I guess you could try it and i don't see why not - but it is probably better to leave it out and up the pottasium permanganate a little. You are spot on about the sonication.
It's greenish because of unreacted graphite. I have had this a couple of times. What I did was dry the whole thing and re run it. On the second go it was much better - bright yellow. There are so many factors influencing it getting it right first time can be a bit challenging. Luckily, it is hard to get completely wrong. As I said I it does go wrong just dry it and do it again. The first run will be like a pre oxidation stage and the second time it is more or less bound to go well
Hiya mate - dry it completely . You have to be gentle in the drying and it takes ages. But, when it is dry powder it in a coffee grinder and wash it with DI water. The sonicate it.
yellow is good mate - the more yellow the more oxygen. it's a complex system there are a ton of variables and it is impossible to say what happened but yellow is good lol - to raise pH to 7 just keep washing with DI water. If you add alkali it will irreversibly coagulate.
Sorry, you must think i'm nit picking. The video is very positive and breaks it down into easy to follow steps. Thank you and I look forward to your next video
Harris seeds sell it in the for US $14. So I guess a farm supply will have it. Or just order online. I followed an order through without a problem. It is also called Chile saltpetre and used as a food preservative.
Well, in a sense you are right I guess. But, as it reduces the reagent count and reduces the time from 5 days to 4 hours start to finish therefore making it so anyone who wants to can now do it as a weekend project makes it worth reporting, don't you think? Plus the video is just that much more 'watchable', better sound, better explanation, clearer instructions - I don't know but I get a sense you should look more at the positives here.
I firmly believe they can - if they take the right amount of care with the chemicals of course - I have tried to include a bit about safety recently too - mostly due to others banging on about it! lol
It's a standard fertiliser but the best thing is to order online. Lower concentrations won't work. The reaction conditions are harse and nee to be in order to get it to work as graphite is so unreactive.
I have found one method (P. Chiu et al) that utilises the Nitronium ion to oxidise graphene without the use of KMnO4, and uses only HNO3 and H2SO4. Makes sense now, it just helps a little to give you a higher yield.
well, you could try filtering first - but that'll take forever - not a problem if you don't have that much and you are patient then wash or keep washing in normal water until the pH is 6 or 7 then wash with DI water to reduce the ion count - it's about all you can do if you are going through gallons of the stuff - i am afraid i have DI water system so it doesn't cost me much for gallons of the stuff.
It would be very helpful to know exactly when the solution becomes *potentially*explosive and at which point it is no longer explosive. Maybe by color? Temp? Basically I am not confident that I could know if I made a mistake in my process whether the solution is now dangerous. Can you please give some criteria for knowing by looking or temp if it is explosive? Having this criteria would give confidence try this and be safe. Thank you for a good step-by-step video. Cheers.
I'm struggling to see the improvements compared to some of your older videos.. you've shortened mixing times at warm stage and used stronger peroxide and more water later on. Good video and I appreciate your contribution to my post schooled education :) I think i'll put your words onto paper so I can pin it to my wall, and avoid the thermo melt down, we can take back the world one jam jar at a time
oh yeah - another interesting way is to ball mill it with solid carbon dioxide - but i think it is a bit beyond home chemists to do it. I may be wrong - it's just my opinion.
a short piece of glass tube taped onto a screwdriver! it's is caustic and hot so glass is best but i didn't have one long enough and i didn't want to get my hand in there.
The tour group think NaNO3 contributes very little which is why they left it out. Myself I think it helps pre oxidise the graphite before the main show - so to speak.
Thank u a lot for sharing this interesting experience.. So, I recuperated graphite from PC batterie and I'will use it for the synthesis of graphene oxide, what's your opinion? ..
One shot instant drain cleaner from B&Q. It's in their plumbing section or bullit drain cleaner which I get from my local hardware store. Spirit of salts I get at a builders merchants.
Well ,in Germany it is compliated to get chemicals in a really pure form ,if you are young and because Germany has strange laws ,which affect me and other people buying chemicals .I´ll tried it with the fertilizer and the pouder from the meat-market ,which contains 50% NaNO3 ,so i must concentrate it .Thanks for the interesting video ;)
Have you tried first microwaving the graphite flakes in a microwave oven? There are some papers that indicate that by prepping the graphite first in this way, you can improve the efficiency of the oxidation process
Very nice video, much more than the older ones.Thanks for your effort. Do you think the Sodium nitrate can be substituted by potassium nitrate ? (maybe some incompatibilities around the potatium permanganate phase) I assume that after cleaning, GO must be sonicated before coating some stuff, is that right ?
nicely done Robert! Another new project for me :) By the way, the graphite,...I have a graphite which has a resistance of 2-3 ohms! is this good for GO?
