CN1323051A - Prepn of ordered nanometer carbon pipe array on silicon chip - Google Patents
Prepn of ordered nanometer carbon pipe array on silicon chip Download PDFInfo
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- CN1323051A CN1323051A CN 01113646 CN01113646A CN1323051A CN 1323051 A CN1323051 A CN 1323051A CN 01113646 CN01113646 CN 01113646 CN 01113646 A CN01113646 A CN 01113646A CN 1323051 A CN1323051 A CN 1323051A
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Abstract
The present invention is the preparation of field emission cathode in the manufacture of plate display. The preparation includes the following processes: deposition of 5-50 micron thick aluminum film on substrate; anode oxidation to nanometer hole array of adjustable 10-100 nanometer holes; reducing the thickness of insulating alumina layer formed in the bottom and by oxidation for penetration while maintaining the completeness of the aluminium layer and electrolysis of ferrous sulfate to obtain deposited catalyst iron grains or nanometer line in the bottom of the holes; cracking of the carbon source gas and dilute gas in the nanometer holes to form nanometer carbon pipe array; and the alkali solution treatment of the nanometer carbon pipe array.
Description
The present invention is a kind of technology of preparing of field emissive cathode, belongs to the technical field that flat-panel display device is made.
Because almost the cathode ray tube (Cathode Ray Tube) with traditional is the same for the operation principle of field emission flat-panel display (Field Emission Display Panel), so it has all advantages of conventional cathode ray tube.In addition, display of field-emitting flat panel also has low-power consumption, low-voltage, slimming, panelized and characteristics such as can work under mal-condition.Field emissive cathode is the core of field emission flat-panel display, and it provides the electric current of work for field emission flat-panel display.According to the mechanism of field emissive cathode work, roughly can be divided into following two kinds dissimilar: micro tips array emission (Microtip Array) and film (ThinFilm) are launched.In the micro tips array emission,, comprise molybdenum awl array and silicon awl array according to the difference of material.The film emission is mainly with oriented diamond film.In the electronics corporation of external development field emission display, Pixtech, Futuba, Candescent, Micron, Motorola, Raytheon and FED Corp. mainly adopt micro tips array (Microtip Array) as field-transmitting cathode, and FEPET then adopts diamond thin (Diamond Thin Film) as electron emission source.
Enter the nineties later stage, the discovery of CNT (carbon nano-tube) with and Development of Preparation Technology, for the breakthrough development of field emission display device provides a good opportunity.CNT (carbon nano-tube) is a kind of important nano material, and it has a lot of particular performances, and most advanced and sophisticated field emission performance wherein provides possibility for the application of CNT (carbon nano-tube) in field emission flat-panel display.In the application of field emission display, require nanometer carbon pipe array to have bigger emission, simultaneously vacuum performance preferably should be arranged.The CNT (carbon nano-tube) field-transmitting cathode adopts the arc process preparation usually, and the CNT (carbon nano-tube) that it produced is made into water soluble colloid, is coated to then on the desirable substrate.Korea S Samsung company utilizes this method to develop 4.5 in 1999 " field emission display, Samsung had showed 9 in 2000 " display of field-emitting flat panel of triode form.Taiwan industrial research institute utilizes the screen coating technology to develop monochromatic Field Emission Display screen, and its explanation reaches 64 * 256 pixels.Japan Ise company cooperates with Mie university, has developed the higher source luminance of an emission.Realize advantages such as large tracts of land transplanting relatively simply, easily though adopt arc process to have preparation technology, adopt the uniformity of the very difficult controlling carbon nanotube of field-transmitting cathode of this method preparation, also be difficult to the height and the orientation of controlling carbon nanotube simultaneously.This will make the carbon nano-tube field emission display brightness irregularities, and the driving voltage between each pixel is inconsistent.
The purpose of this invention is to provide and a kind ofly can adapt to display of field-emitting flat panel high brightness and inhomogeneity requirement, and can compatible existing electrovacuum technology and the silicon chip of CRT manufacturing process on the preparation method of ordered nanometer carbon pipe array.
Nanometer carbon pipe array preparation method proposed by the invention comprises:
1.. deposit thickness is 5 microns aluminium films to 50 microns surface smoothings on silicon chip;
2.. with the anode oxidation method in the electrochemical reaction obtain that the aperture is adjustable in 10～100 nanometers, the hole arranges orderly nanohole array;
3.. attenuate nano-pore bottom and silicon chip because the thickness of the alumina insulating layer that oxidation forms makes its perforation, and keep the residue aluminium lamination complete, the electrolysis copperas solution obtains being deposited on the iron catalyst particle or the nano wire of hole bottom;
4.. with carbon-source gas and diluent gas cracking in nano-pore, form length, diameter is adjustable, contacts good multiple-wall carbon nanotube array with silicon chip;
5.. product is obtained nanometer carbon pipe array with the aqueous slkali processing.
