Introduction: Making Graphene

Picture of Making Graphene

Everything is inspired by the work of this 1 person.

https://www.youtube.com/user/RobertMurraySmith

Grammarly was used to check for mistakes.

https://app.grammarly.com/

Graphene was first discovered in the late 1800's. It had a different name and they did not know what it was.

This instructable is to show at least 6 different ways to make it . I prefer 2 electrochemical methods but it does not always work depending on the starting material. It is also probably the slowest method but it can create a very clean product. Does not work if you are using powdered graphite or artificial (man-made) graphite. Artificial graphite can never be used with any process.

The steps are out of order since I did not take pictures at the start.

WARNING.. The chemicals used are very strong acids , bases, and oxidizers.

You must wear gloves and eye protection. If improperly handled they can blow up and blind you.

I don't and have burnt my fingers several times trying to pull a dead fly out of the solution.

It should also be done in a ventilated area (outside) were the are no animals. I use an old rabbit cage to keep the squirrels, chipmunks, racoons, many many cats and 2 dogs out of the experiment. If you are using just sulfuric acid this is safe and cheap. If you are using 30% H2O2 it can be dangerous. Also, the H2O2 costs a lot more than the graphite so it might not be worth using that method unless you want the produced result.

The H2O2 solutions is a near Piranha solution. This can scar you for life. I am in my seventies so maybe that is a few months for me. If you are 20 then this might be a very long time. You could get a job on the "Walking Dead" without makeup. There is 120 AC and water in the cage but it will be moved outside the cage later.

The 1st section is on cleaning the graphene followed by making it.

Step 1: Wash Out Any Initial Chemicals.

Picture of  Wash Out Any Initial Chemicals.

We must start by removing any extra chemicals that were used.

Unless mentioned otherwise the water used is always Reverse Osmosis water.

Step 1 is to wash the initial product.

I fill up the 1000ml beaker with water and mix gently.

I let it sit for a day to let it settle. It initially takes at least 12 hours.

Drain the water.

Repeat this process at least 3 to 4 times. This takes 3 days and about 1 hour of labour.

Shown is the before and after.

When done we have removed most of the sulfuric acid.

The dangerous hydrogen peroxide will evaporate on its own.

I mix the waste water with baking soda until it stopped bubbling. I tried using just bases but with no buffer, it was just too difficult. When I get to PH 6.5 to 7.5 I would dump the sodium sulphate solution on my gravel road.

I wasted a lot of product but I was in a hurry and I did not care.

Step 2: Wash With Chemicals and RO Water

Picture of Wash With Chemicals and RO Water

Now I wash out any chemicals in the Graphene.

Add water to the 1000 ml mark.

I wash with about a soup spoon of "pure" sodium hydroxide.

Draino is not good enough. Must be pure and dangerous.

This gets rid of any remaining sulfuric acid and any present oils.

The initial product was pulled out of a pile of dirt so it may contain anything including bugs.

After this product is again washed with 1 pass of water.

Add a little HCl to the wash water to change into an acid. Add more baking soda until the bubbles stop and the PH is near 7.0. Throw this water with sodium chloride ( just normal salt ) out.

Add water to the 1000 ml mark and add 20 ml of muriatic acid. Probably too much acid.

Wash this out 3 to 4 times with RO water again.

Again neutralise the waste water with baking soda to change the wash solution to salt and throw out.

We now have a pile of graphene sludge.

These steps took about 12 hours of work.

Our next step is to grade by some sort of size.

Step 3: Grade Product by Size. Not Really Needed.

Picture of  Grade Product by Size.  Not Really Needed.

I am starting from a pile of slushy material. I used kitchen sieves to grade by size. Now stainless steel is not supposed to react to very weak HCl but one of the 3 sieves rusted overnight.

I should have started the last chemical wash over but It mostly affected the largest pieces. I got lazy and pretended it did not happen.

Now I have 5 batches of different sizes of graphene.

The first batch was made from a piece of Plumbago graphite from Russia.

The second batch was an experiment that did not go the way I wanted. Unexpected but a good result.

The 3rd batch and current piece turned out to be a piece of flake graphite.

I did not know it was flake graphite so I divided it into 3 batches by size. The output was run through strainers. I also messed that up too but I ignored my mistake. Some large pieces ended up in the medium grade pile.

Step 4: Break Time

Picture of  Break Time

This is yellow bug pretending to be a tomato flower.

An insect will show up for a meal but becomes a meal.

Graphene is supposed to be 100 times stronger than steel by weight.

But it feels like mush and has no strength at all.

Pretend it is a 100 lb fishing line where you could only push.

The 100 lb fishing line feels like does not have the strength to even catch a minnow.

What we now have is a product that we can only push on.

Graphene does not dissolve into anything. It is a colloid and can mix with only some things.

