Synthesis of Graphene Oxide (GO) by Hummer’s Method

CHECK LIST: Graphite, Sulphuric Acid, Potassium Permanganate (KMnO4), Hydrogen Peroxide (H2O2), Water, Beaker, Measuring Cylinder, Magnetic Stirrer

STEP1: Take Sulphuric Acid (25ml) in Ice Bath and add Graphite (1g) with proper stirring Raw HTML 500 rpm 20°C STEP2: Add Potassium Permanganate(3g) very slowly by keeping the temperature less than 20ºC and stir for more 3 hours (NOTE: You may remove the ice bath after 20 minutes and again setup for STEP3) Raw HTML 500 rpm 20°C KMnO4 STEP3: Add distilled water (50ml) dropwise by keeping the temperature less than 50ºC Raw HTML 500 rpm 32°C after some time 500 rpm 32°C STEP4: Add distilled water (100ml) instantly for complete oxidation. Raw HTML 500 rpm 32°C STEP5: Add Hydrogen Peroxide (5ml) for the completion of the reaction. Raw HTML 500 rpm 32°C

RESULTS: Graphene Oxide (GO) colour would be dark brown; UV-VIs spectroscopy absorbance peak would be obtained around 250nm; Raman spectroscopy D band and G band would be obtained at around 1300cm-1 and 1550cm-1 respectively

FACTORS AFFECTING THE SYNTHESIS:

  • Concentration of Graphite: The amount of Graphite used for the synthesis of Graphene Oxide (GO) is very important factor; because oxidation penetration on Graphite depends on the concentration of the Graphite in the Sulphuric Acid. Higher the concentration of Graphite, lesser the penetration of oxidation. Concentration of Sulphuric Acid: Concentration of Sulphuric Acid is most important in Hummers method. Higher the concentration of Sulphuric Acid, higher the chances of complete exfoliation of Graphite into Graphene Oxide; But also very high chances of unwanted accident.
  • Effect of KMnO4: In this method, KMnO4 acts as Oxidizer, Sulphuric Acid functionalize the Graphite surface to add functional groups in the presence of reagent like KMnO4. KMnO4 should be added slowly because it increases the temperature of the reaction and may lead to incomplete oxidation at the end, if poured instantly and not stirred properly.
  • Rate of Adding Water: Rate at which water is added for the oxidation matters a lot. InstaNANO suggest you to add water drop wise very slowly to avoid unwanted accidents and good quality Graphene Oxide.
  • Role of Hydrogen Peroxide: Main role of Hydrogen Peroxide is to remove the excessive KMnO4 or in other words to stop the reaction.

NOTE: Hummers Method is dangerous and should be done very carefully by wearing the lab coat, hand gloves, eye safety glasses and other lab safety measures; and under the guidance of Lab Incharge

18 comments:

  1. Mehdihasan Shekh17 January 2017 at 22:08

    Its an interesting and most helpful website for researchers and for students.

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  2. Your synthesis is very good. But you didn't clarify DLS of GO. I also prepared GO and size around 280d.nm. But I want to prepare GO around 20d.nm.

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  3. I also prepared GO (my first time) and I saw H.method with NaNO3+ Graphite+ H2SO4 in Step 1, so can you tell me the roles of NaNO3 in this mixture?

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  4. Thanks really practical. Will certainly share website with my buddies.

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  5. is it possible to use sucrose to produce graphite as the starting material before it being oxidized

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  6. For the first time, we also developed a prototype method of post-treating the waste water collected from the systems of synthesizing and purifying graphene oxide.

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  7. NaNO3 and H2SO4 to form HNO3.

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  8. what is conc per ml and per liter how can i prerpare 5mg/ml

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  9. science believe in references, kindly put the reference behind. its most important for researcher. as chemist if i prepare it with above method, what should be my reference. ? Regards

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  10. Dear Visitor

    Sorry for the inconvenience you have encountered at InstaNANO.com
    We can not provide the reference of all the synthesized materials posted on InstaNANO as most of the work is done in the personal laboratories by researchers and not published anywhere. First researchers synthesize the material in lab and then characterize it, only then we make post on the InstaNANO so we can not provide you the reference of our work.

    There are some post also which have written only after reading many research papers by our team. But we try to avoid such post which are only written after reading papers (not synthesized in lab by us) because there are many cases when data is manipulated in papers. So for such post we can provide you the reference if you send us the post url query on asking the reference on info@instanano.com email address.
    Hope you can understand the situation.

    Thanks & Regards,
    InstaNANO Team

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  11. What should be the percentage of H2O2?
    What would be the mg/ml rate of this solution?
    Thank you.

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  12. Pls, is it necessary to carry out the synthesis under reflux while heating at higher temperatures??

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  13. plz can u send ur steps to prepare graphene oxide

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  14. Hello! I am an undergraduate student that plans to work on graphene materials. Can I just ask how much graphene oxide are you able to produce using this method? Thanks!

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  15. Abdalla, that would be 500mg for 100ml and/or 5gr for 1Lt.

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  16. Good evening can help me after the fifth stage when the graphite oxide is formed how laundry product process Yes use extruder Centre and walrashh, are freed from sediment chapter leaky either deposit is alkravin oxide and sell it what do I do thanks

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  17. Soilahoudine Madi Maoulida10 April 2019 at 18:15

    J'ai des difficultés sur l'établissement des équations chimiques pour chaque étape.
    Est-ce quelqu'un peut m'aider en écrivant en détails toutes ces équations?

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  18. Soilahoudine Madi Maoulida12 April 2019 at 02:29

    Il n'y a personne pouvant m'aider à écrire toutes les équations chimiques mises en jeu en détails?

    ReplyDelete