A plywood box with a clear plastic front is shown. Three needle gauges are visible on the front of the box, as well as a digital display, several switches, and some indicator lights. At the right of the box, a short copper tube extends from the box.

Building An X-Ray Crystallography Machine

X-ray crystallography, like mass spectroscopy and nuclear spectroscopy, is an extremely useful material characterization technique that is unfortunately hard for amateurs to perform. The physical operation isn’t too complicated, however, and as [Farben-X] shows, it’s entirely possible to build an X-ray diffractometer if you’re willing to deal with high voltages, ancient X-ray tubes, and soft X-rays.

[Farben-X] based his diffractometer around an old Soviet BSV-29 structural analysis X-ray tube, which emits X-rays through four beryllium windows. Two ZVS drivers power the tube: one to drive the electron gun’s filament, and one to feed a flyback transformer and Cockroft-Walton voltage multiplier which generate a potential across the tube. The most important part of the imaging system is the X-ray collimator, which [Farben-X] made out of a lead disk with a copper tube mounted in it. A 3D printer nozzle screws into each end of the tube, creating a very narrow path for X-rays, and thus a thin, mostly collimated beam.

To get good diffraction patterns from a crystal, it needed to be a single crystal, and to actually let the X-ray beam pass through, it needed to be a thin crystal. For this, [Farben-X] selected a sodium chloride crystal, a menthol crystal, and a thin sheet of mica. To grow large salt crystals, he used solvent vapor diffusion, which slowly dissolves a suitable solvent vapor in a salt solution, which decreases the salt’s solubility, leading to very slow, fine crystal growth. Afterwards, he redissolved portions of the resulting crystal to make it thinner.

The diffraction pattern generated by a sodium chloride crystal. A slide is shown with a dark black dot in the middle, surrounded by fainter dots.
The diffraction pattern generated by a sodium chloride crystal.

For the actual experiment, [Farben-X] passed the X-ray beam through the crystals, then recorded the diffraction patterns formed on a slide of X-ray sensitive film. This created a pattern of dots around the central beam, indicating diffracted beams. The mathematics for reverse-engineering the crystal structure from this is rather complicated, and [Farben-X] hadn’t gotten to it yet, but it should be possible.

We would recommend a great deal of caution to anyone considering replicating this – a few clips of X-rays inducing flashes in the camera sensor made us particularly concerned – but we do have to admire any hack that coaxed such impressive results out of such a rudimentary setup. If you’re interested in further reading, we’ve covered the basics of X-ray crystallography before. We’ve also seen a few X-ray machines.

An electron microscope image of the aluminum alloy from the study.

D20-shaped Quasicrystal Makes High-Strength Alloy Printable

When is a crystal not a crystal? When it’s a quasi-crystal, a paradoxical form of metal recently found in some 3D printed metal alloys by [A.D. Iams et al] at the American National Institute for Standards and Technology (NIST).

As you might remember from chemistry class, crystals are made up of blocks of atoms (usually called ‘unit cells’) that fit together in perfect repetition — baring dislocations, cracks, impurities, or anything else that might throw off a theoretically perfect crystal structure. There are only so many ways to tessellate atoms in 3D space; 230 of them, to be precise. A quasicrystal isn’t any of them. Rather than repeat endlessly in 3D space, a quasicrystal never repeats perfectly, like a 3D dimensional Penrose tile. The discovery of quasicrystals dates back to the 1980s, and was awarded a noble prize in 2011.

Penrose tiling of thick and thin rhombi
Penrose tiling– the pattern never repeats perfectly. Quasicrystals do this in 3D. (Image by Inductiveload, Public Domain)

Quasicrystals aren’t exactly common in nature, so how does 3D printing come into this? Well, it turns out that, quite accidentally, a particular Aluminum-Zirconium alloy was forming small zones of quasicrystals (the black spots in the image above) when used in powder bed fusion printing. Other high strength-alloys tended to be very prone to cracking, to the point of unusability, and this Al-Zr alloy, discovered in 2017, was the first of its class.

You might imagine that the non-regular structure of a quasicrystal wouldn’t propagate cracks as easily as a regular crystal structure, and you would be right! The NIST researchers obviously wanted to investigate why the printable alloy had the properties it does. When their crystallographic analysis showed not only five-fold, but also three-fold and two-fold rotational symmetry when examined from different angles, the researchers realized they had a quasicrystal on their hands. The unit cell is in the form of a 20-sided icosahedron, providing the penrose-style tiling that keeps the alloy from cracking.

You might say the original team that developed the alloy rolled a nat-20 on their crafting skill. Now that we understand why it works, this research opens up the doors for other metallic quasi-crystals to be developed on purpose, in aluminum and perhaps other alloys.

We’ve written about 3D metal printers before, and highlighted a DIY-able plastic SLS kit, but the high-power powder-bed systems needed for aluminum aren’t often found in makerspaces. If you’re building one or know someone who is, be sure to let us know.

Iron Nitrides: Powerful Magnets Without The Rare Earth Elements

Since their relatively recent appearance on the commercial scene, rare-earth magnets have made quite a splash in the public imagination. The amount of magnetic energy packed into these tiny, shiny objects has led to technological leaps that weren’t possible before they came along, like the vibration motors in cell phones, or the tiny speakers in earbuds and hearing aids. And that’s not to mention the motors in electric vehicles and the generators in wind turbines, along with countless medical, military, and scientific uses.

