CN112708937A - Processing method and processing device for GaN single crystal growth substrate - Google Patents
Processing method and processing device for GaN single crystal growth substrate Download PDFInfo
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- CN112708937A CN112708937A CN202011504974.5A CN202011504974A CN112708937A CN 112708937 A CN112708937 A CN 112708937A CN 202011504974 A CN202011504974 A CN 202011504974A CN 112708937 A CN112708937 A CN 112708937A
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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
- C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
- C30B33/08—Etching
- C30B33/10—Etching in solutions or melts
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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
- C30B25/18—Epitaxial-layer growth characterised by the substrate
- C30B25/186—Epitaxial-layer growth characterised by the substrate being specially pre-treated by, e.g. chemical or physical means
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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
- C30B25/18—Epitaxial-layer growth characterised by the substrate
- C30B25/20—Epitaxial-layer growth characterised by the substrate the substrate being of the same materials as the epitaxial layer
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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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Abstract
The invention provides a processing method and a processing device for a GaN single crystal growth substrate, which are characterized in that metal ions are introduced into a hot acid corrosion solution to inhibit the transverse corrosion speed of corrosion pits on the substrate in the hot acid corrosion solution and promote the longitudinal corrosion speed of the corrosion pits on the substrate in the hot acid corrosion solution, so that the GaN single crystal growth substrate with smaller pore diameter and deeper corrosion pit depth is obtained.
Description
Technical Field
The invention relates to a processing method and a processing device for a GaN single crystal growth substrate, belonging to the field of substrate processing.
Background
In the third generation semiconductor, GaN is a wide forbidden band semiconductor material with direct band gap, has the advantages of large forbidden band width, stable physicochemical properties, strong radiation resistance, high saturated electron drift velocity, high breakdown field strength and the like, can be widely applied to high-temperature, high-voltage and high-frequency electronic devices, and can be used for LED illumination and LD laser preparation due to the large forbidden band width. Meanwhile, mixed crystals can be formed with other III group nitride semiconductor materials (AlN, InN and the like), and the luminescence of the mixed crystals can cover the continuous wave band from infrared to ultraviolet and is not possessed by other III group nitride semiconductor materials. Has wide application prospect.
The growth method of GaN includes an ammonothermal method, a high-pressure solution method, a cosolvent method, a Hydride Vapor Phase Epitaxy (HVPE) method, and the like; since the melting point of GaN is as high as 2000 ℃ or higher, and the decomposition pressure is as high as 4.5GPa, it means that decomposition will occur under normal pressure without reaching the melting point. The traditional solution method requires a high-pressure environment and a special corrosion-resistant container, the growth conditions are extremely harsh, and the single crystal grown by the solution method has small size and low growth speed. Therefore, most of the commercial GaN bulk single crystal materials are grown by Hydride Vapor Phase Epitaxy (HVPE).
The HVPE method has the advantages of high growth rate (up to 100-. However, a GaN homogeneous substrate is lacked at present, the growth of GaN single crystal materials is finished on a heterogeneous substrate at present, and due to lattice mismatch and thermal mismatch between the GaN single crystal materials and the heterogeneous substrate, a large amount of dislocation and stress inevitably exist in the grown single crystal materials, so that the quality and the service life of manufactured devices are influenced. Therefore, the processing of the substrate is extremely important in order to reduce the dislocation density and relieve the stress.
The method for carrying out corrosion treatment on the substrate by using hot acid is a simple and practical method, but the substrate obtained by the existing hot acid corrosion treatment has the problems of large aperture and shallow depth of a corrosion pit, and in the subsequent single crystal growth process, the aperture is too large and is not easy to combine, the depth of the hole is shallow, the shallow pit is easy to fill and level, and the effect of making the corrosion pit is lost, so that the extension of dislocation cannot be blocked, the dislocation density cannot be reduced, and the stress is relieved; therefore, a method for processing a substrate for GaN growth having a small etch pit diameter and a deep depth is demanded.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a processing method and a processing device for a GaN single crystal growth substrate.
The treatment method comprises the steps of introducing metal ions into the hot acid corrosive liquid, inhibiting the transverse corrosion speed of the corrosion pit on the substrate in the hot acid corrosive liquid, promoting the longitudinal corrosion speed of the corrosion pit on the substrate in the hot acid corrosive liquid, obtaining the GaN single crystal growth substrate with smaller corrosion pit aperture and deeper corrosion pit depth, wherein deeper holes are not easy to fill and level in the subsequent single crystal growth process and can be covered by a growth layer, pores are left at the interface, the deformability is increased in the cooling process, the stress caused by lattice mismatch and thermal mismatch can be relieved, the extension of dislocation blocking is effectively realized, and the dislocation density in the grown single crystal material is reduced.
The invention is realized by the following technical scheme:
a processing method for a GaN single crystal growth substrate comprises the following steps:
(1) adding a metal ion solution into a phosphoric acid solution to obtain a mixed solution;
(2) and heating the mixed solution to 230-260 ℃, and then placing the substrate in the mixed solution for corrosion for 1-5 min.
Preferably, according to the invention, in step (1), the phosphoric acid solution has a concentration by mass of 80 to 90% by weight.
Preferably, in step (1), the metal ion solution is a saturated metal ion solution.
Further preferably, in the step (1), the saturated metal ion solution is a saturated aluminum ion solution and/or an iron ion solution.
According to the invention, in the step (1), the volume ratio of the metal ion solution to the phosphoric acid solution is (2-6): 1.
Preferably, in step (1), the saturated metal ion solution is a solution which cannot dissolve the solid metal salt any more in 30ml of deionized water at room temperature (25 ℃).
Preferably, in step (2), in order to avoid the sudden temperature drop of the processed substrate in water, the etched substrate taken out from step (2) is placed in deionized water at 90 ℃ after being placed for 30 seconds.
Preferably, in step (2), the substrate is obtained by depositing a 5um gan thin film on sapphire by MOCVD, and the sapphire has a thickness of 430 um.
Preferably, in the step (2), after the etching is finished, the substrate is taken out and kept for 30s, the substrate is slowly placed into deionized water at 90 ℃, the etching is stopped, the substrate is washed clean with the deionized water, then the substrate is placed into a beaker containing the deionized water, the beaker is placed into an ultrasonic machine for ultrasonic cleaning, the substrate is washed clean with the deionized water again after the ultrasonic cleaning, the substrate is dried by a blower after the cleaning, the substrate is placed into a vacuum drying oven for drying, and the substrate is sealed for standby.
The utility model provides a processing apparatus for GaN single crystal growth substrate, includes the warm table, is provided with the beaker that holds mixed solution on the warm table, is provided with the thermoscope of measuring mixed solution temperature in the beaker, and the thermoscope is fixed through the fixed bolster.
The invention has the technical characteristics and advantages that:
1. the treatment method comprises the steps of introducing metal ions into a hot acid corrosion solution, inhibiting the transverse corrosion speed of corrosion pits on a substrate in the hot acid corrosion solution, promoting the longitudinal corrosion speed of the corrosion pits on the substrate in the hot acid corrosion solution, obtaining the GaN monocrystal growth substrate with smaller pore diameter and deeper corrosion pit depth, wherein the corrosion pits with smaller pore diameter are easy to combine and the deeper corrosion pits are difficult to fill and level in the subsequent monocrystal growth process, and after the growth and the combination are completed, pores can be formed at the interface, so that the extension of dislocation can be effectively blocked, the dislocation density in the grown monocrystal material can be reduced, and the deformation degree in the cooling process can be increased by the pores, and the stress caused by lattice mismatch and thermal mismatch can be relieved.
2. The treatment method is simple and easy to implement and easy to popularize and utilize.
Drawings
FIG. 1 is an SEM topography of a substrate treated by a treatment method without introducing metal ions into a hot acid etching solution;
FIG. 2 is an SEM topography of a substrate processed by a processing method of introducing metal ions into a hot acid etching solution;
FIG. 3 is a SEM image of a cross-section of a substrate treated by a treatment method in which no metal ions are introduced into the hot acid etching solution;
FIG. 4 is a SEM image of a cross-section of a substrate processed by a process in which metal ions are introduced into a hot acid etching solution;
FIG. 5 is a schematic view of an apparatus for acid etching a substrate;
1. a heating table, 2, a beaker filled with the mixed solution, 3, a thermometer, 4 and a fixed support.
Detailed Description
The invention will be further illustrated, but not limited, by the following examples and the accompanying drawings.
The processing device for the GaN single crystal growth substrate comprises a heating table 1, a beaker 2 filled with mixed solution is arranged on the heating table, a temperature detector 3 for measuring the temperature of the mixed solution in the beaker is arranged in the beaker, and the temperature detector is fixed through a fixing support 4.
The substrate in the examples was a 2-inch MOCVD-GaN/sapphire substrate with a 5um thick MOCVD-GaN film on a sapphire substrate.
Example 1:
a processing method for a GaN single crystal growth substrate comprises the following steps:
(1) adding 30ml of saturated aluminum chloride solution into 60ml of phosphoric acid solution to obtain a mixed solution; the mass concentration of the phosphoric acid solution is 85 wt%;
(2) pouring the mixed solution into a beaker, adding magnetons, stirring and mixing uniformly on a magnetic stirrer, placing on a heating table,
(3) measuring the temperature by using a thermometer, heating the mixed solution to 250 ℃, and putting the substrate into the hot mixed solution for corrosion for 3 min;
(4) taking out the substrate, staying for 30s, and putting the substrate into prepared hot water at 90 ℃;
(5) taking out the substrate, washing the substrate with deionized water, putting the substrate into a beaker filled with deionized water, putting the substrate into an ultrasonic cleaning machine, and ultrasonically cleaning the substrate for 30 min;
(6) and taking out the substrate subjected to ultrasonic cleaning, washing the substrate with deionized water, drying the substrate by using a blower, drying the substrate in a vacuum drying oven for 30min, and packaging the substrate for later use.
The SEM topography and section SEM images of the processed GaN single crystal growth substrate are shown in figures 2 and 4, and it can be seen from the figures that the aperture of the substrate etch pit is smaller and the depth is deeper compared with the substrate etch pit obtained by the processing method without introducing metal ions.
Example 2:
a processing method for a GaN single crystal growth substrate comprises the following steps:
(1) adding 20ml of saturated aluminum chloride solution into 60ml of phosphoric acid solution to obtain a mixed solution; the mass concentration of the phosphoric acid solution is 85 wt%;
(2) pouring the mixed solution into a beaker, adding magnetons, stirring and mixing uniformly on a magnetic stirrer, placing on a heating table,
(3) measuring the temperature by using a thermometer, heating the mixed solution to 260 ℃, and putting the substrate into the hot mixed solution for corrosion for 2 min;
(4) after the substrate is taken out and stays for 30s, the substrate is put into hot water with the temperature of 90 ℃ prepared in advance;
(5) taking out the substrate, washing the substrate with deionized water, putting the substrate into a beaker filled with deionized water, putting the substrate into an ultrasonic cleaning machine, and ultrasonically cleaning the substrate for 30 min;
(6) and taking out the substrate subjected to ultrasonic cleaning, washing the substrate with deionized water, drying the substrate by using a blower, drying the substrate in a vacuum drying oven for 30min, and packaging the substrate for later use.
Example 3:
a processing method for a GaN single crystal growth substrate comprises the following steps:
(1) adding 20ml of saturated aluminum chloride solution into 80ml of phosphoric acid solution to obtain a mixed solution; the mass concentration of the phosphoric acid solution is 85 wt%;
(2) pouring the mixed solution into a beaker, adding magnetons, stirring and mixing uniformly on a magnetic stirrer, placing on a heating table,
(3) measuring the temperature by using a thermometer, heating the mixed solution to 230 ℃, and putting the substrate into the hot mixed solution for corrosion for 5 min;
(4) after the substrate is taken out and stays for 30s, the substrate is put into hot water with the temperature of 90 ℃ prepared in advance;
(5) taking out the substrate, washing the substrate with deionized water, putting the substrate into a beaker filled with deionized water, putting the substrate into an ultrasonic cleaning machine, and ultrasonically cleaning the substrate for 30 min;
(6) and taking out the substrate subjected to ultrasonic cleaning, washing the substrate with deionized water, drying the substrate by using a blower, drying the substrate in a vacuum drying oven for 30min, and packaging the substrate for later use.
The above examples are only for further details of the steps of the method of treating a substrate with hot phosphoric acid containing metal ions, and are not intended to limit the method. The proportioning, etching temperature, etching time, cleaning time and drying time mentioned in the examples can be adjusted according to different batches of substrates and different external conditions, and the actual conditions are met. All changes that come within the spirit and principles of the invention are intended to be within the scope of the invention.
