Synthesizing graphene in your basement laboratory

graphene-in-the-home-lab

We’re surprised that we haven’t come across any of [Robert Murray-Smith’s] projects before. Looking through his collection of YouTube uploads proves that he’s a very active amateur chemist (we assume this is a hobby because he performs the experiment in a mayonnaise jar). The video we’re featuring today is about ten minutes of his technique for synthesizing graphene. The video can be watched after the break. Be warned that the audio doesn’t sync with the video because he overdubbed the presentation to fix up the poor audio quality from the original.

Graphene is something of a compound-du-jour when it comes to electronic research. You may remember reading about using DVD burners to make graphene film that will go into thinks like super-capacitors to replace batteries. [Robert] starts off his process with a jar of 98% sulfuric acid and 75% phosphoric acid. He pours in powdered graphite (chemical proportions are important here) and gives it a swirl. Next some potassium permanganate is added over about five or ten minutes. From there it goes on the stir plate for three days of constant stirring. During this time the solution will go from green to brown, indicating the presence of graphene oxide.

He goes on from there, but it’s clear he hasn’t found an iron-clad route to his end goal of isolating the graphene for use in constructing things like those super-capcitors we mentioned earlier. If you’ve got a home lab and some interest perhaps you can contribute to his efforts.

[Thanks Bruno]

54 thoughts on “Synthesizing graphene in your basement laboratory

  1. Just a couple of small typos:
    “that will go into think[g]s like super-capacitors”
    “constructing things like those super-cap[a]citors we mentioned”

  2. a jar of 98% sulfuric acid and 75% phosphoric acid.

    say what? I thought effort was the only thing whos sum could exceed 100%…

        1. Why the use of percents anyway? Am I alone in the fact that it is very difficult to conceptualize “75% acid”? What does that even mean? Now if you said it was 10 ml of acid at a certain molality or molarity, then I’d know exactly what you’re talking about.

          1. It’s just a by-volume solution. You can think of it as 3/4 of the total volume of pure acid and the remainder pure water. Similar to white vinegar, which is typically 5% acetic acid by volume, the rest water. Same thing with isopropyl alcohol, 70% solution of pure alcohol, the rest water.

          2. Actually, you’ve provided the proportion for “Rubbing” alcohol. Isospropol is available in a number of water proportions and purities. Long ago when I soldered and restored burnt one-off circuit boards to pay the bills, we used 99.9% filtered technical isopropyl alcohol or pink ethyl for in-work flux cleaning before stripping and re-applying conformal coating.

          3. In chemistry, when a % is indicated by itself, it is always assumed to be % of mass (w/w). This convention is useful because of the various different densities of chemicals and mixtures resulting in different volumes, which can cause quite catastrophic results when you consider Avogadro’s law.

    1. These percentages are the “strength” of the acids, i.e. the Sulfuric Acid is not 100% Sulfuric Acid
      For example, the Hydrogen Peroxide you can purchase OTC (Over The Counter) for home use is (often?) less than 10%.

      1. I have seen 2 and 3% in normal pharmacies. (I use it for mouth wash and to get spots out of white shirts). Go to a hair dresser and they can get up to about 36%. Stronger than that you either need to go to a commercial supply house or concentrate it yourself. The old Bell Rocket Belt used close to 100% Hydrogen Peroxide pushed through a platinum screen by a nitrogen bottle to fly folks around the sky. (See old James Bond movies for graphic reference … my dad worked for Bell Helicopter and they had the ‘rocket belt’ there for special occasions. Good PR)

        H2O2 was used in WWI as a disinfectant for cleaning wounds and in surgery before better stuff became available in WWII time frame.

    1. as well as a part 4 and a video called “Methods of making graphene” – I think it is safe to say that he is spending a fair amount of his time mulling over the techniques. These can all be found on his youtube page. I saw these the other day but didn’t have time to watch them… until now :)

      *getting more coffee*

    2. ..wonders what other intercalation compounds work as well and make the best batteries..

      LiCl instead of Al3Cl? Anyone heard of lithium polysulfidophosphate? o.O Just found it mentioned on Wikipedia for Lithium-sulfur batteries.

      (*grabs a coffee* and thinks long on the subject)

      1. Check out Ignition!, the frightening memoir of a rocket scientist who worked with such breaths of spring air as chlorine trifluoride, the stuff that eats through sand and dissolves teflon.

  3. I remember the joy I felt receiving a super-duper deluxe six-panel chemistry set. Things like that aren’t sold anymore now that amateur chemistry is one indicator of possible terrorist activity. Purchases of strong acids are recorded and reported.

    What a horrible place America has become since the terrorists won.

    1. I concur.

      And be careful with the potassium permanganate… it’s exothermic when mixed with ethylene glycol.

      1. I was so lucky not to be born in time for today’s set of laws. Some of the ad hoc experiments I was involved in then would certainly land me in some ASU today.

