CN112553692A - Large-size gallium nitride single crystal growth equipment and large-size bulk gallium nitride single crystal growth method - Google Patents
Large-size gallium nitride single crystal growth equipment and large-size bulk gallium nitride single crystal growth method Download PDFInfo
- Publication number
- CN112553692A CN112553692A CN202011424545.7A CN202011424545A CN112553692A CN 112553692 A CN112553692 A CN 112553692A CN 202011424545 A CN202011424545 A CN 202011424545A CN 112553692 A CN112553692 A CN 112553692A
- Authority
- CN
- China
- Prior art keywords
- gallium nitride
- single crystal
- nitride single
- size
- crystal growth
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Classifications
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention relates to a large-size gallium nitride single crystal growth device and a large-size bulk gallium nitride single crystal growth method, and the device comprises a growth device furnace body, wherein the growth device furnace body comprises a quartz tube used as a hearth part, one end of the quartz tube is provided with an air inlet flange, the other end of the quartz tube is provided with an air outlet flange, at least one section of resistance heating constant-temperature area is arranged on the quartz tube, an induction heating crystallization area is arranged on the quartz tube between the resistance heating constant-temperature area and the air outlet flange, and the induction heating crystallization area comprises an electromagnetic induction coil arranged on the periphery of the quartz tube and an induction material layer arranged on the inner wall of the quartz tube and matched with the electromagnetic induction. The large-size gallium nitride single crystal growth equipment creatively adds the induction heating crystallization area which is composed of the induction coil and the temperature field induction material, constructs the temperature field suitable for the growth of the gallium nitride single crystal and improves the growth rate and the quality of the gallium nitride crystal.
Description
Technical Field
The invention relates to a large-size gallium nitride single crystal growth device and a large-size bulk gallium nitride single crystal growth method, and belongs to the technical field of crystal growth devices.
Background
With the development of the technology, the optical and electrical properties of the conventional Si and GaAs semiconductor devices have been developed to the utmost, and cannot meet the development of novel short-wavelength light emitting devices and high-frequency devices, and new requirements for high temperature, high frequency, high voltage, radiation resistance, blue light emission and the like are provided. The third generation semiconductor material represented by GaN has the characteristics of large forbidden bandwidth, large heat conductivity, high breakdown electric field, small dielectric constant, high electron saturation drift velocity, good chemical stability, strong radiation resistance and the like, is widely researched, and has very large application potential in the aspects of light emitting devices such as blue light diodes, blue light lasers, ultraviolet detectors and the like and high-temperature, high-frequency and high-power microelectronic devices.
At present, the common equipment for growing the gallium nitride single crystal is HVPE equipment which mainly comprises a plurality of sections of constant temperature areas with different temperatures formed by heating through a plurality of sections of resistors, a crystallization area is also a specific constant temperature area with the temperature between 950 and 1100 ℃, and the temperature gradient is small or not, so that the growth window of the gallium nitride is small, the gallium nitride single crystal film is only suitable for growing the gallium nitride single crystal film with the temperature below 800 mu m, the industrialization efficiency is low, the crystal dislocation density is high, and the like.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a large-size gallium nitride single crystal growth device and a large-size bulk gallium nitride single crystal growth method, which can effectively solve the problems that the growth window of the traditional gallium nitride crystal growth device is small and is only suitable for growing a gallium nitride single crystal film.
In order to solve the problems, the invention is realized by the following technical scheme:
a large-size gallium nitride single crystal growth device comprises a growth device furnace body, a gas control system and a tail gas treatment system, wherein the gas control system and the tail gas treatment system are respectively connected with the growth device furnace body through gas pipelines;
the growth device furnace body includes the quartz capsule as furnace part, quartz capsule one end is provided with the flange that admits air, and the other end of quartz capsule is provided with the flange of giving vent to anger, is provided with one section at least resistance heating thermostatic zone on the quartz capsule, be provided with induction heating crystallization area on the quartz capsule between resistance heating thermostatic zone and the flange of giving vent to anger, induction heating crystallization area includes quartz capsule outlying electromagnetic induction coil and sets up at quartz capsule inner wall and electromagnetic induction coil cooperation production thermal response material layer, and the response material layer is ring shape, and the quartz capsule inside or the outside in induction heating crystallization area is provided with the insulation material layer.
According to the invention, the induction material layer is preferably made of high-density graphite, tungsten and molybdenum, and the heat insulation material layer is preferably made of graphite heat insulation material, zirconia heat insulation material and alumina heat insulation material.
According to the invention, 2-4 sections of resistance heating constant temperature areas are preferably arranged on the quartz tube, each resistance heating constant temperature area comprises a resistance heater, and the resistance heaters are arranged on the periphery of the quartz tube.