For those of you who want to find local dealers for some of your chemicals. NaNO3 is sold at pottery supply centers in 5lb bags for $10 ~98% H2SO4 is sold at hardware stores as "Professional" drain cleaner
Hi Robert, Great job! thank you helping others to get this done... Got a question. I have Graphene (NOT Graphite) source and I used it instead. I went through the mentioned Steps though, I didn't had anything interesting at the end.... Is it applicable to Graphene or .....?what is wrong with Graphene?
hiya mate You will get something but that is quite a low graphite content. if i were you i would go to an art shop and buy a higher graphite content pencil say a 6B or better yet 8B (they do go up to 9B and you can get graphite blocks to draw with) Your room temp is fine for the medium stage. Good luck - let me know how you get on
and I am also trying with Tour's method. Which method do you prefer? I guess Tour's method is more efficient with higher yield of GO production but less safe?? Thanks!
Great video sir, was already planning to try "how to make grphene 2" then i saw this improved version. I'm definitely going to be doing this now... i've got some questions tho: 1)would graphite from ordinary 4B pencils do or would the impurities in the led cause havoc 2)room temperature round here is 28-31C would this do for the medium stage or must it be exactly 35C? #Thanks
Dear Robert, Thank you for this Video, Its really helpful...I am going to try this method... I was wondering if you are going to heat at 98C (high temp zone)as you have mentioned on the notes or procedures on the board.
Hello Dr. Murray-Smith, thank you for making these amazing videos. Currently I am having trouble in the step where I add the water, after heating the mixture for 5 minutes at 100 ºC and right before adding the hydrogen peroxide. Instead of obtaining the orange color (as seen in the 19:00 mark), I obtain a Green/Brown color. Does the reaction needs to take place at a specific temperature? Or do you have any idea of what I may be doing wrong? Thank you very much
Miguel Azori It's very hard to give practical advise i am afraid as i am not there to oversee what you are actually doing. But by the time you add the peroxide it is all done - the fact you get brown green indicates an error in the earlier phases. What they are I don't know as i didn't see you do the whole experiment - sorry i can't be of more help
I agree, microwave-assisted irridation does help in the exfoliaton process. But does NaNO3 produce better results that KNO3? I have wondered about that for some weeks now and wonder if the Na and K are "spectator" ions and if so, will it work just as well or will too much potassium (with the KMnO4) be a problem?
dear Robert, sorry for bothering, could you please give me a favor and answer my question like usual😊I followed a method similar to "massive production of graphene oxide...." and I got a beautiful brown mixture after adding water(slowely) but then when I added H2O2 to quench the reaction I ended up with a greenesh yellow colour😭 I even used less amount than that one mentioned in paper... could you please tell me why?should I add H2O2 as long as the colour turns to brownesh yellow and not more?
Thank you very much Robert, but I have a doubt. When you say 2l acid, a type of acid that you mean? Sulfuric, phosphoric, hydrochloric ... can you tell me what proportion is the most economical for oxide 100gr? Because it is much the acid is spent for the little rust that occurs. Greetings and thanks for all the work you're doing
hello! thank you! excellent information for us!, two questions: 1. what is the best technique for structural and compound characterization graphene oxide?, 2: how long ultrasound is necessary to move from graphite oxide graphene oxide? congratulations! :)
For question 1: For a surface analysis and structural analysis, SEM or AFM is the best to analyze your image. For compound analysis, such as graphene to graphene oxide, FTIR will give the data for functional groups of graphene and which wave number will have occurred. For question 2 : Generally, time is varied by experiment to experiment.
Indeed. I think graphene oxide is a poor name. Originally it was called graphitic acid which is much better as it is actually a graphene basal plane decorated with carboxyl and hydroxyl groups as opposed to oxides per se
Hey Rob. I would like to understand the reason for sittiring the graphite and sulfuric acid for 30 min at the beginning. What is the purpose? Chemistry wise. Thanks!
Hello Robert, thank you for all your great videos!! One question: do you know any alternative for NaNO3, it's not legal to buy it in Germany. Thank you very much for all the inspiration and the great books! Jakob
Thanx Sir for your prompt reply, If I am using the graphite with 45 microns or bigger in size as the starting material, then what pore size PTFE i should use to filter the GO.
