CN107400919A - Ga is grown using stopped pipe chemical vapor transport mode2O3The method of monocrystalline - Google Patents
Ga is grown using stopped pipe chemical vapor transport mode2O3The method of monocrystalline Download PDFInfo
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- CN107400919A CN107400919A CN201610333352.8A CN201610333352A CN107400919A CN 107400919 A CN107400919 A CN 107400919A CN 201610333352 A CN201610333352 A CN 201610333352A CN 107400919 A CN107400919 A CN 107400919A
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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
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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
- C30B29/16—Oxides
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Abstract
One kind grows Ga using stopped pipe chemical vapor transport mode2O3The method of monocrystalline, including：In the quartz ampoule of closing, one end is put into Ga2O3For powder as source, the other end is put into growth Ga2O3Seed crystal；Source region and the Temperature Distribution of vitellarium are controlled to realize that source region to the gas phase transmission of vitellarium, grows Ga2O3Monocrystalline.Moreover, the carbon dust being put into growth course in the source.In the inventive method, from the point of view of growth course, stopped pipe chemical vapor transport mode is lower than the growth temperature of physical vapor transport, and the addition of carbon dust more increases the vapour pressure of catabolite in quartz ampoule, and growth rate is accelerated, thus the cost grown is than relatively low.
Description
Technical field
The present invention relates to compound semiconductor materials preparing technical field, particularly one kind to use stopped pipe
Chemical vapor transport mode grows Ga2O3The method of monocrystalline.
Background technology
Ga2O3As a kind of wide bandgap compound semiconductor material of direct band gap, there is certain electricity
Conductance, it is not easy by chemical attack, and high mechanical strength, stable performance under high temperature, has high visible
Light and ultraviolet transparency, especially it is transparent in ultraviolet and blue region, therefore is widely used
In various gas sensors, ultraviolet detector, solar cell, offset printing, surface modification, DNA
The fields such as the transparency electrode of detection, liquid crystal display and ultraviolet light emitting device.Ga2O3Forbidden band it is wide
Degree is 4.8-4.9ev, is only second to diamond, electrically conducting transparent of the gallium oxide as broad stopband in a semiconductor material
Oxide, it is applied to TFT now.Ga2O3Material is also successfully used in
Power component is manufactured, and cost is low compared with SiC and performance is outstanding, Ga2O3Band gap it is big, breakdown
Electric-field intensity is also very big, its conducting resistance very little, thus uses Ga2O3Power component can not only
Loss during conducting is reduced, but also the loss of switch can be reduced.Ga2O3Film is bluish-green and purple
There is luminescence generated by light peak in addition, it can be realized in the luminous of different-waveband by adulterating, n-type polycrystalline
Ga2O3Film is a kind of new high temperature gas sensitive.The deep-ultraviolet transparent electric conductivity reported at present
Best β-the Ga for Sn doping2O3Film, Ga2O3Mobility up to 46cm2V-1·S-1。
In addition, the research on transistor also has：P-type Ga2O3The field-effect transistor of channel nanowire,
α-Ga2O3Metal-insulator-semiconductor field effect transistor (MISFET) isostructural spy on substrate
Property.
Ga2O3Fusing point it is very high (about 1800 DEG C), and at ambient pressure, when temperature be increased to it is close
During fusing point, Ga2O3Decomposition pressure than relatively low, and easily there is twin and cleavage.At present, it is international
Upper Ga2O3The growth of body monocrystalline is mainly using pressurized melt growth (czochralski method and float-zone method), change
Learn gas phase transmission and solution growth technique.Because the fusing point of gallium oxide is higher, using solution growth
Method has some difficulties, requires higher to equipment and the high temperature resistant of reaction chamber, and can improve life
Produce cost.The Ga that conventional chemical vapor transport technology obtains2O3Monocrystalline size is smaller, and meeting
Substantial amounts of carrier gas is consumed, while the problem of growth rate is slow be present.In addition, also flame method and
Flux growth metrhod, they can not only introduce substantial amounts of impurity, but also be difficult to obtain large-sized Ga2O3
Monocrystalline.Recent report is shown, the Ga of 2 inch diameters has been grown using float-zone method2O3Monocrystalline, and
The block Ga of 50 mm wides has been grown using deckle film hello method (EFG)2O3Monocrystalline (can be cut out
50×50mm2Single-chip).Therefore, there is an urgent need to improve existing growth technique, new life is proposed
Long technique, prepare the Ga of high quality and low cost2O3Monocrystalline.
The content of the invention
In view of this, the purpose of the present invention is grown in offer one kind using stopped pipe chemical vapor transport mode
Ga2O3The method of monocrystalline.
The present invention provides one kind and grows Ga using stopped pipe chemical vapor transport mode2O3The method of monocrystalline,
Including：
In the quartz ampoule of closing, one end is put into Ga2O3Powder is as source；The other end as vitellarium,
It is put into growth Ga2O3Seed crystal；
Source region and the Temperature Distribution of vitellarium are controlled to realize source region to the gas phase transmission of vitellarium, growth
Ga2O3Monocrystalline.
Preferably, the carbon dust being put into growth course in the source.
Preferably, the seed crystal diameter is identical with the internal diameter of the quartz ampoule, makes the Ga2O3Seed crystal
It can be placed in the quartz ampoule.
Preferably, quartz boat is placed with positioned at source region in the quartz ampoule, to hold the source.
Preferably, closed quartz tube concretely comprises the following steps：The use of one end is that the quartz ampoule that plane is sealed is made
For outer tube, seed crystal is placed on the planar ends of outer tube, then from an external diameter and seed wafer diameter identical
Quartzy siphunculus, for withstanding seed wafer, places a diameter and is less than being used for for inner tube diameter as inner tube
The quartz boat in the source is held in inner tube, placement location is relative with seed crystal position, subsequent outer tube connection
Vacuum system, steep tube sealing with quartz envelope after vacuumizing.
Preferably, the seed crystal be sapphire substrate or gallium oxide single crystal piece, GaN single crystal piece,
ZnO single-chips or A1N single-chips.
Preferably, the carbon and the weight ratio of gallium oxide being put into are 1: 100-1: 50.
Preferably, during gas phase transmission, the temperature of source region is 1050-1200 DEG C, and the temperature of vitellarium is
950-1100 DEG C, thermograde is 2-4 DEG C/cm.
Preferably, the time that gas phase transmission is grown is 70-100 hours.
Preferably, the diameter of the seed crystal is 25.4 millimeters -76.2 millimeters.
Pass through above-mentioned technical proposal, the beneficial effect of technical solution of the present invention are：
(1) high-purity carbon dust is uniformly added in source in growth course, makes catabolite in quartz ampoule
Vapour pressure increase, growth rate accelerate；
(2) Ga grown by chemical vapor transport method of the present invention2O3Monocrystalline, growth temperature are far low
In the growth temperature of pressurized melt growth, conventional chemical vapor transmission and physical vapor transport；
(3) the monocrystalline size diameter of growth is 25.4 millimeters -76.2 millimeters, compared to existing vapor phase method
The Ga of technology growth2O3Nano wire and Ga2O3Film, crystalline size is bigger, improves growth efficiency；
(4) it is enclosed in using quartz ampoule as growth apparatus, whole growth course in quartz ampoule, no
Needing to consume substantial amounts of carrier gas as open pipe system, (such as chlorine, chlorination ammonia gas, iodine steam
Gas), therefore cost is low and the quality of growth material is good；
(5) it is used for the heating furnace of chemical vapor transport method growth, the annealing of crystal can also be carried out
Experiment, this will substantially reduce the equipment expense of Material growth.
Brief description of the drawings
Fig. 1 a and 1b are the chemical vapor transport method growth Ga of a specific embodiment of the invention respectively2O3
The gas phase transmission schematic diagram and temperature of monocrystalline change schematic diagram in pipe.
Fig. 2 a and 2b are the chemical vapor transport method growth Ga of a specific embodiment of the invention respectively2O3
The device perspective view and schematic cross-section of monocrystalline.
Embodiment
It is provided by the invention that Ga is grown using stopped pipe chemical vapor transport mode2O3The method of monocrystalline, bag
Include in the quartz ampoule of closing, one end is put into Ga2O3For powder as source, the other end is put into growth Ga2O3
Seed crystal；Control source region and the Temperature Distribution of vitellarium realize source region to the gas phase transmission of vitellarium,
Grow Ga2O3Monocrystalline.The advantages of this method is that growth temperature is relatively low, the speed of growth is fast, growth apparatus
Cost is low, the quality of material is good.
To increase the vapour pressure of catabolite in quartz ampoule, growth rate is accelerated, preferred growth process
In the carbon dust that is put into the source, the carbon dust amount being put into meets：The carbon and the weight of gallium oxide being put into
It is further preferred for 1: 80-1: 60 than for 1: 100-1: 50.
Wherein, closed quartz tube concretely comprises the following steps：Using one end be plane seal quartz ampoule as
Outer tube, seed crystal are placed on the planar ends of outer tube, then from an external diameter and seed wafer diameter identical stone
English siphunculus, for withstanding seed wafer, places a diameter and is used for containing less than inner tube diameter as inner tube
The quartz boat in the source is put in inner tube, placement location is relative with seed crystal position, and subsequent outer tube connection is true
Empty set is united, and steeps tube sealing with quartz envelope after vacuumizing.
Preferably, a diameter of 25.4 millimeters -76.2 millimeters of said inner tube, it is preferred that Ga2O3Monocrystalline,
Seed crystal and diameter of inner pipe are identical, make the Ga2O3Seed crystal can be placed in the quartz ampoule.This hair
In bright embodiment, the length of inner tube is preferably 200-300 millimeters.
Placement for source, the quartz ampoule is interior to be placed with quartz boat positioned at source region, to hold the source,
The size of quartz boat should be limited with that can be put into the inner tube of quartz ampoule.
Selection for seed crystal material, it can be to grow Ga in the prior art2O3The common seed of monocrystalline
Crystalline substance, preferably grow Ga2O3Seed crystal material for sapphire substrate, gallium oxide single crystal piece, ZnO
Single-chip, GaN single crystal piece or AlN single-chips；Further preferably lattice and Ga2O3More
The sapphire substrate or gallium oxide single crystal piece matched somebody with somebody.
In embodiment of the present invention, during gas phase transmission, the temperature of source region is 1050-1200 DEG C, growth
The temperature in area is 950-1100 DEG C, when the length of inner tube is preferably 200-300 millimeters, thermograde
It is 2-4 DEG C/cm.
Preferably, it is fully growth Ga2O3Monocrystalline and sedimentation time is saved, preferable gas phase transmission
The time grown is 70-100 hours.
According to the preferred embodiment of the present invention, there is provided one kind uses stopped pipe chemical vapor transport mode
Grow Ga2O3The method of monocrystalline, it is specially：
Using the circular quartz pipe that one end is plane sealing as outer tube, the internal diameter of quartz ampoule is according to seed crystal
Depending on the diameter of piece, such as using a diameter of 25.4 millimeters of disk as seed crystal, it is necessary to use internal diameter
27 millimeters of quartz ampoule is as outer tube, to ensure that seed wafer can be put into.An external diameter and seed are selected again
Wafer diameter identical quartz siphunculus, for withstanding seed wafer, makes it be fixed on outer tube as inner tube
Planar ends,.The length of inner tube is depending on the Temperature Distribution needed for experiment, length range 200-300
Millimeter.The quartz boat that one diameter is less than inner tube diameter is used for holding raw material, high-purity Ga2O3Powder
It is mounted in with its mass ratio for 1: 100-1: 50 carbon dust in quartz boat, is positioned over the other end of inner tube,
Subsequent outer tube connection vacuum system, steeps tube sealing after vacuumizing with quartz envelope, and the quartz ampoule for sealing mouth is pacified
It is placed in horizontal heating furnace and carries out heat temperature raising, controls the Temperature Distribution of growing system to carry out Ga2O3It is single
Brilliant growth.
In the preferred embodiment, Ga2O3The temperature control of source region at 1080-1100 DEG C, vitellarium
Temperature control is at 980-1000 DEG C, and thermograde is controlled in 2-4 DEG C/cm, and constant temperature growth time is 70-100
Hour.
In the preferred embodiment, the seed crystal of selection is sapphire substrate or gallium oxide single crystal piece.
In the preferred embodiment, the carbon and the weight ratio of gallium oxide that are put into are 1: 100-1: 50.
For the object, technical solutions and advantages of the present invention are more clearly understood, below in conjunction with specific reality
Example is applied, and referring to the drawings, the present invention is described in further detail.It is following referring to the drawings to this hair
The explanation of bright embodiment is intended to explain the present general inventive concept of the present invention, without should be understood
To limit a kind of of the present invention.
