CN102154627A - Method for preparing independent self-supporting transparent aluminium nitride nanocrystalline film - Google Patents
Method for preparing independent self-supporting transparent aluminium nitride nanocrystalline film Download PDFInfo
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- CN102154627A CN102154627A CN 201110023303 CN201110023303A CN102154627A CN 102154627 A CN102154627 A CN 102154627A CN 201110023303 CN201110023303 CN 201110023303 CN 201110023303 A CN201110023303 A CN 201110023303A CN 102154627 A CN102154627 A CN 102154627A
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Abstract
The invention discloses a method for preparing an independent self-supporting transparent aluminium nitride nanocrystalline film, and the method is realized through the following processes: placing a ceramic boat loaded with a certain quantity of absolute AlCl3 (with the purity of 98-99wt%) powder on a position, 6-9cm away from a tube orifice, on the upstream of the airflow direction of a horizontal tube furnace with the length of 100cm; placing a quartz tube, a ceramic sheet and the like on a position 20-25cm away from the ceramic boat so as to be used as a product collector; vacuumizing the sealed tube furnace to 2*10<-2>-10<3>Pa; heating the horizontal tube furnace to 760-900 DEG C in the presence of Ar gas; introducing 200-300sccm of NH3 for reaction for four hours; and naturally cooling to room temperature in the presence of the Ar gas to obtain the independent self-supporting transparent aluminium nitride film on the collector. The film prepared in the invention is the aluminium nitride of a wurtzite structure and is characterized of being a nano crystal array microcosmically and an independent self-supporting and transparent aluminium nitride film macrocosmically.
Description
Technical field
The invention belongs to the nanostructure growth field, is a kind of method for preparing independent self-supporting transparent aluminium nitride nano-crystal film.
Background technology
Aluminium nitride is a kind of direct band gap semiconductor material with wide forbidden band (energy gap is 6.2ev), and materials such as gan, silicon carbide are called as third generation semiconductor material.Because aluminium nitride has high thermal conductivity, high-melting-point, corrosion-resistant, less electron affinity, the band-to-band transition emission wavelength can go deep into the deep ultraviolet wave band, can be widely used in photoelectric device.
Scientific research in recent years shows that nano material can demonstrate some excellent physico-chemical properties, has important use to be worth in the industrial technology field.At present, the research of aluminum nitride nanometer structural growth has been had a lot of achievements reports, some aluminium nitride one dimension Nano structures comprise that nano wire, nano belt, nanotube, nanocone etc. are produced out.
There have been many kinds of methods to prepare the aluminum nitride nanometer structure at present as carbon nanotube template, direct current arc electric discharge, chemical Vapor deposition process, Metalorganic Chemical Vapor Deposition etc.
Carbon nanotube template: synthesized the aluminum nitride nanowire of diameter as human carbon nanotube template such as Y.J.Zhang in 2002, consulted the 3899th page of Chemistry of materials the 13rd volume less than 50nm.Human multi-walled carbon nano-tubes such as L.W.Yin were the monocrystalline aluminum nitride nanowire that template has been synthesized outer wall covering carbon-coating in 2005, consulted the 213rd page of Adv.Mater. the 17th volume.
The direct current arc electric discharge: people such as V.N.Tondare had synthesized a cube polycrystalline aluminum nitride nanometer pipe by the direct current-arc plasma reaction in 2002, consulted the 4813rd page of Appl.Phys.Lett.2002 the 80th volume.
Chemical Vapor deposition process: people such as Haber in 1997 have reported the aluminum nitride nanometer crystalline substance of Al nanocrystal and nitrogen high temperature reaction system down, consult the 5455th page of J.Am.Chem.Soc. the 119th volume.Hu Zhengxiao had been combined into multiaspect aluminum nitride nanometer pipe in 2003, consulted the 10176th page of J.Am.Chem.Soc. the 125th volume.Human chemical Vapor deposition processs such as J.Yang had synthesized the aluminum nitride nanometer array of high densification in 2006, consulted Nanotechnology the 17th volume s321 page or leaf.Human chemical Vapor deposition processs such as J.K.Jian had synthesized nano-pillar, nanometer stick array in 2010, and the variation of product pattern has been discussed, and consulted J.Alloys Compd. the 503rd volume L34 page or leaf.