Being of automobile aftermarket customization, I wonder if this technology can be used to charge capacitors or batteries and extend the range of an electric vehicle. Very curious and ready to develop such an aftermarket addition.
what do you do with the remaining solutions after the washing ie the hydroclotic acid , the deionized water etc ? Can you use them again for the same washing steps respectively?
Hey Robert. First of all, you are amazing =P, now onto my question, I want to make a graphene super cap for a school project by burning GO with a light scribe disc burner. I realise that super caps may not be all that they are made out to be and what not but i really just needed something fun and challenging to do for my science project. Anyway, i was looking for where to buy graphite oxide and i had a lot of difficulty doing so so i did a bit of research. First I found that graphene oxide was a lot more easily obtainable than graphite oxide so I did some research on that. I then found that graphite oxide is being sold in places as graphene oxide. I then found that when you disperse graphite oxide into water it exfoliates into graphene oxide anyway. Please tell me if what I have read is true or if it is false and if I would be able to just disperse what they call "graphene oxide" into water and burn that to make my super caps (graphene oxide is apparently also water soluble). I also wanted to make graphene oxide but my teachers said no because it may be explosive. I then decided to buy some, I am only in year 9 so i have a tight budget and this was the cheapest graphene oxide I found www.ebay.com/itm/Single-Layer-Graphene-Oxide-Solid-150-Milligram-Per-Vial-/111297404661?pt=LH_DefaultDomain_0&hash=item19e9d79ef5 would that be suitable for what i want. Thanks in advanced.
Robert Murray-Smith Wow... O_o that was an amazingly fast reply... If i have anymore questions should i ask you here or would you prefer for me to ask them somewhere else (I shouldn't have that many questions from here on)?
just stop adding the permanganate and chuck a lot of crushed ice into the icebath. It'll calm down. When it is calm again leave it for an hour in ice then dispose of it as it will be ruined beyond redemption - though an easy way would be to run lol
Follow Robert Murray-Smith's videos on creating GO then use his spin coating method to produce a sheet of GO. Next use a xenon flash (dollar store camera flash) after for an extremely high quality cheap graphene sheet of customizable size. Remember the thinner it is, the better it is for super capacitors.
Hello Robert I tried this process in my lab and have some doubts regarding it. 1. Completed the process and kept for drying in a glass tray, it is getting dried by the day time and when I take a look after a night the dried slugger again turns into wet can find waters in it. What is the reason behind this? 2. What are the better methods to test the Graphene oxide, which test can be effective to tell how much graphite is oxidised and what is the percentage of Graphene oxide in it. Thanks buddy
vinodh kumar it's just a modified hummer's mate and subject to the same restrictions any hummer's based methodology is. Test methods are fairly standard - raman and XRD being 2 basic ones - i feel you should know this
It is a great pleasure to see your developmet. In a way, I would like to support it! Please, send the carbon and/or graphene coating sample to me for Raman analysis, I am very interested ;) I will also check the crystalline nature of your samples using advanced X-ray techniques.
You need to add a warning for the person following these instructions to wear eye protection and to have a water fountain nearby to wash off any splashes. Also some sodium bicarbonate solution ready to neutralize the acid. A rubber apron would also be a good idea. Since he'll be outdoors, curious onlookers should be chased away.
Hi Robert. Been experimenting with this over the last few months and I don't know why I didn't see this before, but silly question: When adding the 400mL of water & 50mL of 30% H2O2, you are essentially adding 15mL of "pure" H2O2 and an amount of water. Would this work the same way if you just used 500mL of the cheap 3% H202 (also 15mL of "pure" H2O2 with a little more water), or does it not work this way? -- Thanks!
I just finished my last batch over the weekend. Thanks for the clear and concise directions, I had really great success. 👍 It is a relatively safe, reaction if you obey your advice, I had almost no nasty fuming, it's really critical to keep the temperatures low as you said. The only step that particularly concerns me is adding the water to the mixture, (water into acid, eek!) would it be better to do it the other way around, add true mixture to the water? Also what's the best way to store it? I'm thinking maybe in a dilute H2O2 solution to prevent it reducing back to graphite over time?
I want to make it as well, can someone please let me know ALL the materials i would need to do this procedure SAFELY and with the right equipment? I don't have ready access to equipment so will have to buy what i don't already have. I would greatly appreciate the help!
Hello Mr. Smith I absolutely love your videos and your work!!! My name is Marlo D and I have an awesome idea to make the ultimate SWAG generator. My only problem is that I am afraid to make the graphene myself in fear that I will hurt myself or the children in my house. Can you please sell me a batch that you have made?? I think 15ml should be enough. I also need to clarify how to properly connect the negative and positive terminals. Thank you soooo much Mr. Smith please contact me back with info on how I could purchase. And it is water proof correct?
