{"id":4849,"date":"2026-05-26T13:28:02","date_gmt":"2026-05-26T12:28:02","guid":{"rendered":"https:\/\/lookingatnothing.com\/?p=4849"},"modified":"2026-05-26T13:28:03","modified_gmt":"2026-05-26T12:28:03","slug":"hot-off-the-press-grilling-composites-in-the-beam","status":"publish","type":"post","link":"https:\/\/lookingatnothing.com\/index.php\/archives\/4849","title":{"rendered":"Hot off the press: grilling composites in the beam"},"content":{"rendered":"\n<p>On Monday, I found myself and two students on I22 at the Diamond Light Source, also known as my favourite small-angle scattering synchrotron beamline. There, we&#8217;ve been sintering composites (in atmosphere at up to 1200\u02daC) in a USAXS\/SAXS\/WAXS experiment as part of our long-running collaboration with the group of <a href=\"https:\/\/www.bam.de\/Content\/EN\/Standard-Articles\/Topics\/junio-research-group-johanna-saenger.html\">Dr. Johanna M\u00fcller-Elmau<\/a>. As the beamtime is only 24h, it required careful planning and preparation. Here&#8217;s how it worked out&#8230;<\/p>\n\n\n\n<!--more-->\n\n\n\n<h2 class=\"wp-block-heading\">Why only 24h?<\/h2>\n\n\n\n<p>Synchrotrons are large facilities producing beams with high X-ray fluxes, ideal for fast experiments. The better synchrotrons have oodles of scientists clamouring for a chance to measure, with a peer review panel trying to figure out which experiments should go on in the next period (more on writing beamtime proposals <a href=\"https:\/\/lookingatnothing.com\/index.php\/archives\/3876\">here<\/a>). Despite its age, the I22 beamline at the DLS remains in very high demand due to the quality of data it produces and the amazing scientists that keep it afloat. With the addition of our jointly-developed USAXS module &#8211; now thoroughly improved by the I22 team &#8211; and the universal data correction pipeline we developed, it has everything we need for our upcoming experiment.<\/p>\n\n\n\n<p>That said, 24h is still a very short amount of time, especially considering we&#8217;ll spend 4-8h getting the set-up in place before we can get true measurements. I could have asked for more time in the proposal, with normal experiments asking for two to four days of beamtime. But there are a couple of reasons why I didn&#8217;t for this one:<\/p>\n\n\n\n<ul class=\"wp-block-list\">\n<li>There&#8217;s a law of diminishing returns. For this investigation to be a success, we really only need one measurement series to work well. If we had 24h more, the outcome would not become twice as good or have twice the chance of success. With each measurement series taking at least four hours, this means that we can run three to four full attempts in a 16h period.<\/li>\n\n\n\n<li>This is the first time we try this complex experiment and equipment on the beamline. Either it works and 16h will be sufficient, or something fails, and we&#8217;ll cry for 16h, but there&#8217;s no way I could solve show-stoppers with an additional 24h tacked on. If an unforeseen showstopper appears, it is more than likely that it will need some thoughtful, in-depth solution rather than some duct tape.<\/li>\n\n\n\n<li>As I am painfully aware as a peer review panelist, there are many other good experiments that need I22. I cannot justify taking more time than I would absolutely need. I&#8217;d rather go home, assess and reapply for more beamtime if the data demands it. Trying to avoid the tragedy of the commons, we take only what we need.<\/li>\n<\/ul>\n\n\n\n<h2 class=\"wp-block-heading\">Grilling for pros&#8230;<\/h2>\n\n\n\n<p>When we were preparing the application, we had a good look at the high-temperature stages available to us, and decided in the end to design something new (more on that <a href=\"https:\/\/lookingatnothing.com\/index.php\/archives\/4768\">here<\/a>). Over the last months, the fantastic in-house workshop staff churned out the parts at an astonishing rate, allowing us to thoroughly test the design. One such test even involved me tapping the oven with a spanner to identify another weak spot in the design.