BULK GAN CRYSTAL, C-PLANE GAN WAFER, AND METHOD FOR MANUFACTURING BULK GAN CRYSTAL | Matter42 Literature
Patent
Atlas literature
Patent
US 12,060,653 B2
BULK GAN CRYSTAL, C-PLANE GAN WAFER, AND METHOD FOR MANUFACTURING BULK GAN CRYSTAL
Yutaka Mikawa, Tetsuo Okano
MITSUBISHI CHEMICAL CORPORATION, Tokyo (JP)·Aug. 13, 2024·US
Drawings
Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1
FIG. 1 illustrates one example of a bulk GaN crystal according to a preferred embodiment. Panel (a) of
FIG. 2
FIG. 2 when XRD rocking curves are measured on the measurement line using the c-plane as a reflection surface and their peak angles w are plotted 55 against the …
FIG. 3
FIG. 3 when XRD rocking curves are measured on the measurement line in the same manner and their peak 65 angles Go are plotted against the positions of the …
FIG. 4
FIG. 4. Further, as required, the c-plane wafer 100 may be provided with various markings, such as an orientation flat or notch that 15 indicates the crystal …
FIG. 5
FIG. 5, when the normal vector of the third main surface 101 is a vector N, the off-cut angle of the c-plane wafer 100 is an inclination 6 of the vector N from …
FIG. 6
FIG. 6, the crystal growth apparatus includes an autoclave, and a capsule arranged therein. Inside the capsule, a dissolution zone and a growth zone, which are …
FIG. 7
FIG. 7. The term “large-surface-area” used herein is not limited to a specific area; however, specifically, the bulk GaN crystal has a size in which two 80 …
FIG. 8
apparatus side view
FIG. 8.
FIG. 9
FIG. 9. All of the plural through-holes penetrated through two wafers. That is, the through-holes formed in the portion where the wafers A and C overlapped …
FIG. 10
FIG. 10 is a cross-sectional view that illustrates a type I through-hole pair in which one end and the other end of a Pt wire are passed through the respective …
FIG. 11
FIG. 11, the wafer C whose outline is drawn with a dashed line is arranged on the 35 back side of the seed assembly and plays a role of a connecting plate that …
FIG. 12
FIG. 12. The main surface had an area that could fit a circle of 7.5 cm in diameter (area=approximately 44 cm2) with a margin. 4.2. Evaluation of …
FIG. 13
FIG. 13 are graphs showing the results of measuring the peak angles of (002) XRD rocking curves of a large-surface-area bulk GaN crystal at 5-mm intervals over …
Claims
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
4 independent · 25 dependent
1
IndependentGaN
A bulk GaN crystal, comprising a main surface selected from a surface inclined at 0° to 10° from the (0001) crystal plane and a surface inclined at 0° to 10° from the (000-1) crystal plane, wherein the main surface is a specific main surface A that satisfies the following conditions (i) and (ii): (i) a first line, which is a 80 mm-long virtual line segment extending in a first direction on the specific main surface A, can be drawn, and a difference between a maximum value and a minimum value of peak angles in (002) XRD rocking curves of the GaN crystal, which is measured between 17 measurement points arranged at a 5-mm pitch on the first line with the omega axis being perpendicular to the first direction, is 0.05° or less; and (ii) a second line, which is a 80 mm-long virtual line segment extending in a second direction perpendicular to the first direction on the specific main surface A, can be drawn, and a difference between a maximum value and a minimum value of peak angles in (002) XRD rocking curves of the GaN crystal, which is measured between 17 measurement points arranged at a 5-mm pitch on the second line with the omega axis being perpendicular to the second direction, is 0.05° or less.
3
Dependent← claim 1GaN
The bulk GaN crystal according to claim 1, wherein the difference between the maximum value and the minimum value of the peak angles in the condition (i) and the difference between the maximum value and the minimum value of the peak angles in the condition (ii) are both 0.02° or less.
4
Dependent← claim 1GaN
The bulk GaN crystal according to claim 1, wherein neither the 17 measurement points in the condition (i) nor the 17 measurement points in the condition (ii) includes a measurement point at which the peak angle is different by 0.01° or more from the peak angle at an adjacent measure-ment point.
5
Dependent← claim 1GaN
The bulk GaN crystal according to claim 1, wherein the radius of curvature of the surface along the first direction, which is calculated from a rate of peak angle change in the condition (i), and the radius of curvature of the surface along the second direction, which is calculated from a rate of peak angle change in the condition (ii), are both 300 m or larger.
6
Dependent← claim 1GaN
The bulk GaN crystal according to claim 1, having a dislocation density of lower than 1×106 cm⁻² in all of 100 µm×100 µm virtual regions that can be arbitrarily arranged on the specific main surface A, except for the portion having 35 a distance of less than 5 mm from the outer circumference in a plan view.
7
Dependent← claim 1GaN
The bulk GaN crystal according to claim 1, having a dislocation density of lower than 1×105 cm⁻² in all of 2 mm×2 mm virtual regions that can be arbitrarily arranged on the specific main surface A, except for the portion having a distance of less than 5 mm from the outer circumference in a plan view.
10
Dependent← claim 1GaN
The bulk GaN crystal according to claim 1, satisfying one or more conditions selected from the following (a) to (g): (a) the H concentration is 1×1017 atoms/cm3 or higher; (b) the O concentration is 1×1017 atoms/cm3 or higher; (c) the concentration of at least one of Li, Na, and K is lower than 1×1015 atoms/cm3; (d) the F concentration is 1×1015 atoms/cm3 or higher; B₂ (e) the concentration of at least one of Cl, Br, and I is 1×1015 atoms/cm3 or higher; (f) the I concentration is 1×1015 atoms/cm3 or higher; and (g) the Si concentration is lower than 2×1015 atoms/cm3.
12
Dependent← claim 1GaNGaN
A method of producing a c-plane GaN wafer, the method comprising at least the steps of: preparing the bulk GaN crystal according to claim 1; and slicing the GaN crystal.
2
IndependentGaN
A bulk GaN crystal, comprising a first main surface and a second main surface that face the opposite direction from each other, wherein one of the first main surface and the second main surface is a surface inclined at 0° to 10° from the (0001) crystal plane while the other is a surface inclined at 0° to 10° from the (000-1) crystal plane, and the bulk GaN crystal satisfies the following conditions (i) and (ii): (i) a first line, which is a 80 mm-long virtual line segment extending in a first direction on the first main surface, can be drawn, and a difference between a maximum value and a minimum value of peak angles in (002) XRD rocking curves of the GaN crystal, which is measured between 17 measurement points arranged at a 5-mm pitch on the first line with the omega axis being perpendicular to the first direction, is 0.05° or less; and (ii) a second line, which is a 80 mm-long virtual line segment extending in a second direction perpendicular to the first direction on the first main surface, can be drawn, and a difference between a maximum value and a minimum value of peak angles in (002) XRD rocking curves of the GaN crystal, which is measured between 17 measurement points arranged at a 5-mm pitch on the second line with the omega axis being perpendicular to the second direction, is 0.050 or less.
8
Dependent← claim 2GaN
The bulk GaN crystal according to claim 2, having a dislocation density of lower than 1×106 cm⁻² in all of 100 µm×100 µm virtual regions that can be arbitrarily arranged on the first main surface, except for the portion having a distance of less than 5 mm from the outer circumference in a plan view, which dislocation density is calculated from the number of dislocations existing in each region and the area of the region.
9
Dependent← claim 2GaN
The bulk GaN crystal according to claim 2, having a dislocation density of lower than 1×105 cm⁻² in all of 2 mm×2 mm virtual regions that can be arbitrarily arranged on the first main surface, except for the portion having a distance of less than 5 mm from the outer circumference in a plan view, which dislocation density is calculated from the number of dislocations existing in each region and the area of the region.
14
IndependentGaNc-plane GaN wafer
A c-plane GaN wafer, comprising a main surface selected from a surface inclined at 0° to 10° from the (0001) crystal plane and a surface inclined at 0° to 10° from the (000-1) crystal plane, wherein the main surface is a specific main surface B that satisfies the following condition (111): (111) on the specific main surface B, a virtual line segment of 50 mm or longer can be drawn, and a variation range of an m-axis direction component of an off-cut angle and that of an a-axis direction component of the off-cut angle are both 0.05° or less, except for the portion having a distance of less than 5 mm from the outer circumference in a plan view.
