CN107740189A - 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
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
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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 components wurtzite structure AlxGa1‑xN ternary alloy three-partalloy crystal, Al components adjustable extent are 0.77≤x ＜ 1, and the crystallite mean diameter of a ball is 5.0 μm.The preparation method of the microcrystalline balls is using metallic aluminium powder, gallium and ammonia as reaction raw materials, vacuumize, argon gas is passed through using flow as 300~700sccm, after 10~15min, regulation argon flow amount is 40~60sccm, meanwhile the ammonia with argon flow amount same traffic is passed through, then heat, reaction temperature is 950~1000 DEG C, 1~3h of time, vapour deposition process grow, and prepare the Al of high Al contentsxGa1‑xN ternary alloy three-partalloy microcrystalline balls.This method technique is simple, it is reproducible, without be separated, production cost is low, without any catalyst and template is added, be easy to commercial introduction application.
Description
Technical field
The invention belongs to technical field prepared by semiconductor alloy material, and in particular to a kind of high Al contents AlxGa1-xN tri-
First alloy microcrystalline ball and preparation method thereof.
Background technology
III-nitride AlN and GaN are important wide bandgap semiconductor photoelectric materials, have higher direct band gap 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's greatly enthusiasm.High Al contents AlGaN material is to prepare ultraviolet detector, deep-UV light-emitting diode, FPD
Deng the mainstay material of photoelectric device, deep ultraviolet LED prepared therefrom is due to small volume, simple in construction, integration is good, and the life-span
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, there is major application value in medical treatment, sterilization, printing, data storage and secret communication etc..
At present, the LED of ultraviolet band can be prepared by changing Al components in AlGaN alloys, the increase of Al components makes it
Send it is shorter wavelengths of luminous, but as the increase of Al components, preparation, doping and the luminescent device of AlGaN alloys make
Difficulty is high, and luminous efficiency reduces.Essentially consisting in for deep ultraviolet light source light-emitting efficiency lacks suitable substrate, causes high Al contents
AlGaN extension ply stress is big, and easily cracking, influences crystal mass.In microcrystalline balls epitaxial growth with the lattice mismatch of backing material
It is small, eliminate material extremely strong stress and polarization field be present, you can with will fall with stress major part relaxation caused by substrate or all
Eliminate, so as to improve the raising of LED internal quantum efficiency, overcome along c-axis light-emitting directions it is less efficient the shortcomings that.Therefore, it is based on
The excellent physical property of AlGaN alloy materials and its there is potential application prospect in terms of utility model photoelectric device is made, it is high
The preparation of the AlGaN alloys of Al components has caused extensive concern, but high Al contents AlGaN semiconductor alloy materials
Growth is still also faced with many difficult and challenge.
The synthetic method of AlGaN ternary-alloy materials 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, its reaction raw materials chloride
Easy deliquescence, and it is expensive.The reactant that second of MOCVD preparation method uses is that organic source is arranged, it is necessary to carry out gas defence
Apply.The characteristics of reaction source that the third MBE method uses is simple, but MBE methods are due to itself, and it is costly, no
It is adapted to commercialized development.And all there is spontaneous phenomenon of phase separation in MOCVD and MBE methods.
The present invention utilizes homemade gas-phase deposition system, using gallium and business aluminium powder as reaction raw materials, at ambient pressure, temperature
Area's (950 DEG C -1000 DEG C), by controlling reaction temperature and the distance between gallium source and growth substrates, realizes AlGaN ternarys
The growth of alloy microcrystalline ball.To prepare the Al of high Al contentsxGa1-xN ternary alloy three-partalloy semiconductors, deposit a thin layer on a silicon substrate
Metal Al powder, realize rich Al growing environment.There is presently no realize the adjustable Al of high Al contents using the methodxGa1-xN tri-
The report of first alloy microcrystalline ball.
