Patent
US 11,795,556 B2FE-DOPED MOS₂ NANO-MATERIAL, PREPARATION METHOD THEREFOR AND USE THEREOF
Jianping Lang, Jiangyan Xue, Chunyan Ni, Hong Yu
SOOCHOW UNIVERSITY, Suzhou (CN)·Oct. 24, 2023·US
Copyright © 2026 Matter42. All rights reserved.
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US 11,795,556 B2Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1 is a scanning electron microscopy (SEM) image of Fe-doped molybdenum disulfide nanocanopies;
FIG. 2 is a transmission electron microscopy (TEM) image of Fe-doped molybdenum disulfide nanocanopies;
FIG. 3 is an X-ray powder diffraction (PXRD) pattern of Fe-doped molybdenum disulfide nanocanopies;
FIG. 4 is an energy dispersive X-ray spectrum (EDX) diagram of Fe-doped molybdenum disulfide nanocanopies;
FIG. 5 is an element distribution diagram of Fe-doped molybdenum disulfide nanocanopies;
FIG. 6 is an X-ray photoelectron spectroscopy (XPS) diagram of Fe-doped molybdenum disulfide nanocanopies; 45
FIG. 7 shows a linear scanning voltammetry curve (a), a Tafel slope diagram (b), a double-layer capacitance diagram (c) of Fe-doped molybdenum disulfide …
FIG. 8 is a scanning electron microscopy (SEM) image of a Fe-doped molybdenum disulfide supported by nickel foam;
FIG. 9 is an X-ray powder diffraction (PXRD) pattern of a Fe-doped molybdenum disulfide supported by nickel 55 foam;
FIG. 10 shows an HER polarization curve (a), an HER corresponding Tafel slope diagram (b), an OER polarization curve (c), an OER corresponding Tafel slope …
FIG. 11 shows an apparatus (a) for overall water splitting by using the Fe-doped molybdenum disulfide supported by B₂ nickel foam in 1.0M KOH electrolyte, and a …
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 Fe-doped MoS₂ nano-mate-rial, comprising steps of: dissolving a ferric salt and ammonium tetrathiomolybdate in DMF and reacting at 180-200° C. for 6-24 hrs to obtain the Fe-doped MoS₂ nano-material.
The method according to claim 1, wherein the ferric salt is ferric chloride hexahydrate.
The method according to claim 1, wherein the molar ratio of the ferric salt to ammonium tetrathiomolybdate is 1-5:5.
The method according to claim 1, wherein the method further comprises the steps of washing, centrifuging and drying the reaction product.
A Fe-doped MoS₂ nano-material prepared by the prepa-ration method according to claim 1.
Embodiments described in the patent, grouped by the materials and process steps they use.
5 materials1 process step
Preparation of Fe-doped molybdenum disulfide nanocanopies (Fe0.05-MoS₂) by solvothermal reaction: 13 mg (0.05 mmol) ammonium tetrathiomolybdate and 13.5 mg (0.05 mmol) ferric chloride hexahydrate dissolved in 12 mL DMF, transferred to Teflon-lined stainless autoclave, sealed and reacted at 200°C for 12 hrs. After cooling, washed with deionized water and ethanol, centrifuged and dried to obtain black powdered product with diameter <200 nm and thickness ~30 nm.
4 materials1 process step
Preparation of a Fe-doped molybdenum disulfide nanocanopy electrocatalyst on glassy carbon electrode by mixing Fe0.05-MoS₂ powder and carbon black in isopropanol/Nafion solution, sonicating, and dropcasting onto polished glassy carbon electrode. Controls prepared with undoped MoS₂ and commercial Pt/C.
Layer stacks claimed or described, ordered top of device to substrate.
Fe-doped MoS₂ nanocanopies supported by nickel foam
electrocatalyst for HER/OER/overall water splitting
Materials described outside the worked examples.
ferric salt
nickel foam
Measurements and analyses referenced in the patent, with their drawing references.
