CN112687609A - Method for growing AlN epitaxial layer by using graphite disc and substrate and graphite disc - Google Patents

Method for growing AlN epitaxial layer by using graphite disc and substrate and graphite disc Download PDF

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CN112687609A
CN112687609A CN202011558595.4A CN202011558595A CN112687609A CN 112687609 A CN112687609 A CN 112687609A CN 202011558595 A CN202011558595 A CN 202011558595A CN 112687609 A CN112687609 A CN 112687609A
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graphite
aln
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epitaxial layer
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不公告发明人
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Zhixin Semiconductor Hangzhou Co Ltd
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Abstract

The invention provides a method for growing an AlN epitaxial layer by using a graphite disc and a substrate, which comprises the graphite disc and the substrate for placing the substrate, and is characterized in that: 1) a circle of bulges with the height of 0.1-1mm are arranged on the graphite disc groove for placing the substrate close to the outer boundary and form a concentric ring structure with the bottom of the graphite disc groove; 2) etching the back of the edge of the substrate for one circle to form a groove with the depth of 0.1-0.5mm, wherein the formed annular groove is just matched with the protrusion on the surface of the graphite plate, so that the protrusion of the graphite plate can be embedded into the groove on the back of the etched substrate; 3) growing an AlN epitaxial layer by using the graphite disc and the substrate; the method solves the problem that the AlN layer is easy to crack for obtaining the AlN layer with higher crystal quality, reduces the influence of centrifugal force on the substrate, obtains a sheet source with better uniformity, integrates the two points and integrally improves the yield.