16
Dependent← claim 14GaNc-plane GaN wafer
The c-plane GaN wafer according to claim 14, wherein the variation range of the m-axis direction compo-nent of the off-cut angle and that of the a-axis direction component of the off-cut angle are both 0.02° or less.
17
Dependent← claim 14GaNc-plane GaN wafer
The c-plane GaN wafer according to claim 14, having a diameter selected from 50 mm to 55 mm, 75 mm to 80 mm, 100 mm to 105 mm, and 150 mm to 155 mm.
18
Dependent← claim 14GaNc-plane GaN wafer
The c-plane GaN wafer according to claim 14, having a dislocation density of lower than 1×106 cm⁻² in all of 100 µm×100 µm virtual regions that can be arbitrarily arranged on the specific main surface B, except for the portion having a distance of less than 5 mm from the outer circumference in a plan view.
19
Dependent← claim 14GaNc-plane GaN wafer
The c-plane GaN wafer according to claim 14, having a dislocation density of lower than 1×105 cm⁻² in all of 2 mm×2 mm virtual regions that can be arbitrarily arranged on the specific main surface B, except for the portion having a distance of less than 5 mm from the outer circumference in a plan view.
22
Dependent← claim 14GaNc-plane GaN wafer
The c-plane GaN wafer according to claim 14, satis-fying one or more conditions selected from the following (a) to (g): (a) the H concentration is 1×1017 atoms/cm3 or higher; (b) the O concentration is 1×1017 atoms/cm3 or higher; (c) the concentration of at least one of Li, Na, and K is lower than 1×1015 atoms/cm3; (d) the F concentration is 1×1015 atoms/cm3 or higher; (e) the concentration of at least one of Cl, Br, and I is 1×1015 atoms/cm3 or higher; (f) the I concentration is 1×1015 atoms/cm3 or higher; and (g) the Si concentration is lower than 2×1015 atoms/cm3.
An epitaxial wafer, comprising: the c-plane GaN wafer according to claim 14; and at least one nitride semiconductor layer epitaxially grown on the c-plane GaN wafer.
A method of producing an epitaxial wafer, the method comprising the steps of: preparing the c-plane GaN wafer according to claim 14; and epitaxially growing at least one nitride semiconductor layer on the c-plane GaN wafer.
A method of producing a nitride semiconductor device, the method comprising the steps of: preparing the c-plane GaN wafer according to claim 14; and B₂ epitaxially growing at least one nitride semiconductor layer on the c-plane GaN wafer. 27.Amethod of producing a bulk GaN crystal, the method comprising the steps of: preparing the c-plane GaN wafer according to claim 14; and epitaxially growing a GaN crystal from a vapor phase on the c-plane GaN wafer. 28.Amethod of producing a bulk GaN crystal, the method comprising the step of growing a GaN crystal on a seed assembly by an ammonothermal method, wherein the seed assembly is constituted by plural c-plane GaN wafers, and a metal wire is used for immobilizing the plural c-plane GaN wafers with one another.
15
IndependentGaNc-plane GaN wafer
A c-plane GaN wafer, comprising a third main surface and a fourth main surface that face the opposite direction from each other, one of which third main surface and fourth main surface is a surface inclined at 0° to 10° from the (0001) crystal plane while the other is a surface inclined at 0° to 10° from the (000-1) crystal plane, wherein, on the third main surface, a virtual line segment of 50 mm or longer can be drawn, and a variation range of an m-axis direction component of an off-cut angle and that of an a-axis direction component of the off-cut angle are both 0.05° or less, except for the portion having a distance of less than 5 mm from the outer circumference in a plan view.
20
Dependent← claim 15GaNc-plane GaN wafer
The c-plane GaN wafer according to claim 15, having a dislocation density of lower than 1×106 cm⁻² in all of 100 µm×100 µm virtual regions that can be arbitrarily arranged on the third main surface, except for the portion having a distance of less than 5 mm from the outer circumference in a plan view.
21
Dependent← claim 15GaNc-plane GaN wafer
The c-plane GaN wafer according to claim 15, having a dislocation density of lower than 1×105 cm⁻² in 2 mm×2 mm virtual regions that can be arbitrarily arranged on the third main surface, except for the portion having a distance of less than 5 mm from the outer circumference in a plan view.
29
Dependent← claim 28GaNGaN
The method of producing a bulk GaN crystal accord-ing to claim 28, wherein the orientations of the c-axes, a-axes, and m-axes of all of the c-plane GaN wafers con-stituting the seed assembly are aligned.
30
Dependent← claim 29GaN
The method of producing a bulk GaN crystal accord-ing to claim 29, wherein, when the direction of N-polar side of main surfaces of the c-plane GaN wafers constituting the seed assembly is defined as front direction, two or more c-plane GaN wafers each having a rectangular or substan-tially rectangular main surface are arranged adjacent to each other on the front-direction side of the seed assembly, and a c-plane GaN wafer is arranged on the opposite side of the front direction of the seed assembly.
31
Dependent← claim 28GaNGaN
The method of producing a bulk GaN crystal accord-ing to claim 28, wherein, in the step of growing a GaN crystal by an ammonothermal method, a mineralizer con-taining a halogen-containing compound is used, and at least one metal wire selected from an Ag wire, a Pt wire and an Au wire is used as the metal wire. ∗ ∗ ∗ ∗ ∗
Device structures
Layer stacks claimed or described, ordered top of device to substrate.
c-plane GaN wafer
GaNwafer
epitaxial wafer
nitride semiconductor layerepitaxial layer
GaNsubstrate
Materials
Materials described outside the worked examples.
bulk GaN crystal
GaN
Claimed Bulk Crystal
Claimed Wafer Substrate
nitride semiconductor layer
Claimed Epitaxial Layer
Process steps
Additional fabrication and treatment steps described in the patent.
1
Ammonothermal Growth
Step 1
Ambient
ammonia (ammonothermal)
Process details
seed:plural c-plane GaN wafers constituting seed assembly
mineralizer:halogen-containing compound
wire material:
Characterization
Measurements and analyses referenced in the patent, with their drawing references.
xrd
XRD
FIG. 2 when XRD rocking curves are measured on the measurement line using the c-plane as a reflection surface and their peak angles w are plotted 55 against the …
BULK GAN CRYSTAL, C-PLANE GAN WAFER, AND METHOD FOR MANUFACTURING BULK GAN CRYSTAL
Yutaka Mikawa, Tetsuo Okano
MITSUBISHI CHEMICAL CORPORATION, Tokyo (JP)·Aug. 13, 2024·US
Drawings
Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1
FIG. 1 illustrates one example of a bulk GaN crystal according to a preferred embodiment. Panel (a) of
FIG. 2
FIG. 2 when XRD rocking curves are measured on the measurement line using the c-plane as a reflection surface and their peak angles w are plotted 55 against the …
FIG. 3
FIG. 3 when XRD rocking curves are measured on the measurement line in the same manner and their peak 65 angles Go are plotted against the positions of the …
FIG. 4
FIG. 4. Further, as required, the c-plane wafer 100 may be provided with various markings, such as an orientation flat or notch that 15 indicates the crystal …
FIG. 5
FIG. 5, when the normal vector of the third main surface 101 is a vector N, the off-cut angle of the c-plane wafer 100 is an inclination 6 of the vector N from …
FIG. 6
FIG. 6, the crystal growth apparatus includes an autoclave, and a capsule arranged therein. Inside the capsule, a dissolution zone and a growth zone, which are …
FIG. 7
FIG. 7. The term “large-surface-area” used herein is not limited to a specific area; however, specifically, the bulk GaN crystal has a size in which two 80 …
FIG. 8
apparatus side view
FIG. 8.
