method, which involved two oxidation stages. In a typical procedure, the first oxidation was achieved in the following conditions: 1100 mg of graphite was placed in a 1000 mL boiling flask. Then, 20 g of K$_{2}$S$_{2}$O$_{8}$ , 20 g of P $_{2}$0 5 , and 400 mL of a concentrated aqueous solution of H$_{2}$SO$_{4 }$ (96%) were added in the flask. The mixture was heated under reflux for 6 hours and then let without disturbing for 20 hours at room temperature. Oxidized graphite was filtered and rinsed with abundant distilled water until neutral pH. A wet cake› like material was recovered at the end of this first oxidation. 

[0151] For the second oxidation process, the previously collected wet cake was placed in a boiling flask that contains 69 mL ofa concentrated aqueous solution ofH$_{2}$ SO$_{4 }$ (96%). The flask was kept in an ice bath as 9 g of KMnO$_{4 }$ was slowly added. Care was taken to avoid overheating. The resulting mixture was stirred at 35° C. for 2 hours (the sample color turning dark green), followed by the addition of 140 mL of water. After 15 min, the reaction was halted by adding 420 mL of water and 15 mL of an aqueous solution of30 wt% H$_{2}$O$_{2}$ . The color of the sample at this stage turned bright yellow. To remove the metallic ions, the mixture was filtered and rinsed with a 1: 10 HCl aqueous solution. The collected material was gently centrifuged at 2700 g and rinsed with deionized water. The final product was a wet cake that contained 1.4 wt % of GO, as estimated from dry extracts. Subsequently, liquid dispersions of GO platelets were obtained by lightly sonicating wet-cake materials, which were diluted in deionized water. 

[0152] Surfactant-stabilized RGO (RGO-BS) was obtained by diluting the wet-cake in an aqueous solution of surfactants instead of pure water. A commercially available mixture of cholate sodium (50 wt. %) and deoxycholate sodium (50 wt. %) salts provided by Sigma Aldrich was used. The surfactant weight fraction was 0.5 wt. %. This fraction was kept constant for all samples. Sonication was performed using a Branson Sonifier S-250A equipped with a 13 mm step disruptor horn and a 3 mm tapered micro-tip, operating at a 20 kHz frequency. For instance, 10 mL of aqueous solutions containing 0.1 wt.% of GO was sonicated for 10 min and subsequently centrifuged at 2700 g for 30 min to remove any non-dissolved large particles, aggregates, and impurities. Chemical reduction of as-obtained GO to yield RGO was conducted by following the method, which involved placing 10 mL of a 0.1 wt. % GO aqueous solution in a boiling flask of 50 mL. Then, 10 µL of a 35 wt. % aqueous solution ofN$_{2}$H$_{4 }$ (hydrazine) and 70 mL of a 28 wt. % of an aqueous solution ofNH$_{4}$OH (ammonia) were added to the mixture, which was stabilized by surfactants. The solution was heated to 90° C. and refluxed for 1 h. The pH value measured after the reaction was approximately 9. The color of the sample turned dark black during the reduction reaction. 

[0153] RGO was used as a conductive additive in either or both of the anode and cathode active material in certain lithium batteries presently invented. Pre-lithiated RGO (e.g. RGO+lithium particles or RGO pre-deposited with lithium coating) was also used as an anode active material that was mixed with a liquid electrolyte to form wet anode active material mixtures for selected lithium-ion cells. Selected cathode active materials (TiS$_{2 }$ nano particles and LiCoO$_{2 }$ particles, respectively) and non-lithiated RGO sheets were dispersed in a liquid electrolyte to prepare wet cathode active material mixture. The wet anode active mixture and 

cathode active mixtures were delivered to surfaces of graph› ite foams for forming an anode layer and a cathode layer, respectively. 

[0154] For comparison purposes, slurry coating and dry› ing procedures were conducted to produce conventional electrodes. Electrodes and a separator disposed between two dried electrodes were then assembled and encased in an Al-plastic laminated packaging envelop, followed by liquid electrolyte injection to form a lithium battery cell. 

## Example 2: Preparation of Pristine Graphene Sheets (0% Oxygen) 

[0155] Recognizing the possibility of the high defect population in GO sheets acting to reduce the conductivity of individual graphene plane, we decided to study if the use of pristine graphene sheets (non-oxidized and oxygen-free, non-halogenated and halogen-free, etc.) can lead to a con› ductive additive having a high electrical and thermal con› ductivity. Pre-lithiated pristine graphene and pre-sodiated pristine graphene were also used as an anode active material for a lithium-ion battery and a sodium-ion battery, respec› tively. Pristine graphene sheets were produced by using the direct ultrasonication or liquid-phase production process. 

[0156] In a typical procedure, five grams of graphite flakes, ground to approximately 20 µm or less in sizes, were dispersed in 1,000 mL of deionized water ( containing O .1 % by weight of a dispersing agent, Zonylfi FSO from DuPont) to obtain a suspension. An ultrasonic energy level of 85 W (Branson S450 Ultrasonicator) was used for exfoliation, separation, and size reduction of graphene sheets for a period of 15 minutes to 2 hours. The resulting graphene sheets are pristine graphene that have never been oxidized and are oxygen-free and relatively defect-free. Pristine gra› phene is essentially free from any non-carbon elements. 

[0157] Pristine graphene sheets, as a conductive additive, along with an anode active material ( or cathode active material in the cathode) were then incorporated in a battery using both the presently invented procedure and conven› tional procedure of slurry coating, drying and layer lami› nating. Both lithium-ion batteries and lithium metal batteries ( containing a wet cathode electrode) were investigated. Sodium-ion cells were also studied. 

## Example 3: Preparation of Prelithiated and Pre-Sodiated Graphene Fluoride Sheets as an Anode Active Material of a Lithium-Ion Battery or Sodium-Ion Battery 

[0158] Several processes have been used by us to produce GF, but only one process is herein described as an example. In a typical procedure, highly exfoliated graphite (HEG) was prepared from intercalated compound C$_{2}$F.xClF$_{3}$ . HEG was further fluorinated by vapors of chlorine trifluoride to yield fluorinated highly exfoliated graphite (FHEG). Pre-cooled Teflon reactor was filled with 20-30 mL of liquid pre-cooled ClF$_{3}$ , the reactor was closed and cooled to liquid nitrogen temperature. Then, no more than 1 g of HEG was put in a container with holes for ClF $_{3 }$ gas to access and situated inside the reactor. In 7-10 days a gray-beige product with approximate formula C$_{2}$F was formed. 

[0159] Subsequently, a small amount of FHEG (approxi› mately 0.5 mg) was mixed with 20-30 mL of an organic solvent (methanol and ethanol, separately) and subjected to an ultrasound treatment (280 W) for 30 min, leading to the 