In time, it will always sink or float.

Graphene is a super-sized (jumbo) molecule. You might be comparing 100 787 jumbo jets to an ant.

Step 5: The Equipment Needed for the Electrochemical Method

Picture of The Equipment Needed for the Electrochemical Method

This is what I used. This is a guide as to what you might use.

1) A 12-volt source. I initially used a battery but it drained the battery and you had to disconnect for 12 hours to recharge. I ended up with a 12-volt regulator.from Ebay. Right now I can only find it on Banggood.

2 ) A power output device that used 12-volts as in input and whatever you want as an output I started with a B3603 but ended up with a B3606 for more power. It would display the current and voltage and is short circuit protected.

3) Silicon wire. Can be hard to find. Also on Ebay or from Adafruit in NYC. This is essential... Do not skimp on this. Use 22awg gage or better.

4) A bunch of beakers. Or a bunch of pickle jars. Must be glass. Plastic will not work.

5) Some artificial graphite for the cathode. ( negative side)

6 ) Sulfuric acid. Dangerous 0.5 Molar solution. You must know what a 0.5 molar solution is or read for a while. A 0.5 molar solution is actually quite weak but to make it you need a much stronger starting source. Battery acid will do but you must still make a 0.5 molar solution from it.

7) Optional some 30% H2O2. Dangerous.

8) Some muriatic acid Dangerous.

9) Some sodium hydroxide. Dangerous

9) Some PH paper.

10) A lot 2-3 gallons of Reverse Osmosis water.

11 ) Baking soda. You will use a lot if you make more that 1 batch.

12) a cage to put all this in.

13) An outside area where children do not go. This may be left to run unattended if there are no children.

14) Gloves and glasses to protect you eyes in case anything explodes.

15) a pale of water or a hose to wash yourself if something goes wrong.

16) A power source.

17) some oil to prevent corrosion. I use coconut oil.

18) Some alligator clips.

19) some 2.5 mm plugs Male and female.

20) Some fluid measuring device.

21) A power cord.

22) Finally some real graphite.

Step 6: A Disaster.

Picture of A Disaster.

Started everything up with a 30% H2O2 solution. I have used this before but and I wanted to show 2 methods of electrochemistry. After 4 hours removed some product and restarted.

An alligator clip came free and dropped into the solution Put on gloves and removed it right away. It was under serious attack by the piranha solution. Started things up again.

The solution started to bubble and then boil. Stopped everything and backed away. Once the smoking stopped I went inside for a beer and quit for the night.

I assume the alligator had some magnesium as a rust inhibitor coating. The solution oxidated it to magnesium oxide. Magnesium oxide will make H2O2 boil away until none is left. See YouTube for examples. It is not violent like what some other chemicals can cause. H2O2 can actually explode. That is why 35% is the maximum concentration you can buy. Going to 10% to reduce costs and increase safety. Also, all the metal items will have to be covered with Teflon so they can no longer react.

Torpedoes used to use 100% H2O2 as a fuel with silver as a catalyst. Sometimes they exploded sinking the submarine.

If you do not use H2O2 you do not need these extra steps but you should anyway. If you have chemistry experience you have already seen things like this. Be very careful. The rabbit cage will be rebuilt for improved safety later. It is way too small and should be built as a chamber that might explode. There are many many things wrong with the cage.

Step 7: Restart Successful

Picture of Restart Successful

A couple of days later...

I changed the way I held the cathode. ( the negative side )

Wrapped it up with a dollar store plant holder rubber thing. Too heavy but it is the first attempt. The clips can no longer fall into the fluid.

Also a new solution. I put in 100ml of 30% H2O2 and add 300 ml of the premade 0.5 molar sulfuric acid. You should probably use just the sulfuric acid but then the solution will then end up black. The voltage is 2.0 with a starting current of about 1 amp. We are using 2 watts of power and the solution never heats up.

After 18 hours removed some graphene with a spoon and washed it with rain water. Got a lot of very large flakes because of the low voltage. If you use 10 volts you will get maybe 10 times as much graphene but they will be very small flakes. The large flakes can be made smaller anytime with a sonic vibrator by just shaking it a for a long time. The wind will also break them up (if dry) but then they blow away. The very fine pieces do disappear with a wind gust. The result was washed with rain water and left to dry. If you make a lot you might proceed with the chemical wash. I have over a pound so I did the chemical wash. I intend to make RO and other products so it should be clean. About 50% of the world's graphite is within 200 miles of me. Am about to scavenge for so Mica soon. There are maybe 50 abandoned Mica mines and quarries with 200 miles of me. ( the Ottawa Canada area ) Also old graphite quarries and mines. It is free but it takes a day to collect 5 to 6 pounds of rocks that might contain 20% graphite. It is worth about $5.00 but you cannot buy flake. I also have about a pound of amorphous graphite from England ( no flakes ) .that I will process next.