Metalorganic Chemical Vapor Deposition: human Metalorganic Chemical Vapor Depositions such as V.Cimalla prepared flap aluminum nitride nanometer line structure in 2006, consulted the 1476th page of Phys.Stat.sol (b) the 243rd volume.
The above prepared aluminum nitride nanometer structure of Bao Dao several different methods, all be to be attached on certain substrate, or unordered dispersive powder, with simpler method obtain on the microcosmic by nanocrystallinely form, the transparent brilliant film of aluminum nitride nanometer of independent self-supporting yet there are no report on the macroscopic view.
The present invention adopts chemical vapor deposition method to synthesize the aluminum nitride nanometer structure, and products therefrom shows as the transparent film of independent self-supporting on macroscopical form.Independent transparent aluminium nitride film prepared among the present invention all has structure preferably at microcosmic and macroscopic view, makes it that great potential using value be arranged in the photoelectric device field.
Summary of the invention
The object of the present invention is to provide a kind of method for preparing independent self-supporting transparent aluminium nitride nano-crystal film.
The present invention realizes by following technology:
In a boiler tube length is in the horizontal pipe furnace of 100cm, and a certain amount of (purity is mass percent 99%) anhydrous AlCl will be housed
3The ceramic boat of powder is placed into the upstream of horizontal pipe furnace apart from mouth of pipe 6cm-9cm place, placing substrate from ceramic boat 20cm-25cm place, be evacuated down to a certain degree behind the sealing horizontal pipe furnace, in the Ar atmosphere, be raised to 760 ℃-900 ℃ then, feed the NH of 200sccm-300sccm
3Reacted four hours, and under the Ar gas shiled, naturally cooled to room temperature at last, on substrate, obtain the transparent aluminium nitride film of independent self-supporting.
Gained aluminium nitride film surface topography is a nano particle, shows as the transparent aluminium nitride film of independent self-supporting on the macroscopic view, and overall dimension is about 2cm * 2cm.
The prepared independent self-supporting transparent aluminium nitride film of the present invention is the aluminium nitride of wurtzite structure, and its X-ray diffraction (XRD) is schemed as shown in Figure 1, its scanning electron microscope diagram such as Fig. 2, and shown in 3, its optical photograph in kind is as shown in Figure 4.The aluminium nitride film light transmission rate height that gained independence self-supporting of the present invention is transparent possesses nanocrystalline and feature film simultaneously, and potential industrial technology using value is arranged.Used growth method is simple, cost is low, is fit to promote scale operation.
Description of drawings
Fig. 1 is the XRD figure of embodiment 1 gained sample, and ★ represents the diffraction peak of aluminium nitride.
Fig. 2 is the scanning electron microscope picture of embodiment 1 gained sample.
Fig. 3 is the scanning electron microscope picture of embodiment 1 gained sample.
Fig. 4 is the picture in kind of embodiment 1 gained sample, and the arrow indication is the transparent aluminium nitride film of independent self-supporting, is common Signing refill under film.
Embodiment
Embodiment 1
A certain amount of anhydrous AlCl will be housed
3The ceramic boat of (purity is mass percent 99%) powder is placed into the free mouth of pipe 6cm place of going up of horizontal pipe furnace, is placing ceramic plate and the quartz plate collection substrate as product from ceramic boat 25cm place, and airtight horizontal pipe furnace is evacuated down to 2 * 10 then
-2Pa, heating tube furnace to 850 ℃ stops to feed Ar in the Ar atmosphere, feeds the NH of 200sccm
3Solid/liquid/gas reactions 4 hours naturally cools to room temperature at last under the Ar atmosphere, obtain breaking away from transparent film product substrate, independent self-supporting on the collection substrate.The XRD figure analytical results of products therefrom shows that it is the wurtzite structure aluminium nitride along (002) direction preferential growth, as shown in Figure 1.Its Scanning Electron Microscope photos reveal products therefrom microtexture is a nano crystal array, as Fig. 2, shown in 3.The optical photograph in kind of gained sample shows that product is a film independent, self-supporting, and has the good transparency as shown in Figure 4.
Embodiment 2
A certain amount of anhydrous AlCl will be housed
3The ceramic boat of (purity is mass percent 99%) powder is placed into free mouth of pipe 6cm place on the horizontal pipe furnace, (diameter is 2cm to a plurality of little silica tubes of the parallel placement in ceramic boat 20cm place dissociating down, be about 10cm) as product collector, airtight tubular type stove evacuation to 2 * 10
-2Pa, heating tube furnace to 900 ℃ stops to feed Ar in the Ar atmosphere, feeds the NH of 250sccm
3Gas reacted 4 hours, naturally cooled to room temperature at last under the Ar atmosphere, obtained the transparent aluminium nitride film of a large amount of independent self-supportings in downstream silica tube.
Embodiment 3
A certain amount of anhydrous AlCl will be housed
3The ceramic boat of (purity is mass percent 99%) powder is placed into the free mouth of pipe 6cm place of going up of horizontal pipe furnace, is placing graphite paper from ceramic boat 25cm place as product collector, and airtight horizontal pipe furnace is evacuated down to 2 * 10 then
-2Pa, heating tube furnace to 850 ℃ in the Ar atmosphere feeds the NH of 200sccm
3Gas also is adjusted into 50sccm with the Ar flow, reacts 4 hours, naturally cools to room temperature at last under the Ar atmosphere, collects the transparent aluminium nitride film of a large amount of self-supportings on graphite paper.
Embodiment 4
A certain amount of anhydrous AlCl will be housed
3The ceramic boat of (purity is mass percent 98%) powder is placed into free mouth of pipe 6cm place on the horizontal pipe furnace, is placing a short silica tube (diameter is that 2cm is about 10cm), airtight tubular type stove evacuation to 9 * 10 from ceramic boat 25cm place
-3Pa, heating tube furnace to 800 ℃ stops to feed Ar in the Ar atmosphere, feeds the NH of 300sccm
3Gas continues to be heated to 900 ℃ and keeps NH
3Flow is constant, reacts 4 hours down at 900 ℃, naturally cools to room temperature at last under the Ar atmosphere, obtains the transparent aluminium nitride film of independent self-supporting in silica tube.
Embodiment 5
A certain amount of anhydrous AlCl will be housed
3The ceramic boat of (purity is mass percent 99%) powder is placed into free mouth of pipe 9cm place on the horizontal pipe furnace, is placing a ceramic boat from ceramic boat 20cm place as product collector, airtight tubular type stove evacuation to 2 * 10
-2Pa, heating tube furnace to 900 ℃ stops to feed Ar in the Ar atmosphere, feeds the NH of 200sccm
3Gas reacted 4 hours, naturally cooled to room temperature at last under the Ar atmosphere, obtained the transparent AlN film of independent self-supporting in ceramic boat.
Embodiment 6
A certain amount of anhydrous AlCl will be housed
3The ceramic boat of (purity is mass percent 98%) powder is placed into the free mouth of pipe 7cm place of going up of horizontal pipe furnace, (diameter is 2cm place a ceramic boat and a short silica tube from ceramic boat 25cm place, be about 10cm) as product collector, airtight horizontal pipe furnace is evacuated down to 2 * 10 then
-2Pa, heating tube furnace to 760 ℃ stops to feed Ar in the Ar atmosphere, feeds the NH of 200sccm
3Gas continues to be heated to 850 ℃ of reactions 4 hours, naturally cools to room temperature at last under the Ar atmosphere, obtains the transparent film of independent self-supporting in ceramic boat and silica tube.
Embodiment 7
A certain amount of anhydrous AlCl will be housed
3The ceramic boat of (purity is mass percent 98%) powder is placed into the free mouth of pipe 6cm place of going up of horizontal pipe furnace, is placing ceramic plate from ceramic boat 30cm place as product collector, and airtight horizontal pipe furnace is evacuated down to 9 * 10 then
-3Pa, heating tube furnace to 800 ℃ stops to feed Ar in the Ar atmosphere, feeds the NH of 300sccm
3Gas continues to be heated to 900 ℃ of reactions 4 hours, naturally cools to room temperature at last under the Ar atmosphere, obtains breaking away from transparent aluminium nitride film substrate, independent self-supporting on ceramic plate.
