CN106517109A - A preparing method of gallium nitride nanorods - Google Patents
A preparing method of gallium nitride nanorods Download PDFInfo
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- CN106517109A CN106517109A CN201610916919.4A CN201610916919A CN106517109A CN 106517109 A CN106517109 A CN 106517109A CN 201610916919 A CN201610916919 A CN 201610916919A CN 106517109 A CN106517109 A CN 106517109A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/0632—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with gallium, indium or thallium
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- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
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- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
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Abstract
The invention relates to a preparing method of gallium nitride nanorods, and belongs to the field of morphology control materials. A soluble gallium salt and urea are adopted as raw materials and are subjected to a hydro-thermal reaction under argon protection, and a reaction product is then reacted with NH3 at 900-1100 DEG C. The morphology of gallium oxide hydroxide is regulated through a hydrothermal method and nitridation is further performed to prepare the gallium nitride nanorods with uniform morphology, thus overcoming a problem that gallium nitride morphology in traditional processes is difficult to control and requires a substrate, and the like. The preparing method has characteristics of no substrate, a low cost, a simple process and reliable quality.
Description
Technical field
The present invention relates to a kind of preparation method of GaN nanorods, belongs to morphology control field of material preparation.
Background technology
In recent years, one-dimensional nano structure because its size, shape and with excellent electricity, light, magnetic physical property, in optics,
The numerous areas such as electronics, magnetics, catalysis, biological detection, medicament transport are with a wide range of applications.Gallium nitride is a kind of straight
Tape splicing gap semiconductor material with wide forbidden band(Energy gap is 3.39eV), the material such as gallium nitride, carborundum is referred to as the third generation partly leads
Body material.Gallium nitride has that larger electron mobility, good electrical and thermal conductivity, high disruptive field intensity be high, preferable anti-spoke
The thermal conductivity of many characteristics such as penetrating property and high temperature resistant and resistance to chemical corrosion, meanwhile, its luminous efficiency is high, it is ultraviolet, purple,
There is very big application prospect in terms of blue, green luminescent device, be that manufacture blue light diode and high-power opto-electronic device are the most superior
One of material.
At present, preparing raw material price is partially expensive, and there is a certain degree of corrosion and pollution to environment and equipment, while preparing
The most pattern heterogeneity of GaN nanorods for going out, this seriously restricts its performance and is improved.In recent years, to inorganic compound nitrogen
The preparation research for changing gallium nanometer rods is increasingly important, and the growing method of GaN nanorods mainly has:Chemical vapour deposition technique, molecule
Beam epitaxy growth method, hydride vapour phase epitaxy method, the substrate of selection mostly are Si, sapphire, SiC substrate.But substrate and nitridation
Between gallium material to there is lattice mismatch, when causing epitaxial growth, the crystal defect such as dislocation is thought inside GaN crystal by backing material more
Propagate, reduce crystal mass.
Above technology is all, for synthesizing the gallium nitride nano material of different-shape, how to find a kind of simple using substrate
It is cheap at the same to pattern be easy to regulate and control without substrate fabrication method become solution GaN nanorods can be applied to nanometer electricity
The key of sub- device, and the target of the unremitting pursuit of field researcher.
The content of the invention
It is an object of the invention to provide a kind of preparation method of GaN nanorods, is characterized in regulating and controlling by hydro-thermal method
Hydroxide oxygen gallium pattern, further nitrogenizes, and is prepared for pattern with two-step method (forced hydrolysis method-two step of direct nitridation method synthesis) equal
One GaN nanorods, in can solving traditional handicraft, gallium nitride pattern is difficult to control to, the problems such as need substrate.The present invention exists
Prepare in the method for GaN nanorods without substrate, low cost, process is simple, reliable in quality.
The preparation method of the GaN nanorods that the present invention is provided is to be with solubility gallium salt and carbamide under argon protection
Raw material through hydro-thermal reaction, product again with NH3Reacted at a temperature of 900-1100 DEG C.
What the preparation method of the GaN nanorods that the present invention is provided included concretely comprises the following steps:
1)The mixed liquor of Ganite (Fujisawa). aqueous solution and aqueous solution of urea stirring reaction 8-10 hour under the conditions of 90 DEG C of waters bath with thermostatic control,
Natural cooling, stands 8-12 hours, and centrifugation goes out precipitation, respectively with ethanol and water washing three times, dries 12-16 at 80 DEG C
Hour, obtain white product.
