CN106149058A - A kind of nanocrystalline for the GaN preparation method of controllable appearance - Google Patents
A kind of nanocrystalline for the GaN preparation method of controllable appearance Download PDFInfo
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- CN106149058A CN106149058A CN201610510347.XA CN201610510347A CN106149058A CN 106149058 A CN106149058 A CN 106149058A CN 201610510347 A CN201610510347 A CN 201610510347A CN 106149058 A CN106149058 A CN 106149058A
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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
- C30B25/18—Epitaxial-layer growth characterised by the substrate
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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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- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The present invention relates to gallium nitride preparing technical field, particularly to the preparation method that the GaN of a kind of controllable appearance is nanocrystalline: use light float zone growth technology growth to mix the β Ga of Mg2O3Monocrystalline;At β Ga2O3Formed in the cleavage surface of monocrystalline to damage or choose surface and have the β Ga of lattice defect2O3Monocrystalline, by chemical gaseous phase depositing process, GaN is nanocrystalline in growth.The defective β Ga on surface2O3Growing gan crystal in the cleavage surface of monocrystalline, substantially reduces the formation time of GaN crystal, improves efficiency;The method can be without mask, it is to avoid pollutes, obtains the GaN crystal of different-shape, arbitrary trajectory, and the use that further expands for GaN crystal provides probability;The GaN crystal that obtains of growth, pattern is uniform, can large area deposition, and there is good repeatability.
Description
Technical field
The present invention relates to gallium nitride preparing technical field, particularly to the system that the GaN of a kind of controllable appearance is nanocrystalline
Preparation Method.
Background technology
GaN is a kind of semiconductor material with wide forbidden band, is to make light emitting diode (LED) blue, green and laser diode (LD)
Ideal material.Owing to GaN single crystal growth size is little and cost is the highest, general employing growth technology prepares GaN film
Or low-dimensional GaN nano material.β-Ga2O3Monocrystalline as the backing material that GaN epitaxy grows have the advantage that from visible ray to
Ultraviolet band transparency is high, and electrical conductivity and heat stability are high.In recent years, existing research group by chemical gaseous phase be deposited on β-
Ga2O3Prepare GaN film or low-dimensional GaN nano material in (100) cleavage surface of monocrystalline, manufacturing cycle typically 6 hours with
On, preparation condition is required harsher, the factor considered in preparation process is the most more, the pressure in such as reative cell, temperature, gas
The flow rate etc. of body, especially for preparing patterned thin film or low-dimension nano material, it is desirable to fully examine in deposition process
Consider the uniformity of deposit and coverage property good on figure.
Summary of the invention
In order to solve in above prior art, at β-Ga2O3GaN film or low-dimensional is prepared in (100) cleavage surface of monocrystalline
Manufacturing cycle length that GaN nano material exists, GaN nucleation difficulty, pattern can not the effective problem such as control, this application provides one
Plant the nanocrystalline preparation side of GaN that manufacturing cycle preparation short, graphical easily operates, can effectively control pattern by adjusting preparation parameter
Method.
Utilize β-Ga2O3The surface defect of monocrystalline preferentially forms the feature of GaN core, to GaN film or low-dimensional GaN nanometer material
The pattern of material regulates and controls, and the GaN preparing controllable appearance is nanocrystalline.
The present invention is obtained through the following steps:
The preparation method nanocrystalline for GaN of a kind of controllable appearance, comprises the following steps:
(1) light float zone growth technology growth is used to mix the β-Ga of Mg2O3Monocrystalline;
(2) at β-Ga2O3Formed in (100) cleavage surface of monocrystalline to damage or choose surface and have the β-Ga of lattice defect2O3
Monocrystalline, by chemical gaseous phase depositing process, is mixing the β-Ga of Mg2O3(100) cleavage surface Epitaxial growth GaN of monocrystalline is nanocrystalline.
Described preparation method, the operation of preferred steps (2) is: mix the β-Ga of Mg2O3Single-chip is placed in quartz boat, logical
NH3Flow is maintained at 400sccm, 5 hours heating-up times, constant temperature 950 DEG C 4 hours, lowers the temperature 5 hours.
Described preparation method, the operation of preferred steps (1) is: high-purity gallium oxide powder and magnesium oxide powder are based on chemistry
Amount, than weighing, grinding, mix homogeneously, makes charge bar, uses vacuum oil pump to take out the air in charge bar, static pressure 5 points under 68MPa
Clock, then fires 4 hours at 1100 DEG C.
Described preparation method, in preferred steps (1), the doping content of Mg is 0.1at%.
Described preparation method, in preferred steps (1), crystal growth step includes temperature programming, receives neck, shouldering, isometrical life
Grow, finish up, lower the temperature.
Described preparation method, the light float zone growth selecting model to be FZ-T-12000-X-I-S-SU in preferred steps (1)
Stove.
