CN113463200B - Limited area growth ring for HVPE reaction furnace and nitride crystal growth method - Google Patents

Limited area growth ring for HVPE reaction furnace and nitride crystal growth method Download PDF

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CN113463200B
CN113463200B CN202110711924.2A CN202110711924A CN113463200B CN 113463200 B CN113463200 B CN 113463200B CN 202110711924 A CN202110711924 A CN 202110711924A CN 113463200 B CN113463200 B CN 113463200B
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CN113463200A (en
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王新强
刘强
刘放
盛博文
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Peking University
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    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10—Inorganic compounds or compositions
    • C30B29/40—AIIIBV compounds wherein A is B, Al, Ga, In or Tl and B is N, P, As, Sb or Bi
    • C30B29/403—AIII-nitrides
    • C30B29/406—Gallium nitride
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    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
    • C30B25/02—Epitaxial-layer growth

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Abstract

The invention discloses a limited-area growth ring for an HVPE reaction furnace and a nitride crystal growth method. The method adopts one of tungsten, ruthenium and molybdenum, or adopts a carbide or nitride of one of tungsten, ruthenium and molybdenum to make the functional surface of the confinement growth ring have chemical activity through cleaning, annealing and activation; the limited-area growth ring is placed in a growth area of a reaction furnace, and the limited-area growth ring limits the lateral growth of the crystal in the growth process, so that the edge growth of the crystal is prevented, the edge effect in the growth process is prevented, the stress generated in the growth process is reduced, and the growth of centimeter-level GaN bulk crystals is finally realized; the method is simple, can be easily realized according to the prior art level, and is widely popularized; the zone-limited growth ring can be repeatedly used after being thermally cleaned, so that the manufacturing cost of the zone-limited growth ring is saved, and the method is economical and practical; the zone-limited growth ring can be optimally designed according to different structures of growth areas of different HVPE reaction furnaces, and the universality is high.

Description

Limited area growth ring for HVPE reaction furnace and nitride crystal growth method
Technical Field
The invention relates to a nitride crystal growth technology, in particular to a limited-area growth ring for an HVPE reaction furnace and a nitride crystal growth method.
Background
The III-V nitride material has good optical and electrical properties, so that the III-V nitride material has great application value in the fields of high-efficiency light-emitting devices, photoelectric conversion devices, power electronic devices, integrated circuits, sensing devices and the like. In recent years, nitride crystal growth technology has become the core of strategic development of high technology industries in various countries, and a Hydride Vapor Phase Epitaxy (HVPE) reactor is a common nitride (GaN) crystal growth apparatus. In recent years, the growth technology of GaN free-standing substrates based on HVPE method has become the mainstream technology for producing commercial GaN free-standing substrates. In order to obtain a GaN crystal body with a thickness of centimeter level, the edge effect of GaN in an HVPE growth furnace needs to be solved, namely, the edge is easy to grow polycrystal due to the sudden change of physical parameters such as an airflow field, temperature, growth crystal face and the like, the growth rate of the edge is higher than that of a central area, the crystal lattice constant and impurity concentration of the edge are different from those of the central area and the like.
At present, the thickness of the gallium nitride self-supporting substrate is generally less than 1 millimeter, so the problem of the edge effect is not serious, and the problem caused by the edge effect can be relieved by reducing the growth rate or using a seed crystal groove with proper depth. For the next generation of GaN crystal growth technology, the problem of edge effect cannot be solved by the conventional method in order to realize the growth of cm-thick GaN crystal, so it is necessary to develop a new technology to solve the problem of edge effect.
Disclosure of Invention
Aiming at the problem of edge effect generated in the growth process of a GaN crystal in an HVPE reaction furnace, the invention provides a limited-area growth ring for the HVPE reaction furnace and a nitride crystal growth method.
One object of the present invention is to provide a confinement growth ring for use in crystal growth that inhibits lateral growth.
The invention relates to a limited-area growth ring for inhibiting lateral growth in crystal growth, which is made of one of tungsten, ruthenium and molybdenum or carbide or nitride of one of tungsten, ruthenium and molybdenum; forming the material of the limited area growth ring into a block material by adopting a powder metallurgy method, a smelting method, a chemical vapor deposition method or a hot-pressing sintering technology, forming a flat plate with a through hole in the center by machining and forming, wherein the through hole is circular or polygonal, or forming a plurality of limited area sections, each limited area section is a part of a circular ring or a polygonal ring, the plurality of limited area sections are positioned on the same circular ring or the polygonal ring, the distance between the adjacent limited area sections is not more than 3mm, preparing the limited area growth ring, and the shape of the inner edge of the limited area growth ring is consistent with the shape of the outer edge of a seed crystal for growing the gallium nitride crystal; the ring surface parallel to the growth surface of one crystal seed for gallium nitride crystal growth on the limited-area growth ring is the functional surface of the limited-area growth ring, and the functional surface of the limited-area growth ring is mechanically treated to ensure that the surface roughness of the limited-area growth ring is 0.1 nm-10 mu m, enhance the limited areaChemical catalytic performance of the functional surface of the domain growth ring; the thickness of the limited area growth ring is 0.5 mm-1 cm; the inner diameter of the zone-limited growth ring is D1The outer diameter of the zone-limited growth ring is D2A seed crystal for gallium nitride crystal growth having a diameter D satisfying D1≤d+3mm，D2D +5 mm; the purity of the material of the confinement growth ring needs to be higher than 99%.
Further, the inner diameter and the outer diameter of the zone-limited growth ring respectively satisfy: d1≥2mm；D2≤d+100mm。
The thickness of the limited area growth ring is larger than that of a seed crystal for growing the gallium nitride crystal.
Another object of the present invention is to provide a confinement growth ring for use in a nitride crystal growth method.
The method for growing the nitride crystal by using the limited-area growth ring comprises the following steps:
1) preparing a limited-area growth ring:
forming the material of the limited area growth ring into a block material by adopting a powder metallurgy method, a smelting method, a chemical vapor deposition method or a hot-pressing sintering technology, and then forming a flat plate with a through hole in the center through machining and forming, wherein the through hole is circular or polygonal, or forming a plurality of limited area sections, the plurality of limited area sections are positioned on the same circular ring or polygonal ring, the distance between adjacent limited area sections is not more than 3mm, and the limited area growth ring is prepared, wherein the shape of the inner edge of the limited area growth ring is consistent with the shape of the outer edge of a seed crystal for gallium nitride crystal growth; the ring surface parallel to a crystal seed growth surface for growing the gallium nitride crystal on the limited-area growth ring is a functional surface of the limited-area growth ring, and the functional surface of the limited-area growth ring is mechanically processed, so that the surface roughness of the limited-area growth ring is 0.1 nm-10 mu m, and the performance of the functional surface of the limited-area growth ring is enhanced; the thickness of the limited area growth ring is 0.5 mm-1 cm; the inner diameter of the zone-limited growth ring is D1The outer diameter of the zone-limited growth ring is D2A seed crystal for gallium nitride crystal growth having a diameter D satisfying D1≤d+3mm，D2≥d+5mm；
2) Cleaning a limited growth ring:
firstly, organic cleaning is carried out on the limited area growth ring by adopting an inorganic cleaning solution, then organic cleaning is carried out on the limited area growth ring by adopting an organic cleaning solution, residues and dirt on the functional surface of the limited area growth ring during mechanical processing and forming are removed, and the surface of the functional surface of the limited area growth ring is cleaned;
