Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1 is a schematic diagram of a chemical vapor deposition chamber for the controlled synthesis of hBN films or nanotubes.
FIG. 2 includes a characteristic Raman spectra of hBN synthesized in accordance with the method of the present invention.
FIG. 3 includes characteristic SEM images of hBN mul- tilayer (top) and monolayer (bottom) synthesized in accor- 5 dance with the method of the present …
FIG. 4 includes a characteristic XRD graph of hBN grown on Fe foil in accordance with a non-limiting example of the present invention.
FIG. 5 includes SEM images of BN nanotubes grown in 10 accordance with the present invention using solid boron and molecular nitrogen and hydrogen as …
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 of synthesizing hexagonal boron nitride, the method comprising: positioning a solid boron-containing precursor and a continuous growth substrate within a chemical vapor deposition chamber, wherein the solid boron-contain-ing precursor includes boron powders, boron frag-ments, or boron platelets and does not directly contact the continuous growth substrate, wherein the continu-ous growth substrate includes nickel, iron, copper, chromium, or alloys thereof, and wherein the continu-ous growth substrate is unwound from a supply reel; heating an interior of the chemical vapor deposition chamber to between 800° C. and 1200° C., inclusive; flowing a nitrogen-containing reaction gas mixture into the chemical vapor deposition chamber, the reaction gas mixture including a nitrogen compound and hydro-gen gas, wherein the reaction gas mixture is pressurized between 10 mTorr and 800 Torr, inclusive, wherein the reaction gas mixture includes a ratio of a partial pres-sure of nitrogen to a partial pressure of hydrogen of greater than 30, and wherein the continuous growth substrate reacts with boron released from the solid boron-containing precursor and the nitrogen compound to form a single-layer or multi-layer hexagonal boron nitride film on the continuous growth substrate; and taking up the continuous growth substrate onto a take-up reel after formation of the hexagonal boron nitride film on the continuous growth substrate.
The method of claim 1, wherein the nitrogen compound comprises molecular nitrogen (N₂).
The method of claim 1, wherein the nitrogen compound comprises ammonia (NH₃).
The method of claim 1, wherein the reaction gas mixture includes a concentration of between 0.01% and 25% of hydrogen gas (H₂).
The method of claim 1, wherein the solid boron-containing precursor is supported above the continuous growth substrate.
The method of claim 1, wherein the solid boron-containing precursor is supported below the continuous growth substrate.
The method of claim 1, wherein the solid boron-containing precursor is supported laterally adjacent to the continuous growth substrate.
The method of claim 1, wherein the solid boron precursor includes elemental boron (B), boron oxide (B₂O₃), or boron carbide (B₄C).
The method of claim 1, wherein the solid boron-containing precursor includes metal borides such as iron borides (FexB), nickel boride (NixB) and magnesium diboride (MgB₂).
A method of synthesizing hexagonal boron nitride, the method comprising: positioning a solid boron-containing precursor and a growth substrate within a chemical vapor deposition chamber, wherein the solid boron-containing precursor includes boron powders, boron fragments, or boron platelets and does not directly contact the growth substrate, and wherein the growth substrate includes nickel, iron, copper, chromium, or alloys thereof; heating an interior of the chemical vapor deposition chamber to between 800° C. and 1200° C., inclusive; and flowing a nitrogen-containing reaction gas mixture into the chemical vapor deposition chamber, the reaction gas mixture including a nitrogen compound and hydro-gen gas; wherein the reaction gas mixture is pressurized between 10 mTorr and 800 Torr, inclusive, wherein the growth substrate reacts with boron released from the solid boron-containing precursor and the nitrogen compound to form a single-layer or multi-layer hexagonal boron nitride film, and wherein the growth substrate com-prises a film having a thickness of between 0.1 µm and 5.0 µm, inclusive.
A method of synthesizing hexagonal boron nitride, the method comprising: positioning a solid boron-containing precursor and a growth substrate within a chemical vapor deposition chamber, wherein the solid boron-containing precursor includes boron powders, boron fragments, or boron platelets and does not directly contact the growth substrate, and wherein the growth substrate includes nickel, iron, copper, chromium, or alloys thereof; heating an interior of the chemical vapor deposition chamber to between 800° C. and 1200° C., inclusive; and flowing a nitrogen-containing reaction gas mixture into the chemical vapor deposition chamber, the reaction gas mixture including a nitrogen compound and hydro-gen gas; wherein the reaction gas mixture is pressurized between 10 mTorr and 800 Torr, inclusive, wherein the growth substrate reacts with boron released from the solid boron-containing precursor and the nitrogen compound to form a single-layer or multi-layer hexagonal boron nitride film, and wherein the growth substrate com-prises a foil having a thickness of between 5.0 µm and 150 µm, inclusive.
A method of synthesizing hexagonal boron nitride, the method comprising: positioning a solid boron-containing precursor and a growth substrate within a chemical vapor deposition chamber, wherein the solid boron-containing precursor includes boron powders, boron fragments, or boron platelets and does not directly contact the growth substrate, and wherein the growth substrate includes nickel, iron, copper, chromium, or alloys thereof; heating an interior of the chemical vapor deposition chamber to between 800° C. and 1200° C., inclusive; and flowing a nitrogen-containing reaction gas mixture into the chemical vapor deposition chamber, the reaction gas mixture including a nitrogen compound and hydro-gen gas; wherein the reaction gas mixture is pressurized between 10 mTorr and 800 Torr, inclusive, wherein the growth substrate reacts with boron released from the solid boron-containing precursor and the nitrogen compound to form a single-layer or multi-layer hexagonal boron nitride film, and wherein the growth substrate com-prises a sheet having a thickness of between 0.15 mm and 5 mm, inclusive.
