CN107740189B - High Al contents AlxGa1-xN ternary alloy three-partalloy microcrystalline balls and preparation method thereof - Google Patents
High Al contents AlxGa1-xN ternary alloy three-partalloy microcrystalline balls and preparation method thereof Download PDFInfo
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- 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
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Abstract
A kind of high Al contents AlxGa1‑xN ternary alloy three-partalloy microcrystalline balls and preparation method thereof belong to the technical field of semiconductor alloy material preparation.The microcrystalline balls are different Al component wurtzite structure AlxGa1‑xN ternary alloy three-partalloy crystal, Al component adjustable extent are 0.77≤x < 1, which is 5.0 μm.The preparation method of the microcrystalline balls is using metallic aluminium powder, gallium and ammonia as reaction raw materials, it vacuumizes, is that 300~700sccm is passed through argon gas with flow, after 10~15min, adjusting argon flow is 40~60sccm, meanwhile it being passed through the ammonia with argon flow same traffic, then heat, reaction temperature is 950~1000 DEG C, 1~3h of time, vapour deposition process growth, prepares the Al of high Al contentsxGa1‑xN ternary alloy three-partalloy microcrystalline balls.This method simple process, it is reproducible, without mutually separation, production cost it is low, without adding any catalyst and template, be easy to commercial introduction application.
Description
Technical field
The invention belongs to the technical fields of semiconductor alloy material preparation, and in particular to a kind of high Al contents AlxGa1-xN tri-
First alloy microcrystalline ball and preparation method thereof.
Background technique
Tri-nitride AlN and GaN are important wide bandgap semiconductor photoelectric material, direct band gap with higher and excellent
Good photoelectric properties.With the fast development of GaN base blue-ray LED, the research of shorter wavelength ultraviolet LED light source has also evoked scientific research
Worker is greatly enthusiastic.High Al contents AlGaN material is to prepare ultraviolet detector, deep-UV light-emitting diode, FPD
The mainstay material of equal photoelectric devices, deep ultraviolet LED prepared therefrom is since small in size, structure is simple, integration is good, and the service life
It is long, power consumption is low, environment-protecting and non-poisonous, has greater advantages than the traditional gas ultraviolet source such as mercury lamp and xenon lamp, have huge society and
Economic benefit.In addition, medical treatment, sterilization, printing, data storage and in terms of have major application value.
Currently, can prepare the LED of ultraviolet band by changing Al component in AlGaN alloy, the increase of Al component makes it
Issue it is shorter wavelengths of shine, but with the increase of Al component, preparation, doping and the luminescent device production of AlGaN alloy
Difficulty is high, and luminous efficiency reduces.Essentially consisting in for deep ultraviolet light source light-emitting efficiency lacks suitable substrate, leads to high Al contents
AlGaN extension ply stress is big, is easy cracking, influences crystal quality.In microcrystalline balls epitaxial growth with the lattice mismatch of substrate material
It is small, eliminate material there are extremely strong stress and polarization fields, it can by the stress major part relaxation generated with substrate fall or all
It eliminates, to improve the raising of LED internal quantum efficiency, overcomes the disadvantage lower along c-axis light-emitting directions efficiency.Therefore, it is based on
The excellent physical property of AlGaN alloy material and its there is potential application prospect in terms of making utility model photoelectric device, it is high
The preparation of the AlGaN alloy of Al component has caused extensive concern, but high Al contents AlGaN semiconductor alloy material
Growth be still also faced with many difficult and challenge.
The synthetic method of AlGaN ternary-alloy material mainly has at present: (1) chloride chemical vapour deposition process；(2) metal
Organic chemical vapor deposition (MOCVD)；(3) molecular beam epitaxy (MBE).The first preparation method, reaction raw materials chloride
It is easy to deliquesce, and price is more expensive.The reactant that second of MOCVD preparation method uses is organic source, needs to carry out gas defence and arranges
It applies.The characteristics of reaction source that the third MBE method uses is simple, but MBE method is due to itself, and it is expensive, no
It is suitble to commercialized development.And all there is spontaneous phenomenon of phase separation in MOCVD and MBE method.
