Patent
US 9,923,200METHOD FOR MAKING SULFUR-GRAPHENE COMPOSITE MATERIAL
LI WANG
US
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Patent
Atlas literature
Patent
US 9,923,200Claims 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 making a sulfur-graphene composite material, the method comprises:,,, providing an elemental sulfur solution, wherein the elemental sulfur solution comprises a CS? solvent and an elemental sulfur dissolved in the CS 2 solvent, and a concentration of the elemental sulfur solution is about 60/L; adding a plurality of graphene sheets to an ethanol to form a graphene solution and then ultrasonically vibrating the graphene solution to form a graphene dispersion, wherein a power of the ultrasonically vibrating is about 150 watt, and a mass percentage of the plurality of graphene sheets in the graphene dispersion is about 0.5 wt%, adding the elemental sulfur solution to the 2raphene dispersion, wherein a plurality of elemental sulfur particles are precipitated from a liquid solvent and combine to surfaces of the plurality of graphene sheets to form a sulfur-graphene composite, and the plurality of elemental sulfur particles are needle-shaped; and SVG 15341004.09-13-2017.J₇M₀NTEKPXXIFW1.CLM.1.svg 0.12 0.58 Black and white separating the sulfur-graphene composite material from the liquid solvent, wherein the sulfur-graphene composite material is first separated by leaching and then air-dried, and there is no heating and stirring during the separating process so that the plurality of graphene sheets to self-assemble as a layered sandwich structure comprising an elemental sulfur layer being sandwiched by two of the plurality of graphene sheets. Currently amended
: The method of claim 1, further comprises adding a surfactant in the graphene [[oxide]] dispersion before the elemental sulfur solution is added. Currently amended
: The method of claim 1, wherein the elemental sulfur solution is dripped in the graphene [[oxide]] dispersion. Currently amended
: The method of claim 1, wherein the plurality of elemental sulfur particles in the sulfur-graphene composite material are attracted to the surface of each graphene sheet. Original
: The method of claim 1, wherein a diameter of the plurality of elemental sulfur particles is in a range from about 20 nanometers to about 200 nanometers. Original
: The method of claim 1, wherein the elemental sulfur is obtained by the following substeps: providing a thiosulfate solution; adding a surfactant to the thiosulfate solution to form a first mixed solution; adding a hydrochloric acid to the first mixed solution and reacting with thiosulfate of the first mixed solution to obtain a second mixed solution comprising the elemental sulfur; and separating the elemental sulfur from the second mixed solution. Previously presented
: The method of claim 1, wherein the plurality of elemental sulfur particles is precipitated from the liquid solvent comprising the [[first]] CS 2 solvent and the ethanol solvent. Currently amended
2-6. Canceled
Canceled
10-11.. Canceled
Canceled
. Canceled
Embodiments described in the patent, grouped by the materials and process steps they use.
5 materials1 process step
Sublimed sulfur dissolved in CS₂ solvent at ~40 g/L concentration to form elemental sulfur solution. Graphene sheets added to ethanol and ultrasonically vibrated (150 W) to form graphene dispersion at 1 wt%. Elemental sulfur solution added to graphene dispersion; elemental sulfur particles precipitated and combined to graphene sheet surfaces. Mixture leached to remove liquid and air-dried to obtain sulfur-graphene composite material. SEM showed uniform small elemental sulfur particle diameter. Material used as cathode active material for Li-S battery showing good capacity retention and charge-discharge efficiency.
5 materials1 process step
Same process as Example 1 except concentration of elemental sulfur solution is about 60 g/L and mass percentage of graphene sheets is 0.5 wt% (as specified in claim 1). Needle-shaped elemental sulfur particles are formed.
Layer stacks claimed or described, ordered top of device to substrate.