FIG. 9
FIG. 9. All of the plural through-holes penetrated through two wafers. That is, the through-holes formed in the portion where the wafers A and C overlapped …
FIG. 10
FIG. 10 is a cross-sectional view that illustrates a type I through-hole pair in which one end and the other end of a Pt wire are passed through the respective …
FIG. 11
FIG. 11, the wafer C whose outline is drawn with a dashed line is arranged on the 35 back side of the seed assembly and plays a role of a connecting plate that …
FIG. 12
FIG. 12. The main surface had an area that could fit a circle of 7.5 cm in diameter (area=approximately 44 cm2) with a margin. 4.2. Evaluation of …
FIG. 13
FIG. 13 are graphs showing the results of measuring the peak angles of (002) XRD rocking curves of a large-surface-area bulk GaN crystal at 5-mm intervals over …
Claims
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
4 independent · 25 dependent
1
IndependentGaN
A bulk GaN crystal, comprising a main surface selected from a surface inclined at 0° to 10° from the (0001) crystal plane and a surface inclined at 0° to 10° from the (000-1) crystal plane, wherein the main surface is a specific main surface A that satisfies the following conditions (i) and (ii): (i) a first line, which is a 80 mm-long virtual line segment extending in a first direction on the specific main surface A, can be drawn, and a difference between a maximum value and a minimum value of peak angles in (002) XRD rocking curves of the GaN crystal, which is measured between 17 measurement points arranged at a 5-mm pitch on the first line with the omega axis being perpendicular to the first direction, is 0.05° or less; and (ii) a second line, which is a 80 mm-long virtual line segment extending in a second direction perpendicular to the first direction on the specific main surface A, can be drawn, and a difference between a maximum value and a minimum value of peak angles in (002) XRD rocking curves of the GaN crystal, which is measured between 17 measurement points arranged at a 5-mm pitch on the second line with the omega axis being perpendicular to the second direction, is 0.05° or less.
3
Dependent← claim 1GaN
The bulk GaN crystal according to claim 1, wherein the difference between the maximum value and the minimum value of the peak angles in the condition (i) and the difference between the maximum value and the minimum value of the peak angles in the condition (ii) are both 0.02° or less.
4
Dependent← claim 1GaN
The bulk GaN crystal according to claim 1, wherein neither the 17 measurement points in the condition (i) nor the 17 measurement points in the condition (ii) includes a measurement point at which the peak angle is different by 0.01° or more from the peak angle at an adjacent measure-ment point.
5
Dependent← claim 1GaN
The bulk GaN crystal according to claim 1, wherein the radius of curvature of the surface along the first direction, which is calculated from a rate of peak angle change in the condition (i), and the radius of curvature of the surface along the second direction, which is calculated from a rate of peak angle change in the condition (ii), are both 300 m or larger.
6
Dependent← claim 1GaN
The bulk GaN crystal according to claim 1, having a dislocation density of lower than 1×106 cm⁻² in all of 100 µm×100 µm virtual regions that can be arbitrarily arranged on the specific main surface A, except for the portion having 35 a distance of less than 5 mm from the outer circumference in a plan view.
7
Dependent← claim 1GaN
The bulk GaN crystal according to claim 1, having a dislocation density of lower than 1×105 cm⁻² in all of 2 mm×2 mm virtual regions that can be arbitrarily arranged on the specific main surface A, except for the portion having a distance of less than 5 mm from the outer circumference in a plan view.
10
Dependent← claim 1GaN
The bulk GaN crystal according to claim 1, satisfying one or more conditions selected from the following (a) to (g): (a) the H concentration is 1×1017 atoms/cm3 or higher; (b) the O concentration is 1×1017 atoms/cm3 or higher; (c) the concentration of at least one of Li, Na, and K is lower than 1×1015 atoms/cm3; (d) the F concentration is 1×1015 atoms/cm3 or higher; B₂ (e) the concentration of at least one of Cl, Br, and I is 1×1015 atoms/cm3 or higher; (f) the I concentration is 1×1015 atoms/cm3 or higher; and (g) the Si concentration is lower than 2×1015 atoms/cm3.
12
Dependent← claim 1GaNGaN
A method of producing a c-plane GaN wafer, the method comprising at least the steps of: preparing the bulk GaN crystal according to claim 1; and slicing the GaN crystal.
2
IndependentGaN
A bulk GaN crystal, comprising a first main surface and a second main surface that face the opposite direction from each other, wherein one of the first main surface and the second main surface is a surface inclined at 0° to 10° from the (0001) crystal plane while the other is a surface inclined at 0° to 10° from the (000-1) crystal plane, and the bulk GaN crystal satisfies the following conditions (i) and (ii): (i) a first line, which is a 80 mm-long virtual line segment extending in a first direction on the first main surface, can be drawn, and a difference between a maximum value and a minimum value of peak angles in (002) XRD rocking curves of the GaN crystal, which is measured between 17 measurement points arranged at a 5-mm pitch on the first line with the omega axis being perpendicular to the first direction, is 0.05° or less; and (ii) a second line, which is a 80 mm-long virtual line segment extending in a second direction perpendicular to the first direction on the first main surface, can be drawn, and a difference between a maximum value and a minimum value of peak angles in (002) XRD rocking curves of the GaN crystal, which is measured between 17 measurement points arranged at a 5-mm pitch on the second line with the omega axis being perpendicular to the second direction, is 0.050 or less.
8
Dependent← claim 2GaN
The bulk GaN crystal according to claim 2, having a dislocation density of lower than 1×106 cm⁻² in all of 100 µm×100 µm virtual regions that can be arbitrarily arranged on the first main surface, except for the portion having a distance of less than 5 mm from the outer circumference in a plan view, which dislocation density is calculated from the number of dislocations existing in each region and the area of the region.
9
Dependent← claim 2GaN
The bulk GaN crystal according to claim 2, having a dislocation density of lower than 1×105 cm⁻² in all of 2 mm×2 mm virtual regions that can be arbitrarily arranged on the first main surface, except for the portion having a distance of less than 5 mm from the outer circumference in a plan view, which dislocation density is calculated from the number of dislocations existing in each region and the area of the region.
14
IndependentGaNc-plane GaN wafer
A c-plane GaN wafer, comprising a main surface selected from a surface inclined at 0° to 10° from the (0001) crystal plane and a surface inclined at 0° to 10° from the (000-1) crystal plane, wherein the main surface is a specific main surface B that satisfies the following condition (111): (111) on the specific main surface B, a virtual line segment of 50 mm or longer can be drawn, and a variation range of an m-axis direction component of an off-cut angle and that of an a-axis direction component of the off-cut angle are both 0.05° or less, except for the portion having a distance of less than 5 mm from the outer circumference in a plan view.
16
Dependent← claim 14GaNc-plane GaN wafer
The c-plane GaN wafer according to claim 14, wherein the variation range of the m-axis direction compo-nent of the off-cut angle and that of the a-axis direction component of the off-cut angle are both 0.02° or less.
17
Dependent← claim 14GaNc-plane GaN wafer
The c-plane GaN wafer according to claim 14, having a diameter selected from 50 mm to 55 mm, 75 mm to 80 mm, 100 mm to 105 mm, and 150 mm to 155 mm.
18
Dependent← claim 14GaNc-plane GaN wafer
The c-plane GaN wafer according to claim 14, having a dislocation density of lower than 1×106 cm⁻² in all of 100 µm×100 µm virtual regions that can be arbitrarily arranged on the specific main surface B, except for the portion having a distance of less than 5 mm from the outer circumference in a plan view.
19
Dependent← claim 14GaNc-plane GaN wafer
The c-plane GaN wafer according to claim 14, having a dislocation density of lower than 1×105 cm⁻² in all of 2 mm×2 mm virtual regions that can be arbitrarily arranged on the specific main surface B, except for the portion having a distance of less than 5 mm from the outer circumference in a plan view.
22
Dependent← claim 14GaNc-plane GaN wafer
The c-plane GaN wafer according to claim 14, satis-fying one or more conditions selected from the following (a) to (g): (a) the H concentration is 1×1017 atoms/cm3 or higher; (b) the O concentration is 1×1017 atoms/cm3 or higher; (c) the concentration of at least one of Li, Na, and K is lower than 1×1015 atoms/cm3; (d) the F concentration is 1×1015 atoms/cm3 or higher; (e) the concentration of at least one of Cl, Br, and I is 1×1015 atoms/cm3 or higher; (f) the I concentration is 1×1015 atoms/cm3 or higher; and (g) the Si concentration is lower than 2×1015 atoms/cm3.
An epitaxial wafer, comprising: the c-plane GaN wafer according to claim 14; and at least one nitride semiconductor layer epitaxially grown on the c-plane GaN wafer.
A method of producing an epitaxial wafer, the method comprising the steps of: preparing the c-plane GaN wafer according to claim 14; and epitaxially growing at least one nitride semiconductor layer on the c-plane GaN wafer.