According to the invention, the resistance heating constant temperature area and the induction heating crystallization area are preferably arranged at a distance, and the heating parts of the resistance heating constant temperature area and the induction heating crystallization area are controlled independently of each other.
Further preferably, the distance between the resistance heating constant temperature region and the induction heating crystallization region is 6-50 cm.
According to the invention, a gallium boat is preferably arranged in the quartz tube of the resistance heating constant-temperature area.
Preferably, according to the invention, the temperature of the thermostatic zone for resistance heating ranges from 700 ℃ to 950 ℃ and the temperature of the crystallization zone for induction heating ranges from 1000 ℃ to 1700 ℃.
The method for growing the large-size bulk gallium nitride single crystal by using the large-size gallium nitride single crystal growth equipment comprises the following steps of:
(1) placing metal gallium in a gallium boat in a resistance heating constant-temperature area;
(2) sealing large-size gallium nitride single crystal growth equipment, and introducing chlorine-containing atmosphere, carrier gas and ammonia gas from a gas inlet flange by a gas control system;
(3) the chlorine-containing atmosphere reacts with the metal gallium in the gallium boat to generate GaCl gas, and the GaCl and ammonia gas react in the induction heating crystallization area to generate bulk gallium nitride crystals.
The invention has the following beneficial effects:
1. the large-size gallium nitride single crystal growth equipment creatively adds the induction heating crystallization area which is composed of the induction coil and the temperature field induction material, and constructs the temperature field suitable for the growth of the gallium nitride single crystal.
2. The induction coil, the temperature field induction material and the heat preservation are mutually matched, so that the temperature field suitable for the growth of the gallium nitride crystal can be adjusted, and the growth rate and the quality of the gallium nitride crystal can be improved by adjusting the temperature gradient.
3. The large-size gallium nitride single crystal growth equipment has a crystal growth environment with adjustable temperature gradient, and better accords with crystal growth thermodynamics and crystal growth kinetics.
Drawings
FIG. 1 is a schematic structural diagram of an apparatus for growing a large-sized gallium nitride single crystal according to the present invention.
Wherein: 1 air inlet flange, 2 quartz tubes, 3 resistance heating constant temperature zones, 4 induction heating crystallization zones, 5 air outlet flanges and 6 electromagnetic induction coils.
Detailed Description
The invention will be further explained with reference to the drawings and examples.
Example 1
As shown in figure 1, the growth equipment of the large-size gallium nitride single crystal can effectively solve the problem that the growth window of the traditional gallium nitride crystal growth equipment is small and is only suitable for growing a gallium nitride single crystal film, thereby growing the bulk gallium nitride single crystal with the thickness of more than 3 millimeters.
The device comprises a growth equipment furnace body, a gas control system and a tail gas treatment system, wherein the gas control system and the tail gas treatment system are respectively connected with the growth equipment furnace body through gas pipelines.
The growth device furnace body includes as the partial quartz capsule 2 of furnace, and 2 left ends of quartz capsule are provided with air intake flange 1, and 2 right-hand members of quartz capsule are provided with air outlet flange 5, are provided with one section at least resistance heating thermostatic zone 3 on the quartz capsule 2, be provided with induction heating crystallization area 4 on the quartz capsule 2 between resistance heating thermostatic zone 3 and the air outlet flange 5, induction heating crystallization area 4 includes electromagnetic induction coil 6 outside quartz capsule 2 and sets up and can produce thermal response material layer with the cooperation of electromagnetic induction coil 6 at 2 inner walls of quartz capsule, and the quartz capsule 2 inside or the outside of induction heating crystallization area 4 is provided with the insulation material layer. The resistance heating constant temperature area 3 can be a section of constant temperature area or a plurality of sections of constant temperature areas, a gallium boat is placed in the resistance heating constant temperature area 3, reaction gas in the gallium boat is heated gradually, and the temperature of the resistance heating constant temperature area 3 is between 700 ℃ and 950 ℃.
The induction material layer is made of high-density graphite, tungsten and molybdenum, and the heat insulation material layer is made of graphite heat insulation materials, zirconium oxide heat insulation materials and aluminum oxide heat insulation materials. A gallium boat is arranged in the quartz tube 2 of the resistance heating constant temperature area 3. The utility model relates to a use method of a novel gallium nitride single crystal growth device, wherein the temperature of a resistance heating constant temperature area 3 is 700 ℃ to 950 ℃, and the temperature of an induction heating crystallization area 4 is 1000 ℃ to 1700 ℃.
