CN101104509A - Method for preparing single nano material in pore space structure - Google Patents
Method for preparing single nano material in pore space structure Download PDFInfo
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- CN101104509A CN101104509A CNA2007100297836A CN200710029783A CN101104509A CN 101104509 A CN101104509 A CN 101104509A CN A2007100297836 A CNA2007100297836 A CN A2007100297836A CN 200710029783 A CN200710029783 A CN 200710029783A CN 101104509 A CN101104509 A CN 101104509A
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- 238000001259 photo etching Methods 0.000 claims description 4
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- 229910045601 alloy Inorganic materials 0.000 claims description 2
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- 239000010941 cobalt Substances 0.000 claims description 2
- 229910017052 cobalt Inorganic materials 0.000 claims description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 239000010949 copper Substances 0.000 claims description 2
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- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 2
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- 150000002739 metals Chemical class 0.000 abstract 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 9
- 239000007789 gas Substances 0.000 description 8
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- 229910021393 carbon nanotube Inorganic materials 0.000 description 7
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- MVFCKEFYUDZOCX-UHFFFAOYSA-N iron(2+);dinitrate Chemical compound [Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MVFCKEFYUDZOCX-UHFFFAOYSA-N 0.000 description 5
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- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 4
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 4
- 238000004026 adhesive bonding Methods 0.000 description 3
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- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
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- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
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- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 description 2
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Abstract
The present invention relates to the preparation field of nanometer materials, disclosing a method for producing a single piece of nanometer material in a hole-shaped structure. First, a tiny hole is etched on a substrate, then metals or oxide films are positionally deposited on the bottom of the tiny hole, so that a single nanometer particle is formed in high-temperature annealing; or a single piece of one-dimensional nanometer material can be vegetated under the effects of metals or oxide films (such as catalytic action) through gas phase or liquid phase. The method has the advantages of simple technology and controllable location, which can realize the orientation growth of a single piece of nanometer material through controlling the position of the hole. The invention enables large-scale array type preparation with high efficiency.
Description
Technical field
The present invention relates to the preparation field of nano material, relate in particular to a kind of preparation method of single nano material.
Background technology
Single nano material, such as single nanotube, single nano-wire, single nanometer rods and single nano particle etc., owing to have unique quantum size effect, the ballistic transport effect, and superior photoelectric properties, therefore, they are at the high-performance nano opto-electronic device in future, for example: fields such as the flat-panel monitor of light emitting diode, super-resolution, high sensor have potential application prospect.In order to promote the device exploitation based on single nano material, a problem that at first will solve is to realize the location preparation of single nano material and array thereof.The method that the location prepares single nano material mainly comprises the direct growth method, little sharp welding and solution dispersion method etc.Wherein the direct growth method is a kind of technical method that generally adopts at present, and most researchers adopts beamwriter lithography to carry out the location preparation of nanocatalyst, realizes the growth of single nano material and array thereof then.But the electron beam exposure process system is very expensive, and the technology cost is higher.Therefore, develop a kind of simply and method in common prepares single nano material, have great significance receiving the application of low-light electronic applications promoting it.
Summary of the invention
For addressing the above problem, the object of the present invention is to provide a kind of method of in pore space structure, making single nano material, its technology is simple, and cost is low.
The object of the present invention is achieved like this: a kind of method of making single nano material in pore space structure is characterized in that following sequential steps: (a) etch pore space structure in substrate; (b) at the hole bottom deposit metal or the sull of substrate; (c) adopt the nano material growing technology, in pore space structure, make single nano material.
Among the described step a, at first in substrate, deposit one deck masking layer, the perforate on photoresist of spin coating one deck photoresist, and employing photoetching technique then; Use etching technics to remove not masking layer in the perforate of being protected by photoresist, expose substrate surface, then remove photoresist; Base material in the masking layer perforate is carried out etching, in substrate, form pore space structure, remove the masking layer on top layer then.
Among the described step b, at first at sample superficial deposit layer of metal or sull, then at surface deposition last layer film as sacrifice layer, this thin film sacrificial layer can be a photoresist, phosphorosilicate glass (PSG) or other material; Adopt the method for etching that thin film sacrificial layer is carried out attenuate; leave thin film sacrificial layer less than 100nm thickness up to hole bottom; then remove metal or the sull of not protected, remove thin film sacrificial layer at last, obtained metal or sull in the hole bottom by thin film sacrificial layer.
Described substrate is metal, semiconductor or insulator, or the sandwich of above-mentioned two or more combination of materials formation.