A method of producing a nitride semiconductor device, the method comprising the steps of: preparing the c-plane GaN wafer according to claim 14; and B₂ epitaxially growing at least one nitride semiconductor layer on the c-plane GaN wafer. 27.Amethod of producing a bulk GaN crystal, the method comprising the steps of: preparing the c-plane GaN wafer according to claim 14; and epitaxially growing a GaN crystal from a vapor phase on the c-plane GaN wafer. 28.Amethod of producing a bulk GaN crystal, the method comprising the step of growing a GaN crystal on a seed assembly by an ammonothermal method, wherein the seed assembly is constituted by plural c-plane GaN wafers, and a metal wire is used for immobilizing the plural c-plane GaN wafers with one another.
15
IndependentGaNc-plane GaN wafer
A c-plane GaN wafer, comprising a third main surface and a fourth main surface that face the opposite direction from each other, one of which third main surface and fourth main surface is a surface inclined at 0° to 10° from the (0001) crystal plane while the other is a surface inclined at 0° to 10° from the (000-1) crystal plane, wherein, on the third main surface, a virtual line segment of 50 mm or longer can be drawn, and a variation range of an m-axis direction component of an off-cut angle and that of an a-axis direction component of the off-cut angle are both 0.05° or less, except for the portion having a distance of less than 5 mm from the outer circumference in a plan view.
20
Dependent← claim 15GaNc-plane GaN wafer
The c-plane GaN wafer according to claim 15, having a dislocation density of lower than 1×106 cm⁻² in all of 100 µm×100 µm virtual regions that can be arbitrarily arranged on the third main surface, except for the portion having a distance of less than 5 mm from the outer circumference in a plan view.
21
Dependent← claim 15GaNc-plane GaN wafer
The c-plane GaN wafer according to claim 15, having a dislocation density of lower than 1×105 cm⁻² in 2 mm×2 mm virtual regions that can be arbitrarily arranged on the third main surface, except for the portion having a distance of less than 5 mm from the outer circumference in a plan view.
29
Dependent← claim 28GaNGaN
The method of producing a bulk GaN crystal accord-ing to claim 28, wherein the orientations of the c-axes, a-axes, and m-axes of all of the c-plane GaN wafers con-stituting the seed assembly are aligned.
30
Dependent← claim 29GaN
The method of producing a bulk GaN crystal accord-ing to claim 29, wherein, when the direction of N-polar side of main surfaces of the c-plane GaN wafers constituting the seed assembly is defined as front direction, two or more c-plane GaN wafers each having a rectangular or substan-tially rectangular main surface are arranged adjacent to each other on the front-direction side of the seed assembly, and a c-plane GaN wafer is arranged on the opposite side of the front direction of the seed assembly.
31
Dependent← claim 28GaNGaN
The method of producing a bulk GaN crystal accord-ing to claim 28, wherein, in the step of growing a GaN crystal by an ammonothermal method, a mineralizer con-taining a halogen-containing compound is used, and at least one metal wire selected from an Ag wire, a Pt wire and an Au wire is used as the metal wire. ∗ ∗ ∗ ∗ ∗
Device structures
Layer stacks claimed or described, ordered top of device to substrate.
c-plane GaN wafer
GaNwafer
epitaxial wafer
nitride semiconductor layerepitaxial layer
GaNsubstrate
Materials
Materials described outside the worked examples.
bulk GaN crystal
GaN
Claimed Bulk Crystal
Claimed Wafer Substrate
nitride semiconductor layer
Claimed Epitaxial Layer
Process steps
Additional fabrication and treatment steps described in the patent.
1
Ammonothermal Growth
Step 1
Ambient
ammonia (ammonothermal)
Process details
seed:plural c-plane GaN wafers constituting seed assembly
mineralizer:halogen-containing compound
wire material:
Characterization
Measurements and analyses referenced in the patent, with their drawing references.
xrd
XRD
FIG. 2 when XRD rocking curves are measured on the measurement line using the c-plane as a reflection surface and their peak angles w are plotted 55 against the …
BULK GAN CRYSTAL, C-PLANE GAN WAFER, AND METHOD FOR MANUFACTURING BULK GAN CRYSTAL
Yutaka Mikawa, Tetsuo Okano
MITSUBISHI CHEMICAL CORPORATION, Tokyo (JP)·Aug. 13, 2024·US
Drawings
Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1
FIG. 1 illustrates one example of a bulk GaN crystal according to a preferred embodiment. Panel (a) of
FIG. 2
FIG. 2 when XRD rocking curves are measured on the measurement line using the c-plane as a reflection surface and their peak angles w are plotted 55 against the …
FIG. 3
FIG. 3 when XRD rocking curves are measured on the measurement line in the same manner and their peak 65 angles Go are plotted against the positions of the …
FIG. 4
FIG. 4. Further, as required, the c-plane wafer 100 may be provided with various markings, such as an orientation flat or notch that 15 indicates the crystal …
FIG. 5
FIG. 5, when the normal vector of the third main surface 101 is a vector N, the off-cut angle of the c-plane wafer 100 is an inclination 6 of the vector N from …
FIG. 6
FIG. 6, the crystal growth apparatus includes an autoclave, and a capsule arranged therein. Inside the capsule, a dissolution zone and a growth zone, which are …
FIG. 7
FIG. 7. The term “large-surface-area” used herein is not limited to a specific area; however, specifically, the bulk GaN crystal has a size in which two 80 …
FIG. 8
apparatus side view
FIG. 8.
FIG. 9
FIG. 9. All of the plural through-holes penetrated through two wafers. That is, the through-holes formed in the portion where the wafers A and C overlapped …
FIG. 10
FIG. 10 is a cross-sectional view that illustrates a type I through-hole pair in which one end and the other end of a Pt wire are passed through the respective …
FIG. 11
FIG. 11, the wafer C whose outline is drawn with a dashed line is arranged on the 35 back side of the seed assembly and plays a role of a connecting plate that …
FIG. 12
FIG. 12. The main surface had an area that could fit a circle of 7.5 cm in diameter (area=approximately 44 cm2) with a margin. 4.2. Evaluation of …
FIG. 13
FIG. 13 are graphs showing the results of measuring the peak angles of (002) XRD rocking curves of a large-surface-area bulk GaN crystal at 5-mm intervals over …
Claims
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
4 independent · 25 dependent
1
IndependentGaN
A bulk GaN crystal, comprising a main surface selected from a surface inclined at 0° to 10° from the (0001) crystal plane and a surface inclined at 0° to 10° from the (000-1) crystal plane, wherein the main surface is a specific main surface A that satisfies the following conditions (i) and (ii): (i) a first line, which is a 80 mm-long virtual line segment extending in a first direction on the specific main surface A, can be drawn, and a difference between a maximum value and a minimum value of peak angles in (002) XRD rocking curves of the GaN crystal, which is measured between 17 measurement points arranged at a 5-mm pitch on the first line with the omega axis being perpendicular to the first direction, is 0.05° or less; and (ii) a second line, which is a 80 mm-long virtual line segment extending in a second direction perpendicular to the first direction on the specific main surface A, can be drawn, and a difference between a maximum value and a minimum value of peak angles in (002) XRD rocking curves of the GaN crystal, which is measured between 17 measurement points arranged at a 5-mm pitch on the second line with the omega axis being perpendicular to the second direction, is 0.05° or less.
3
Dependent← claim 1GaN
The bulk GaN crystal according to claim 1, wherein the difference between the maximum value and the minimum value of the peak angles in the condition (i) and the difference between the maximum value and the minimum value of the peak angles in the condition (ii) are both 0.02° or less.
4
Dependent← claim 1GaN
The bulk GaN crystal according to claim 1, wherein neither the 17 measurement points in the condition (i) nor the 17 measurement points in the condition (ii) includes a measurement point at which the peak angle is different by 0.01° or more from the peak angle at an adjacent measure-ment point.
5
Dependent← claim 1GaN
The bulk GaN crystal according to claim 1, wherein the radius of curvature of the surface along the first direction, which is calculated from a rate of peak angle change in the condition (i), and the radius of curvature of the surface along the second direction, which is calculated from a rate of peak angle change in the condition (ii), are both 300 m or larger.
6
Dependent← claim 1GaN
The bulk GaN crystal according to claim 1, having a dislocation density of lower than 1×106 cm⁻² in all of 100 µm×100 µm virtual regions that can be arbitrarily arranged on the specific main surface A, except for the portion having 35 a distance of less than 5 mm from the outer circumference in a plan view.
7
Dependent← claim 1GaN
The bulk GaN crystal according to claim 1, having a dislocation density of lower than 1×105 cm⁻² in all of 2 mm×2 mm virtual regions that can be arbitrarily arranged on the specific main surface A, except for the portion having a distance of less than 5 mm from the outer circumference in a plan view.
10
Dependent← claim 1GaN
The bulk GaN crystal according to claim 1, satisfying one or more conditions selected from the following (a) to (g): (a) the H concentration is 1×1017 atoms/cm3 or higher; (b) the O concentration is 1×1017 atoms/cm3 or higher; (c) the concentration of at least one of Li, Na, and K is lower than 1×1015 atoms/cm3; (d) the F concentration is 1×1015 atoms/cm3 or higher; B₂ (e) the concentration of at least one of Cl, Br, and I is 1×1015 atoms/cm3 or higher; (f) the I concentration is 1×1015 atoms/cm3 or higher; and (g) the Si concentration is lower than 2×1015 atoms/cm3.
12
Dependent← claim 1GaNGaN
A method of producing a c-plane GaN wafer, the method comprising at least the steps of: preparing the bulk GaN crystal according to claim 1; and slicing the GaN crystal.
2
IndependentGaN
A bulk GaN crystal, comprising a first main surface and a second main surface that face the opposite direction from each other, wherein one of the first main surface and the second main surface is a surface inclined at 0° to 10° from the (0001) crystal plane while the other is a surface inclined at 0° to 10° from the (000-1) crystal plane, and the bulk GaN crystal satisfies the following conditions (i) and (ii): (i) a first line, which is a 80 mm-long virtual line segment extending in a first direction on the first main surface, can be drawn, and a difference between a maximum value and a minimum value of peak angles in (002) XRD rocking curves of the GaN crystal, which is measured between 17 measurement points arranged at a 5-mm pitch on the first line with the omega axis being perpendicular to the first direction, is 0.05° or less; and (ii) a second line, which is a 80 mm-long virtual line segment extending in a second direction perpendicular to the first direction on the first main surface, can be drawn, and a difference between a maximum value and a minimum value of peak angles in (002) XRD rocking curves of the GaN crystal, which is measured between 17 measurement points arranged at a 5-mm pitch on the second line with the omega axis being perpendicular to the second direction, is 0.050 or less.
8
Dependent← claim 2GaN
The bulk GaN crystal according to claim 2, having a dislocation density of lower than 1×106 cm⁻² in all of 100 µm×100 µm virtual regions that can be arbitrarily arranged on the first main surface, except for the portion having a distance of less than 5 mm from the outer circumference in a plan view, which dislocation density is calculated from the number of dislocations existing in each region and the area of the region.
9
Dependent← claim 2GaN
The bulk GaN crystal according to claim 2, having a dislocation density of lower than 1×105 cm⁻² in all of 2 mm×2 mm virtual regions that can be arbitrarily arranged on the first main surface, except for the portion having a distance of less than 5 mm from the outer circumference in a plan view, which dislocation density is calculated from the number of dislocations existing in each region and the area of the region.
14
IndependentGaNc-plane GaN wafer
A c-plane GaN wafer, comprising a main surface selected from a surface inclined at 0° to 10° from the (0001) crystal plane and a surface inclined at 0° to 10° from the (000-1) crystal plane, wherein the main surface is a specific main surface B that satisfies the following condition (111): (111) on the specific main surface B, a virtual line segment of 50 mm or longer can be drawn, and a variation range of an m-axis direction component of an off-cut angle and that of an a-axis direction component of the off-cut angle are both 0.05° or less, except for the portion having a distance of less than 5 mm from the outer circumference in a plan view.
16
Dependent← claim 14GaNc-plane GaN wafer
The c-plane GaN wafer according to claim 14, wherein the variation range of the m-axis direction compo-nent of the off-cut angle and that of the a-axis direction component of the off-cut angle are both 0.02° or less.
17
Dependent← claim 14GaNc-plane GaN wafer
The c-plane GaN wafer according to claim 14, having a diameter selected from 50 mm to 55 mm, 75 mm to 80 mm, 100 mm to 105 mm, and 150 mm to 155 mm.
18
Dependent← claim 14GaNc-plane GaN wafer
The c-plane GaN wafer according to claim 14, having a dislocation density of lower than 1×106 cm⁻² in all of 100 µm×100 µm virtual regions that can be arbitrarily arranged on the specific main surface B, except for the portion having a distance of less than 5 mm from the outer circumference in a plan view.
19
Dependent← claim 14GaNc-plane GaN wafer
The c-plane GaN wafer according to claim 14, having a dislocation density of lower than 1×105 cm⁻² in all of 2 mm×2 mm virtual regions that can be arbitrarily arranged on the specific main surface B, except for the portion having a distance of less than 5 mm from the outer circumference in a plan view.
22
Dependent← claim 14GaNc-plane GaN wafer
The c-plane GaN wafer according to claim 14, satis-fying one or more conditions selected from the following (a) to (g): (a) the H concentration is 1×1017 atoms/cm3 or higher; (b) the O concentration is 1×1017 atoms/cm3 or higher; (c) the concentration of at least one of Li, Na, and K is lower than 1×1015 atoms/cm3; (d) the F concentration is 1×1015 atoms/cm3 or higher; (e) the concentration of at least one of Cl, Br, and I is 1×1015 atoms/cm3 or higher; (f) the I concentration is 1×1015 atoms/cm3 or higher; and (g) the Si concentration is lower than 2×1015 atoms/cm3.
An epitaxial wafer, comprising: the c-plane GaN wafer according to claim 14; and at least one nitride semiconductor layer epitaxially grown on the c-plane GaN wafer.
A method of producing an epitaxial wafer, the method comprising the steps of: preparing the c-plane GaN wafer according to claim 14; and epitaxially growing at least one nitride semiconductor layer on the c-plane GaN wafer.
A method of producing a nitride semiconductor device, the method comprising the steps of: preparing the c-plane GaN wafer according to claim 14; and B₂ epitaxially growing at least one nitride semiconductor layer on the c-plane GaN wafer. 27.Amethod of producing a bulk GaN crystal, the method comprising the steps of: preparing the c-plane GaN wafer according to claim 14; and epitaxially growing a GaN crystal from a vapor phase on the c-plane GaN wafer. 28.Amethod of producing a bulk GaN crystal, the method comprising the step of growing a GaN crystal on a seed assembly by an ammonothermal method, wherein the seed assembly is constituted by plural c-plane GaN wafers, and a metal wire is used for immobilizing the plural c-plane GaN wafers with one another.
15
IndependentGaNc-plane GaN wafer
A c-plane GaN wafer, comprising a third main surface and a fourth main surface that face the opposite direction from each other, one of which third main surface and fourth main surface is a surface inclined at 0° to 10° from the (0001) crystal plane while the other is a surface inclined at 0° to 10° from the (000-1) crystal plane, wherein, on the third main surface, a virtual line segment of 50 mm or longer can be drawn, and a variation range of an m-axis direction component of an off-cut angle and that of an a-axis direction component of the off-cut angle are both 0.05° or less, except for the portion having a distance of less than 5 mm from the outer circumference in a plan view.
20
Dependent← claim 15GaNc-plane GaN wafer
The c-plane GaN wafer according to claim 15, having a dislocation density of lower than 1×106 cm⁻² in all of 100 µm×100 µm virtual regions that can be arbitrarily arranged on the third main surface, except for the portion having a distance of less than 5 mm from the outer circumference in a plan view.
21
Dependent← claim 15GaNc-plane GaN wafer
The c-plane GaN wafer according to claim 15, having a dislocation density of lower than 1×105 cm⁻² in 2 mm×2 mm virtual regions that can be arbitrarily arranged on the third main surface, except for the portion having a distance of less than 5 mm from the outer circumference in a plan view.
29
Dependent← claim 28GaNGaN
The method of producing a bulk GaN crystal accord-ing to claim 28, wherein the orientations of the c-axes, a-axes, and m-axes of all of the c-plane GaN wafers con-stituting the seed assembly are aligned.
30
Dependent← claim 29GaN
The method of producing a bulk GaN crystal accord-ing to claim 29, wherein, when the direction of N-polar side of main surfaces of the c-plane GaN wafers constituting the seed assembly is defined as front direction, two or more c-plane GaN wafers each having a rectangular or substan-tially rectangular main surface are arranged adjacent to each other on the front-direction side of the seed assembly, and a c-plane GaN wafer is arranged on the opposite side of the front direction of the seed assembly.