A method of synthesizing hexagonal boron nitride, the method comprising: positioning a solid boron-containing precursor and a growth substrate within a chemical vapor deposition chamber, wherein the solid boron-containing precursor includes boron powders, boron fragments, or boron platelets and does not directly contact the growth substrate, and wherein the growth substrate includes nickel, iron, copper, chromium, or alloys thereof; heating an interior of the chemical vapor deposition chamber to between 800° C. and 1200° C., inclusive; and flowing a nitrogen-containing reaction gas mixture into the chemical vapor deposition chamber, the reaction gas mixture including a nitrogen compound and hydro-gen gas; wherein the reaction gas mixture is pressurized between 10 mTorr and 800 Torr, inclusive, wherein the growth substrate reacts with boron released from the solid boron-containing precursor and the nitrogen compound to form a single-layer or multi-layer hexagonal boron nitride film, and wherein the growth substrate com-prises a plate having a thickness of between 5 mm and 100 mm, inclusive.
A method of synthesizing hexagonal boron nitride, the method comprising: positioning a solid boron-containing precursor and a growth substrate within a chemical vapor deposition chamber, wherein the solid boron-containing precursor includes boron powders, boron fragments, or boron platelets and does not directly contact the growth substrate, and wherein the growth substrate includes nickel, iron, copper, chromium, or alloys thereof; heating an interior of the chemical vapor deposition chamber to between 800° C. and 1200° C., inclusive; and flowing a nitrogen-containing reaction gas mixture into the chemical vapor deposition chamber, the reaction gas mixture including a nitrogen compound and hydro-gen gas; wherein the reaction gas mixture is pressurized between 10 mTorr and 800 Torr, inclusive, wherein the growth substrate reacts with boron released from the solid boron-containing precursor and the nitrogen compound to form a single-layer or multi-layer hexagonal boron nitride film, and wherein the growth substrate com-prises includes a three-dimensional geometry including at least one of nails, tubes, and ball bearings.
A method of synthesizing boron nitride nanotubes, the method comprising: positioning a solid boron-containing precursor and metal-lic nanoparticles within a chemical vapor deposition chamber, wherein the solid boron-containing precursor includes boron powders, boron fragments, or boron platelets and does not directly contact the metallic nanotubes, and wherein the metallic nanoparticles include nickel, iron, copper, chromium, or alloys thereof; heating an interior of the chemical vapor deposition chamber to between 800° C. and 1200° C., inclusive; and flowing a nitrogen-containing reaction gas mixture into the chemical vapor deposition chamber, the reaction gas mixture including a nitrogen compound and hydro-gen gas; wherein the reaction gas mixture is pressurized between 10 mTorr and 800 Torr, inclusive, and wherein the metallic nanotubes react with boron released from the solid boron-containing precursor and the nitrogen com-pound to form boron nitride nanotubes.
The method of claim 15, further including forming the metallic nanotubes by dewetting a metallic film having a thickness less than 100 nm at a temperature greater than 800° C.
The method of claim 15, wherein the boron nitride nanotubes have a mean diameter of between 0.5 nm and 100 nm, inclusive.
The method of claim 15, wherein the nitrogen com-pound comprises molecular nitrogen (N₂).
The method of claim 15, wherein the nitrogen com-pound comprises ammonia (NH₃).
The method of claim 15, wherein the reaction gas mixture includes a concentration of between 0.01% and 25% of hydrogen gas (H₂).
The method of claim 15, wherein the reaction gas mixture includes an inert gas and wherein the reaction gas mixture is maintained at atmospheric pressure.
The method of claim 15, wherein the solid boron-containing precursor is supported above the metallic nan-oparticles.
The method of claim 15, wherein the solid boron-containing precursor is supported below the metallic nan-oparticles.
The method of claim 15, wherein the solid boron-containing precursor is supported laterally adjacent to the metallic nanoparticles.
The method of claim 15, wherein the reaction mixture includes a ratio of a partial pressure of nitrogen and a partial pressure of hydrogen of at least 30. ∗ ∗ ∗ ∗ ∗
Layer stacks claimed or described, ordered top of device to substrate.
boron nitride nanotubes
Materials described outside the worked examples.
solid boron-containing precursor (boron powders, boron fragments, or boron platelets)
growth substrate (nickel, iron, copper, chromium, or alloys thereof)
hexagonal boron nitride film (single-layer or multi-layer)
hBN
hydrogen gas
H₂
molecular nitrogen
N₂
ammonia
NH₃
elemental boron
B
boron oxide
B₂O₃
boron carbide
B₄C
iron borides
FexB
nickel boride
NixB
magnesium diboride
MgB₂
boron nitride nanotubes
BN
metallic nanoparticles (nickel, iron, copper, chromium, or alloys thereof)
argon (inert/buffer gas)
Ar
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
FIG. 2 includes a characteristic Raman spectra of hBN synthesized in accordance with the method of the present invention.
FIG. 3 includes characteristic SEM images of hBN mul- tilayer (top) and monolayer (bottom) synthesized in accor- 5 dance with the method of the present …
FIG. 4 includes a characteristic XRD graph of hBN grown on Fe foil in accordance with a non-limiting example of the present invention.
FIG. 4 includes a characteristic XRD graph of hBN grown on Fe foil in accordance with a non-limiting example of the present invention.
FIG. 5 includes SEM images of BN nanotubes grown in 10 accordance with the present invention using solid boron and molecular nitrogen and hydrogen as …
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Temperature | 800–1200 °C | — |
Thickness | 0.1–5 µm | — |
Thickness | 5–150 µm | — |
Thickness | 0.15–5 mm | — |
Thickness | 0.1–1000 µm | — |
Thickness | 1–100 mm | — |
Pressure | 0.01–800 Torr | — |
Thickness | 0.5–100 nm | — |
Thickness | 5–100 mm | — |
Duration | 30–60 minutes | — |
Thickness | 0.3–1 µm | — |
Thickness | ≤ 1 nm | — |
Thickness | ≥ 5 mm | — |
Temperature | ≥ 800 °C | — |
Duration | ≤ 120 minutes | — |
Patents and literature cited by this patent (applicant and examiner references).