<\/p>\n\n\n\n<figure class=\"wp-block-image size-medium is-resized\"><a href=\"https:\/\/lookingatnothing.com\/wp-content\/uploads\/2026\/05\/image.png\"><img loading=\"lazy\" decoding=\"async\" width=\"300\" height=\"209\" src=\"https:\/\/lookingatnothing.com\/wp-content\/uploads\/2026\/05\/image-300x209.png\" alt=\"\" class=\"wp-image-4850\" style=\"width:800px\" srcset=\"https:\/\/lookingatnothing.com\/wp-content\/uploads\/2026\/05\/image-300x209.png 300w, https:\/\/lookingatnothing.com\/wp-content\/uploads\/2026\/05\/image-1024x712.png 1024w, https:\/\/lookingatnothing.com\/wp-content\/uploads\/2026\/05\/image-768x534.png 768w, https:\/\/lookingatnothing.com\/wp-content\/uploads\/2026\/05\/image-1536x1068.png 1536w, https:\/\/lookingatnothing.com\/wp-content\/uploads\/2026\/05\/image-2048x1424.png 2048w\" sizes=\"auto, (max-width: 300px) 100vw, 300px\" \/><\/a><figcaption class=\"wp-element-caption\">Figure 1: An early test of the &#8220;Hot Pocket&#8221;. At full blast, this requires ~250 W of low-voltage DC power to reach 1200\u02daC. The water-cooled aluminium housing remains at room temperature and can be safely handled. <\/figcaption><\/figure>\n\n\n\n<p>The result is an amazing tiny tube oven (now dubbed the &#8220;Hot Pocket&#8221; as it&#8217;s uncannily hot inside the cold exterior). It measures 20 mm in the beam direction, and about 40&#215;50 mm perpendicular to the beam, not counting connections and cables. Its capabilities have not been fully tested, but it is capable of heating rates in excess of 200\u02daC\/min, at least at the lower end of the temperature range. After a few more iterations, the design now seems very sturdy, though it still requires additional air cooling of the positive coil terminal. We even developed 3D-printed coil winding tools, prepared and pre-treated a total of three coils for the experiment in case of failure, and have a host of spare parts with us. A little L-bracket with collet has been added to mount the thermocouple and sample.<\/p>\n\n\n\n<figure class=\"wp-block-image size-medium is-resized\"><a href=\"https:\/\/lookingatnothing.com\/wp-content\/uploads\/2026\/05\/image-1.png\"><img loading=\"lazy\" decoding=\"async\" width=\"300\" height=\"300\" src=\"https:\/\/lookingatnothing.com\/wp-content\/uploads\/2026\/05\/image-1-edited-300x300.png\" alt=\"\" class=\"wp-image-4852\" style=\"width:800px\" srcset=\"https:\/\/lookingatnothing.com\/wp-content\/uploads\/2026\/05\/image-1-edited-300x300.png 300w, https:\/\/lookingatnothing.com\/wp-content\/uploads\/2026\/05\/image-1-edited-1024x1024.png 1024w, https:\/\/lookingatnothing.com\/wp-content\/uploads\/2026\/05\/image-1-edited-150x150.png 150w, https:\/\/lookingatnothing.com\/wp-content\/uploads\/2026\/05\/image-1-edited-768x768.png 768w, https:\/\/lookingatnothing.com\/wp-content\/uploads\/2026\/05\/image-1-edited.png 1244w\" sizes=\"auto, (max-width: 300px) 100vw, 300px\" \/><\/a><figcaption class=\"wp-element-caption\">Figure 2: The pre-baked coil, Macor lid, and ceramic tube with the X-ray beam hole in place. the inside diameter of the ceramic tube, i.e. the space available for samples, measures 5 mm. <\/figcaption><\/figure>\n\n\n\n<p>Advantages of this design include its minuscule footprint, safe operation (low-voltage DC power, no easily accessible hotspots on the outside even at full power), and the ability to insert a range of samples including samples mounted in capillaries. The disadvantage of this design is that it requires the insertion of an N-type thermocouple into the tube as well. In our case, we&#8217;re mounting the sample on the tip of a thermocouple, so it doubles as a sample mount, but in the case of capillaries, one will need to carefully consider its position.