Patent
US 11,133,185Patent
Atlas literature
Patent
US 11,133,185Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 2. Step 4. Transferring the 1 u m GaN film onto a silicon substrate. 4a) A thermal release tape was slowly adhered to an upper surface of the GaN epitaxial …
FIG. 3. Example 2, transferring 2 u m GaN grown on four-layer graphene to a flexible PET substrate. Step A. Growing graphene on a copper foil by CVD method. The …
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
An epitaxial lift-off process for graphene-based gallium nitride (GaN), comprising the following steps: (1) growing graphene on a well-polished copper foil: (la) folding a well-polished copper foil into a moderate-sized purse, putting the purse in a quartz boat, pushing the boat to a constant temperature zone in the middle of a quartz tube, and turning on a vacuum pump to vacuumize to 0.6-2 Pa; (l b) introducing 20-25 s cc m H 2 into the quartz tube, while heating the quartz tube; introducing both 20-25 s cc m H 2 and 700-720 s cc m Ar into the quartz tube when reaching a temperature of 700 ° C, and continuing heating until the quartz tube reaches a temperature of 1,045-1,050 °C; (1c) holding the temperature, closing all inlet valves, and vacuumizing the quartz tube to 0.6-2 Pa with the vacuum pump; (1 d) holding the temperature, introducing 2 s ccm 02 into the quartz tube, and maintaining for 2 min; (le) holding the temperature, closing all inlet valves, and vacuumizing the quartz tube to around 1 Pa with the vacuum pump; (i f) holding the temperature, introducing both 100 s cc m H 2 and 700 s cc m Ar, and maintaining for 60 m in; (1 g) holding the temperature, closing an Ar gas valve, introducing both 0.1-1 s cc m CH₄ and 400-600 s cc m H 2, and maintaining for 60 m in; and (1 h) maintaining the fl ow rates of H 2 and CH4, rapidly cooling down the quartz tube to room temperature, and removing the graphene grown on the copper foil, which is 0.34 nm thick; (2) transferring the graphene grown on the copper foil onto a sapphire substrate: (2a) manually coating a layer of polymethyl methacrylate (PMMA) fi lm on the surface of the graphene-grown copper foil, and spin-coating PMMA uniformly with a spin coater, to obtain a copper foil spin-coated with PMMA; (2b) placing the copper foil spin-coated with PMMA on a heating stage, setting a temperature thereof at 50-70 ° C, and drying for 20 m in to cure the PMMA fi lm; (2c) cutting the PMMA-cured copper foil into a plurality of small sheets of equivalent size and soaking in 64-68 g/L ammonium persulfate solution; with a graphene side facing upward, dipping for 4-12 h, and removing a metal substrate, to obtain a plurality of monolayer graphene fi lms with PMMA; (2d) using a clean glass sheet to transfer a plurality of PMMA/graphene sheets from the ammonium persulfate solution into deionized water; after soaking for 30 m in, using a sapphire substrate to pull out one of the small PMMA/monolayer graphene sheets therefrom, to obtain a sapphire substrate coated with PMMA/monolayer graphene; (2e) adding 100-200 ml of acetone solution into a glass container, and immersing the PMMA/monolayer graphene/substrate thoroughly for 12-24 h to dissolve and remove PMMA fully, to obtain a PMMA-free monolayer graphene/substrate; (2f) transferring the PMMA-free monolayer graphene/substrate from the acetone solution into an ethanol solution to be allowed to stand for 30 m in, pulling out the monolayer graphene/substrate subsequently, and air-drying to complete the transfer of the monolayer graphene; and (2g) using a monolayer graphene-transferred sapphire substrate to pull out a second PMMA/monolayer graphene fi lm, to obtain a substrate coated with PMMA/bilayer graphene; repeating steps (2e) to (2f) to complete the transfer of the second layer of graphene; similarly, pulling out the third to the fi nal PMMA/graphene fi lms to complete the