Li-S battery cathode
Materials described outside the worked examples.
surfactant
sorbitan oleate (sorbitan (Z)-mono-9-octadecenoate, Span 80)
Additional fabrication and treatment steps described in the patent.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
elemental sulfur particle diameter range | 20–200 nm | S |
Thickness | 50–200 nm |
Patent
Atlas literature
Patent
US 9,923,200Claims 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 making a sulfur-graphene composite material, the method comprises:,,, providing an elemental sulfur solution, wherein the elemental sulfur solution comprises a CS? solvent and an elemental sulfur dissolved in the CS 2 solvent, and a concentration of the elemental sulfur solution is about 60/L; adding a plurality of graphene sheets to an ethanol to form a graphene solution and then ultrasonically vibrating the graphene solution to form a graphene dispersion, wherein a power of the ultrasonically vibrating is about 150 watt, and a mass percentage of the plurality of graphene sheets in the graphene dispersion is about 0.5 wt%, adding the elemental sulfur solution to the 2raphene dispersion, wherein a plurality of elemental sulfur particles are precipitated from a liquid solvent and combine to surfaces of the plurality of graphene sheets to form a sulfur-graphene composite, and the plurality of elemental sulfur particles are needle-shaped; and SVG 15341004.09-13-2017.J₇M₀NTEKPXXIFW1.CLM.1.svg 0.12 0.58 Black and white separating the sulfur-graphene composite material from the liquid solvent, wherein the sulfur-graphene composite material is first separated by leaching and then air-dried, and there is no heating and stirring during the separating process so that the plurality of graphene sheets to self-assemble as a layered sandwich structure comprising an elemental sulfur layer being sandwiched by two of the plurality of graphene sheets. Currently amended
: The method of claim 1, further comprises adding a surfactant in the graphene [[oxide]] dispersion before the elemental sulfur solution is added. Currently amended
: The method of claim 1, wherein the elemental sulfur solution is dripped in the graphene [[oxide]] dispersion. Currently amended
: The method of claim 1, wherein the plurality of elemental sulfur particles in the sulfur-graphene composite material are attracted to the surface of each graphene sheet. Original
: The method of claim 1, wherein a diameter of the plurality of elemental sulfur particles is in a range from about 20 nanometers to about 200 nanometers. Original
: The method of claim 1, wherein the elemental sulfur is obtained by the following substeps: providing a thiosulfate solution; adding a surfactant to the thiosulfate solution to form a first mixed solution; adding a hydrochloric acid to the first mixed solution and reacting with thiosulfate of the first mixed solution to obtain a second mixed solution comprising the elemental sulfur; and separating the elemental sulfur from the second mixed solution. Previously presented
: The method of claim 1, wherein the plurality of elemental sulfur particles is precipitated from the liquid solvent comprising the [[first]] CS 2 solvent and the ethanol solvent. Currently amended
2-6. Canceled
Canceled
10-11.. Canceled
Canceled
. Canceled
Embodiments described in the patent, grouped by the materials and process steps they use.
5 materials1 process step
Sublimed sulfur dissolved in CS₂ solvent at ~40 g/L concentration to form elemental sulfur solution. Graphene sheets added to ethanol and ultrasonically vibrated (150 W) to form graphene dispersion at 1 wt%. Elemental sulfur solution added to graphene dispersion; elemental sulfur particles precipitated and combined to graphene sheet surfaces. Mixture leached to remove liquid and air-dried to obtain sulfur-graphene composite material. SEM showed uniform small elemental sulfur particle diameter. Material used as cathode active material for Li-S battery showing good capacity retention and charge-discharge efficiency.
5 materials1 process step
Same process as Example 1 except concentration of elemental sulfur solution is about 60 g/L and mass percentage of graphene sheets is 0.5 wt% (as specified in claim 1). Needle-shaped elemental sulfur particles are formed.
Layer stacks claimed or described, ordered top of device to substrate.
Li-S battery cathode
Materials described outside the worked examples.
