Hydrothermal carbonization and other nano particle work

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  • edited July 2015
    When I get home, I'll play around with it some. Would a small convection oven(one of the ones with the glass doors that fit on a countertop) be sufficient as a heat source? Also, murray mentioned that solution concentration would effect particle size. Any idea whether a more concentrated solution would produce larger particles, or smaller ones?
    One of murray's later videos explains that a less concentrated solution with a lot of capping agent will lead to smaller particles.
  • There are zero papers on these particles, at least non formed via this method and as such we are the first to my knowledge to play around with this so all of these questions are literal cause for new information humans never knew before. This is all very cool but as such I don't have the answers to these things XD But I do have a lab and a fair bit of iron chloride. So I can and will happily try this out. By the end of this we're gonna have so much of this stuff lying around we'll end up making it into paints and inks. im excited. I love nanochemistry. It's so weird and wonderfully complex. 

    Solution concentration will only increase the number of particles to a point, after that you run out of carbon and end up with a bunch of random iron oxide nanoparticles clouding up your solution. it's best to go on the lower end and keep carbon in excess. The iron nanoparticles will be largely the same size but what changes the size so much is the amount of carbon that sticks to the particles. You can vary the size, far as i can tell from other experiments by changing the temperature and the time it's kept under pressure. This is the longest run that we do, most other experiments only need an hour, 3 max. We could try other transition metals as im seeing more and more synthesis that use this process, a metal chloride then an organic and a catalyst. Iron is unique since it forms the particles so readily. I'm interested to see if we can switch out the tea as well for something else, ideally pure, ethanol maybe? and use that as the carbon source. would make the particles much more uniform. That said this is largely speculation based on papers i've been reading and the few runs we've done so who knows. Science awaits!
  • From what I read, the reason the tea was used was because the polyphenols act as capping agents.
  • Tea is also being used as a reducing agent in green chemistry so that could play a role as well. I hadn't read that but if that's the case it's certainly interesting.We'l try a few reaction with them and hopefully that'll shed some light on what exactly these thing are. 
  • On another note, perhaps we could use this manufacturing method to produce titanium nanoparticles, and sinter our own components.
  • Maybe but I doubt it. titanium is famously a pain in the ass to work with. I saw a similair procedure used to make paladium carbon particles. formed little paladium core carbon worm looking particles. Apparently great catalytic properties. We're actually exploring if you can fuse some of these particles to make slightly larger particles with unique functions. I feel that is one of the most important thing we could work on since once you can stick things together how you want you cna build nanites... at least in theory and we're a long way off but this could be a good step. That said we're running a few things today, wood, copper chloride (rather than the copper sulfate we tried last time) and seeing if we can turn the regular iron particles into hydrophobic ones. 
  • edited July 2015
    Oh that's right! I forgot that little detail about titanium... Do you have anyway of observing the morphology of the particles in your lab? 
  • Not in our lab but we're talking with one of our professors, one awstin's friendly with. The guy is the big nanoparticles researcher here so if it goes well he may give us access to his lab to take a peak. Im looking into getting a spectrophotometer. It'll let us find out quite a bit about the particles so I'm hoping i can find one for cheap. 
  • Made an update video of the days progress: Video

    Gonna try making a clear layer of graphene that's conductive and am trying the iron nanoparticles to see if i can make them hydrophobic. Also tried some wood.
  • Sucess! The iron nanoparticles were succefully made hydrophobic. there is a layer of them floating at the top of my solution. now to modify the process to work way bette cause it only affected a small portion of the particles. My thoughts are increase amount of oil and time I run it for. Also I recently found that it's possible to make carbon xerogels/aerogels. this is rather exciting as I thought that was only possible at very high temperatures. Should have very interesting properties and im excited to try and make it!
  • Aerogels? If you have much success with those, let me know. I've been looking for ways of getting aerogels for some projects involving extreme heat, but been unsuccessful, because of the price. So, you added oil to the mix in your "pipe bomb" and it produced hydrophobic particles? 