The present invention utilizes homemade gas-phase deposition system, using gallium and business aluminium powder as reaction raw materials, under normal pressure, temperature
Area's (950 DEG C -1000 DEG C) realizes AlGaN tri- by control reaction temperature and the distance between gallium source and growth substrates
The growth of first alloy microcrystalline ball.For the Al for preparing high Al contentsxGa1-xIt is thin to deposit one on a silicon substrate for N ternary alloy three-partalloy semiconductor
Layer metal Al powder, realizes the growing environment of richness Al.There is presently no realize the adjustable Al of high Al contents using the methodxGa1-xN
The report of ternary alloy three-partalloy microcrystalline balls.
Summary of the invention
It is that the present invention solves it is a key issue that providing a kind of high Al contents AlxGa1-xN ternary alloy three-partalloy microcrystalline balls and its preparation
Method, high Al contents AlxGa1-xN ternary alloy three-partalloy microcrystalline balls, Al component adjustable extent are 0.77≤x < 1, and microcrystalline balls are averaged
Diameter is 5 μm, and the preparation method of the microcrystalline balls is the range of reaction temperature using metallic aluminium powder, gallium and ammonia as reaction raw materials
950 DEG C -1000 DEG C, the Al of high Al contents is prepared in vapour deposition process growthxGa1-xN ternary alloy three-partalloy microcrystalline balls.This method work
Skill is simple, it is reproducible, without mutually separation, production cost it is low, without adding any catalyst and template, be easy to commercial introduction and answer
With.
A kind of high Al contents Al of the inventionxGa1-xN ternary alloy three-partalloy microcrystalline balls are different Al component wurtzite structures
AlxGa1-xN ternary alloy three-partalloy crystal, Al component adjustable extent are 0.77≤x < 1, which has regular and uniform
Chondritic, average diameter are 5.0 μm.
The adjustable mode of Al component is to have the silicon chip of thin layer aluminium powder according to reaction temperature and Ga liquid synsedimentary
Distance difference can be adjusted.
The high Al contents AlxGa1-xN ternary alloy three-partalloy microcrystalline balls are canescence.
A kind of high Al contents Al of the inventionxGa1-xThe preparation method of N ternary alloy three-partalloy microcrystalline balls, comprising the following steps:
Step 1, pre-deposition thin layer aluminium powder
(1) silicon chip is ultrasonically treated, the silicon chip after obtaining ultrasound；
Aluminium powder is added in reagent, ultrasonic vibration is carried out and is uniformly dispersed, the aluminium powder mixed liquor after obtaining ultrasound；
(2) in the aluminium powder mixed liquor after the silicon chip after ultrasound to be put into ultrasound, natural air drying obtains being deposited with thin layer of aluminum
The silicon chip of powder；Wherein, the deposition thickness of thin layer aluminium powder is 0.5~1.0mm.
Step 2, preparation is prepared
Metal Al powder is evenly laid out in reaction boat one end, the silicon chip for being deposited with thin layer aluminium powder is being placed in metal Al powder just
Upper vertical distance is to be deposited with the one side of thin layer aluminium powder upward at 5~6mm；
Ga drop is placed in the reaction boat other end, Ga liquid and level of the silicon chip close to Ga liquid end for being deposited with thin layer aluminium powder
Distance is 10~15mm；Wherein, in mass ratio, metal Al powder: Ga=(1~2): 1；
It is spare after entire reaction unit is arranged according to the above method；
Step 3, it vacuumizes, ventilates, heating
(1) reaction unit after arranging is put into quartz test tube open at one end, wherein the reaction dress after arranging
The axis set is parallel with the axis of quartz test tube open at one end, and reacts boat and be put into one end of Ga liquid far from quartz test tube
Opening；
(2) quartz test tube equipped with reaction unit is placed in the reaction zone of horizontal quartz tube furnace, it is closed, start to take out true
It is empty；
As vacuum degree≤5Pa of horizontal quartz tube furnace, it is passed through argon gas, the flow that is passed through of argon gas is 300~700sccm,
After argon gas stream keeps 10~15min, adjusting argon gas and being passed through flow is 40~60sccm, meanwhile, it is passed through ammonia, by flow-rate ratio, argon
Gas: then ammonia=1:1 starts to heat reaction system, and heating rate is 30~50 DEG C/min, when the furnace of reaction system
Temperature reach set temperature be 950~1000 DEG C when, keep 1~3h after, stop heating；
(3) furnace cooling, when temperature is down to 650~750 DEG C, closing ammonia flow is continually fed into argon gas, guarantees argon atmospher
It encloses, cools to room temperature with the furnace；
(4) completely after cooling, reaction unit is taken out, being deposited on substance on thin layer aluminium powder silicon substrate surface is AlxGa1-xN
Ternary alloy three-partalloy microcrystalline balls.