Fe-doped molybdenum disulfide nanocanopies have uniform morphology, high quality and high yield, diameter less than 200 nm and thickness about 30 nm (FIG. 1 and FIG. 2).
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Xrd D Spacing | 9.4 Å | Fe0.05-MoS₂ (Fe-doped molybdenum disulfide nanocanopies) |
Patents and literature cited by this patent (applicant and examiner references).
Cited patents · 14
Related documents with shared materials, methods, properties, or citations.
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Patent
US 11,795,556 B2Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1 is a scanning electron microscopy (SEM) image of Fe-doped molybdenum disulfide nanocanopies;
FIG. 2 is a transmission electron microscopy (TEM) image of Fe-doped molybdenum disulfide nanocanopies;
FIG. 3 is an X-ray powder diffraction (PXRD) pattern of Fe-doped molybdenum disulfide nanocanopies;
FIG. 4 is an energy dispersive X-ray spectrum (EDX) diagram of Fe-doped molybdenum disulfide nanocanopies;
FIG. 5 is an element distribution diagram of Fe-doped molybdenum disulfide nanocanopies;
FIG. 6 is an X-ray photoelectron spectroscopy (XPS) diagram of Fe-doped molybdenum disulfide nanocanopies; 45
FIG. 7 shows a linear scanning voltammetry curve (a), a Tafel slope diagram (b), a double-layer capacitance diagram (c) of Fe-doped molybdenum disulfide …
FIG. 8 is a scanning electron microscopy (SEM) image of a Fe-doped molybdenum disulfide supported by nickel foam;
FIG. 9 is an X-ray powder diffraction (PXRD) pattern of a Fe-doped molybdenum disulfide supported by nickel 55 foam;
FIG. 10 shows an HER polarization curve (a), an HER corresponding Tafel slope diagram (b), an OER polarization curve (c), an OER corresponding Tafel slope …
FIG. 11 shows an apparatus (a) for overall water splitting by using the Fe-doped molybdenum disulfide supported by B₂ nickel foam in 1.0M KOH electrolyte, and a …
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 Fe-doped MoS₂ nano-mate-rial, comprising steps of: dissolving a ferric salt and ammonium tetrathiomolybdate in DMF and reacting at 180-200° C. for 6-24 hrs to obtain the Fe-doped MoS₂ nano-material.
The method according to claim 1, wherein the ferric salt is ferric chloride hexahydrate.
The method according to claim 1, wherein the molar ratio of the ferric salt to ammonium tetrathiomolybdate is 1-5:5.
The method according to claim 1, wherein the method further comprises the steps of washing, centrifuging and drying the reaction product.
A Fe-doped MoS₂ nano-material prepared by the prepa-ration method according to claim 1.
Embodiments described in the patent, grouped by the materials and process steps they use.
5 materials1 process step
Preparation of Fe-doped molybdenum disulfide nanocanopies (Fe0.05-MoS₂) by solvothermal reaction: 13 mg (0.05 mmol) ammonium tetrathiomolybdate and 13.5 mg (0.05 mmol) ferric chloride hexahydrate dissolved in 12 mL DMF, transferred to Teflon-lined stainless autoclave, sealed and reacted at 200°C for 12 hrs. After cooling, washed with deionized water and ethanol, centrifuged and dried to obtain black powdered product with diameter <200 nm and thickness ~30 nm.
4 materials1 process step
Preparation of a Fe-doped molybdenum disulfide nanocanopy electrocatalyst on glassy carbon electrode by mixing Fe0.05-MoS₂ powder and carbon black in isopropanol/Nafion solution, sonicating, and dropcasting onto polished glassy carbon electrode. Controls prepared with undoped MoS₂ and commercial Pt/C.
Layer stacks claimed or described, ordered top of device to substrate.