    2. Back in the day, the things now being sold as “chemistry sets” would then have been referred to as “spice racks.”

    3. Purchasing strong acids wont get you on any list. You can easily buy 80% phosphoric and 99% sulfuric from Bio Diesel supply companies like Duda Diesel. They’ll even sell you 51 gallon drums if you really want. Hell, even if you want to buy explosives grade Ammonium Nitrate and Dark Aluminum Powder you can walk in to a big box store like Gander Mountain and pick up Tannerite Exploding Target Indicators with cash, no ID required.

    4. I have a copy of the ‘Scientific American Book of Projects for the Amatuer Scientist’ edited by C.L.Stong. It is great but the stuff to build the projects is getting to be harder to find. (I built the low speed wind tunnel and the NMR – that used TUBES for the electronics .. and yes, it worked) … Metallic mercury in 10 or 20 lb flask is now considered dangerous because folks are not considered able to not eat anything they have around. Fertilizer we can buy at the local co-op (my wife orders 2000lbs at a time to fertilize fields) now get reported to the Feds. The largest non-nuke man-made explosion was in early 1900’s in Texas City, TX, when a freighter of diesel ran into a large barge of chemical fertilizer. It was a bit smaller than the bombs dropped on Japan. Flattened ‘everything’ for a mile+ and broke glass a long ways past that. Considering the explosion was a ground level, that was a HUGE amount of force

    5. I have fond memories of having one of those sets as a kid too. I was born a little late: they were no longer sold in stores… but garage sales still had the good stuff. It’s the same story with textbooks: some of the old ones were free to cover the science of subjects considered too controversial today. I carefully guard a few good ones :)

      I became quite good at tinkering with chemistry/biology/electronics/programming, finished a couple of university degrees, and when amateur research became discouraged in these fields… I ended up moving to a developing country (writing grant applications is doubleplus boring). Since things are always breaking here, I have lots of interesting and rewarding work, and access to more or less any substance, component (or even medication) you can think of. Sure, various tropical diseases can be a problem… but I’m sure I’m not the only one willing to trade a little safety for a little liberty.

    6. Not really. Though some live in fear of being on some terrorist list, you can still get your hands on some really interesting chemicals. Ammonium Nitrate is not unobtainable despite the harsh focus on terrorists using it to make ANFO. I say, put me on your list if you want. Heck, feel free to knock on my door and ask me what I’m using those chemicals for and I’ll be happy to tell you that greek fire is a rather interesting reaction to play around with. It’s still a free world even though the media would have you believe otherwise.

      1. The world is free, but those in the US are not as free as they once were. Drop us a postcard when you find the GPS tracker stuck to your car ;-)

  4. I’ve watched several of his videos and I must say I’m mightily impressed by what he’s attempting. He seems to really know his chemistry.

  5. I want to point out this reaction is incredibly hazardous and produces Mn2O7, Manganese Heptoxide, a very unstable compound that will ignite on contact with many organic materials. On this large of a scale, it is producing copious quantities of ozone and it also is sublimating.

    1. He discusses this in video 4 – you have to keep the reaction below 55 deg C to avoid creating Mn2O7. That’s why you add the permanganate slowly.

  6. This is dangerous crap, this guy seems to be trying to kill you or hurt your health. Don’t follow these instructions. Batteries and capacitators use activated carbon sheets, activated carbon is expanded by heating. But ask yourself what you are going to do with the supposed graphene when you’re done. This is like hiking through Chernobyl for the fun of it.

    Reminds me of the alchemist that wrote up the formula for gunpower and added a last phase “Heat under pressure” to eliminate any spies.

    1. Tour the Chernobyl exclusion zone you say?

      http://www.benlovejoy.com/journeys/chernobyl/exclusion/

      Also, one of the SparkFun guys is heading there with his GPS enabled logging Geiger Counter.

      If I was a nuclear physicists I would want to don protective gear and get as close as possible to that train-wreck. It’s a reminder of what happens when poor engineering intersects with cronies that have no clue.

      Your attitude towards risk is exactly why kids chemistry sets are lame and there are disclaimers on everything (Contents are Hot? Lolwhut?). If you can’t take responsibility for your activities, please go back to video games and TV and leave the real world to those of us who are prepared to educate ourselves and take our chances.

  7. Ok, for everyone here who’s skeptical,mainly this guy /\ this is actually a pretty standard way to make graphene oxide. It’s called the modified hummer’s method, and there’s a paper writtenn on it by a malaysian dude. The guy in the video has simply translated the paper into his own words and made a video on it here’s the link http://www.ncbi.nlm.nih.gov/pmc/articles/PMC3260037/pdf/ijn-6-3443.pdf . I have personally tried out his methods to the word, and it has produced the same results….

  8. I get a bit annoyed by the over cautious – I mean if you suggested that they sit on several kilos of high explosive and set alight to it they would be up in arms! but this is what millions of people do everyday when they get into their cars. Of course it is a controlled situation and so is making graphene – it is no more dangerous than driving a car. I have a suggestion for those cautious guys – don’t do it – then they probably don’t do anything – just try to tell other who want to experiment not to do it.