transfer of the third to the fi nal layers of graphene fi lms; (3) growing GaN epitaxial layer by the metal organic chemical vapor deposition (MOCVD) method (3a) placing the graphene-transferred substrate in a reaction chamber and introducing ammonia thereinto; heating the reaction chamber to 900 0 C, and adjusting the pressure of the reaction chamber to 300 mbar; (3b) maintaining the reaction chamber at a constant pressure, heating the reaction chamber to a temperature of 1,1 00 0 C, and simultaneously introducing H 2, ammonia, and Ga source thereinto, wherein fl ow rates of the three gases are 800-1,000 s c cm, 9,600-10,500 s c cm, and 230-260 s c cm, respectively; using the MOCVD method, growing 1-3 um GaN on the graphene-transferred substrate; and (3d) removing a sample after cooling down the reaction chamber to room temperature, to obtain GaN grown on the graphene; (4) lifting off the GaN epitaxial layer: (4a) slowly adhering a thermal release tape to an upper surface of the GaN epitaxial layer, applying a uniform force to lift the tape having the GaN epitaxial layer adhered thereto off the original substrate completely; (4b) adhering the GaN-adhered side of the thermal release tape to a target substrate tightly, heating the heating stage to 120 0 C, subsequently placing the target substrate on the heating stage wholly, and heating for 5 m in, wherein, the thermal release tape loses viscosity after foaming and will spontaneously lift off the surface of GaN; and (4c) removing the lift-off tape using tweezers, and leaving the GaN epitaxial layer on the target substrate to realize the lift-off and transfer of the GaN epitaxial layer.
The process according to claim 1, wherein spin-coating PMMA uniformly with the spin coater in step (2a) is realized by adjusting the rotational speed of the spin coater, i.e., se tt ing the rotational speed of the spin coater at 1,000 rps for low-speed spinning for 30 s, followed by increasing the rotational speed to 3,000 rps for spinning for 60 s.
The process according to claim 1 wherein 2 to 6 graphene sheets are cut in step (2c).
The process according to claim 1, w herein the sapphire substrate in step (2d) is 0. 43- 0. 5 mm thick.
The process according to claim 1. w herein 2 to 6 graphene layers are t ransferred in step (2g).
The process according to claim 1, w herein the target substrate in step (4b) may be any one of silicon substrate, flexible PET substrate, and diamond substrate.
Embodiments described in the patent, grouped by the materials and process steps they use.
7 materials3 process steps
Transferring 1 µm thick GaN grown on bilayer graphene to a silicon substrate. Graphene grown by CVD on copper foil, bilayer graphene transferred to sapphire substrate using PMMA-assisted wet transfer with ammonium persulfate etching, 1 µm GaN grown by MOCVD at 1100°C and 300 mbar for 35 min, then GaN lifted off and transferred to silicon substrate using thermal release tape at 120°C.
7 materials3 process steps
Transferring 2 µm GaN grown on four-layer graphene to a flexible PET substrate. Graphene grown by CVD on copper foil (same as Example 1), four-layer graphene transferred to sapphire substrate using PMMA-assisted wet transfer, 2 µm GaN grown by MOCVD at 1100°C and 300 mbar for 70 min, then GaN lifted off and transferred to flexible PET substrate using thermal release tape at 120°C.
7 materials3 process steps
Transferring 3 µm GaN grown on six-layer graphene to a diamond substrate. Graphene grown by CVD on copper foil (same as Example 1), six-layer graphene transferred to sapphire substrate using PMMA-assisted wet transfer, 3 µm GaN grown by MOCVD, then GaN lifted off and transferred to diamond substrate using thermal release tape.
Layer stacks claimed or described, ordered top of device to substrate.
GaN epitaxial layer on graphene-transferred sapphire substrate
Materials described outside the worked examples.