Cited patents · 11
Cited non-patent literature · 2
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Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1 is a schematic diagram of a chemical vapor deposition chamber for the controlled synthesis of hBN films or nanotubes.
FIG. 2 includes a characteristic Raman spectra of hBN synthesized in accordance with the method of the present invention.
FIG. 3 includes characteristic SEM images of hBN mul- tilayer (top) and monolayer (bottom) synthesized in accor- 5 dance with the method of the present …
FIG. 4 includes a characteristic XRD graph of hBN grown on Fe foil in accordance with a non-limiting example of the present invention.
FIG. 5 includes SEM images of BN nanotubes grown in 10 accordance with the present invention using solid boron and molecular nitrogen and hydrogen as …
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 of synthesizing hexagonal boron nitride, the method comprising: positioning a solid boron-containing precursor and a continuous growth substrate within a chemical vapor deposition chamber, wherein the solid boron-contain-ing precursor includes boron powders, boron frag-ments, or boron platelets and does not directly contact the continuous growth substrate, wherein the continu-ous growth substrate includes nickel, iron, copper, chromium, or alloys thereof, and wherein the continu-ous growth substrate is unwound from a supply reel; heating an interior of the chemical vapor deposition chamber to between 800° C. and 1200° C., inclusive; flowing a nitrogen-containing reaction gas mixture into the chemical vapor deposition chamber, the reaction gas mixture including a nitrogen compound and hydro-gen gas, wherein the reaction gas mixture is pressurized between 10 mTorr and 800 Torr, inclusive, wherein the reaction gas mixture includes a ratio of a partial pres-sure of nitrogen to a partial pressure of hydrogen of greater than 30, and wherein the continuous growth substrate reacts with boron released from the solid boron-containing precursor and the nitrogen compound to form a single-layer or multi-layer hexagonal boron nitride film on the continuous growth substrate; and taking up the continuous growth substrate onto a take-up reel after formation of the hexagonal boron nitride film on the continuous growth substrate.
The method of claim 1, wherein the nitrogen compound comprises molecular nitrogen (N₂).
The method of claim 1, wherein the nitrogen compound comprises ammonia (NH₃).
The method of claim 1, wherein the reaction gas mixture includes a concentration of between 0.01% and 25% of hydrogen gas (H₂).
The method of claim 1, wherein the solid boron-containing precursor is supported above the continuous growth substrate.
The method of claim 1, wherein the solid boron-containing precursor is supported below the continuous growth substrate.
The method of claim 1, wherein the solid boron-containing precursor is supported laterally adjacent to the continuous growth substrate.
The method of claim 1, wherein the solid boron precursor includes elemental boron (B), boron oxide (B₂O₃), or boron carbide (B₄C).
The method of claim 1, wherein the solid boron-containing precursor includes metal borides such as iron borides (FexB), nickel boride (NixB) and magnesium diboride (MgB₂).
A method of synthesizing hexagonal boron nitride, the method comprising: positioning a solid boron-containing precursor and a growth substrate within a chemical vapor deposition chamber, wherein the solid boron-containing precursor includes boron powders, boron fragments, or boron platelets and does not directly contact the growth substrate, and wherein the growth substrate includes nickel, iron, copper, chromium, or alloys thereof; heating an interior of the chemical vapor deposition chamber to between 800° C. and 1200° C., inclusive; and flowing a nitrogen-containing reaction gas mixture into the chemical vapor deposition chamber, the reaction gas mixture including a nitrogen compound and hydro-gen gas; wherein the reaction gas mixture is pressurized between 10 mTorr and 800 Torr, inclusive, wherein the growth substrate reacts with boron released from the solid boron-containing precursor and the nitrogen compound to form a single-layer or multi-layer hexagonal boron nitride film, and wherein the growth substrate com-prises a film having a thickness of between 0.1 µm and 5.0 µm, inclusive.
A method of synthesizing hexagonal boron nitride, the method comprising: positioning a solid boron-containing precursor and a growth substrate within a chemical vapor deposition chamber, wherein the solid boron-containing precursor includes boron powders, boron fragments, or boron platelets and does not directly contact the growth substrate, and wherein the growth substrate includes nickel, iron, copper, chromium, or alloys thereof; heating an interior of the chemical vapor deposition chamber to between 800° C. and 1200° C., inclusive; and flowing a nitrogen-containing reaction gas mixture into the chemical vapor deposition chamber, the reaction gas mixture including a nitrogen compound and hydro-gen gas; wherein the reaction gas mixture is pressurized between 10 mTorr and 800 Torr, inclusive, wherein the growth substrate reacts with boron released from the solid boron-containing precursor and the nitrogen compound to form a single-layer or multi-layer hexagonal boron nitride film, and wherein the growth substrate com-prises a foil having a thickness of between 5.0 µm and 150 µm, inclusive.
A method of synthesizing hexagonal boron nitride, the method comprising: positioning a solid boron-containing precursor and a growth substrate within a chemical vapor deposition chamber, wherein the solid boron-containing precursor includes boron powders, boron fragments, or boron platelets and does not directly contact the growth substrate, and wherein the growth substrate includes nickel, iron, copper, chromium, or alloys thereof; heating an interior of the chemical vapor deposition chamber to between 800° C. and 1200° C., inclusive; and flowing a nitrogen-containing reaction gas mixture into the chemical vapor deposition chamber, the reaction gas mixture including a nitrogen compound and hydro-gen gas; wherein the reaction gas mixture is pressurized between 10 mTorr and 800 Torr, inclusive, wherein the growth substrate reacts with boron released from the solid boron-containing precursor and the nitrogen compound to form a single-layer or multi-layer hexagonal boron nitride film, and wherein the growth substrate com-prises a sheet having a thickness of between 0.15 mm and 5 mm, inclusive.