The material of the induction material layer in the induction heating crystallization zone 4 is made of high-density graphite, tungsten, molybdenum and other conductive and high-temperature resistant materials, and the shape of the induction material layer is mainly circular. The inner diameter of the induction material layer is larger than the diameter of the seed crystal, and the outer diameter of the induction material layer is smaller than the inner diameter of the quartz hearth. The heat insulation material layer is made of high-temperature resistant materials such as graphite heat insulation materials, zirconium oxide heat insulation materials, aluminum oxide heat insulation materials and the like. The temperature is between 1000 ℃ and 1700 ℃.
The induction material layer is in the furnace, the heat preservation material layer can be in the furnace, also can be outside the furnace, and the temperature gradient of induction heating crystallization zone 4 is built by induction material layer and heat preservation material layer jointly. It is also within the scope of this patent to sense various modifications of the material. The invention creatively adds an induction heating crystallization area 4 on the basis of the traditional gallium nitride single crystal growth equipment, the area is composed of an induction coil and a temperature field induction material, and a temperature field suitable for the growth of the gallium nitride single crystal is constructed. The device can be changed into a novel bedroom gallium nitride device and a novel vertical gallium nitride growth device according to the patent, and is also protected by the patent.
Example 2
The method for growing a large-size bulk gallium nitride single crystal using the large-size gallium nitride single crystal growth apparatus of example 1, comprising the steps of:
(1) placing metal gallium in a gallium boat in a resistance heating constant-temperature area;
(2) sealing large-size gallium nitride single crystal growth equipment, and introducing chlorine-containing atmosphere, carrier gas and ammonia gas from a gas inlet flange by a gas control system;
(3) the chlorine-containing atmosphere reacts with the metal gallium in the gallium boat to generate GaCl gas, and the GaCl and ammonia gas react in the induction heating crystallization area to generate bulk gallium nitride crystals.
The foregoing is only a preferred embodiment of this patent, and it should be noted that, for those skilled in the art, various modifications and substitutions can be made without departing from the technical principle of this patent, and these modifications and substitutions should also be regarded as the protection scope of this patent.
Claims (8)
1. A large-size gallium nitride single crystal growth device comprises a growth device furnace body, a gas control system and a tail gas treatment system, wherein the gas control system and the tail gas treatment system are respectively connected with the growth device furnace body through gas pipelines;
the growth device furnace body includes the quartz capsule as furnace part, quartz capsule one end is provided with the flange that admits air, and the other end of quartz capsule is provided with the flange of giving vent to anger, is provided with one section at least resistance heating thermostatic zone on the quartz capsule, be provided with induction heating crystallization area on the quartz capsule between resistance heating thermostatic zone and the flange of giving vent to anger, induction heating crystallization area includes quartz capsule outlying electromagnetic induction coil and sets up at quartz capsule inner wall and electromagnetic induction coil cooperation production thermal response material layer, and the response material layer is ring shape, and the quartz capsule inside or the outside in induction heating crystallization area is provided with the insulation material layer.
2. The growth device of large-size gallium nitride single crystal according to claim 1, wherein the induction material layer is made of high-density graphite, tungsten or molybdenum, and the heat insulation material layer is made of graphite heat insulation material, zirconia heat insulation material or alumina heat insulation material.
3. A large-size gallium nitride single crystal growth apparatus according to claim 1, wherein the quartz tube is provided with 2-4 sections of resistive heating constant temperature zones, the resistive heating constant temperature zones comprise resistive heaters, and the resistive heaters are arranged on the periphery of the quartz tube.
4. A large-size gallium nitride single crystal growth apparatus according to claim 1, wherein there is a space between the resistance heating constant temperature region and the induction heating crystallization region, and heating elements of the resistance heating constant temperature region and the induction heating crystallization region are controlled independently of each other.
5. A large-size gallium nitride single crystal growth apparatus according to claim 4, wherein the distance between the resistance heating constant temperature region and the induction heating crystallization region is 6-50 cm.
6. The apparatus for growing a large-sized gallium nitride single crystal according to claim 1, wherein a gallium boat is placed in the quartz tube of the resistance heating constant temperature zone.
7. A large-size gallium nitride single crystal growth apparatus according to claim 1, wherein the temperature of the resistance heating thermostatic zone is 700 ℃ to 950 ℃, and the temperature of the induction heating crystallization zone is 1000 ℃ to 1700 ℃.
