Microwave Exfoliation of Intercalated Graphite
Ғылым және технология
About halfway through i cracked the glass. Boy did it make me jump. Next time i think i will do 10 seconds then 10 seconds rather than 20 all at once. Still the exfoliation volume was truely astounding. In the first experiment i put a tespoon of the intercalated graphite in a jam jar and it filled the jar!
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Robert, you bring experimenting down to a level many can get involved with. Thanks for continuing to help us better understand the possibilities!
The exfoliated graphite reminds me of a thing we called "snakes" in America during the 60's. "Snakes" started out as a black cube. We would light this black cube with a match, and it would expand into something that appeared into a "Snake". This "Snake" appeared to be just like the expanded graphite.
Robert Murray-Smith,Thanks for the SUPER Video, I get a lot from them. I like how you have shown and actually comment about ALL THE MISTAKES. I thought I must be an awful Amateur Chemist/Student by making so many. Then you come along and admit more mistakes than successes and I feel much better about it now. Would be helpful if you actually put a few in the videos occasionally showing what CAN go wrong so us dummies can fallow. It is very helpful to me to see a few of the mistakes and what can happen. Keeps me on board with my own experiments. Thanks so much.
And again, thank you for sharing this with us, it was really cool and useful.
I did starting to learn it now. You do probably not realize how great you are.
@ThinkingandTinkering
8 жыл бұрын
+Bartosz Barejko thanks mate
@libertariamemes
8 жыл бұрын
I fully agree! :D
I love this stuff it's absolutely fascinating
The possibilities that immediately ran through my mind for that foil.... WOW
@magnuswootton6181
Жыл бұрын
yeh flexable carbon!!! amazing thought defying stuff.
hiya mate, thanks for your comments. The chicken feathers could be carbonised using a HTC process I think. I haven't tried it but I think it would work. Havea look at the hydrothermal carbonisation video for details. As for storing hydrogen. I am not sure but I will look into it
This is fascinating stuff, I'm about 7 years late but still think is worth a thumbs up 🙂
Cheers for that. As far as I know the expansion depends on rapid gasification of the intercalant. I'm not sure lower power will be successful. But I would certainly like to know.
I kept breaking glass - lots of glass - too until I came up with a twist; now I use kiln paper to hold the graphite. I fill a bowl with sand, then place the kiln paper holding the graphite on top of that. *many pieces of glassware were harmed in the making of this comment. Keep up the great work!
Thank you very much for all of your amazing work... Have you interrelated G with HF acid before??
Thank you for all the info! Hopefully, very soon, I will be trying out a 10kv setup I have rigged up for instant exfoliation. (I hope) I guess while I wait for shipping, I can set up a roller press for foil production...
no probs mate - good to hear it is going well
The foil would be a great battery plate. The pipe autoclave I have used is a good acid alternative for intercalation. If you want exfoliated graphite you are going to have to intercalate
Me neither I am fascinated to see if it works. If it does you have a real winner there
Brilliant as usual.
It does work well doesn't it. Sonicate it and it should disperse reasonably well in a solvent. Don't expect high concentrations though. In order to get higher concentrations you will have to add a surfactant to prevent graphenes natural desire to agglomerate
pretty much. Leave out the water add three times as much ferric chloride and a gram of aluminium chloride and what you get out will be ferric chloride intercalated graphite. Check out my gic video for details
All I can really say is I have done this quite a few times with no real problems but i did use bought reagents most of the time. Now I just stick it in the house oven as the insulation is so much better than my little shed oven and I don't worry much about it. Familiarity breeding contempt and all that - so basically i jam all the chemicals inside the pipe leave it and go back to it when i think it is done. But as I said before - safety first!
I live in Houston, TX. There aren't many supplies in any of the hardware stores near here. I got weird looks when asking about potassium permanganate. I thought it better experience for me to make the stuff I need myself. Kinda like a refresher course since high school was over a decade ago. My expertise is in electronics and control wiring, so once I have some intercalated compound, the rest will be easy! I decided to use an old curb-side wall oven to save my hide also...
where are you from that chemicals are so hard to get hold of?
no arcing is incidental - it's the sudden increase in heat - graphite is a microwave susceptor
Hi Mr Smith. I've been following with great interest your teachings. I would like to ask you what is the fastest way to produce carbon nanotubes from chicken feathers in order to store hydrogen in a solid state. And how it is done. How can we store hydrogen at a low pressure and how to release it. Many thanks in advance. I'm looking forward for your response. Kind regards, Joao
Interesting reaction with no toxic fumes, since the ratio is 4 sucrose (used powder sugar) to 1 sodium bicarbonate then 2 mol of NaHCO3 deoxidizing 8 mol of C12H22O11 produces 96 mol of Carbon-12, 1 mol sodium carbonate, 12 mol H2O and 1 mol CO2. Any suggestion on how to remove the washing soda from the resulting product? Baking soda reacts at 50 C, I wonder if the reaction under pressure will yield a carbon lattice but the resulting pressure might be too high at 186 C sugar melting point.