Claims (6)
1. method for preparing independent self-supporting transparent aluminium nitride nano-crystal film, it is characterized in that prepared product surface topography is nanometer rod or nano-grain array, be the brilliant film of the transparent aluminum nitride nanometer of independent self-supporting on the macroscopic view, and realize: a certain amount of anhydrous AlCl will be housed by following approach
3The ceramic boat of (purity is mass percent 98%-99%) powder is placed into certain position in the horizontal pipe furnace, place the product collection substrate from ceramic boat a distance, is evacuated down to 2 * 10 behind the sealing horizontal pipe furnace
-2-10
-3Handkerchief feeds Ar gas then and in the Ar atmosphere horizontal pipe furnace is warmed up to preset temp, stops to feed Ar, feeds the NH of predetermined amount of flow
3Gas reacted four hours, naturally cooled to room temperature under the last Ar gas shiled, can collect the transparent aluminium nitride film of independent self-supporting on substrate.
2. according to claim 1, it is characterized in that product synthesizes in horizontal pipe furnace and carries out, the raw material that uses is AlCl
3Powder.
3. according to claim 1, it is characterized in that used product collection substrate can be ceramic boat, silica tube, graphite paper, ceramic plate, quartz plate.
4. according to claim 1, it is characterized in that the horizontal pipe furnace preset temp is between 760 ℃-900 ℃.
5. according to claim 1, it is characterized in that predetermined NH
3The flow of gas is 200sccm-300sccm.
6. according to claim 1, it is characterized in that, at distance dress AlCl
3The ceramic boat 20cm-25cm place of powder obtains the brilliant film of the transparent aluminum nitride nanometer of independent self-supporting.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103204537A (en) * | 2013-02-06 | 2013-07-17 | 内蒙古大学 | Preparation method for nano-material with wurtzite structure |
| CN106517113A (en) * | 2016-12-27 | 2017-03-22 | 哈尔滨理工大学 | Preparation method of AlN |
| CN109627012A (en) * | 2018-12-17 | 2019-04-16 | 福州大学 | A kind of preparation method of self-supporting graphite phase carbon nitride film |
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| US20040137732A1 (en) * | 2000-07-07 | 2004-07-15 | Eric Frayssinet | Process for producing an epitaxial layer of gallium nitride |
| CN101060102A (en) * | 2006-04-21 | 2007-10-24 | 日立电线株式会社 | Nitride semiconductor substrate, method of making the same and epitaxial substrate for nitride semiconductor light emitting device |
| CN101205627A (en) * | 2006-12-21 | 2008-06-25 | 中国科学院半导体研究所 | Hydride gas-phase epitaxy apparatus for preparing nitride monocrystalline substrate |
| CN101281863A (en) * | 2008-01-11 | 2008-10-08 | 南京大学 | Method for preparing large scale nonpolar surface GaN self-supporting substrate |
| CN101580224A (en) * | 2009-06-01 | 2009-11-18 | 南京大学 | Patterning preparation method for nano array |
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2011
- 2011-01-21 CN CN 201110023303 patent/CN102154627A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040137732A1 (en) * | 2000-07-07 | 2004-07-15 | Eric Frayssinet | Process for producing an epitaxial layer of gallium nitride |
| CN101060102A (en) * | 2006-04-21 | 2007-10-24 | 日立电线株式会社 | Nitride semiconductor substrate, method of making the same and epitaxial substrate for nitride semiconductor light emitting device |
| CN101205627A (en) * | 2006-12-21 | 2008-06-25 | 中国科学院半导体研究所 | Hydride gas-phase epitaxy apparatus for preparing nitride monocrystalline substrate |
| CN101281863A (en) * | 2008-01-11 | 2008-10-08 | 南京大学 | Method for preparing large scale nonpolar surface GaN self-supporting substrate |
| CN101580224A (en) * | 2009-06-01 | 2009-11-18 | 南京大学 | Patterning preparation method for nano array |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103204537A (en) * | 2013-02-06 | 2013-07-17 | 内蒙古大学 | Preparation method for nano-material with wurtzite structure |
| CN106517113A (en) * | 2016-12-27 | 2017-03-22 | 哈尔滨理工大学 | Preparation method of AlN |
| CN109627012A (en) * | 2018-12-17 | 2019-04-16 | 福州大学 | A kind of preparation method of self-supporting graphite phase carbon nitride film |
| CN109627012B (en) * | 2018-12-17 | 2021-06-22 | 福州大学 | Preparation method of self-supporting graphite phase carbon nitride film |
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Application publication date: 20110817 |