2)Under argon protection and vacuum condition, white product is placed in the quartz boat of tube furnace, temperature programming 400-
450 DEG C, 4-6 hours are heated, room temperature is naturally cooled to;Continue temperature programming to 900-1100 DEG C, be passed through 100-300sccm's
NH3, after maintaining 2-4 hours, room temperature is cooled under argon protection, obtains faint yellow product.
Step 1)The mol ratio of described Ganite (Fujisawa). and carbamide is 1:4-6.
Step 1)Carbamide molar concentration final in described mixed liquor is 0.18M;Described pH of mixed=9-10.
Step 1)Described centrifugation is 8000-10000 r/min, centrifugation 5-10min.
Step 2)400-450 DEG C of described temperature programming be:2 DEG C/min, from room temperature, 20 DEG C start to warm up, intensification 190-
215min。
Step 2)Into 900-1100 DEG C, described temperature programming is 5 DEG C/minute, from 400-450 DEG C for described temperature programming
Start to warm up, intensification 90-140min.
Step 2)Described vacuum is -0.1Mpa.
It is raw material through hydro-thermal with solubility gallium salt and carbamide that the preparation method of the GaN nanorods that the present invention is provided is
Reaction, obtains product through accompanying burning, at high temperature through NH3Reduction.It is characterized in regulating and controlling hydroxide oxygen by hydro-thermal method
Gallium pattern, further nitrogenizes, and is prepared for the homogeneous GaN nanorods of pattern, and in can solving traditional handicraft, gallium nitride pattern is difficult
To control, the problems such as need substrate.The present invention in the method for prepare GaN nanorods without substrate, low cost, process is simple,
Reliable in quality.
Description of the drawings
Fig. 1 is schemed for high power SEM of gallium oxide nanometer rods prepared by embodiment 1.
Fig. 2 is schemed for low power SEM of gallium oxide nanometer rods prepared by embodiment 1.
Fig. 3 is schemed for high power SEM of GaN nanorods prepared by embodiment 2.
Fig. 4 is schemed for low power SEM of GaN nanorods prepared by embodiment 2.
X-ray diffractograms of the Fig. 5 for hydroxide oxygen gallium, gallium oxide and gallium nitride.
Specific embodiment
Embodiment 1
A certain amount of gallium nitrate hydrate is taken respectively(Purity is mass percent 99.99%)And carbamide(Purity is mass percent
99.999%)It is dissolved in deionized water, it is 1 to take Ganite (Fujisawa). with urea mol ratio:6 amount is placed in constant pressure funnel;Take appropriate
Deionized water is put in the there-necked flask of 500ml, and the content of deionized water needs to ensure that final carbamide molar concentration is
0.18M.Constant pressure funnel is connected with there-necked flask, and is connected with mechanical agitation.90 DEG C of water bath with thermostatic control, during water-bath
Need constantly to add water to make up evaporation of water loss in water-bath.After temperature stabilization, in vigorous mechanical agitation similarly hereinafter
When be slowly added dropwise Ganite (Fujisawa). aqueous solution and aqueous solution of urea, completely, 90 DEG C of holding 9h of water bath with thermostatic control stand 8 hours to Deca, natural
After cooling, 10min clocks are centrifuged under 8000r/min, respectively with ethanol and deionized water wash three times after, dry within 12 hours at 80 DEG C
It is dry.Obtain white product.The white product after drying is taken, is placed in the middle part of quartz boat, quartz boat is placed in into the horizontal tube of 100cm length
In the middle of formula stove, airtight tube type stove evacuation to -0.1Mpa.From 20 DEG C of beginnings of room temperature with 2 DEG C/min program liters under argon protection
Warm 215min to 450 DEG C, after maintaining 4 hours, under argon protection, naturally cool to room temperature.Sampling obtains white product, sample shape
Looks such as Fig. 1, shown in 2.