surfactant
sorbitan oleate (sorbitan (Z)-mono-9-octadecenoate, Span 80)
Additional fabrication and treatment steps described in the patent.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
elemental sulfur particle diameter range | 20–200 nm | S |
Thickness | 50–200 nm |
Patent
Atlas literature
Patent
US 9,923,200Claims 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 making a sulfur-graphene composite material, the method comprises:,,, providing an elemental sulfur solution, wherein the elemental sulfur solution comprises a CS? solvent and an elemental sulfur dissolved in the CS 2 solvent, and a concentration of the elemental sulfur solution is about 60/L; adding a plurality of graphene sheets to an ethanol to form a graphene solution and then ultrasonically vibrating the graphene solution to form a graphene dispersion, wherein a power of the ultrasonically vibrating is about 150 watt, and a mass percentage of the plurality of graphene sheets in the graphene dispersion is about 0.5 wt%, adding the elemental sulfur solution to the 2raphene dispersion, wherein a plurality of elemental sulfur particles are precipitated from a liquid solvent and combine to surfaces of the plurality of graphene sheets to form a sulfur-graphene composite, and the plurality of elemental sulfur particles are needle-shaped; and SVG 15341004.09-13-2017.J₇M₀NTEKPXXIFW1.CLM.1.svg 0.12 0.58 Black and white separating the sulfur-graphene composite material from the liquid solvent, wherein the sulfur-graphene composite material is first separated by leaching and then air-dried, and there is no heating and stirring during the separating process so that the plurality of graphene sheets to self-assemble as a layered sandwich structure comprising an elemental sulfur layer being sandwiched by two of the plurality of graphene sheets. Currently amended
: The method of claim 1, further comprises adding a surfactant in the graphene [[oxide]] dispersion before the elemental sulfur solution is added. Currently amended
: The method of claim 1, wherein the elemental sulfur solution is dripped in the graphene [[oxide]] dispersion. Currently amended
: The method of claim 1, wherein the plurality of elemental sulfur particles in the sulfur-graphene composite material are attracted to the surface of each graphene sheet. Original
: The method of claim 1, wherein a diameter of the plurality of elemental sulfur particles is in a range from about 20 nanometers to about 200 nanometers. Original
: The method of claim 1, wherein the elemental sulfur is obtained by the following substeps: providing a thiosulfate solution; adding a surfactant to the thiosulfate solution to form a first mixed solution; adding a hydrochloric acid to the first mixed solution and reacting with thiosulfate of the first mixed solution to obtain a second mixed solution comprising the elemental sulfur; and separating the elemental sulfur from the second mixed solution. Previously presented
: The method of claim 1, wherein the plurality of elemental sulfur particles is precipitated from the liquid solvent comprising the [[first]] CS 2 solvent and the ethanol solvent. Currently amended
2-6. Canceled
Canceled
10-11.. Canceled
Canceled
. Canceled
Embodiments described in the patent, grouped by the materials and process steps they use.
5 materials1 process step
Sublimed sulfur dissolved in CS₂ solvent at ~40 g/L concentration to form elemental sulfur solution. Graphene sheets added to ethanol and ultrasonically vibrated (150 W) to form graphene dispersion at 1 wt%. Elemental sulfur solution added to graphene dispersion; elemental sulfur particles precipitated and combined to graphene sheet surfaces. Mixture leached to remove liquid and air-dried to obtain sulfur-graphene composite material. SEM showed uniform small elemental sulfur particle diameter. Material used as cathode active material for Li-S battery showing good capacity retention and charge-discharge efficiency.
5 materials1 process step
Same process as Example 1 except concentration of elemental sulfur solution is about 60 g/L and mass percentage of graphene sheets is 0.5 wt% (as specified in claim 1). Needle-shaped elemental sulfur particles are formed.
Layer stacks claimed or described, ordered top of device to substrate.
Li-S battery cathode
Materials described outside the worked examples.
