CN101255064B - Method for preparing quasi-one-dimensional doping AIN array by catalyst - Google Patents
Method for preparing quasi-one-dimensional doping AIN array by catalyst Download PDFInfo
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- CN101255064B CN101255064B CN2007100105183A CN200710010518A CN101255064B CN 101255064 B CN101255064 B CN 101255064B CN 2007100105183 A CN2007100105183 A CN 2007100105183A CN 200710010518 A CN200710010518 A CN 200710010518A CN 101255064 B CN101255064 B CN 101255064B
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Abstract
A catalyst 'seed' method for producing a AlN-doped quasi-one-dimensional array includes the following steps: evenly dispersing catalyst particles with diameters of 1-3um according to a concentration of 0.05-3.0 g/ml in a copolymer solution; magnetic stirring for 25-35 minutes to form a uniform suspension emulsion which is then dropped on silicon wafers; putting the air-dried silicon wafers into an annealing furnace which is injected with H2 at 400 DEG C-600 DEG C for insulation for 10-30 minutes and removing residual polymers; placing the silicon wafers with catalyst particles into a CVD furnace and injecting NH3 into the furnace at 800-1100 DEG C for insulation for 20-60 minutes; injecting SiCl4 into the furnace and a plurality of flower-shaped, Si-doped AlN nanometer arrays growing from the catalysts after reactions. The positioning growth (the array density is controllable) of quasi-one-dimensional AlN which is vertical to the substrate and the synchronous in situ doping are realized by combing the catalyst 'seed' method and a gas doping method and by regulating the nuclear-location and preferring precipitation supersaturation, so that the problem that the nanometer units are difficult in controlling, operation and assembling is effectively solved.
Description
Technical field
The present invention relates to the method that a kind of catalyzer " seed " legal system is equipped with accurate one dimension doped with Al N array.
Background technology
AlN is a kind of semiconductor material with wide forbidden band, can potential application be arranged at ultraviolet light photo device, piezoelectric device etc. after the doping.Particularly it have low electron affinity (＜0.25eV) and electron work functon; Make accurate one dimension AlN (the tip curvature radius is a nanometer scale) array add under the very low electric field; Can realize very high transmitter current; Moreover; Its HMP (2800 ℃), high thermal conductivity, calorifics, chemistry, the mechanical stability of its accurate one-dimensional array be can effectively improve, and then the field emission stability and the safety of device improved with advantages such as the matched well of Si substrate (as: thermal expansivity is close etc.), anti-oxidant, HS and rigidity.Therefore, accurate one dimension doped with Al N array is expected to become the ideal field emmision material.
Summary of the invention
The purpose of this invention is to provide the method that a kind of catalyzer " seed " legal system is equipped with accurate one dimension doped with Al N array.
A kind of catalyzer " seed " legal system is equipped with the method for accurate one dimension doped with Al N array; It is characterized in that: described catalyzer " seed " legal system is equipped with the method for accurate one dimension doped with Al N array; By concentration is 0.05-3g/ml, is that the granules of catalyst of 1-3um is dispersed in the copolymer solution with particle diameter, stirs evenly to drop in it on silicon chip after forming milk sap after 25 minutes to 35 minutes; Put into lehre Deng silicon chip under 400 ℃ of-600 ℃ of situation after air-dry, logical H
2Be incubated 10 minutes to 30 minutes to remove residual polymer; Having the Si sheet of granules of catalyst to cover kind is being equipped with on the porcelain boat of AlCl3; Put into the logical NH3 of CVD stove under 800-1100 ℃ of situation, be incubated 20 minutes to 60 minutes, meanwhile; Inject stove to SiCl4 lentamente, reaction finishes a large amount of colored shape AlN nano needle arrays in back and grows from catalyzer.
Described catalyzer is Co, Fe, one of Ni.
Described copolymer solution is P123, sodium laurylsulfonate, one of sodium lauryl sulphate.
The method of the accurate one dimension AlN of a kind of catalyzer " seed " the method located growth array of setting up; Through the size of optimizing ' seed ' and the control AlN heterogeneous nucleation position that distributes; The degree of closing of accurate one dimension AlN array be can effectively control, simultaneously, Si or Mg doping atmosphere contained through optimization; Realize aiming at effective doping treatment of one dimension AlN, and then prepare accurate one dimension doped with Al N array.Solve the shielding effect and a big electric current difficult problem of cold-cathode field emissive display.Because array is crossed and is dredged that to cause collected current very few; Cross secret meeting and produce the electric field shielding effect, reduce the electric field reinforcing effect, cut-in voltage increases.