The content 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-partalloys microcrystalline balls and its preparation
Method, high Al contents AlxGa1-xN ternary alloy three-partalloy microcrystalline balls, Al components adjustable extent are 0.77≤x ＜ 1, and microcrystalline balls are averaged
A diameter of 5 μm, 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, vapour deposition process grows, and prepares the Al of high Al contentsxGa1-xN ternary alloy three-partalloy microcrystalline balls.This method technique
Simply, it is reproducible, without be separated, production cost is low, without any catalyst and template is added, be easy to commercial introduction application.
A kind of high Al contents Al of the present inventionxGa1-xN ternary alloy three-partalloy microcrystalline balls, it is different Al components wurtzite structures
AlxGa1-xN ternary alloy three-partalloy crystal, Al components adjustable extent are 0.77≤x ＜ 1, and the microcrystalline balls have regular and uniform
Chondritic, average diameter are 5.0 μm.
The described adjustable mode of Al components is to have the silicon chip of thin layer aluminium powder according to reaction temperature and Ga liquid synsedimentarys
Distance difference can be adjusted.
Described high Al contents AlxGa1-xN ternary alloy three-partalloys microcrystalline balls are canescence.
A kind of high Al contents Al of the present inventionxGa1-xThe preparation method of N ternary alloy three-partalloy microcrystalline balls, comprises the following steps：
Step 1, pre-deposition thin layer aluminium powder
(1) silicon chip is ultrasonically treated, obtains the silicon chip after ultrasound；
Aluminium powder is added in reagent, ultrasonic vibration is carried out and is uniformly dispersed, obtain the aluminium powder mixed liquor after ultrasound；
(2) silicon chip after ultrasound is put into the aluminium powder mixed liquor after ultrasound, natural air drying, obtaining deposition has thin layer of aluminum
The silicon chip of powder；Wherein, the deposit 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 that deposition has thin layer aluminium powder is being placed in metal Al powder just
Upper vertical distance is at 5~6mm, deposition has the one side of thin layer aluminium powder upward；
Ga drops are placed in the reaction boat other end, Ga liquid has level of the silicon chip close to Ga liquid end of thin layer aluminium powder with deposition
Distance is 10~15mm；Wherein, in mass ratio, metal Al powder：Ga=(1~2):1；
It is standby after whole reaction unit is arranged as stated above；
Step 3, vacuumize, ventilate, heating
(1) reaction unit after arranging is put into the quartz test tube of one end open, wherein, the reaction dress after arranging
The axis and the diameter parallel of the quartz test tube of one end open put, and react boat and be put into one end of Ga liquid away from quartz test tube
Opening；
(2) quartz test tube equipped with reaction unit is placed in the reaction zone of horizontal quartz tube stove, it is closed, start to take out very
It is empty；
As vacuum≤5Pa of horizontal quartz tube stove, argon gas is passed through, the flow that is passed through of argon gas is 300~700sccm,
After argon gas stream keeps 10~15min, it is 40~60sccm that regulation argon gas, which is passed through flow, meanwhile, ammonia is passed through, by flow-rate ratio, argon
Gas：Ammonia=1:1, then start to heat reaction system, heating rate is 30~50 DEG C/min, when the stove of reaction system
Temperature reach design temperature for 950~1000 DEG C when, keep 1~3h after, stop heating；
(3) furnace cooling, when temperature is down to 650~750 DEG C, ammonia flow is closed, is continually fed into argon gas, ensures argon atmospher
Enclose, cool to room temperature with the furnace；
(4) completely after cooling, reaction unit is taken out, it is Al to be deposited on material on thin layer aluminium powder silicon substrate surfacexGa1-xN
Ternary alloy three-partalloy microcrystalline balls.
It is described supersound process is carried out to silicon chip to concretely comprise the following steps in described step 1 (1)：With deionized water or second
Alcohol is cleaned by ultrasonic to silicon chip, and its object is to be cleaned by ultrasonic the surface impurity of silicon chip.
In described step 1 (1), the purity of described aluminium powder is >=99.999%, and its average grain diameter is 5~10 μm.
