Shimadzu EPMA instruments

[Probeman]

This board is for discussion of Shimadzu hardware (and software).  Probe Software does not support the Shimadzu EPMA instrument, but to be fair it makes sense to provide a forum for Shimadzu EPMA users, just in case any would like to share information or questions about their EPMA instruments.

Interestingly, my first EPMA instrument was an ARL SEMQ at UC Berkeley. The ARL SEMQ was an American made EPMA instrument during the 1970s and 1980s. But the company was bought by Bausch and Lomb and later sold off in the late 1980s. For the record, very early versions of the Probe software actually supported the ARL SEMQ instrument, through a computer hardware interface developed at UC Berkeley by myself and John Friday (now retired).

Now you might ask, what does this have to do with a Shimadzu instrument? But in fact the Shimadzu EPMA instrument, with it's unusual 52.5 deg takeoff angle and six tunable spectrometer layout, is originally based on the ARL SEMQ instrument. In fact, the rights to the ARL instrument division were sold to Advanced Microbeam (USA) and Shimadzu (Japan) many years ago.

Now some of you might have noticed that Probe for EPMA still has support for six tunable spectrometers in its various dialogs (it used to support fixed monochromators tuned to specific emission lines, but no longer!):



And that was because of the early support for a 6 spectrometer ARL instrument, which Shimadzu currently makes. Here is a topic on EPMA history where I discuss some history of this instrument:

https://smf.probesoftware.com/index.php?topic=924.0

and here is a web page I found with some old pictures from a publication by Rinaldi and Llovet:

https://www.researchgate.net/figure/A-more-modern-American-microprobe-of-the-mid-1970s-ARL-SEMQ-at-the-beginning-of_fig2_284187581

I'll try and find some old pictures of my own and scan them... In the meantime for those unfamiliar with the modern Shimadzu EPMA instrument, here is their web page:

https://www.shimadzu.com/an/surface/epma/epma1720.html

[Probing]

Can we make it compatible with SHIMADZU instruments just by adjusting the "take off" to 52.5？

[John Donovan]

Can we make it compatible with SHIMADZU instruments just by adjusting the "take off" to 52.5？

One can certainly edit the takeoff field in Probe for EPMA for 52.5 degrees, as the software was originally written for the ARL SEMQ microprobe, which had a takeoff angle of 52.5 degrees and was what the modern Shimadzu instrument is based on.

Here is an old picture of me on the ARL SEMQ instrument:



On that ARL instrument the Probe for EPMA instrument interface was based on PC boards for ISA (originally) and PCI (later) boards for motion control, pulse counting and A/D and D/A for imaging. However these boards became harder and harder to source and eventually as JEOL (8900) and Cameca (SX100) came out with (TCP/IP) network based instruments, Probe for EPMA dropped support for the ARL SEMQ instrument and was modified for TCP/IP interfacing. Though as shown in the previous post, PFE still (in theory) supports a 6 spectrometer instrument!

So while one can configure Probe for EPMA for a 6 spectrometer 52.5 degree takeoff angle instrument there is currently no network communication interface for the Shimadzu instrument. At one time we had some discussions with Shimadzu as to whether they could provide a TCP/IP network based interface, as we have for the JEOL and Cameca instruments, but it seems that their instrument interface is, like the old ARL SEMQ, based on PCI boards in a single PC, though that could have changed since our discussions many years ago.

It would be possible to add an additional instrument interface to Probe for EPMA, but I am afraid that network interface does not exist on the Shimadzu instrument. Basically a TCP/IP network interface is required in order for multiple computers to connect to and control the instrument at the same time.

[Probing]

Thanks for sharing the story about the  ARL SEMQ, SHIMADZU, PFE and the  links between them, I really appreciate it.

[Anette von der Handt]

I just stumbled over a promovideo on Youtube showing some details of the hardware and software of a Shimadzu EPMA-1720 HT. Maybe of interest to others.

https://www.youtube.com/watch?v=ybJFPa1v3Mc

[ShimXrayEPMA]

A little background. I have been at Shimadzu for over seven years and prior to that I was a PhD student that concentrated on X-ray based spectroscopies like XRD and XRF, as well as ultra-high vacuum electron spectroscopy techniques like XPS, TPD, HREELS, and AES. I was originally hired for my background in XRD and XRF, however, as time went by, I have morphed myself into being somewhat dangerous with a microprobe.
 
Approximately five years ago, Shimadzu's USA branch, called Shimadzu scientific instruments, sold its first field emission probe to the materials science department at University of Rhode Island. A few years later another probe was sold to University of Texas at Austin in their geological sciences department. There have also been other probes sold to industry partners, both field and thermionic emission. 
Besides the actual research that is done with the probes in Texas and Rhode Island, they also are used to perform demos and run proof of concept samples.

And yes, as mentioned throughout the forum Shimadzu's probe is not compatible with PFE. I get this question a lot.

If you have any questions regarding Shimadzu's probes you can post on the forum and I will do my best to answer. You can also email me at jmlangford@shimadzu.com.

Below is the link to the field emission microprobe EPMA-8050G.
https://www.ssi.shimadzu.com/products/surface-analysis/electron-probe-microanalyzer/epma-8050g/index.html

Below is the link to the thermionic emission microprobe EPMA-1720G.
https://www.ssi.shimadzu.com/products/surface-analysis/electron-probe-microanalyzer/epma-1720/index.html

[Ben Buse]

A very interesting post rgd history.

Lack of Shimadzu compatible with PFE seems major drawback, @ShimXrayEPMA does it now use a TCP/IP interface?