Its roughness of aluminium film that deposits on silicon chip is lower than 0.2 micron.Carbon-source gas is an acetylene, and diluent gas is hydrogen, argon gas, nitrogen, and the mol ratio of carbon source and diluent gas is in 0.1～0.5 scope; Catalyst is iron, nickel, cobalt, 650～750 ℃ of reaction temperatures, and used heating rate is 20～30 ℃/min, is incubated 0.5～3 hour
Preparation method proposed by the invention has following several characteristics than other methods of carbon nano-tube on silicon chip:
1.. carbon nanometer tube array growing purity is higher, and arranges in order.All carbon nano-tube are all vertical with substrate surface, help the field emission of electronics;
2.. adopt the orientation of the carbon nano-tube that this method obtains, highly, density is even, and can be by to these Parameter Optimization, the surface field that obtains designing distributes and emission;
3.. adopt this method can obtain the equally distributed nanometer carbon pipe array of large tracts of land simultaneously, for the preparation of large scale field emission display device provides technology may;
4.. owing to be grown on the low-expansion coefficient silicon chip with the nanometer carbon pipe array of this method preparation, the encapsulation and the vacuum degree that therefore more help whole field emission display are kept;
5.. with this method growing nano carbon pipe array, can be with the microelectronic processing technology compatibility, for integrated and selector preparation technology provide convenience.
Embodiment of the present invention are as follows:
1. deposition of aluminum film on silicon chip:
A. n type silicon chip is used hydrofluoric acid dips 2 minutes, cleaning dries up;
B. deposited by electron beam evaporation aluminium film on silicon chip evaporates 20 microns of thickness, 300 ℃ of underlayer temperatures;
2. preparing the aperture with anode oxidation method is that orderly nano-pore preface is arranged in 20 nanometers (adjustable), hole
Row:
A. the electrolytic cell of the aluminium film being packed into was with alcohol immersion 30 minutes;
B. make electrolyte with the aqueous sulfuric acid of 0.3 molar concentration, graphite is made negative electrode, electrode spacing 50
Millimeter, 20 volts of response voltage, 20 ℃ of reaction temperatures, 2.5 hours reaction time;
C. after reaction finished, interrupt voltage remained on sulfuric acid solution 40 minutes with reacted silicon chip;
3. clean the back and add 0.2 mole of boric acid as electrolyte, with 18 volts with the ferrous sulfate saturated aqueous solution
2 volts of direct currents of 50 hertz of stacks connect negative pole as deposition voltage with silicon chip, deposit 5 minutes;
4. will deposit good silicon chip and carry out chemical vapour deposition (CVD), handle 1 hour with pure hydrogen at 500 ℃,
Be warming up to 700 ℃, pressure 200 holders, flow 200 ml/min, composition 9: 1
In nitrogen, the acetylene gaseous mixture, deposit after 2 hours, under pure nitrogen gas, reduce to room temperature with stove;
5. the sample that reaction is good was handled 5 hours with aqueous sodium carbonate, obtained marshalling, spacing is equal
Even, vertical silicon chip surface, top height tolerance are little, the multiple-wall carbon nanotube of diameter 20 ± 5 nanometers
Array.
Claims (4)
1. the preparation method of an ordered nanometer carbon pipe array on silicon chip is characterized in that its preparation method is as follows:
(1) deposit thickness is 5 microns to 50 microns an aluminium film on the silicon chip;
(2) with the anode oxidation method in the electrochemical reaction obtain that the aperture is adjustable in 10～100 nanometers, the hole arranges orderly nanohole array;
(3) attenuate nano-pore bottom and silicon chip because the thickness of the alumina insulating layer that oxidation forms makes its perforation, and keep the residue aluminium lamination complete, the electrolysis copperas solution obtains being deposited on the iron catalyst particle or the nano wire of hole bottom;
(4), form length, diameter is adjustable, contacts good multiple-wall carbon nanotube array with silicon chip with carbon-source gas and diluent gas cracking in nano-pore;
(5) product is handled with aqueous slkali, obtained nanometer carbon pipe array.
2. the preparation method of ordered nanometer carbon pipe array on silicon chip according to claim 1 is characterized in that its roughness of aluminium film that deposits is lower than 0.2 micron on silicon chip.
3. the preparation method of ordered nanometer carbon pipe array on silicon chip according to claim 1 and 2 is characterized in that carbon-source gas is an acetylene, and diluent gas is hydrogen or nitrogen or argon gas, and the mol ratio of carbon-source gas and diluent gas is in 0.1～0.5 scope.
