Patent
US 9,672,951METHOD FOR PREPARING GRAPHENE-BASED LiFePO₄/C COMPOSITE MATERIAL
Guorong Hu
US
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Patent
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US 9,672,951Patent drawings and their descriptions. Click a drawing to enlarge it.
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
A method for preparing a graphene-based LiFeP O 4/C composite material, comprising: dissolving a graphene oxide and an iron salt in a deionized water, a mass ratio of the graphene oxide over an iron element in the iron salt being 0.1-0.3:1 0.1:1-0.3:1; dispersing the graphene oxide by ultrasonic to obtain an iron salt solution having the graphene oxide dispersed therein; mixing the iron salt solution with a phosphate solution to obtain a reaction mixture, in which a molar ratio of Fe:P is 1:1~1.2 1:1~1:1.2; adjusting a pH value of the reaction mixture to 2 to 4; controlling a temperature of the reaction mixture to allow the reaction mixture to react at 60 0C to 80 0C to obtain an emulsion; filtering the emulsion to obtain a ferric phosphate/graphene oxide precursor; blending the ferric phosphate/graphene oxide precursor with a lithium salt at a Li:Fe molar ratio of 1-1.n5:1 1:1~1.05:1 to form a first mixture; adding a carbon source to the first mixture to form a second mixture; and sintering the second mixture under a reducing atmosphere condition at 600 0C to 700 0 C, to obtain the graphene-based LiFeP O 4/C composite material. -2-Application No.: 14/401,489 Attorney Docket No.: 51BE-241057-US
The method according to claim 1, wherein an iron ion concentration in the iron salt solution is 0.5 to 2 mol/L.
The method according to claim 1, wherein dispersing the graphene oxide by ultrasonic includes dispersing the graphene oxide by ultrasonic for 2 to 5 hours.
The method according to claim 1, wherein[[:]] controlling the temperature of the reaction mixture to allow the reaction mixture to react includes allowing the reaction mixture to react for 3 to 6 hours; and sintering includes sintering for 5 to 10 hours.
The method according to claim 1, wherein dissolving the iron salt solution in the deionized water includes dissolving at least one of a ferric sulphate, a ferric chloride, or a ferric nitrate in the deionized water.
The method according to claim 1, wherein mixing the iron salt solution with the phosphate solution includes mixing the iron salt solution with a solution of at least one of a phosphoric acid, an ammonium biphosphate, an ammonium monoacid phosphate, an ammonium phosphate, a sodium biphosphate, a sodium monoacid phosphate, or a sodium phosphate. -3- Application No.: 14/401,489 Attorney Docket No.: 51BE-241057-US
The method according to claim 1, wherein adjusting the [[PH]] pI value of the reaction mixture includes adjusting the [[PH]] pH. value of the reaction mixture using an alkaline solution having a concentration of 0.5 to 5 mol/L, the alkaline solution including a solution of a sodium hydroxide, a sodium carbonate, or an ammonia.
The method according to claim 1, wherein blending the ferric phosphate/graphene oxide precursor with the lithium salt includes blending the ferric phosphate/graphene oxide precursor with at least one of a lithium carbonate, a lithium hydroxide, or a lithium acetate.
The method according to claim 1, wherein adding the carbon source includes adding at least one of a glucose, a sucrose, a fructose, a lactose, a citric acid, a starch, a polyvinyl alcohol, a polypropylene, or a phenolic resin, having an amount equaling to 5 to 20% of a theoretical mass of a lithium iron phosphate.
The method according to claim 1, wherein sintering under the reducing atmosphere condition includes sintering in a mixed gas having a volume ratio of Ar:H 2 =90:10 to 95:5 or of N 2:H 2 =90:10 to 95:5.
The method according to claim 1, further comprising: washing and drying the emulsion after filtering the emulsion. -4- Application No.: 14/401,489 Attorney Docket No.: 5 1BE-241057-US
The method according to claim 1, further comprising: performing a ball milling on the second mixture.
The method according to claim 1, wherein dissolving the iron salt in the deionized water includes: dissolving a ferrous salt in the deionized water, the ferrous salt including at least one of a ferrous sulfate, a ferrous chloride, or a ferrous nitrate; and oxidizing the ferrous salt using an excess H 2 0 2. -5-
Embodiments described in the patent, grouped by the materials and process steps they use.