Description

Method for growing AlN epitaxial layer by using graphite disc and substrate and graphite disc
Technical Field
The invention relates to the technical field of semiconductor device manufacturing, in particular to a method for growing an AlN epitaxial layer by using a graphite disc and a substrate.
Background
A Light Emitting Diode (abbreviated as LED) is a solid semiconductor Diode Light Emitting device and is widely used in illumination fields such as indicator lights and display screens. The method for manufacturing the LED wafer at the present stage is mainly realized by Metal-organic Chemical Vapor Deposition (MOCVD), and the flow can be briefly described as follows: an epitaxial Wafer substrate (such as a sapphire substrate/a Si substrate) is placed on a groove of a graphite disc (Wafer carrier), the epitaxial Wafer substrate and the graphite disc are conveyed into an MOCVD reaction chamber together, the temperature of the reaction chamber is heated to a set temperature, and organic metal compounds and gases of five groups are introduced in a matched mode, so that chemical bonds of the epitaxial Wafer substrate and the organic metal compounds are broken on the Wafer substrate and the epitaxial Wafer substrate is polymerized again to form an LED epitaxial layer.
During the MOCVD epitaxy process, the phenomenon of excessive warping of the epitaxial wafer often occurs. Because the warped surface deflects the reflected light, temperature control is inaccurate, the epitaxial wafer is heated unevenly, distribution consistency of temperature-sensitive parameters such as wavelength and doping level in epitaxial growth cannot be controlled, and product performance is influenced finally. When the substrate is rotated at a high speed (200-1200 RPM), due to the action of centrifugal force, the crystal quantity at the central position of the substrate is possibly slightly smaller than that at the edge position in the epitaxial process, the stress distribution on the surface of the whole epitaxial wafer is possibly changed in the growth process, so that the central area of the substrate is tilted, the temperature of the area is low, on one hand, the phenomenon that the AlN part area grows and is not complete is caused, the AlN part area is scrapped, on the other hand, the wavelength of the subsequent LED epitaxial wafer is shifted, and the STD deviation is caused.
AlN belongs to a third-generation wide-bandgap semiconductor material, the crystal of AlN has a stable hexagonal wurtzite structure, the largest direct band gap is formed in the III-V semiconductor material, the AlN has high thermal conductivity, high resistivity, strong breakdown field and small dielectric coefficient, and is an excellent electronic material for high-temperature high-frequency and high-power devices. Further, AlN oriented along the c-axis has excellent piezoelectric characteristics and high-speed propagation of surface acoustic waves, and is an excellent piezoelectric material for surface acoustic wave devices. Meanwhile, AlN crystal and GaN crystal have very close lattice constants and thermal expansion coefficients, and are preferred substrate materials for epitaxially growing AlGaN photoelectric devices.
Although AlN has many advantages, AlN materials are very difficult to prepare. High temperature and high pressure equipment and a precise source flow control system are required for preparing AlN. Generally, the thicker the AlN film thickness deposited, the better the crystal quality of the AlN film. When the prepared AlN thin film has a certain thickness, surface cracks are easy to form because the lattice mismatch between AlN and the substrate is large, cracks are easy to generate from the edge of the substrate, and the cracks extend from the edge area to the central area along with the increase of the thickness, so that the yield is influenced. In order to obtain an AlN thin film with high crystal quality, the thickness of the thin film layer needs to be increased, but cracks are easily introduced, resulting in poor yield. In order to obtain a higher surface yield, the thickness of the AlN thin film layer is reduced, which in turn leads to a poorer crystal quality of the AlN thin film. This growth conflict of AlN thin films makes it currently difficult to obtain high quality crack-free AlN thin film substrates, resulting in very limited applications of AlN thin films.
Based on the reasons, the method for growing the AlN epitaxial layer by using the graphite plate and the substrate and the graphite plate can improve the crystal quality of the AlN thin film, reduce surface cracks of the AlN thin film, improve the yield and be beneficial to improving the performance of a device prepared on the AlN thin film material.
Disclosure of Invention
Aiming at the existing problems, the invention provides a method for growing an AlN epitaxial layer by using a graphite disc and a substrate and the graphite disc.
The invention provides a method for growing an AlN epitaxial layer by using a graphite disc and a substrate, which is characterized by comprising the following steps of:
1) a circle of bulges are formed on the graphite disc groove for placing the substrate close to the outer boundary, and a concentric ring structure is formed at the bottom of the graphite disc groove;
2) etching the back of the edge of the substrate to form an annular groove, wherein the formed annular groove is just matched with the protrusion on the surface of the graphite disc, so that the annular protrusion can be embedded into the groove on the back of the substrate;
3) and growing an AlN epitaxial layer on the substrate.
Furthermore, the raised structure in the graphite disc for placing the substrate is 0.5-5mm away from the groove boundary of the graphite disc, and the height of each region is consistent, the height is 0.1-1mm, and the width is 0.1-5 mm.
Furthermore, an annular groove with the depth of 0.1-0.5mm is etched on the back of the edge of the substrate, the formed annular groove is just matched with the protrusion on the surface of the graphite plate, the etching width is 0.1-5mm, and the distance between the etching position of the back of the substrate and the edge is 0.1-2 mm.
Further, the specially designed graphite plate and the substrate are placed in a reaction chamber of growth equipment, the temperature of the reaction chamber is controlled to be 600-;