Do you think this is more cost effective than flash graphene? The only difference would be supplying your own renewable energy. A “flash graphene foundry” still requires a Lot Of Power, and the quality I’d still wonder about. For anyone making this business, you would need to employ multiple methods. Just to see your output quality, which in my opinion is everything right now. I still consider a lot of stuff out there with Graphene essentially snake oil:-/
Dear Sir, My 1st question is what kind of filter you used to get the final product as GO. Is it a normal filter paper, can you specify the pore size or it's detail? My 2nd question is, Does this GO you obtained can be used to get the LC phase?
getting LC phase and filter size depends on starting material - tto get LC phase you need graphite of 45 microns or larger. You need to use a PTFE or similar filter with correct pore size mate
So I should use the dried result of that attempt and use it as the input graphite and the next attempt? Should I extend the medium temperature stage at all? Because on the first try it didn't thicken up at all and didn't change to a brown/purple. It just got a little darker. That could be because my graphite is a fine powder.
Hello, What are you using to stir with during the KmnO₄ addition? I assume the solution is very acidic at this stage and wonder if an impermeable material is needed.
To your knowledge, what is the importance of the temperature in the "hot" step? While performing this experiment the heating portion of my stirrer got shorted out. So while I wait til tomorrow for it to dry out, I was only able to keep it around 70ºC with a bath. Do you know how I should expect my end product to be affected?
Hi Robert thanks for video. So after I mixed KMnO4 with solution in an ice bath, I increased temp to 35 Celcius degree and it started to explode a little bit. I put back right away in the ice bath and explosion stopped. But, solutions turned to be pasty grey mud-like solution. Can I still use this solution for further procedure? Thanks Rob
Do you recommend a specific particle size (mesh) for the initial 5 grams of graphite, or is it of little importance? Your final graphene oxide looks quiet homogeneous. How much of the initial graphite was oxidized accoprding to your numbers. Thank you.
it depends what you want - if you want large flakes you will need to have a large grade - you might want this for liquid crystal type that can be electrospun or you might want small for inkjet printing - so it is up to you - typically i use 45 microns but i have usedd 150 micron and 5 micron. depending on reaction time you can get 95% but be careful of overoxidation
I am using the same method but instead of getting black powder i am getting white color substance which is not a graphene oxide please help me with this .
Hello .. I stirred graphite, NaNO3 annd H2SO4 in ice bath..and also during the addition of water, i did use ice bath for precaution.Do u think the outcome still ok?
I never say something can be done unless i have done it and as i haven't i just don't know the answers - but that is all part of the excitement and fun of doing this - if you choose to do it you are breaking new ground - i would encourage you to try
I guess you could try it and i don't see why not - but it is probably better to leave it out and up the pottasium permanganate a little. You are spot on about the sonication.
It's greenish because of unreacted graphite. I have had this a couple of times. What I did was dry the whole thing and re run it. On the second go it was much better - bright yellow. There are so many factors influencing it getting it right first time can be a bit challenging. Luckily, it is hard to get completely wrong. As I said I it does go wrong just dry it and do it again. The first run will be like a pre oxidation stage and the second time it is more or less bound to go well
Hiya mate - dry it completely . You have to be gentle in the drying and it takes ages. But, when it is dry powder it in a coffee grinder and wash it with DI water. The sonicate it.
Bought your ebook yesterday. Great read. Many thanks for your efforts in educating the masses. Cheers, Vince - Canada
yellow is good mate - the more yellow the more oxygen. it's a complex system there are a ton of variables and it is impossible to say what happened but yellow is good lol - to raise pH to 7 just keep washing with DI water. If you add alkali it will irreversibly coagulate.
Sorry, you must think i'm nit picking. The video is very positive and breaks it down into easy to follow steps. Thank you and I look forward to your next video
It seemed easy before, but with this video, it seems anyone could make GO! Well done!
Harris seeds sell it in the for US $14. So I guess a farm supply will have it. Or just order online. I followed an order through without a problem. It is also called Chile saltpetre and used as a food preservative.
Well, in a sense you are right I guess. But, as it reduces the reagent count and reduces the time from 5 days to 4 hours start to finish therefore making it so anyone who wants to can now do it as a weekend project makes it worth reporting, don't you think? Plus the video is just that much more 'watchable', better sound, better explanation, clearer instructions - I don't know but I get a sense you should look more at the positives here.