The present embodiment provides one kind and grows Ga using stopped pipe chemical vapor transport mode2O3The method of monocrystalline,
Specifically include：The use of one end is that the circular quartz pipe that plane is sealed is as outer tube, the internal diameter of quartz ampoule
27 millimeters, 35 millimeters of external diameter, make seed crystal with 25.4 millimeters of sapphire wafers of diameter.From one
Overall diameter be 25.4 millimeters of quartzy siphunculus as inner tube, then from a diameter of stone of 20 millimeters
Ying Zhou.
Quartz ampoule used, quartz boat, Feng Pao, seed wafer are carried out corroding cleaning and dried first.
The planar ends first seed wafer being positioned in outer tube, inner tube insertion outer tube is then withstood into seed wafer, then
By the Ga that 20 grams of purity are 4N2O3Uniformly mix, fill for 4N carbon dust powder with 0.2 gram of purity
Enter quartz boat and be placed on the other end of inner tube.
Fig. 1 a are chemical vapor transport method growth Ga2O3The gas phase transmission schematic diagram of monocrystalline, can see
Go out, when being heated to source region, gas phase Ga2O3Move to seed crystal end, progressively carried out on seed crystal
Deposition, Ga of the generation with specific orientation2O3Monocrystalline.In addition, Fig. 1 b are chemical vapor transport methods
Grow Ga2O3The temperature during monocrystalline change schematic diagram in pipe, it can be seen that in the drive of thermograde
Under dynamic, gas phase Ga caused by source region2O3Also tend to the vitellarium being moved to where seed crystal.
Fig. 2 a are chemical vapor transport method growth Ga2O3The device perspective view of monocrystalline, Fig. 2 b are
Chemical vapor transport method grows Ga2O3The device schematic cross-section of monocrystalline.As shown in figures 2 a and 2b,
Envelope bubble is positioned over the openend of outer tube, while holds out against inner tube, for withstanding seed wafer, is fixed on it
The planar ends of outer tube.Then outer tube connection vacuum system, tube sealing is steeped with quartz envelope after vacuumizing, envelope
The quartz ampoule of good mouth, which is placed in horizontal heating furnace, carries out heat temperature raising, controls the temperature point of growing system
Cloth carries out Ga2O3The growth of monocrystalline.Ga2O3The temperature control of source region is at 1080-1100 DEG C, vitellarium
Temperature control at 980-1000 DEG C, thermograde control is in 2-4 DEG C/cm, constant temperature growth time
70-100 hours.
Particular embodiments described above, the purpose of the present invention, technical scheme and beneficial effect are carried out
It is further described, it should be understood that the specific embodiment of the present invention is the foregoing is only,
It is not intended to limit the invention, within the spirit and principles of the invention, any modification for being made,
Equivalent substitution, improvement etc., should be included in the scope of the protection.
Claims (10)
1. one kind grows Ga using stopped pipe chemical vapor transport mode2O3The method of monocrystalline, its feature
It is to include：
In the quartz ampoule of closing, one end is put into Ga2O3Powder is as source；The other end as vitellarium,
It is put into growth Ga2O3Seed crystal；
Source region and the Temperature Distribution of vitellarium are controlled to realize source region to the gas phase transmission of vitellarium, growth
Ga2O3Monocrystalline.
2. according to claim 1 grow Ga using stopped pipe chemical vapor transport mode2O3It is single
Brilliant method, it is characterised in that the carbon dust being put into growth course in the source.
3. according to claim 1 grow Ga using stopped pipe chemical vapor transport mode2O3It is single
Brilliant method, it is characterised in that the seed crystal diameter is identical with the internal diameter of the quartz ampoule, makes described
Ga2O3Seed crystal can be placed in the quartz ampoule.
4. according to claim 1 or 2 grow Ga using stopped pipe chemical vapor transport mode2O3
The method of monocrystalline, it is characterised in that quartz boat is placed with positioned at source region in the quartz ampoule, to hold
The source.
5. according to claim 1 grow Ga using stopped pipe chemical vapor transport mode2O3It is single
Brilliant method, it is characterised in that closed quartz tube concretely comprises the following steps：Sealed using one end for plane
Quartz ampoule as outer tube, seed crystal is placed on the planar ends of outer tube, then from an external diameter and seed wafer
Diameter identical quartz siphunculus, for withstanding seed wafer, places a diameter and is less than inner tube as inner tube
For the quartz boat for being used for holding the source of internal diameter in inner tube, placement location is relative with seed crystal position, with
Outer tube connection vacuum system afterwards, steep tube sealing with quartz envelope after vacuumizing.