compared with the prior art, the invention has the following advantages and beneficial effects:
1) during epitaxy, the stone is rotated at high speed, and the substrate is usually laid on the stone in the prior art and then rotates along with the stone, and the rotation amplitude is large, so that the substrate sometimes deviates from the initial position greatly, and the substrate epitaxy positions at different positions on the disc are different greatly. In this case, the initial positions of crystal growth may be different as the epitaxial wafer rotates, and the number of crystals at the central position of the substrate may be smaller than that at the edge position under the action of centrifugal force, which may cause the stress distribution on the surface of the entire epitaxial wafer to change during the growth process, thereby tilting the central region of the substrate. According to the invention, the graphite disc and the substrate adopt a fit mode, so that the substrate cannot rotate greatly, the position of each substrate in the large disc is consistent, the uniformity between wafers can be improved, the warpage can be reduced, the uniformity in the wafers can be improved, the problem of large warpage of the central region of the substrate caused by large centrifugal force is solved, the phenomenon that the AlN partial region grows and is combined incompletely due to low temperature of the central region of the epitaxial wafer is avoided, the rejection rate is greatly reduced, the wavelength uniformity of the subsequently grown LED is improved, and the STD deviation is reduced.
2) The temperature of the area where the graphite plate and the substrate are in direct contact is higher than that of the other areas which are not in contact. Therefore, during AlN growth, in the region where the graphite disk and the substrate are in direct contact, the longitudinal growth rate is higher than the lateral growth rate, and thus the contacted region may generate a dense hexagonal columnar structure. The stress buffer area formed by the defects can prevent the cracks of the substrate edge layer from extending to the center, thereby improving the yield.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed to be used in the description of the embodiments or the prior art will be briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a schematic cross-sectional view of a substrate groove of a graphite disk according to an embodiment of the present invention;
fig. 2 is a schematic cross-sectional view of a substrate groove of a graphite disk according to yet another embodiment of the present invention;
FIG. 3 is a schematic cross-sectional view of a substrate groove of a graphite disk according to yet another embodiment of the present invention;
FIG. 4 is a top view of the back side of a substrate according to the present invention;
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more apparent, embodiments of the present invention will be described in detail below with reference to the accompanying drawings. However, it will be appreciated by those of ordinary skill in the art that numerous technical details are set forth in order to provide a better understanding of the present application in various embodiments of the present invention. However, the technical solution claimed in the present application can be implemented without these technical details and various changes and modifications based on the following embodiments. The following embodiments are divided for convenience of description, and should not constitute any limitation to the specific implementation manner of the present invention, and the embodiments may be mutually incorporated and referred to without contradiction.
The present invention will be described in detail with reference to specific examples.
Example 1
A method for growing an AlN epitaxial layer by using a graphite plate and a substrate comprises the following specific steps:
1) the schematic cross-sectional view of the graphite disc groove is shown in fig. 1 and is in an inverted trapezoid shape. A circle of convex structures are arranged on the graphite plate groove for placing the substrate close to the outer boundary, and a concentric ring structure is formed at the bottom of the graphite plate groove. The protruding structure 1 in the graphite plate groove is of a continuous circular ring structure, the distance from the upper boundary of the graphite plate groove is 1.5mm, and the heights of all the areas of the circular ring protruding structure are consistent. The height of the annular convex structure is higher than the thickness of the substrate, and the wider the annular convex structure is, the better the effect is, but the surface yield of the epitaxial wafer is seriously influenced by the too wide annular convex structure, and the annular convex structure is preferably 0.5mm high and 1mm wide.
2) A substrate is provided having a backside top view as shown in fig. 4. The back of the edge of the substrate is etched to form an annular groove 4 with the depth of 0.2mm and the width of 1.1mm, the distance between the annular groove 4 and the edge of the back of the substrate is 1mm, the formed annular groove 4 is just matched with the surface protrusion of the graphite plate, and the annular protrusion can be embedded into the groove 4 of the back of the substrate. Meanwhile, the height of the protruding structure 1 of the graphite disc is 0.5mm, the depth of the annular groove 4 of the substrate is 0.2mm, after the protrusion is embedded into the groove 4 on the back of the substrate, the back of the substrate is not contacted with the groove surface of the graphite disc, namely only the groove surface of the substrate is contacted with the surface of the protruding structure of the graphite disc, and the part outside the groove of the substrate is not contacted with the groove of the graphite disc, so that when AlN grows, the temperature of the area where the protruding structure of the graphite disc is directly contacted with the groove of the substrate is higher than that of other areas which are not contacted, the longitudinal growth speed of the area is higher than the transverse growth speed, and the contacted area can generate an intensive hexagonal columnar structure. The thickness of the substrate is usually within 0.5mm, the annular groove 4 cannot be etched too deeply, otherwise the substrate is easy to break; the width of the groove is not too large, otherwise, the area of the substrate in direct contact with the stone grinding disc is increased, the area generated by dense hexagon is increased, the area with rough surface is increased, and the surface yield is influenced.
3) Placing the substrate in the step 2) in the graphite disc in the step 1) and transferring the substrate into a reaction chamber of MOCVD.
Specifically, the temperature of the reaction chamber is controlled to be 650 DEG C50ml of TMAl and 2500ml of NH are introduced into the reaction chamber3And controlling the pressure of the reaction chamber to be 100mbar, and growing the AlN buffer layer with the thickness of 30 nm. Controlling the temperature of the reaction chamber to 1400 ℃ and the pressure to 50mbar, and introducing 150ml of TMAl and 5000ml of NH into the reaction chamber3After that, growth was carried out for 2 hours, to obtain an AlN layer having a thickness of 2000 nm.
The edge of the AlN layer is a dense hexagonal area, surface cracks are few, the cracks are blocked outside the hexagonal area, no extension exists, and no atomization area exists on the surface of the whole AlN layer.
The obtained AlN layer having high crystal quality and a good surface was subjected to XRD testing, in which the half width in the (002) direction was 150arcsec and the half width in the (102) direction was 380 arcsec.
Example 2
A method for growing an AlN epitaxial layer by using a graphite plate and a substrate comprises the following specific steps:
1) a graphite disk groove is provided, the schematic cross-sectional view of which is shown in fig. 2. A circle of convex structures are arranged on the graphite plate groove for placing the substrate close to the outer boundary, and a concentric ring structure is formed at the bottom of the graphite plate groove. The raised structure 2 in the graphite plate groove is a discontinuous columnar structure, all columnar structures are combined together to form a ring shape, the distance from the graphite plate groove boundary is 1.5mm, the heights of all regions of the raised structure are consistent, the raised size is preferably 0.5mm high and 0.9mm wide, and the distance between the front columnar raised structure and the rear columnar raised structure is 0.01 mm.
2) A substrate is provided having a backside top view as shown in fig. 4. The back of the edge of the substrate is etched to form an annular groove 4 with the depth of 0.2mm and the width of 1mm, the distance between the annular groove 4 and the edge of the back of the substrate is 0.7mm, and the formed annular groove 4 is just matched with the surface protrusion of the graphite plate, so that the columnar protrusion can be embedded into the groove 4 of the back of the substrate.
3) Placing the substrate in the step 2) in the graphite disc in the step 1), transferring the substrate into a reaction chamber of MOCVD (metal organic chemical vapor deposition), controlling the temperature of the reaction chamber to be 650 ℃, and introducing 50ml of TMAl and 2500ml of NH into the reaction chamber3And controlling the pressure of the reaction chamber to be 100mbar, and growing the AlN buffer layer with the thickness of 30 nm. The temperature of the reaction chamber is controlled at 1400 ℃ and the pressure is controlled at 50mbar180ml of TMAl and 5000ml of NH are introduced into the reaction chamber3After that, the growth was carried out for 2 hours, to obtain an AlN layer having a thickness of 2500 nm.
The edge of the AlN layer is a dense hexagonal area, surface cracks are few, the cracks are blocked outside the hexagonal area, no extension exists, and no atomization area exists on the surface of the whole AlN layer.
The obtained AlN layer having high crystal quality and a good surface was subjected to XRD testing, in which the half width in the (002) direction was 130arcsec and the half width in the (102) direction was 350 arcsec.
Example 3
A method for growing an AlN epitaxial layer by using a graphite plate and a substrate comprises the following specific steps:
1) a graphite disk groove is provided, the schematic cross-sectional view of which is shown in fig. 3. A circle of convex structures are arranged on the graphite plate groove for placing the substrate close to the outer boundary, and a concentric ring structure is formed at the bottom of the graphite plate groove. Protruding structure 3 is discontinuous pile column structure in the graphite plate recess, and apart from graphite plate recess boundary 1.5mm, and each regional highly unanimous of protruding structure, height 0.5mm, upward wide 0.5mm, lower wide 0.9mm, and the interval is 0.015mm between the preceding back pile column protruding structure.
2) A substrate is provided having a backside top view as shown in fig. 4. The back of the edge of the substrate is etched to form an annular groove 4 with the depth of 0.25mm and the width of 1mm, the distance between the annular groove 4 and the edge of the back of the substrate is 0.5mm, and the formed annular groove 4 is just matched with the surface protrusion of the graphite plate, so that the columnar protrusion can be embedded into the groove 4 of the back of the substrate.
3) Placing the substrate in the step 2) in the graphite disc in the step 1), transferring the substrate into a reaction chamber of MOCVD (metal organic chemical vapor deposition), controlling the temperature of the reaction chamber to be 650 ℃, and introducing 50ml of TMAl and 2500ml of NH into the reaction chamber3And controlling the pressure of the reaction chamber to be 100mbar, and growing the AlN buffer layer with the thickness of 30 nm. Controlling the temperature of the reaction chamber to 1400 ℃ and the pressure to 50mbar, and introducing 200ml of TMAl and 5000ml of NH into the reaction chamber3After that, growth was carried out for 2.5h, to obtain an AlN layer having a thickness of 4500 nm.
The edge of the AlN layer is a dense hexagonal area, surface cracks are few, the cracks are blocked outside the hexagonal area, no extension exists, and no atomization area exists on the surface of the whole AlN layer.
The obtained AlN layer having high crystal quality and a good surface was subjected to XRD testing, in which the half width in the (002) direction was 95arcsec and the half width in the (102) direction was 280 arcsec.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.

Claims (14)

1. A method for growing an AlN epitaxial layer by using a graphite plate and a substrate is characterized by comprising the following steps:
1) a circle of bulges with the height of 0.1-1mm are formed on the graphite disc groove for placing the substrate close to the outer boundary, and the bulges and the bottom of the graphite disc groove form a concentric ring structure;
2) etching the back of the edge of the substrate to form an annular groove with the depth of 0.1-0.5mm, and fitting the formed annular groove with the annular bulge on the surface of the graphite plate to embed the annular bulge on the surface of the graphite plate into the groove on the back of the substrate;
3) and growing an AlN epitaxial layer on the substrate.
2. The method for growing the AlN epitaxial layer by using the graphite disc and the substrate according to claim 1, wherein the raised structures in the graphite disc for placing the substrate are 0.5-5mm away from the groove boundaries of the graphite disc.
3. The method for growing the AlN epitaxial layer by using the graphite disc and the substrate according to claim 1, wherein the raised structures in the graphite disc for placing the substrate are selected from one of a circular ring structure, a plurality of discontinuous columnar structures, a plurality of discontinuous truncated-cone-shaped structures or a conical-shaped structure.
4. A method for growing AlN epitaxial layers by using a graphite plate and a substrate according to claim 1 or 3, wherein the height of each region of the convex structure of the graphite plate is consistent and is 0.1-1 mm.
5. A method of growing AlN epitaxial layer using graphite disks and substrates according to any of claims 1-3, wherein the graphite disk projection structures are 0.1-5mm wide.
6. A method for growing AlN epitaxial layer using graphite disks and substrates according to any one of claims 1-3, wherein the graphite disk protrusion structures form concentric circular ring structures with the bottom of the graphite disk groove.
7. The method for growing the AlN epitaxial layer by using the graphite disc and the substrate according to claim 1, wherein the width of the back side etching of the substrate is 0.1-5 mm.
8. The method for growing the AlN epitaxial layer by using the graphite disc and the substrate according to claim 1, wherein the back side of the substrate is etched at a position 0.1-2mm away from the edge.
9. The method for growing the AlN epitaxial layer by using the graphite plate and the substrate according to claim 1, wherein the AlN epitaxial layer in the step 3) comprises an AlN buffer layer and an AlN layer grown on the AlN buffer layer.
10. The method for growing the AlN epitaxial layer by using the graphite disc and the substrate according to claim 1, wherein the step 3) specifically comprises the following steps: and placing the graphite disc and the substrate into a reaction chamber of growth equipment, controlling the temperature of the reaction chamber to be 600-1200 ℃, introducing trimethylaluminum and ammonia gas into the reaction chamber to grow an AlN buffer layer, then controlling the temperature of the reaction chamber to be 1100-1500 ℃, and introducing the trimethylaluminum and the ammonia gas into the reaction chamber at a pressure of 20-400mbar to generate an AlN layer on the AlN buffer layer.
11. The method for growing the AlN epitaxial layer by using the graphite plate and the substrate as claimed in claim 10, wherein the AlN epitaxial layer has a thickness of a, and 0.5. ltoreq. a.ltoreq.5 μm.
12. A graphite disk for growing AlN epitaxial layers, comprising: the graphite plate groove for placing the substrate is inverted trapezoid in longitudinal section, a circle of protruding structures are arranged on the graphite plate groove close to the outer boundary, the protruding structures and the bottom of the graphite plate groove form a concentric ring structure, and the heights of all the regions of the ring protruding structures are consistent.
13. A graphite disk for growing AlN epitaxial layers according to claim 12, wherein the raised structures are 1.5mm from the upper boundary of the graphite disk recess, and the annular raised structures are 0.5mm high and 1mm wide.
14. A graphite disk for growing AlN epitaxial layer according to claim 12, wherein the raised structures in the graphite disk on which the substrate is placed are selected from one of a circular ring structure, a plurality of discontinuous columnar structures, a plurality of discontinuous mesa-like or pyramidal structures.
CN202011558595.4A 2020-12-25 Method for growing AlN epitaxial layer by using graphite plate and substrate and graphite plate Active CN112687609B (en)

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Cited By (1)

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Publication number Priority date Publication date Assignee Title
CN114645324A (en) * 2022-03-29 2022-06-21 江苏鹏举半导体设备技术有限公司 Graphite plate based on MOCVD equipment

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CN105442039A (en) * 2015-12-30 2016-03-30 晶能光电(常州)有限公司 Graphite disc for accommodating silicon substrate for MOCVD (metal-organic chemical vapor deposition)
CN109183001A (en) * 2018-11-27 2019-01-11 中山德华芯片技术有限公司 A kind of graphite plate applied to epitaxial growth of semiconductor material growth
CN210314481U (en) * 2019-07-31 2020-04-14 安徽三安光电有限公司 Graphite plate and matched substrate thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2006222134A (en) * 2005-02-08 2006-08-24 Hitachi Cable Ltd Tray for semiconductor wafer
CN103824796A (en) * 2014-01-07 2014-05-28 苏州新纳晶光电有限公司 Graphite bearing disc for LED epitaxial process, and matching substrate thereof
CN203839357U (en) * 2014-05-12 2014-09-17 保定天威英利新能源有限公司 Fixing pallet for chip carrying boxes for silicon chips
CN105442039A (en) * 2015-12-30 2016-03-30 晶能光电(常州)有限公司 Graphite disc for accommodating silicon substrate for MOCVD (metal-organic chemical vapor deposition)
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Publication number Priority date Publication date Assignee Title
CN114645324A (en) * 2022-03-29 2022-06-21 江苏鹏举半导体设备技术有限公司 Graphite plate based on MOCVD equipment

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