I firmly believe they can - if they take the right amount of care with the chemicals of course - I have tried to include a bit about safety recently too - mostly due to others banging on about it! lol
It's a standard fertiliser but the best thing is to order online. Lower concentrations won't work. The reaction conditions are harse and nee to be in order to get it to work as graphite is so unreactive.
I have found one method (P. Chiu et al) that utilises the Nitronium ion to oxidise graphene without the use of KMnO4, and uses only HNO3 and H2SO4. Makes sense now, it just helps a little to give you a higher yield.
well, you could try filtering first - but that'll take forever - not a problem if you don't have that much and you are patient then wash or keep washing in normal water until the pH is 6 or 7 then wash with DI water to reduce the ion count - it's about all you can do if you are going through gallons of the stuff - i am afraid i have DI water system so it doesn't cost me much for gallons of the stuff.
It would be very helpful to know exactly when the solution becomes *potentially*explosive and at which point it is no longer explosive. Maybe by color? Temp?
Basically I am not confident that I could know if I made a mistake in my process whether the solution is now dangerous.
Can you please give some criteria for knowing by looking or temp if it is explosive?
Having this criteria would give confidence try this and be safe.
Thank you for a good step-by-step video.
Cheers.
Thanks for the kind words.
Whats great about you si your enthusiasm. It makes me happy to see u happy. And you love what you do so that give you the will to produce good video
I'm struggling to see the improvements compared to some of your older videos.. you've shortened mixing times at warm stage and used stronger peroxide and more water later on. Good video and I appreciate your contribution to my post schooled education :)
I think i'll put your words onto paper so I can pin it to my wall, and avoid the thermo melt down, we can take back the world one jam jar at a time
oh yeah - another interesting way is to ball mill it with solid carbon dioxide - but i think it is a bit beyond home chemists to do it. I may be wrong - it's just my opinion.
a short piece of glass tube taped onto a screwdriver! it's is caustic and hot so glass is best but i didn't have one long enough and i didn't want to get my hand in there.
The tour group think NaNO3 contributes very little which is why they left it out. Myself I think it helps pre oxidise the graphite before the main show - so to speak.
Thank u a lot for sharing this interesting experience..
So, I recuperated graphite from PC batterie and I'will use it for the synthesis of graphene oxide, what's your opinion? ..
One shot instant drain cleaner from B&Q. It's in their plumbing section or bullit drain cleaner which I get from my local hardware store. Spirit of salts I get at a builders merchants.
No I haven't but I like the idea and can see the sense of it. Cheers for the heads up
Well ,in Germany it is compliated to get chemicals in a really pure form ,if you are young and because Germany has strange laws ,which affect me and other people buying chemicals .I´ll tried it with the fertilizer and the pouder from the meat-market ,which contains 50% NaNO3 ,so i must concentrate it .Thanks for the interesting video ;)
Looks like the way forward to me.
nice advice mate cheers
The stirrer is easy to make. The water bath would be nice
Well, you make your choice and run with it.
It would be cool - maybe one day . But right now I think you are right the chemical method is far more practical.
Have you tried first microwaving the graphite flakes in a microwave oven? There are some papers that indicate that by prepping the graphite first in this way, you can improve the efficiency of the oxidation process
Very nice video, much more than the older ones.Thanks for your effort. Do you think the Sodium nitrate can be substituted by potassium nitrate ? (maybe some incompatibilities around the potatium permanganate phase)
I assume that after cleaning, GO must be sonicated before coating some stuff, is that right ?
nicely done Robert! Another new project for me :) By the way, the graphite,...I have a graphite which has a resistance of 2-3 ohms! is this good for GO?
For those of you who want to find local dealers for some of your chemicals.
NaNO3 is sold at pottery supply centers in 5lb bags for $10
~98% H2SO4 is sold at hardware stores as "Professional" drain cleaner
Hi Robert,
Great job! thank you helping others to get this done...
Got a question. I have Graphene (NOT Graphite) source and I used it instead. I went through the mentioned Steps though, I didn't had anything interesting at the end....
Is it applicable to Graphene or .....?what is wrong with Graphene?
hiya mate
You will get something but that is quite a low graphite content. if i were you i would go to an art shop and buy a higher graphite content pencil say a 6B or better yet 8B (they do go up to 9B and you can get graphite blocks to draw with)
Your room temp is fine for the medium stage. Good luck - let me know how you get on
It'll be fine.