4. the preparation method of ordered nanometer carbon pipe array on silicon chip according to claim 1 and 2 is characterized in that catalyst is iron or nickel or cobalt, and reaction temperature is 650～750 ℃.Used heating rate is 20～30 ℃/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 01113646 CN1323051A (en) | 2001-05-28 | 2001-05-28 | Prepn of ordered nanometer carbon pipe array on silicon chip |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 01113646 CN1323051A (en) | 2001-05-28 | 2001-05-28 | Prepn of ordered nanometer carbon pipe array on silicon chip |
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| CN1323051A true CN1323051A (en) | 2001-11-21 |
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| CN 01113646 Pending CN1323051A (en) | 2001-05-28 | 2001-05-28 | Prepn of ordered nanometer carbon pipe array on silicon chip |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1302857C (en) * | 2003-11-19 | 2007-03-07 | 佳能株式会社 | Liquid discharge apparatus and method for aligning needle-like substances |
| CN100336201C (en) * | 2002-12-23 | 2007-09-05 | 三星电子株式会社 | Method for manufacturing memory with nanometer point |
| CN100355649C (en) * | 2006-06-09 | 2007-12-19 | 清华大学 | Method of in-situ filling symbiotic iron nanometer wire on thin wall nanometer pipe |
| CN100375235C (en) * | 2005-01-18 | 2008-03-12 | 中国科学院半导体研究所 | Growth controlling method for preparation of silicon dioxide or silicon nanowire in large area |
| CN100456418C (en) * | 2003-04-21 | 2009-01-28 | 三星电子株式会社 | Method of mfg. self-collating nanotube array and nano points |
| CN100558628C (en) * | 2005-12-27 | 2009-11-11 | 北京大学 | Si base membrane nanometer pore canal and preparation method thereof |
| US7755264B2 (en) | 2004-02-26 | 2010-07-13 | Samsung Sdi Co., Ltd. | Composition for formatting an electron emission source for use in an electron emission device and an electron emission source fabricated using the same |
| CN101104513B (en) * | 2006-07-12 | 2010-09-29 | 清华大学 | Growth method for single-wall carbon nano-tube |
| CN102064102B (en) * | 2004-06-08 | 2013-10-30 | 桑迪士克公司 | Methods and devices for forming nanostructure monolayers and devices including such monolayers |
| CN105136870A (en) * | 2015-09-22 | 2015-12-09 | 电子科技大学 | Hydrogen gas sensor and production method thereof |
| CN110980692A (en) * | 2019-11-26 | 2020-04-10 | 中国科学院合肥物质科学研究院 | Conical carbon nanotube array and preparation method thereof |
-
2001
- 2001-05-28 CN CN 01113646 patent/CN1323051A/en active Pending
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100336201C (en) * | 2002-12-23 | 2007-09-05 | 三星电子株式会社 | Method for manufacturing memory with nanometer point |
| CN100456418C (en) * | 2003-04-21 | 2009-01-28 | 三星电子株式会社 | Method of mfg. self-collating nanotube array and nano points |
| CN1302857C (en) * | 2003-11-19 | 2007-03-07 | 佳能株式会社 | Liquid discharge apparatus and method for aligning needle-like substances |
| US7755264B2 (en) | 2004-02-26 | 2010-07-13 | Samsung Sdi Co., Ltd. | Composition for formatting an electron emission source for use in an electron emission device and an electron emission source fabricated using the same |
| CN102064102B (en) * | 2004-06-08 | 2013-10-30 | 桑迪士克公司 | Methods and devices for forming nanostructure monolayers and devices including such monolayers |
| CN100375235C (en) * | 2005-01-18 | 2008-03-12 | 中国科学院半导体研究所 | Growth controlling method for preparation of silicon dioxide or silicon nanowire in large area |
| CN100558628C (en) * | 2005-12-27 | 2009-11-11 | 北京大学 | Si base membrane nanometer pore canal and preparation method thereof |
| CN100355649C (en) * | 2006-06-09 | 2007-12-19 | 清华大学 | Method of in-situ filling symbiotic iron nanometer wire on thin wall nanometer pipe |
| CN101104513B (en) * | 2006-07-12 | 2010-09-29 | 清华大学 | Growth method for single-wall carbon nano-tube |
| CN105136870A (en) * | 2015-09-22 | 2015-12-09 | 电子科技大学 | Hydrogen gas sensor and production method thereof |
| CN110980692A (en) * | 2019-11-26 | 2020-04-10 | 中国科学院合肥物质科学研究院 | Conical carbon nanotube array and preparation method thereof |
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