1 material
Preparation of graphene-based LiFePO₄/C composite material. Figure 3 shows the charge-discharge curve at different rates of the lithium ion battery using the composite material obtained in this example.
Materials described outside the worked examples.
graphene oxide
iron salt
Additional fabrication and treatment steps described in the patent.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
theoretical capacity of LiFePO4 | 170 mAh/g | LiFePO₄ |
Duration | 2–5 hours |
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CARBON NITRIDE MODIFIED WITH PERYLENETETRACARBOXYLIC DIANHYDRIDE / GRAPHENE OXIDE AEROGEL COMPOSITE MATERIAL, PREPARATION METHOD AND APPLICATION THEREOF
Machine Learning Accelerated Computational Surface-Specific Vibrational Spectroscopy Reveals Oxidation Level of Graphene in Contact with Water
Patent
Atlas literature
Patent
US 9,672,951Patent drawings and their descriptions. Click a drawing to enlarge it.
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
A method for preparing a graphene-based LiFeP O 4/C composite material, comprising: dissolving a graphene oxide and an iron salt in a deionized water, a mass ratio of the graphene oxide over an iron element in the iron salt being 0.1-0.3:1 0.1:1-0.3:1; dispersing the graphene oxide by ultrasonic to obtain an iron salt solution having the graphene oxide dispersed therein; mixing the iron salt solution with a phosphate solution to obtain a reaction mixture, in which a molar ratio of Fe:P is 1:1~1.2 1:1~1:1.2; adjusting a pH value of the reaction mixture to 2 to 4; controlling a temperature of the reaction mixture to allow the reaction mixture to react at 60 0C to 80 0C to obtain an emulsion; filtering the emulsion to obtain a ferric phosphate/graphene oxide precursor; blending the ferric phosphate/graphene oxide precursor with a lithium salt at a Li:Fe molar ratio of 1-1.n5:1 1:1~1.05:1 to form a first mixture; adding a carbon source to the first mixture to form a second mixture; and sintering the second mixture under a reducing atmosphere condition at 600 0C to 700 0 C, to obtain the graphene-based LiFeP O 4/C composite material. -2-Application No.: 14/401,489 Attorney Docket No.: 51BE-241057-US
The method according to claim 1, wherein an iron ion concentration in the iron salt solution is 0.5 to 2 mol/L.
The method according to claim 1, wherein dispersing the graphene oxide by ultrasonic includes dispersing the graphene oxide by ultrasonic for 2 to 5 hours.
The method according to claim 1, wherein[[:]] controlling the temperature of the reaction mixture to allow the reaction mixture to react includes allowing the reaction mixture to react for 3 to 6 hours; and sintering includes sintering for 5 to 10 hours.
The method according to claim 1, wherein dissolving the iron salt solution in the deionized water includes dissolving at least one of a ferric sulphate, a ferric chloride, or a ferric nitrate in the deionized water.
The method according to claim 1, wherein mixing the iron salt solution with the phosphate solution includes mixing the iron salt solution with a solution of at least one of a phosphoric acid, an ammonium biphosphate, an ammonium monoacid phosphate, an ammonium phosphate, a sodium biphosphate, a sodium monoacid phosphate, or a sodium phosphate. -3- Application No.: 14/401,489 Attorney Docket No.: 51BE-241057-US
The method according to claim 1, wherein adjusting the [[PH]] pI value of the reaction mixture includes adjusting the [[PH]] pH. value of the reaction mixture using an alkaline solution having a concentration of 0.5 to 5 mol/L, the alkaline solution including a solution of a sodium hydroxide, a sodium carbonate, or an ammonia.
The method according to claim 1, wherein blending the ferric phosphate/graphene oxide precursor with the lithium salt includes blending the ferric phosphate/graphene oxide precursor with at least one of a lithium carbonate, a lithium hydroxide, or a lithium acetate.
The method according to claim 1, wherein adding the carbon source includes adding at least one of a glucose, a sucrose, a fructose, a lactose, a citric acid, a starch, a polyvinyl alcohol, a polypropylene, or a phenolic resin, having an amount equaling to 5 to 20% of a theoretical mass of a lithium iron phosphate.
The method according to claim 1, wherein sintering under the reducing atmosphere condition includes sintering in a mixed gas having a volume ratio of Ar:H 2 =90:10 to 95:5 or of N 2:H 2 =90:10 to 95:5.