I'd definitely like to see it
I'll give it a go mate cheers
Go for it. I just have too much to do. Doing write ups and instructables is just too much
That's what I use. But I also rigged up a vacuum filtration unit to speed it up
Absolutely right! Thought it was a good article because of how simple the method is(yes, takes a lot of time) but very high yield and little work:)
dedlunch good points mate
and I am also trying with Tour's method. Which method do you prefer? I guess Tour's method is more efficient with higher yield of GO production but less safe?? Thanks!
Great video sir, was already planning to try "how to make grphene 2" then i saw this improved version. I'm definitely going to be doing this now... i've got some questions tho: 1)would graphite from ordinary 4B pencils do or would the impurities in the led cause havoc 2)room temperature round here is 28-31C would this do for the medium stage or must it be exactly 35C? #Thanks
Cheers mate, 400g potassium permanganate, 2 litres of acid
Transcript? Add to? Where are they?
Yes and yes. Lol. Re-input the dried material and lengthen both the cold and warm stage
burning magnesium ribbon in a dry ice! It's is quick and good method?! i will tried and reported the progress
Sounds like it. You can buy concentrated sulphuric acid as drain cleaner. It 98% and says so on the label
Dear Robert,
Thank you for this Video, Its really helpful...I am going to try this method...
I was wondering if you are going to heat at 98C (high temp zone)as you have mentioned on the notes or procedures on the board.
+Nireeksha Karode I have done quite a few videos on GO methods mate
Cheers mate
Hello Dr. Murray-Smith, thank you for making these amazing videos.
Currently I am having trouble in the step where I add the water, after heating the mixture for 5 minutes at 100 ºC and right before adding the hydrogen peroxide. Instead of obtaining the orange color (as seen in the 19:00 mark), I obtain a Green/Brown color.
Does the reaction needs to take place at a specific temperature? Or do you have any idea of what I may be doing wrong?
Thank you very much
Miguel Azori It's very hard to give practical advise i am afraid as i am not there to oversee what you are actually doing. But by the time you add the peroxide it is all done - the fact you get brown green indicates an error in the earlier phases. What they are I don't know as i didn't see you do the whole experiment - sorry i can't be of more help
What acid strength did you use?
I agree, microwave-assisted irridation does help in the exfoliaton process. But does NaNO3 produce better results that KNO3? I have wondered about that for some weeks now and wonder if the Na and K are "spectator" ions and if so, will it work just as well or will too much potassium (with the KMnO4) be a problem?
dear Robert, sorry for bothering, could you please give me a favor and answer my question like usual😊I followed a method similar to "massive production of graphene oxide...." and I got a beautiful brown mixture after adding water(slowely) but then when I added H2O2 to quench the reaction I ended up with a greenesh yellow colour😭 I even used less amount than that one mentioned in paper... could you please tell me why?should I add H2O2 as long as the colour turns to brownesh yellow and not more?
Thank you very much Robert, but I have a doubt. When you say 2l acid, a type of acid that you mean? Sulfuric, phosphoric, hydrochloric ... can you tell me what proportion is the most economical for oxide 100gr? Because it is much the acid is spent for the little rust that occurs. Greetings and thanks for all the work you're doing
Yes. Jimmy, you are clearly an intelligent guy, but don't do this by yourself. Have a friend on hand. Just in case.
Did you reference any papers to create this method?
Good luck with it mate and post a vid so I can see how you get on
hello! thank you! excellent information for us!, two questions: 1. what is the best technique for structural and compound characterization graphene oxide?, 2: how long ultrasound is necessary to move from graphite oxide graphene oxide? congratulations! :)
+Edgardo Gabriel Casas Rodriguez Raman and I don't know.
PMSL ... i don,t know either
For question 1: For a surface analysis and structural analysis, SEM or AFM is the best to analyze your image. For compound analysis, such as graphene to graphene oxide, FTIR will give the data for functional groups of graphene and which wave number will have occurred. For question 2 : Generally, time is varied by experiment to experiment.
Indeed. I think graphene oxide is a poor name. Originally it was called graphitic acid which is much better as it is actually a graphene basal plane decorated with carboxyl and hydroxyl groups as opposed to oxides per se
Hey Rob. I would like to understand the reason for sittiring the graphite and sulfuric acid for 30 min at the beginning. What is the purpose? Chemistry wise. Thanks!
to allow a bit of intercalation to happen and seperate the layers out a bit
Hello Robert, thank you for all your great videos!! One question: do you know any alternative for NaNO3, it's not legal to buy it in Germany.
Thank you very much for all the inspiration and the great books!