Looking at brochure it seems only has 5 spectrometers now - 4 inch so comparable to h-type. And a interesting selection of crystals, ADP at 1.064 which might be better for some elements and a LSA55 at 5.5 wonder if better resolution than 6nm crystals.https://www.shimadzu.com/an/sites/shimadzu.com.an/files/pim/pim_document_file/brochures/24276/c143-e012.pdf

And there is a working ALR SEMQ at concord it seems https://www.concord.edu/academics/college-of-science-mathematics-and-health/department-of-physical-and-environmental-sciences/labs-equipment/electron-microprobe-lab

[sem-geologist]

I also have some questions:
1. When it will be available in Europe? It needs to pass only class A (for industrial/commercial use, not class B - much stricter for household items) EMC/EMI tests for CE mark, with this kind of shielding (As we see in the picture) it should be just very easy to pass.
2. As this EPMA-8050G is equipped with larger Schottky emitter specifically tailored for EPMA, how much time it needs to stabilize beam current within 0.5% of the set value, counting from after changing EHT (For comparison Tungsten V-fillament EPMA can be used right after switching into other EHT in few seconds, which makes composite (layered) material measurements and other techniques easy. In Contrast, other EPMAs equipped with SEM-tailored Schottky's emitters (Jeol and Cameca FE models) normally require a significant delay after EHT switching for current to stabilize enough so that beam regulator would regulate it within specification)?
3. Do OEM software have these:
 a) peak-overlap correction
 b) negative overlap correction (correcting overlapped  background position)
 c) ability to use only a single background measurement and slope (instead of two background positions)
4. Is it possible to get all schematics and service manual when buying Shimadzu EPMA?
5. Is it possible to get some API for direct control of EPMA by custom software?
6. Is it possible to mount CL alongside the optical microscope?

[Nicholas Ritchie]

FWIW: Shimadzu is in the process of buying Tescan. (https://www.shimadzu.com/sites/shimadzu.com/files/ir/ugq2/9gwn9rgijjzm2gya.pdf)

[John Donovan]

5. Is it possible to get some API for direct control of EPMA by custom software?

I can answer this question I think. The last time we talked to Shimadzu they did not have an TCP/IP instrument firmware interface as we do with Cameca and JEOL instruments.  Instead they offer a application library going through their software (boards in a PC).

[sem-geologist]

FWIW: Shimadzu is in the process of buying Tescan. (https://www.shimadzu.com/sites/shimadzu.com/files/ir/ugq2/9gwn9rgijjzm2gya.pdf)

The slides have December 25th!
These guys work even during holidays? or they look to Tescan as Xmas present...

[ShimXrayEPMA]

Question 1: When it will be available in Europe? It needs to pass only class A (for industrial/commercial use, not class B - much stricter for household items) EMC/EMI tests for CE mark, with this kind of shielding (As we see in the picture) it should be just very easy to pass.

1) No comment, given that I work in the United States and have no knowledge of how the European Union works.
 
Question 2: As this EPMA-8050G is equipped with larger Schottky emitter specifically tailored for EPMA, how much time it needs to stabilize beam current within 0.5% of the set value, counting from after changing EHT (For comparison Tungsten V-fillament EPMA can be used right after switching into other EHT in few seconds, which makes composite (layered) material measurements and other techniques easy. In Contrast, other EPMAs equipped with SEM-tailored Schottky's emitters (Jeol and Cameca FE models) normally require a significant delay after EHT switching for current to stabilize enough so that beam regulator would regulate it within specification)?

2) As an example, if you went from 15 kV to 30 kV beam stability occurs on the scale of a minute provided the EOC has recent preset alignment settings for both 15 and 30 kV. It does not occur on the timescale of seconds, more like within a minute. If the column for a specified EHT has not been used in some time, for example days, it may take longer to get an actual useable electron probe, however, this does not have to do with stability but more with EOC settings themselves.
 
Question 3) Do OEM software have these:
 a) peak-overlap correction
For qualitative spot analysis, if there is a 100 percent overlap/self-interferent then another main line needs to be used for quantification. If there is a neighboring peak, i.e. a peak that does not completely overlap with the analysis peak there is processing software in Shimadzu EPMA that allows you to fit a curve to further deconvolute the two peaks.


 b) negative overlap correction (correcting overlapped  background position)
Not 100 percent sure what you mean by this. I believe the answer is yes, as in you can select a background and subtract from the spectrum/peak, in qualitative analysis, and reprocess the data to further improve the accuracy.
For quantitative ZAF analysis the peak intensity, and I am not 100 percent about this and currently validating, is a peak height that is gauged by the average of the two background points. The background points are selected by typically peak searching off the standards.

 c) ability to use only a single background measurement and slope (instead of two background positions)
Yes. You can disable one BG point and only measure one BG and one Peak position.
 

Question 4: Is it possible to get all schematics and service manual when buying Shimadzu EPMA?

4) I can only speak for the United States, and for the field emission probe specifically, the answer is no. This has to do with the specifics on how Shimadzu facilitates service on the probe, and the actual design of the probe itself.  Due to how service is implemented in the United States service manuals are not distributed to end-users for the current time.
 
Question 5: Is it possible to get some API for direct control of EPMA by custom software?

5) Like the earlier post mentioned, the boards that control both the column and spectrometers are inside a control unit for the instrument. The application side is handled by libraries with a PC that is external to the control unit. A connection facilitated by TCP/IP protocol is not possible at the given time, and therefore, for similar reasons to PFE not being compatible, an API cannot be established.

Question 6: Is it possible to mount CL alongside the optical microscope?

6) Yes, it is possible to mount a CL with the optical microscope in place. UT Austin has a CL system that works in tandem with the optical microscope. In addition, the optical microscope has both the standard reflection mode as well as a polarization transmission mode where both non-polarized and Nicols/polarized images can be obtained.