Shed Synthesis of Lithium Niobate 

The music in this episode is by an artist called Corticyte, check them out here: soundcloud.com/corticyte

NileRed, Nurdrage and Extractions&Ire in the same day. The chemistry gods smile upon us.

For a hot minute I genuinely thought a "Shed Synthesis" was some advanced chemistry technique I'd never heard of, maybe discovered by Dr Gustav Shed.

Well, there's only one thing for me to do I guess. Make a protein based OPO, but make it so it's only emission is bright yellow.

Tom, re-melt the lithium niobate you made but use an oxygen rich oxidizing flame instead of the reducing fuel rich flame you used, it will oxidize out all the carbon that it got impregnated with and clear up. Don't be afraid to get the whole crucible glowing hot, it just means a slower cooling time that will yield better crystals.

"600-900 degrees. It's not super hot". Spoken like a true solid state chemist

Here's a fun fact about niobium, it's one of the most problematic trace contaminants in steel for the future fusion reactors. Nb has a huge neutron capture cross-section and it gets activated into a nasty Nb-94 isotope with 20000 year half-life and high decay energy. As a result, normal steel activated by fast neutrons from fusion will have to be treated as a low-level nuclear waste basically forever. One of my classmates worked on a project to make low-niobium steels, but they kinda gave up on that.

When I was a kid I wrote to a Niobium mine not too far from where I lived to see if they would send me some for my elements collection. They didn't send me pure niobium, but they did sent me a cool shiny rock of ferroniobium.

NZ based organic chemist here - I share your sadness about the loss of plastic utensils from supermarkets. I use a lot of sodium azide and needed some plastic spoons because the azide forms explosive compounds when exposed to transition metals. Ended up finding a lot of plastic spoons at a chinese takeaways and pocketed them :)

The reason why it went black is because your flame wasn't neutral. It was orange. You need to give it a little more oxygen until the flame turns blue then it won't deposit Carbon on anyting

You know it's a good episode if he needs 2+ new equipment for it 🥰

Lithium-Niobate was the second harmonic-generating material I used for frequency doubling a 844 nm laser to 422 nm for my senior thesis in college :) nice to see it getting some love

At my old job i was in charge of the nickel niobate synthesis, for that synthesis the homogeniation of the powder was extremely important. We ball milled the Carbonate and niobium pentoxide together for ~16 hrs to homogenize it. We also used extremely large kilns, that hit 1600C, but idk if the that temp would be transferable to getting purer lithium niobate

Shoutout to the people doing research on these esoteric compounds that have like 6 useful applications. Incredible work! 100% +/- 10% yield! Thats way better than single digits

There are a few gem cutters who facet pieces of Lithium Niobate into gemstones. They are quite beautiful since they have a refractive index and dispersion much greater than diamond, so they sparkle with insanely bright colors. The only catch is their Mohs hardness is only about 5.5-ish, so you wouldn't want to have them set in like a ring or other heavy-use jewelry.

Actually, you can get hot enough with your microwave, I played with this about 20 years ago (for fun) and I reached about 2400°c . I used a old analog pyrometer from the sixties so not ultra-precise but I have definitely melted alumina. I used polishing grade coarse SiC as the microwave absorber (susceptor), I think it is the black thing rather than graphite that is placed inside your kiln but there is not enough to absorb all microwaves (it is on purpose i guess). My advice in the same kiln put a thick bed of alumina power put some SiC powder on top ,cover it with alumina powder and then put your alumina crucible on top (of course try to have a good contact area with crucible and the powder below but without direct contact crucible-SiC). If you put the alumina crucible directly on top of the SiC, it will shatter due to the thermal shock.

Tip for the acetylene torch. Your inner flame cone is too large. Less acetylene or more oxygen to get a neutral to oxidizing flame. Right now it's more carburizing. You're putting carbon into your product. Also for lighting it: half a turn oxygen then quarter turn acetylene to start with, adjust it from there. If your pressure is to high or low the flame will go out. To turn it off, first the acetylene then the oxygen. If you do it the other way around you get a lot of soot that is actually a little carcinogenic. And for the love of fuck don't light it with a liquid or gas fuel lighter. Use a striker. There's a tiny explosion every time you light your torch. If this damages your lighter it can catch fire in your hand. Which can be kinda bad since the torch is blowing oxygen at it. If you smother you torch by accident and the flame goes into it. Just turn it off like normal. The torch will start getting hot pretty quickly as the brass sucks the heat out of the flame and it travels up the torch. If it goes past that into the hose, shut off the valves to the bottles. to prevent them from further turning into little rockets. be safe and happy lighting shit on fire!