Beneficial effects of the present invention:
1) at surface defective β-Ga2O3Growing gan crystal in (100) cleavage surface of monocrystalline, relative to flawless β-
Ga2O3(100) cleavage surface of monocrystalline, substantially reduces the formation time of GaN crystal, improves efficiency;
2) by β-Ga2O3Growing gan crystal in the defect of (100) cleavage surface of monocrystalline, it is not necessary to carry out mask, keep away
Exempt to introduce impurity, the GaN crystal of different-shape, arbitrary trajectory can be obtained, use offer for further expanding of GaN crystal
Probability;
3) β-Ga is utilized2O3The defect preferred growth GaN crystal of (100) cleavage surface of monocrystalline, the crystal morphology obtained is equal
Even, can large area deposition, and there is good repeatability.
Accompanying drawing explanation
Fig. 1 is the β-Ga mixing Mg2O3(100) cleavage surface scanning electron microscope (SEM) photograph (amplifying 50K times, embodiment 1) of monocrystalline;
Fig. 2 is the β-Ga mixing Mg having cut2O3Monocrystalline (100) cleavage surface, in chemical gaseous phase deposition stove, leads to NH3Flow
Being maintained at 400sccm, thermostat temperature is 950 DEG C, heats up and temperature fall time is 5 hours, and constant temperature time is the scanning electricity of 4 hours
Mirror figure (amplifies 50K times, embodiment 1);
Fig. 3 is the TEM figure of (a) low amplification of GaN nano-particle, and (b) high-resolution TEM schemes, (c) SEAD
Figure (embodiment 1);
Fig. 4 is the β-Ga mixing Mg having lattice defect2O3Monocrystalline (100) cleavage surface, in chemical gaseous phase deposition stove, leads to NH3
Flow is maintained at 400sccm, and thermostat temperature is 950 DEG C, heats up and temperature fall time is 5 hours, and constant temperature time is 4 hours sweeps
Retouch Electronic Speculum figure (amplifying 1K times, embodiment 2);
Fig. 5 is the β-Ga mixing Mg having lattice defect2O3Monocrystalline (100) cleavage surface, in chemical gaseous phase deposition stove, leads to NH3
Flow is maintained at 400sccm, and thermostat temperature is 950 DEG C, heats up and temperature fall time is 5 hours, and constant temperature time is 4 hours sweeps
Retouch Electronic Speculum figure (amplifying 9K times, embodiment 2);
Fig. 6 is the smooth β-Ga mixing Mg2O3Monocrystalline (100) cleavage surface, in chemical gaseous phase deposition stove, leads to NH3Flow is protected
Holding at 400sccm, thermostat temperature is 950 DEG C, heats up and temperature fall time is 5 hours, and constant temperature time is the scanning electron microscope of 7 hours
Figure (amplifying 60K times, embodiment 3);
Fig. 7 is the smooth β-Ga mixing Mg2O3Monocrystalline (100) cleavage surface, in chemical gaseous phase deposition stove, leads to NH3Flow is protected
Holding at 400sccm, thermostat temperature is 950 DEG C, heats up and temperature fall time is 5 hours, and constant temperature time is the scanning electron microscope of 9 hours
Figure (amplifying 80K times, embodiment 4).
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is further described:
Embodiment one:
First, light float zone growth technology growth is used to mix the β-Ga of Mg2O3Monocrystalline: use conventional solid reaction to prepare raw material
Rod, utilizing high-purity gallium oxide powder and magnesium oxide powder is raw material, carries out accurate dosing according to stoichiometric proportion, the doping of Mg
Concentration is 0.1at%, by ball mill grinding, mix homogeneously, makes charge bar, uses vacuum oil pump to take out the air in charge bar,
Static pressure 5 minutes under 68MP, then fire 4 hours at 1100 DEG C so that it is abundant reaction obtains uniform diameter, and (diameter is about
6mm, length is about 10cm) polycrystalline charge bar.The light float zone growth stove selecting model to be FZ-T-12000-X-I-S-SU, crystal
Growth step mainly include temperature programming, receive neck, shouldering, isodiametric growth, finish up, the step such as cooling;
Then, due to β-Ga2O3Monocrystalline easily along (100) face cleavage, is therefore readily available smooth (100) wafer,
(100) gently with blade standardized road cut on wafer, wafer acetone is cleaned up standby, by chemical gaseous phase deposition side
Method, is mixing the β-Ga of Mg2O3(100) cleavage surface Epitaxial growth GaN of monocrystalline is nanocrystalline: mix the β-Ga of Mg2O3Single-chip is placed on
In quartz boat, logical NH3Flow is maintained at 400sccm, and the heating-up time is 5 hours, and constant temperature time is 4 hours, and thermostat temperature is 950
DEG C, temperature fall time is 5 hours.