<\/p>\n\n\n\n<p>We had made an attempt to also use custom 3D-printed ceramic components inside (a custom tube as well as a ceramic sample carrier), but unfortunately these did not survive their final sintering step. Maybe next time. <\/p>\n\n\n\n<figure class=\"wp-block-image size-medium is-resized\"><a href=\"https:\/\/lookingatnothing.com\/wp-content\/uploads\/2026\/05\/image-4.png\"><img loading=\"lazy\" decoding=\"async\" width=\"300\" height=\"174\" src=\"https:\/\/lookingatnothing.com\/wp-content\/uploads\/2026\/05\/image-4-300x174.png\" alt=\"\" class=\"wp-image-4859\" style=\"width:800px\" srcset=\"https:\/\/lookingatnothing.com\/wp-content\/uploads\/2026\/05\/image-4-300x174.png 300w, https:\/\/lookingatnothing.com\/wp-content\/uploads\/2026\/05\/image-4-1024x593.png 1024w, https:\/\/lookingatnothing.com\/wp-content\/uploads\/2026\/05\/image-4-768x445.png 768w, https:\/\/lookingatnothing.com\/wp-content\/uploads\/2026\/05\/image-4-1536x890.png 1536w, https:\/\/lookingatnothing.com\/wp-content\/uploads\/2026\/05\/image-4-2048x1186.png 2048w\" sizes=\"auto, (max-width: 300px) 100vw, 300px\" \/><\/a><figcaption class=\"wp-element-caption\">Figure 3: the temperature controller and the DC power supply connected to it, at the maximum temperature we tested. <\/figcaption><\/figure>\n\n\n\n<p>At the beamline, the oven performed very well. We connected the DC power supply up to the proportional output of a Eurotherm controller, which, when tuned at 1000\u02daC, managed very well to keep the ramps and temperatures. The proportional output was used to control the voltage on the coil, leading to a smooth response. At the maximum temperature of the experiment, the glow emitted by the oven is something to behold. <\/p>\n\n\n\n<figure class=\"wp-block-image size-large is-resized\"><a href=\"https:\/\/lookingatnothing.com\/wp-content\/uploads\/2026\/05\/image-3.png\"><img loading=\"lazy\" decoding=\"async\" width=\"1024\" height=\"768\" src=\"https:\/\/lookingatnothing.com\/wp-content\/uploads\/2026\/05\/image-3-1024x768.png\" alt=\"\" class=\"wp-image-4858\" style=\"width:800px\" srcset=\"https:\/\/lookingatnothing.com\/wp-content\/uploads\/2026\/05\/image-3-1024x768.png 1024w, https:\/\/lookingatnothing.com\/wp-content\/uploads\/2026\/05\/image-3-300x225.png 300w, https:\/\/lookingatnothing.com\/wp-content\/uploads\/2026\/05\/image-3-768x576.png 768w, https:\/\/lookingatnothing.com\/wp-content\/uploads\/2026\/05\/image-3-1536x1151.png 1536w, https:\/\/lookingatnothing.com\/wp-content\/uploads\/2026\/05\/image-3-2048x1535.png 2048w, https:\/\/lookingatnothing.com\/wp-content\/uploads\/2026\/05\/image-3-678x509.png 678w, https:\/\/lookingatnothing.com\/wp-content\/uploads\/2026\/05\/image-3-326x245.png 326w, https:\/\/lookingatnothing.com\/wp-content\/uploads\/2026\/05\/image-3-80x60.png 80w\" sizes=\"auto, (max-width: 1024px) 100vw, 1024px\" \/><\/a><figcaption class=\"wp-element-caption\">Figure 4: The glow of the oven at full power nicely illuminates the equipment at the beamline. The two USAXS crystal cages can be seen on either side of the oven. <\/figcaption><\/figure>\n\n\n\n<h2 class=\"wp-block-heading\">&#8230;with a little help from our friends<\/h2>\n\n\n\n<p>None of this would have even been developed if we did not have engaged and helpful colleagues from the synchrotron to help with the development and set-up process. Regular cross-checking with them to leverage their experience led to a few early adaptations of the design to make it easier to handle and integrate on the end station. When it seemed we would be facing issues with the availability of the N-type thermocouples, they ordered a spare. They received and tested our secondary DC power supply beforehand as well.<\/p>\n\n\n\n<p>The short experiment also relied on the time savings from the USAXS being in place already (from previous experiments) and configured for a photon energy of 14 keV. This energy is one of the modes of their undulator and optics, and neatly avoids the absorption\/fluorescence edge of the elements in our composites.<\/p>\n\n\n\n<p>All this highlights how important it is to talk to your beamline manager \/ beamline responsible before your experiment so that any details can be ironed out *before* they become a problem. <\/p>\n\n\n\n<h2 class=\"wp-block-heading\">Samples and dumps<\/h2>\n\n\n\n<p>While we knew that in this experiment we would only be able to measure at most a handful of samples (due to the slow ramp profile), we still prepared about 20 disc-shaped samples in total of the same resin. The samples &#8211; consisting of zirconia nanoparticles in a polymer matrix &#8211; were prepared in different thicknesses to be able to address potential problems with sensitivity or multiple scattering. Several of each thickness were prepared to make sure we had enough spares in case the loading would prove more difficult. These discs were then cut to 4 mm by about 10 mm and mounted in a platinum wire structure attached to the thermocouple end.<\/p>\n\n\n\n<figure class=\"wp-block-image size-medium is-resized\"><a href=\"https:\/\/lookingatnothing.com\/wp-content\/uploads\/2026\/05\/image-5.png\"><img loading=\"lazy\" decoding=\"async\" width=\"300\" height=\"150\" src=\"https:\/\/lookingatnothing.com\/wp-content\/uploads\/2026\/05\/image-5-300x150.png\" alt=\"\" class=\"wp-image-4864\" style=\"width:800px\" srcset=\"https:\/\/lookingatnothing.com\/wp-content\/uploads\/2026\/05\/image-5-300x150.png 300w, https:\/\/lookingatnothing.com\/wp-content\/uploads\/2026\/05\/image-5-1024x512.png 1024w, https:\/\/lookingatnothing.com\/wp-content\/uploads\/2026\/05\/image-5-768x384.png 768w, https:\/\/lookingatnothing.com\/wp-content\/uploads\/2026\/05\/image-5-1536x769.png 1536w, https:\/\/lookingatnothing.com\/wp-content\/uploads\/2026\/05\/image-5-2048x1025.png 2048w\" sizes=\"auto, (max-width: 300px) 100vw, 300px\" \/><\/a><figcaption class=\"wp-element-caption\">Figure 5: one toasted sample. The total height of the sample holder is about 4 mm, the diameter of the N-type thermocouple it&#8217;s mounted on is 1.5 mm. <\/figcaption><\/figure>\n\n\n\n<p>Minor issues with scripting and a very careful initial temperature profile meant the first sample took almost 7h to finish. At the very end of that run, a beam dump meant we could not start with the second sample for several hours, and that the downstream USAXS crystal was out of alignment. A second sample was measured with only SAXS\/WAXS up to 1000\u02daC, and immediately after that, a second beam dump occurred which unfortunately meant we reached the end of our experiment. Nevertheless, we collected two very rich datasets of grilling composite samples, and were lucky to have the beam dumps at the end of the individual ramps, when valuable data had already been collected.<\/p>\n\n\n\n<figure class=\"wp-block-image size-medium is-resized\"><a href=\"https:\/\/lookingatnothing.com\/wp-content\/uploads\/2026\/05\/image-6.png\"><img loading=\"lazy\" decoding=\"async\" width=\"300\" height=\"206\" src=\"https:\/\/lookingatnothing.com\/wp-content\/uploads\/2026\/05\/image-6-300x206.png\" alt=\"\" class=\"wp-image-4868\" style=\"width:800px\" srcset=\"https:\/\/lookingatnothing.com\/wp-content\/uploads\/2026\/05\/image-6-300x206.png 300w, https:\/\/lookingatnothing.com\/wp-content\/uploads\/2026\/05\/image-6-1024x703.png 1024w, https:\/\/lookingatnothing.com\/wp-content\/uploads\/2026\/05\/image-6-768x528.png 768w, https:\/\/lookingatnothing.com\/wp-content\/uploads\/2026\/05\/image-6-1536x1055.png 1536w, https:\/\/lookingatnothing.com\/wp-content\/uploads\/2026\/05\/image-6-2048x1407.png 2048w\" sizes=\"auto, (max-width: 300px) 100vw, 300px\" \/><\/a><figcaption class=\"wp-element-caption\">Figure 6: Tom, me and Finn at the I22 beamline after the experiment<\/figcaption><\/figure>\n\n\n\n<h2 class=\"wp-block-heading\">Where are we now?<\/h2>\n\n\n\n<p>The two datasets now require careful reprocessing to bring them in line (and to absolute units), after which we have to sit down and do some serious analysis of the data. Separate models are needed for the WAXS, SAXS and USAXS data, the latter of which is slit-smeared. In the composite, we have (very) densely packed, polydisperse particles, so we may have a bit of a challenge on our hands there. We will also remeasure the material on the MOUSE for checks of scaling and signal, so there&#8217;s still a bit of work to be done. <\/p>\n\n\n\n<figure class=\"wp-block-image size-large\"><a href=\"https:\/\/lookingatnothing.com\/wp-content\/uploads\/2026\/05\/almost_processed_data.png\"><img loading=\"lazy\" decoding=\"async\" width=\"943\" height=\"1024\" src=\"https:\/\/lookingatnothing.com\/wp-content\/uploads\/2026\/05\/almost_processed_data-943x1024.png\" alt=\"\" class=\"wp-image-4875\" srcset=\"https:\/\/lookingatnothing.com\/wp-content\/uploads\/2026\/05\/almost_processed_data-943x1024.png 943w, https:\/\/lookingatnothing.com\/wp-content\/uploads\/2026\/05\/almost_processed_data-276x300.png 276w, https:\/\/lookingatnothing.com\/wp-content\/uploads\/2026\/05\/almost_processed_data-768x834.png 768w, https:\/\/lookingatnothing.com\/wp-content\/uploads\/2026\/05\/almost_processed_data.png 972w\" sizes=\"auto, (max-width: 943px) 100vw, 943px\" \/><\/a><figcaption class=\"wp-element-caption\">Figure 7: A portion of the semi-processed USAXS, SAXS and WAXS dataset of the experiments, showing a detailed evolution of the materials structure on sintering across all regions. <\/figcaption><\/figure>\n\n\n\n<p>Despite the challenges, I&#8217;m very happy with the result: we got the dataset we were aiming for, and the equipment performed flawlessly. The results will hopefully tie in very well with the in-situ TEM sintering that was done on these materials a while back, and should make for a very interesting story. Eventually, when we have milked the data for the knowledge, we may return with a more targeted plan for a new adventure. <\/p>\n\n\n\n<p><\/p>\n","protected":false},"excerpt":{"rendered":"<div class=\"mh-excerpt\"><p>On Monday, I found myself and two students on I22 at the Diamond Light Source, also known as my favourite small-angle scattering synchrotron beamline. There, <a class=\"mh-excerpt-more\" href=\"https:\/\/lookingatnothing.com\/index.php\/archives\/4849\" title=\"Hot off the press: grilling composites in the beam\">[&#8230;]<\/a><\/p>\n<\/div>","protected":false},"author":2,"featured_media":4858,"comment_status":"closed","ping_status":"open","sticky":false,"template":"","format":"standard","meta":{"jetpack_post_was_ever_published":false,"_jetpack_newsletter_access":"","_jetpack_dont_email_post_to_subs":false,"_jetpack_newsletter_tier_id":0,"_jetpack_memberships_contains_paywalled_content":false,"_jetpack_memberships_contains_paid_content":false,"activitypub_content_warning":"","activitypub_content_visibility":"","activitypub_max_image_attachments":4,"activitypub_interaction_policy_quote":"anyone","activitypub_status":"federated","footnotes":"","jetpack_publicize_message":"","jetpack_publicize_feature_enabled":true,"jetpack_social_post_already_shared":true,"jetpack_social_options":{"image_generator_settings":{"template":"highway","default_image_id":0,"font":"","enabled":false},"version":2}},"categories":[1],"tags":[],"class_list":["post-4849","post","type-post","status-publish","format-standard","has-post-thumbnail","hentry","category-uncategorized"],"jetpack_publicize_connections":[],"jetpack_featured_media_url":"https:\/\/lookingatnothing.com\/wp-content\/uploads\/2026\/05\/image-3.png","jetpack_shortlink":"https:\/\/wp.me\/p1gZ2v-1gd","jetpack_sharing_enabled":true,"_links":{"self":[{"href":"https:\/\/lookingatnothing.com\/index.php\/wp-json\/wp\/v2\/posts\/4849","targetHints":{"allow":["GET"]}}],"collection":[{"href":"https:\/\/lookingatnothing.com\/index.php\/wp-json\/wp\/v2\/posts"}],"about":[{"href":"https:\/\/lookingatnothing.com\/index.php\/wp-json\/wp\/v2\/types\/post"}],"author":[{"embeddable":true,"href":"https:\/\/lookingatnothing.com\/index.php\/wp-json\/wp\/v2\/users\/2"}],"replies":[{"embeddable":true,"href":"https:\/\/lookingatnothing.com\/index.php\/wp-json\/wp\/v2\/comments?post=4849"}],"version-history":[{"count":19,"href":"https:\/\/lookingatnothing.com\/index.php\/wp-json\/wp\/v2\/posts\/4849\/revisions"}],"predecessor-version":[{"id":4877,"href":"https:\/\/lookingatnothing.com\/index.php\/wp-json\/wp\/v2\/posts\/4849\/revisions\/4877"}],"wp:featuredmedia":[{"embeddable":true,"href":"https:\/\/lookingatnothing.com\/index.php\/wp-json\/wp\/v2\/media\/4858"}],"wp:attachment":[{"href":"https:\/\/lookingatnothing.com\/index.php\/wp-json\/wp\/v2\/media?parent=4849"}],"wp:term":[{"taxonomy":"category","embeddable":true,"href":"https:\/\/lookingatnothing.com\/index.php\/wp-json\/wp\/v2\/categories?post=4849"},{"taxonomy":"post_tag","embeddable":true,"href":"https:\/\/lookingatnothing.com\/index.php\/wp-json\/wp\/v2\/tags?post=4849"}],"curies":[{"name":"wp","href":"https:\/\/api.w.org\/{rel}","templated":true}]}}