A method of synthesizing hexagonal boron nitride, the method comprising: positioning a solid boron-containing precursor and a growth substrate within a chemical vapor deposition chamber, wherein the solid boron-containing precursor includes boron powders, boron fragments, or boron platelets and does not directly contact the growth substrate, and wherein the growth substrate includes nickel, iron, copper, chromium, or alloys thereof; heating an interior of the chemical vapor deposition chamber to between 800° C. and 1200° C., inclusive; and flowing a nitrogen-containing reaction gas mixture into the chemical vapor deposition chamber, the reaction gas mixture including a nitrogen compound and hydro-gen gas; wherein the reaction gas mixture is pressurized between 10 mTorr and 800 Torr, inclusive, wherein the growth substrate reacts with boron released from the solid boron-containing precursor and the nitrogen compound to form a single-layer or multi-layer hexagonal boron nitride film, and wherein the growth substrate com-prises a plate having a thickness of between 5 mm and 100 mm, inclusive.
A method of synthesizing hexagonal boron nitride, the method comprising: positioning a solid boron-containing precursor and a growth substrate within a chemical vapor deposition chamber, wherein the solid boron-containing precursor includes boron powders, boron fragments, or boron platelets and does not directly contact the growth substrate, and wherein the growth substrate includes nickel, iron, copper, chromium, or alloys thereof; heating an interior of the chemical vapor deposition chamber to between 800° C. and 1200° C., inclusive; and flowing a nitrogen-containing reaction gas mixture into the chemical vapor deposition chamber, the reaction gas mixture including a nitrogen compound and hydro-gen gas; wherein the reaction gas mixture is pressurized between 10 mTorr and 800 Torr, inclusive, wherein the growth substrate reacts with boron released from the solid boron-containing precursor and the nitrogen compound to form a single-layer or multi-layer hexagonal boron nitride film, and wherein the growth substrate com-prises includes a three-dimensional geometry including at least one of nails, tubes, and ball bearings.
A method of synthesizing boron nitride nanotubes, the method comprising: positioning a solid boron-containing precursor and metal-lic nanoparticles within a chemical vapor deposition chamber, wherein the solid boron-containing precursor includes boron powders, boron fragments, or boron platelets and does not directly contact the metallic nanotubes, and wherein the metallic nanoparticles include nickel, iron, copper, chromium, or alloys thereof; heating an interior of the chemical vapor deposition chamber to between 800° C. and 1200° C., inclusive; and flowing a nitrogen-containing reaction gas mixture into the chemical vapor deposition chamber, the reaction gas mixture including a nitrogen compound and hydro-gen gas; wherein the reaction gas mixture is pressurized between 10 mTorr and 800 Torr, inclusive, and wherein the metallic nanotubes react with boron released from the solid boron-containing precursor and the nitrogen com-pound to form boron nitride nanotubes.
The method of claim 15, further including forming the metallic nanotubes by dewetting a metallic film having a thickness less than 100 nm at a temperature greater than 800° C.
The method of claim 15, wherein the boron nitride nanotubes have a mean diameter of between 0.5 nm and 100 nm, inclusive.
The method of claim 15, wherein the nitrogen com-pound comprises molecular nitrogen (N₂).
The method of claim 15, wherein the nitrogen com-pound comprises ammonia (NH₃).
The method of claim 15, wherein the reaction gas mixture includes a concentration of between 0.01% and 25% of hydrogen gas (H₂).
The method of claim 15, wherein the reaction gas mixture includes an inert gas and wherein the reaction gas mixture is maintained at atmospheric pressure.
The method of claim 15, wherein the solid boron-containing precursor is supported above the metallic nan-oparticles.
The method of claim 15, wherein the solid boron-containing precursor is supported below the metallic nan-oparticles.
The method of claim 15, wherein the solid boron-containing precursor is supported laterally adjacent to the metallic nanoparticles.
The method of claim 15, wherein the reaction mixture includes a ratio of a partial pressure of nitrogen and a partial pressure of hydrogen of at least 30. ∗ ∗ ∗ ∗ ∗
Layer stacks claimed or described, ordered top of device to substrate.
boron nitride nanotubes
Materials described outside the worked examples.
solid boron-containing precursor (boron powders, boron fragments, or boron platelets)
growth substrate (nickel, iron, copper, chromium, or alloys thereof)
hexagonal boron nitride film (single-layer or multi-layer)
hBN
hydrogen gas
H₂
molecular nitrogen
N₂
ammonia
NH₃
elemental boron
B
boron oxide
B₂O₃
boron carbide
B₄C
iron borides
FexB
nickel boride
NixB
magnesium diboride
MgB₂
boron nitride nanotubes
BN
metallic nanoparticles (nickel, iron, copper, chromium, or alloys thereof)
argon (inert/buffer gas)
Ar
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
FIG. 2 includes a characteristic Raman spectra of hBN synthesized in accordance with the method of the present invention.
FIG. 3 includes characteristic SEM images of hBN mul- tilayer (top) and monolayer (bottom) synthesized in accor- 5 dance with the method of the present …
FIG. 4 includes a characteristic XRD graph of hBN grown on Fe foil in accordance with a non-limiting example of the present invention.
FIG. 4 includes a characteristic XRD graph of hBN grown on Fe foil in accordance with a non-limiting example of the present invention.
FIG. 5 includes SEM images of BN nanotubes grown in 10 accordance with the present invention using solid boron and molecular nitrogen and hydrogen as …
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Temperature | 800–1200 °C | — |
Thickness | 0.1–5 µm | — |
Thickness | 5–150 µm | — |
Thickness | 0.15–5 mm | — |
Thickness | 0.1–1000 µm | — |
Thickness | 1–100 mm | — |
Pressure | 0.01–800 Torr | — |
Thickness | 0.5–100 nm | — |
Thickness | 5–100 mm | — |
Duration | 30–60 minutes | — |
Thickness | 0.3–1 µm | — |
Thickness | ≤ 1 nm | — |
Thickness | ≥ 5 mm | — |
Temperature | ≥ 800 °C | — |
Duration | ≤ 120 minutes | — |
Patents and literature cited by this patent (applicant and examiner references).
Cited patents · 11
Cited non-patent literature · 2
Related documents with shared materials, methods, properties, or citations.
