Kingswell Labs - 2019-02-16
This is the first video in a two part series. I had to split this into two videos because the vacuum pump in my freeze dryer needs some maintenance which should be done very soon. I apologize for my voice, I am getting over a cold and still stuffed up. Full synthesis process: - Graphene oxide dispersion of 3-4 mg/ml of de-ionized water mixed uniformly with ethylenediamine at 20 μl/5ml and then sealed in a glass vial and heated for 6 -8 hours at 95 ° C (~205 ° F) for synthesis of functionalized graphene hydrogel (FGH). - After cleaning in de-ionized water and freeze-drying, functionalized graphene aerogel (FGA) is produced. - Last, the aerogel is exposed to MWI in an inert atmosphere for 1 min to give rise to the final ULGA.
This morning I had an asterisk above my head and searched YT for ~ Carbon Areogel. I love You Tube!
Awesome! Look forward to part 2 and 3
Thank you!
Very cool project! Good job!
More than Awesome, you promised this one ages ago lol.
But i forgive you ha ha can't wait for part 2 😎
Haha thanks! Yeah I wish I could have posted this way sooner but too many problems made it more difficult than it should have been.
@@KingswellLabs yes have been wanting to synthesise this stuff and try it out in my Batteries as a storage medium, but could not work it out properly from papers that i read.
But i do have some nice GO made with 5 micron flake Graphite on the shelf, only prob i got now is filtering the damn stuff lol 😎
@@mouldykev If it's clean there's no need to filter it, just mix it in DI water and ultrasonicate it... That will break it into graphene oxide!
@@mouldykev I had the same problem, I went through several papers trying to find something that worked. I had many failures until I settled on the methods of two papers by chance.
Awesome!
WYA Kingswell! we love you!
You are too kind! I am sorry I have been running into equipment issues and time constraints, I think I will be uploading part 2 very soon but will be short. I was hoping to have more samples to make some batteries/capacitors with to show but that will take longer.
@@KingswellLabs good science takes time, don't stress, take care of yourself first. I just wanted you to know you're still wanted
This is super interesting
@KingswellLabs thanks for your video, i have synthesized GO but after several time of washing and centrifuge the final ph of dispersion doesn't increase above 3 what can i do? iam going to synthsis aerogel and my reducing agent is LAA but first i need to increase ph of GO dispersion to 6
Spin a variable electromagnetic cylinder in a beaker of graphite oxide solution, make sure the liquid is spinning within the container as a result of the em cylinder motion. Add in your reducing solvent dropwise and Increase the magnetic field strength slowly, watch your graphene aerogel crystal puk grow. You're welcome ftf
Thank you very much for this comment! It sounds very interesting and I will give it a go, but I have a few questions if you don't mind.
How fast do I need to spin the magnet?
I assume the cylinder is oriented lengthwise in the solution not perpendicular like a stirring bar? Does it matter which pole goes into the solution?
Last, what strength of electromagnet do you recommend? Feel free to PM me.
Hi Kingswell Labs, may I know the molarity of the EDA? What is the properties of the reducing agent so that it able to reduce the GO to aerogel form? I used pyrrole but it ends up like a dust particles
We are looking for a method to synthesize highly oxidized graphene oxide by electrochemical exfoliation.
How did you synthesize your graphene oxide?
I done it, but after removing the container from the oven, the separate particles were at the bottom of the container and were not compact and in a molded form. I cant find the problem that is very kind of you to help me to find the problem
I think you should look at your Graphene Oxide, that seems to be the problem with most people. Ultrasonicating the GO can easily destroy and reduce the GO. If you ultrasonicate, only use 50% duty cycle for one hour. The formation of the hydrogel should be the easiest part of this method, it is very forgiving if you have good GO. Good luck!