The present invention is in manufacture craft, in substrate, etch earlier small hole, then metal or sull localization are deposited on the bottom of hole, under high annealing, form needed single nanoparticle, perhaps adopt vapor phase method or liquid phase method to grow single monodimension nanometer material down in the effect (for example catalytic action) of metal or sull.This method has advantages such as technology is simple, position-controllable, by the position of control hole, can realize the located growth of single nano material.But the preparation of the present invention's large tracts of land array, the efficient height.
Description of drawings
Fig. 1 is the process flow diagram at silicon hole bottom growth single-root carbon nano-tube;
Fig. 2 (a) is the SEM profile of the bottom localization deposition single nanoparticle in micropore hole;
Fig. 2 (b) is the SEM vertical view of the bottom localization deposition single nanoparticle in micropore hole;
Fig. 2 (c) is the SEM vertical view of the single-root carbon nano-tube of growing in the micropore hole;
Fig. 2 (d) is the SEM vertical view of the single-root carbon nano-tube array of growing in the micropore hole.
The specific embodiment
The present invention is a kind of method of making single nano material in pore space structure, comprises following sequential steps:
(a) etching pore space structure in the substrate: at first in substrate, deposit one deck masking layer, the perforate on photoresist of spin coating one deck photoresist, and employing photoetching technique then; Use etching technics to remove not masking layer in the perforate of being protected by photoresist, expose substrate surface, then remove photoresist; Base material in the masking layer perforate is carried out etching, in substrate, form pore space structure, remove the masking layer on top layer then.Substrate can be selected metal, semiconductor or insulator as required for use, or the sandwich of above-mentioned two or more combination of materials formation.Etching using plasma etching or chemical solution etching.
(b) at the hole bottom deposit metal or the sull of substrate: at first at sample superficial deposit layer of metal or sull, then at surperficial spin coating last layer photoetching glue victim layer; Adopt the method for etching that photoresist is carried out attenuate, leave photoresist up to the hole bottom, then remove metal or the sull of not protected, remove photoresist at last, obtained metal or sull in the hole bottom by photoresist less than 100nm thickness.Preferable, metal or sull are iron, cobalt, nickel, gold, copper, aluminium or zinc metal, or the oxide of above-mentioned metal, or the alloy firm of above-mentioned metal.The photoresist attenuate preferably adopts oxygen gas plasma reactive ion etching technology, by the thickness of etching parameters control photoresist.
(c) adopt the nano material growing technology, for example under high annealing, form single nanoparticle, perhaps adopt vapor phase method or liquid phase method, in pore space structure, make nano materials such as single nano-wire, single nanometer rods or single nano particle.
Below in conjunction with accompanying drawing, be that embodiment comes the present invention is done further detailed description with the single-root carbon nano-tube of growing in silicon hole bottom.
1. adopt＜100〉monocrystalline silicon piece as base material.
2. adopt Oxford Plus 80+ chemical gas-phase deposition system, deposition one layer thickness is the silica (SiO of 0.4 μ m on silicon chip
2) film is as masking layer.The preparation condition of film is as follows: process gas: the N of 710sccm
2The SiH of O and 170sccm5%
4Gas; Underlayer temperature: 350 ℃; Microwave radio source power: 20W; Operating air pressure: 1000mT; Time: 10mins.
3. utilize Karl Suss R8 glue spreader at the even spin coating last layer of silica laminar surface RZJ390PG eurymeric photoresist, the gluing rotating speed is 3000rpm, and the time is 60 seconds.
4. gluing sample is carried out the heat baking, baking temperature is 110 ℃, and the time is 90s.
5. adopt Karl Suss MA45 optical lithography machine that sample is carried out 15 seconds uv-exposure, adopt micropore (diameter 5 μ m) domain mask plate in the exposure process as mask.Exposure mode is hard contact.
6. adopt 0.3% KOH alkalies that gluing exposed sample is developed, developing time is 25 seconds, and the back of developing forms little circular hole on the sample surfaces photoresist.
7. the sample that develops is carried out the heat baking, baking temperature is 130 ℃, and the time is 200 seconds.
8. adopt reactive ion etching machine (RIE), use CHF
3(30sccm) the gaseous plasma etching is removed the silica membrane in the little circular hole of photoresist; Etching power is 100W; Etch period is 50min; Operating air pressure is 5Pa.
9. with sample each ultrasonic 5min in acetone, ethanolic solution, remove the photoresist on top layer.
10. sample is put into the corrosive liquid (46gKOH+26gIPA+128gH of silicon
2O) in, the base material silicon in the little circular hole of silica is carried out wet etching, form hole with inverted pyramid shape.Solution temperature is 80 ℃, and etching time is 45min.
11. adopt 17% hydrofluoric acid solution wet etching to fall the silicon dioxide layer on sample top layer.Etching time is 1min, and temperature is a room temperature.