Fe-doped MoS₂ nanocanopies supported by nickel foam
electrocatalyst for HER/OER/overall water splitting
Materials described outside the worked examples.
ferric salt
nickel foam
Measurements and analyses referenced in the patent, with their drawing references.
Fe-doped molybdenum disulfide nanocanopies have uniform morphology, high quality and high yield, diameter less than 200 nm and thickness about 30 nm (FIG. 1 and FIG. 2).
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Xrd D Spacing | 9.4 Å | Fe0.05-MoS₂ (Fe-doped molybdenum disulfide nanocanopies) |
Patents and literature cited by this patent (applicant and examiner references).
Cited patents · 14
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 11,795,556 B2Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1 is a scanning electron microscopy (SEM) image of Fe-doped molybdenum disulfide nanocanopies;
FIG. 2 is a transmission electron microscopy (TEM) image of Fe-doped molybdenum disulfide nanocanopies;
FIG. 3 is an X-ray powder diffraction (PXRD) pattern of Fe-doped molybdenum disulfide nanocanopies;
FIG. 4 is an energy dispersive X-ray spectrum (EDX) diagram of Fe-doped molybdenum disulfide nanocanopies;
FIG. 5 is an element distribution diagram of Fe-doped molybdenum disulfide nanocanopies;
FIG. 6 is an X-ray photoelectron spectroscopy (XPS) diagram of Fe-doped molybdenum disulfide nanocanopies; 45
FIG. 7 shows a linear scanning voltammetry curve (a), a Tafel slope diagram (b), a double-layer capacitance diagram (c) of Fe-doped molybdenum disulfide …
FIG. 8 is a scanning electron microscopy (SEM) image of a Fe-doped molybdenum disulfide supported by nickel foam;
FIG. 9 is an X-ray powder diffraction (PXRD) pattern of a Fe-doped molybdenum disulfide supported by nickel 55 foam;
FIG. 10 shows an HER polarization curve (a), an HER corresponding Tafel slope diagram (b), an OER polarization curve (c), an OER corresponding Tafel slope …
FIG. 11 shows an apparatus (a) for overall water splitting by using the Fe-doped molybdenum disulfide supported by B₂ nickel foam in 1.0M KOH electrolyte, and a …
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 Fe-doped MoS₂ nano-mate-rial, comprising steps of: dissolving a ferric salt and ammonium tetrathiomolybdate in DMF and reacting at 180-200° C. for 6-24 hrs to obtain the Fe-doped MoS₂ nano-material.
The method according to claim 1, wherein the ferric salt is ferric chloride hexahydrate.
The method according to claim 1, wherein the molar ratio of the ferric salt to ammonium tetrathiomolybdate is 1-5:5.
The method according to claim 1, wherein the method further comprises the steps of washing, centrifuging and drying the reaction product.
A Fe-doped MoS₂ nano-material prepared by the prepa-ration method according to claim 1.
Embodiments described in the patent, grouped by the materials and process steps they use.
5 materials1 process step
Preparation of Fe-doped molybdenum disulfide nanocanopies (Fe0.05-MoS₂) by solvothermal reaction: 13 mg (0.05 mmol) ammonium tetrathiomolybdate and 13.5 mg (0.05 mmol) ferric chloride hexahydrate dissolved in 12 mL DMF, transferred to Teflon-lined stainless autoclave, sealed and reacted at 200°C for 12 hrs. After cooling, washed with deionized water and ethanol, centrifuged and dried to obtain black powdered product with diameter <200 nm and thickness ~30 nm.
4 materials1 process step
Preparation of a Fe-doped molybdenum disulfide nanocanopy electrocatalyst on glassy carbon electrode by mixing Fe0.05-MoS₂ powder and carbon black in isopropanol/Nafion solution, sonicating, and dropcasting onto polished glassy carbon electrode. Controls prepared with undoped MoS₂ and commercial Pt/C.
Layer stacks claimed or described, ordered top of device to substrate.