  9. I mean Tech 2007 and Greencheck – who are these guys – graphene salesmen who don’t want you making your own (have you seen the price – we are talking big bucks here!) or health and safety police who want you to dress in cotton wool suits and travel everywhere in safety bubbles – these are the kind of guys who suck the fun out of everything

    1. Agreed.

      People like these project their own minimal understanding and lack of safety skills upon others when they proclaim something shouldn’t be done. It’s scary to them, so they think it should be scary to everyone. Sadly, I think this is why we have some of our laws and restrictions here in the US. People have come to expect safety to be the same as legality, so if it’s not illegal it must be safe! And if I come to discover something is unsafe, we must outlaw it to protect our citizens! Take away a little of my freedom so I don’t hurt myself. Why not just educate me and treat me like an adult who can make his own decisions?

      1. ” Sadly, I think this is why we have some of our laws and restrictions here in the US”

        And you would be incorrect in that thinking.
        The reason we have some of the laws we do in the US is because some greedy cesspool bottom feeder figured it was better to make money at the expense of an innocent bystanders health and life. Implemented enough safety precautions to keep himself safe but ignored the precautions necessary to keep the environment and community safe.

        The end result is that tax dollars went into cleaning up the environment that the greedy cesspool bottom feeder polluted. Thereby robbing the public of both health, time and money.

        It is never OK to make a profit when doing so will hurt others, even if doing so is not illegal. A person has to be pretty sick in the head if they can sleep at night knowing that their wealth came by way of sacrificing the health and lives of others.

        Keep in mind that it was the deregulation of the financial community that lead up to the recession we continue to find ourselves in. It was allowing businesses to ship jobs over seas for their greed of profit that has prevented the US economy to return a productive job creating boom.

        If you will allow your employer, or anyone Else’s employer to come into your home and poison your bed or your children’s beds in the name of having a job, then you are nothing more than a slave that is owned by those who would do so in the name of profit. We have regulations because not having those regulations costs more money to correct than what those regulations cost to prevent.

        Despite the weeping of the greedy business man, regulations have never cost jobs or prevented the creation of jobs. The real culprit is allowing products to be imported into the US from countries that do not have the same safety standards and environmental regulations as the US. Historically, no country has been able to compete with US workers that have had to do so on the same level playing field, and that still stands today.

        Globalization is what is harmful, not safety regulations. That said, if one wishes to put themselves into harms way, one should be allowed to do so as long as in doing so one does not endanger innocent bystanders. You don’t have the liberty to jump off an overpass into traffic as doing so may cause a multi car pile up and take another’s life. If however, you choose to jump off a cliff where there is no one below that you can harm, you are within your liberties to do so.

        1. Indeed, but I suspect that his statement still stands. There are certainly *some* laws in place to protect people from themselves. Some are largely just in my mind (Seatbelts are cool with me; people are terrible at judging how risky driving actually is and it’s so pervasive that legislating using safety devices is okay with me. If you don’t want to wear safety glasses in your shop isn’t for me to decide, though it’s foolhardy), many are irritants to those willing to take their existence into their own hands.

  10. Scott missed the point – we are not talking about public safety and global issues – who can disagree with that – we are talking about private choice and why some people deem it necessary to treat us all like children. I find myself agreeing with the alchemist – but perhaps what is even more interesting is that we are now talking about safety instead of about making graphene, graphene based supercapacitors and graphene based batteries – isn’t this what these posts should be about? Shouldn’t we be exciting ourselves and our youth into creating a new world for ourselves? or should we be bitching about using knitting needles without corks on the sharp end? after all those little devils are sharp! If we get too distracted by this everybody is left feeling cold to the subject and it goes nowhere – which is what I suspect was the point of the earlier posts – how about we just agree to take proper precautions and leave it at that then get on with discussing the real issues – like how to make it and how to make your own batteries etc without paying a fortune to ‘the big boys’

    1. Have you tried this method at home – I sincerely doubt it. For the home chemist this is not easier. Check out the electrochemical method.

  11. Graphene oxide is not the same as graphene. Yes, it can be reduced to a highly defected, small domain, low mobility form of graphene (possibly good for some things), but it will not have many of the interesting properties of pristine graphene.

  12. Robert did a good one on making Graphene directly. I hope he does another step by adding spacers between the graphene to avoid restacking and to get higher capacitance

    Well done Robert keep up the good work.

    Salam from Cairo Egypt

    Alaa

  13. Have a look at this

    is a possible engine made from a naturally occurring high crystalline high diamagnetic graphite and then have a look at this

    it is for a conductive ink that’s makes the competition look like pants.
    You can get these things really easily from

    https://sites.google.com/site/thinkinkfactory123

    for the ink and diamagnetic graphite. And they are cheap!

  14. I comment when I like a post on a site or if I have something to add to the discussion. Usually it is a result of the fire communicated in the post I browsed. And after this post %BLOGTITLE%. I was excited enough to post a leave a responsea response ;) I do have a few questions for you if it’s okay. Could it be simply me or do some of these comments look as if they are coming from brain dead people? :-P And, if you are posting at other online sites, I’d like to follow you. Would you list the complete urls of your shared pages like your Facebook page, twitter feed, or linkedin profile?

      1. … and because it was written in dos batch language? I think I might like to see the rest of the code. Scraping a site to post a comment in that language might show some interesting tricks….or it will be a horrible mess ;-)

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