The bed of a small CNC machine is shown. A plastic tub is on the bed, and in the tub is a sheet of metal under a pale green solution. In place of the spindle of the CNC, there is a rectangular orange tube extending down into the solution. A red wire runs to this tube, and a black wire runs to the sheet of metal in the tub.

Painting In Metal With Selective Electroplating

Most research on electroplating tries to find ways to make it plate parts more uniformly. [Ajc150] took the opposite direction, though, with his selective electroplating project, which uses an electrode mounted on a CNC motion system to electrochemically print images onto a metal sheet (GitHub repository).

Normally, selective electroplating would use a mask, but masks don’t allow gradients to be deposited. However, electroplating tends to occur most heavily at the point closest to the anode, and the effect gets stronger the closer the anode is. To take advantage of this effect, [ajc150] replaced the router of an inexpensive 3018 CNC machine with a nickel anode, mounted an electrolyte bath in the workspace, and laid a flat steel cathode in it. When the anode moves close to a certain point on the steel cathode, most of the plating takes place there.

To actually print an image with this setup, [ajc150] wrote a Python program to convert an image into set of G-code instructions for the CNC. The darker a pixel of the image was, the longer the electrode would spend over the corresponding part of the metal sheet. Since darkness wasn’t linearly proportional to plating time, the program used a gamma correction function to adjust times, though this did require [ajc150] to recalibrate the setup after each change. The system works well enough to print recognizable images, but still has room for improvement. In particular, [ajc150] would like to extend this to a faster multi-nozzle system, and have the algorithm take into account spillover between the pixel being plated and its neighbors.

This general technique is reminiscent of a metal 3D printing method we’ve seen before. We more frequently see this process run in reverse to cut metal.

A cylindrical red furnace is in the center of the image. To the left of it is a black power supply. A stand is in front of the furnace, with an arm extending over the furnace. To the right of the furnace, a pair of green-handled crucible tongs sit on an aluminium pan.

The Hall-Héroult Process On A Home Scale

Although Charles Hall conducted his first successful run of the Hall-Héroult aluminium smelting process in the woodshed behind his house, it has ever since remained mostly out of reach of home chemists. It does involve electrolysis at temperatures above 1000 ℃, and can involve some frighteningly toxic chemicals, but as [Maurycy Z] demonstrates, an amateur can now perform it a bit more conveniently than Hall could.

[Maurycy] started by finding a natural source of aluminium, in this case aluminosilicate clay. He washed the clay and soaked it in warm hydrochloric acid for two days to extract the aluminium as a chloride. This also extracted quite a bit of iron, so [Maurycy] added sodium hydroxide to the solution until both aluminium and iron precipitated as hydroxides, added more sodium hydroxide until the aluminium hydroxide redissolved, filtered the solution to remove iron hydroxide, and finally added hydrochloric acid to the solution to precipitate aluminium hydroxide. He heated the aluminium hydroxide to about 800 ℃ to decompose it into the alumina, the starting material for electrolysis.

To turn this into aluminium metal, [Maurycy] used molten salt electrolysis. Alumina melts at a much higher temperature than [Maurycy]’s furnace could reach, so he used cryolite as a flux. He mixed this with his alumina and used an electric furnace to melt it in a graphite crucible. He used the crucible itself as the cathode, and a graphite rod as an anode. He does warn that this process can produce small amounts of hydrogen fluoride and fluorocarbons, so that “doing the electrolysis without ventilation is a great way to poison yourself in new and exciting ways.” The first run didn’t produce anything, but on a second attempt with a larger anode, 20 minutes of electrolysis produced 0.29 grams of aluminium metal.

[Maurycy]’s process follows the industrial Hall-Héroult process quite closely, though he does use a different procedure to purify his raw materials. If you aren’t interested in smelting aluminium, you can still cast it with a microwave oven.

Researching Glow-Powder Left A Few Scars

Content warning: Human alteration and scalpels.
General warning: We are not speaking as doctors. Or lawyers.

If you watch sci-fi, you probably do not have to think hard to conjure a scene in a trendy bar where the patrons have glowing make-up or tattoos. That bit of futuristic flair was possible years ago with UV-reactive tattoo ink, but it has the unfortunate tendency to permanently fade faster than traditional ink. [Miana], a biohacker, wanted something that could last forever and glow on its own. After months of research and testing, she presents a technique with a silica-coated powder and scarification. Reddit post with graphic content.

Continue reading “Researching Glow-Powder Left A Few Scars”

An aluminium frame is visible, supporting several connected pieces of chemistry equipment. At the left, there is a tube containing a clear solution, with a tube leading to a clear tube heated by a gas flame, with another tube leading to a clear bottle, which has a tube leading to a bubbling orange solution.

A Miniature Ostwald Reactor To Make Nitric Acid

Modern fertilizer manufacturing uses the Haber-Bosch and Ostwald processes to fix aerial nitrogen as ammonia, then oxidize the ammonia to nitric acid. Having already created a Haber-Bosch reactor for ammonia production, [Markus Bindhammer] took the obvious next step and created an Ostwald reactor to make nitric acid.

[Markus]’s first step was to build a sturdy frame for his apparatus, since most inexpensive lab stands are light and tip over easily – not a good trait in the best of times, but particularly undesirable when working with nitrogen dioxide and nitric acid. Instead, [Markus] built a frame out of aluminium extrusion, T-nuts, threaded rods, pipe clamps, and a few cut pieces of aluminium.