6. according to claim 1 grow Ga using stopped pipe chemical vapor transport mode2O3It is single
Brilliant method, it is characterised in that the seed crystal is sapphire substrate or gallium oxide single crystal piece, GaN
Single-chip, ZnO single-chips or A1N single-chips.
7. according to claim 2 grow Ga using stopped pipe chemical vapor transport mode2O3It is single
Brilliant method, it is characterised in that the carbon and the weight ratio of gallium oxide being put into are 1: 100-1: 50.
8. according to claim 1 grow Ga using stopped pipe chemical vapor transport mode2O3It is single
Brilliant method, it is characterised in that during gas phase transmission, the temperature of source region is 1050-1200 DEG C, growth
The temperature in area is 950-1100 DEG C, and thermograde is 2-4 DEG C/cm.
9. according to claim 1 grow Ga using stopped pipe chemical vapor transport mode2O3It is single
Brilliant method, it is characterised in that the time that gas phase transmission is grown is 70-100 hours.
10. according to claim 1 grow Ga using stopped pipe chemical vapor transport mode2O3It is single
Brilliant method, it is characterised in that the diameter of the seed crystal is 25.4 millimeters -76.2 millimeters.
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Cited By (7)
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|---|---|---|---|---|
| CN112522789A (en) * | 2020-11-30 | 2021-03-19 | 中国科学院福建物质结构研究所 | Monoclinic phase Ga2S3Method and apparatus for vapor phase growth of crystal |
| CN112663135A (en) * | 2020-11-30 | 2021-04-16 | 中国科学院福建物质结构研究所 | Monoclinic phase Ga2S3Method and apparatus for physical vapor phase growth of single crystal |
| CN113293429A (en) * | 2021-05-31 | 2021-08-24 | 福州大学 | Monoclinic phase Ga2S3Method for producing single crystal |
| CN114516658A (en) * | 2020-11-18 | 2022-05-20 | 香港城市大学深圳研究院 | Two-step chemical vapor deposition method for growing rare nitride GaNSb nanowire |
| CN115029780A (en) * | 2022-08-11 | 2022-09-09 | 苏州燎塬半导体有限公司 | Growth device and method of N-type conductive gallium oxide single crystal film |
| EP4215649A1 (en) | 2022-01-24 | 2023-07-26 | Ivan Timokhin | Preparation of shaped crystalline layers by use of the inner shape/surface of the ampule as a shape forming surface |
| CN117822107A (en) * | 2024-03-05 | 2024-04-05 | 南京大学 | Method and equipment for generating topological insulator film by chemical vapor deposition method |
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| CN114516658A (en) * | 2020-11-18 | 2022-05-20 | 香港城市大学深圳研究院 | Two-step chemical vapor deposition method for growing rare nitride GaNSb nanowire |
| CN114516658B (en) * | 2020-11-18 | 2023-07-25 | 香港城市大学深圳研究院 | Two-step chemical vapor deposition method for growing dilute nitrided GaNSb nanowire |
| CN112522789A (en) * | 2020-11-30 | 2021-03-19 | 中国科学院福建物质结构研究所 | Monoclinic phase Ga2S3Method and apparatus for vapor phase growth of crystal |
| CN112663135A (en) * | 2020-11-30 | 2021-04-16 | 中国科学院福建物质结构研究所 | Monoclinic phase Ga2S3Method and apparatus for physical vapor phase growth of single crystal |
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| CN113293429A (en) * | 2021-05-31 | 2021-08-24 | 福州大学 | Monoclinic phase Ga2S3Method for producing single crystal |
| EP4215649A1 (en) | 2022-01-24 | 2023-07-26 | Ivan Timokhin | Preparation of shaped crystalline layers by use of the inner shape/surface of the ampule as a shape forming surface |
| CN115029780A (en) * | 2022-08-11 | 2022-09-09 | 苏州燎塬半导体有限公司 | Growth device and method of N-type conductive gallium oxide single crystal film |
| CN117822107A (en) * | 2024-03-05 | 2024-04-05 | 南京大学 | Method and equipment for generating topological insulator film by chemical vapor deposition method |
| CN117822107B (en) * | 2024-03-05 | 2024-05-28 | 南京大学 | Method and equipment for generating topological insulator film by chemical vapor deposition method |
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Application publication date: 20171128 |