »
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Dan R

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Re: Issues for Low kV Analyses that need to be addressed by PfE
« Reply #7 on: October 21, 2013, 12:00:35 PM »
Thanks for the discussion John. I have found the beam scan/spot mode error to be a stupid mistake on my part. Apparently the default setting for a new sample was specified in the .ini file as:
[general]
BeamMode=1                      ;Need to set to 0 when EIKS fixed  0=analog spot, 1=analog scan for default analysis mode

Apparently EIKS has been fixed!

I did not realize this, but now I have set my .ini file to BeamMode = 0 as default. Now my spots appear to be working correctly. Thanks again for your help!

I did not realize just how important this setting was when analyzing small interaction volumes!

-Dan

John Donovan

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Re: Issues for Low kV Analyses that need to be addressed by PfE
« Reply #8 on: October 21, 2013, 02:20:36 PM »
I did not realize just how important this setting was when analyzing small interaction volumes!
No worries Dan, that is what this forum is for!

In any case, I'm going to continue with this short tutorial on modeling interaction volumes using CalcZAF, but I'm going to move it to a thread on the CalcZAF board here:

http://probesoftware.com/smf/index.php?topic=86.0
« Last Edit: October 21, 2013, 02:27:01 PM by John Donovan »
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John Donovan

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Re: Issues for Low kV Analyses that need to be addressed by PfE
« Reply #9 on: October 21, 2013, 03:33:47 PM »
I did not realize this, but now I have set my .ini file to BeamMode = 0 as default. Now my spots appear to be working correctly. Thanks again for your help!
-Dan

It is probably obvious now, but the Probewin.INI keyword (BeamMode), only sets the *default* state of the beam mode on startup. You can of course change that setting in Probe for EPMA by simply clicking the desired mode from the Analytical Conditions dialog as seen here:



But while we're looking at the Analytical Conditions dialog, allow me to point out a couple of other features that are related to high resolution analysis.

But first it should be mentioned that one can read the current state of the instrument by clicking the Read Conditions button as seen here:



Next note that one can also utilize scan mode for analysis by first clicking the Analog Scan option and then setting the analytical magnification as seen here where 400Kx gives a 0.95 um scan area.


John J. Donovan, Pres. 
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