Jakob
+Jakob Elias that is only one method mate - you don't 100% need it - you can just use potassium permanganate
If time doesn't bug me, would it be smarter (and safer) to use the 3 day method? or do you recommend that I use this method anyway?
You could try it as a school project and get your teacher to help or ask your parents to help order
Thanx Sir for your prompt reply, If I am using the graphite with 45 microns or bigger in size as the starting material, then what pore size PTFE i should use to filter the GO.
i wouldn't use less than 45 microns if i were you lol - try a few and see mate
Being of automobile aftermarket customization, I wonder if this technology can be used to charge capacitors or batteries and extend the range of an electric vehicle. Very curious and ready to develop such an aftermarket addition.
countrywideprocess i am working on exactly that
what do you do with the remaining solutions after the washing ie
the hydroclotic acid , the deionized water etc ? Can you use them again for the same washing steps respectively?
Thanks I will try that. Could anything negative happen if I do the cold and warm stage too long? Would it over oxidize? If so, is that bad?
I got the motor from a rechargeable drill. It cost £5 which is 6 euros I think.
Hey Robert. First of all, you are amazing =P, now onto my question, I want to make a graphene super cap for a school project by burning GO with a light scribe disc burner. I realise that super caps may not be all that they are made out to be and what not but i really just needed something fun and challenging to do for my science project. Anyway, i was looking for where to buy graphite oxide and i had a lot of difficulty doing so so i did a bit of research. First I found that graphene oxide was a lot more easily obtainable than graphite oxide so I did some research on that. I then found that graphite oxide is being sold in places as graphene oxide. I then found that when you disperse graphite oxide into water it exfoliates into graphene oxide anyway. Please tell me if what I have read is true or if it is false and if I would be able to just disperse what they call "graphene oxide" into water and burn that to make my super caps (graphene oxide is apparently also water soluble). I also wanted to make graphene oxide but my teachers said no because it may be explosive. I then decided to buy some, I am only in year 9 so i have a tight budget and this was the cheapest graphene oxide I found www.ebay.com/itm/Single-Layer-Graphene-Oxide-Solid-150-Milligram-Per-Vial-/111297404661?pt=LH_DefaultDomain_0&hash=item19e9d79ef5
would that be suitable for what i want. Thanks in advanced.
cheers mate- and yes it would be fine
Robert Murray-Smith Wow... O_o that was an amazingly fast reply... If i have anymore questions should i ask you here or would you prefer for me to ask them somewhere else (I shouldn't have that many questions from here on)?
no sorry mate, the acid has to be pretty strong 94% is about as low as you can go
just stop adding the permanganate and chuck a lot of crushed ice into the icebath. It'll calm down. When it is calm again leave it for an hour in ice then dispose of it as it will be ruined beyond redemption - though an easy way would be to run lol
Follow Robert Murray-Smith's videos on creating GO then use his spin coating method to produce a sheet of GO. Next use a xenon flash (dollar store camera flash) after for an extremely high quality cheap graphene sheet of customizable size. Remember the thinner it is, the better it is for super capacitors.
Dear Dr. RMS
you are adding powder KMnO4, what if you first dissolve and add slowly in similar manner?
you rock doc robert!!!!!
lol - cheers mate
Hello Robert I tried this process in my lab and have some doubts regarding it.
1. Completed the process and kept for drying in a glass tray, it is getting dried by the day time and when I take a look after a night the dried slugger again turns into wet can find waters in it. What is the reason behind this?
2. What are the better methods to test the Graphene oxide, which test can be effective to tell how much graphite is oxidised and what is the percentage of Graphene oxide in it.
Thanks buddy
vinodh kumar it's just a modified hummer's mate and subject to the same restrictions any hummer's based methodology is. Test methods are fairly standard - raman and XRD being 2 basic ones - i feel you should know this
I did say in the video 55 degrees centigrade
Okey thanks, for the awnser mate
Do you want pH 1 or 7?
I would use this method from preference
It is a great pleasure to see your developmet. In a way, I would like to support it! Please, send the carbon and/or graphene coating sample to me for Raman analysis, I am very interested ;) I will also check the crystalline nature of your samples using advanced X-ray techniques.
Algirdas Lazauskas please don't repeat post mate - i reply to all posts where my input is required
You need to add a warning for the person following these instructions to wear eye protection and to have a water fountain nearby to wash off any splashes. Also some sodium bicarbonate solution ready to neutralize the acid. A rubber apron would also be a good idea. Since he'll be outdoors, curious onlookers should be chased away.
well - we have that now lol
Hi Robert. Been experimenting with this over the last few months and I don't know why I didn't see this before, but silly question:
When adding the 400mL of water & 50mL of 30% H2O2, you are essentially adding 15mL of "pure" H2O2 and an amount of water. Would this work the same way if you just used 500mL of the cheap 3% H202 (also 15mL of "pure" H2O2 with a little more water), or does it not work this way? -- Thanks!