Niobium makes for really great nickel superalloys as well. There's a ton of interesting research being conducted on them in the aeronautics industry

Tom's Shed Microwave: What is my purpose? Tom: You heat up dangerous chemicals until you die Microwave: *oh my god*

There is nothing considered "weird" that is beyond this man's challenge! Next week: DIY Fluoroantimonic Acid!

i love the term "shed synthesis". that's such a good word for what you do.

Really excited to see this video from my favorite chemistry youtuber! I just had my PhD thesis on using lithium niobate piezoelectric resonators for power conversion.

After just finishing a class on superconducting RF cavities where Niobium seemed like the miracle element that makes the whole field possible its very funny to hear it being considered not very important

the cat slapping around your metals was by far the best part of my day.

That was a nice video! I've actually worked with amorphous niobium oxide (sometimes called "niobic acid"), which I believe is the exact material you made here (didn't make it myself, we ordered it from a supplier). It has a very high surface area, and can hold on to a non negligible amount of water, even as dissociatively chemisorbed species (i.e; surface hydroxyls). We used it as a support for catalysts. So that extra water might explain why you got 100% yield despite the mechanical losses. And cool to see you got an acetylene torch! You may want to try making an oxidizing flame, so that you don't leave carbon on your metal oxides... (I think "cutting tips" are designed specifically for that. I've only used those torches to seal glass ampules though, so don't take my word on it.)

The way Niobium hardens steel , is by making the grains in steel very tiny which makes steel harder but not brittle! It's kinda crazy

"Lithium Niobate is an optical material. It was used in the 60s I think? to make the first OPO" Fuck me I love the 60s

Niobium is a great addition to certain knife blade steels as well. It helps form a finer grain structure. A little bit goes a long way, too. S110V has about 3%, for example.

i would like to thank u for ur decision to start off this pride month with some Nb representation on ur channel.

This man gives the vibe of an innocent side character of a show who ends up being master manipulator behind everything

I'm a big fan of lithium niobate crystals. If you put a c-axis cut under weak vacuum (like 10^-4 torr) and cycle the temperature the uncompensated charges exposed on the ends act like a particle accellerator and you can achieve electron and ion beams up to ~200KeV. That's without any moving parts or high voltage. If the crystal is radially symmetric the beam self focuses. If the residual gas in the weak vaccuum is deuterium and you have a deuterated plastic target you can even make a linear accellerator fusion device for making small neutron fluxes. Definitely a fan.

Camera work in this one really nice, the sequence of setting up the torch for the first time was more professional than anything I expected on this channel and it honestly caught me off guard. Great video mate, perfect mix of beauty and jank

YES! I LOVE VIDEOS ON ELEMENTS WHICH I'VE ONLY SEEN ON THE PERIODIC TABLE

Tom: "People in the comments will have done their entire PHD thesis on Niobium" Me in the comments who has no PHD at all and only comes here for Tom's personality and for him to call things cunt: "Yea... I totally know what Niobium is"

Very amusing that the cat saw identical metals that are hard to visually distinguish and immediately stirred them with a paw, truely masters of malice.

An Extractions & Ire release and a Nile Red release within the same hour. The stars have aligned.

For a cleaner product after melting with the torch you will need to have complete combustion of the acetylene. This is a achieved by using more oxygen as I’m sure you know. If you watch a RU-vid video about acetylene welding I think it would help you get the flame profile you are looking for

First Nile, now Tom uploads. This smells like a conspiracy. A ... chemistry conspiracy!

I’ve never felt so secure about watching someone else try to do the really challenging and frankly dangerous and impossible things I can only dream about. Never ever stop being You Sir. You’re an inspiration 😊

If you had a neutral flame on the torch it would've melted better, it looks like you were running acetylene rich by how orange the flame was. For a neutral flame you want to balance them so that there is a single bright cone in the middle of the flame, and most of the flame should be blue with just the end of the flame starting to turn to orange

I care a lot! Lithium Niobate is one of my favorite gem materials.