It is described that ultrasonic treatment specific steps are carried out to silicon chip are as follows: to spend ionized water or second in the step 1 (1)
Alcohol is cleaned by ultrasonic silicon chip, and its object is to be cleaned by ultrasonic the surface impurity of silicon chip.
In the step 1 (1), the purity of the aluminium powder is >=99.999%, and average grain diameter is 5~10 μm.
In the step 1 (1), the reagent of the aluminium powder ultrasonic vibration is one in ethyl alcohol, methanol, acetone or hexane
Kind or several mixing, the additional amount of reagent be that be subject to aluminium powder fully dispersed in reagent；
In the step 1 (1), the time of the ultrasonic vibration is 10~60min.
In the step 2, the purity of the metal Al powder is >=99.999%, and average grain diameter is 5~10 μm.
In the step 2, the silicon chip of thin layer aluminium powder will be deposited with as growth substrates.
In the step 2, the reaction boat is aluminium oxide ceramics boat.
In the step 3 (2), described vacuum degree≤5Pa when horizontal quartz tube furnace, the purpose for being passed through argon gas exists
In to reaction system progress gas washing, being passed through the time is 10~15min.
It is above-mentioned, the flow control of gas is passed through using mass flowmenter.
A kind of high Al contents Al of the inventionxGa1-xN ternary alloy three-partalloy microcrystalline balls and preparation method thereof, compared to existing skill
Art, the beneficial effect is that:
1. synthetic method of the invention is a kind of vapor transport deposition method, on a silicon substrate the thin aluminium of the one of pre-deposition layer
Powder is AlxGa1-xN ternary alloy three-partalloy microcrystalline balls can on silicon chip substrate epitaxial growth key, one layer deposited on silicon chip
Thin aluminium powder is on the one hand can to make AlN self-catalysis nucleation on a silicon substrate, to realize AlxGa1-xThe extension of N alloy microcrystalline ball
Growth, overcomes under condition of normal pressure, 900 DEG C of -1000 DEG C of warm area pure metal sources and NH3It can not be on silicon substrate in reaction system
The difficulty that core, nucleation rate are low and binding force is poor；On the other hand the growing environment of rich Al can be provided, promotes high Al contents
AlxGa1-xThe growth of N semiconducting alloy, and inhibit the phenomenon that mutually to separate.
2. the quartz test tube open at one end that the present invention uses facilitates the vapour pressure concentration of concentrating metals Ga and Al, metal
The difference of Ga drop and silicon chip distance results in different Al component AlxGa1-xThe formation of N alloy.
3. the present invention has reaction raw materials simple, preparation process is simple, range of deposition is larger, reproducible, without mutually separating,
The features such as production cost is low and easy to spread is applicable to largely industrialize growth AlGaN crystallite sphere.
4. any catalyst is not used in the present invention, using Al self-catalysis Direct-Nitridation method, it is fine to realize different Al components
Zinc ore structure AlxGa1-xN ternary alloy three-partalloy microcrystalline balls.
Detailed description of the invention
Fig. 1 is present invention growth AlxGa1-xThe experiment schematic diagram of N ternary alloy three-partalloy microcrystalline balls.
It is 10-15mm, the Al prepared under the conditions of 950 DEG C that Fig. 2, which is the source Ga away from silicon chip distance,xGa1-xThe XRD diagram of N alloy
Spectrum: x is the ratio of Al component.
Fig. 3 is Al0.77Ga0.23The scanning electron microscopic picture of N ternary alloy three-partalloy microcrystalline balls；Wherein, amplification factor 2000 ×.
Specific embodiment
Below with reference to embodiment, the present invention is described in further detail.
In following embodiment, the quartz test tube diameter used is 20mm, a length of 150mm.
In following embodiment, the quartz tube 80mm of horizontal quartz tube furnace, constant temperature section length is 34.5cm, uses quality
Flowmeter controls gas flow.
In following embodiment, the growth Al of usexGa1-xThe experiment schematic diagram of N ternary alloy three-partalloy microcrystalline balls is shown in Fig. 1.
Embodiment 1
A kind of high Al contents AlxGa1-xN ternary alloy three-partalloy microcrystalline balls are the Al of x=0.77xGa1-xN semiconducting alloy, XRD
TuPu method peak (100), the angle of diffraction of (002) and (101) show to produce between the angle of diffraction of wurtzite structure AlN and GaN
Object is to see Fig. 2 with wurtzite structure AlGaN crystal.
To high Al contents AlxGa1-xN (x=0.77) microcrystalline balls are scanned analysis, and scanning electron microscope (SEM) photograph is shown in Fig. 3, from figure
In it can be concluded that, Al0.77Ga0.23The pattern of N ternary alloy three-partalloy microcrystalline balls, the microcrystalline balls have rule and uniform spherical knot
Structure, average diameter are 5.0 μm.
A kind of high Al contents AlxGa1-xThe preparation method of N ternary alloy three-partalloy microcrystalline balls, comprising the following steps:
Step 1, pre-deposition thin layer aluminium powder
(1) silicon chip is ultrasonically treated with deionized water, the silicon chip after cleaning, after obtaining ultrasound；
It is that the aluminium powder that 99.999 average grain diameters are 5 μm is added in ethyl alcohol by purity, carries out ultrasonic vibration 20min, work as aluminium powder
Aluminium powder mixed liquor after being uniformly dispersed, after obtaining ultrasound；
(2) in the aluminium powder mixed liquor after the silicon chip after ultrasound to be put into ultrasound, natural air drying obtains being deposited with thin layer of aluminum
The silicon chip of powder；The deposition thickness of thin layer aluminium powder is 0.5mm.
Step 2, preparation is prepared
The metal Al powder for being 99.999% by 10g purity is evenly laid out in aluminium oxide ceramics boat one end, will be deposited with thin layer
For the silicon chip of aluminium powder as growth substrates, being placed in vertical range right above metal Al powder is to be deposited with thin layer aluminium powder at 5~6mm
One side upward；
5g Ga drop is placed in the aluminium oxide ceramics boat other end, Ga liquid and is deposited with the silicon chip of thin layer aluminium powder close to Ga
The horizontal distance at liquid end is 10mm；
It is spare after entire reaction unit is arranged according to the above method；
Step 3, it vacuumizes, ventilates, heating
(1) reaction unit after arranging is put into quartz test tube open at one end, wherein the reaction dress after arranging
The axis set is parallel with the axis of quartz test tube open at one end, and aluminium oxide ceramics boat is put into one end of Ga liquid far from quartz
The opening of test tube；
(2) quartz test tube equipped with reaction unit is placed in the reaction zone of horizontal quartz tube furnace, it is closed, start to take out true
It is empty；
As vacuum degree≤5Pa of horizontal quartz tube furnace, it is passed through argon gas and gas washing is carried out to reaction system, argon gas is passed through stream
Measuring is 500sccm, and after 15min, adjusting argon gas and being passed through flow is 50sccm, and being passed through ammonia flow is 50sccm, is then started
Reaction system is heated, heating rate is 30 DEG C/min, when it is 950 DEG C that the furnace temperature of reaction system, which reaches set temperature,
After keeping 2h, stop heating；
(3) furnace cooling, when temperature is down to 700 DEG C, closing ammonia flow is continually fed into argon gas, guarantees argon atmosphere, with
Furnace is cooled to room temperature；
(4) completely after cooling, taking-up reaction unit, the greyish white substance being deposited on thin layer aluminium powder silicon substrate surface, as
AlxGa1-xN ternary alloy three-partalloy microcrystalline balls.