31
Dependent← claim 28GaNGaN
The method of producing a bulk GaN crystal accord-ing to claim 28, wherein, in the step of growing a GaN crystal by an ammonothermal method, a mineralizer con-taining a halogen-containing compound is used, and at least one metal wire selected from an Ag wire, a Pt wire and an Au wire is used as the metal wire. ∗ ∗ ∗ ∗ ∗
Device structures
Layer stacks claimed or described, ordered top of device to substrate.
c-plane GaN wafer
GaNwafer
epitaxial wafer
nitride semiconductor layerepitaxial layer
GaNsubstrate
Materials
Materials described outside the worked examples.
bulk GaN crystal
GaN
Claimed Bulk Crystal
Claimed Wafer Substrate
nitride semiconductor layer
Claimed Epitaxial Layer
Process steps
Additional fabrication and treatment steps described in the patent.
1
Ammonothermal Growth
Step 1
Ambient
ammonia (ammonothermal)
Process details
seed:plural c-plane GaN wafers constituting seed assembly
mineralizer:halogen-containing compound
wire material:
Characterization
Measurements and analyses referenced in the patent, with their drawing references.
xrd
XRD
FIG. 2 when XRD rocking curves are measured on the measurement line using the c-plane as a reflection surface and their peak angles w are plotted 55 against the …
BULK GAN CRYSTAL, C-PLANE GAN WAFER, AND METHOD FOR MANUFACTURING BULK GAN CRYSTAL
Yutaka Mikawa, Tetsuo Okano
MITSUBISHI CHEMICAL CORPORATION, Tokyo (JP)·Aug. 13, 2024·US
Drawings
Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1
FIG. 1 illustrates one example of a bulk GaN crystal according to a preferred embodiment. Panel (a) of
FIG. 2
FIG. 2 when XRD rocking curves are measured on the measurement line using the c-plane as a reflection surface and their peak angles w are plotted 55 against the …
FIG. 3
FIG. 3 when XRD rocking curves are measured on the measurement line in the same manner and their peak 65 angles Go are plotted against the positions of the …
FIG. 4
FIG. 4. Further, as required, the c-plane wafer 100 may be provided with various markings, such as an orientation flat or notch that 15 indicates the crystal …
FIG. 5
FIG. 5, when the normal vector of the third main surface 101 is a vector N, the off-cut angle of the c-plane wafer 100 is an inclination 6 of the vector N from …
FIG. 6
FIG. 6, the crystal growth apparatus includes an autoclave, and a capsule arranged therein. Inside the capsule, a dissolution zone and a growth zone, which are …
FIG. 7
FIG. 7. The term “large-surface-area” used herein is not limited to a specific area; however, specifically, the bulk GaN crystal has a size in which two 80 …
FIG. 8
apparatus side view
FIG. 8.
FIG. 9
FIG. 9. All of the plural through-holes penetrated through two wafers. That is, the through-holes formed in the portion where the wafers A and C overlapped …
FIG. 10
FIG. 10 is a cross-sectional view that illustrates a type I through-hole pair in which one end and the other end of a Pt wire are passed through the respective …
FIG. 11
FIG. 11, the wafer C whose outline is drawn with a dashed line is arranged on the 35 back side of the seed assembly and plays a role of a connecting plate that …
FIG. 12
FIG. 12. The main surface had an area that could fit a circle of 7.5 cm in diameter (area=approximately 44 cm2) with a margin. 4.2. Evaluation of …
FIG. 13
FIG. 13 are graphs showing the results of measuring the peak angles of (002) XRD rocking curves of a large-surface-area bulk GaN crystal at 5-mm intervals over …
Claims
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
4 independent · 25 dependent
1
IndependentGaN
A bulk GaN crystal, comprising a main surface selected from a surface inclined at 0° to 10° from the (0001) crystal plane and a surface inclined at 0° to 10° from the (000-1) crystal plane, wherein the main surface is a specific main surface A that satisfies the following conditions (i) and (ii): (i) a first line, which is a 80 mm-long virtual line segment extending in a first direction on the specific main surface A, can be drawn, and a difference between a maximum value and a minimum value of peak angles in (002) XRD rocking curves of the GaN crystal, which is measured between 17 measurement points arranged at a 5-mm pitch on the first line with the omega axis being perpendicular to the first direction, is 0.05° or less; and (ii) a second line, which is a 80 mm-long virtual line segment extending in a second direction perpendicular to the first direction on the specific main surface A, can be drawn, and a difference between a maximum value and a minimum value of peak angles in (002) XRD rocking curves of the GaN crystal, which is measured between 17 measurement points arranged at a 5-mm pitch on the second line with the omega axis being perpendicular to the second direction, is 0.05° or less.
3
Dependent← claim 1GaN
The bulk GaN crystal according to claim 1, wherein the difference between the maximum value and the minimum value of the peak angles in the condition (i) and the difference between the maximum value and the minimum value of the peak angles in the condition (ii) are both 0.02° or less.
4
Dependent← claim 1GaN
The bulk GaN crystal according to claim 1, wherein neither the 17 measurement points in the condition (i) nor the 17 measurement points in the condition (ii) includes a measurement point at which the peak angle is different by 0.01° or more from the peak angle at an adjacent measure-ment point.
5
Dependent← claim 1GaN
The bulk GaN crystal according to claim 1, wherein the radius of curvature of the surface along the first direction, which is calculated from a rate of peak angle change in the condition (i), and the radius of curvature of the surface along the second direction, which is calculated from a rate of peak angle change in the condition (ii), are both 300 m or larger.
6
Dependent← claim 1GaN
The bulk GaN crystal according to claim 1, having a dislocation density of lower than 1×106 cm⁻² in all of 100 µm×100 µm virtual regions that can be arbitrarily arranged on the specific main surface A, except for the portion having 35 a distance of less than 5 mm from the outer circumference in a plan view.
7
Dependent← claim 1GaN
The bulk GaN crystal according to claim 1, having a dislocation density of lower than 1×105 cm⁻² in all of 2 mm×2 mm virtual regions that can be arbitrarily arranged on the specific main surface A, except for the portion having a distance of less than 5 mm from the outer circumference in a plan view.
10
Dependent← claim 1GaN
The bulk GaN crystal according to claim 1, satisfying one or more conditions selected from the following (a) to (g): (a) the H concentration is 1×1017 atoms/cm3 or higher; (b) the O concentration is 1×1017 atoms/cm3 or higher; (c) the concentration of at least one of Li, Na, and K is lower than 1×1015 atoms/cm3; (d) the F concentration is 1×1015 atoms/cm3 or higher; B₂ (e) the concentration of at least one of Cl, Br, and I is 1×1015 atoms/cm3 or higher; (f) the I concentration is 1×1015 atoms/cm3 or higher; and (g) the Si concentration is lower than 2×1015 atoms/cm3.
12
Dependent← claim 1GaNGaN
A method of producing a c-plane GaN wafer, the method comprising at least the steps of: preparing the bulk GaN crystal according to claim 1; and slicing the GaN crystal.
2
IndependentGaN
A bulk GaN crystal, comprising a first main surface and a second main surface that face the opposite direction from each other, wherein one of the first main surface and the second main surface is a surface inclined at 0° to 10° from the (0001) crystal plane while the other is a surface inclined at 0° to 10° from the (000-1) crystal plane, and the bulk GaN crystal satisfies the following conditions (i) and (ii): (i) a first line, which is a 80 mm-long virtual line segment extending in a first direction on the first main surface, can be drawn, and a difference between a maximum value and a minimum value of peak angles in (002) XRD rocking curves of the GaN crystal, which is measured between 17 measurement points arranged at a 5-mm pitch on the first line with the omega axis being perpendicular to the first direction, is 0.05° or less; and (ii) a second line, which is a 80 mm-long virtual line segment extending in a second direction perpendicular to the first direction on the first main surface, can be drawn, and a difference between a maximum value and a minimum value of peak angles in (002) XRD rocking curves of the GaN crystal, which is measured between 17 measurement points arranged at a 5-mm pitch on the second line with the omega axis being perpendicular to the second direction, is 0.050 or less.