Embodiment 2
A certain amount of gallium nitrate hydrate is taken respectively(Purity is mass percent 99.99%)And carbamide(Purity is mass percent
99.999%)It is dissolved in deionized water, it is 1 to take Ganite (Fujisawa). with urea mol ratio:6 amount is placed in constant pressure funnel;Take appropriate
Deionized water is put in the there-necked flask of 500ml, and the content of deionized water needs to ensure that final carbamide molar concentration is
0.18M.Constant pressure funnel is connected with there-necked flask, and is connected with mechanical agitation.90 DEG C of water bath with thermostatic control, during water-bath
Need constantly to add water to make up evaporation of water loss in water-bath.After temperature stabilization, in vigorous mechanical agitation similarly hereinafter
When be slowly added dropwise Ganite (Fujisawa). aqueous solution and aqueous solution of urea, completely, 90 DEG C of holding 9h of water bath with thermostatic control stand 8 hours to Deca, natural
After cooling, 10min clocks are centrifuged under 8000r/min, respectively with ethanol and deionized water wash three times after, dry within 12 hours at 80 DEG C
It is dry.Obtain white product.The white product after drying is taken, is placed in the middle part of quartz boat, quartz boat is placed in into the horizontal tube of 100cm length
In the middle of formula stove, airtight tube type stove evacuation to -0.1Mpa.From 20 DEG C of beginnings of room temperature with 2 DEG C/min program liters under argon protection
Warm 215min to 450 DEG C, it is passed through from 450 DEG C of temperature programmings to 950 DEG C with 5 DEG C/min under after maintaining 4 hours, argon is protected
The NH of 200sccm3, after maintaining 2 hours, room temperature is cooled under argon protection, obtains faint yellow product, sample topography such as Fig. 3,
Shown in 4.
Embodiment 3
A certain amount of gallium nitrate hydrate is taken respectively(Purity is mass percent 99.99%)And carbamide(Purity is mass percent
99.999%)It is dissolved in deionized water, it is 1 to take Ganite (Fujisawa). with urea mol ratio:6 amount is placed in constant pressure funnel;Take appropriate
Deionized water is put in the there-necked flask of 500ml, and the content of deionized water needs to ensure that final carbamide molar concentration is
0.18M.Constant pressure funnel is connected with there-necked flask, and is connected with mechanical agitation.90 DEG C of water bath with thermostatic control, during water-bath
Need constantly to add water to make up evaporation of water loss in water-bath.After temperature stabilization, in vigorous mechanical agitation similarly hereinafter
When be slowly added dropwise Ganite (Fujisawa). aqueous solution and aqueous solution of urea, completely, 90 DEG C of holding 9h of water bath with thermostatic control stand 10h to Deca, naturally cold
But, after, 10min clocks are centrifuged under 8000r/min, respectively with ethanol and deionized water wash three times after, dry 12h at 80 DEG C.
To white product.The white product after drying is taken, is placed in the middle part of quartz boat, quartz boat is placed in into the horizontal pipe furnace of 100cm length
Centre, airtight tube type stove evacuation to -0.1Mpa.From 20 DEG C of beginnings of room temperature with 2 DEG C/min temperature programmings under argon protection
215min to 450 DEG C, it is passed through from 450 DEG C of temperature programmings to 950 DEG C with 5 DEG C/min under after maintaining 4 hours, argon is protected
The NH of 200sccm3, after maintaining 2 hours, room temperature is cooled under argon protection, obtains light yellow product.
Embodiment 4
A certain amount of gallium nitrate hydrate is taken respectively(Purity is mass percent 99.99%)And carbamide(Purity is mass percent
99.999%)It is dissolved in deionized water, it is 1 to take Ganite (Fujisawa). with urea mol ratio:6 amount is placed in constant pressure funnel;Take appropriate
Deionized water is put in the there-necked flask of 500ml, and the content of deionized water needs to ensure that final carbamide molar concentration is
0.18M.Constant pressure funnel is connected with there-necked flask, and is connected with mechanical agitation.90 DEG C of water bath with thermostatic control, during water-bath
Need constantly to add water to make up evaporation of water loss in water-bath.After temperature stabilization, in vigorous mechanical agitation similarly hereinafter
When be slowly added dropwise Ganite (Fujisawa). aqueous solution and aqueous solution of urea, completely, 90 DEG C of holding 8h of water bath with thermostatic control stand 10h to Deca, naturally cold
But, after, 10min clocks are centrifuged under 8000r/min, respectively with ethanol and deionized water wash three times after, dry 16h at 80 DEG C.
To white product.The white product after drying is taken, is placed in the middle part of quartz boat, quartz boat is placed in into the horizontal pipe furnace of 100cm length
Centre, airtight tube type stove evacuation to -0.1Mpa.From 20 DEG C of beginnings of room temperature with 2 DEG C/min temperature programmings under argon protection
215min to 450 DEG C, led to from 450 DEG C temperature programming 90min to 900 DEG C with 5 DEG C/min under after maintaining 4 hours, argon is protected
Enter the NH of 100sccm3, after maintaining 3 hours, room temperature is cooled under argon protection, obtains light yellow product.
Embodiment 5
A certain amount of gallium nitrate hydrate is taken respectively(Purity is mass percent 99.99%)And carbamide(Purity is mass percent
99.999%)It is dissolved in deionized water, it is 1 to take Ganite (Fujisawa). with urea mol ratio:5 amount is placed in constant pressure funnel;Take appropriate
Deionized water is put in the there-necked flask of 500ml, and the content of deionized water needs to ensure that final carbamide molar concentration is
0.18M.Constant pressure funnel is connected with there-necked flask, and is connected with mechanical agitation.90 DEG C of water bath with thermostatic control, during water-bath
Need constantly to add water to make up evaporation of water loss in water-bath.After temperature stabilization, in vigorous mechanical agitation similarly hereinafter
When be slowly added dropwise Ganite (Fujisawa). aqueous solution and aqueous solution of urea, completely, 90 DEG C of holding 8h of water bath with thermostatic control stand 12h to Deca, naturally cold
But, after, 10min clocks are centrifuged under 8000r/min, respectively with ethanol and deionized water wash three times after, dry 12h at 80 DEG C.
To white product.The white product after drying is taken, is placed in the middle part of quartz boat, quartz boat is placed in into the horizontal pipe furnace of 100cm length
Centre, airtight tube type stove evacuation to -0.1Mpa.From 20 DEG C of beginnings of room temperature with 2 DEG C/min temperature programmings under argon protection
215min to 450 DEG C, led to from 450 DEG C temperature programming 100min to 950 DEG C with 5 DEG C/min under after maintaining 4 hours, argon is protected
Enter the NH of 200sccm3, after maintaining 3 hours, room temperature is cooled under argon protection, obtains yellow product.
Embodiment 6
A certain amount of gallium nitrate hydrate is taken respectively(Purity is mass percent 99.99%)And carbamide(Purity is mass percent
99.999%)It is dissolved in deionized water, it is 1 to take Ganite (Fujisawa). with urea mol ratio:5 amount is placed in constant pressure funnel;Take appropriate
Deionized water is put in the there-necked flask of 500ml, and the content of deionized water needs to ensure that final carbamide molar concentration is
0.18M.Constant pressure funnel is connected with there-necked flask, and is connected with mechanical agitation.90 DEG C of water bath with thermostatic control, during water-bath
Need constantly to add water to make up evaporation of water loss in water-bath.After temperature stabilization, in vigorous mechanical agitation similarly hereinafter
When be slowly added dropwise Ganite (Fujisawa). aqueous solution and aqueous solution of urea, completely, 90 DEG C of holding 10h of water bath with thermostatic control stand 12h to Deca, natural
After cooling, 10min clocks are centrifuged under 8000r/min, respectively with ethanol and deionized water wash three times after, dry 16h at 80 DEG C.
Obtain white product.The white product after drying is taken, is placed in the middle part of quartz boat, quartz boat is placed in into the horizontal tube of 100cm length
In the middle of stove, airtight tube type stove evacuation to -0.1Mpa.From 20 DEG C of beginnings of room temperature with 2 DEG C/min temperature programmings under argon protection
215min to 450 DEG C, with 5 DEG C/min from 450 DEG C temperature programming 110min to 1000 DEG C under after maintaining 4 hours, argon is protected,
It is passed through the NH of 100sccm3, after maintaining 4 hours, room temperature is cooled under argon protection, obtains yellow product.
Embodiment 7
A certain amount of gallium nitrate hydrate is taken respectively(Purity is mass percent 99.99%)And carbamide(Purity is mass percent
99.999%)It is dissolved in deionized water, it is 1 to take Ganite (Fujisawa). with urea mol ratio:4 amount is placed in constant pressure funnel;Take appropriate
Deionized water is put in the there-necked flask of 500ml, and the content of deionized water needs to ensure that final carbamide molar concentration is
0.18M.Constant pressure funnel is connected with there-necked flask, and is connected with mechanical agitation.90 DEG C of water bath with thermostatic control, during water-bath
Need constantly to add water to make up evaporation of water loss in water-bath.After temperature stabilization, in vigorous mechanical agitation similarly hereinafter
When be slowly added dropwise Ganite (Fujisawa). aqueous solution and aqueous solution of urea, Deca completely, 90 DEG C of holding 10h of water bath with thermostatic control, stand it is one late, it is natural
After cooling, 10min clocks are centrifuged under 8000r/min, respectively with ethanol and deionized water wash three times after, overnight dry at 80 DEG C
It is dry.Obtain white product.The white product after drying is taken, is placed in the middle part of quartz boat, quartz boat is placed in into the horizontal tube of 100cm length
In the middle of formula stove, airtight tube type stove evacuation to -0.1Mpa.From 20 DEG C of beginnings of room temperature with 2 DEG C/min program liters under argon protection
Warm 215min to 450 DEG C, after maintaining 4 hours, under argon protection, 1050 are warming up to from 450 DEG C of programs 120min with 5 DEG C/min
DEG C, it is passed through the NH of 200sccm3, after maintaining 4 hours, room temperature is cooled under argon protection, obtains buff product.
Embodiment 8
A certain amount of gallium nitrate hydrate is taken respectively(Purity is mass percent 99.99%)And carbamide(Purity is mass percent
99.999%)It is dissolved in deionized water, it is 1 to take Ganite (Fujisawa). with urea mol ratio:4 amount is placed in constant pressure funnel;Take appropriate
Deionized water is put in the there-necked flask of 500ml, and the content of deionized water needs to ensure that final carbamide molar concentration is
0.18M.Constant pressure funnel is connected with there-necked flask, and is connected with mechanical agitation.90 DEG C of water bath with thermostatic control, during water-bath
Need constantly to add water to make up evaporation of water loss in water-bath.After temperature stabilization, in vigorous mechanical agitation similarly hereinafter
When be slowly added dropwise Ganite (Fujisawa). aqueous solution and aqueous solution of urea, completely, 90 DEG C of holding 10h of water bath with thermostatic control stand 10h to Deca, natural
After cooling, 10min clocks are centrifuged under 8000r/min, respectively with ethanol and deionized water wash three times after, dry 14h at 80 DEG C.
Obtain white product.The white product after drying is taken, is placed in the middle part of quartz boat, quartz boat is placed in into the horizontal tube of 100cm length
In the middle of stove, airtight tube type stove evacuation to -0.1Mpa.From 20 DEG C of beginnings of room temperature with 2 DEG C/min temperature programmings under argon protection
215min to 450 DEG C, with 5 DEG C/min from 450 DEG C temperature programming 130min to 1100 DEG C under after maintaining 4 hours, argon is protected,
It is passed through the NH of 300sccm3, after maintaining 4 hours, room temperature is cooled under argon protection, obtains brown color product.
Claims (9)
1. a kind of preparation method of GaN nanorods, it is characterised in that it is with solubility gallium salt and carbamide under argon protection
Be raw material through hydro-thermal reaction, product again with NH3Reacted at a temperature of 900-1100 DEG C.
2. a kind of preparation method of GaN nanorods, it is characterised in that what is included concretely comprises the following steps:
1)The mixed liquor of Ganite (Fujisawa). aqueous solution and aqueous solution of urea stirring reaction 8-10 hour under the conditions of 90 DEG C of waters bath with thermostatic control,
Natural cooling, stands 8-12 hours, and centrifugation goes out precipitation, respectively with ethanol and water washing three times, dries 12-16 at 80 DEG C
Hour, obtain white product;
2)Under argon protection and vacuum condition, white product is placed in the quartz boat of tube furnace, temperature programming 400-450
DEG C, 4-6 hours are heated, room temperature is naturally cooled to;Continue temperature programming to 900-1100 DEG C, be passed through the NH of 100-300sccm3,
After maintaining 2-4 hours, room temperature is cooled under argon protection, obtains faint yellow product.
3. preparation method according to claim 2, it is characterised in that step 1)The mol ratio of described Ganite (Fujisawa). and carbamide
For 1:4-6.
4. preparation method according to claim 2, it is characterised in that step 1)In described mixed liquor, final carbamide rubs
Your concentration is 0.18M;Described pH of mixed=9-10.
5. preparation method according to claim 2, it is characterised in that step 1)Described centrifugation is 8000-10000
R/min, centrifugation 5-10min.
6. preparation method according to claim 2, it is characterised in that step 2)400-450 DEG C of described temperature programming be:2
DEG C/min, from room temperature, 20 DEG C start to warm up, intensification 190-215min.
7. preparation method according to claim 2, it is characterised in that step 2)Described temperature programming is to 900-1100 DEG C
In, described temperature programming is 5 DEG C/minute, is started to warm up from 400-450 DEG C, intensification 90-140min.
8. preparation method according to claim 2, it is characterised in that step 2)Described vacuum is -0.1Mpa.
9. preparation method according to claim 2, it is characterised in that step 1)The purity of described Ganite (Fujisawa). is 99.99%;
The purity of carbamide is 99.999%.
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CN107628637A (en) * | 2017-08-14 | 2018-01-26 | 南京大学 | A kind of method for preparing III oxide and nitride nano post |
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CN107628637A (en) * | 2017-08-14 | 2018-01-26 | 南京大学 | A kind of method for preparing III oxide and nitride nano post |
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