Fe-doped MoS₂ nanocanopies supported by nickel foam
electrocatalyst for HER/OER/overall water splitting
Materials described outside the worked examples.
ferric salt
nickel foam
Measurements and analyses referenced in the patent, with their drawing references.
Fe-doped molybdenum disulfide nanocanopies have uniform morphology, high quality and high yield, diameter less than 200 nm and thickness about 30 nm (FIG. 1 and FIG. 2).
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Xrd D Spacing | 9.4 Å | Fe0.05-MoS₂ (Fe-doped molybdenum disulfide nanocanopies) |
Patents and literature cited by this patent (applicant and examiner references).
Cited patents · 14
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 11,795,556 B2Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1 is a scanning electron microscopy (SEM) image of Fe-doped molybdenum disulfide nanocanopies;
FIG. 2 is a transmission electron microscopy (TEM) image of Fe-doped molybdenum disulfide nanocanopies;
FIG. 3 is an X-ray powder diffraction (PXRD) pattern of Fe-doped molybdenum disulfide nanocanopies;
FIG. 4 is an energy dispersive X-ray spectrum (EDX) diagram of Fe-doped molybdenum disulfide nanocanopies;
FIG. 5 is an element distribution diagram of Fe-doped molybdenum disulfide nanocanopies;
FIG. 6 is an X-ray photoelectron spectroscopy (XPS) diagram of Fe-doped molybdenum disulfide nanocanopies; 45
FIG. 7 shows a linear scanning voltammetry curve (a), a Tafel slope diagram (b), a double-layer capacitance diagram (c) of Fe-doped molybdenum disulfide …
FIG. 8 is a scanning electron microscopy (SEM) image of a Fe-doped molybdenum disulfide supported by nickel foam;
FIG. 9 is an X-ray powder diffraction (PXRD) pattern of a Fe-doped molybdenum disulfide supported by nickel 55 foam;
FIG. 10 shows an HER polarization curve (a), an HER corresponding Tafel slope diagram (b), an OER polarization curve (c), an OER corresponding Tafel slope …
FIG. 11 shows an apparatus (a) for overall water splitting by using the Fe-doped molybdenum disulfide supported by B₂ nickel foam in 1.0M KOH electrolyte, and a …
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 Fe-doped MoS₂ nano-mate-rial, comprising steps of: dissolving a ferric salt and ammonium tetrathiomolybdate in DMF and reacting at 180-200° C. for 6-24 hrs to obtain the Fe-doped MoS₂ nano-material.
The method according to claim 1, wherein the ferric salt is ferric chloride hexahydrate.
The method according to claim 1, wherein the molar ratio of the ferric salt to ammonium tetrathiomolybdate is 1-5:5.
The method according to claim 1, wherein the method further comprises the steps of washing, centrifuging and drying the reaction product.
A Fe-doped MoS₂ nano-material prepared by the prepa-ration method according to claim 1.
Embodiments described in the patent, grouped by the materials and process steps they use.
5 materials1 process step
Preparation of Fe-doped molybdenum disulfide nanocanopies (Fe0.05-MoS₂) by solvothermal reaction: 13 mg (0.05 mmol) ammonium tetrathiomolybdate and 13.5 mg (0.05 mmol) ferric chloride hexahydrate dissolved in 12 mL DMF, transferred to Teflon-lined stainless autoclave, sealed and reacted at 200°C for 12 hrs. After cooling, washed with deionized water and ethanol, centrifuged and dried to obtain black powdered product with diameter <200 nm and thickness ~30 nm.
4 materials1 process step
Preparation of a Fe-doped molybdenum disulfide nanocanopy electrocatalyst on glassy carbon electrode by mixing Fe0.05-MoS₂ powder and carbon black in isopropanol/Nafion solution, sonicating, and dropcasting onto polished glassy carbon electrode. Controls prepared with undoped MoS₂ and commercial Pt/C.