In described step 1 (1), the reagent of described aluminium powder ultrasonic vibration is one in ethanol, methanol, acetone or hexane
Kind or several mixing, the addition of reagent be to be defined so that aluminium powder is fully dispersed in reagent；
In described step 1 (1), the time of described ultrasonic vibration is 10~60min.
In described step 2, the purity of described metal Al powder is >=99.999%, and its average grain diameter is 5~10 μm.
In described step 2, the silicon chip for having thin layer aluminium powder will be deposited as growth substrates.
In described step 2, described reaction boat is aluminium oxide ceramics boat.
It is described when vacuum≤5Pa of horizontal quartz tube stove, the purpose for being passed through argon gas exist in described step 3 (2)
In to reaction system progress gas washing, it is 10~15min to be passed through the time.
Above-mentioned, the flow control for being passed through gas uses mass flowmenter.
A kind of high Al contents Al of the present inventionxGa1-xN ternary alloy three-partalloy microcrystalline balls and preparation method thereof, compared to existing skill
Art, its advantage are：
1. the synthetic method of the present invention is a kind of vapor transport deposition method, one layer of thin aluminium of its pre-deposition on a silicon substrate
Powder is AlxGa1-xN ternary alloy three-partalloys microcrystalline balls can deposit one layer thin in the key of silicon chip substrate Epitaxial growth, silicon chip
Aluminium powder is on the one hand can to make AlN self-catalysis nucleation on a silicon substrate, so as to realize AlxGa1-xThe extension life of N alloy microcrystalline balls
It is long, overcome under condition of normal pressure, 900 DEG C of -1000 DEG C of warm area pure metal sources and NH3Can not be nucleated on silicon substrate in reaction system,
The difficulty that nucleation rate is low and adhesion is poor；On the other hand rich Al growing environment can be provided, promote high Al contents AlxGa1-xN
The growth of semiconducting alloy, and suppress the phenomenon being separated.
2. the quartz test tube for the one end open that the present invention uses contributes to concentrating metals Ga and Al vapour pressure concentration, metal
Ga drops and the difference of silicon chip distance, result in different Al components AlxGa1-xThe formation of N alloys.
3. the present invention has, reaction raw materials are simple, and preparation technology is simple, range of deposition is larger, reproducible, no phase separation,
The features such as production cost is low and easy to spread, it is applicable to substantial amounts of industrialization growth AlGaN crystallite spheroids.
4. any catalyst is not used in the present invention, using Al self-catalysis Direct-Nitridation methods, it is fine to realize different Al components
Zinc ore structure AlxGa1-xN ternary alloy three-partalloy microcrystalline balls.
Brief description of the drawings
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 Ga sources away from silicon chip distance,xGa1-xThe XRD of N alloys
Spectrum：X is the ratio of Al components.
Fig. 3 is Al0.77Ga0.23The scanning electron microscopic picture of N ternary alloy three-partalloy microcrystalline balls；Wherein, multiplication factor 2000 ×.
Embodiment
With reference to embodiment, the present invention is described in further detail.
In following examples, the quartz test tube a diameter of 20mm, a length of 150mm of use.
In following examples, the quartz tube 80mm of horizontal quartz tube stove, constant temperature section length is 34.5cm, uses quality
Flowmeter controls gas flow.
In following examples, 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, it is x=0.77 AlxGa1-xN semiconducting alloys, its XRD
TuPu method peak (100), the angle of diffraction of (002) and (101) show to produce between the wurtzite structure AlN and GaN angle of diffraction
Thing is with wurtzite structure AlGaN crystal, sees Fig. 2.
To high Al contents AlxGa1-xN (x=0.77) microcrystalline balls are scanned analysis, and its scanning electron microscope (SEM) photograph is shown in Fig. 3, from figure
In can draw, Al0.77Ga0.23The pattern of N ternary alloy three-partalloy microcrystalline balls, the microcrystalline balls have regular and uniform spherical knot
Structure, its average diameter are 5.0 μm.
