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. Sohel Rana7 February 2017 at 10:16

    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. Nguyenchi Thang17 February 2017 at 18:52

    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. 4rx8 April 2017 at 02:33

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

    ReplyDelete
  5. peter ayo2 May 2017 at 06:24

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

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  6. helenoftroyusa.com16 June 2017 at 17:53

    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.

    ReplyDelete
  7. PadPab11 October 2017 at 07:33

    NaNO3 and H2SO4 to form HNO3.

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  8. abdalla7 November 2017 at 14:33

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

    ReplyDelete
  9. khan17 January 2018 at 13:48

    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

    ReplyDelete
  10. instanano19 January 2018 at 12:47

    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

    ReplyDelete
  11. Turgut Belen31 May 2018 at 01:09

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

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  12. Vincent15 June 2018 at 21:36

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

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  13. Mahmoud Ahmed6 July 2018 at 00:45

    plz can u send ur steps to prepare graphene oxide

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  14. Ian23 July 2018 at 18:21

    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. Turgut Belen4 October 2018 at 09:19

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

    ReplyDelete
  16. fouad26 February 2019 at 21:48

    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

    ReplyDelete
  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?

    ReplyDelete
  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