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Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1 is a schematic diagram of a chemical vapor deposition chamber for the controlled synthesis of hBN films or nanotubes.
FIG. 2 includes a characteristic Raman spectra of hBN synthesized in accordance with the method of the present invention.
FIG. 3 includes characteristic SEM images of hBN mul- tilayer (top) and monolayer (bottom) synthesized in accor- 5 dance with the method of the present …
FIG. 4 includes a characteristic XRD graph of hBN grown on Fe foil in accordance with a non-limiting example of the present invention.
FIG. 5 includes SEM images of BN nanotubes grown in 10 accordance with the present invention using solid boron and molecular nitrogen and hydrogen as …
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 of synthesizing hexagonal boron nitride, the method comprising: positioning a solid boron-containing precursor and a continuous growth substrate within a chemical vapor deposition chamber, wherein the solid boron-contain-ing precursor includes boron powders, boron frag-ments, or boron platelets and does not directly contact the continuous growth substrate, wherein the continu-ous growth substrate includes nickel, iron, copper, chromium, or alloys thereof, and wherein the continu-ous growth substrate is unwound from a supply reel; heating an interior of the chemical vapor deposition chamber to between 800° C. and 1200° C., inclusive; flowing a nitrogen-containing reaction gas mixture into the chemical vapor deposition chamber, the reaction gas mixture including a nitrogen compound and hydro-gen gas, wherein the reaction gas mixture is pressurized between 10 mTorr and 800 Torr, inclusive, wherein the reaction gas mixture includes a ratio of a partial pres-sure of nitrogen to a partial pressure of hydrogen of greater than 30, and wherein the continuous growth substrate reacts with boron released from the solid boron-containing precursor and the nitrogen compound to form a single-layer or multi-layer hexagonal boron nitride film on the continuous growth substrate; and taking up the continuous growth substrate onto a take-up reel after formation of the hexagonal boron nitride film on the continuous growth substrate.
The method of claim 1, wherein the nitrogen compound comprises molecular nitrogen (N₂).
The method of claim 1, wherein the nitrogen compound comprises ammonia (NH₃).
The method of claim 1, wherein the reaction gas mixture includes a concentration of between 0.01% and 25% of hydrogen gas (H₂).
The method of claim 1, wherein the solid boron-containing precursor is supported above the continuous growth substrate.
The method of claim 1, wherein the solid boron-containing precursor is supported below the continuous growth substrate.
The method of claim 1, wherein the solid boron-containing precursor is supported laterally adjacent to the continuous growth substrate.
The method of claim 1, wherein the solid boron precursor includes elemental boron (B), boron oxide (B₂O₃), or boron carbide (B₄C).
The method of claim 1, wherein the solid boron-containing precursor includes metal borides such as iron borides (FexB), nickel boride (NixB) and magnesium diboride (MgB₂).
A method of synthesizing hexagonal boron nitride, the method comprising: positioning a solid boron-containing precursor and a growth substrate within a chemical vapor deposition chamber, wherein the solid boron-containing precursor includes boron powders, boron fragments, or boron platelets and does not directly contact the growth substrate, and wherein the growth substrate includes nickel, iron, copper, chromium, or alloys thereof; heating an interior of the chemical vapor deposition chamber to between 800° C. and 1200° C., inclusive; and flowing a nitrogen-containing reaction gas mixture into the chemical vapor deposition chamber, the reaction gas mixture including a nitrogen compound and hydro-gen gas; wherein the reaction gas mixture is pressurized between 10 mTorr and 800 Torr, inclusive, wherein the growth substrate reacts with boron released from the solid boron-containing precursor and the nitrogen compound to form a single-layer or multi-layer hexagonal boron nitride film, and wherein the growth substrate com-prises a film having a thickness of between 0.1 µm and 5.0 µm, inclusive.
A method of synthesizing hexagonal boron nitride, the method comprising: positioning a solid boron-containing precursor and a growth substrate within a chemical vapor deposition chamber, wherein the solid boron-containing precursor includes boron powders, boron fragments, or boron platelets and does not directly contact the growth substrate, and wherein the growth substrate includes nickel, iron, copper, chromium, or alloys thereof; heating an interior of the chemical vapor deposition chamber to between 800° C. and 1200° C., inclusive; and flowing a nitrogen-containing reaction gas mixture into the chemical vapor deposition chamber, the reaction gas mixture including a nitrogen compound and hydro-gen gas; wherein the reaction gas mixture is pressurized between 10 mTorr and 800 Torr, inclusive, wherein the growth substrate reacts with boron released from the solid boron-containing precursor and the nitrogen compound to form a single-layer or multi-layer hexagonal boron nitride film, and wherein the growth substrate com-prises a foil having a thickness of between 5.0 µm and 150 µm, inclusive.
A method of synthesizing hexagonal boron nitride, the method comprising: positioning a solid boron-containing precursor and a growth substrate within a chemical vapor deposition chamber, wherein the solid boron-containing precursor includes boron powders, boron fragments, or boron platelets and does not directly contact the growth substrate, and wherein the growth substrate includes nickel, iron, copper, chromium, or alloys thereof; heating an interior of the chemical vapor deposition chamber to between 800° C. and 1200° C., inclusive; and flowing a nitrogen-containing reaction gas mixture into the chemical vapor deposition chamber, the reaction gas mixture including a nitrogen compound and hydro-gen gas; wherein the reaction gas mixture is pressurized between 10 mTorr and 800 Torr, inclusive, wherein the growth substrate reacts with boron released from the solid boron-containing precursor and the nitrogen compound to form a single-layer or multi-layer hexagonal boron nitride film, and wherein the growth substrate com-prises a sheet having a thickness of between 0.15 mm and 5 mm, inclusive.