A kind of high Al contents AlxGa1-xThe preparation method of N ternary alloy three-partalloy microcrystalline balls, comprises the following steps：
Step 1, pre-deposition thin layer aluminium powder
(1) silicon chip is ultrasonically treated with deionized water, after cleaning, obtains the silicon chip after ultrasound；
It is that the aluminium powder that 99.999 average grain diameters are 5 μm is added in ethanol by purity, carries out ultrasonic vibration 20min, work as aluminium powder
After being uniformly dispersed, the aluminium powder mixed liquor after ultrasound is obtained；
(2) silicon chip after ultrasound is put into the aluminium powder mixed liquor after ultrasound, natural air drying, obtaining deposition has thin layer of aluminum
The silicon chip of powder；The deposit thickness of thin layer aluminium powder is 0.5mm.
Step 2, preparation is prepared
10g purity is evenly laid out in aluminium oxide ceramics boat one end for 99.999% metal Al powder, deposition there is into thin layer
The silicon chip of aluminium powder is as growth substrates, and it is at 5~6mm to be placed in vertical range directly over metal Al powder, and deposition has thin layer aluminium powder
One side upward；
5g Ga drops are placed in the aluminium oxide ceramics boat other end, Ga liquid has the silicon chip of thin layer aluminium powder close to Ga with deposition
The horizontal range at liquid end is 10mm；
It is standby after whole reaction unit is arranged as stated above；
Step 3, vacuumize, ventilate, heating
(1) reaction unit after arranging is put into the quartz test tube of one end open, wherein, the reaction dress after arranging
The axis and the diameter parallel of the quartz test tube of one end open put, and aluminium oxide ceramics boat is put into one end of Ga liquid away 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 stove, it is closed, start to take out very
It is empty；
As vacuum≤5Pa of horizontal quartz tube stove, it is passed through argon gas and gas washing is carried out to reaction system, argon gas is passed through stream
Measure as 500sccm, after 15min, it is 50sccm that regulation argon gas, which is passed through flow, and it is 50sccm to be passed through ammonia flow, 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 design temperature,
After keeping 2h, stop heating；
(3) furnace cooling, when temperature is down to 700 DEG C, ammonia flow is closed, is continually fed into argon gas, ensures argon atmosphere, with
Stove is cooled to room temperature；
(4) completely after cooling, reaction unit is taken out, the greyish white material being deposited on thin layer aluminium powder silicon substrate surface, is
AlxGa1-xN ternary alloy three-partalloy microcrystalline balls.
Embodiment 2
A kind of high Al contents AlxGa1-xN ternary alloy three-partalloy microcrystalline balls, it is AlxGa1-xN semiconducting alloys, there is wurtzite structure
AlGaN crystal.The microcrystalline balls have regular and uniform chondritic, and its average diameter is 5.0 μm.
A kind of high Al contents AlxGa1-xThe preparation method of N ternary alloy three-partalloy microcrystalline balls, comprises the following steps：
Step 1, pre-deposition thin layer aluminium powder
(1) silicon chip is ultrasonically treated with ethanol, after cleaning, obtains the silicon chip after 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
After being uniformly dispersed, the aluminium powder mixed liquor after ultrasound is obtained；
(2) silicon chip after ultrasound is put into the aluminium powder mixed liquor after ultrasound, natural air drying, obtaining deposition has thin layer of aluminum
The silicon chip of powder；The deposit 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,
For the silicon chip for having thin layer aluminium powder using depositing as growth substrates, it is at 5~6mm to be placed in vertical range directly over metal Al powder, is sunk
Product has the one side of thin layer aluminium powder upward；
5g Ga drops are placed in the aluminium oxide ceramics boat other end, Ga liquid has the silicon chip of thin layer aluminium powder close to Ga with deposition
The horizontal range at liquid end is 15mm；
It is standby after whole reaction unit is arranged as stated above；
Step 3, vacuumize, ventilate, heating
(1) reaction unit after arranging is put into the quartz test tube of one end open, wherein, the reaction dress after arranging
The axis and the diameter parallel of the quartz test tube of one end open put, and aluminium oxide ceramics boat is put into one end of Ga liquid away 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 stove, it is closed, start to take out very
It is empty；
As vacuum≤5Pa of horizontal quartz tube stove, it is passed through argon gas and gas washing is carried out to reaction system, argon gas is passed through stream
Measure as 700sccm, after 10min, it is 50sccm that regulation argon gas, which is passed through flow, and it is 50sccm to be passed through ammonia flow, 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 design temperature,
After keeping 1h, stop heating；
(3) furnace cooling, when temperature is down to 750 DEG C, ammonia flow is closed, is continually fed into argon gas, ensures argon atmosphere, with
Stove is cooled to room temperature；
(4) completely after cooling, reaction unit is taken out, the greyish white material being deposited on thin layer aluminium powder silicon substrate surface, is
AlxGa1-xN ternary alloy three-partalloy microcrystalline balls.