The method according to claim 1, further comprising: washing and drying the emulsion after filtering the emulsion. -4- Application No.: 14/401,489 Attorney Docket No.: 5 1BE-241057-US
The method according to claim 1, further comprising: performing a ball milling on the second mixture.
The method according to claim 1, wherein dissolving the iron salt in the deionized water includes: dissolving a ferrous salt in the deionized water, the ferrous salt including at least one of a ferrous sulfate, a ferrous chloride, or a ferrous nitrate; and oxidizing the ferrous salt using an excess H 2 0 2. -5-
Embodiments described in the patent, grouped by the materials and process steps they use.
1 material
Preparation of graphene-based LiFePO₄/C composite material. Figure 3 shows the charge-discharge curve at different rates of the lithium ion battery using the composite material obtained in this example.
Materials described outside the worked examples.
graphene oxide
iron salt
Additional fabrication and treatment steps described in the patent.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
theoretical capacity of LiFePO4 | 170 mAh/g | LiFePO₄ |
Duration | 2–5 hours |
Related documents with shared materials, methods, properties, or citations.
CARBON NITRIDE MODIFIED WITH PERYLENETETRACARBOXYLIC DIANHYDRIDE / GRAPHENE OXIDE AEROGEL COMPOSITE MATERIAL, PREPARATION METHOD AND APPLICATION THEREOF
Machine Learning Accelerated Computational Surface-Specific Vibrational Spectroscopy Reveals Oxidation Level of Graphene in Contact with Water
Patent
Atlas literature
Patent
US 9,672,951Patent drawings and their descriptions. Click a drawing to enlarge it.
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
A method for preparing a graphene-based LiFeP O 4/C composite material, comprising: dissolving a graphene oxide and an iron salt in a deionized water, a mass ratio of the graphene oxide over an iron element in the iron salt being 0.1-0.3:1 0.1:1-0.3:1; dispersing the graphene oxide by ultrasonic to obtain an iron salt solution having the graphene oxide dispersed therein; mixing the iron salt solution with a phosphate solution to obtain a reaction mixture, in which a molar ratio of Fe:P is 1:1~1.2 1:1~1:1.2; adjusting a pH value of the reaction mixture to 2 to 4; controlling a temperature of the reaction mixture to allow the reaction mixture to react at 60 0C to 80 0C to obtain an emulsion; filtering the emulsion to obtain a ferric phosphate/graphene oxide precursor; blending the ferric phosphate/graphene oxide precursor with a lithium salt at a Li:Fe molar ratio of 1-1.n5:1 1:1~1.05:1 to form a first mixture; adding a carbon source to the first mixture to form a second mixture; and sintering the second mixture under a reducing atmosphere condition at 600 0C to 700 0 C, to obtain the graphene-based LiFeP O 4/C composite material. -2-Application No.: 14/401,489 Attorney Docket No.: 51BE-241057-US
The method according to claim 1, wherein an iron ion concentration in the iron salt solution is 0.5 to 2 mol/L.
The method according to claim 1, wherein dispersing the graphene oxide by ultrasonic includes dispersing the graphene oxide by ultrasonic for 2 to 5 hours.
The method according to claim 1, wherein[[:]] controlling the temperature of the reaction mixture to allow the reaction mixture to react includes allowing the reaction mixture to react for 3 to 6 hours; and sintering includes sintering for 5 to 10 hours.
The method according to claim 1, wherein dissolving the iron salt solution in the deionized water includes dissolving at least one of a ferric sulphate, a ferric chloride, or a ferric nitrate in the deionized water.
The method according to claim 1, wherein mixing the iron salt solution with the phosphate solution includes mixing the iron salt solution with a solution of at least one of a phosphoric acid, an ammonium biphosphate, an ammonium monoacid phosphate, an ammonium phosphate, a sodium biphosphate, a sodium monoacid phosphate, or a sodium phosphate. -3- Application No.: 14/401,489 Attorney Docket No.: 51BE-241057-US
The method according to claim 1, wherein adjusting the [[PH]] pI value of the reaction mixture includes adjusting the [[PH]] pH. value of the reaction mixture using an alkaline solution having a concentration of 0.5 to 5 mol/L, the alkaline solution including a solution of a sodium hydroxide, a sodium carbonate, or an ammonia.
The method according to claim 1, wherein blending the ferric phosphate/graphene oxide precursor with the lithium salt includes blending the ferric phosphate/graphene oxide precursor with at least one of a lithium carbonate, a lithium hydroxide, or a lithium acetate.
The method according to claim 1, wherein adding the carbon source includes adding at least one of a glucose, a sucrose, a fructose, a lactose, a citric acid, a starch, a polyvinyl alcohol, a polypropylene, or a phenolic resin, having an amount equaling to 5 to 20% of a theoretical mass of a lithium iron phosphate.
The method according to claim 1, wherein sintering under the reducing atmosphere condition includes sintering in a mixed gas having a volume ratio of Ar:H 2 =90:10 to 95:5 or of N 2:H 2 =90:10 to 95:5.
The method according to claim 1, further comprising: washing and drying the emulsion after filtering the emulsion. -4- Application No.: 14/401,489 Attorney Docket No.: 5 1BE-241057-US
The method according to claim 1, further comprising: performing a ball milling on the second mixture.
The method according to claim 1, wherein dissolving the iron salt in the deionized water includes: dissolving a ferrous salt in the deionized water, the ferrous salt including at least one of a ferrous sulfate, a ferrous chloride, or a ferrous nitrate; and oxidizing the ferrous salt using an excess H 2 0 2. -5-
Embodiments described in the patent, grouped by the materials and process steps they use.
1 material
Preparation of graphene-based LiFePO₄/C composite material. Figure 3 shows the charge-discharge curve at different rates of the lithium ion battery using the composite material obtained in this example.
Materials described outside the worked examples.
graphene oxide
iron salt
Additional fabrication and treatment steps described in the patent.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
theoretical capacity of LiFePO4 | 170 mAh/g | LiFePO₄ |
Duration | 2–5 hours |
Related documents with shared materials, methods, properties, or citations.
CARBON NITRIDE MODIFIED WITH PERYLENETETRACARBOXYLIC DIANHYDRIDE / GRAPHENE OXIDE AEROGEL COMPOSITE MATERIAL, PREPARATION METHOD AND APPLICATION THEREOF
Machine Learning Accelerated Computational Surface-Specific Vibrational Spectroscopy Reveals Oxidation Level of Graphene in Contact with Water
Patent
Atlas literature
Patent
US 9,672,951Patent drawings and their descriptions. Click a drawing to enlarge it.
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
A method for preparing a graphene-based LiFeP O 4/C composite material, comprising: dissolving a graphene oxide and an iron salt in a deionized water, a mass ratio of the graphene oxide over an iron element in the iron salt being 0.1-0.3:1 0.1:1-0.3:1; dispersing the graphene oxide by ultrasonic to obtain an iron salt solution having the graphene oxide dispersed therein; mixing the iron salt solution with a phosphate solution to obtain a reaction mixture, in which a molar ratio of Fe:P is 1:1~1.2 1:1~1:1.2; adjusting a pH value of the reaction mixture to 2 to 4; controlling a temperature of the reaction mixture to allow the reaction mixture to react at 60 0C to 80 0C to obtain an emulsion; filtering the emulsion to obtain a ferric phosphate/graphene oxide precursor; blending the ferric phosphate/graphene oxide precursor with a lithium salt at a Li:Fe molar ratio of 1-1.n5:1 1:1~1.05:1 to form a first mixture; adding a carbon source to the first mixture to form a second mixture; and sintering the second mixture under a reducing atmosphere condition at 600 0C to 700 0 C, to obtain the graphene-based LiFeP O 4/C composite material. -2-Application No.: 14/401,489 Attorney Docket No.: 51BE-241057-US
The method according to claim 1, wherein an iron ion concentration in the iron salt solution is 0.5 to 2 mol/L.
The method according to claim 1, wherein dispersing the graphene oxide by ultrasonic includes dispersing the graphene oxide by ultrasonic for 2 to 5 hours.
The method according to claim 1, wherein[[:]] controlling the temperature of the reaction mixture to allow the reaction mixture to react includes allowing the reaction mixture to react for 3 to 6 hours; and sintering includes sintering for 5 to 10 hours.
The method according to claim 1, wherein dissolving the iron salt solution in the deionized water includes dissolving at least one of a ferric sulphate, a ferric chloride, or a ferric nitrate in the deionized water.
The method according to claim 1, wherein mixing the iron salt solution with the phosphate solution includes mixing the iron salt solution with a solution of at least one of a phosphoric acid, an ammonium biphosphate, an ammonium monoacid phosphate, an ammonium phosphate, a sodium biphosphate, a sodium monoacid phosphate, or a sodium phosphate. -3- Application No.: 14/401,489 Attorney Docket No.: 51BE-241057-US
The method according to claim 1, wherein adjusting the [[PH]] pI value of the reaction mixture includes adjusting the [[PH]] pH. value of the reaction mixture using an alkaline solution having a concentration of 0.5 to 5 mol/L, the alkaline solution including a solution of a sodium hydroxide, a sodium carbonate, or an ammonia.
The method according to claim 1, wherein blending the ferric phosphate/graphene oxide precursor with the lithium salt includes blending the ferric phosphate/graphene oxide precursor with at least one of a lithium carbonate, a lithium hydroxide, or a lithium acetate.
The method according to claim 1, wherein adding the carbon source includes adding at least one of a glucose, a sucrose, a fructose, a lactose, a citric acid, a starch, a polyvinyl alcohol, a polypropylene, or a phenolic resin, having an amount equaling to 5 to 20% of a theoretical mass of a lithium iron phosphate.
The method according to claim 1, wherein sintering under the reducing atmosphere condition includes sintering in a mixed gas having a volume ratio of Ar:H 2 =90:10 to 95:5 or of N 2:H 2 =90:10 to 95:5.
The method according to claim 1, further comprising: washing and drying the emulsion after filtering the emulsion. -4- Application No.: 14/401,489 Attorney Docket No.: 5 1BE-241057-US
The method according to claim 1, further comprising: performing a ball milling on the second mixture.
The method according to claim 1, wherein dissolving the iron salt in the deionized water includes: dissolving a ferrous salt in the deionized water, the ferrous salt including at least one of a ferrous sulfate, a ferrous chloride, or a ferrous nitrate; and oxidizing the ferrous salt using an excess H 2 0 2. -5-
Embodiments described in the patent, grouped by the materials and process steps they use.
1 material
Preparation of graphene-based LiFePO₄/C composite material. Figure 3 shows the charge-discharge curve at different rates of the lithium ion battery using the composite material obtained in this example.
Materials described outside the worked examples.
graphene oxide
iron salt
Additional fabrication and treatment steps described in the patent.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
theoretical capacity of LiFePO4 | 170 mAh/g | LiFePO₄ |
Duration | 2–5 hours |
Related documents with shared materials, methods, properties, or citations.
CARBON NITRIDE MODIFIED WITH PERYLENETETRACARBOXYLIC DIANHYDRIDE / GRAPHENE OXIDE AEROGEL COMPOSITE MATERIAL, PREPARATION METHOD AND APPLICATION THEREOF
Machine Learning Accelerated Computational Surface-Specific Vibrational Spectroscopy Reveals Oxidation Level of Graphene in Contact with Water
ferric phosphate/graphene oxide precursor
FePO₄
carbon source
ferric sulphate
Fe₂(SO₄)3
ferric chloride
FeCl₃
ferric nitrate
Fe(NO₃)3
phosphate source
alkaline solution
lithium salt
reducing atmosphere gas mixture
ferrous salt
hydrogen peroxide
H₂O₂
| — |
Duration | 3–6 hours | — |
Duration | 5–10 hours | — |
ferric phosphate/graphene oxide precursor
FePO₄
carbon source
ferric sulphate
Fe₂(SO₄)3
ferric chloride
FeCl₃
ferric nitrate
Fe(NO₃)3
phosphate source
alkaline solution
lithium salt
reducing atmosphere gas mixture
ferrous salt
hydrogen peroxide
H₂O₂
| — |
Duration | 3–6 hours | — |
Duration | 5–10 hours | — |
ferric phosphate/graphene oxide precursor
FePO₄
carbon source
ferric sulphate
Fe₂(SO₄)3
ferric chloride
FeCl₃
ferric nitrate
Fe(NO₃)3
phosphate source
alkaline solution
lithium salt
reducing atmosphere gas mixture
ferrous salt
hydrogen peroxide
H₂O₂
| — |
Duration | 3–6 hours | — |
Duration | 5–10 hours | — |
ferric phosphate/graphene oxide precursor
FePO₄
carbon source
ferric sulphate
Fe₂(SO₄)3
ferric chloride
FeCl₃
ferric nitrate
Fe(NO₃)3
phosphate source
alkaline solution
lithium salt
reducing atmosphere gas mixture
ferrous salt
hydrogen peroxide
H₂O₂
| — |
Duration | 3–6 hours | — |
Duration | 5–10 hours | — |