surfactant
sorbitan oleate (sorbitan (Z)-mono-9-octadecenoate, Span 80)
Additional fabrication and treatment steps described in the patent.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
elemental sulfur particle diameter range | 20–200 nm | S |
Thickness | 50–200 nm |
Patent
Atlas literature
Patent
US 9,923,200Claims 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 making a sulfur-graphene composite material, the method comprises:,,, providing an elemental sulfur solution, wherein the elemental sulfur solution comprises a CS? solvent and an elemental sulfur dissolved in the CS 2 solvent, and a concentration of the elemental sulfur solution is about 60/L; adding a plurality of graphene sheets to an ethanol to form a graphene solution and then ultrasonically vibrating the graphene solution to form a graphene dispersion, wherein a power of the ultrasonically vibrating is about 150 watt, and a mass percentage of the plurality of graphene sheets in the graphene dispersion is about 0.5 wt%, adding the elemental sulfur solution to the 2raphene dispersion, wherein a plurality of elemental sulfur particles are precipitated from a liquid solvent and combine to surfaces of the plurality of graphene sheets to form a sulfur-graphene composite, and the plurality of elemental sulfur particles are needle-shaped; and SVG 15341004.09-13-2017.J₇M₀NTEKPXXIFW1.CLM.1.svg 0.12 0.58 Black and white separating the sulfur-graphene composite material from the liquid solvent, wherein the sulfur-graphene composite material is first separated by leaching and then air-dried, and there is no heating and stirring during the separating process so that the plurality of graphene sheets to self-assemble as a layered sandwich structure comprising an elemental sulfur layer being sandwiched by two of the plurality of graphene sheets. Currently amended
: The method of claim 1, further comprises adding a surfactant in the graphene [[oxide]] dispersion before the elemental sulfur solution is added. Currently amended
: The method of claim 1, wherein the elemental sulfur solution is dripped in the graphene [[oxide]] dispersion. Currently amended
: The method of claim 1, wherein the plurality of elemental sulfur particles in the sulfur-graphene composite material are attracted to the surface of each graphene sheet. Original
: The method of claim 1, wherein a diameter of the plurality of elemental sulfur particles is in a range from about 20 nanometers to about 200 nanometers. Original
: The method of claim 1, wherein the elemental sulfur is obtained by the following substeps: providing a thiosulfate solution; adding a surfactant to the thiosulfate solution to form a first mixed solution; adding a hydrochloric acid to the first mixed solution and reacting with thiosulfate of the first mixed solution to obtain a second mixed solution comprising the elemental sulfur; and separating the elemental sulfur from the second mixed solution. Previously presented
: The method of claim 1, wherein the plurality of elemental sulfur particles is precipitated from the liquid solvent comprising the [[first]] CS 2 solvent and the ethanol solvent. Currently amended
2-6. Canceled
Canceled
10-11.. Canceled
Canceled
. Canceled
Embodiments described in the patent, grouped by the materials and process steps they use.
5 materials1 process step
Sublimed sulfur dissolved in CS₂ solvent at ~40 g/L concentration to form elemental sulfur solution. Graphene sheets added to ethanol and ultrasonically vibrated (150 W) to form graphene dispersion at 1 wt%. Elemental sulfur solution added to graphene dispersion; elemental sulfur particles precipitated and combined to graphene sheet surfaces. Mixture leached to remove liquid and air-dried to obtain sulfur-graphene composite material. SEM showed uniform small elemental sulfur particle diameter. Material used as cathode active material for Li-S battery showing good capacity retention and charge-discharge efficiency.
5 materials1 process step
Same process as Example 1 except concentration of elemental sulfur solution is about 60 g/L and mass percentage of graphene sheets is 0.5 wt% (as specified in claim 1). Needle-shaped elemental sulfur particles are formed.
Layer stacks claimed or described, ordered top of device to substrate.
Li-S battery cathode
Materials described outside the worked examples.
surfactant
sorbitan oleate (sorbitan (Z)-mono-9-octadecenoate, Span 80)
Additional fabrication and treatment steps described in the patent.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
elemental sulfur particle diameter range | 20–200 nm | S |
Thickness | 50–200 nm |
octylphenolpoly(ethyleneglycolether) x, x=9-10 (Triton X-100)
tetrahydrofuran
C₄H₈O
thiosulfate
hydrochloric acid
HCl
graphene oxide sheets
reducing agent
| — |
octylphenolpoly(ethyleneglycolether) x, x=9-10 (Triton X-100)
tetrahydrofuran
C₄H₈O
thiosulfate
hydrochloric acid
HCl
graphene oxide sheets
reducing agent
| — |
octylphenolpoly(ethyleneglycolether) x, x=9-10 (Triton X-100)
tetrahydrofuran
C₄H₈O
thiosulfate
hydrochloric acid
HCl
graphene oxide sheets
reducing agent
| — |
octylphenolpoly(ethyleneglycolether) x, x=9-10 (Triton X-100)
tetrahydrofuran
C₄H₈O
thiosulfate
hydrochloric acid
HCl
graphene oxide sheets
reducing agent
| — |