Embodiment 3
A kind of high Al contents AlxGa1-xN ternary alloy three-partalloy microcrystalline balls, it is AlxGa1-xN semiconducting alloys, there is wurtzite structure
AlGaN crystal.The microcrystalline balls have regular and uniform chondritic, and its average diameter is 5.0 μm.
A kind of high Al contents AlxGa1-xThe preparation method of N ternary alloy three-partalloy microcrystalline balls, comprises the following steps：
Step 1, pre-deposition thin layer aluminium powder
(1) silicon chip is ultrasonically treated with deionized water, after cleaning, obtains the silicon chip after 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
After being uniformly dispersed, the aluminium powder mixed liquor after ultrasound is obtained；
(2) silicon chip after ultrasound is put into the aluminium powder mixed liquor after ultrasound, natural air drying, obtaining deposition has thin layer of aluminum
The silicon chip of powder；The deposit 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,
For the silicon chip for having thin layer aluminium powder using depositing as growth substrates, it is at 5~6mm to be placed in vertical range directly over metal Al powder, is sunk
Product has the one side of thin layer aluminium powder upward；
5g Ga drops are placed in the aluminium oxide ceramics boat other end, Ga liquid has the silicon chip of thin layer aluminium powder close to Ga with deposition
The horizontal range at liquid end is 13mm；
It is standby after whole reaction unit is arranged as stated above；
Step 3, vacuumize, ventilate, heating
(1) reaction unit after arranging is put into the quartz test tube of one end open, wherein, the reaction dress after arranging
The axis and the diameter parallel of the quartz test tube of one end open put, and aluminium oxide ceramics boat is put into one end of Ga liquid away 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 stove, it is closed, start to take out very
It is empty；
As vacuum≤5Pa of horizontal quartz tube stove, it is passed through argon gas and gas washing is carried out to reaction system, argon gas is passed through stream
Measure as 300sccm, after 15min, it is 60sccm that regulation argon gas, which is passed through flow, and it is 60sccm to be passed through ammonia flow, 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 design temperature,
After keeping 3h, stop heating；
(3) furnace cooling, when temperature is down to 650 DEG C, ammonia flow is closed, is continually fed into argon gas, ensures argon atmosphere, with
Stove is cooled to room temperature；
(4) completely after cooling, reaction unit is taken out, the greyish white material being deposited on thin layer aluminium powder silicon substrate surface, is
AlxGa1-xN ternary alloy three-partalloy microcrystalline balls.
Claims (10)
- A kind of 1. high Al contents AlxGa1-xN ternary alloy three-partalloy microcrystalline balls, it is characterised in that high Al contents AlxGa1-xN ternary alloy three-partalloys Microcrystalline balls are different Al components wurtzite structure AlxGa1-xN ternary alloy three-partalloy crystal, Al components adjustable extent are 0.77≤x ＜ 1, The microcrystalline balls have regular and uniform chondritic, and average diameter is 5.0 μm.
- 2. high Al contents Al as claimed in claim 1xGa1-xN ternary alloy three-partalloy microcrystalline balls, it is characterised in that described Al components Adjustable mode is that can be adjusted according to the distance difference that reaction temperature has the silicon chip of thin layer aluminium powder with Ga liquid synsedimentarys Section.
- 3. the high Al contents Al described in claim 1xGa1-xThe preparation method of N ternary alloy three-partalloy microcrystalline balls, it is characterised in that including Following steps：Step 1, pre-deposition thin layer aluminium powder(1) silicon chip is ultrasonically treated, obtains the silicon chip after ultrasound；Aluminium powder is added in reagent, ultrasonic vibration is carried out and is uniformly dispersed, obtain the aluminium powder mixed liquor after ultrasound；(2) silicon chip after ultrasound is put into the aluminium powder mixed liquor after ultrasound, natural air drying, obtaining deposition has thin layer aluminium powder Silicon chip；Wherein, the deposit thickness of thin layer aluminium powder is 0.5~1.0mm；Step 2, preparation is preparedMetal Al powder is evenly laid out in reaction boat one end, the silicon chip that deposition has thin layer aluminium powder is placed in directly over metal Al powder Vertical range is at 5~6mm, and deposition has the one side of thin layer aluminium powder upward；Ga drops are placed in the reaction boat other end, Ga liquid has horizontal range of the silicon chip close to Ga liquid end of thin layer aluminium powder with deposition For 10~15mm；Wherein, in mass ratio, metal Al powder：Ga=(1~2):1；It is standby after whole reaction unit is arranged as stated above；Step 3, vacuumize, ventilate, heating(1) reaction unit after arranging is put into the quartz test tube of one end open, wherein, reaction unit after arranging The diameter parallel of axis and the quartz test tube of one end open, and react one end opening away 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 stove, it is closed, start to vacuumize；As vacuum≤5Pa of horizontal quartz tube stove, argon gas is passed through, the flow that is passed through of argon gas is 300~700sccm, argon gas After stream keeps 10~15min, it is 40~60sccm that regulation argon gas, which is passed through flow, meanwhile, ammonia is passed through, by flow-rate ratio, argon gas：Ammonia Gas=1:1, then start to heat reaction system, heating rate is 30~50 DEG C/min, when the furnace temperature of reaction system reaches To design 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, ammonia flow is closed, is continually fed into argon gas, ensures argon atmosphere, Cool to room temperature with the furnace；(4) completely after cooling, reaction unit is taken out, it is Al to be deposited on material on thin layer aluminium powder silicon substrate surfacexGa1-xN ternarys Alloy microcrystalline ball.
- 4. high Al contents Al as claimed in claim 3xGa1-xThe preparation method of N ternary alloy three-partalloy microcrystalline balls, it is characterised in that institute It is described supersound process is carried out to silicon chip to concretely comprise the following steps in the step 1 (1) stated：With deionized water or ethanol 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, it is characterised in that institute In the step 1 (1) stated, the purity of described aluminium powder is >=99.999%, and its 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, it is characterised in that institute In the step 1 (1) stated, the reagent of described aluminium powder ultrasonic vibration mixes for the one or more in ethanol, methanol, acetone or hexane Close, the addition of reagent is to be defined so that aluminium powder is 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, it is characterised in that institute In the step 1 (1) stated, the time of described 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, it is characterised in that institute In the step 2 stated, the purity of described metal Al powder is >=99.999%, and its 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, it is characterised in that institute In the step 2 stated, described reaction boat is aluminium oxide ceramics boat.
- 10. high Al contents Al as claimed in claim 3xGa1-xThe preparation method of N ternary alloy three-partalloy microcrystalline balls, it is characterised in that institute It is described as vacuum≤5Pa of horizontal quartz tube stove in the step 3 (2) stated, be passed through argon gas, be passed through the time for 10~ 15min。
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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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| Publication number | Priority date | Publication date | Assignee | Title |
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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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