8
Dependent← claim 2GaN
The bulk GaN crystal according to claim 2, having a dislocation density of lower than 1×106 cm⁻² in all of 100 µm×100 µm virtual regions that can be arbitrarily arranged on the first main surface, except for the portion having a distance of less than 5 mm from the outer circumference in a plan view, which dislocation density is calculated from the number of dislocations existing in each region and the area of the region.
9
Dependent← claim 2GaN
The bulk GaN crystal according to claim 2, having a dislocation density of lower than 1×105 cm⁻² in all of 2 mm×2 mm virtual regions that can be arbitrarily arranged on the first main surface, except for the portion having a distance of less than 5 mm from the outer circumference in a plan view, which dislocation density is calculated from the number of dislocations existing in each region and the area of the region.
14
IndependentGaNc-plane GaN wafer
A c-plane GaN wafer, comprising a main surface selected from a surface inclined at 0° to 10° from the (0001) crystal plane and a surface inclined at 0° to 10° from the (000-1) crystal plane, wherein the main surface is a specific main surface B that satisfies the following condition (111): (111) on the specific main surface B, a virtual line segment of 50 mm or longer can be drawn, and a variation range of an m-axis direction component of an off-cut angle and that of an a-axis direction component of the off-cut angle are both 0.05° or less, except for the portion having a distance of less than 5 mm from the outer circumference in a plan view.
16
Dependent← claim 14GaNc-plane GaN wafer
The c-plane GaN wafer according to claim 14, wherein the variation range of the m-axis direction compo-nent of the off-cut angle and that of the a-axis direction component of the off-cut angle are both 0.02° or less.
17
Dependent← claim 14GaNc-plane GaN wafer
The c-plane GaN wafer according to claim 14, having a diameter selected from 50 mm to 55 mm, 75 mm to 80 mm, 100 mm to 105 mm, and 150 mm to 155 mm.
18
Dependent← claim 14GaNc-plane GaN wafer
The c-plane GaN wafer according to claim 14, having a dislocation density of lower than 1×106 cm⁻² in all of 100 µm×100 µm virtual regions that can be arbitrarily arranged on the specific main surface B, except for the portion having a distance of less than 5 mm from the outer circumference in a plan view.
19
Dependent← claim 14GaNc-plane GaN wafer
The c-plane GaN wafer according to claim 14, having a dislocation density of lower than 1×105 cm⁻² in all of 2 mm×2 mm virtual regions that can be arbitrarily arranged on the specific main surface B, except for the portion having a distance of less than 5 mm from the outer circumference in a plan view.
22
Dependent← claim 14GaNc-plane GaN wafer
The c-plane GaN wafer according to claim 14, satis-fying one or more conditions selected from the following (a) to (g): (a) the H concentration is 1×1017 atoms/cm3 or higher; (b) the O concentration is 1×1017 atoms/cm3 or higher; (c) the concentration of at least one of Li, Na, and K is lower than 1×1015 atoms/cm3; (d) the F concentration is 1×1015 atoms/cm3 or higher; (e) the concentration of at least one of Cl, Br, and I is 1×1015 atoms/cm3 or higher; (f) the I concentration is 1×1015 atoms/cm3 or higher; and (g) the Si concentration is lower than 2×1015 atoms/cm3.
An epitaxial wafer, comprising: the c-plane GaN wafer according to claim 14; and at least one nitride semiconductor layer epitaxially grown on the c-plane GaN wafer.
A method of producing an epitaxial wafer, the method comprising the steps of: preparing the c-plane GaN wafer according to claim 14; and epitaxially growing at least one nitride semiconductor layer on the c-plane GaN wafer.
A method of producing a nitride semiconductor device, the method comprising the steps of: preparing the c-plane GaN wafer according to claim 14; and B₂ epitaxially growing at least one nitride semiconductor layer on the c-plane GaN wafer. 27.Amethod of producing a bulk GaN crystal, the method comprising the steps of: preparing the c-plane GaN wafer according to claim 14; and epitaxially growing a GaN crystal from a vapor phase on the c-plane GaN wafer. 28.Amethod of producing a bulk GaN crystal, the method comprising the step of growing a GaN crystal on a seed assembly by an ammonothermal method, wherein the seed assembly is constituted by plural c-plane GaN wafers, and a metal wire is used for immobilizing the plural c-plane GaN wafers with one another.
15
IndependentGaNc-plane GaN wafer
A c-plane GaN wafer, comprising a third main surface and a fourth main surface that face the opposite direction from each other, one of which third main surface and fourth main surface is a surface inclined at 0° to 10° from the (0001) crystal plane while the other is a surface inclined at 0° to 10° from the (000-1) crystal plane, wherein, on the third main surface, a virtual line segment of 50 mm or longer can be drawn, and a variation range of an m-axis direction component of an off-cut angle and that of an a-axis direction component of the off-cut angle are both 0.05° or less, except for the portion having a distance of less than 5 mm from the outer circumference in a plan view.
20
Dependent← claim 15GaNc-plane GaN wafer
The c-plane GaN wafer according to claim 15, having a dislocation density of lower than 1×106 cm⁻² in all of 100 µm×100 µm virtual regions that can be arbitrarily arranged on the third main surface, except for the portion having a distance of less than 5 mm from the outer circumference in a plan view.
21
Dependent← claim 15GaNc-plane GaN wafer
The c-plane GaN wafer according to claim 15, having a dislocation density of lower than 1×105 cm⁻² in 2 mm×2 mm virtual regions that can be arbitrarily arranged on the third main surface, except for the portion having a distance of less than 5 mm from the outer circumference in a plan view.
29
Dependent← claim 28GaNGaN
The method of producing a bulk GaN crystal accord-ing to claim 28, wherein the orientations of the c-axes, a-axes, and m-axes of all of the c-plane GaN wafers con-stituting the seed assembly are aligned.
30
Dependent← claim 29GaN
The method of producing a bulk GaN crystal accord-ing to claim 29, wherein, when the direction of N-polar side of main surfaces of the c-plane GaN wafers constituting the seed assembly is defined as front direction, two or more c-plane GaN wafers each having a rectangular or substan-tially rectangular main surface are arranged adjacent to each other on the front-direction side of the seed assembly, and a c-plane GaN wafer is arranged on the opposite side of the front direction of the seed assembly.
31
Dependent← claim 28GaNGaN
The method of producing a bulk GaN crystal accord-ing to claim 28, wherein, in the step of growing a GaN crystal by an ammonothermal method, a mineralizer con-taining a halogen-containing compound is used, and at least one metal wire selected from an Ag wire, a Pt wire and an Au wire is used as the metal wire. ∗ ∗ ∗ ∗ ∗
Device structures
Layer stacks claimed or described, ordered top of device to substrate.
c-plane GaN wafer
GaNwafer
epitaxial wafer
nitride semiconductor layerepitaxial layer
GaNsubstrate
Materials
Materials described outside the worked examples.
bulk GaN crystal
GaN
Claimed Bulk Crystal
Claimed Wafer Substrate
nitride semiconductor layer
Claimed Epitaxial Layer
Process steps
Additional fabrication and treatment steps described in the patent.
1
Ammonothermal Growth
Step 1
Ambient
ammonia (ammonothermal)
Process details
seed:plural c-plane GaN wafers constituting seed assembly
mineralizer:halogen-containing compound
wire material:
Characterization
Measurements and analyses referenced in the patent, with their drawing references.
xrd
XRD
FIG. 2 when XRD rocking curves are measured on the measurement line using the c-plane as a reflection surface and their peak angles w are plotted 55 against the …
FIG. 3 when XRD rocking curves are measured on the measurement line in the same manner and their peak 65 angles Go are plotted against the positions of the …
FIG. 13 are graphs showing the results of measuring the peak angles of (002) XRD rocking curves of a large-surface-area bulk GaN crystal at 5-mm intervals over …
IR absorption peak attributed to gallium vacancy-hydrogen complex
3140–3200 cm⁻¹
GaN
Thickness
50–55 mm
—
Thickness
75–80 mm
—
Thickness
100–105 mm
—
Thickness
150–155 mm
—
Thickness
3140–3200 cm
—
Thickness
≤ 5 mm
—
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JP 2014534941 AJP 2014534941 A 12/2014
JP 2016088756 AJP 2016088756 A 5/2016
JP 2017031029 AJP 2017031029 A 2/2017
JP 2018024538 AJP 2018024538 A 2/2018
JP 2018024539 AJP 2018024539 A 2/2018
Cited non-patent literature · 2
JP 2018-024538 (Year: 2018).