8. The method for growing the large-size bulk gallium nitride single crystal by using the large-size gallium nitride single crystal growth equipment comprises the following steps of:
(1) placing metal gallium in a gallium boat in a resistance heating constant-temperature area;
(2) sealing large-size gallium nitride single crystal growth equipment, and introducing chlorine-containing atmosphere, carrier gas and ammonia gas from a gas inlet flange by a gas control system;
(3) the chlorine-containing atmosphere reacts with the metal gallium in the gallium boat to generate GaCl gas, and the GaCl and ammonia gas react in the induction heating crystallization area to generate bulk gallium nitride crystals.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011424545.7A CN112553692A (en) | 2020-12-08 | 2020-12-08 | Large-size gallium nitride single crystal growth equipment and large-size bulk gallium nitride single crystal growth method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011424545.7A CN112553692A (en) | 2020-12-08 | 2020-12-08 | Large-size gallium nitride single crystal growth equipment and large-size bulk gallium nitride single crystal growth method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112553692A true CN112553692A (en) | 2021-03-26 |
Family
ID=75059750
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011424545.7A Pending CN112553692A (en) | 2020-12-08 | 2020-12-08 | Large-size gallium nitride single crystal growth equipment and large-size bulk gallium nitride single crystal growth method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112553692A (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040244680A1 (en) * | 2001-06-06 | 2004-12-09 | Robert Dwilinski | Method of manufacturing bulk single crystal of gallium nitride |
| US20050263065A1 (en) * | 2004-05-26 | 2005-12-01 | Negley Gerald H | Vapor assisted growth of gallium nitride |
| CN102465333A (en) * | 2010-11-18 | 2012-05-23 | 南京大学 | Vertical hydride vapor phase epitaxy growth system |
| CN107574479A (en) * | 2017-08-14 | 2018-01-12 | 南京大学 | A kind of multi-functional hydride vapor phase epitaxy growth system and application |
| CN107587190A (en) * | 2017-08-14 | 2018-01-16 | 南京大学 | A kind of method for preparing GaN substrate material |
-
2020
- 2020-12-08 CN CN202011424545.7A patent/CN112553692A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040244680A1 (en) * | 2001-06-06 | 2004-12-09 | Robert Dwilinski | Method of manufacturing bulk single crystal of gallium nitride |
| US20050263065A1 (en) * | 2004-05-26 | 2005-12-01 | Negley Gerald H | Vapor assisted growth of gallium nitride |
| CN102465333A (en) * | 2010-11-18 | 2012-05-23 | 南京大学 | Vertical hydride vapor phase epitaxy growth system |
| CN107574479A (en) * | 2017-08-14 | 2018-01-12 | 南京大学 | A kind of multi-functional hydride vapor phase epitaxy growth system and application |
| CN107587190A (en) * | 2017-08-14 | 2018-01-16 | 南京大学 | A kind of method for preparing GaN substrate material |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US5253266A (en) | MBE effusion source with asymmetrical heaters | |
| US5155062A (en) | Method for silicon carbide chemical vapor deposition using levitated wafer system | |
| CN106048729B (en) | A kind of PVT method major diameter silicon carbide monocrystal growth device | |
| CN107223168B (en) | The furnace of the brilliant distillation of kind for wide bandgap crystal | |
| CN109825875A (en) | Carrier gas auxiliary PVT method prepares the device and method of wide bandgap semiconductor monocrystal material | |
| CN104878450A (en) | AlN single crystal substrate production apparatus and application method thereof | |
| US6800136B2 (en) | Axial gradient transport apparatus and process | |
| CN112663134A (en) | Double-temperature-zone independently controlled silicon carbide single crystal growth device and growth method | |
| CN113652740A (en) | Preparation method of silicon carbide single crystal, single crystal growing furnace and heating device of single crystal growing furnace | |
| CN112064110A (en) | Temperature control device for growth of silicon carbide crystal | |
| CN103451621B (en) | MOCVD reaction chamber and processing unit | |
| CN112553692A (en) | Large-size gallium nitride single crystal growth equipment and large-size bulk gallium nitride single crystal growth method | |
| JP2011026161A (en) | Nitride single crystal and apparatus for producing the same | |
| CN106521615B (en) | InP crystal growth furnace based on VGF method | |
| CN116463728A (en) | Device and method for growing high-quality silicon carbide crystal and silicon carbide crystal | |
| CN108286074B (en) | Large-size SiC single crystal growth device and working method thereof | |
| JP2003086516A (en) | Susceptor, cvd unit, film-forming method and semiconductor device | |
| CN206396351U (en) | A kind of InP crystal growing furnaces based on VGF methods | |
| CN114686963A (en) | GaAs single crystal growth equipment and GaAs single crystal growth process | |
| CN103276444A (en) | Dual heating vapor phase epitaxial growth system | |
| CN110499532B (en) | Device for rapidly preparing silicon carbide | |
| CN112458532A (en) | Device and method for preparing silicon carbide single crystal through high-temperature chemical deposition | |
| CN219157036U (en) | Eight inches PVT growth furnaces of adjustable growth rate | |
| CN115125617B (en) | Method for preparing self-supporting gallium nitride bulk single crystal by setting temperature gradient | |
| CN220619188U (en) | Crystal growth device |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |