FriskyBismuth
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YInMn Blue Synthesis Video Series
Hello Mad Scientists!
I've been working on a longer project lately, the synthesis of YInMn Blue starting from Indium, MnO2, and Y2O3. I have successfully completed the
project and have been barely able to find time to edit the videos I made along the way. I just decided my intro was good enough, and I have finished
the Indium video so it went up as well. I have someone on here to thank for sending me some research papers in a zip archive but I honestly can't
remember right now who it was! This was in response to my previous project of making ultramarine blue.
Anyway here's the links:
Introduction to the Project:
https://www.youtube.com/watch?v=OEYDD99f6FQ
Here I briefly talk about the product and the plan for the project, and how I heard about it, and who helped me.
Synthesis Part 1: Oxidation of Indium
https://www.youtube.com/watch?v=PGb8y-S6e8w
In this video, I start by playing around with Indium in my backyard "foundry" then go to the lab at the community college I attend and work at (I'm
the chemistry lab tech....very fun job!) where I oxidize Indium with hydrochloric acid to produce a solution of InCl3, then do a
precipitation reaction with this solution and a solution of sodium hydroxide to precipitate In(OH)3, and finally I end up taking the indium
hydroxide home and doing a thermolysis/dehydration reaction to produce In2O3. Also I made the music, it's a jazz/rock project
I've been writing and recording for several years and you can tell I'm eager to share it with the world now that I've finished mixing and mastering
it.
Cheers! Hope you like it!
[Edited on 12-4-2022 by FriskyBismuth]
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CaCl2
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Nice to see someone making YInMn.
When I made mine I oxidized the indium just by heating it in air, which seemed to work fine. Your method has the advantage of needing much lower
temperatures for this step at the cost of some HCl and NaOH. I guess YInMn isn't too sensitive to Na/Cl impurities?
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FriskyBismuth
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I didn't have much luck with oxidizing indium in air - one time I was able to get some indium oxide to fume onto a homemade ceramic crucible but it
sank in to the material and made a nice glossy yellow on the rim! So I decided to do the chemical oxidation.
There are some things I forgot to film and include in the video - specifically, after thermal degradation of indium hydroxide to indium oxide, I
thoroughly washed the oxide with hot water several times then heat-dried it again, which resulted in what appears to be a fairly clean product. This
hopefully removed enough Na and Cl that it doesn't make a huge difference. Similarly, I had forgotten to film the "precipitato-metric" titration
which showed me the hydration level of my two manganese (II) chloride samples. I'll try to remember to include that in the narration for that video!
I'm also planning to make a couple non-manganese chromophore compounds, we'll see how that goes!
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FriskyBismuth
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A nice little update: While I'm still working on editing some of the videos from this series of procedures, I decided to do some analytical work on
the synthesis products. Since I'm at a small community college, we do not have analytical equipment of reasonable quality.
To get some information about the material itself, I contacted Dr. Mas Subramanian, the inventor of YInMn blue and its newer non-blue derivatives, to
see if I could obtain some raw spectral data to which I could apply some chemometric techniques. Briefly afterward, I decided to build a
spectrophotometer using a 3D printer, a diffraction grating, and a digital camera, with the goal of obtaining vis spectral data.
After 2 weeks, Dr. Subramanian responded to me and offered to analyze some of my samples using IR-vis reflectance spectroscopy and x-ray diffraction.
So....I will be sending him some of my samples and analyzing these same samples on my own home-made setup, comparing the two datasets, and generally
having a great time doing some cool chemistry and physics stuff!
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DrRadium
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I had heard Dr. Subramanianwas a righteous dude, glad to hear the rumor was correct!
I'm interested to know some details of how you made your spec. Especially since you'll need reflectance data, which I would think makes the geometry
more challenging and software. The last time I programmed anything more than an arduino it was the Bush administration... George Herbert Walker Bush.
I was surprised to learn there are some decent vis spec instruments cheap. I've spoken with someone who has been using The variable inc Spectro 1 for
analysis of pigments for his watercolor paints and found it very consistent. I got one of their colorimeters cheap off ebay and have been impressed
with its consistency and replicability.
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DrRadium
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Quote: Originally posted by CaCl2  | Nice to see someone making YInMn.