thermal release tape
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
graphene monolayer thickness | 0.34 nm | C |
GaN epitaxial layer thickness range |
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 11,133,185Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 2. Step 4. Transferring the 1 u m GaN film onto a silicon substrate. 4a) A thermal release tape was slowly adhered to an upper surface of the GaN epitaxial …
FIG. 3. Example 2, transferring 2 u m GaN grown on four-layer graphene to a flexible PET substrate. Step A. Growing graphene on a copper foil by CVD method. The …
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
An epitaxial lift-off process for graphene-based gallium nitride (GaN), comprising the following steps: (1) growing graphene on a well-polished copper foil: (la) folding a well-polished copper foil into a moderate-sized purse, putting the purse in a quartz boat, pushing the boat to a constant temperature zone in the middle of a quartz tube, and turning on a vacuum pump to vacuumize to 0.6-2 Pa; (l b) introducing 20-25 s cc m H 2 into the quartz tube, while heating the quartz tube; introducing both 20-25 s cc m H 2 and 700-720 s cc m Ar into the quartz tube when reaching a temperature of 700 ° C, and continuing heating until the quartz tube reaches a temperature of 1,045-1,050 °C; (1c) holding the temperature, closing all inlet valves, and vacuumizing the quartz tube to 0.6-2 Pa with the vacuum pump; (1 d) holding the temperature, introducing 2 s ccm 02 into the quartz tube, and maintaining for 2 min; (le) holding the temperature, closing all inlet valves, and vacuumizing the quartz tube to around 1 Pa with the vacuum pump; (i f) holding the temperature, introducing both 100 s cc m H 2 and 700 s cc m Ar, and maintaining for 60 m in; (1 g) holding the temperature, closing an Ar gas valve, introducing both 0.1-1 s cc m CH₄ and 400-600 s cc m H 2, and maintaining for 60 m in; and (1 h) maintaining the fl ow rates of H 2 and CH4, rapidly cooling down the quartz tube to room temperature, and removing the graphene grown on the copper foil, which is 0.34 nm thick; (2) transferring the graphene grown on the copper foil onto a sapphire substrate: (2a) manually coating a layer of polymethyl methacrylate (PMMA) fi lm on the surface of the graphene-grown copper foil, and spin-coating PMMA uniformly with a spin coater, to obtain a copper foil spin-coated with PMMA; (2b) placing the copper foil spin-coated with PMMA on a heating stage, setting a temperature thereof at 50-70 ° C, and drying for 20 m in to cure the PMMA fi lm; (2c) cutting the PMMA-cured copper foil into a plurality of small sheets of equivalent size and soaking in 64-68 g/L ammonium persulfate solution; with a graphene side facing upward, dipping for 4-12 h, and removing a metal substrate, to obtain a plurality of monolayer graphene fi lms with PMMA; (2d) using a clean glass sheet to transfer a plurality of PMMA/graphene sheets from the ammonium persulfate solution into deionized water; after soaking for 30 m in, using a sapphire substrate to pull out one of the small PMMA/monolayer graphene sheets therefrom, to obtain a sapphire substrate coated with PMMA/monolayer graphene; (2e) adding 100-200 ml of acetone solution into a glass container, and immersing the PMMA/monolayer graphene/substrate thoroughly for 12-24 h to dissolve and remove PMMA fully, to obtain a PMMA-free monolayer graphene/substrate; (2f) transferring the PMMA-free monolayer graphene/substrate from the acetone solution into an ethanol solution to be allowed to stand for 30 m in, pulling out the monolayer graphene/substrate subsequently, and air-drying to complete the transfer of the monolayer graphene; and (2g) using a monolayer graphene-transferred sapphire substrate to pull out a second PMMA/monolayer graphene fi lm, to obtain a substrate coated with PMMA/bilayer graphene; repeating steps (2e) to (2f) to complete the transfer of the second layer of graphene; similarly, pulling out the third to the fi nal PMMA/graphene fi lms to complete the transfer of the third to the fi nal layers of graphene fi lms; (3) growing GaN epitaxial layer by the metal organic chemical vapor deposition (MOCVD) method (3a) placing the graphene-transferred substrate in a reaction chamber and introducing ammonia thereinto; heating the reaction chamber to 900 0 C, and adjusting the pressure of the reaction chamber to 300 mbar; (3b) maintaining the reaction chamber at a constant pressure, heating the reaction chamber to a temperature of 1,1 00 0 C, and simultaneously introducing H 2, ammonia, and Ga source thereinto, wherein fl ow rates of the three gases are 800-1,000 s c cm, 9,600-10,500 s c cm, and 230-260 s c cm, respectively; using the MOCVD method, growing 1-3 um GaN on the graphene-transferred substrate; and (3d) removing a sample after cooling down the reaction chamber to room temperature, to obtain GaN grown on the graphene; (4) lifting off the GaN epitaxial layer: (4a) slowly adhering a thermal release tape to an upper surface of the GaN epitaxial layer, applying a uniform force to lift the tape having the GaN epitaxial layer adhered thereto off the original substrate completely; (4b) adhering the GaN-adhered side of the thermal release tape to a target substrate tightly, heating the heating stage to 120 0 C, subsequently placing the target substrate on the heating stage wholly, and heating for 5 m in, wherein, the thermal release tape loses viscosity after foaming and will spontaneously lift off the surface of GaN; and (4c) removing the lift-off tape using tweezers, and leaving the GaN epitaxial layer on the target substrate to realize the lift-off and transfer of the GaN epitaxial layer.