Layer stacks claimed or described, ordered top of device to substrate.
Fe-doped MoS₂ nanocanopies supported by nickel foam
electrocatalyst for HER/OER/overall water splitting
Materials described outside the worked examples.
ferric salt
nickel foam
Measurements and analyses referenced in the patent, with their drawing references.
Fe-doped molybdenum disulfide nanocanopies have uniform morphology, high quality and high yield, diameter less than 200 nm and thickness about 30 nm (FIG. 1 and FIG. 2).
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Xrd D Spacing | 9.4 Å | Fe0.05-MoS₂ (Fe-doped molybdenum disulfide nanocanopies) |
Patents and literature cited by this patent (applicant and examiner references).
Cited patents · 14
Related documents with shared materials, methods, properties, or citations.
X-ray powder diffraction pattern of Fe-doped MoS₂ nanocanopies conforms with reported interlayer spacing of 9.4 Å for MoS₂ (FIG. 3).
Fe-doped MoS₂ nanocanopies composed of Mo, Fe, S, and O, each element evenly distributed (FIG. 4 and FIG. 5).
Photoelectron spectroscopy shows valences of Mo, Fe, S, and O are +4, +2, −2, and −2, respectively (FIG. 6).
| 173 mV |
Fe0.05-MoS₂ (Fe-doped molybdenum disulfide nanocanopies) |
Electrocatalytic Tafel Slope HER Acid | 40.1 mV/dec | Fe0.05-MoS₂ (Fe-doped molybdenum disulfide nanocanopies) |
Electrocatalytic Overpotential HER Alkaline | 153 mV | Fe-doped MoS₂ nano-material (nanocanopies) |
Electrocatalytic Tafel Slope HER Alkaline | 85.6 mV/dec | Fe-doped MoS₂ nano-material (nanocanopies) |
Electrocatalytic Overpotential OER Alkaline | 230 mV | Fe-doped MoS₂ nano-material (nanocanopies) |
Electrocatalytic Tafel Slope OER Alkaline | 78.7 mV/dec | Fe-doped MoS₂ nano-material (nanocanopies) |
Electrocatalytic Overall Water Splitting Voltage | 1.52 V | Fe-doped MoS₂ nano-material (nanocanopies) |
Voltage | 0–0.8 V | — |
Voltage | 0.8–2 V | — |
Thickness | ≤ 200 nm | — |
Temperature | 180–200 °C | — |
Temperature | 40–60 °C | — |
Duration | ≤ 3 minutes | — |
Cited non-patent literature · 3
X-ray powder diffraction pattern of Fe-doped MoS₂ nanocanopies conforms with reported interlayer spacing of 9.4 Å for MoS₂ (FIG. 3).
Fe-doped MoS₂ nanocanopies composed of Mo, Fe, S, and O, each element evenly distributed (FIG. 4 and FIG. 5).
Photoelectron spectroscopy shows valences of Mo, Fe, S, and O are +4, +2, −2, and −2, respectively (FIG. 6).
| 173 mV |
Fe0.05-MoS₂ (Fe-doped molybdenum disulfide nanocanopies) |
Electrocatalytic Tafel Slope HER Acid | 40.1 mV/dec | Fe0.05-MoS₂ (Fe-doped molybdenum disulfide nanocanopies) |
Electrocatalytic Overpotential HER Alkaline | 153 mV | Fe-doped MoS₂ nano-material (nanocanopies) |
Electrocatalytic Tafel Slope HER Alkaline | 85.6 mV/dec | Fe-doped MoS₂ nano-material (nanocanopies) |
Electrocatalytic Overpotential OER Alkaline | 230 mV | Fe-doped MoS₂ nano-material (nanocanopies) |
Electrocatalytic Tafel Slope OER Alkaline | 78.7 mV/dec | Fe-doped MoS₂ nano-material (nanocanopies) |
Electrocatalytic Overall Water Splitting Voltage | 1.52 V | Fe-doped MoS₂ nano-material (nanocanopies) |
Voltage | 0–0.8 V | — |
Voltage | 0.8–2 V | — |
Thickness | ≤ 200 nm | — |
Temperature | 180–200 °C | — |
Temperature | 40–60 °C | — |
Duration | ≤ 3 minutes | — |
Cited non-patent literature · 3
X-ray powder diffraction pattern of Fe-doped MoS₂ nanocanopies conforms with reported interlayer spacing of 9.4 Å for MoS₂ (FIG. 3).