Another amazing video! 20 seconds shouldn't blow the fuse but might weaken it after 10 runs like this. You could replace the fuse with a circuit breaker with a pop up button so it won't slow you down replacing fuses, if it becomes an issue...
amazing. thanks Robert!
I just wanted you to know I am still on the case to find the limits of voltage and amperage and possibly resonant frequency to preform the exfoliation asap. I don't have access to many chemicals, so I made hcl, ferrous chloride solution fairly weak, and alcl3 powder. I am going to use the autoclave method at 450F for 8hrs. Can I forego dessicating the ferrous chloride and use solution? My graphite is from many pencils and in short supply...
That foil would make a Positive battery plate ? While the Pos is the one to crumble in lead/acid batteries, it would at least extend the life of the battery (as long as not reactive to alum+water say as electrolyte). "intercalates the sulphate", hmm, am trying to think of a way of doing this at the bottom of the fridge with epsom salts and vinegar or something similar. Got no sulphuric acid and no budget. Are there options for intercalating ? Cracking video - in more ways than one :)
Very good idea. I will do this. Mostly I use a cheap microwave for these experiments so I don't worry too much about blowing it up. But I will do as you suggest I think.
Thanks for that. I will make one soon
" The pipe autoclave I have used is a good acid alternative for intercalation. " Does this equate to bunging some of the RS graphite into a pipe (with water?) and cooking it for a few hours in the oven?
hey robert, i was unable to find graphite in my locality ... somehow i arranged to get 20gms of it thru an old chemist and it was all he had ... and i m not sure whether i could find more..... so 20 gms is the limit .... can you please suggest the best method for preparation of GO in your experience ... with most success rate... also some prerequisite tips and don'ts
Hiya mate, phosphoric acid to 80% is sold as a food additive from industrial catering supplies. If you can't get con sulphuric you can distil battery acid, by heat or freeze distillation bullit is 98% you could order online. I use a local chemical supplier. But you have mcmasters Carr they sell everything
good luck with it let me know how you get on.
That looks a lot to what you get when you dehydrate sucrose with sulfuric acid or if you combine the sucrose 4/1 ratio with baking soda and burn it with a clean burning alchohol. That is used to do those wimpy fireworks called black snakes. I might try to make some at home to see if it's the same stuff. I would doubt it will be graphene like some claim but it could at least be exfoliated graphite.
I made 2 Fe3Cl solutions, both I made using 100ml distilled water, 100ml HCl at 37%, one fine grade steel wool pad, and later 200ml hydrogen peroxide 3%. First one I boiled for 2 hours and got fairly concentrated solution. That is dessicating in with some NaOH crystals. The other solution is pale at 400ml, but dissolves copper rather quickly. I'm thinking of just using 10ml with the 12g AlCl3 and 4g graphite. Will this destroy my wife's kitchen when I pop it in the oven for 8hrs?
impressiv reaction!
I was only concerned about using Al and Fe together in a pressure cooker causing some thermite reaction... the oxygen would be present as a miniscule amount of water from the solution. I'm thinking it would not be enough energy to set it off, but I was looking for confirmation.
Hi Mr Smith, I've heard about an ultrasonic way of producing huge amount of Graphene. In this process, Graphite is added in a mixture of dilute organic acid, alcohol, and water, and then the mixture is exposed to ultrasonic cavity. The acid works as a “molecular wedge” which separates sheets of Graphene from the parent Graphite. According to them, by this simple process, a large quantity of undamaged, high-quality Graphene dispersed in water is created. Let me know what do you think about it?
Sorry to spam, but the more I think of this, it seems the sodium bicarbonate to sodium carbonate reaction causes the structure of any carbon lattice to break because of the water and CO2 vapor pushing the column. What you really want is to take the water out of the sugar and that is what caramelization does, although you will have to go to the point to make a bitter caramel with almost no water (graphene oxide?) and by baking it further you will get graphene? or caramel with all the water gone?
Having a bit of trouble finding chemists who will sell me the chemicals locally. It seems everyone I talk to is terror struck and scared to sell to just anyone off the street...this country (US) is so set against innovation it is very frustrating. Is there a good online chemist you would recommend?
yea! my fist batch of intercalated graphite should be ready to wash tomorrow. Sounds like a fun week end coming up... ;)
Cheers mate
Just had a thought...try a teaspoon in the jam jar with leads from the capacitor bank in it, with a loose cover on it of course...lol. With the press of a button presto! Exfoliation complete! Seems the added energy input would shorten the time needed...
