CN104495766B - A kind of preparation method of unidimensional aluminium nitride nanometer structure material - Google Patents
A kind of preparation method of unidimensional aluminium nitride nanometer structure material Download PDFInfo
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- CN104495766B CN104495766B CN201410764375.5A CN201410764375A CN104495766B CN 104495766 B CN104495766 B CN 104495766B CN 201410764375 A CN201410764375 A CN 201410764375A CN 104495766 B CN104495766 B CN 104495766B
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Abstract
The invention discloses the preparation method of a kind of unidimensional aluminium nitride nanometer structure material, comprise the steps of step 1: take in the reative cell that a substrate puts into hydride gas-phase epitaxy equipment；Step 2: in hydride gas-phase epitaxy equipment, substrate surface is carried out high-temperature ammonolysis process；Step 3: each lead in aluminum source region and reative cell by hydride source and nitrogen source, prepared by the aluminum nitride nanometer structural material that the substrate after nitridation carries out columnar arrangement；Step 4: after terminating growth, closes hydride source；Step 5: when reaction chamber temperature drops to less than 550 DEG C, closes nitrogen source；Step 6: after reaction chamber temperature drops to room temperature, takes out sample.
Description
Technical field
The present invention relates to semiconductor material growing technical field, refer in particular to a kind of by controlling growth temperature
Degree, reactant source flow and growth pressure prepare the method for different unidimensional aluminium nitride nanometer structure material.
Background technology
Aluminium nitride (AlN) is important III-nitride semiconductor material, and energy gap is 6.2eV,
Group III-nitride is the highest, there is again extraordinary piezoelectric property, thermal conductivity (3.2W simultaneously
Cm-1K-1) and chemical stability, the distinctive low defect of one-dimensional nano structure material, quantum size is imitated
Should wait so that AlN nanostructured shows the physical property different from body structure and membrane structure.Example
Electron affinity energy such as the AlN material of one-dimensional nano structure is the lowest, has extraordinary Flied emission effect
Should；Vertical one-dimensional nano-array structure has good piezoelectric property, can be used in nano generator
On.
Unidimensional aluminium nitride nanometer structure material includes numerous shape, as nano wire, nanoneedle, nanometer rods,
Nano-pillar, nano belt, nanotube etc..Its preparation method is mainly chemical vapour deposition technique (CVD).
But general CVD method, Al source uses Al powder or AlCl3Powder, in preparation
During along with reaction carrying out, Al powder or AlCl3Powder gradually decreases, and easily generates complexity
Pattern, can not generate single nanostructured, and the growth temperature of CVD method is typically wanted
More than 1000 DEG C；HVPE method uses gaseous source, it is ensured that reactant enters with constant flow
Reative cell, prepares highdensity one-dimensional nano-array structure, fast growth, and growth temperature is low,
Therefore practicality is had more.
Summary of the invention
It is an object of the invention to provide the preparation method of a kind of unidimensional aluminium nitride nanometer structure material.Pass through
The technological parameters such as control growth temperature, reactant source flow, growth pressure realize different structure and (receive
Rice pin, nanometer rods), prepared by the nano material of different length.
The preparation method of a kind of unidimensional aluminium nitride nanometer structure material that the present invention provides, comprises following step
Rapid:
Step 1: take in the reative cell that a substrate puts into hydride gas-phase epitaxy equipment；
Step 2: in hydride gas-phase epitaxy equipment, substrate surface is carried out high-temperature ammonolysis process；
Step 3: hydride source and nitrogen source are each led in aluminum source region and reative cell, after nitridation
Prepared by the aluminum nitride nanometer structural material carrying out columnar arrangement on substrate；
Step 4: after terminating growth, closes hydride source；
Step 5: when reaction chamber temperature drops to less than 550 DEG C, closes nitrogen source；
Step 6: after reaction chamber temperature drops to room temperature, takes out sample.
Accompanying drawing explanation
For further illustrating present disclosure, below in conjunction with specific embodiment and accompanying drawing, the present invention is done
Detailed description, wherein:
Fig. 1 is the flow chart of AlN one-dimensional nano structure material prepared by the present invention
Fig. 2 is X-ray diffraction θ-2 θ scanning spectra of AlN nanoneedle prepared by the present invention；
Fig. 3 is the SEM scanned photograph of AlN nanoneedle prepared by the present invention；
Fig. 4 is X-ray diffraction θ-2 θ scanning spectra of AlN nanometer rods prepared by the present invention；
Fig. 5 is the SEM scanned photograph of AlN nanometer rods prepared by the present invention.
Detailed description of the invention
For making the object, technical solutions and advantages of the present invention clearer, below in conjunction with concrete real
Execute example, and referring to the drawings, the present invention is described in further detail.
Fig. 1 shows the preparation method of a kind of unidimensional aluminium nitride nanometer structure material that the present invention proposes
Flow chart.As it is shown in figure 1, the method includes:
Step 1: take in the reative cell that a substrate puts into hydride gas-phase epitaxy (HVPE) equipment.
Specifically, first use acetone ultrasonic 5 to 10 minutes, rinse for several times with deionized water (DIW), so
After H again2SO4∶HNO3The corrosive liquid of=1: 1 boils 10 minutes, with a large amount of DIW, substrate is rinsed
Totally, subsequently substrate is steeped the H at 200 DEG C2SO4∶H3PO4The corrosive liquid of=3: 1 corrodes 20 minutes,
Rinse for several times with DIW, with infrared lamp, substrate is dried, put in HVPE equipment, described substrate
Can be sapphire or silicon substrate.
