CN104495766A - Preparation method of aluminium nitride one-dimensional nanostructured material - Google Patents
Preparation method of aluminium nitride one-dimensional nanostructured material Download PDFInfo
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- CN104495766A CN104495766A CN201410764375.5A CN201410764375A CN104495766A CN 104495766 A CN104495766 A CN 104495766A CN 201410764375 A CN201410764375 A CN 201410764375A CN 104495766 A CN104495766 A CN 104495766A
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Abstract
The invention discloses a preparation method of an aluminium nitride one-dimensional nanostructured material. The preparation method comprises the following steps: step 1, putting a substrate into hydride vapour phase epitaxy equipment; step 2, performing high-temperature nitriding treatment on the surface of the substrate in the hydride vapour phase epitaxy equipment; step 3, feeding a hydride source and a nitrogen source into an aluminum source region and a reaction chamber respectively and preparing an aluminium nitride nanostructured material in a columnar arrangement on the surface of the nitridined substrate; step 4, by the end of the growth of the aluminium nitride nanostructured material, closing the hydride source; step 5, closing the nitrogen source when the temperature of the reaction chamber is reduced to be lower than 550 DEG C; and step 6, taking out a sample when the temperature of the reaction chamber is reduced to room temperature.
Description
Technical field
The present invention relates to semiconductor material growing technical field, referring in particular to a kind of method preparing different unidimensional aluminium nitride nanometer structure material by controlling growth temperature, reactant source flow and growth pressure.
Background technology
Aluminium nitride (AlN) is important III-nitride semiconductor material, energy gap is 6.2eV, be the highest in group III-nitride, there is again extraordinary piezoelectric property, thermal conductivity (3.2Wcm-1K-1) and chemical stability simultaneously, the distinctive low defect of one-dimensional nano structure material, quantum size effects etc., make AlN nanostructure show the physical properties different from body structure and membrane structure.The electron affinity of the AlN material of such as one dimension Nano structure is very low, has extraordinary field emission effect; Vertical one-dimensional nano-array structure has good piezoelectric property, can be used on nano generator.
Unidimensional aluminium nitride nanometer structure material comprises numerous shape, as nano wire, nanoneedle, nanometer rod, nano-pillar, nano belt, nanotube etc.Its preparation method is chemical Vapor deposition process (CVD) mainly.But general CVD method, Al source uses Al powder or AlCl
3powder, along with the carrying out of reaction in preparation process, Al powder or AlCl
3powder reduces gradually, easily generates complicated pattern, can not generate single nanostructure, and the growth temperature of CVD method generally wants more than 1000 DEG C; HVPE method uses gaseous source, and can ensure that reactant enters reaction chamber with constant flow, prepare highdensity one-dimensional nano-array structure, fast growth, growth temperature is low, therefore has more practicality.
Summary of the invention
The object of this invention is to provide a kind of preparation method of unidimensional aluminium nitride nanometer structure material.The nano material preparation of different structure (nanoneedle, nanometer rod), different lengths is realized by controlling the processing parameters such as growth temperature, reactant source flow, growth pressure.
The preparation method of a kind of unidimensional aluminium nitride nanometer structure material provided by the invention, comprises following steps:
Step 1: get the reaction chamber that a substrate puts into hydride gas-phase epitaxy equipment;
Step 2: in hydride gas-phase epitaxy equipment, high-temperature ammonolysis process is carried out to substrate surface;
Step 3: pass in aluminium source region and reaction chamber respectively by hydride source and nitrogenous source, the substrate after nitrogenize carries out the aluminum nitride nanometer structured material preparation of columnar arrangement;
Step 4: after terminating growth, closes hydride source;
Step 5: when reaction chamber temperature drops to less than 550 DEG C, closes nitrogenous source;
Step 6: after reaction chamber temperature drops to room temperature, takes out sample.
Accompanying drawing explanation
For further illustrating content of the present invention, below in conjunction with specific embodiment and accompanying drawing, the present invention is described in detail, wherein:
Fig. 1 is the schema 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 rod prepared by the present invention;
Fig. 5 is the SEM scanned photograph of AlN nanometer rod prepared by the present invention.
Embodiment
For making the object, technical solutions and advantages of the present invention clearly understand, below in conjunction with specific embodiment, and with reference to accompanying drawing, the present invention is described in further detail.
Fig. 1 shows the schema of the preparation method of a kind of unidimensional aluminium nitride nanometer structure material that the present invention proposes.As shown in Figure 1, the method comprises:
Step 1: get the reaction chamber that a substrate puts into hydride gas-phase epitaxy (HVPE) equipment.Particularly, first use acetone ultrasonic 5 to 10 minutes, rinse for several times with deionized water (DIW), and then H
2sO
4: HNO
3boil 10 minutes in the corrosive fluid of=1: 1, with a large amount of DIW, substrate is rinsed well, subsequently by the H of substrate bubble at 200 DEG C
2sO
4: H
3pO
4corrode 20 minutes in the corrosive fluid of=3: 1, rinse for several times with DIW, dried by substrate with infrared lamp, put into HVPE equipment, described substrate can be sapphire or silicon substrate.