Thanks for the info. I have a big stick type graphite pencil (actually shaped like a pencil by Faber Castell) about the size of a finger, so would want to try that. It's a 2B I just noticed lol
one experiment that I'm on right now with graphite is the fact that graphite floats on top of a liquid ...I believe that there is a way and various applications actually that involves graphite and various liquids ...if graphite covers a surface area of a liquid then there is forcibly graphene equally spread out onto the surface are of the top surface of the liquid .... extraction could be possible by freezing the liquid and repeating the process at this point it's just an idea I have but will experiment further would you have any insight on this or have you done any experiments to this nature
@ThinkingandTinkering
7 жыл бұрын
no mate - sorry
@tiekauntan3264
7 жыл бұрын
I had the same idea a while back. What if you keep the graphite flake at the interface of two immiscible liquid, then freeze both and shear them apart?
and then we get the brown coloured dispersion of graphene oxide right?
Don't forget that the Plasmoid generates ozone (O3) and nitrogen oxydes ( NO and NO2), so you need to do this experiment in an open and well ventiled area.
it does sound like fun ahead lol
I just use a long wire with a safety cut out for this sort of stuff. Switch at one end of the wire dangerous experiment at the other and an rcd between the supply and switch. Saves pressing the button and running for it lol.
i did this... i got fairly good exfoliation... but is this dispersible in any solvent? my purpose is to make conductive ink
Ran out of space on my reply, what I mean by too much pressure is that the heat needed would be higher under pressure and the expansion and gases might be too much for a home made autoclave with no release valve set to whatever psi your weaker (nipple) pipe fitting could stand. Trying it on a water solution might not help since it will prevent the temperature to reach the sugar melting point, but I'm not sure that's needed for the reaction to start I guess I could try at one atmosphere first.
None of the drain cleaners locally sold contain sulfuric acid, and the only source of phosphoric acid I can get is around 3% in the diet cola. I have shopped walmart, home depot, lowes, garden ridge, food town, krogers, and the dollar store... everything says, "NO PHOSPHATES"
I agree absolutely with making the stuff yourself. You learn so much more from doing than reading. You can order this stuff - and so much more - from mcmasters carr - I am actually a bit jealous of you living in the States because mcmasters carr only deliver in the US. I wish I could order from them!
@zenmanproject
6 жыл бұрын
If McMasters still doesn't ship outside the US, let me know and I can act as a go between for you whenever you need something from them. We can have them ship to me, then I'll ship it to you.
I will try. It is only a question of time
My intercalated compound seems to be good. I will post video for my results soon. I'm hoping the resistance will be very low in foil form for use in capacitors. Sorry I can't use the reply function through this mobile youtube app...
4/21/14 the sound is so bad I can not hear. is it possible to turn up the sound
My attitude only appears relaxed. I take a stupid amount of precuations
Are you a health and safety officer? This is a kitchen experiment not an industrial process. If you do too much you will blow up the microwave - kind of self limiting I guess. However, the experiment is no more dangerous than driving a car. Stop warning people of how dangerous it is to live - we know! And don't write a long missive back defending your viewpoint - I understand it perfectly - I just disagree with this kind of fear mongering under the guise of safety
Cheers mate and thanks for the plug lol
Following the microwave, you mentioned sonicator but would further reduction to graphene happen in a water/acetone wash you described elsewhere?
@ThinkingandTinkering
7 жыл бұрын
i believe it would mate
@deangermeten5629
7 жыл бұрын
Oh, I just found your H2O3 method, so never mind! ;) Hey, might you know how to turn bio-char/organic charcoal into graphite?
@ThinkingandTinkering
7 жыл бұрын
yes search google scholar for graphetisation
I will video this, just working out a rapid fire mechanism with a timer and relay I think.
How is it exactly that you prepare the lead? I was planning on doing it with one solid stick/piece of lead that is used in mechanical pencils. How would I prepare it in that case.
@ThinkingandTinkering
9 жыл бұрын
i buy graphite flake powder at 5 microns - i guess you would grind the graphite down - beyond that i have no idea as i don't use that
@tiekauntan3264
7 жыл бұрын
Maybe it's a little late. I've tried grounded pencil lead and it tend to explode into splinters in the microwave. Maybe I didn't grind them fine enough but the clay is really troublesome.
My friend what you are prosperingseems similar to tang lau method interesting
the master wizard!!!! :)
Sorted. Will PM you when I have one.
no worries
Yeah, it yielded amorphous carbon with some sodium carbonate (tried the baking soda and sugar) it obviously doesn't compress like exfoliated graphite at all :) but hey it did yield quite a bit of amorphous carbon.
Have you tried to build a supercapacitor with this material and aluminium foil? I think you've made quite a discovery...
Lol. I will definitely take you up on the microwave offer lol
oh have I got an idea!!!!!!!!! I'll let you know how it goes.
intercalating carbon with an acetate?