The process according to claim 1, wherein spin-coating PMMA uniformly with the spin coater in step (2a) is realized by adjusting the rotational speed of the spin coater, i.e., se tt ing the rotational speed of the spin coater at 1,000 rps for low-speed spinning for 30 s, followed by increasing the rotational speed to 3,000 rps for spinning for 60 s.
The process according to claim 1 wherein 2 to 6 graphene sheets are cut in step (2c).
The process according to claim 1, w herein the sapphire substrate in step (2d) is 0. 43- 0. 5 mm thick.
The process according to claim 1. w herein 2 to 6 graphene layers are t ransferred in step (2g).
The process according to claim 1, w herein the target substrate in step (4b) may be any one of silicon substrate, flexible PET substrate, and diamond substrate.
Embodiments described in the patent, grouped by the materials and process steps they use.
7 materials3 process steps
Transferring 1 µm thick GaN grown on bilayer graphene to a silicon substrate. Graphene grown by CVD on copper foil, bilayer graphene transferred to sapphire substrate using PMMA-assisted wet transfer with ammonium persulfate etching, 1 µm GaN grown by MOCVD at 1100°C and 300 mbar for 35 min, then GaN lifted off and transferred to silicon substrate using thermal release tape at 120°C.
7 materials3 process steps
Transferring 2 µm GaN grown on four-layer graphene to a flexible PET substrate. Graphene grown by CVD on copper foil (same as Example 1), four-layer graphene transferred to sapphire substrate using PMMA-assisted wet transfer, 2 µm GaN grown by MOCVD at 1100°C and 300 mbar for 70 min, then GaN lifted off and transferred to flexible PET substrate using thermal release tape at 120°C.
7 materials3 process steps
Transferring 3 µm GaN grown on six-layer graphene to a diamond substrate. Graphene grown by CVD on copper foil (same as Example 1), six-layer graphene transferred to sapphire substrate using PMMA-assisted wet transfer, 3 µm GaN grown by MOCVD, then GaN lifted off and transferred to diamond substrate using thermal release tape.
Layer stacks claimed or described, ordered top of device to substrate.
GaN epitaxial layer on graphene-transferred sapphire substrate
Materials described outside the worked examples.
thermal release tape
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
graphene monolayer thickness | 0.34 nm | C |
GaN epitaxial layer thickness range |
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 11,133,185Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 2. Step 4. Transferring the 1 u m GaN film onto a silicon substrate. 4a) A thermal release tape was slowly adhered to an upper surface of the GaN epitaxial …
FIG. 3. Example 2, transferring 2 u m GaN grown on four-layer graphene to a flexible PET substrate. Step A. Growing graphene on a copper foil by CVD method. The …
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
An epitaxial lift-off process for graphene-based gallium nitride (GaN), comprising the following steps: (1) growing graphene on a well-polished copper foil: (la) folding a well-polished copper foil into a moderate-sized purse, putting the purse in a quartz boat, pushing the boat to a constant temperature zone in the middle of a quartz tube, and turning on a vacuum pump to vacuumize to 0.6-2 Pa; (l b) introducing 20-25 s cc m H 2 into the quartz tube, while heating the quartz tube; introducing both 20-25 s cc m H 2 and 700-720 s cc m Ar into the quartz tube when reaching a temperature of 700 ° C, and continuing heating until the quartz tube reaches a temperature of 1,045-1,050 °C; (1c) holding the temperature, closing all inlet valves, and vacuumizing the quartz tube to 0.6-2 Pa with the vacuum pump; (1 d) holding the temperature, introducing 2 s ccm 02 into the quartz tube, and maintaining for 2 min; (le) holding the temperature, closing all inlet valves, and vacuumizing the quartz tube to around 1 Pa with the vacuum pump; (i f) holding the temperature, introducing both 100 s cc m H 2 and 700 s cc m Ar, and maintaining for 60 m in; (1 g) holding the temperature, closing an Ar gas valve, introducing both 0.1-1 s cc m CH₄ and 400-600 s cc m H 2, and maintaining for 60 m in; and (1 h) maintaining the fl ow rates of H 2 and CH4, rapidly cooling down the quartz tube to room temperature, and removing the graphene grown on the copper foil, which is 0.34 nm thick; (2) transferring the graphene grown on the copper foil onto a sapphire substrate: (2a) manually coating a layer of polymethyl methacrylate (PMMA) fi lm on the surface of the graphene-grown copper foil, and spin-coating PMMA uniformly with a spin coater, to obtain a copper foil spin-coated with PMMA; (2b) placing the copper foil spin-coated with PMMA on a heating stage, setting a temperature thereof at 50-70 ° C, and drying for 20 m in to cure the PMMA fi lm; (2c) cutting the PMMA-cured copper foil into a plurality of small sheets of equivalent size and soaking in 64-68 g/L ammonium persulfate solution; with a graphene side facing upward, dipping for 4-12 h, and removing a metal substrate, to obtain a plurality of monolayer graphene fi lms with PMMA; (2d) using a clean glass sheet to transfer a plurality of PMMA/graphene sheets from the ammonium persulfate solution into deionized water; after soaking for 30 m in, using a sapphire substrate to pull out one of the small PMMA/monolayer graphene sheets therefrom, to obtain a sapphire substrate coated with PMMA/monolayer graphene; (2e) adding 100-200 ml of acetone solution into a glass container, and immersing the PMMA/monolayer graphene/substrate thoroughly for 12-24 h to dissolve and remove PMMA fully, to obtain a PMMA-free monolayer graphene/substrate; (2f) transferring the PMMA-free monolayer graphene/substrate from the acetone solution into an ethanol solution to be allowed to stand for 30 m in, pulling out the monolayer graphene/substrate subsequently, and air-drying to complete the transfer of the monolayer graphene; and (2g) using a monolayer graphene-transferred sapphire substrate to pull out a second PMMA/monolayer graphene fi lm, to obtain a substrate coated with PMMA/bilayer graphene; repeating steps (2e) to (2f) to complete the transfer of the second layer of graphene; similarly, pulling out the third to the fi nal PMMA/graphene fi lms to complete the transfer of the third to the fi nal layers of graphene fi lms; (3) growing GaN epitaxial layer by the metal organic chemical vapor deposition (MOCVD) method (3a) placing the graphene-transferred substrate in a reaction chamber and introducing ammonia thereinto; heating the reaction chamber to 900 0 C, and adjusting the pressure of the reaction chamber to 300 mbar; (3b) maintaining the reaction chamber at a constant pressure, heating the reaction chamber to a temperature of 1,1 00 0 C, and simultaneously introducing H 2, ammonia, and Ga source thereinto, wherein fl ow rates of the three gases are 800-1,000 s c cm, 9,600-10,500 s c cm, and 230-260 s c cm, respectively; using the MOCVD method, growing 1-3 um GaN on the graphene-transferred substrate; and (3d) removing a sample after cooling down the reaction chamber to room temperature, to obtain GaN grown on the graphene; (4) lifting off the GaN epitaxial layer: (4a) slowly adhering a thermal release tape to an upper surface of the GaN epitaxial layer, applying a uniform force to lift the tape having the GaN epitaxial layer adhered thereto off the original substrate completely; (4b) adhering the GaN-adhered side of the thermal release tape to a target substrate tightly, heating the heating stage to 120 0 C, subsequently placing the target substrate on the heating stage wholly, and heating for 5 m in, wherein, the thermal release tape loses viscosity after foaming and will spontaneously lift off the surface of GaN; and (4c) removing the lift-off tape using tweezers, and leaving the GaN epitaxial layer on the target substrate to realize the lift-off and transfer of the GaN epitaxial layer.
The process according to claim 1, wherein spin-coating PMMA uniformly with the spin coater in step (2a) is realized by adjusting the rotational speed of the spin coater, i.e., se tt ing the rotational speed of the spin coater at 1,000 rps for low-speed spinning for 30 s, followed by increasing the rotational speed to 3,000 rps for spinning for 60 s.
The process according to claim 1 wherein 2 to 6 graphene sheets are cut in step (2c).
The process according to claim 1, w herein the sapphire substrate in step (2d) is 0. 43- 0. 5 mm thick.
The process according to claim 1. w herein 2 to 6 graphene layers are t ransferred in step (2g).
The process according to claim 1, w herein the target substrate in step (4b) may be any one of silicon substrate, flexible PET substrate, and diamond substrate.
Embodiments described in the patent, grouped by the materials and process steps they use.
7 materials3 process steps
Transferring 1 µm thick GaN grown on bilayer graphene to a silicon substrate. Graphene grown by CVD on copper foil, bilayer graphene transferred to sapphire substrate using PMMA-assisted wet transfer with ammonium persulfate etching, 1 µm GaN grown by MOCVD at 1100°C and 300 mbar for 35 min, then GaN lifted off and transferred to silicon substrate using thermal release tape at 120°C.
7 materials3 process steps
Transferring 2 µm GaN grown on four-layer graphene to a flexible PET substrate. Graphene grown by CVD on copper foil (same as Example 1), four-layer graphene transferred to sapphire substrate using PMMA-assisted wet transfer, 2 µm GaN grown by MOCVD at 1100°C and 300 mbar for 70 min, then GaN lifted off and transferred to flexible PET substrate using thermal release tape at 120°C.
7 materials3 process steps
Transferring 3 µm GaN grown on six-layer graphene to a diamond substrate. Graphene grown by CVD on copper foil (same as Example 1), six-layer graphene transferred to sapphire substrate using PMMA-assisted wet transfer, 3 µm GaN grown by MOCVD, then GaN lifted off and transferred to diamond substrate using thermal release tape.
Layer stacks claimed or described, ordered top of device to substrate.
GaN epitaxial layer on graphene-transferred sapphire substrate
Materials described outside the worked examples.
thermal release tape
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
graphene monolayer thickness | 0.34 nm | C |
GaN epitaxial layer thickness range |
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 11,133,185Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 2. Step 4. Transferring the 1 u m GaN film onto a silicon substrate. 4a) A thermal release tape was slowly adhered to an upper surface of the GaN epitaxial …
FIG. 3. Example 2, transferring 2 u m GaN grown on four-layer graphene to a flexible PET substrate. Step A. Growing graphene on a copper foil by CVD method. The …
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
An epitaxial lift-off process for graphene-based gallium nitride (GaN), comprising the following steps: (1) growing graphene on a well-polished copper foil: (la) folding a well-polished copper foil into a moderate-sized purse, putting the purse in a quartz boat, pushing the boat to a constant temperature zone in the middle of a quartz tube, and turning on a vacuum pump to vacuumize to 0.6-2 Pa; (l b) introducing 20-25 s cc m H 2 into the quartz tube, while heating the quartz tube; introducing both 20-25 s cc m H 2 and 700-720 s cc m Ar into the quartz tube when reaching a temperature of 700 ° C, and continuing heating until the quartz tube reaches a temperature of 1,045-1,050 °C; (1c) holding the temperature, closing all inlet valves, and vacuumizing the quartz tube to 0.6-2 Pa with the vacuum pump; (1 d) holding the temperature, introducing 2 s ccm 02 into the quartz tube, and maintaining for 2 min; (le) holding the temperature, closing all inlet valves, and vacuumizing the quartz tube to around 1 Pa with the vacuum pump; (i f) holding the temperature, introducing both 100 s cc m H 2 and 700 s cc m Ar, and maintaining for 60 m in; (1 g) holding the temperature, closing an Ar gas valve, introducing both 0.1-1 s cc m CH₄ and 400-600 s cc m H 2, and maintaining for 60 m in; and (1 h) maintaining the fl ow rates of H 2 and CH4, rapidly cooling down the quartz tube to room temperature, and removing the graphene grown on the copper foil, which is 0.34 nm thick; (2) transferring the graphene grown on the copper foil onto a sapphire substrate: (2a) manually coating a layer of polymethyl methacrylate (PMMA) fi lm on the surface of the graphene-grown copper foil, and spin-coating PMMA uniformly with a spin coater, to obtain a copper foil spin-coated with PMMA; (2b) placing the copper foil spin-coated with PMMA on a heating stage, setting a temperature thereof at 50-70 ° C, and drying for 20 m in to cure the PMMA fi lm; (2c) cutting the PMMA-cured copper foil into a plurality of small sheets of equivalent size and soaking in 64-68 g/L ammonium persulfate solution; with a graphene side facing upward, dipping for 4-12 h, and removing a metal substrate, to obtain a plurality of monolayer graphene fi lms with PMMA; (2d) using a clean glass sheet to transfer a plurality of PMMA/graphene sheets from the ammonium persulfate solution into deionized water; after soaking for 30 m in, using a sapphire substrate to pull out one of the small PMMA/monolayer graphene sheets therefrom, to obtain a sapphire substrate coated with PMMA/monolayer graphene; (2e) adding 100-200 ml of acetone solution into a glass container, and immersing the PMMA/monolayer graphene/substrate thoroughly for 12-24 h to dissolve and remove PMMA fully, to obtain a PMMA-free monolayer graphene/substrate; (2f) transferring the PMMA-free monolayer graphene/substrate from the acetone solution into an ethanol solution to be allowed to stand for 30 m in, pulling out the monolayer graphene/substrate subsequently, and air-drying to complete the transfer of the monolayer graphene; and (2g) using a monolayer graphene-transferred sapphire substrate to pull out a second PMMA/monolayer graphene fi lm, to obtain a substrate coated with PMMA/bilayer graphene; repeating steps (2e) to (2f) to complete the transfer of the second layer of graphene; similarly, pulling out the third to the fi nal PMMA/graphene fi lms to complete the transfer of the third to the fi nal layers of graphene fi lms; (3) growing GaN epitaxial layer by the metal organic chemical vapor deposition (MOCVD) method (3a) placing the graphene-transferred substrate in a reaction chamber and introducing ammonia thereinto; heating the reaction chamber to 900 0 C, and adjusting the pressure of the reaction chamber to 300 mbar; (3b) maintaining the reaction chamber at a constant pressure, heating the reaction chamber to a temperature of 1,1 00 0 C, and simultaneously introducing H 2, ammonia, and Ga source thereinto, wherein fl ow rates of the three gases are 800-1,000 s c cm, 9,600-10,500 s c cm, and 230-260 s c cm, respectively; using the MOCVD method, growing 1-3 um GaN on the graphene-transferred substrate; and (3d) removing a sample after cooling down the reaction chamber to room temperature, to obtain GaN grown on the graphene; (4) lifting off the GaN epitaxial layer: (4a) slowly adhering a thermal release tape to an upper surface of the GaN epitaxial layer, applying a uniform force to lift the tape having the GaN epitaxial layer adhered thereto off the original substrate completely; (4b) adhering the GaN-adhered side of the thermal release tape to a target substrate tightly, heating the heating stage to 120 0 C, subsequently placing the target substrate on the heating stage wholly, and heating for 5 m in, wherein, the thermal release tape loses viscosity after foaming and will spontaneously lift off the surface of GaN; and (4c) removing the lift-off tape using tweezers, and leaving the GaN epitaxial layer on the target substrate to realize the lift-off and transfer of the GaN epitaxial layer.