Fe-doped MoS₂ nanocanopies composed of Mo, Fe, S, and O, each element evenly distributed (FIG. 4 and FIG. 5).
Photoelectron spectroscopy shows valences of Mo, Fe, S, and O are +4, +2, −2, and −2, respectively (FIG. 6).
| 173 mV |
Fe0.05-MoS₂ (Fe-doped molybdenum disulfide nanocanopies) |
Electrocatalytic Tafel Slope HER Acid | 40.1 mV/dec | Fe0.05-MoS₂ (Fe-doped molybdenum disulfide nanocanopies) |
Electrocatalytic Overpotential HER Alkaline | 153 mV | Fe-doped MoS₂ nano-material (nanocanopies) |
Electrocatalytic Tafel Slope HER Alkaline | 85.6 mV/dec | Fe-doped MoS₂ nano-material (nanocanopies) |
Electrocatalytic Overpotential OER Alkaline | 230 mV | Fe-doped MoS₂ nano-material (nanocanopies) |
Electrocatalytic Tafel Slope OER Alkaline | 78.7 mV/dec | Fe-doped MoS₂ nano-material (nanocanopies) |
Electrocatalytic Overall Water Splitting Voltage | 1.52 V | Fe-doped MoS₂ nano-material (nanocanopies) |
Voltage | 0–0.8 V | — |
Voltage | 0.8–2 V | — |
Thickness | ≤ 200 nm | — |
Temperature | 180–200 °C | — |
Temperature | 40–60 °C | — |
Duration | ≤ 3 minutes | — |
Cited non-patent literature · 3
X-ray powder diffraction pattern of Fe-doped MoS₂ nanocanopies conforms with reported interlayer spacing of 9.4 Å for MoS₂ (FIG. 3).
Fe-doped MoS₂ nanocanopies composed of Mo, Fe, S, and O, each element evenly distributed (FIG. 4 and FIG. 5).
Photoelectron spectroscopy shows valences of Mo, Fe, S, and O are +4, +2, −2, and −2, respectively (FIG. 6).
| 173 mV |
Fe0.05-MoS₂ (Fe-doped molybdenum disulfide nanocanopies) |
Electrocatalytic Tafel Slope HER Acid | 40.1 mV/dec | Fe0.05-MoS₂ (Fe-doped molybdenum disulfide nanocanopies) |
Electrocatalytic Overpotential HER Alkaline | 153 mV | Fe-doped MoS₂ nano-material (nanocanopies) |
Electrocatalytic Tafel Slope HER Alkaline | 85.6 mV/dec | Fe-doped MoS₂ nano-material (nanocanopies) |
Electrocatalytic Overpotential OER Alkaline | 230 mV | Fe-doped MoS₂ nano-material (nanocanopies) |
Electrocatalytic Tafel Slope OER Alkaline | 78.7 mV/dec | Fe-doped MoS₂ nano-material (nanocanopies) |
Electrocatalytic Overall Water Splitting Voltage | 1.52 V | Fe-doped MoS₂ nano-material (nanocanopies) |
Voltage | 0–0.8 V | — |
Voltage | 0.8–2 V | — |
Thickness | ≤ 200 nm | — |
Temperature | 180–200 °C | — |
Temperature | 40–60 °C | — |
Duration | ≤ 3 minutes | — |
Cited non-patent literature · 3