Find that through characterizing the Si atom successfully is incorporated in the AlN nanoneedle.Growth mechanism to this structure has carried out preliminary discussion simultaneously, and its process of growth is considered to controlled and the catalytic gas-solid liquid of Co growth model.Research shows: the adulterated AlN nanoneedle of this Si has very low cut-in voltage and threshold value, and the maximum current density of acquisition surpasses 20mA/cm
2, and high like this current density can make most display of field-emitting flat panel produce enough brightness.This catalyzer seed law can grow through the way of further mask to be had Si doped with Al N and receives the matrix pattern of ` rice material, thereby the field emission that realizes the AlN nano material is used.
Advantage of the present invention:
Catalyzer ' seed ' method and gas phase doping method are combined; Through regulating and control the nucleation site and separating out degree of supersaturation etc. according to qualifications; Realize the located growth (the array degree of closing is controlled) of accurate one dimension AlN, perpendicular to the oriented growth of substrate, and realized aiming at the in-situ doped synchronously of one dimension AlN crystalline structure.Effectively solve the difficulty of nano unit at control, operation and fit on.
Description of drawings
Below in conjunction with accompanying drawing and embodiment the present invention is done further detailed explanation.
Fig. 1 is a preparation process synoptic diagram.
Embodiment
Embodiment 1
Adopt the catalyzer seed law successfully to prepare colored shape AlN nano needle arrays.0.1 gram particle directly for the Co granules of catalyst of 1-3 μ m is dispersed in the P123 multipolymer of 30ml, is evenly dropped in it on silicon chip behind the formation milk sap behind the stirring 30min.Put into lehre after air-dry at 500 ℃ of down logical H Deng silicon chip
2Insulation 20min clock is to remove residual polymer.There is the Si sheet of granules of catalyst to cover kind AlCl is being housed
3Porcelain boat on put into the logical NH of CVD stove
3At 900 ℃ of insulation 30min, meanwhile, with the SiCl of 20ml
4Inject stove lentamente with syringe.Reaction finishes a large amount of colored shape AlN nano needle arrays in back and grows from the Co catalyzer.
Embodiment 2
A kind of catalyzer " seed " legal system is equipped with the method for accurate one dimension doped with Al N array; It is characterized in that: described catalyzer " seed " legal system is equipped with the method for accurate one dimension doped with Al N array; Pressing the concentration of 0.05g/ml, is that the Fe granules of catalyst of 1-3um is dispersed in copolymer p 123 solution with particle diameter, and magnetic agitation evenly drops in it on silicon chip after forming even suspension emulsion after 25 minutes; Put into lehre Deng silicon chip under 400 ℃ of situation after air-dry, logical H
2Be incubated 10 minutes to remove residual polymer, have the Si sheet of granules of catalyst to cover kind AlCl is being housed
3Porcelain boat on, put into the logical NH of CVD stove
3Under 800 ℃ of situation, be incubated 20 minutes, adopt the pin hole syringe with SiCl simultaneously
4Inject stove lentamente, reaction finishes a large amount of adulterated AlN nano needle arrays of colored shape Si in back and grows from the Fe catalyzer.
Embodiment 3
A kind of catalyzer " seed " legal system is equipped with the method for accurate one dimension doped with Al N array; It is characterized in that: described catalyzer " seed " legal system is equipped with the method for accurate one dimension doped with Al N array; Pressing the concentration of 3.0g/ml, is that the Ni granules of catalyst of 1-3um is dispersed in the multipolymer sodium dodecyl sulfate solution with particle diameter, and magnetic agitation evenly drops in it on silicon chip after forming even suspension emulsion after 35 minutes; Put into lehre Deng silicon chip under 500 ℃ of situation after air-dry, logical H
2Be incubated 20 minutes to remove residual polymer, have the Si sheet of granules of catalyst to cover kind AlCl is being housed
3Porcelain boat on, put into the logical NH of CVD stove
3Under 1000 ℃ of situation, be incubated 40 minutes, adopt the pin hole syringe that SiCl4 is injected stove lentamente simultaneously, reaction finishes a large amount of adulterated AlN nano needle arrays of colored shape Si in back and grows from the Ni catalyzer.
Embodiment 4
A kind of catalyzer " seed " legal system is equipped with the method for accurate one dimension doped with Al N array; It is characterized in that: described catalyzer " seed " legal system is equipped with the method for accurate one dimension doped with Al N array; Pressing the concentration of 3.0g/ml, is that the Co granules of catalyst of 1-3um is dispersed in the multipolymer sodium dodecyl sulfate solution with particle diameter, and magnetic agitation evenly drops in it on silicon chip after forming even suspension emulsion after 35 minutes; Put into lehre Deng silicon chip under 500 ℃ of situation after air-dry, logical H
2Be incubated 30 minutes to remove residual polymer, have the Si sheet of granules of catalyst to cover kind AlCl is being housed
3Porcelain boat on, put into the logical NH of CVD stove
3Under 1100 ℃ of situation, be incubated 60 minutes, adopt the pin hole syringe with SiCl simultaneously
4Inject stove lentamente, reaction finishes a large amount of adulterated AlN nano needle arrays of colored shape Si in back and grows from the Co catalyzer.