The process according to claim 1, wherein spin-coating PMMA uniformly with the spin coater in step (2a) is realized by adjusting the rotational speed of the spin coater, i.e., se tt ing the rotational speed of the spin coater at 1,000 rps for low-speed spinning for 30 s, followed by increasing the rotational speed to 3,000 rps for spinning for 60 s.
The process according to claim 1 wherein 2 to 6 graphene sheets are cut in step (2c).
The process according to claim 1, w herein the sapphire substrate in step (2d) is 0. 43- 0. 5 mm thick.
The process according to claim 1. w herein 2 to 6 graphene layers are t ransferred in step (2g).
The process according to claim 1, w herein the target substrate in step (4b) may be any one of silicon substrate, flexible PET substrate, and diamond substrate.
Embodiments described in the patent, grouped by the materials and process steps they use.
7 materials3 process steps
Transferring 1 µm thick GaN grown on bilayer graphene to a silicon substrate. Graphene grown by CVD on copper foil, bilayer graphene transferred to sapphire substrate using PMMA-assisted wet transfer with ammonium persulfate etching, 1 µm GaN grown by MOCVD at 1100°C and 300 mbar for 35 min, then GaN lifted off and transferred to silicon substrate using thermal release tape at 120°C.
7 materials3 process steps
Transferring 2 µm GaN grown on four-layer graphene to a flexible PET substrate. Graphene grown by CVD on copper foil (same as Example 1), four-layer graphene transferred to sapphire substrate using PMMA-assisted wet transfer, 2 µm GaN grown by MOCVD at 1100°C and 300 mbar for 70 min, then GaN lifted off and transferred to flexible PET substrate using thermal release tape at 120°C.
7 materials3 process steps
Transferring 3 µm GaN grown on six-layer graphene to a diamond substrate. Graphene grown by CVD on copper foil (same as Example 1), six-layer graphene transferred to sapphire substrate using PMMA-assisted wet transfer, 3 µm GaN grown by MOCVD, then GaN lifted off and transferred to diamond substrate using thermal release tape.
Layer stacks claimed or described, ordered top of device to substrate.
GaN epitaxial layer on graphene-transferred sapphire substrate
Materials described outside the worked examples.
thermal release tape
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
graphene monolayer thickness | 0.34 nm | C |
GaN epitaxial layer thickness range |
Related documents with shared materials, methods, properties, or citations.
| 1–3 µm |
GaN |
GaN thickness Example 1 | 1 µm | GaN |
GaN thickness Example 2 | 2 µm | GaN |
GaN thickness Example 3 | 3 µm | GaN |
sapphire substrate thickness range | 0.43–0.5 mm | Al₂O₃ |
Pressure | 0.6–2 Pa | — |
Temperature | 1045–1050 °C | — |
Temperature | 50–70 °C | — |
Thickness | 1–3 um | — |
| 1–3 µm |
GaN |
GaN thickness Example 1 | 1 µm | GaN |
GaN thickness Example 2 | 2 µm | GaN |
GaN thickness Example 3 | 3 µm | GaN |
sapphire substrate thickness range | 0.43–0.5 mm | Al₂O₃ |
Pressure | 0.6–2 Pa | — |
Temperature | 1045–1050 °C | — |
Temperature | 50–70 °C | — |
Thickness | 1–3 um | — |
| 1–3 µm |
GaN |
GaN thickness Example 1 | 1 µm | GaN |
GaN thickness Example 2 | 2 µm | GaN |
GaN thickness Example 3 | 3 µm | GaN |
sapphire substrate thickness range | 0.43–0.5 mm | Al₂O₃ |
Pressure | 0.6–2 Pa | — |
Temperature | 1045–1050 °C | — |
Temperature | 50–70 °C | — |
Thickness | 1–3 um | — |
| 1–3 µm |
GaN |
GaN thickness Example 1 | 1 µm | GaN |
GaN thickness Example 2 | 2 µm | GaN |
GaN thickness Example 3 | 3 µm | GaN |
sapphire substrate thickness range | 0.43–0.5 mm | Al₂O₃ |
Pressure | 0.6–2 Pa | — |
Temperature | 1045–1050 °C | — |
Temperature | 50–70 °C | — |
Thickness | 1–3 um | — |