By mixing the β-Ga of Mg before and after chemical gaseous phase is deposited2O3Monocrystalline (100) cleavage surface is scanned Electronic Speculum and characterizes, and changes
It is the smooth β-Ga mixing Mg before learning vapour deposition2O3(100) cleavage surface of monocrystalline, as it is shown in figure 1, chemical gaseous phase deposition after
Preferred growth GaN nano-particle at cut, and the nanocrystalline uniformity of scored area is fine, as shown in Figure 2.To GaN nanometer
Grain carries out low amplification and high-resolution TEM and selected area electron diffraction analysis, high-resolution TEM show GaN nanocrystalline be single
Crystal structure, and (100) interplanar distance is 0.262nm;SEAD figure illustrate GaN nanocrystalline be hexagonal structure, such as Fig. 3 institute
Show.
Embodiment two:
First, light float zone growth technology growth is used to mix the β-Ga of Mg2O3Monocrystalline: use conventional solid reaction to prepare raw material
Rod, utilizing high-purity gallium oxide powder and magnesium oxide powder is raw material, carries out accurate dosing according to stoichiometric proportion, the doping of Mg
Concentration is 0.1at%, by ball mill grinding, mix homogeneously, makes charge bar, uses vacuum oil pump to take out the air in charge bar,
Static pressure 5 minutes under 68MP, then fire 4 hours at 1100 DEG C so that it is abundant reaction obtains uniform diameter, and (diameter is about
6mm, length is about 10cm) polycrystalline charge bar.The light float zone growth stove selecting model to be FZ-T-12000-X-I-S-SU, crystal
Growth step mainly include temperature programming, receive neck, shouldering, isodiametric growth, finish up, the step such as cooling;
Then, due to β-Ga2O3Monocrystalline easily along (100) face cleavage, is therefore readily available smooth (100) wafer, choosing
Pick and place surface in shoulder growth course and produce the wafer of lattice defect, wafer acetone is cleaned up standby, passes through chemical gaseous phase
Deposition process, is mixing the β-Ga of Mg2O3(100) cleavage surface Epitaxial growth GaN of monocrystalline is nanocrystalline: mix the β-Ga of Mg2O3Monocrystalline
Sheet is placed in quartz boat, logical NH3Flow is maintained at 400sccm, and the heating-up time is 5 hours, and constant temperature time is 4 hours, constant temperature temperature
Degree is 950 DEG C, and temperature fall time is 5 hours.
β-the Ga of Mg is mixed by lattice defect region after chemical gaseous phase is deposited2O3Monocrystalline (100) cleavage surface is scanned
Electronic Speculum characterizes, and finds lattice defect area preference growth GaN nano-particle, such as Fig. 4, shown in 5.
Embodiment three:
First, light float zone growth technology growth is used to mix the β-Ga of Mg2O3Monocrystalline: use conventional solid reaction to prepare raw material
Rod, utilizing high-purity gallium oxide powder and magnesium oxide powder is raw material, carries out accurate dosing according to stoichiometric proportion, the doping of Mg
Concentration is 0.1at%, by ball mill grinding, mix homogeneously, makes charge bar, uses vacuum oil pump to take out the air in charge bar,
Static pressure 5 minutes under 68MP, then fire 4 hours at 1100 DEG C so that it is abundant reaction obtains uniform diameter, and (diameter is about
6mm, length is about 10cm) polycrystalline charge bar.The light float zone growth stove selecting model to be FZ-T-12000-X-I-S-SU, crystal
Growth step mainly include temperature programming, receive neck, shouldering, isodiametric growth, finish up, the step such as cooling;
Then, due to β-Ga2O3Monocrystalline easily along (100) face cleavage, is therefore readily available smooth, nearly defect-free
(100) wafer, cleans up standby by wafer acetone, by chemical gaseous phase depositing process, is mixing the β-Ga of Mg2O3Monocrystalline
(100) cleavage surface Epitaxial growth GaN is nanocrystalline: mix the β-Ga of Mg2O3Single-chip is placed in quartz boat, logical NH3Flow is maintained at
400sccm, the heating-up time is 5 hours, and constant temperature time is 7 hours, and thermostat temperature is 950 DEG C, and temperature fall time is 5 hours.
By the β-Ga that mix Mg post-depositional to chemical gaseous phase2O3Monocrystalline (100) cleavage surface is scanned Electronic Speculum and characterizes, and sends out
Showing the sample surfaces extension GaN nano-particle being scattered, uniformity is fine, from the pattern of GaN nano-particle it can be seen that be six
Square structure, as shown in Figure 6.