When I made mine I oxidized the indium just by heating it in air, which seemed to work fine. Your method has the advantage of needing much lower
temperatures for this step at the cost of some HCl and NaOH. I guess YInMn isn't too sensitive to Na/Cl impurities?
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Hey you already know someone making YInMn! Just not from indium metal.
I've made enough batches of YInMn blue with components from various places and screwed up enough to have gotten a sense of how things tend to fail and
what they look like when they do. While I haven't formally tested various contaminants, I have developed some general observations through things
like tipping a crucible, scraping up the material off the counter and into a separate crucible then calcining it anyway.
In general the YInMn solid state synthesis seems fairly tolerant, more so than for the YAlCuTi greens, which are by far the most sensitive compared to
the blues and purples.
With whatever impurities are problematic, both the blues and purples tend to get grayer to a point and then as the concentration of whatever is
causing problems rises, fail altogether as some threshold is crossed. They come out ashen grey to various browns: light tan to deep chocolate. I've
seen the greens get blueish once (it's in my composite image of all the weigh boats and caps with green, blues, or purples). It was probably
contaminated with extremely trace amounts of laundry detergent. Otherwise they just fail to make shades of brown.
I have had batches of yttrium oxide with some impurity in it such that could not make YAlCuTi greens at all (or YInCuTi or YCuTi green) but which made
YInMn blues that were at worst only faintly grey. Made me think my copper oxide was bad for a while as I would test each component from the the
green in a blue or purple. The yttrium, aluminium, titantium, all seemed fine. I replaced the old copper with some ultrapure stuff and still didn't
work. Tried different yttrium and the old copper oxide was fine.
Since then I've stocked away aliquots of metal oxides that have performed well across the board as controls and i try not to have more than one new
stock of anything at a time.
I do have to say though that some of the failed reactions made damn good earth tone pigments!
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DrRadium
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| Quote: Originally posted by FriskyBismuth | | This hopefully removed enough Na and Cl that it doesn't make a huge difference. Similarly, I had forgotten to film the "precipitato-metric"
titration which showed me the hydration level of my two manganese (II) chloride samples. I'll try to remember to include that in the narration for
that video!! |
Just FYI I'm going to doing a YInMn synthesis run soon, so if you see trace ions in your future that may or may not interfere and would prefer not to
have to go in blind, I'm happy to check to see how they affect the reaction. Let me know. I have a bunch of thimble crucibles and can easily take
small aliquots and dope them to see what happens.
Mike
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FriskyBismuth
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I finally got it together to post the next video in this series, in which I use HCl to reduce Mn(IV) to Mn(II), and encounter a variety of hassles
along the way.
A personal update - I was accepted as a transfer student to UC Berkeley and my wife and I spent the summer moving from Tahoe to Berkeley, which was a
whole stressful crazy thing, and then classes started which have been a bit more in-depth and fast-paced than what I was accustomed to. It's been a
difficult transition to this new life, living in an urban environment covered in concrete and surrounded by sharp geometrical buildings and lots of
noise and people. Studying at Berkeley has been generally pretty awesome but has had its challenges as well, since I'm still getting used to midterm
exams as a form of assault (seriously the class average for a midterm was around 65/100 which I am accustomed to being a D letter grade). In other
news, our car was stolen a few weeks ago so that's been fun to deal with. I'm kinda used to living somewhere that I don't even bother to lock my car
doors though I have been doing so here in the city. (I know people call SF "the city" and elsewhere...not the city....but it's all a huge city). We
actually got it back today, and it seems like it probably won't need all that much work to get it back in working order, so that's nice. And right
now it's study week before finals. So the stress is high. Anyway, thank you for being the cool community that has supported me so much as an amateur
chemist (though I was a lurker until recently).
Focusing on the positives: tons of knowledgeable folks here, opportunities to get involved in research, possibilities for grad school opening up. I
can walk to a grocery store, or a brewery, or a variety of music venues and restaurants. Been making friends, slowly, very slowly. But it's
happening. Yes. Things are good if I average it out and try to decide whether or not moving here to do this was a good idea. I think it is.
Anyway, here's the video.
https://www.youtube.com/watch?v=4ZN6OlZLwgE
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