12. weighing Fe (NO
3)
39H
2O solid 1g, citric acid 2g, polyethylene glycol 2g, the ethanol that mixes adding 35ml and the deionized water of 160ml form iron nitrate solution.Sample is put into sonic oscillation 1min in the iron nitrate solution, takes out and place and carry out the high speed rotation on the Karl Suss R8 glue spreader, rotating speed is 3000rpm, and rotational time is 60 seconds, covers one deck iron nitrate solution at sample surfaces.
13. the sample of spin coating iron nitrate solution at 400 ℃ of baking 100min down, is removed moisture and organic matter in the iron nitrate solution, and ferric nitrate is decomposed into Fe
2O
3
14. adopt Karl Suss R8 glue spreader at sample surfaces spin coating RZJ390PG eurymeric photoresist, rotary speed is 3000rpm, rotational time is 60s.
15. the sample to the spin coating photoresist carries out the heat baking, baking temperature is 120 ℃, and the time is 10min.
16. adopt Oxford Plasmalab System100-ICP180 electric induction coupled plasma reactive ion etching system that photoresist is carried out uniform etching attenuate.Etching gas is the O of 50sccm
2, etching air pressure is 20mTorr, and RF radio-frequency power supply power is 60W, and ICP radio-frequency power supply power is 750W, and etch period is 5min.Behind over etching, only the lowest part at hole also leaves the thick photoresist of about 100nm.
17. utilize 18% hydrochloric acid solution corrosion Fe
2O
3Catalyst, etching time are 3min, and temperature is a room temperature, and the ferric oxide film of hole bottom is owing to the protection that is subjected to photoresist has kept.
18. with sample each ultrasonic 10min in acetone, ethanolic solution, remove the photoresist of hole bottom, the ferric oxide film of bottom revealed.
19. above-mentioned sample is placed in thermal chemical vapor deposition (CVD) system; under the protection of Ar gas, be warming up to 650 ℃; turn off Ar gas and feed the hydrogen of 200sccm, ferric oxide film is reduced processing, the ferric oxide film of hole bottom is reduced and forms single iron particle.
20. after finishing the hydrogen processing, turn off hydrogen, under the protection of Ar gas, continue to be warming up to 700 ℃, then feed the Ar of 150sccm and the C of 10sccm
2H
2Gas.Under the effect of iron particle, acetylene gas decomposites carbon atom and resets and form single carbon nano pipe array.
What Fig. 1 showed is the schematic diagram of above-mentioned technological process.To the product of above-mentioned single-root carbon nano-tube array manufacturing process different phase, adopt SEM (SEM) to analyze.What Fig. 2 a and Fig. 2 b showed is to handle single the nano particle that forms in the hole bottom behind the 30min through 650 ℃ of following hydrogen, and particle diameter is about 60nm, and this particle of energy spectrum analysis surface is the iron particle.What Fig. 2 c and Fig. 2 d showed is to utilize single iron particle to be catalyst, the single-root carbon nano-tube that adopts chemical gas-phase deposition system to grow out in the hole bottom.
Present embodiment is whole manufacturing process of the single carbon nano pipe array of preparation.It combines the technology of preparing of micro-nano process technology and nano material, can realize the localization deposition of single nano particle and the localization growth of single nanometer materials, but be a kind of method of easy large-area preparation single nano material array.The present invention is not limited to the preparation of single-root carbon nano-tube, adopts same technology at other single nano material of pore space structure the inside preparation equally within the protection domain at this patent.
Claims (9)
1. method of making single nano material in pore space structure is characterized in that following sequential steps:
(a) in substrate, etch pore space structure;
(b) locate plated metal or sull in the hole bottom of substrate;
(c) adopt the nano material growing technology, in pore space structure, make single nano material.
2. a kind of method of making single nano material in pore space structure as claimed in claim 1 is characterized in that: among the described step a, at first deposit one deck masking layer in substrate, the perforate on photoresist of spin coating one deck photoresist, and employing photoetching technique then; Use etching technics to remove not masking layer in the perforate of being protected by photoresist, expose substrate surface, then remove photoresist; Base material in the masking layer perforate is carried out etching, in substrate, form pore space structure, remove the masking layer on top layer then.
3. method of in pore space structure, making single nano material as claimed in claim 1, it is characterized in that: among the described step b, at first at sample superficial deposit layer of metal or sull, then at surface deposition last layer film as sacrifice layer, this thin film sacrificial layer can be a photoresist, phosphorosilicate glass (PSG) or other material; Adopt the method for etching that thin film sacrificial layer is carried out attenuate; leave thin film sacrificial layer less than 100nm thickness up to hole bottom; then remove metal or the sull of not protected, remove thin film sacrificial layer at last, obtained metal or sull in the hole bottom by thin film sacrificial layer.
