Paper highlight, Madrid meeting and Detector electronics

A few things came up in the last two weeks which may be of interest.

Firstly, I will be in Madrid for a magnesium alloys conference next week Tuesday to Friday. If anyone wants to meet up there, please let me know through e-mail (check the “about” page), message below or send me a direct message on Twitter (@drheaddamage).

Then there was a paper which made me quite happy. This paper by Brûlet discusses in detail how to correct for samples sandwiched between two sample-holder walls. It contains a detailed description of the sample direction-dependent absorption (derived separately in a previous post here, and further discussed here for capillaries and spherical samples here). It furthermore indicates that you have to be careful with such sandwiched samples, as the sample receives an attenuated  radiation flux from the first wall. Secondly, the background scattering from the upstream wall is absorbed with direction-dependence by the sample and both walls, the sample-scattered radiation absorbed with direction dependence by the sample and the downstream wall, and the latter again scattering and exhibiting direction-dependent absorption from itself. As you can see, it is a very well put together experimental consideration. Definitely one to add to the reference list!

Lastly I wanted to give a quick update on Bonse Hart instrument construction status. I have been handed a scintillation detector tube to use by one of my advisors. After scrounging through some storerooms in the building, I came across some useful stuff:

Scrounged from the storerooms!

Scrounged from the storerooms!

The owner was quick to point out that it was slightly aged (15 years) but that I was welcome to take it. I collected the following bits: a NIM bin with some NIM modules (bottom left, the modules are a Tennelec high voltage power supply, Ortec amplifier and NAIG single channel analyser), an oscilloscope (top right), a fancy multimeter (top left) and a power supply (bottom right). The beefy power supply is overkill for powering the small detector preamplifier, but it was what I could find. The NIM stuff, for those not familiar with it, is a modular system for analog signal processing developed in the 1960′s. It can house a wide variety of modules, each geared towards a specific task. I am still missing two modules: a pulse counter and a ratemeter (which come at about 5 kEuro each), but I figure I may abuse an Arduino Uno to do those tasks for me if I do not stumble across another stash somewhere. Still, I am very happy to have come across the most tricky bits. Soon I will get the chance to try it all out! See you then!

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Public day demonstration

I think it is safe to say that “everyone” is familiar with electron microscopy for looking at small things, but the same cannot be said for small-angle scattering. Introducing more people to the wonderful world of small-angle scattering may be one of the ways of getting more support for and interest in the technique. With this in mind, and with some contacts in the PR department, we managed to get last-minute approval to do a demonstration at the public day at NIMS.

hairlaserteam

The team of the 2013 NIMS public day with Martin, me, Novi and Ryo. Missing from the picture is Julian.

The plan was to have people measure their own hair diameter using a laser in a similar way as demonstrated before in these youtube videos. As I was not expecting more than a few visitors per hour, 5 minutes per visitor was considered a suitable amount of time. To help them, we prepared a step-by-step instruction sheet and some “tools” that the people could cut out and use for their experiment. The procedure was as follows:

  1. Visitors would be lured in by our blatant advertising to “measure the diameter of your hair using a laser!” (stuck in big letters on the wall, taking up lots of floor space and having a big screen with the program running on it. Also, we had foreigners at our desk in an otherwise very much Japanese event. There was even some Dutch candy!). Visitors would then be given an instruction sheet and some tools.
  2. They would cut out the tools (one target and one holder for their hair), find a hair and stick it on the paper. Surprisingly, almost everyone could spare one (or had one cut off by one of the staff), and they very much enjoyed the bit of manual labour of cutting out pieces of paper, sticking hair on it and so on.
  3. Going over to the laser, where the staff mounted the hair in front of the laser (which was a bit finicky work to get it to sit right) using a couple of paper clamps. The laser pointer was forced “on” using another paper clamp holding down the button (the laser pointer itself managed about half a day on a set of batteries, surprisingly).
  4. Clamping the target onto a clipboard stuck to a tripod, and aligning the central black spot on target with the laser pointer beam, the scattering from a hair becomes clearly visible. The clipboard was about 2m from the hair and laserpointer. At this point I would always take a moment to explain that the central spot was from the laserpointer, but the oscillations were coming from their hair (in my best Japanese).
  5. We would then ask them to draw arrows in the center of the oscillation spots. This is where it would most often go wrong, as people were unsure on where to draw the points and my Japanese would not be sufficient to explain this. Nevertheless, they had fun drawing points.
  6. Taking that piece of paper, I would take them to measure the required values: the distance from hair to the target (in meter, with a tape measure if there was time), the number of spots from the target center they could see, the distance from the target center to that last spot (in mm), and reading the wavelength from the laser (green=532 nm, now forever etched in my memory).
  7. Filling in these values in a Python program (available here) they were then given the diameter of their hair. In the beginning this was set to display the diameter in micrometer, but after an hour or two it became evident that that was not very well known with the public. We therefore changed this to mm. We had our Japanese staff stand at the computer, so he could explain a little about common hair diameters (European: 40 micron, Japanese: 80 micron with the occasional outlier at 110 or 120 micron). Significant digits and uncertainty were a bit of an issue, some wrote down all nine digits resulting from the calculation.

Before I tell a bit more about the experiences on the day, here are the tools you can use (conveniently in English and Japanese):

As this was the first time we did this, we had no idea what to expect. We shared the big lecture hall with three other demonstrations, which helped to draw people to us. We set up the demonstration in a slightly inefficient way, whereas we should have considered the flow of people through the steps. This was exacerbated by the sheer number of visitors. Visitors tended to come in groups of four or more (with the occasional elementary school class to make things really hectic), after which it would be quiet again. Overall, we “served” an estimated 70 people during the 6 hours, which were about 50% schoolchildren and about 50% adults. We had two to four people staffing the set-up at any time.

Ideas we have gained for next time include:

  • Setting up the tables a bit better, so that there can be a more logical flow from stage to stage (whilst still keeping it compact), and reserving a separate table for the cutting and sticking-work.
  • The set-up using commonly available bits and pieces worked in our favour. Some said they intended to repeat the experiment at home, showing that they noticed it consisted of nothing more than a laser pointer and some paper clamps.
  • If we prepare for groups we can explain only once for a group of four or five.
  • Staffed stages could be three stages (cutting, measuring and computation) or four stages (cutting, “laser”-ing, measuring, computation). Parallel laser stations would be preferred, perhaps of different wavelength.
  • A microscope table can be included for people who want to verify (which should be encouraged if there is time).
  • It would be nice if a form was printed with a picture of the measurement with maybe a picture of them, their hair oscillations and the “scientist”-guaranteed number (signatures and such).

I strongly encourage people to try this demonstration at their institute as it was good fun! We’ll do this next year again if we have the chance so do drop by if you have the chance!

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Build Your Own Instrument update: Making it cool

Some of you have asked about the current state of the Bonse-Hart USAXS instrument I have been building (reported here). Well, it has seen some progress here and there, though  there was no pressure to get it finished quickly as the X-ray generator was not working yet due to high-vacuum troubles.

Unfortunately, just when the offending x-ray generator components were replaced and the molybdenum rotating anode target was about to arrive, there was a bit of a snag. My advisor was fortunate enough to land a professorship at another place to focus on a very cool new development: compact neutron sources. Sadly, his imminent move meant that I would “lose” a very good colleague and advisor, and easy access to some of his good instruments which would follow him to his new position (though he did leave a large amount of really useful parts, almost enough to build a complete instrument!). The cooling system of the Bonse-Hart rotating anode generator had to go too, leaving me with a working rotating anode generator, but no way to cool it. His moving away got me a bit down but such is the way of science (“kenkyudo”, or 研究道): the path of you and your colleagues only runs parallel for a short time, so you better make the most out of it.

Anyway, ballpark figures for a cooling system come to about 20 kEuro which are slightly above my available budget. The one large budget proposal I had submitted came back negative (which I had pinned my hopes on), so that’s not going to be a solution. If I would have gotten it, I would have had the chance to buy a cooling system and maybe even one of these microfocus X-ray sources to see if the Bonse-Hart instrument would work on those relatively inexpensive radiation sources (which come to about 75-100 kEuro). Coolness aside, it would have been genuinely useful to find out if such sources are a viable option.

Not all is lost, though, and it will only take some time to find a suitable solution. In short the Bonse-Hart instrument is aligned with a laser now, and even has some shielding. It should now be ready, though it still lacks a detection system. Help is always welcome, though, so please feel free to drop me a line in the comments or find my e-mail address on the “About Me”-page. Until then, here is a picture of the instrument in its current state showing part of the outer radiation shielding in place:

Bonse-Hart today

Happy Scattering!

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Conference plan and a new poster…

A day later than planned, but here’s another post…

I am planning to speak at the TMS Magnesium Workshop Madrid 2013, some time during the conference lasting from May 21 to May 25. During this conference I will be focusing on the results we obtained for ex-situ and the preliminary in-situ results studying the growth of precipitates in MgZn alloys. Naturally, I will be heavily plugging SAXS and the MC analysis methods. If you are in Madrid or at the conference at that time and want to meet, please leave a message…

Secondly, For a recent conference I had the chance to make another poster. It has been a while since I posted any posters on this site, so if you want to get an idea what they look like these days, take a look here. The design is still a bit full of text but in a font large enough to read. Additionally, the text is laid out in a newspaper column-format to make it easier on the eye to move from the end of one line to the beginning of the next line (some info here). The whitespace at the right-hand side should make it easier to distinguish the section headers, and given that this poster was presented in Japan, where comics are read from right to left, this poster has section headers rightmost, followed by an image left of the header, and then two columns of text (which are read left-to-right, unfortunately breaking the mould). The introduction and conclusion section is typeset to a larger font as this is what most people are interested in, and the authors and affiliations is at the bottom (because that is what people should remember at the end). The space at the bottom should contain my business cards in a pocket so people can grab one if I am not around. Lastly, the background is meant to appeal at large distance for its colour, but set to a transparency which does not hinder reading at close distances.

Despite these considerations, the poster has not enjoyed much success, so for the next one I may employ a different style.

 

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Monte-Carlo: now in 2D!

Small-angle scattering analysis has never been easy for those working with oriented nanostructures (e.g. fibres, processed polymers, rolled metal alloys), whose structure may lead to anisotropic small-angle scattering. Upon the collection of such 2D scattering patterns, one can integrate thin pie-slices of the data to obtain 1D curves and analyse them in the same way as “normal”, isotropic scattering patterns. This way, however, important cross-correlation information is lost. Alternative full-pattern fitting methods have been developed (amongst others during my Ph.D. studies), but they are complicated to tune to the system at hand and can be quite unstable in least-squares optimisations.

One alternative is to analyse the scattering pattern by using Norbert Stribeck‘s 2D inversion method to obtain a two-dimensional pair-correlation function. Unfortunately, correlation functions are not always the easiest for the researcher to understand. Recently, I presented a 1D Monte Carlo method for obtaining form-free particle size distributions from isotropic scattering patterns, which —as it turns out— can be adapted to analyse anisotropic scattering patterns as well. The first results of this two-dimensional Monte Carlo analysis was presented at the SAS2012 conference, at which it was shown that it can obtain three distributions: the width and length distribution and an orientation distribution.

These initial results were written down for the conference proceedings, which have been submitted recently. The pre-submission manuscript is available (as before) on ArXiv here. Now is the time to try to apply this method to a variety of samples, so if you are working with oriented structures (and their scattering) and you are interested, please drop me a line!

 

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Papers! One of mine and one on detector data read-in

It has been a long time in the making, but now the day has finally come where the 1D Monte Carlo method has been published! To top it off, the publication is open access (courtesy of my current institute: NIMS), and has a wicked showcase document as supplementary material. Feel (very) free to check it out here!

In short: the MC method can retrieve form-free particle size distributions from isotropic scattering patterns, complete with uncertainties. There is more to it than that, but the details are in the paper. The Python 2.7 code is available in a Git repository as indicated in this post, available under a creative commons attribution sharealike license.

In the same J. Appl. Cryst. edition that my paper appears in, there is another paper which caught my interest. This is a paper by E. B. Knudsen, et al., which presents a bunch of code under the name of FabIO that can be used in Python to read in detector images (under a GPL license). There is even some code there for the more obscure of image formats, with improvements to follow. For me, this is part of what I was looking for to augment my own procedures, so I really appreciate it when others make their stuff available with a suitable license!

That FabIO package is part of larger programs for XRD and data reduction, respectively. Given that this is a program which is sustained by the efforts of a variety of user-driven institutes (ESRF, for example), I am very much looking forward to see which direction it will be taken into. One of the authors has assured me that if there is a need and an example (say, for supporting an imageplate image format or some of the stranger wire-arrays), they are more than willing to implement that particular image format. Naturally, that open-source project is available for collaborative efforts as well!

 

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Job offer: Anything you want!

It is that time of the season again, when the group I am working in is hiring. In short: if you are a fresh Ph.D. graduate or a post-doc within 10 years of obtaining your Ph.D., and you want to do your own research with at least a tenuous link to materials science, this is the place for you. The job opening is advertised here: http://www.nims.go.jp/icys/recruitment.html and the application deadline is March 29.

In a little more detail, this is what it entails:

  • The program is intended to offer tenure-track positions to scientists, i.e. if you are in ICYS (this group) and apply for a permanent position at NIMS (the institute where the group is located), you have automatically passed the first round of application. Despite that, many people use this as a stepping stone for positions in other institutes and universities as well.
  • Officially, the ICYS program is intended to improve communication between foreigners and Japanese scientists.
  • It is a project for 2 years, with a possible (not so difficult) extension to three years.
  • The salary is quite decent, in line with the scandinavian salaries after subtraction of tax.
  • You have a research budget of 20 million yen per year (about 20kEuro/year) for anything you want: travel, stuff and even Open Access fees. You can also apply for one of the many funds available in Japan if you need more money.
  • You get secretarial support to take care of most of the paperwork, and further support for getting settled in Japan by another organisation.
  • You are assigned two “advisers”, but it is up to you how much you use them. They can be useful for getting contacts or access to instruments. Essentially you are free to research anything you want, you are an independent scientist. They may also help you get a permanent position.
  • Tsukuba is a great city to live in: quite inexpensive and only 45 minutes by train from Akihabara in the heart of Tokyo.
  • The ICYS group is definitely fun, with young people from all over the world, so apply!

Now I understand that it can be quite tricky to think what projects would be considered, so let me give some examples of what some of the ICYS researchers do:

  1. One researcher is developing new, stable field-effect electron sources for electron microscopes from LaB6 nanowires.
  2. Another is working on a theoretical project calculating magnetic structures, and a third is measuring and simulating magnetic behaviour at various temperatures of permanent magnets.
  3. One is calculating the photonic properties of a variety of hypothetical and practical situations
  4. Some are working on developing better organic and inorganic solar cells
  5. Others are studying phosphors and ways of improving them
  6. There have been chemists working on fundamental behaviour of functionalized materials in liquids, and another working on practical, green synthesis routes for a variety of industrially relevant materials.
  7. There are those of us improving the methods used for studying materials, such as improving SPM systems for nanofabrication and analysis and my research to improve the SAXS methodology.
  8. There are many working on polymers and biological systems as well, but they work in another building so I am not fully aware of what they do.

So you can research a wide variety of topics, as long as it somehow has something to do with materials science. I found this place a pleasure to work at, with uncommon amounts of freedom. No-one is standing over my shoulder which allowed me to do weird things like spend many days in the workshop milling, drilling and cutting my own instrument. I can go to whatever conference I like, I can collaborate with whomever I want. NIMS also has an enormous amount of instrumentation available, some quite specialised, and money doesn’t seem to be much of an issue.

So, if you want to work here, and are not yet convinced by what I wrote, if you have any further questions, please drop me a line.

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Paper highlights: Prior art and detector trouble

Hello everyone, and welcome to the remaining 90% of 2013 (as of February 4), surely you’ve made good use of the first 10!

I’ve been tasked with writing a review paper which made me come across several noteworthy papers. Two topics in particular surprised me: the history of instrumentation and the depth of detector corrections. In the hope that they may be of some interest to some of you, a few words on them might not be amiss.

What may come as a bit of a surprise, as it did to me, is that the history of SAXS instrumentation turns out to have been quite advanced right from the start. Current papers on instrumentation discuss the benefits of the technological advances from focusing optics, three-pinhole systems, crystal monochromators and so on, so here is a quote from O. E. A. Bolduan in 1949: “Investigators have attempted to solve the peculiar requirements of this field by use of longer wave- lengths to increase diffraction angles [3] crystals for monochromatization and collimation [4-7] high intensity x-ray tubes [8,9] or cameras with focusing by means of curves [sic] crystals [9,1o] or totally reflecting plates [11] to increase the level of useful radiation [...], with Bolduan himself discussing three-slit collimation to reduce parasitic scattering from slit #2. Publications of SAXS instruments on home-built rotating anode generators appear already in the 1950′s. After reading a lot of papers discussing the finer details of those instruments leaves me wondering what major improvements we have made in the 60 years since that paper, and one of them is of course in the field of detectors.

Before the advent of more advanced 2D wire-detectors, imageplates and CCD-based detectors, one was pretty much stuck with using either Geiger counters (0D) or photographic film for 2D images. The photographic film, though, behaves rather nonlinearly vis-a-vis incident radiation amounts, necessitating serious corrections before it could be used. 2D wire detectors were an improvement, but only suitable for quite low countrates (<100 Hz/pixel) and show a rather large point-spread function. CCD-based detectors brought improvements there but their dynamic range is typically not much higher than 3 to 4 orders of magnitude. Imageplates brought improvements with up to 6 orders of magnitude of dynamic range, but necessitate laborious read-out and erasure procedures and thus are ill-suited for time-resolved experimentation. Recently, direct-detection detectors appear to solve the majority of the issues of all prior detectors, at a hefty price (conveniently, the price-tag of the Pilatus detector comes permanently written on its housing: a Pilatus 100k costs about 100k-euro, a 300k costs 300k-euro and so forth).

Nevertheless, each of these detectors produces intensity that is in dire need of corrections. Reading up on these, here are my recommended papers for getting more insight into some of these. Firstly, there is S. L. Barna with a good list of corrections, with some focus on distortions found in CCD’s. Furthermore, in results shown by V. Le Flanchec that even image plate data needs to be corrected for read-out positional inaccuracies as well as some other effects. F. Né also indicates their darkcurrent corrections need special treatment, in particular to start counting from the time of their last erasure.  Other names to look for insights on this topic are, amongst others, P. Boesecke, T. Zemb, A. Rennie, P. Jemian, and many more, especially those in the CANSAS groups. Through their work, my list of corrections (of a month ago) has by now increased to a whopping 20(!) data corrections that could be considered applicable for small-angle scattering data. This space is too small to describe them all, but there will be space elsewhere later on this year, so stay tuned!

Lastly, in unrelated news: we applied the previously presented MC method to obtain radius distributions for isotropically oriented, rod-like precipitates in metals, the draft has been made publication-ready and can be found here. We are looking for a journal to publish this in at the moment.

Keep scattering!

Barna: Barna, S. L. and Tate, M. W. and Gruner, S. M. and Eikenberry, E. F., “Calibration procedures for charge-coupled device x-ray detectors”, Rev. Sci. Instrum. 70 (1999), pp. 2927

Le Flanchec: V Le Flanchec, D Gazeau, J Taboury, and T Zemb, ”Two-Dimensional Desmearing of Centrosymmetric Small-Angle X-ray Scattering Diffraction Patterns”, J. Appl. Cryst., 29 (1996), pp. 110–117

Ne-1993: F Ne, D Gazeau, J Lambard, P Lesieur, T Zemb, and A Gabriel, “Characterization of an image-plate detector used for quantitative small-angle-scattering studies”, J. Appl. Cryst. 26 (1993), pp. 763-773

Bolduan-1949: Orvil E. A. Bolduan and Richard S. Bear, ”Effective Use of Collimating Apertures in SmallAngle XRay Diffraction Cameras”, J. Appl. Phys. 20, 983 (1949); doi: 10.1063/1.1698263

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Free Code! McSAS: A Monte-Carlo way for retrieving particle size distributions.

Good news for those of you on the hunt for a way to get polydispersity (size distribution) information from your scattering patterns. Two pieces of good news, to be precise!

A combined dataset (left) fitted using a Monte-Carlo method for size distribution retrieval. The volume-weighted size distribution is shown on the right on arbitrary scale.

A combined dataset (left) fitted using the Monte-Carlo method for size distribution retrieval. The volume-weighted size distribution is shown on the right on arbitrary scale.

Firstly, the paper that describes my implementation of the method that does exactly this has just been accepted earlier this month for publication in J. Appl. Cryst, though it will probably not make it into the February issue. With a bit of luck, I will be able to make it open access, though! I have talked about the method before (e.g. here) so I will not spend more words on it.

The second news is that the Python code with the fitting procedure is now available in an online repository here, thanks to Pawel Kwasniew at ESRF for his efforts in setting up the repository. The code comes complete with a quickstart guide with several pictures and some test data. If you are reasonably familiar with Python, why not grab a copy and try the method on your data? Reports from early testers have been positive, and everyone is encouraged to comment or send me an e-mail so it can be improved. License-wise, the code is released under a creative-commons-attribution-sharealike license.

Lastly, if you want to contribute to the code you are more than welcome to. Currently, the code is being recoded in object-oriented form to improve flexibility, with the first release of the OO version expected later this month. Afterwards, a smearing function will be implemented for directly fitting slit-smeared data, and more shape functions should be included. As it is intended to be integrated in existing SAS analysis GUI’s (of which there are quite a few), there is no graphical user interface, and as such the focus is on getting the base functionality implemented right.

As usual, drop me a line or leave a comment!

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A new year, seven publications to write and a short movie

Dear scatterers,

First of all, allow me to wish you a very happy 2013, wishing you much comfort, many good meetings and world peace.

With that out of the way, this year might be different from others on this weblog, as I have to spend oodles of time on my “favourite” activity: trying to publish. Since there were hardly any publications last year, this year must be better (or I will “perish”, as the saying goes). There are seven publications in the pipeline as indicated by the title, though only three with me as first author. So please check the website’s “publications” section by the end of this year, and you will see how far I’ve managed to come with that by then.

One of the publications that hopefully will come out first is on the 1D Monte-Carlo method, which will allow for the retrieval of form-free size distributions after assuming an elementary shape (spheres are the prime choice, but it also works with isotropic cylinders). On top of that, it will give you uncertainties on the size distributions the quality and reliability of which are directly related to the uncertainties on your measured intensities. Anyway, once that is published, rest assured that I will announce it here (it has been one hurdle for me, so I will be very happy to see it out there).

The Python code used for this is freely available, currently the final touches are being put on a good, clean variant which should be available very soon. For the restless, please drop me a line and the code can be sent your way.

Other publications will be about (amongst others) the 2D Monte-Carlo method for anisotropic scattering patterns, as presented at the SAS2012 conference, and a paper applying the 1D Monte-Carlo method to precipitate growth in magnesium alloys (the ArXiv link to an early draft was posted a few weeks ago here: arXiv:1210.5366). So all in all, this will be a busy year when it comes to paperwork.

Anyway, I do not want to remain in the shadows for the entire year, so I decided to upload some more videos this year. I started the series off with a short explanation on the “classical” way of fitting scattering patterns, in a short demonstration that I used at SAS2012. This recording (shown below, or on youtube here) was simple and quick, and your host was suffering from an allergy attack, so please forgive the movie its faults. I hope it is fun nonetheless, and with this, I will sign off on this blog post. Another post will be ready in a few weeks!

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