Niobium isn't obscure! It's a part of one of my favourite minerals - columbite-tantalite (or coltan), which is (Fe, Mn)Ta2O6-(Fe, Mn)Nb2O6. This mineral is primarily mined for the tantalum therein, as it is used in capacitors in modern electronic devices, but niobium has a lot of extremely high-tech, science-y applications too, mainly in the steel industry (where it is alloyed with stainless steel to give it strength at low temperatures, which is handy for a lot of aerospace applications*), superconducting magnets (600 tonnes of Nb3Sn alloy is in the Large Hadron Collider, while the International Thermonuclear Experimental Reactor uses 600 tonnes of Nb3Sn alloy, and another 250 tonnes of NbTi alloy), and high-performance lithium batteries. It can even be used to make people's glasses thinner, as it increases the refractive index of glass. *The Gemini and Apollo space programs both relied on niobium to make their rocket engines, and SpaceX is currently using such an alloy for the engine of the upper stage of the Falcon 9.

A big use for lithium niobate is as the substrate for making bulk acoustic wave resonators, which are signal filters used in cell phones and other digital communications hardware.

Niobium alloys are common in rocket engines because of the high temperature material properties. They're a bit of a pain but sometimes you just need it.

The world needs more science like this maybe shedology 101, keep up the awesome work man.

True niobium lover here, I am doing a PhD on niobium alloys

The Way He Said I Don’t Wanna Go Into Made Me Feel Like He Really Wanted to Go Off On a Tangent to Talk About it in Depth…. 🤦‍♂️🤷‍♂️😂😂😂 Live These Videos & This RU-vid Channel!!!!!

A Nile vid AND an Extractions and Ire vid on the same day?! We have been blessed

Niobium was named after Niobe, the daughter of Tantalus, the Greek character the element Tantalum is named after because it’s so similar in properties to tantalum

I like niobium. I have a few big chunks of it. It's a neat metal, it can be oxidized to form some nicely colored layers on its surface (due to interference in various thicknesses of oxide). It's also biologically inert and used for jewelry, piercings, surgical hardware etc. But that's not why I have it. It's also a grain refiner and very strong carbide forming element in steel. Sorta like vanadium. I want to use some of the niobium I have to make wootz steel, i.e. ancient Damascus steel.

As a gem cutter and jeweler, niobium is awesome and lithium niobate is amazing as a cut gem!

21:27 You are a comedic genious. The way you placed your glove over the heat exhaust of the microwave here had me cracking up! :D

I remember seeing that niobium has pretty looking oxide, a sort of violet or indigo. At least, that's what I recall it being from reading about it on Wikipedia ages ago

What a perfect resolution to a shitty day in the lab than unwinding to a video of Tom doing transition element chemistry

Niobium fan here! I don't know much about the element itself but I have a 1cm cube of it on my desk because it's anodized purple and I like that color :3

Bingo! I knew it was was the Niobium, that goldish luster in the light is a dead giveaway. Some idiots might confuse it with the Tungsten but not this laddy. Fantastic video, as usual.

May look into HHO torches to reach your fusion temperature. Nighthawkinlight had one that was desktop-sized and could fuse alumina into rubies.

Attempts inorganic chemistry. Generates tar.

i took an art class at my local college and they had these microwave crucibles, they put ceramic shards on the plate to allow the crucible to continue to rotate without damaging the plate. also i noticed in that class that different microwaves heat faster so if you hate the 30 minute wait you should consider testing your friends microwaves and buy the hottest one you tested.

Well Tom, I took the entire transcript of this video and copy-pasted it into GPT3.5, and this is what it had to say: "Thank you for sharing this detailed episode on the extraction and use of niobium. It seems like you had an adventurous journey in working with niobium metal and converting it into niobium pentoxide. The process of dissolving niobium metal in sulfuric acid, followed by the formation of niobium pentoxide and its subsequent reactions with lithium carbonate, demonstrated your exploration of different chemical reactions. The use of a microwave furnace to achieve the required temperatures for the reactions, as well as your attempt to fuse the niobium pentoxide using an oxy-acetylene torch, showcased your resourcefulness and experimental approach. While the results may not have been as expected, it's clear that you enjoyed the process and learned along the way. If you have any specific questions or need further information about niobium or any other topic, feel free to ask!"

It's always an adventure watching your videos wondering how long it will take you to break down into explaining the process with "We're gonna do something with some amount of stuff for some period of time and hopefully that works 🤪" We got there in 6 minutes this time, that might be a new record, I have high hopes for the rest of this video 😄

With everyday the PhD grows closer to completion. Keep going!!

I really love the mad scientist working in a shed with trash equipment (no offense) vibe we get here. This channel deserves more views. It would probably help to "spice" up the production value (but keep the vibe!).

E&I is like a box of Whizzo Quality Assortment, you never know what you're going to get next. It could be Crunchy Frog, or it could be the Steel spring surprise.

>100% yield >starts turning yellow hmmm

ive heard a lot that you generally shouldnt use a flame to light an oxy-axxetylene torch because if the gas flow blows out your flame youre now filling the area with toxic flammable gas mix. also going to echo the others in the ocmments saying your flame was a reducing flame because you didnt have enough oxygen in it, and the excess carbon from that got deposited on your product

you're one of my like, favorite people I've never met. Thanks for making videos, you're rad as hecc.

styropyro:gets chemistry degree, but makes laser Extractions&ire: gets degree related to making lasers, but does chemistry

Hey! I work in natural user interface, robotics, and computer vision. A while back when you were talking about your phd you were talking about OPO and it really cracked my head open on silicon photonics, which has changed my life. I completely forgot what you called the spinning prism by the time I got to the other side of that rabbit hole but a couple days ago I saw someone making a little portable laser galvo setup out of an old hard drive and just started geeking out about spinning a prism or a series of prisms and mirrors on the dead hard drive that was sitting on my desk but I could not remember the thing to google. Anyway, thanks for before and thanks again now. You just keep hooking me up. You're a saint and I'll drop you some stacks on that Patreon for it. Tell my girl to put you on the holiday card list. Lol.

Always a great day when there’s a new Tom video!

I won’t lie, I was on explosions and fire and thought you just stopped uploading, but seeing this was a bastion of hope

In college I was an intern on the Stanford Free Electron Laser facility (now torn down) which used a niobium superconducting array as its electron accelerator.

i actually cracked a liebig once using a forced air condenser when distilling sulfuric acid (similarly to how you did a few years ago, right on the jacket), id recommend using a vigreux column instead and keeping the sulfuric at such a rate so that the convection cooled vigreux can keep up with it. that glass stir bar had me worried a little since glass can scratch glass and with hot sulfuric acid you dont really want score marks on the glassware for obvious reasons, though i still probably will buy some as theyll be perfect for something i have planned. as for that SO2 like you mentioned its probably the reaction, ive dissolved copper in hot sulfuric acid and the sulfuric acid gets reduced to sulfur dioxide while the copper oxidized to copper oxide which then forms copper sulfate so that blue tint may have been niobium sulfate or sulfite but unfortunately i cant find pictures of those so idk. cracking the flask like that ive done too many times, its not a good idea to heat a wet flask with a flame or run liquid onto hot glass like that, as for melting maybe an arc furnace though that may spit graphite in from the electrodes, neat video like always

Caught it right as you went public with it. This is gonna be a cool one. It also makes an excellent gemstone, although IIRC it's a bit soft for a ring. Good for earrings and pendants. After watching the video, I think you may need to go ahead and melt all your product but heat it longer, leave it in the molten state for a longer period with the torch, then dissolve it and re-crystallize the product to grow actual crystals of the product for clarity.

A guy made Cubane and called you out but we all know you are still the best chemist on youtube.

So I just got done watching a NileRed video, and the way each of you go about things is so vastly different, its both jarring and amusing

Wait wait wait, your phd is in physics, and you do exclusively chemistry content. Styropyros degree is in chemistry, and he does almost exclusively physics content. Wtf.

So happy to get more extractions and ire/fire vids while you are procrastinating your thesis. 😂 For real though best of luck/skill on your doctorate sir!

I used to be a niobium man myself. Built RF cavities for linear particle accelerators out of it. Definitely in my top 3 superconductors.

I love that Tom is doing crazy technical chemistry, and says 'I think' and 'I don't know l, we'll see' so much more than the average person does doing mundane things they've never done before. (Most people don't ever attempt anything they don't know how to do, lol)

Moon is going to explone on monday.

One of my early papers was using an old kitchen microwave to make lithium battery materials - made writing the experimental interesting with scientific phrases such as 'high for 2 mins!' It was old-school and used graphite powder in devitrified quartz crucibles as a 'microwave furnace' - it got hot as hell in a hurry 😆

I enjoy this so much! Amazing content, best wishes to you and your future projects! 🌻

If you want to get real heat out of your acetylene torch you need to adjust the gas ratio until you have short (a few millimeters), sharp blue flames. Then holding it within a few centimeters / a centimeter of what you are heating. I learned to cut with a torch and adjusting the flames to be short and intensely bright increases the heat (and cutting in speed in my application, not so applicable to you) significantly. Using enough oxygen is key to complete combustion and will cut down on the soot output too. Heating the crucible could get the job done too, but the correct gas mixture should eliminate most of the soot issue.