Embodiment four:
First, light float zone growth technology growth is used to mix the β-Ga of Mg2O3Monocrystalline: use conventional solid reaction to prepare raw material
Rod, utilizing high-purity gallium oxide powder and magnesium oxide powder is raw material, carries out accurate dosing according to stoichiometric proportion, the doping of Mg
Concentration is 0.1at%, by ball mill grinding, mix homogeneously, makes charge bar, uses vacuum oil pump to take out the air in charge bar,
Static pressure 5 minutes under 68MP, then fire 4 hours at 1100 DEG C so that it is abundant reaction obtains uniform diameter, and (diameter is about
6mm, length is about 10cm) polycrystalline charge bar.The light float zone growth stove selecting model to be FZ-T-12000-X-I-S-SU, crystal
Growth step mainly include temperature programming, receive neck, shouldering, isodiametric growth, finish up, the step such as cooling;
Then, due to β-Ga2O3Monocrystalline easily along (100) face cleavage, is therefore readily available smooth, nearly defect-free
(100) wafer, cleans up standby by wafer acetone, by chemical gaseous phase depositing process, is mixing the β-Ga of Mg2O3Monocrystalline
(100) cleavage surface Epitaxial growth GaN is nanocrystalline: mix the β-Ga of Mg2O3Single-chip is placed in quartz boat, logical NH3Flow is maintained at
400sccm, the heating-up time is 5 hours, and constant temperature time is 9 hours, and thermostat temperature is 950 DEG C, and temperature fall time is 5 hours.
By mixing the β-Ga of Mg after chemical gaseous phase is deposited2O3Monocrystalline (100) cleavage surface is scanned Electronic Speculum and characterizes, and finds
Sample surfaces has been covered with GaN nano-particle, and uniformity is fine, as shown in Figure 7.
Comparative example 1,2 and 3,4, find to exist the β-Ga of cut and lattice defect2O3(100) cleavage surface of crystal, outward
Time nanocrystalline for epitaxial growth GaN is greatly shortened, and improves efficiency, reduces cost.Utilize β-Ga2O3The defect area of crystal
The feature of preferential epitaxial growth GaN, by controlling defect pattern and then can regulate and control the nanocrystalline pattern of GaN.
Above-described embodiment is the present invention preferably embodiment, but embodiments of the present invention are not limited by embodiment
System, the change made, modifies, combines, substitutes, simplifies and all should be under other any spirit without departing from the present invention and principle
Equivalence substitute mode, within being included in protection scope of the present invention.
Claims (6)
1. preparation method nanocrystalline for the GaN of a controllable appearance, it is characterised in that comprise the following steps:
(1) light float zone growth technology growth is used to mix the β-Ga of Mg2O3Monocrystalline;
(2) at β-Ga2O3Form damage in (100) cleavage surface of monocrystalline, or choose surface and have the β-Ga of lattice defect2O3Single
Crystalline substance, by chemical gaseous phase depositing process, is mixing the β-Ga of Mg2O3(100) cleavage surface Epitaxial growth GaN of monocrystalline is nanocrystalline.
Preparation method the most according to claim 1, it is characterised in that the operation of step (2) is: mix the β-Ga of Mg2O3Monocrystalline
Sheet is placed in quartz boat, logical NH3Flow is maintained at 400 sccm, 5 hours heating-up times, and constant temperature 950 DEG C 4 hours, cooling 5 is little
Time.
Preparation method the most according to claim 1, it is characterised in that the operation of step (1) is: gallium oxide powder and oxidation
Magnesium dust grinds, mix homogeneously, makes charge bar, uses vacuum oil pump to take out the air in charge bar, static pressure 5 minutes under 68MPa,
Then fire at 1100 DEG C 4 hours.
Preparation method the most according to claim 1, it is characterised in that in step (1), the doping content of Mg is 0.1at%.
Preparation method the most according to claim 1, it is characterised in that in step (1), crystal growth step includes program liter
Temperature, receive neck, shouldering, isodiametric growth, finish up, lower the temperature.
Preparation method the most according to claim 1, it is characterised in that selecting model in step (1) is FZ-T-12000-X-
The light float zone growth stove of I-S-SU.
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Cited By (2)
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CN106601880A (en) * | 2016-11-21 | 2017-04-26 | 华灿光电(浙江)有限公司 | Epitaxial wafer of gallium-nitride-based light emitting diode, and preparation method of epitaxial wafer |
CN110678990A (en) * | 2017-04-10 | 2020-01-10 | 挪威科技大学 | Nano-structure |
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106601880A (en) * | 2016-11-21 | 2017-04-26 | 华灿光电(浙江)有限公司 | Epitaxial wafer of gallium-nitride-based light emitting diode, and preparation method of epitaxial wafer |
CN110678990A (en) * | 2017-04-10 | 2020-01-10 | 挪威科技大学 | Nano-structure |
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CN110678990B (en) * | 2017-04-10 | 2024-02-06 | 挪威科技大学 | Nanostructure |
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