These advances come at a cost, though, as the rare earth elements needed to make them are getting harder to come by. It’s not that rare earth elements like neodymium are all that rare geologically; rather, deposits are unevenly distributed, making it easy for the metals to become pawns in a neverending geopolitical chess game. What’s more, extracting them from their ores is a tricky business in an era of increased sensitivity to environmental considerations.

Luckily, there’s more than one way to make a magnet, and it may soon be possible to build permanent magnets as strong as neodymium magnets, but without any rare earth metals. In fact, the only thing needed to make them is iron and nitrogen, plus an understanding of crystal structure and some engineering ingenuity.

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Ask Hackaday: What Can Only A Computer Do?

It is easy to apply computers to improve things we already understand. For example, instead of a piano today, you might buy a synthesizer. It looks and works — sometimes — as a piano. But it can also do lots of other things like play horns, or accompany you with a rhythm track or record and playback your music. There’s plenty of examples of this: word processors instead of typewriters, MP3 players instead of tape decks, and PDF files instead of printed material. But what about something totally new? I was thinking of this while looking at Sonic Pi, a musical instrument you play by coding.

But back to the keyboard, the word processor, and the MP3 player. Those things aren’t so much revolutionary as they are evolutionary. Even something like digital photography isn’t all that revolutionary. Sure, most of us couldn’t do all the magic you can do in PhotoShop in a dark room, but some wizards could. Most of us couldn’t lay out a camera-ready brochure either, but people did it every day without the benefit of computers. So what are the things that we are using computers for that are totally new? What can you do with the help of a computer that you absolutely couldn’t without?

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Kathleen Lonsdale Saw Through The Structure Of Benzene

The unspoken promise of new technologies is that they will advance and enhance our picture of the world — that goes double for the ones that are specifically designed to let us look closer at the physical world than we’ve ever been able to before. One such advancement was the invention of X-ray crystallography that let scientists peer into the spatial arrangements of atoms within a molecule. Kathleen Lonsdale got in on the ground floor of X-ray crystallography soon after its discovery in the early 20th century, and used it to prove conclusively that the benzene molecule is a flat hexagon of six carbon atoms, ending a decades-long scientific dispute once and for all.

Benzene is an organic chemical compound in the form of a colorless, flammable liquid. It has many uses as an additive in gasoline, and it is used to make plastics and synthetic rubber. It’s also a good solvent. Although the formula for benzene had been known for a long time, the dimensions and atomic structure remained a mystery for more than sixty years.

Kathleen Lonsdale was a crystallography pioneer and developed several techniques to study crystal structures using X-rays. She was brilliant, but she was also humble, hard-working, and adaptable, particularly as she managed three young children and a budding chemistry career. At the outbreak of World War II, she spent a month in jail for reasons related to her staunch pacifism, and later worked toward prison reform, visiting women’s prisons habitually.

After the war, Kathleen traveled the world to support movements that promote peace and was often asked to speak on science, religion, and the role of women in science. She received many honors in her lifetime, and became a Dame of the British Empire in 1956. Before all of that, she honored organic chemistry with her contributions.

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A Beginner’s Guide To X-Ray Crystallography

In graduate school, I had a seminar course where one of the sections was about X-ray crystallography. I was excited, because being able to discern the three-dimensional structure of macromolecules just by shining X-rays on them seemed like magic to me. And thanks to a lackluster professor, after the section it remained just as much of a mystery.

If only I’d had [Steve Mould] as a teacher back then. His latest video does an outstanding job explaining X-ray crystallography by scaling up the problem considerably, using the longer wavelength of light and a macroscopic target. He begins with a review of diffraction patterns, those alternating light and dark bands of constructive and destructive interference that result when light shines on two closely spaced slits — the famous “Double-Slit Experiment” that showed light behaves both as a particle and as a wave and provided our first glimpse of quantum mechanics. [Steve] then doubled down on the double-slit, placing another pair of slits in the path of the first. This revealed a grid of spots rather than alternating bands, with the angle between axes dependent on the angle of the slit pairs to each other.

 

To complete the demonstration, [Steve] then used diffraction to image the helical tungsten filament of an incandescent light bulb. Shining a laser through the helix resulted in a pattern bearing a striking resemblance to what’s probably the most famous X-ray crystallogram ever: [Rosalind Franklin]’s portrait of DNA. It all makes perfect sense, and it’s easy to see how the process works when scaled down both in terms of the target size and the wavelength of light used to probe it.

Hats off to [Steve] for making something that’s ordinarily complex so easily understandable, and for filling in a long-standing gap in my knowledge.

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Rosalind Franklin Saw DNA First

It’s a standard science trivia question: Who discovered the structure of DNA? With the basic concepts of molecular biology now taught at a fairly detailed level in grade school, and with DNA being so easy to isolate that it makes a good demonstration project for school or home, everyone knows the names of Watson and Crick. But not many people know the story behind one of the greatest scientific achievements of the 20th century, or the name of the scientist without whose data Watson and Crick were working blind: Rosalind Franklin.

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