Step 2: in HVPE equipment, substrate surface is carried out high-temperature ammonolysis process.Specifically, beat
Open nitrogen valve, hvpe reactor room is taken out and makes up the number time, get rid of the air in reative cell.Set growth
Pressure, carrier gas flux, open heating system and carrier gas, when aluminum source region and reaction chamber temperature rise respectively
To design temperature, carrier gas is changed to hydrogen, toasts 10 minutes.After baking terminates, open ammonia
With ammonia carrier gas valve, carrier gas is changed to nitrogen, and ammonia is passed through reative cell with carrier gas to substrate nitrogen after mixing
Change 3 minutes.Concrete growth parameter(s) is as follows: aluminum source region temperature 500 DEG C to 550 DEG C, growth pressure 100
To 760Torr, growth temperature is 750 DEG C to 1000 DEG C, flow 500 to the 1000sccm of ammonia,
Carrier gas flux 500 to the 1000sccm of ammonia, the carrier gas of ammonia is nitrogen or hydrogen.
Step 3: hydride source and nitrogen source are each led in aluminum source region and reative cell, after nitridation
Prepared by the aluminum nitride nanometer structural material carrying out columnar arrangement on substrate.Specifically, described hydride source
Can be hydrogen chloride, described nitrogen source can be ammonia, after underlayer nitriding terminates, keeps ammonia and ammonia carrier gas
Be passed through, open hydrogen chloride and hydrogen chloride carrier gas valve, after hydrogen chloride and carrier gas mixing, be first passed through aluminum source
District, the aluminum shot of hydrogen chloride and aluminum source region reacts, reaction product enter hvpe reactor room again with
Ammonia mixes, and at Grown unidimensional aluminium nitride nanometer structure, the purity of described aluminum shot is 5N level.
Concrete growth parameter(s) is as follows: aluminum source region temperature 500 DEG C to 550 DEG C, growth pressure 100 to 760Torr,
Growth temperature is 750 DEG C to 1000 DEG C, and the flow of hydrogen chloride is 50 to 200sccm, hydrogen chloride carrier gas
Flow 1000 to 2000sccm, flow 500 to the 1000sccm of ammonia, the carrier gas flux of ammonia
The carrier gas of 500 to 1000sccm, ammonia and hydrogen chloride is nitrogen, and growth time is 15 to 30 minutes.
Step 4: after growth terminates, closes hydride source, closes heating system, in the process of cooling
In, keep ammonia flow until temperature is reduced to less than 550 DEG C.When reaction chamber temperature drops to 550 DEG C
Below degree Celsius, close nitrogen source.After temperature is down to room temperature, take out sample.
Particular embodiments described above, is carried out the purpose of the present invention, technical scheme and beneficial effect
Further describe it should be understood that the foregoing is only the specific embodiment of the present invention,
Be not limited to the present invention, all within the spirit and principles in the present invention, any amendment of being made,
Equivalent, improvement etc., should be included within the scope of the present invention.
Claims (6)
1. a preparation method for unidimensional aluminium nitride nanometer structure material, comprises the steps of
Step 1: take in the reative cell that a substrate puts into hydride gas-phase epitaxy equipment；
Step 2: in hydride gas-phase epitaxy equipment, substrate surface is carried out high-temperature ammonolysis process；
Step 3: hydride source and nitrogen source are each led in aluminum source region and reative cell, after nitridation
Prepared by the aluminum nitride nanometer structural material carrying out columnar arrangement on substrate；
Step 4: after terminating growth, closes hydride source；
Step 5: when reaction chamber temperature drops to less than 550 DEG C, closes nitrogen source；
Step 6: after reaction chamber temperature drops to room temperature, takes out sample；
Wherein, the nitrogen treatment described in step 2, detailed process includes:
Step 21: after reaction chamber temperature rises to preset temperature, is first passed through hydrogen, toasts 10 minutes；
Step 22: be passed through nitrogen and ammonia again to underlayer nitriding 3 minutes.
The preparation method of unidimensional aluminium nitride nanometer structure material the most according to claim 1, wherein,
Substrate described in step 1 is sapphire or silicon substrate.
The preparation method of unidimensional aluminium nitride nanometer structure material the most according to claim 1, wherein,
Hydride source described in step 3 and nitrogen source are respectively hydrogen chloride and ammonia.
The preparation method of unidimensional aluminium nitride nanometer structure material the most according to claim 1, wherein,
Aluminum source region described in step 3 place for aluminum shot, purity is 5N level.
The preparation method of unidimensional aluminium nitride nanometer structure material the most according to claim 1, wherein,
The carrier gas in the hydride source described in step 3 and nitrogen source is nitrogen or hydrogen.
The preparation method of unidimensional aluminium nitride nanometer structure material the most according to claim 1, wherein,
The preparation technology ginseng of the Grown aluminum nitride nanometer structural material after nitridation described in step 3
Number is:
Aluminum source region temperature 500 DEG C to 550 DEG C, growth temperature 750 DEG C to 1000 DEG C, reative cell pressure
100 to 760Torr, flow 50 to the 200sccm of hydride source, hydride source carrier gas flux 1000
To 2000sccm, flow 500 to the 1000sccm in nitrogen source, the carrier gas flux 500 in nitrogen source to
1000sccm, growth time 15 to 30 minutes.
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