Process for preparation of nanoporous graphene and graphene quantum dots

Patent metadata

Field	Value
Publication number	US-9637388-B2
Application number	US-201414893658-A
Country	US
Kind code	B2
Filing date	May 26, 2014
Priority date	May 24, 2013
Publication date	May 2, 2017
Grant date	May 2, 2017

Abstract

The present invention discloses a simple and easily scalable process for preparation of two potentially value added carbonaceous materials from graphene. The invention further discloses simultaneous preparation of graphene quantum dots (GQDs,) and porous graphene (pGr) from graphene. The invention further relates to nitrogen doped porous graphene having excellent activity towards electrochemical oxygen reduction reaction (ORR).

First claim

We claim:

1. An in-situ process for simultaneous synthesis of nanoporous graphene (pGr) and photo luminescent graphene quantum dots (GQDs) with no wastage of carbonaceous material comprising;
i. dispersing graphene with 25-35% hydrogen peroxide (H 2 O 2 ) at room temperature ranging between 25-35° C. followed by increasing the temperature to 60 to 70° C. for 24 to 72 hrs to obtain a mixture of porous graphene (pGr) and graphene quantum dots (GQDs);
ii. filtering the resulting mixture to obtain the solution of GQDs as filtrate and residue of pGr;
iii. drying the residue as pGr as obtained in step (ii) at a temperature in the range of 40° C.-60° C. for 1-3 h;
iv. dialysing the filtrate as obtained in step (ii) in dialysis bag for 1-3 days at 27 to 30° C. to obtain solution of GQD;
v. nitrogen doping of the porous graphene as obtained in step (iii) to obtain nitrogen doped porous graphene.

2. The process according to claim 1 , wherein the average size of graphene quantum dots as obtained in step (iv) in a single layer is 3-5 nm.

3. The process according to claim 1 , wherein the BET surface area of pGr as obtained in step (iii) is in the range of 204 to 240 m 2 g −1 .

4. The process according to claim 1 , wherein the nitrogen doping of the porous graphene surface (pGr)was carried out by, mixing of ethanolic solution of porous graphene (pGr) as obtained in step (iii) with 1, 10 Phenanthroline mixture at 27 to 30° C. for a period ranging between 20-24 hrs followed by evaporating the solvent by thermal evaporation at temperature ranging between 50 to 60° C. for a period ranging between 10-12 hrs to obtain the composite material subsequently heating at temperature ranging between 800 to 900° C. for a period ranging between 1-3 hrs in a furnace saturated with inert atmosphere and cooling, washing to obtain nitrogen doped porous graphene.

5. The process according to claim 4 , further comprising at least one of:
performing gas separation using the nitrogen doped porous graphene nano pores (pGr);
performing water desalination using the nitrogen doped porous graphene nano pores (pGr);
performing single atom doping (Pt, Co and In) using the nitrogen doped porous graphene nano pores (pGr); or
manufacturing Li-ion batteries Li-air battery, solar cells, super capacitors, gas sensors or polymer electrolyte membrane fuel cells (PEMFCs) using the nitrogen doped porous graphene nano pores (pGr).

Assignees

• Council Scient Ind Res

Inventors

• Kurungot Sreekumar
• Palaniselvam Thangavelu

Classifications

• C01B32/194

  After-treatment · CPC title

• Y10S977/774

  Exhibiting three-dimensional carrier confinement, e.g. quantum dots · CPC title

• B01J20/20 Primary

  comprising free carbon; comprising carbon obtained by carbonising processes · CPC title

• C01B32/184

  Preparation · CPC title

• C01B2204/065

  characterized by their width or by their aspect ratio · CPC title