Step 2: in HVPE equipment, high-temperature ammonolysis process is carried out to substrate surface.Particularly, open nitrogen valve, hvpe reactor room is taken out and to make up the number time, get rid of the air in reaction chamber.Setting growth pressure, carrier gas flux, opens heating system and carrier gas, after aluminium source region and reaction chamber temperature rise to design temperature respectively, carrier gas is changed to hydrogen, toasts 10 minutes.After baking terminates, open ammonia and ammonia carrier gas valve, carrier gas is changed to nitrogen, passes into reaction chamber to underlayer nitriding 3 minutes after ammonia mixes with carrier gas.Concrete growth parameter(s) is as follows: aluminium 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: pass in aluminium source region and reaction chamber respectively by hydride source and nitrogenous source, the substrate after nitrogenize carries out the aluminum nitride nanometer structured material preparation of columnar arrangement.Particularly, described hydride source can be hydrogenchloride, described nitrogenous source can be ammonia, after underlayer nitriding terminates, keeps passing into of ammonia and ammonia carrier gas, open hydrogenchloride and hydrogenchloride carrier gas valve, first pass into aluminium source region after hydrogenchloride and carrier gas mixing, the aluminum shot in hydrogenchloride and aluminium source region reacts, and resultant of reaction enters hvpe reactor room and mixes with ammonia, at Grown unidimensional aluminium nitride nanometer structure, the purity of described aluminum shot is 5N level.Concrete growth parameter(s) is as follows: aluminium 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, the flow of hydrogenchloride is 50 to 200sccm, flow 1000 to the 2000sccm of hydrogenchloride carrier gas, flow 500 to the 1000sccm of ammonia, carrier gas flux 500 to the 1000sccm of ammonia, the carrier gas of ammonia and hydrogenchloride 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, keeps ammonia flow until temperature is reduced to less than 550 DEG C.When reaction chamber temperature drops to less than 550 DEG C degrees Celsius, close nitrogenous source.After temperature is down to room temperature, take out sample.
Above-described specific embodiment; object of the present invention, technical scheme and beneficial effect are further described; be understood that; the foregoing is only specific embodiments of the invention; be not limited to the present invention; within the spirit and principles in the present invention all, any amendment made, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (7)
1. a preparation method for unidimensional aluminium nitride nanometer structure material, comprises following steps:
Step 1: get the reaction chamber that a substrate puts into hydride gas-phase epitaxy equipment;
Step 2: in hydride gas-phase epitaxy equipment, high-temperature ammonolysis process is carried out to substrate surface;
Step 3: pass in aluminium source region and reaction chamber respectively by hydride source and nitrogenous source, the substrate after nitrogenize carries out the aluminum nitride nanometer structured material preparation of columnar arrangement;
Step 4: after terminating growth, closes hydride source;
Step 5: when reaction chamber temperature drops to less than 550 DEG C, closes nitrogenous source;
Step 6: after reaction chamber temperature drops to room temperature, takes out sample.
2. the preparation method of unidimensional aluminium nitride nanometer structure material according to claim 1, wherein, the substrate described in step 1 is sapphire or silicon substrate.
3. the preparation method of unidimensional aluminium nitride nanometer structure material according to claim 1, wherein, the nitriding treatment described in step 2, detailed process comprises:
Step 21: after reaction chamber temperature rises to preset temp, first passes into hydrogen, toasts 10 minutes;
Step 22: pass into nitrogen and krypton again to underlayer nitriding 3 minutes.
4. the preparation method of unidimensional aluminium nitride nanometer structure material according to claim 1, wherein, the hydride source described in step 3 and nitrogenous source are respectively hydrogenchloride and ammonia.
5. the preparation method of unidimensional aluminium nitride nanometer structure material according to claim 1, wherein, what the aluminium source region described in step 3 was placed is aluminum shot, and purity is 5N level.
6. the preparation method of unidimensional aluminium nitride nanometer structure material according to claim 1, wherein, the carrier gas of the hydride source described in step 3 and nitrogenous source is nitrogen or hydrogen.
7. the preparation method of unidimensional aluminium nitride nanometer structure material according to claim 1, wherein, the preparation technology parameter of the Grown aluminum nitride nanometer structured material after nitrogenize described in step 3 is:
Aluminium source region temperature 500 DEG C to 550 DEG C, growth temperature 750 DEG C to 1000 DEG C, reaction chamber 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 of nitrogenous source, carrier gas flux 500 to the 1000sccm of nitrogenous source, growth time 15 to 30 minutes.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104952986A (en) * | 2015-06-03 | 2015-09-30 | 西安交通大学 | Production method of GaN-based white LED epitaxial structure |
| CN114574961A (en) * | 2022-03-23 | 2022-06-03 | 广东省智能机器人研究院 | Zinc oxide film growth method |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103539087A (en) * | 2013-10-23 | 2014-01-29 | 北京邮电大学 | Method of preparing aluminum nitride nanowire |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103539087A (en) * | 2013-10-23 | 2014-01-29 | 北京邮电大学 | Method of preparing aluminum nitride nanowire |
Non-Patent Citations (1)
| Title |
|---|
| JIE ZHENG ET AL: "Oriented Aluminum Nitride One-Dimensional Nanostructures: Synthesis，Structure Evolution, and Electrical Properties", 《ACS NANO》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104952986A (en) * | 2015-06-03 | 2015-09-30 | 西安交通大学 | Production method of GaN-based white LED epitaxial structure |
| CN104952986B (en) * | 2015-06-03 | 2017-12-08 | 西安交通大学 | A kind of preparation method of GaN base white light LEDs epitaxial structure |
| CN114574961A (en) * | 2022-03-23 | 2022-06-03 | 广东省智能机器人研究院 | Zinc oxide film growth method |
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