Claims (10)
1. A processing method for a GaN single crystal growth substrate comprises the following steps:
(1) adding a metal ion solution into a phosphoric acid solution to obtain a mixed solution;
(2) and heating the mixed solution to 230-260 ℃, and then placing the substrate in the mixed solution for corrosion for 1-5 min.
2. The treatment method according to claim 1, wherein the phosphoric acid solution in the step (1) has a mass concentration of 80 to 90 wt%.
3. The process according to claim 1, wherein in the step (1), the metal ion solution is a saturated metal ion solution.
4. The treatment method according to claim 1, wherein in the step (1), the saturated metal ion solution is a saturated aluminum ion solution and/or an iron ion solution.
5. The treatment method according to claim 1, wherein in the step (1), the volume ratio of the metal ion solution to the phosphoric acid solution is (2-6): 1.
6. The process of claim 1, wherein in step (1), the saturated metal ion solution is a solution in which solid metal salts cannot be further dissolved in 30ml of deionized water at room temperature (25 ℃).
7. The process of claim 1, wherein in step (2), in order to prevent the temperature of the treated substrate from suddenly dropping in water, the treated substrate is taken out from step (2), and is placed in deionized water at 90 ℃ after being left for 30 seconds.
8. The process of claim 1, wherein in the step (2), the substrate is obtained by depositing a 5 μm GaN film on sapphire with a thickness of 430 μm by MOCVD.
9. The treatment method according to claim 1, wherein in the step (2), the substrate is taken out and kept for 30s after the etching is finished, the substrate is slowly placed into deionized water at 90 ℃, the etching is stopped, the substrate is cleaned by the deionized water, the substrate is placed into a beaker containing the deionized water and is placed into an ultrasonic machine for ultrasonic cleaning, the substrate is cleaned by the deionized water again after being cleaned by the ultrasonic cleaning, the substrate is dried by a blower after being cleaned by the deionized water, the substrate is placed into a vacuum drying oven for drying, and the substrate is sealed for standby.
10. The utility model provides a processing apparatus for GaN single crystal growth substrate, includes the warm table, is provided with the beaker that holds mixed solution on the warm table, is provided with the thermoscope of measuring mixed solution temperature in the beaker, and the thermoscope is fixed through the fixed bolster.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102169930A (en) * | 2011-03-07 | 2011-08-31 | 山东大学 | Method for coarsening surface of light-emitting diode (LED) with the aid of metal nanoparticles |
| CN102286777A (en) * | 2011-08-26 | 2011-12-21 | 山东天岳先进材料科技有限公司 | H3PO4 corrosive seed crystal for growing GaN (Gallium Nitride) single crystal by using HVPE (Hydride Vapor Phase Epitaxial) and preparation method thereof |
| US20140048097A1 (en) * | 2012-08-17 | 2014-02-20 | Idev Technologies, Inc. | Surface oxide removal methods |
| CN108570284A (en) * | 2018-06-05 | 2018-09-25 | 朱东洋 | A kind of alumina polishing solution preparation method |
-
2020
- 2020-12-18 CN CN202011504974.5A patent/CN112708937A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102169930A (en) * | 2011-03-07 | 2011-08-31 | 山东大学 | Method for coarsening surface of light-emitting diode (LED) with the aid of metal nanoparticles |
| CN102286777A (en) * | 2011-08-26 | 2011-12-21 | 山东天岳先进材料科技有限公司 | H3PO4 corrosive seed crystal for growing GaN (Gallium Nitride) single crystal by using HVPE (Hydride Vapor Phase Epitaxial) and preparation method thereof |
| US20140048097A1 (en) * | 2012-08-17 | 2014-02-20 | Idev Technologies, Inc. | Surface oxide removal methods |
| CN108570284A (en) * | 2018-06-05 | 2018-09-25 | 朱东洋 | A kind of alumina polishing solution preparation method |
Non-Patent Citations (2)
| Title |
|---|
| M.G.MYNBAEVA等: "Wet Chemical Etching of GaN in H3PO4 with Al Ions", 《ELECTROCHEMICAL AND SOLID STATE LETTERS》 * |
| 梅俊平: "预处理与离子注入GaN外延材料的性能研究", 《中国优秀博硕士学位论文全文数据库(博士) 信息科技辑 (月刊)》 * |
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