3) thermal annealing of the limited-area growth ring:
in a set gas atmosphere, controlling annealing temperature and annealing time, carrying out thermal annealing on the confinement growth ring, removing residual stress in the confinement growth ring, and preliminarily activating a functional surface of the confinement growth ring;
4) activation of the surface of the confinement growth ring:
controlling the temperature and the pressure to enable the functional surface of the limited area growth ring to be in an activated gas atmosphere, maintaining the set time, and activating the functional surface of the limited area growth ring;
5) for the growth of nitride crystals:
placing a limited-area growth ring in a growth area of an HVPE reaction furnace, placing a seed crystal for growing a gallium nitride crystal in the growth area of the HVPE reaction furnace, and enabling a functional surface of the limited-area growth ring to surround an outer ring area of the seed crystal for growing the gallium nitride crystal or cover or partially cover the edge of the seed crystal for growing the gallium nitride crystal to grow a nitride crystal, wherein the nitride crystal can not grow on the functional surface of the limited-area growth ring completely, so that the limited-area growth ring limits the lateral growth of the crystal in the growth process, prevents the edge of the crystal from growing, inhibits the edge effect in the growth process, and finally obtains a centimeter-level GaN bulk crystal;
6) thermal cleaning of the confinement growth ring:
after the primary crystal growth is finished, taking out the limited-area growth ring from the growth area of the HVPE reaction furnace, controlling the temperature and the pressure, using cleaning gas, adopting a thermal cleaning process to clean the functional surface of the limited-area growth ring, and removing residues on the surface of the functional surface of the limited-area growth ring in the growth process, so that the limited-area growth ring can be recycled;
7) and (4) starting the next round of crystal growth according to the steps 4) to 6), and realizing the recycling of the limited area growth ring.
In step 1), one of tungsten, ruthenium and molybdenum or a carbide or a nitride of one of tungsten, ruthenium and molybdenum is used as the material of the domain-limited growth ring. The purity of the material of the confinement growth ring needs to be higher than 99%. And (3) carrying out mechanical treatment on the functional surface of the confinement growth ring, and adopting one of mechanical grinding, chemical mechanical polishing and electrolytic grinding to ensure that the surface roughness of the confinement growth ring meets the requirement.
In the step 2), the inorganic cleaning solution is one or a mixture of any more of acetone, isopropanol and deionized water, and one-step or multi-step inorganic cleaning is carried out; the inorganic cleaning condition is ultrasonic cleaning at normal temperature of 40 kHz-80 kHz, and the cleaning time is from 5 minutes to 30 minutes. The organic cleaning melt is a mixed solution of hydrochloric acid, hydrogen peroxide and water in any proportion, the cleaning temperature is 50-120 ℃, and the cleaning time is 5-30 minutes.
In the step 3), the gas atmosphere of the thermal annealing is vacuum, the pressure during the thermal annealing is less than 10Pa, the temperature of the thermal annealing is 1000-1500 ℃, and the time is 30 minutes to 10 hours.
In the step 4), activating gas is one or more of nitrogen, hydrogen and ammonia; the temperature is 1000-1500 ℃, and the pressure is 10-101 kPa; the treatment time is 30 minutes to 5 hours. The step of activating the gas to process the confinement growth ring is one-step processing or multi-step processing, wherein the multi-step processing is to sequentially introduce different gases for thermal cleaning according to a time sequence.
In step 5), when the inner diameter is larger than the diameter of the seed crystal, the distance between the inner diameter of the limited area growth ring and the outer edge of the seed crystal for gallium nitride crystal growth is less than 3 mm.
In the step 6), the gas is a plurality of combinations of nitrogen, hydrogen and hydrogen chloride; the temperature is 1000-1500 ℃, and the pressure is 10-101 kPa; the treatment time is 30 minutes to 5 hours.
The invention has the advantages that:
the method adopts one of tungsten, ruthenium and molybdenum, or adopts a carbide or nitride of one of tungsten, ruthenium and molybdenum to make the functional surface of the confinement growth ring have chemical activity through cleaning, annealing and activation; placing the limited-area growth ring in a growth area of a reaction furnace, and enabling a functional surface of the limited-area growth ring to surround an outer ring area of a seed crystal for gallium nitride crystal growth or cover the edge of the seed crystal for gallium nitride crystal growth to perform nitride crystal growth, wherein the limited-area growth ring limits the lateral growth of the crystal in the growth process, so that the edge growth of the crystal is prevented, the edge effect generated in the growth process is restrained, the stress generated in the growth process is reduced, and the centimeter-level GaN bulk crystal growth is finally realized; the method for realizing the limited domain growth ring is simple, can be easily realized according to the prior art level, and is widely popularized; the zone-limited growth ring can be repeatedly used after being thermally cleaned, so that the manufacturing cost of the zone-limited growth ring is saved, and the method is economical and practical; the zone-limited growth ring can be optimally designed according to different structures of growth areas of different HVPE reaction furnaces, and the universality is high.
Drawings
FIG. 1 is a flow chart of a method of using a confined growth ring of the present invention for nitride crystal growth;
FIG. 2 is a schematic view of an embodiment of a confined growth ring for inhibiting lateral growth in crystal growth of the present invention placed in a growth furnace, wherein (a) is a side view and (b) is a top view;
FIG. 3 is a schematic view of a second embodiment of a confinement growth ring for inhibiting lateral growth in crystal growth in accordance with the invention;
FIG. 4 is a schematic view of a third embodiment of a confinement growth ring for inhibiting lateral growth in crystal growth in accordance with the present invention.
Detailed Description
The invention will be further elucidated by means of specific embodiments in the following with reference to the drawing.
Example one
In this embodiment, the through hole at the center of the growth-limited ring is circular, and the growth-limited ring is a complete circular ring.
As shown in fig. 1, the limited growth ring of the present embodiment is used in a nitride crystal growth method, including the steps of:
1) preparing a limited-area growth ring:
tungsten with the purity higher than 99.95% is formed into a block material by a powder metallurgy method, and then is formed into a ring shape by machining, so that a limited-area growth ring is prepared; the ring surface parallel to a crystal seed growth surface for growing the gallium nitride crystal on the limited-area growth ring is a functional surface of the limited-area growth ring, and the functional surface of the limited-area growth ring is mechanically processed, so that the surface roughness of the limited-area growth ring is 5 microns, and the performance of the functional surface of the limited-area growth ring is enhanced; the thickness of the confinement growth ring is 2 mm; inner diameter D of the confinement growth ring150.8mm, the outer diameter D of the limited area growth ring2Is 55 mm;
2) cleaning a limited growth ring:
cleaning a confinement ring for 15 minutes by using acetone under the ultrasonic condition of 40kHz, and then sequentially cleaning for 15 minutes by using isopropanol and deionized water respectively; after washing, hydrochloric acid was used: hydrogen peroxide: water 1: 1: 1 for 15 minutes at 80 ℃, and removing residues and dirt on the functional surface of the limited area growth ring during mechanical processing and molding, so that the surface of the functional surface of the limited area growth ring is clean;
3) thermal annealing of the limited-area growth ring:
carrying out thermal annealing on the limited domain growth ring for 1 hour in a vacuum atmosphere of 0.01Pa and at the temperature of 1200 ℃, removing residual stress in the limited domain growth ring, and preliminarily activating a functional surface of the limited domain growth ring;
4) activation of the surface of the confinement growth ring:
controlling the temperature and the pressure to enable the functional surface of the limited area growth ring to be in a nitrogen state: hydrogen gas: ammonia gas 5: 2: 3, treating the surface of the confinement ring at 1100 ℃ for 30 minutes by using the mixed gas, and activating a functional surface of the confinement growth ring;
5) for the growth of nitride crystals:
the center of the tray 203 has a groove having the same depth as the thickness of the gallium nitride crystal growth seed 202, the gallium nitride crystal growth seed 202 is placed in the groove of the tray 203, the tray 203 is placed in the growth zone of the HVPE reactor, the limited area growth ring 201 is placed on the edge of the tray 203, the thickness of the limited area growth ring is larger than that of a seed crystal used for growing the gallium nitride crystal, the HVPE reaction furnace growth area is placed in such a way that the functional surface of the limited area growth ring surrounds the outer ring area of the seed crystal used for growing the gallium nitride crystal, the distance between the inner edge of the limited area growth ring and the outer edge of the seed crystal is 0.5mm, as shown in fig. 2, nitride crystal growth is carried out, the growth of the crystal in the lateral direction is limited by a limited-area growth ring during the growth process, thereby preventing the edge growth of the crystal, inhibiting the edge effect generated in the growth process and finally obtaining the centimeter-level GaN bulk crystal;
6) thermal cleaning of the confinement growth ring:
after the primary crystal growth is finished, 1% hydrogen chloride gas and 99% hydrogen gas are subjected to a thermal cleaning process for 1 hour, the functional surface of the confinement growth ring is cleaned, and residues on the surface of the functional surface of the confinement growth ring in the growth process are removed, so that the confinement growth ring can be recycled;
7) and (4) starting the next round of crystal growth according to the steps 4) to 6), and realizing the recycling of the limited area growth ring.
Example two
In this embodiment, the through hole at the center of the growth-limiting ring is an irregular polygon, as shown in fig. 3, which is the same as the first embodiment.
EXAMPLE III
In this embodiment, the confinement growth ring includes multiple confinement sections, each of which is a part of a circular ring, the multiple confinement sections are located in the same circular ring shape, and the distance between adjacent confinement sections is 2mm, as shown in fig. 4, other embodiments are the same as those of the first embodiment.
Finally, it is noted that the disclosed embodiments are intended to aid in further understanding of the invention, but those skilled in the art will appreciate that: various substitutions and modifications are possible without departing from the spirit and scope of the invention and the appended claims. Therefore, the invention should not be limited to the embodiments disclosed, but the scope of the invention is defined by the appended claims.

Claims (7)

1. A method for nitride crystal growth using a confinement growth ring for an HVPE reactor, the method comprising the steps of:
1) preparing a limited-area growth ring:
forming the material of the limited-area growth ring into a block material by adopting a powder metallurgy method, a smelting method, a chemical vapor deposition method or a hot-pressing sintering technology, wherein the material of the limited-area growth ring adopts one of tungsten, ruthenium and molybdenum, or adopts carbide or nitride of one of tungsten, ruthenium and molybdenum; the purity of the material of the limited growth ring needs to be higher than 99%; then, a flat plate with a through hole in the center is formed through machining forming, the through hole is in a circular or polygonal shape, or a plurality of sections of limited area sections are formed, the plurality of sections of limited area sections are positioned on the same circular or polygonal ring, the distance between adjacent limited area sections is not more than 3mm, a limited area growth ring is prepared, and the shape of the inner edge of the limited area growth ring is consistent with the shape of the outer edge of a seed crystal for growing the gallium nitride crystal; an annular surface parallel to a crystal seed growth surface for gallium nitride crystal growth on the limited-area growth ring is a functional surface of the limited-area growth ring, and the functional surface of the limited-area growth ring is mechanically treated, so that the surface roughness of the limited-area growth ring is 0.1 nm-10 mu m, and the performance of the functional surface of the limited-area growth ring is enhanced; the thickness of the confinement growth ring is 0.5 mm-1 cm; the inner diameter of the confinement growth ring isD 1 The outside diameter of the zone-limited growth ring isD 2 One seed crystal for gallium nitride crystal growth has a diameter ofdSatisfy 2mm ≤D 1 ≤d+3mm，d+5mm≤D 2 ≤d+100mm；
2) Cleaning a limited growth ring:
firstly, organic cleaning is carried out on the limited area growth ring by adopting an inorganic cleaning solution, then organic cleaning is carried out on the limited area growth ring by adopting an organic cleaning solution, residues and dirt on the functional surface of the limited area growth ring during mechanical processing and forming are removed, and the surface of the functional surface of the limited area growth ring is cleaned;
3) thermal annealing of the limited-area growth ring:
in a set gas atmosphere, controlling annealing temperature and annealing time, carrying out thermal annealing on the confinement growth ring, removing residual stress in the confinement growth ring, and preliminarily activating a functional surface of the confinement growth ring;
4) activation of the surface of the confinement growth ring:
controlling the temperature and the pressure to enable the functional surface of the limited area growth ring to be in an activated gas atmosphere, maintaining the set time, and activating the functional surface of the limited area growth ring;
5) for the growth of nitride crystals:
placing a limited-area growth ring in a growth area of an HVPE reaction furnace, placing a seed crystal for growing a gallium nitride crystal in the growth area of the HVPE reaction furnace, and enabling a functional surface of the limited-area growth ring to surround an outer ring area of the seed crystal for growing the gallium nitride crystal or cover or partially cover the edge of the seed crystal for growing the gallium nitride crystal to grow a nitride crystal, wherein the nitride crystal can not grow on the functional surface of the limited-area growth ring completely, so that the limited-area growth ring limits the lateral growth of the crystal in the growth process, prevents the edge of the crystal from growing, inhibits the edge effect in the growth process, and finally obtains a centimeter-level GaN bulk crystal;
6) thermal cleaning of the confinement growth ring:
after the primary crystal growth is finished, taking out the limited-area growth ring from the growth area of the HVPE reaction furnace, controlling the temperature and the pressure, using cleaning gas, adopting a thermal cleaning process to clean the functional surface of the limited-area growth ring, and removing residues on the surface of the functional surface of the limited-area growth ring in the growth process, so that the limited-area growth ring can be recycled;
7) and 4) starting the next round of crystal growth according to the steps 4) -6), and realizing the recycling of the limited area growth ring.
2. The method of claim 1, wherein in step 1), the functional surface of the growth-limiting ring is mechanically treated by one of mechanical grinding, chemical mechanical polishing and electrolytic grinding to achieve a desired surface roughness of the growth-limiting ring.
3. The method as claimed in claim 1, wherein in step 2), the inorganic cleaning solution is one or a mixture of any of acetone, isopropanol and deionized water, and one or more steps of inorganic cleaning are carried out; the inorganic cleaning condition is ultrasonic cleaning of 40 kHz-80 kHz at normal temperature, and the cleaning time is from 5 minutes to 30 minutes.
4. The method as claimed in claim 1, wherein in the step 2), the organic cleaning solution is a mixed solution of hydrochloric acid, hydrogen peroxide and water in any proportion, the cleaning temperature is 50 ℃ to 120 ℃, and the cleaning time is 5 minutes to 30 minutes.
5. The method of claim 1, wherein in step 3), the gas atmosphere for thermal annealing is vacuum, the pressure for thermal annealing is less than 10Pa, and the temperature for thermal annealing is 1000 ℃ to 1500 ℃ for 30 minutes to 10 hours.
6. The method of claim 1, wherein in step 4), the activating gas is one or more of nitrogen, hydrogen, and ammonia; the temperature is 1000-1500 ℃, and the pressure is 10-101 kPa; the treatment time is 30 minutes to 5 hours; the step of activating the gas to process the confinement growth ring is one-step processing or multi-step processing, wherein the multi-step processing is to sequentially introduce different gases for thermal cleaning according to a time sequence.
7. The method of claim 1, wherein in step 6), the gas is a combination of nitrogen, hydrogen, and hydrogen chloride; the temperature is 1000-1500 ℃, and the pressure is 10-101 kPa; the treatment time is 30 minutes to 5 hours.
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