Once the frame was built, [Markus] mounted a section of quartz glass tubing above a gas burner intended for camping, and connected the output of the quartz tube to a gas washing bottle. The high-temperature resistant quartz tube held a mixture of alumina and platinum wool (as we’ve seen him use before), which acted as a catalyst for the oxidation of ammonia. The input to the tube was connected to a container of ammonia solution, and the output of the gas washing bottle fed into a solution of universal pH indicator. A vacuum ejector pulled a mixture of air and ammonia vapors through the whole system, and a copper wool flashback arrestor kept that mixture from having explosive side reactions.

After [Markus] started up the ejector and lit the burner, it still took a few hours of experimentation to get the conditions right. The issue seems to be that even with catalysis, ammonia won’t oxidize to nitrogen oxides at too low a temperature, and nitrogen oxides break down to nitrogen and oxygen at too high a temperature. Eventually, though, he managed to get the flow rate right and was rewarded with the tell-tale brown fumes of nitrogen dioxide in the gas washing bottle. The universal indicator also turned red, further confirming that he had made nitric acid.

Thanks to the platinum catalyst, this reactor does have the advantage of not relying on high voltages to make nitric acid. Of course, you’ll still need get ammonia somehow.

Big Chemistry: Seawater Desalination

For a world covered in oceans, getting a drink of water on Planet Earth can be surprisingly tricky. Fresh water is hard to come by even on our water world, so much so that most sources are better measured in parts per million than percentages; add together every freshwater lake, river, and stream in the world, and you’d be looking at a mere 0.0066% of all the water on Earth.

Of course, what that really says is that our endowment of saltwater is truly staggering. We have over 1.3 billion cubic kilometers of the stuff, most of it easily accessible to the billion or so people who live within 10 kilometers of a coastline. Untreated, though, saltwater isn’t of much direct use to humans, since we, our domestic animals, and pretty much all our crops thirst only for water a hundred times less saline than seawater.

While nature solved the problem of desalination a long time ago, the natural water cycle turns seawater into freshwater at too slow a pace or in the wrong locations for our needs. While there are simple methods for getting the salt out of seawater, such as distillation, processing seawater on a scale that can provide even a medium-sized city with a steady source of potable water is definitely a job for Big Chemistry.

Continue reading “Big Chemistry: Seawater Desalination”

Saving Green Books From Poison Paranoia

You probably do not need us to tell you that Arsenic is not healthy stuff. This wasn’t always such common knowledge, as for a time in the 19th century a chemical variously known as Paris or Emerald Green, but known to chemists as copper(II) acetoarsenite was a very popular green pigment. While this pigment is obviously not deadly on-contact, given that it’s taken 200 years to raise the alarm about these books (and it used to be used in candy (!)), arsenic is really not something you want in your system. Libraries around the world have been quarantining vintage green books ̶f̶o̶r̶ ̶f̶e̶a̶r̶ ̶b̶i̶b̶l̶i̶o̶p̶h̶i̶l̶i̶es ̶m̶i̶g̶h̶t̶ ̶b̶e̶ ̶t̶e̶m̶p̶t̶e̶d̶ ̶t̶o̶ ̶l̶i̶c̶k̶ ̶t̶h̶e̶m̶  out of an abundance of caution, but researchers at The University of St. Andrews have found a cheaper method to detect the poison pigment than XRF or Raman Spectroscopy previously employed.

The hack is simple, and in retrospect, rather obvious: using a a hand-held vis-IR spectrometer normally used by geologists for mineral ID, they analyzed the spectrum of the compound on book covers. (As an aside, Emerald Green is similar in both arsenic content and color to the mineral conichalcite, which you also should not lick.)  The striking green colour obviously has a strong response in the green range of the spectrum, but other green pigments can as well. A second band in the near-infrared clinches the identification.

A custom solution was then developed, which sadly does not seem to have been documented as of yet. From the press release it sounds like they are using LEDs and photodetectors for color detection in the green and IR at least, but there might be more to it, like a hacked version of common colour sensors that put filters on the photodetectors.

While toxic books will still remain under lock and key, the hope is that with quick and easy identification tens of thousands of currently-quarantined texts that use safer green pigments can be returned to circulation.

Tip of the hat to [Jamie] for the tip off, via the BBC.

Two clear phials are shown in the foreground, next to a glass flask. One phial is labelled “P,” and the other is labelled “N”.

Designing A Hobbyist’s Semiconductor Dopant

[ProjectsInFlight] has been on a mission to make his own semiconductors for about a year now, and recently shared a major step toward that goal: homemade spin-on dopants. Doping semiconductors has traditionally been extremely expensive, requiring either ion-implantation equipment or specialized chemicals for thermal diffusion. [ProjectsInFlight] wanted to use thermal diffusion doping, but first had to formulate a cheaper dopant.

Thermal diffusion doping involves placing a source of dopant atoms (phosphorus or boron in this case) on top of the chip to be doped, heating the chip, and letting the dopant atoms diffuse into the silicon. [ProjectsInFlight] used spin-on glass doping, in which an even layer of precursor chemicals is spin-coated onto the chip. Upon heating, the precursors decompose to leave behind a protective film of glass containing the dopant atoms, which diffuse out of the glass and into the silicon.

After trying a few methods to create a glass layer, [ProjectsInFlight] settled on a composition based on tetraethyl orthosilicate, which we’ve seen used before to create synthetic opals. After finding this method, all he had to do was find the optimal reaction time, heating, pH, and reactant proportions. Several months of experimentation later, he had a working solution.

After some testing, he found that he could bring silicon wafers from their original light doping to heavy doping. This is particularly impressive when you consider that his dopant is about two orders of magnitude cheaper than similar commercial products.

Of course, after doping, you still need to remove the glass layer with an oxide etchant, which we’ve covered before. If you prefer working with lasers, we’ve also seen those used for doping. Continue reading “Designing A Hobbyist’s Semiconductor Dopant”