Embodiment 2
A kind of high Al contents AlxGa1-xN ternary alloy three-partalloy microcrystalline balls are AlxGa1-xN semiconducting alloy has wurtzite structure
AlGaN crystal.The microcrystalline balls have rule and uniform chondritic, and average diameter is 5.0 μm.
A kind of high Al contents AlxGa1-xThe preparation method of N ternary alloy three-partalloy microcrystalline balls, comprising the following steps:
Step 1, pre-deposition thin layer aluminium powder
(1) silicon chip is ultrasonically treated with ethyl alcohol, the silicon chip after cleaning, after obtaining ultrasound；
It is that the aluminium powder that 99.999 average grain diameters are 10 μm is added in methanol by purity, carries out ultrasonic vibration 60min, work as aluminium powder
Aluminium powder mixed liquor after being uniformly dispersed, after obtaining ultrasound；
(2) in the aluminium powder mixed liquor after the silicon chip after ultrasound to be put into ultrasound, natural air drying obtains being deposited with thin layer of aluminum
The silicon chip of powder；The deposition thickness of thin layer aluminium powder is 1.0mm.
Step 2, preparation is prepared
It is that metal Al powder that 99.999% average grain diameter is 5 μm is evenly laid out in aluminium oxide ceramics boat one end by 5g purity,
Using the silicon chip for being deposited with thin layer aluminium powder as growth substrates, being placed in vertical range right above metal Al powder is to sink at 5~6mm
Product has the one side of thin layer aluminium powder upward；
5g Ga drop is placed in the aluminium oxide ceramics boat other end, Ga liquid and is deposited with the silicon chip of thin layer aluminium powder close to Ga
The horizontal distance at liquid end is 15mm；
It is spare after entire reaction unit is arranged according to the above method；
Step 3, it vacuumizes, ventilates, heating
(1) reaction unit after arranging is put into quartz test tube open at one end, wherein the reaction dress after arranging
The axis set is parallel with the axis of quartz test tube open at one end, and aluminium oxide ceramics boat is put into one end of Ga liquid far from quartz
The opening of test tube；
(2) quartz test tube equipped with reaction unit is placed in the reaction zone of horizontal quartz tube furnace, it is closed, start to take out true
It is empty；
As vacuum degree≤5Pa of horizontal quartz tube furnace, it is passed through argon gas and gas washing is carried out to reaction system, argon gas is passed through stream
Measuring is 700sccm, and after 10min, adjusting argon gas and being passed through flow is 50sccm, and being passed through ammonia flow is 50sccm, is then started
Reaction system is heated, heating rate is 50 DEG C/min, when it is 950 DEG C that the furnace temperature of reaction system, which reaches set temperature,
After keeping 1h, stop heating；
(3) furnace cooling, when temperature is down to 750 DEG C, closing ammonia flow is continually fed into argon gas, guarantees argon atmosphere, with
Furnace is cooled to room temperature；
(4) completely after cooling, taking-up reaction unit, the greyish white substance being deposited on thin layer aluminium powder silicon substrate surface, as
AlxGa1-xN ternary alloy three-partalloy microcrystalline balls.
Embodiment 3
A kind of high Al contents AlxGa1-xN ternary alloy three-partalloy microcrystalline balls are AlxGa1-xN semiconducting alloy has wurtzite structure
AlGaN crystal.The microcrystalline balls have rule and uniform chondritic, and average diameter is 5.0 μm.
A kind of high Al contents AlxGa1-xThe preparation method of N ternary alloy three-partalloy microcrystalline balls, comprising the following steps:
Step 1, pre-deposition thin layer aluminium powder
(1) silicon chip is ultrasonically treated with deionized water, the silicon chip after cleaning, after obtaining ultrasound；
It is that the aluminium powder that 99.999 average grain diameters are 8 μm is added in methanol by purity, carries out ultrasonic vibration 40min, work as aluminium powder
Aluminium powder mixed liquor after being uniformly dispersed, after obtaining ultrasound；
(2) in the aluminium powder mixed liquor after the silicon chip after ultrasound to be put into ultrasound, natural air drying obtains being deposited with thin layer of aluminum
The silicon chip of powder；The deposition thickness of thin layer aluminium powder is 0.8mm.