A method of synthesizing hexagonal boron nitride, the method comprising: positioning a solid boron-containing precursor and a growth substrate within a chemical vapor deposition chamber, wherein the solid boron-containing precursor includes boron powders, boron fragments, or boron platelets and does not directly contact the growth substrate, and wherein the growth substrate includes nickel, iron, copper, chromium, or alloys thereof; heating an interior of the chemical vapor deposition chamber to between 800° C. and 1200° C., inclusive; and flowing a nitrogen-containing reaction gas mixture into the chemical vapor deposition chamber, the reaction gas mixture including a nitrogen compound and hydro-gen gas; wherein the reaction gas mixture is pressurized between 10 mTorr and 800 Torr, inclusive, wherein the growth substrate reacts with boron released from the solid boron-containing precursor and the nitrogen compound to form a single-layer or multi-layer hexagonal boron nitride film, and wherein the growth substrate com-prises a plate having a thickness of between 5 mm and 100 mm, inclusive.
A method of synthesizing hexagonal boron nitride, the method comprising: positioning a solid boron-containing precursor and a growth substrate within a chemical vapor deposition chamber, wherein the solid boron-containing precursor includes boron powders, boron fragments, or boron platelets and does not directly contact the growth substrate, and wherein the growth substrate includes nickel, iron, copper, chromium, or alloys thereof; heating an interior of the chemical vapor deposition chamber to between 800° C. and 1200° C., inclusive; and flowing a nitrogen-containing reaction gas mixture into the chemical vapor deposition chamber, the reaction gas mixture including a nitrogen compound and hydro-gen gas; wherein the reaction gas mixture is pressurized between 10 mTorr and 800 Torr, inclusive, wherein the growth substrate reacts with boron released from the solid boron-containing precursor and the nitrogen compound to form a single-layer or multi-layer hexagonal boron nitride film, and wherein the growth substrate com-prises includes a three-dimensional geometry including at least one of nails, tubes, and ball bearings.
A method of synthesizing boron nitride nanotubes, the method comprising: positioning a solid boron-containing precursor and metal-lic nanoparticles within a chemical vapor deposition chamber, wherein the solid boron-containing precursor includes boron powders, boron fragments, or boron platelets and does not directly contact the metallic nanotubes, and wherein the metallic nanoparticles include nickel, iron, copper, chromium, or alloys thereof; heating an interior of the chemical vapor deposition chamber to between 800° C. and 1200° C., inclusive; and flowing a nitrogen-containing reaction gas mixture into the chemical vapor deposition chamber, the reaction gas mixture including a nitrogen compound and hydro-gen gas; wherein the reaction gas mixture is pressurized between 10 mTorr and 800 Torr, inclusive, and wherein the metallic nanotubes react with boron released from the solid boron-containing precursor and the nitrogen com-pound to form boron nitride nanotubes.
The method of claim 15, further including forming the metallic nanotubes by dewetting a metallic film having a thickness less than 100 nm at a temperature greater than 800° C.
The method of claim 15, wherein the boron nitride nanotubes have a mean diameter of between 0.5 nm and 100 nm, inclusive.
The method of claim 15, wherein the nitrogen com-pound comprises molecular nitrogen (N₂).
The method of claim 15, wherein the nitrogen com-pound comprises ammonia (NH₃).
The method of claim 15, wherein the reaction gas mixture includes a concentration of between 0.01% and 25% of hydrogen gas (H₂).
The method of claim 15, wherein the reaction gas mixture includes an inert gas and wherein the reaction gas mixture is maintained at atmospheric pressure.
The method of claim 15, wherein the solid boron-containing precursor is supported above the metallic nan-oparticles.
The method of claim 15, wherein the solid boron-containing precursor is supported below the metallic nan-oparticles.
The method of claim 15, wherein the solid boron-containing precursor is supported laterally adjacent to the metallic nanoparticles.
The method of claim 15, wherein the reaction mixture includes a ratio of a partial pressure of nitrogen and a partial pressure of hydrogen of at least 30. ∗ ∗ ∗ ∗ ∗
Layer stacks claimed or described, ordered top of device to substrate.
boron nitride nanotubes
Materials described outside the worked examples.
solid boron-containing precursor (boron powders, boron fragments, or boron platelets)
growth substrate (nickel, iron, copper, chromium, or alloys thereof)
hexagonal boron nitride film (single-layer or multi-layer)
hBN
hydrogen gas
H₂
molecular nitrogen
N₂
ammonia
NH₃
elemental boron
B
boron oxide
B₂O₃
boron carbide
B₄C
iron borides
FexB
nickel boride
NixB
magnesium diboride
MgB₂
boron nitride nanotubes
BN
metallic nanoparticles (nickel, iron, copper, chromium, or alloys thereof)
argon (inert/buffer gas)
Ar
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
FIG. 2 includes a characteristic Raman spectra of hBN synthesized in accordance with the method of the present invention.
FIG. 3 includes characteristic SEM images of hBN mul- tilayer (top) and monolayer (bottom) synthesized in accor- 5 dance with the method of the present …
FIG. 4 includes a characteristic XRD graph of hBN grown on Fe foil in accordance with a non-limiting example of the present invention.
FIG. 4 includes a characteristic XRD graph of hBN grown on Fe foil in accordance with a non-limiting example of the present invention.
FIG. 5 includes SEM images of BN nanotubes grown in 10 accordance with the present invention using solid boron and molecular nitrogen and hydrogen as …
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Temperature | 800–1200 °C | — |
Thickness | 0.1–5 µm | — |
Thickness | 5–150 µm | — |
Thickness | 0.15–5 mm | — |
Thickness | 0.1–1000 µm | — |
Thickness | 1–100 mm | — |
Pressure | 0.01–800 Torr | — |
Thickness | 0.5–100 nm | — |
Thickness | 5–100 mm | — |
Duration | 30–60 minutes | — |
Thickness | 0.3–1 µm | — |
Thickness | ≤ 1 nm | — |
Thickness | ≥ 5 mm | — |
Temperature | ≥ 800 °C | — |
Duration | ≤ 120 minutes | — |
Patents and literature cited by this patent (applicant and examiner references).