4. as claim 1,2 or 3 described methods of making single nano material in pore space structure, it is characterized in that: described substrate is metal, semiconductor or insulator, or the sandwich of above-mentioned two or more combination of materials formation.
5. method of making single nano material in pore space structure as claimed in claim 1 or 2, it is characterized in that: described etching is plasma etching or chemical solution etching.
6. as claim 1,2 or 3 described methods of in pore space structure, making single nano material, it is characterized in that: described metal or sull are iron, cobalt, nickel, gold, copper, aluminium or zinc metal, or the oxide of above-mentioned metal, or the alloy firm of above-mentioned metal.
7. method of making single nano material in pore space structure as claimed in claim 3 is characterized in that: described thin film sacrificial layer attenuate using plasma reactive ion etching technology or chemical solution etching, and by the thickness of etching parameters control thin film sacrificial layer.
8. method of making single nano material in pore space structure as claimed in claim 1 is characterized in that: among the described step c, the nano material growing technology adopts vapor phase method or liquid phase method, perhaps forms single nanoparticle under high annealing.
9. method of making single nano material in pore space structure as claimed in claim 1 is characterized in that: among the described step c, prepare single nano-wire, single nanometer rods or single nano particle in pore space structure.
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|---|---|---|---|
| CNA2007100297836A CN101104509A (en) | 2007-08-20 | 2007-08-20 | Method for preparing single nano material in pore space structure |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007100297836A CN101104509A (en) | 2007-08-20 | 2007-08-20 | Method for preparing single nano material in pore space structure |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101823685A (en) * | 2010-04-30 | 2010-09-08 | 华中科技大学 | Bionic micro/nano structure preparing method |
| CN102789008A (en) * | 2012-09-06 | 2012-11-21 | 电子科技大学 | Manufacture method of infrared optical window with double face anti-reflection structure |
| CN102789009A (en) * | 2012-09-06 | 2012-11-21 | 电子科技大学 | Infrared optical window with double-sided anti-reflection structure |
| CN102854548A (en) * | 2012-09-26 | 2013-01-02 | 电子科技大学 | Infrared optical window and manufacturing method thereof |
| CN104401936A (en) * | 2014-12-19 | 2015-03-11 | 武汉大学 | Method for controlling growth of carbon nanotube bundle in horizontal direction of substrate |
| CN104401935A (en) * | 2014-12-19 | 2015-03-11 | 武汉大学 | Method for controlling growth of carbon nanotube bundle in horizontal direction of substrate |
| CN110155986A (en) * | 2018-02-13 | 2019-08-23 | 中国科学院金属研究所 | With single or mini-tube bundle size single-walled carbon nanotube transparent conductive film preparation |
-
2007
- 2007-08-20 CN CNA2007100297836A patent/CN101104509A/en active Pending
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101823685A (en) * | 2010-04-30 | 2010-09-08 | 华中科技大学 | Bionic micro/nano structure preparing method |
| CN102789008A (en) * | 2012-09-06 | 2012-11-21 | 电子科技大学 | Manufacture method of infrared optical window with double face anti-reflection structure |
| CN102789009A (en) * | 2012-09-06 | 2012-11-21 | 电子科技大学 | Infrared optical window with double-sided anti-reflection structure |
| CN102789008B (en) * | 2012-09-06 | 2015-03-04 | 电子科技大学 | Manufacture method of infrared optical window with double face anti-reflection structure |
| CN102854548A (en) * | 2012-09-26 | 2013-01-02 | 电子科技大学 | Infrared optical window and manufacturing method thereof |
| CN104401936A (en) * | 2014-12-19 | 2015-03-11 | 武汉大学 | Method for controlling growth of carbon nanotube bundle in horizontal direction of substrate |
| CN104401935A (en) * | 2014-12-19 | 2015-03-11 | 武汉大学 | Method for controlling growth of carbon nanotube bundle in horizontal direction of substrate |
| CN104401936B (en) * | 2014-12-19 | 2016-04-13 | 武汉大学 | A kind of method at substrate level direction controllable growth carbon nano-tube bundle |
| CN104401935B (en) * | 2014-12-19 | 2016-04-27 | 武汉大学 | A kind of method at substrate level direction controllable growth carbon nano-tube bundle |
| CN110155986A (en) * | 2018-02-13 | 2019-08-23 | 中国科学院金属研究所 | With single or mini-tube bundle size single-walled carbon nanotube transparent conductive film preparation |
| CN110155986B (en) * | 2018-02-13 | 2023-01-13 | 中国科学院金属研究所 | Preparation of single-walled carbon nanotube transparent conductive film with single or small tube bundle size |
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