Extended European Search Report issued Jun. 27, 2022 in EP Patent Application No. 20835168.4, 8 pages. English translation International Preliminary Report on Patentabil- ity and Written Opinion issued Dec. 28, 2021 in PCT/JP2020/025626, 6 pages. International Search Report issued Sep. 1, 2020 in PCT/JP2020/025626, 2 pages. Combined Chinese Office Action and Search Report issued Jul. 11, 2023 in Patent Application No. 202080047247.2 with Machine English translation, 37 pages. Combined Taiwanese Office Action and Search Report issued Feb. 7, 2024 in correspondingTaiwanese PatentApplication No. 109122058 (with machine English translation), 36 pages. Office Action issued Mar. 12, 2024 in corresponding Chinese Patent Application No. 202080047247.2 (with machine English transla- tion), 32 pages. Office Action issued Jun. 11, 2024 in corresponding Japanese Patent Application No. 2021-530031 (with machine English translation), 8 pages. Office Action issued May 28, 2024 in corresponding Korean Patent Application No. 10-2022-7003363 (with machine English transla- tion), 18 pages.
characterization XRDproperty XRD structurematerial GaN
FIG. 3 when XRD rocking curves are measured on the measurement line in the same manner and their peak 65 angles Go are plotted against the positions of the …
FIG. 13 are graphs showing the results of measuring the peak angles of (002) XRD rocking curves of a large-surface-area bulk GaN crystal at 5-mm intervals over …
IR absorption peak attributed to gallium vacancy-hydrogen complex
3140–3200 cm⁻¹
GaN
Thickness
50–55 mm
—
Thickness
75–80 mm
—
Thickness
100–105 mm
—
Thickness
150–155 mm
—
Thickness
3140–3200 cm
—
Thickness
≤ 5 mm
—
US 2017/0352721 A12017/0352721 A1 12/2017 Iso et al.
US 2019/0003078 A12019/0003078 A1 1/2019 D’Evelyn et al.
CN 109563642 ACN 109563642 A 4/2019
JP 2009018983 AJP 2009018983 A 1/2009
JP 2014534941 AJP 2014534941 A 12/2014
JP 2016088756 AJP 2016088756 A 5/2016
JP 2017031029 AJP 2017031029 A 2/2017
JP 2018024538 AJP 2018024538 A 2/2018
JP 2018024539 AJP 2018024539 A 2/2018
Cited non-patent literature · 2
JP 2018-024538 (Year: 2018).
Extended European Search Report issued Jun. 27, 2022 in EP Patent Application No. 20835168.4, 8 pages. English translation International Preliminary Report on Patentabil- ity and Written Opinion issued Dec. 28, 2021 in PCT/JP2020/025626, 6 pages. International Search Report issued Sep. 1, 2020 in PCT/JP2020/025626, 2 pages. Combined Chinese Office Action and Search Report issued Jul. 11, 2023 in Patent Application No. 202080047247.2 with Machine English translation, 37 pages. Combined Taiwanese Office Action and Search Report issued Feb. 7, 2024 in correspondingTaiwanese PatentApplication No. 109122058 (with machine English translation), 36 pages. Office Action issued Mar. 12, 2024 in corresponding Chinese Patent Application No. 202080047247.2 (with machine English transla- tion), 32 pages. Office Action issued Jun. 11, 2024 in corresponding Japanese Patent Application No. 2021-530031 (with machine English translation), 8 pages. Office Action issued May 28, 2024 in corresponding Korean Patent Application No. 10-2022-7003363 (with machine English transla- tion), 18 pages.
characterization XRDproperty XRD structurematerial GaN
FIG. 3 when XRD rocking curves are measured on the measurement line in the same manner and their peak 65 angles Go are plotted against the positions of the …
FIG. 13 are graphs showing the results of measuring the peak angles of (002) XRD rocking curves of a large-surface-area bulk GaN crystal at 5-mm intervals over …
IR absorption peak attributed to gallium vacancy-hydrogen complex
3140–3200 cm⁻¹
GaN
Thickness
50–55 mm
—
Thickness
75–80 mm
—
Thickness
100–105 mm
—
Thickness
150–155 mm
—
Thickness
3140–3200 cm
—
Thickness
≤ 5 mm
—
US 2017/0352721 A12017/0352721 A1 12/2017 Iso et al.
US 2019/0003078 A12019/0003078 A1 1/2019 D’Evelyn et al.
CN 109563642 ACN 109563642 A 4/2019
JP 2009018983 AJP 2009018983 A 1/2009
JP 2014534941 AJP 2014534941 A 12/2014
JP 2016088756 AJP 2016088756 A 5/2016
JP 2017031029 AJP 2017031029 A 2/2017
JP 2018024538 AJP 2018024538 A 2/2018
JP 2018024539 AJP 2018024539 A 2/2018
Cited non-patent literature · 2
JP 2018-024538 (Year: 2018).
Extended European Search Report issued Jun. 27, 2022 in EP Patent Application No. 20835168.4, 8 pages. English translation International Preliminary Report on Patentabil- ity and Written Opinion issued Dec. 28, 2021 in PCT/JP2020/025626, 6 pages. International Search Report issued Sep. 1, 2020 in PCT/JP2020/025626, 2 pages. Combined Chinese Office Action and Search Report issued Jul. 11, 2023 in Patent Application No. 202080047247.2 with Machine English translation, 37 pages. Combined Taiwanese Office Action and Search Report issued Feb. 7, 2024 in correspondingTaiwanese PatentApplication No. 109122058 (with machine English translation), 36 pages. Office Action issued Mar. 12, 2024 in corresponding Chinese Patent Application No. 202080047247.2 (with machine English transla- tion), 32 pages. Office Action issued Jun. 11, 2024 in corresponding Japanese Patent Application No. 2021-530031 (with machine English translation), 8 pages. Office Action issued May 28, 2024 in corresponding Korean Patent Application No. 10-2022-7003363 (with machine English transla- tion), 18 pages.
characterization XRDproperty XRD structurematerial GaN
FIG. 3 when XRD rocking curves are measured on the measurement line in the same manner and their peak 65 angles Go are plotted against the positions of the …
FIG. 13 are graphs showing the results of measuring the peak angles of (002) XRD rocking curves of a large-surface-area bulk GaN crystal at 5-mm intervals over …
IR absorption peak attributed to gallium vacancy-hydrogen complex
3140–3200 cm⁻¹
GaN
Thickness
50–55 mm
—
Thickness
75–80 mm
—
Thickness
100–105 mm
—
Thickness
150–155 mm
—
Thickness
3140–3200 cm
—
Thickness
≤ 5 mm
—
US 2017/0352721 A12017/0352721 A1 12/2017 Iso et al.
US 2019/0003078 A12019/0003078 A1 1/2019 D’Evelyn et al.
CN 109563642 ACN 109563642 A 4/2019
JP 2009018983 AJP 2009018983 A 1/2009
JP 2014534941 AJP 2014534941 A 12/2014
JP 2016088756 AJP 2016088756 A 5/2016
JP 2017031029 AJP 2017031029 A 2/2017
JP 2018024538 AJP 2018024538 A 2/2018
JP 2018024539 AJP 2018024539 A 2/2018
Cited non-patent literature · 2
JP 2018-024538 (Year: 2018).
Extended European Search Report issued Jun. 27, 2022 in EP Patent Application No. 20835168.4, 8 pages. English translation International Preliminary Report on Patentabil- ity and Written Opinion issued Dec. 28, 2021 in PCT/JP2020/025626, 6 pages. International Search Report issued Sep. 1, 2020 in PCT/JP2020/025626, 2 pages. Combined Chinese Office Action and Search Report issued Jul. 11, 2023 in Patent Application No. 202080047247.2 with Machine English translation, 37 pages. Combined Taiwanese Office Action and Search Report issued Feb. 7, 2024 in correspondingTaiwanese PatentApplication No. 109122058 (with machine English translation), 36 pages. Office Action issued Mar. 12, 2024 in corresponding Chinese Patent Application No. 202080047247.2 (with machine English transla- tion), 32 pages. Office Action issued Jun. 11, 2024 in corresponding Japanese Patent Application No. 2021-530031 (with machine English translation), 8 pages. Office Action issued May 28, 2024 in corresponding Korean Patent Application No. 10-2022-7003363 (with machine English transla- tion), 18 pages.
characterization XRDproperty XRD structurematerial GaN