Cited patents · 11
Cited non-patent literature · 2
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Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1 is a schematic diagram of a chemical vapor deposition chamber for the controlled synthesis of hBN films or nanotubes.
FIG. 2 includes a characteristic Raman spectra of hBN synthesized in accordance with the method of the present invention.
FIG. 3 includes characteristic SEM images of hBN mul- tilayer (top) and monolayer (bottom) synthesized in accor- 5 dance with the method of the present …
FIG. 4 includes a characteristic XRD graph of hBN grown on Fe foil in accordance with a non-limiting example of the present invention.
FIG. 5 includes SEM images of BN nanotubes grown in 10 accordance with the present invention using solid boron and molecular nitrogen and hydrogen as …
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 of synthesizing hexagonal boron nitride, the method comprising: positioning a solid boron-containing precursor and a continuous growth substrate within a chemical vapor deposition chamber, wherein the solid boron-contain-ing precursor includes boron powders, boron frag-ments, or boron platelets and does not directly contact the continuous growth substrate, wherein the continu-ous growth substrate includes nickel, iron, copper, chromium, or alloys thereof, and wherein the continu-ous growth substrate is unwound from a supply reel; heating an interior of the chemical vapor deposition chamber to between 800° C. and 1200° C., inclusive; flowing a nitrogen-containing reaction gas mixture into the chemical vapor deposition chamber, the reaction gas mixture including a nitrogen compound and hydro-gen gas, wherein the reaction gas mixture is pressurized between 10 mTorr and 800 Torr, inclusive, wherein the reaction gas mixture includes a ratio of a partial pres-sure of nitrogen to a partial pressure of hydrogen of greater than 30, and wherein the continuous growth substrate reacts with boron released from the solid boron-containing precursor and the nitrogen compound to form a single-layer or multi-layer hexagonal boron nitride film on the continuous growth substrate; and taking up the continuous growth substrate onto a take-up reel after formation of the hexagonal boron nitride film on the continuous growth substrate.
The method of claim 1, wherein the nitrogen compound comprises molecular nitrogen (N₂).
The method of claim 1, wherein the nitrogen compound comprises ammonia (NH₃).
The method of claim 1, wherein the reaction gas mixture includes a concentration of between 0.01% and 25% of hydrogen gas (H₂).
The method of claim 1, wherein the solid boron-containing precursor is supported above the continuous growth substrate.
The method of claim 1, wherein the solid boron-containing precursor is supported below the continuous growth substrate.
The method of claim 1, wherein the solid boron-containing precursor is supported laterally adjacent to the continuous growth substrate.
The method of claim 1, wherein the solid boron precursor includes elemental boron (B), boron oxide (B₂O₃), or boron carbide (B₄C).
The method of claim 1, wherein the solid boron-containing precursor includes metal borides such as iron borides (FexB), nickel boride (NixB) and magnesium diboride (MgB₂).
A method of synthesizing hexagonal boron nitride, the method comprising: positioning a solid boron-containing precursor and a growth substrate within a chemical vapor deposition chamber, wherein the solid boron-containing precursor includes boron powders, boron fragments, or boron platelets and does not directly contact the growth substrate, and wherein the growth substrate includes nickel, iron, copper, chromium, or alloys thereof; heating an interior of the chemical vapor deposition chamber to between 800° C. and 1200° C., inclusive; and flowing a nitrogen-containing reaction gas mixture into the chemical vapor deposition chamber, the reaction gas mixture including a nitrogen compound and hydro-gen gas; wherein the reaction gas mixture is pressurized between 10 mTorr and 800 Torr, inclusive, wherein the growth substrate reacts with boron released from the solid boron-containing precursor and the nitrogen compound to form a single-layer or multi-layer hexagonal boron nitride film, and wherein the growth substrate com-prises a film having a thickness of between 0.1 µm and 5.0 µm, inclusive.
A method of synthesizing hexagonal boron nitride, the method comprising: positioning a solid boron-containing precursor and a growth substrate within a chemical vapor deposition chamber, wherein the solid boron-containing precursor includes boron powders, boron fragments, or boron platelets and does not directly contact the growth substrate, and wherein the growth substrate includes nickel, iron, copper, chromium, or alloys thereof; heating an interior of the chemical vapor deposition chamber to between 800° C. and 1200° C., inclusive; and flowing a nitrogen-containing reaction gas mixture into the chemical vapor deposition chamber, the reaction gas mixture including a nitrogen compound and hydro-gen gas; wherein the reaction gas mixture is pressurized between 10 mTorr and 800 Torr, inclusive, wherein the growth substrate reacts with boron released from the solid boron-containing precursor and the nitrogen compound to form a single-layer or multi-layer hexagonal boron nitride film, and wherein the growth substrate com-prises a foil having a thickness of between 5.0 µm and 150 µm, inclusive.
A method of synthesizing hexagonal boron nitride, the method comprising: positioning a solid boron-containing precursor and a growth substrate within a chemical vapor deposition chamber, wherein the solid boron-containing precursor includes boron powders, boron fragments, or boron platelets and does not directly contact the growth substrate, and wherein the growth substrate includes nickel, iron, copper, chromium, or alloys thereof; heating an interior of the chemical vapor deposition chamber to between 800° C. and 1200° C., inclusive; and flowing a nitrogen-containing reaction gas mixture into the chemical vapor deposition chamber, the reaction gas mixture including a nitrogen compound and hydro-gen gas; wherein the reaction gas mixture is pressurized between 10 mTorr and 800 Torr, inclusive, wherein the growth substrate reacts with boron released from the solid boron-containing precursor and the nitrogen compound to form a single-layer or multi-layer hexagonal boron nitride film, and wherein the growth substrate com-prises a sheet having a thickness of between 0.15 mm and 5 mm, inclusive.