I just finished my last batch over the weekend. Thanks for the clear and concise directions, I had really great success. 👍
It is a relatively safe, reaction if you obey your advice, I had almost no nasty fuming, it's really critical to keep the temperatures low as you said.
The only step that particularly concerns me is adding the water to the mixture, (water into acid, eek!) would it be better to do it the other way around, add true mixture to the water?
Also what's the best way to store it? I'm thinking maybe in a dilute H2O2 solution to prevent it reducing back to graphite over time?
I want to make it as well, can someone please let me know ALL the materials i would need to do this procedure SAFELY and with the right equipment? I don't have ready access to equipment so will have to buy what i don't already have. I would greatly appreciate the help!
Hello Mr. Smith I absolutely love your videos and your work!!! My name is Marlo D and I have an awesome idea to make the ultimate SWAG generator. My only problem is that I am afraid to make the graphene myself in fear that I will hurt myself or the children in my house.
Can you please sell me a batch that you have made?? I think 15ml should be enough. I also need to clarify how to properly connect the negative and positive terminals. Thank you soooo much Mr. Smith please contact me back with info on how I could purchase. And it is water proof correct?
thank you man you are legend..
cheers mate
Do you think this is more cost effective than flash graphene?
The only difference would be supplying your own renewable energy.
A “flash graphene foundry” still requires a Lot Of Power, and the quality I’d still wonder about.
For anyone making this business, you would need to employ multiple methods. Just to see your output quality, which in my opinion is everything right now.
I still consider a lot of stuff out there with Graphene essentially snake oil:-/
Dear Sir, My 1st question is what kind of filter you used to get the final product as GO. Is it a normal filter paper, can you specify the pore size or it's detail? My 2nd question is, Does this GO you obtained can be used to get the LC phase?
getting LC phase and filter size depends on starting material - tto get LC phase you need graphite of 45 microns or larger. You need to use a PTFE or similar filter with correct pore size mate
Lol. I'm a chemist. I guess I learnt the basics at uni but that was 32 years ago so a lot more has been learnt by experience lol
what is the pH?
So I should use the dried result of that attempt and use it as the input graphite and the next attempt? Should I extend the medium temperature stage at all? Because on the first try it didn't thicken up at all and didn't change to a brown/purple. It just got a little darker. That could be because my graphite is a fine powder.
Hello,
What are you using to stir with during the KmnO₄ addition? I assume the solution is very acidic at this stage and wonder if an impermeable material is needed.
Seems like a good idea but I can't make any good comments on it because I just don't know enough about it
To your knowledge, what is the importance of the temperature in the "hot" step? While performing this experiment the heating portion of my stirrer got shorted out. So while I wait til tomorrow for it to dry out, I was only able to keep it around 70ºC with a bath. Do you know how I should expect my end product to be affected?
Hi Robert thanks for video. So after I mixed KMnO4 with solution in an ice bath, I increased temp to 35 Celcius degree and it started to explode a little bit. I put back right away in the ice bath and explosion stopped. But, solutions turned to be pasty grey mud-like solution. Can I still use this solution for further procedure? Thanks Rob
no mate it's ruined - you have to start again
Do you recommend a specific particle size (mesh) for the initial 5 grams of graphite, or is it of little importance? Your final graphene oxide looks quiet homogeneous. How much of the initial graphite was oxidized accoprding to your numbers. Thank you.
it depends what you want - if you want large flakes you will need to have a large grade - you might want this for liquid crystal type that can be electrospun or you might want small for inkjet printing - so it is up to you - typically i use 45 microns but i have usedd 150 micron and 5 micron. depending on reaction time you can get 95% but be careful of overoxidation
Robert Murray-Smith
Thanks for your answer
Can I make it without the Sodium Nitrate? Maybe use more potassium permanganate?
I am using the same method but instead of getting black powder i am getting white color substance which is not a graphene oxide please help me with this .
Hello .. I stirred graphite, NaNO3 annd H2SO4 in ice bath..and also during the addition of water, i did use ice bath for precaution.Do u think the outcome still ok?
I never say something can be done unless i have done it and as i haven't i just don't know the answers - but that is all part of the excitement and fun of doing this - if you choose to do it you are breaking new ground - i would encourage you to try