Dear mr.Murray No intention to alarm But as you rightly say "This is a kitchen experiment" and there may be people (especially kids) think that by using a microwave is not going to happen. I just wanted to give some advice of what we also happens in this experiment and nothing more ... Anyway Thanks for your experience ..and sorry for my bad English..
It's cool isn't it
Cool cheers mate
Lol. Bless you but no way. Acid dehydration of sugars will give you an amorphous carbon. If you try to compress it you will get a powder. If you compress exfoliated graphite you get a graphite foil. Try it and see you will quickly note the differences
I tried exfoliating my GIC (FeCl3 one) in a microwave. I did not get expansion anywhere near what you got and the arcing was limited to few tiny sparks. Can you tell me what could be possible reasons?
@ThinkingandTinkering
10 жыл бұрын
Insufficient intercalation maybe? Did you overwash it/ or maybe used too weak an acid or the temperature of the GIC synthesis was too low or not enough time - anyway the root cause is from having too little FeCl3 intercalated into the graphite. The microwave exfoliation process will work just as well on bisulphide intercalated graphite - which is an easier synthesis - but the fumes it produces are not pleasant -so you would need to do it in a fume hood - or outside and dedicate a microwave to doing it - or a microwave you just use for experiments - whatever - it wouldn't be good for food after you exfoliated a bit of it
@sukumarhonkote9936
10 жыл бұрын
Robert Murray-Smith Thanks for the tips. I had put two reactions yesterday. Hope they yield better results.
@ThinkingandTinkering
10 жыл бұрын
good luck mate
Well.. I was just watching this and I thought "when does he pull out the multimeter on that foil??" - Then it happens!! :D
@ThinkingandTinkering
7 жыл бұрын
lol
That's because I was using the house microwave. My wife will kill me if, actually when, she finds out lol
Lol give it a go. Stand well back though!
Cool
how to make graphene from this expanded graphite
@ThinkingandTinkering
7 жыл бұрын
lots of ways - have a look on google scholar
can we use it for filteration
@ThinkingandTinkering
7 жыл бұрын
dunno
I use a separate cheap oven so never worry - but I would advise being prepared for your wife's wrath - always better safe than sorry
The microwave stuff reminds me of vermiculite..
I love chemistry lol
charcoal animal powder and graphite same ?
@ThinkingandTinkering
7 жыл бұрын
no mate - please don't ask me how they differ this can be found by a quick read of wikipaedia
@galax2928
5 жыл бұрын
Robert Murray-Smith Hello do YOU make graphene in the macro we?
so how's exfoliated graphite different from graphene?
@ThinkingandTinkering
9 жыл бұрын
mukund srinivas oh mate - you need to have a read - or watch the video on doing the work - this is a question you can easily answer for yourself by reading around a bit and would take me a lot to describe to you
@mukundsrinivas8426
9 жыл бұрын
I found it man :p so I am confused if I should go with the tour method or if I should go with this microwave method. What do u reckon?
@ThinkingandTinkering
9 жыл бұрын
mukund srinivas depends on what you want it for
@mukundsrinivas8426
9 жыл бұрын
Well say super caps for now.
I'm given them all the time. The next that I find works I will send to you. You will live longer that way. LOL. Oh and I don't take no for an answer. This thicko needs your chemistry videos. You can't do that with a microwave sticking out of your head. LOL. SSSSHHHHH everybody. Don't tell his wife.
Sir, do you believe in Patents?
@ThinkingandTinkering
7 жыл бұрын
nope - i did a couple of videos on my views on patents mate - they are in the discussion playlist
@arrowstheorem1881
7 жыл бұрын
Robert Murray-Smith Ok, thanks, will look up on those videos.
If your microwave is 1kw, and you cooked for 20s... need about 4Gw for about .005s. Or hit it with the 4 capacitor bank about 32 times in rapid fire mode. I am going to wear a face shield I think...
no - you get grapheme - to get grapheme oxide you will have to oxidise it
Amazing results. Got to have a go. Time situation this end to overcome. Oh by the way. This video shouts "I AM NOT USING MY CAMERA PERSON!". You can tell that by chopped head and you have the shakes. LOL LOL LOL. Come back camera person. Our eyes can't take much more. LOL.
how I wish you could upload it in Spanish would greatly appreciate it
lol - you MUST video it!!!!!!!!! - and post it if you survive lol
Cool lol
Lol I agree
isn't it lol
Grumble grumble...2 Pyrex's later and I discover the microwave is crap and only seems to heats on one side. UGH ever forward
@ThinkingandTinkering
7 жыл бұрын
i should show the 99 failures for every success mate - i don't but i broke quite a few myself getting here
@zenmanproject
6 жыл бұрын
I just broke a pyrex... How did you figure out where it is heating?