Hi, Kingswell Labs, I did enjoy your video it helped me a lot to understand the freeze-drying process, I have a question I don t want to synthesis an aerogel but a graphene oxide sponge. I use 10 mg/ml as a concentration and dispersed it in 200ml of water. after the ultrasonication process, I applied the hydrothermal method and freeze the solution before taking it to the freeze-dryer. but in the end, I did not get a sponge but the dust of particles. I try to understand what I have done wrong? Could you please assist? Thank you
How much of the 10mg/ml GO solution did you disperse into the 200ml water? You want to keep a concentration of GO to 2-5mg/ml. Also make sure you are using deionized water.
You will need to determine where in the process it failed. You should get a good solid hydrogel sponge after the hydrothermal process. If is not, than your reducing agent is bad or not the correct amount used. Also be careful with ultrasonication, you can damage the GO and will not produce a solid hydrogel. This is usually where people have problems. If you get a good solid hydrogel and it turns to particles when freezedrying, it could be the freezedrying process failed (allowed ice to change to water before gas).
I hope this helps!
Sir ant alternative to EDA? Can I use DEA
Could you just use graphene instead of GO? I'm just not a fan of the modified hummers method to make GO
Unfortunately there is no way I know to make graphene into a 3D structure, The O and H molecules are needed for bonding and ordering.
I am not a fan of the current process of making GO as well, which is why I am exploring different/environmentally friendly synthesis methods (without success).
@@KingswellLabs I'll look too, if I find anything, I'll share it
I make a lot of graphene by electrochemical exfoliation
@@KingswellLabs what about graphene surface functionalization? Cooh groups
Does the graphene oxide dispersion have to be 3-4 mg/ml? is it like the best concentration to use or can you use another concentration? Thank you!
Good question! I have used 2mg/ml-5mg/ml concentrations and the only difference is the size resulting sponge. With less concentration, the sponge is smaller, the higher concentration the sponge is bigger. But, I do not know if the structure of the sponge is affected by the concentration, which it could be. I have noticed better results using smaller concentrations but I have not quantified the aerogel yet, so I don't know for sure. I would recommend not going above 5mg/ml.
Kingswell Labs thank you so much for the reply 😊 i was going to do 5 mg/ml but i wasn't sure, so thanks!
Hi! do you mind to share the reference of the experimental procedure?
This method was taken from a combination of papers which are lost in a mess unfortunately.
Here is one of them:
https://onlinelibrary.wiley.com/doi/abs/10.1002/adma.201204530
How do you remove the gel from the water without breaking it?
You should be able to just dump it into a glass of water without breaking, the hydrogel is fairly easy to handle. If it is breakng up, something didn't go right. How bad is it breaking up?
@@KingswellLabs Very bad ... It forms nicely but when removing it to put it in the freezer it breaks
@@gianniskarnis7898 OK so there could be a few things wrong. Check that your GO solution is at PH of 5-6. Make sure the solution doesn't heat past 25C when sonicating. Last make sure EDA is thoroughly mixed.
I am going to post an update to clarify a few things and make some corrections that I am running across now.
@@KingswellLabs thank you very much for your advice... I will be sure to check everything you told me
can i use it for 3d printing?
There is a similar technique used to 3d print graphene, basically you would extrude the graphene oxide solution onto a very cold surface so it freezes immediately. After printing, you would freeze dry or use liquid nitrogen to remove the ice water. lastly it's heated to remove the oxygen to produce graphene. There is not much information on how well the structure holds up to stresses, but I could imagine a hybrid technique with something similar to what I show that would increse is cohesion.
From what I have tested, heating GO to remove oxygen leaves the material crumbly and not very useful.
@@KingswellLabsThanks for tour answer
So now I need a 3D printer, vacuum chamber piece of dry ice and a non-stick thermal conductive surface, so many ideas not enough money....
Have you done hydrothermal reduction
Yes, however using a hydrothermal autoclave and increasing the temperature does not produce a good solid form form my experience.
@reallyMika - 2020-04-14
This was satisfying on multiple levels. I could totally fall asleep to your voice lol.