    On another note, I wonder if it's possible to make aerogels using the carbon-capped iron nanoparticles. Magnetic Aerogels, anyone? Also, from a  biocompatibility standpoint, where do aerogels fall?
  • Aerogels are only as safe as what you make them out of. An aerogel really is just a material which you've sort of held together as a foam and then use either a solvent to make a xerogel or a gas to make an aerogel to remove the stuff you use to hold the matrix and lock it in place. In this case the carbon xerogel will likely be contaminated with all kinds of stuff you don't want in your body but perhaps after enough processing it may be possible. That said the paper I read the details the xerogell synthesis activated the carbon with potassium hydroxide to use it for it's catalytic abilities, something we certainly can make use of. Maybe even for power generation. At this point im sufficiently impressed with the carbon nano stuctures im quite certain that if you try you can make some rather impressive things for biohacking with them
  • Also areogel is dirt cheap dude. A monolith is expensive sure but you can get pellets which frankly are easier to handle for dirt cheap. Could you mix in some irn sure but i don't really see the point. if anything it may just screw with your xerogel and make it heavier. But it may add interesting catalytic properties as well
  • Update time. So I keep my room fairly cold. And it actually let my discover something interesting. When I made the hydrophobic nanoparticles I used coconut oil as I'd heard good things about it's properties. Here's the rub, it's a solid at room temperature and below. My room being rather cold solidified the samll amount that's in the container with the hydrophobic nanoparticles. But here's the thing. Since sme of the oil is now bound to the particles, they solidfy as well. I have no idea if this property will be useful at any point, I just thought it was neat. Also did some chemistry with the mystery solution I made. The solution was made by running hydrothermal carbonization of a piece of wood. The chamber was filled with 5% acetic acid and a single drop of honey as a carbon source to help kick start the reaction. It was cooked at 220 c for 6 hours. The solution was black but it sparkled. Was very strange. So i poured 2 portions off and reacted each with either hcl and aluminium or NaOH and alumnium. The hcl left a clear solution with white particulate floating around. The naOH left a brown yellow solution with a thick layer of black precipitate. I don't know what I made but I think it's cool XD I'm gonna harass my professors till one of them lets me use a spectrophotometer cause I wanna know what this shit is. If anyones interested lemme know and i'll post pictures. 
  • More success!!!!!!!!! The uv light I ordered arrived and I could test the particles. The ones made with gelatin fluoresced light blue while the ones we made with ethanol and orange juice had a dark green color. I need to now get them out of the synthesis solution and purify them to make them much brighter. Also I'm going to try and get a whole spectrum of colors. I'll have pictures and a write up later most likely.
  • Do you have videos or write-ups on how you did all these different preparations? Also, I think it might be interesting to see how biocompatible Titanium Dioxide nanoparticles are. Might be able to make tattoo-able sunscreen.
  • edited July 2015
    you want a full body tattoo, just so you don't have to wear sunscreen? I feel this defeats the purpose at that point. lol Im working on a writeup now. Normally I wont write a writeup until I have confirmation that the procedure works, hence why I'm only writing now. I literally only got this shit working an hour or two ago. lol

    That said the writeup is a few pages worth of writing and a whole bunch of graphic work so may be a little bit. 

    Edit: there is now a post on the thought emporium facebook page with a bunch of pictures of the particles. There will be more in the writeup but for those curious now. The way they react in solution is super weird. Makes the solution go opaque, yet glow. 
  • Ok write up with pictures is up! link
  • edited July 2015
    So, the ethanol and orange juice were mixed together? Or do each of those liquids, on their own, form green particles? Also, was it just gelatin in the tube, or did you add in iron chloride, or something similar?
  • edited July 2015
    I used 25% ethanol, 25% orange juice and the rest was water

    EDIT: blog post was updated for clarity. Thanks
  • edited July 2015
    Have you considered increasing the amount of ethanol in proportion to the orange juice and water? Might make it more green, considering the fact that citric acid makes blue nanodots, so the ethanol is likely the substance that's causing the color shift.

  • I've considered it. The paper actually calls for less. 25% orange juice to 19% ethanol. Also I used whiskey rather than pure ethanol. I want to switch out the orange juice for pure citric acid and see what happens. 
  • On a sidenote, I bet doing HTC on the contents of a glowstick (prior to activating it) could yield something interesting. And what variety of whiskey did you use?
  • I'm gonna try HTC on some Noopept I have. No clue if it'll work but it has some interesting groups that I see breaking into something interesting. I'll graba  glowstick in the next little bit and give it a try too.  Or leaving you with interestingly reactive particles. Candian club, rye. 
  • Is this turning into nanoparticle mixology? 
  • Here's an image from the paper. It's the table of recipies at it were. Im telling you, it reads like the shopping list of a grad student. It's hilarious. They use seemingly random shit they had lying around. But im taking it past that. Im keeping detailed notes of how things are interacting and trying to learn the system as it were. Like knowing how a molecule will break and stuff. I wanna see if there's a system to this that lets you really control the process.image
  • Another success! Re attempted the hydrophobic iron nanoparticles. This time I used less water, cleaned the particles before use, used safflower oil and much more of it. So about 2 parts water to 1 part oil. Left it to react for 3 hours at 170. When I pulled it out I added both more water and more oil all in a new clean container. Then gave it all a good mix. Sure enough there's is now a distinct black layer, about 4mm thick of black oily liquid between the water and oil layer. It is very magnetic and mixes back into solution. They don't move nearly as fast though. Also not all particles were converted. Some still sit in the bottom, no lipids on them.
  • Perhaps an emulsifier would improve the yield. Not sure whether or not that would change the output, though.
  • Turns out the bit on the bottom is no longer even magnetic, probably just crap from the reactor. Also I was wrong they move way faster, but only when the oil isn't all mixed with water. I'm gonna get them into clean oil tomorrow and it should be quite good.
  • edited July 2015
    Done anymore reactor runs?
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