Step 2, preparation is prepared
It is that metal Al powder that 99.999% average grain diameter is 10 μm is evenly laid out in aluminium oxide ceramics boat one end by 5g purity,
Using the silicon chip for being deposited with thin layer aluminium powder as growth substrates, being placed in vertical range right above metal Al powder is to sink at 5~6mm
Product has the one side of thin layer aluminium powder upward；
5g Ga drop is placed in the aluminium oxide ceramics boat other end, Ga liquid and is deposited with the silicon chip of thin layer aluminium powder close to Ga
The horizontal distance at liquid end is 13mm；
It is spare after entire reaction unit is arranged according to the above method；
Step 3, it vacuumizes, ventilates, heating
(1) reaction unit after arranging is put into quartz test tube open at one end, wherein the reaction dress after arranging
The axis set is parallel with the axis of quartz test tube open at one end, and aluminium oxide ceramics boat is put into one end of Ga liquid far from quartz
The opening of test tube；
(2) quartz test tube equipped with reaction unit is placed in the reaction zone of horizontal quartz tube furnace, it is closed, start to take out true
It is empty；
As vacuum degree≤5Pa of horizontal quartz tube furnace, it is passed through argon gas and gas washing is carried out to reaction system, argon gas is passed through stream
Measuring is 300sccm, and after 15min, adjusting argon gas and being passed through flow is 60sccm, and being passed through ammonia flow is 60sccm, is then started
Reaction system is heated, heating rate is 40 DEG C/min, when it is 1000 DEG C that the furnace temperature of reaction system, which reaches set temperature,
After keeping 3h, stop heating；
(3) furnace cooling, when temperature is down to 650 DEG C, closing ammonia flow is continually fed into argon gas, guarantees argon atmosphere, with
Furnace is cooled to room temperature；
(4) completely after cooling, taking-up reaction unit, the greyish white substance being deposited on thin layer aluminium powder silicon substrate surface, as
AlxGa1-xN ternary alloy three-partalloy microcrystalline balls.
Claims (9)
1. a kind of high Al contents AlxGa1-xN ternary alloy three-partalloy microcrystalline balls, which is characterized in that high Al contents AlxGa1-xN ternary alloy three-partalloy
Microcrystalline balls are different Al component wurtzite structure AlxGa1-xN ternary alloy three-partalloy crystal, Al component adjustable extent are 0.77≤x < 1,
The microcrystalline balls have rule and uniform chondritic, and average diameter is 5.0 μm.
2. high Al contents Al as described in claim 1xGa1-xN ternary alloy three-partalloy microcrystalline balls, which is characterized in that the Al component
Adjustable mode is, has the distance difference of the silicon chip of thin layer aluminium powder that can be adjusted according to reaction temperature and Ga liquid synsedimentary
Section.
3. high Al contents Al described in claim 1xGa1-xThe preparation method of N ternary alloy three-partalloy microcrystalline balls, which is characterized in that including
Following steps:
Step 1, pre-deposition thin layer aluminium powder
(1) silicon chip is ultrasonically treated, the silicon chip after obtaining ultrasound；
Aluminium powder is added in reagent, ultrasonic vibration is carried out and is uniformly dispersed, the aluminium powder mixed liquor after obtaining ultrasound；
(2) in the aluminium powder mixed liquor after the silicon chip after ultrasound to be put into ultrasound, natural air drying obtains being deposited with thin layer aluminium powder
Silicon chip；Wherein, the deposition thickness of thin layer aluminium powder is 0.5 ~ 1.0mm；
Step 2, preparation is prepared
Metal Al powder is evenly laid out in reaction boat one end, the silicon chip for being deposited with thin layer aluminium powder is placed in right above metal Al powder
Vertical range is to be deposited with the one side of thin layer aluminium powder upward at 5 ~ 6mm；
Ga drop is placed in the reaction boat other end, Ga liquid and horizontal distance of the silicon chip close to Ga liquid end for being deposited with thin layer aluminium powder
For 10 ~ 15mm；Wherein, in mass ratio, metal Al powder: Ga=(1 ~ 2): 1；
It is spare after entire reaction unit is arranged according to the above method；
Step 3, it vacuumizes, ventilates, heating
(1) reaction unit after arranging is put into quartz test tube open at one end, wherein reaction unit after arranging
Axis is parallel with the axis of quartz test tube open at one end, and reacts one end opening far from quartz test tube that boat is put into Ga liquid
Mouthful；
(2) quartz test tube equipped with reaction unit is placed in the reaction zone of horizontal quartz tube furnace, it is closed, start to vacuumize；
As vacuum degree≤5Pa of horizontal quartz tube furnace, it is passed through argon gas, the flow that is passed through of argon gas is 300 ~ 700sccm, argon gas stream
After keeping 10 ~ 15min, adjusting argon gas and being passed through flow is 40 ~ 60sccm, meanwhile, it is passed through ammonia, by flow-rate ratio, argon gas: ammonia=
Then 1:1 starts to heat reaction system, heating rate is 30 ~ 50 DEG C/min, when the furnace temperature of reaction system reaches setting
When temperature is 950 ~ 1000 DEG C, after keeping 1 ~ 3h, stop heating；
(3) furnace cooling, when temperature is down to 650 ~ 750 DEG C, closing ammonia flow is continually fed into argon gas, guarantees argon atmosphere, with
Furnace is cooled to room temperature；
(4) completely after cooling, reaction unit is taken out, being deposited on substance on thin layer aluminium powder silicon substrate surface is AlxGa1-xN ternary
Alloy microcrystalline ball.
4. high Al contents Al as claimed in claim 3xGa1-xThe preparation method of N ternary alloy three-partalloy microcrystalline balls, which is characterized in that institute
It is described that ultrasonic treatment specific steps are carried out to silicon chip in the step 1 (1) stated are as follows: to spend ionized water or ethyl alcohol to silicon chip
It is cleaned by ultrasonic.
5. high Al contents Al as claimed in claim 3xGa1-xThe preparation method of N ternary alloy three-partalloy microcrystalline balls, which is characterized in that institute
In the step 1 (1) stated, the purity of the aluminium powder is >=99.999%, and average grain diameter is 5 ~ 10 μm.
6. high Al contents Al as claimed in claim 3xGa1-xThe preparation method of N ternary alloy three-partalloy microcrystalline balls, which is characterized in that institute
In the step 1 (1) stated, the reagent of the aluminium powder ultrasonic vibration is that one or more of ethyl alcohol, methanol, acetone or hexane are mixed
It closes, the additional amount of reagent is that be subject to aluminium powder fully dispersed in reagent.
7. high Al contents Al as claimed in claim 3xGa1-xThe preparation method of N ternary alloy three-partalloy microcrystalline balls, which is characterized in that institute
In the step 1 (1) stated, the time of the ultrasonic vibration is 10 ~ 60min.
8. high Al contents Al as claimed in claim 3xGa1-xThe preparation method of N ternary alloy three-partalloy microcrystalline balls, which is characterized in that institute
In the step 2 stated, the purity of the metal Al powder is >=99.999%, and average grain diameter is 5 ~ 10 μm.
9. high Al contents Al as claimed in claim 3xGa1-xThe preparation method of N ternary alloy three-partalloy microcrystalline balls, which is characterized in that institute
In the step 2 stated, the reaction boat is aluminium oxide ceramics boat.
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| CN101477950A (en) * | 2009-01-20 | 2009-07-08 | 苏州纳米技术与纳米仿生研究所 | Synthesizing process for InN, GaN and AIN low-dimensional nano structure material |
| CN102127807A (en) * | 2011-01-31 | 2011-07-20 | 南京大学 | Method for preparing ternary-component AlxGaI-xN nanocone |
| CN104313548A (en) * | 2014-10-08 | 2015-01-28 | 上海理工大学 | Preparation method of gallium nitride nanowires |
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| CN101477950A (en) * | 2009-01-20 | 2009-07-08 | 苏州纳米技术与纳米仿生研究所 | Synthesizing process for InN, GaN and AIN low-dimensional nano structure material |
| CN102127807A (en) * | 2011-01-31 | 2011-07-20 | 南京大学 | Method for preparing ternary-component AlxGaI-xN nanocone |
| CN104313548A (en) * | 2014-10-08 | 2015-01-28 | 上海理工大学 | Preparation method of gallium nitride nanowires |
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