We use plenty of niobium... mainly in the NbTi alloy for superconductive magnets, cables and resonant cavity coatings. Sheets of the alloy would also be good for magnetic shielding, but softer materials like lead or aluminum are much easier to handle

Try putting a lid on it and blasting the outside of it with the torch. It would be better to have some enclosure around the whole thing to retain the heat as well. Might be able to prop one side of that microwave kiln up and place the flame to swirl around the crucible . I use insulating firebrick. You can carve them out with a spoon , although hole saws make quick work of it. I use 3. One for the base, one with a hole through it and a hole in the side at the bottom for a propane torch tip, and one brick for a lid with a smaller hole for the exhaust. I’ve melted aluminum many times this way, and for you, it would allow a semi controlled cooling by simply turning the flame down a bit over time.

In solid state synthesis it's usually a good idea to get your particles as close together as you can before sintering/firing. Our lab commonly uses a hydraulic press to press the powders into pallets before they're heated. Since you are going above the melting point of lithium carbonate, and the reaction is thus not entirely solid state, paletting might be a bit of an overkill.Still getting it ground as finely as possible and than compacted should help. Also it's completely normal that the grinding/firing stage might have to be repeated several times, some solid state synthesis require up to a dozen repetitons of this steps to get decent yields.

Loving the disconnect from "The atmosphere is nature's bin!" ---> "it's not my fault the rivers and the oceans are f*****" hahaha

Something else interesting and exciting about photonic computing is that recently a group over at Stanford was able to implement back-propagation, which lets you train neural networks. For like, AI. And shit.

Ah another inorganic chem episode. Gotta love when stuff just wants to kills you rather than both wanting to kill you and turn to tar at the same time.

Huh, what a happy coincidence, I just recently got some faceted iron-doped Lithium Niobate. Apparently used in research as a holographic storage medium. Sure is a pretty shiny rock, too. Would definitely like to hear more about your PhD thesis when you're able to.

Shake the Future has an excellent RU-vid video on smelting metal in a microwave, including how to make a crucible and how long it takes to melt various amounts of metals. In particular, I think it's worth trying the microwave furnace without the brick in the oven absorbing a ton of energy and slowing down the melting of the metal.

Don't get tired of saying. I know sh** about chemistry, and this is one of my favorite channels. So much fun

There were some strange materials used back then for lasers; one was trivalent uranium doped calcium fluoride, which Peter Sorokin developed while he was at IBM. It had to be cooled with liquid helium, and it lased in the infrared around 2.5 microns when pumped with a flashlamp. It was the second laser developed after Maiman's ruby laser.

27:09 - I choked when you said "there are not even crystals in the slightest" Dude... under a chaotic blow torch you expected crystals? If you weren't australian I'd call you Jesse Pinkman at this point...

Ok, here's a suggestion in case you ever want to dissolve niobium again (I don't have much to back this up, but listen): selenic acid should work. Here's a cool fact about selenic acid: it can dissolve gold (it first oxidises it (producing selenous acid), and then the remaining acid dissolves it). Source: Wikipedia for selenic acid. Also, selenic acid is similar to sulphuric acid but just stronger and also an oxidant, so it seems to me rather likely that it would do the job, maybe not at room temperature, but likely not nearly as hot as what the sulphuric acid needs to be. Cool video! Niobium chemistry, yay!

youre amazing dude. a year ago, you single-handedly re-sparked my interest in chemistry. youre a natural comedian, combined with being an all around smart human being. yours is one of my favorite channels on youtube. i hope you keep creating some form of content, whether its funny chemistry videos or phds in chemistry or physics. just brilliant! (im american btw, we dont use brilliant to describe cool stuff and its reserved for only the brightest people).

Your comment about crystallization "never happens to your product but always happens to the impurities" felt personal

“Concentrated, boiling sulfuric acid” is the most violent string of words I’ve heard in a long time.

Glad someone was there to guide ya on that kit. Acetylene is some dangerous shit if you don't know what you're doing. Glad to see another vid!