Embodiment 5
A kind of catalyzer " seed " legal system is equipped with the method for accurate one dimension doped with Al N array; It is characterized in that: described catalyzer " seed " legal system is equipped with the method for accurate one dimension doped with Al N array; Pressing the concentration of 3.0g/ml, is that the Fe granules of catalyst of 1-3um is dispersed in the multipolymer sodium dodecyl sulfate solution with particle diameter, and magnetic agitation evenly drops in it on silicon chip after forming even suspension emulsion after 35 minutes; Put into lehre Deng silicon chip under 500 ℃ of situation after air-dry, logical H
2Be incubated 30 minutes to remove residual polymer, have the Si sheet of granules of catalyst to cover kind and be equipped with on the porcelain boat of AlCl3, put into the logical NH of CVD stove
3Under 1100 ℃ of situation, be incubated 60 minutes, adopt the pin hole syringe with SiCl simultaneously
4Inject stove lentamente, reaction finishes a large amount of adulterated AlN nano needle arrays of colored shape Si in back and grows from the Fe catalyzer.
Embodiment 6
A kind of catalyzer " seed " legal system is equipped with the method for accurate one dimension doped with Al N array; It is characterized in that: described catalyzer " seed " legal system is equipped with the method for accurate one dimension doped with Al N array; Pressing the concentration of 2.0g/ml, is that the Ni granules of catalyst of 1-3um is dispersed in the multipolymer sodium dodecyl sulfate solution with particle diameter, and magnetic agitation evenly drops in it on silicon chip after forming even suspension emulsion after 35 minutes; Put into lehre Deng silicon chip under 550 ℃ of situation after air-dry, logical H
2Be incubated 25 minutes to remove residual polymer, have the Si sheet of granules of catalyst to cover kind AlCl is being housed
3Porcelain boat on, put into the logical NH of CVD stove
3Under 900 ℃ of situation, be incubated 50 minutes, adopt the pin hole syringe with SiCl simultaneously
4Inject stove lentamente, reaction finishes a large amount of adulterated AlN nano needle arrays of colored shape Si in back and grows from the Ni catalyzer.
Claims (1)
1. a catalyzer " seed " legal system is equipped with the method for accurate one dimension doped with Al N array; It is characterized in that: described catalyzer " seed " legal system is equipped with the method for accurate one dimension doped with Al N array, and the concentration of pressing 0.05-3.0g/ml is that the granules of catalyst of 1-3um is dispersed in the copolymer solution with particle diameter; Magnetic agitation evenly drops in it on silicon chip after forming even suspension emulsion after 25 minutes to 35 minutes; After silicon chip is air-dry, put into lehre under 400 ℃ of-600 ℃ of situation, logical H
2Be incubated 10-30 minute and remove residual polymer, have the Si sheet of granules of catalyst to cover kind AlCl is being housed
3Porcelain boat on, put into the logical NH of CVD stove
3Under 800-1100 ℃ of situation, be incubated 20-60 minute, adopt the pin hole syringe with SiCl simultaneously
4Inject stove lentamente, reaction finishes a large amount of adulterated AlN nano needle arrays of colored shape Si in back and grows from catalyzer; Wherein, described catalyzer is Co, Fe, one of Ni; Described copolymer solution is P123, sodium laurylsulfonate, one of sodium lauryl sulphate.
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| CN2007100105183A CN101255064B (en) | 2007-03-01 | 2007-03-01 | Method for preparing quasi-one-dimensional doping AIN array by catalyst |
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| CN2007100105183A CN101255064B (en) | 2007-03-01 | 2007-03-01 | Method for preparing quasi-one-dimensional doping AIN array by catalyst |
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| CN101255064B true CN101255064B (en) | 2012-08-22 |
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| CN106206212A (en) * | 2016-07-25 | 2016-12-07 | 六盘水师范学院 | A kind of method growing controlled AlN ordered nano array |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1184488A2 (en) * | 2000-09-01 | 2002-03-06 | Ngk Insulators, Ltd. | An apparatus for fabricating a III-V nitride film and a method for fabricating the same |
| CN1733600A (en) * | 2005-07-22 | 2006-02-15 | 西安交通大学 | Method for solid-phase double decomposition to synthesize nanometer aluminium nitride |
| CN1857994A (en) * | 2005-04-30 | 2006-11-08 | 中国科学院金属研究所 | Nano conic array material and its preparing method |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1184488A2 (en) * | 2000-09-01 | 2002-03-06 | Ngk Insulators, Ltd. | An apparatus for fabricating a III-V nitride film and a method for fabricating the same |
| CN1857994A (en) * | 2005-04-30 | 2006-11-08 | 中国科学院金属研究所 | Nano conic array material and its preparing method |
| CN1733600A (en) * | 2005-07-22 | 2006-02-15 | 西安交通大学 | Method for solid-phase double decomposition to synthesize nanometer aluminium nitride |
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