This is one site. Rock hounds only.

http://www.mindat.org/article.php/1354/10.+Graphit...

t will take a few days to finish this piece. I throw the little pieces out or you could use them the way it is done commercially. They grind graphite rocks into a powder. Keep what floats. Wash it with with a base solution and then an acid solution. If you start from flake ( common where I live) it sells for $10,000 to $20,000 per ton plus shipping It is NOT graphene but multi-layer graphene I might be way wrong about the price. Each provider gives different numbers. This same process can be scaled up ( but different ) to provide hundreds of pounds of graphene per day. If scaled up H2O2 cannot be used since any 1 piece of graphite might contain a raw chemical that could make it all go wrong. Graphene can be used to instantly remove oil from water in an oil spill. Graphene hates water

I am going to end this instructable for now. I hope I can edit later to add in more chapters and products you can make from this.

Step 8: The Original Method

Picture of The Original Method

Well, I know I can add stuff.

This is the scotch tape method. First, you have to verify that the tape can be dissolved by acetone or your fluid of choice. Then you keep you peeling off a layer. After 8 separations the original piece is now 256 times thinner. This is not actually true since the pieces do not divide in half. Let's pretend.

Dump the tape into an acetone bath. Once the tape is dissolved I use a fine coffee mesh to separate out the pieces.

If you peel off 16 separations you might have something that is 64K times thinner.

I found this piece in a pile of sand. Weighs about 0.1 gram and is worthless.

I will mix the pieces with some clear polyurethane It might make a corner splash..Makes a corner stand out Maybe it could be a boat trim to help it stand out in the dark when searching for it using a flashlight. There are better ways.


Step 9: TBD

Well, I was going to show a lot of different methods but after 2 weeks I am publishing what I have done.
This is my 1st instructable so I do not know if can add more chapters later. I want to make some GO from the larger flakes and some nanotubes. Nanotubes are supposed to transfer heat at the speed of sound???

I also want to write some cell phone code for a handheld spectrometer. Using 100W single spectrum led's and I hope I can identify rocks from the spectrum database. Kind of like Raman. Means you can rock hound and take samples with exact GPS info, pictures and a spectrum of the samples while exploring the bush. Any suggestions or corrections would be helpful. Thanks

Comments

acolomitchi (author)2016-07-18

https://arxiv.org/pdf/1310.7371.pdf

Electrochemical method with alkaline electrolyte seems to work better.

Works at 10V, uses KOH at pH13, the graphene sheets are less wrinkled, needs alternating the polarity though (every 5 seconds) to obtain 2-4 layers sheets of graphene (i.e. you'll need to use some electronics to do it for hours)

cgendron (author)acolomitchi2016-07-18

I read the article and it has lots of new info. But he makes very small flakes but that can depend on the starting graphite I am using some pieces with 1/2 inch flakes.

With the 2-volt acid method, I get millions of exfoliated 1/4 inch flakes. Still looking for an application for them.

acolomitchi (author)cgendron2016-07-18

> With the 2-volt acid method, I get millions of exfoliated 1/4 inch flakes.

By the look on the photos you have, your flakes are still graphite rather than graphene - i.e still in the micron rather than nanometre thin. Maybe it's a fine graphite, but still graphite only.

The $20000/tonne the scientists are after is graphene - sheets up to 10 layers of carbon, a single layer preferred.

> Still looking for an application for them.

Continue watching RobertMurraySmith until you get to supercapacitors. Or conductive ink.

cgendron (author)acolomitchi2016-07-18

There is another article that says I can use a spark plug and the coil to make nanotubes directly but under water. It is a little different in that you must have CNC control of the spark plug or the sample. Used spark plugs, wires, and coils are cheap.

The same ESC is used to drive it. If a raspberry pi is attached one can directly control the timing via a keyboard. A raspberry pi supports an SPI interface.

acolomitchi (author)cgendron2016-07-18

Would you mind to link that article? Or provide a DOI number at least?

cgendron (author)acolomitchi2016-07-18

I have an ESC from the USA that will do the voltage swap. Up to about 1 Mz to any lower frequency. I will try it out and upload the result. About $60.
The ESC was meant for a motor but the code is new and I can upload it. It also provides bi-direction SPI info. ie debug messages etc.
The is also a Lithium chemical that is supposed to provide a direct graphene oxide.

Robert101010 (author)2016-07-12

So do you have any conclusions of your two weeks worth of effort? I personally have never seen a rabbit hutch lab! I fear for the rabbits who might inhabit the hutch next go around! Ha-ha! I also have followed Robert Murray Smith in his shotgun approach to grapheme discoveries, he keeps me amused, as does your approach to this exciting new yet old discovery of grapheme today!

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