A method of synthesizing hexagonal boron nitride, the method comprising: positioning a solid boron-containing precursor and a growth substrate within a chemical vapor deposition chamber, wherein the solid boron-containing precursor includes boron powders, boron fragments, or boron platelets and does not directly contact the growth substrate, and wherein the growth substrate includes nickel, iron, copper, chromium, or alloys thereof; heating an interior of the chemical vapor deposition chamber to between 800° C. and 1200° C., inclusive; and flowing a nitrogen-containing reaction gas mixture into the chemical vapor deposition chamber, the reaction gas mixture including a nitrogen compound and hydro-gen gas; wherein the reaction gas mixture is pressurized between 10 mTorr and 800 Torr, inclusive, wherein the growth substrate reacts with boron released from the solid boron-containing precursor and the nitrogen compound to form a single-layer or multi-layer hexagonal boron nitride film, and wherein the growth substrate com-prises a plate having a thickness of between 5 mm and 100 mm, inclusive.
A method of synthesizing hexagonal boron nitride, the method comprising: positioning a solid boron-containing precursor and a growth substrate within a chemical vapor deposition chamber, wherein the solid boron-containing precursor includes boron powders, boron fragments, or boron platelets and does not directly contact the growth substrate, and wherein the growth substrate includes nickel, iron, copper, chromium, or alloys thereof; heating an interior of the chemical vapor deposition chamber to between 800° C. and 1200° C., inclusive; and flowing a nitrogen-containing reaction gas mixture into the chemical vapor deposition chamber, the reaction gas mixture including a nitrogen compound and hydro-gen gas; wherein the reaction gas mixture is pressurized between 10 mTorr and 800 Torr, inclusive, wherein the growth substrate reacts with boron released from the solid boron-containing precursor and the nitrogen compound to form a single-layer or multi-layer hexagonal boron nitride film, and wherein the growth substrate com-prises includes a three-dimensional geometry including at least one of nails, tubes, and ball bearings.
A method of synthesizing boron nitride nanotubes, the method comprising: positioning a solid boron-containing precursor and metal-lic nanoparticles within a chemical vapor deposition chamber, wherein the solid boron-containing precursor includes boron powders, boron fragments, or boron platelets and does not directly contact the metallic nanotubes, and wherein the metallic nanoparticles include nickel, iron, copper, chromium, or alloys thereof; heating an interior of the chemical vapor deposition chamber to between 800° C. and 1200° C., inclusive; and flowing a nitrogen-containing reaction gas mixture into the chemical vapor deposition chamber, the reaction gas mixture including a nitrogen compound and hydro-gen gas; wherein the reaction gas mixture is pressurized between 10 mTorr and 800 Torr, inclusive, and wherein the metallic nanotubes react with boron released from the solid boron-containing precursor and the nitrogen com-pound to form boron nitride nanotubes.
The method of claim 15, further including forming the metallic nanotubes by dewetting a metallic film having a thickness less than 100 nm at a temperature greater than 800° C.
The method of claim 15, wherein the boron nitride nanotubes have a mean diameter of between 0.5 nm and 100 nm, inclusive.
The method of claim 15, wherein the nitrogen com-pound comprises molecular nitrogen (N₂).
The method of claim 15, wherein the nitrogen com-pound comprises ammonia (NH₃).
The method of claim 15, wherein the reaction gas mixture includes a concentration of between 0.01% and 25% of hydrogen gas (H₂).
The method of claim 15, wherein the reaction gas mixture includes an inert gas and wherein the reaction gas mixture is maintained at atmospheric pressure.
The method of claim 15, wherein the solid boron-containing precursor is supported above the metallic nan-oparticles.
The method of claim 15, wherein the solid boron-containing precursor is supported below the metallic nan-oparticles.
The method of claim 15, wherein the solid boron-containing precursor is supported laterally adjacent to the metallic nanoparticles.
The method of claim 15, wherein the reaction mixture includes a ratio of a partial pressure of nitrogen and a partial pressure of hydrogen of at least 30. ∗ ∗ ∗ ∗ ∗
Layer stacks claimed or described, ordered top of device to substrate.
boron nitride nanotubes
Materials described outside the worked examples.
solid boron-containing precursor (boron powders, boron fragments, or boron platelets)
growth substrate (nickel, iron, copper, chromium, or alloys thereof)
hexagonal boron nitride film (single-layer or multi-layer)
hBN
hydrogen gas
H₂
molecular nitrogen
N₂
ammonia
NH₃
elemental boron
B
boron oxide
B₂O₃
boron carbide
B₄C
iron borides
FexB
nickel boride
NixB
magnesium diboride
MgB₂
boron nitride nanotubes
BN
metallic nanoparticles (nickel, iron, copper, chromium, or alloys thereof)
argon (inert/buffer gas)
Ar
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
FIG. 2 includes a characteristic Raman spectra of hBN synthesized in accordance with the method of the present invention.
FIG. 3 includes characteristic SEM images of hBN mul- tilayer (top) and monolayer (bottom) synthesized in accor- 5 dance with the method of the present …
FIG. 4 includes a characteristic XRD graph of hBN grown on Fe foil in accordance with a non-limiting example of the present invention.
FIG. 4 includes a characteristic XRD graph of hBN grown on Fe foil in accordance with a non-limiting example of the present invention.
FIG. 5 includes SEM images of BN nanotubes grown in 10 accordance with the present invention using solid boron and molecular nitrogen and hydrogen as …
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Temperature | 800–1200 °C | — |
Thickness | 0.1–5 µm | — |
Thickness | 5–150 µm | — |
Thickness | 0.15–5 mm | — |
Thickness | 0.1–1000 µm | — |
Thickness | 1–100 mm | — |
Pressure | 0.01–800 Torr | — |
Thickness | 0.5–100 nm | — |
Thickness | 5–100 mm | — |
Duration | 30–60 minutes | — |
Thickness | 0.3–1 µm | — |
Thickness | ≤ 1 nm | — |
Thickness | ≥ 5 mm | — |
Temperature | ≥ 800 °C | — |
Duration | ≤ 120 minutes | — |
Patents and literature cited by this patent (applicant and examiner references).
Cited patents · 11
Cited non-patent literature · 2
Related documents with shared materials, methods, properties, or citations.
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