CN101133190A - Producing a stable catalyst for nanotube growth - Google Patents
Producing a stable catalyst for nanotube growth Download PDFInfo
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- CN101133190A CN101133190A CNA200680004863XA CN200680004863A CN101133190A CN 101133190 A CN101133190 A CN 101133190A CN A200680004863X A CNA200680004863X A CN A200680004863XA CN 200680004863 A CN200680004863 A CN 200680004863A CN 101133190 A CN101133190 A CN 101133190A
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- carbon
- catalyzer
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- inculating crystal
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/127—Carbon filaments; Apparatus specially adapted for the manufacture thereof by thermal decomposition of hydrocarbon gases or vapours or other carbon-containing compounds in the form of gas or vapour, e.g. carbon monoxide, alcohols
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/127—Carbon filaments; Apparatus specially adapted for the manufacture thereof by thermal decomposition of hydrocarbon gases or vapours or other carbon-containing compounds in the form of gas or vapour, e.g. carbon monoxide, alcohols
- D01F9/1271—Alkanes or cycloalkanes
- D01F9/1272—Methane
Abstract
A process ( 40 ) is provided for preparing a catalyst ( 20 ). A catalyst ( 20 ) is formed over a substrate ( 12 ). A gas ( 24 ) comprising hydrogen and carbon is applied to the catalyst ( 20 ), wherein a carbon seeding layer ( 26 ) is formed on the catalyst ( 20 ). Carbon nanotubes ( 28 ) may then be grown from the catalyst ( 20 ) having the carbon seeding layer thereon ( 26 ).
Description
Technical field
Present invention relates in general to a kind of catalysis process that is used for carbon nano-tube, relate more particularly to the method that a kind of preparation is used for the stable and high activated catalyst of carbon nano tube growth.
Background technology
Carbon is one of most important element in the known elements, and can combine with oxygen, hydrogen and nitrogen etc.Carbon has four kinds of unique crystal structures that comprise diamond, graphite, soccerballene and carbon nanotube.Especially, carbon nanotube is meant that growth has the helical tubular structure of single wall or many walls, and generally is known as single-walled nanotube (SWNT) or many walls nanotube (MWNT) respectively.Obtain the structure of these types by the curling sheet that forms by a plurality of hexagons.By wherein each carbon atom is combined with three adjacent carbon atoms forming described, thereby form spiral element.Carbon nanotube has usually at the diameter of part nanometer to the magnitude of hundreds of nanometer.
Known carbon nanotube can be used for providing for example interior electron emission of Field Emission Display of vacuum unit.Carbon nanotube is used as the cost that electron emitter has reduced vacuum unit, comprising the cost of Field Emission Display.Replace other electron emitter (for example, the little point of Spindt) to realize the reduction of the cost of Field Emission Display with carbon nanotube, other electron emitter is compared with carbon nanotube-based electron emitter, has higher manufacturing cost usually.
If use chemical vapour deposition or other film deposition technique make at the bottom of the carbon nanotube launching base on the scene on from the catalytic surface growth, then can further reduce the manufacturing cost of the vacuum unit (for example, Field Emission Display) that uses carbon nanotube.As the nearest deposition method that prevents the electron emitter performance degradation, can carry out the growth of nanotube by other device processing technology or step (for example, wet method).
According to the diameter of shape that is rolled into and spiral element, carbon nanotube also can play conductor as metal, perhaps play semi-conductive effect.For metallic-like nanotubes, found that unidimensional carbon back structure can at room temperature essentially no resistance ground conduction current.In addition, can think that the electronics free migration passes this structure, make metallic-like nanotubes can be used as ideal interconnection body.When semiconducting nanotubes was connected to two metal electrodes, this structure can play field-effect transistor, wherein can make nanotube switch to state of insulation by conduction by apply voltage to grid.Therefore, because carbon nanotube particular structure, physics and chemical property, they are the potential members that are used for the nanoelectronic device.
The method of existing preparation nanotube comprises arc-discharge technique and laser ablation technology.Regrettably, these methods are produced the loose material with the nanotube that interweaves usually.Recently, J.Kong, A.M.Cassell and H Dai be at Chem.Phys.Lett.292, in 567 (1988) and J.Hafner, and M.Bronikowski, B.Azamian, P.Nikoleav, D.Colbert, K.Smith and R.Smalley are at Chem.Phys Lett.296, reported in 195 (1998) by thermal chemical vapor deposition (CVD) method and use Fe/Mo or the Fe nanoparticle as catalyzer, prove to have formed high-quality single Single Walled Carbon Nanotube (SWNT).The CVD method makes the alternative growth of single SWNT, and has simplified the method for preparing the SWNT based devices.Yet, can be used in the CVD method, promoting that the selection of the catalystic material that SWNT grows is restricted to the Fe/Mo nanoparticle usually.In addition, catalytic nanoparticles is obtained by wet chemical method usually, and it is consuming time and be difficult to use in and make little characteristic patternization.
The other method of making nanotube is to come depositing metallic films to form catalytic nanoparticles with ion beam sputtering.At L.Delzeit, B.Chen, A.Cassell, R.Stevens, C.Nguyen and M.Meyyappan are in Chem.Phys.Lett.348, in one piece of article in 368 (2002), describe the CVD growth of SWNT under 900 ℃ and above temperature, wherein used the Fe or the Fe/Mo bilayer film of thin bottom layer of aluminum load.Yet required high growth temperature has hindered the fusion of CNT growth with other device producing method.
As A.Thess, R.Lee, P.Nikolaev, H.Dai, P.Petit, J.Robert, C.Xu, Y.H.Lee, S.G.Kim, A.G.Rinzler, D.T.Colbert, G.E.Scuseria, D.Tomanet, J.E.Fischer and R.E.Smalley be at Science, and 273, reach D.S.Bethune in 483 (1996), C.H.Kiang, M.S.de Vries, G.Gorman, R.Savory, J.Vazquez and R.Beyers are at Nature, described in 363,605 (1993), in laser ablation and arc discharge method, Ni is used as one of catalytic material that is used to form SWNTs always.
Form the nickel catalyzator nanoparticle in any case, all formed zone of oxidation around under the environment on the catalyst nanoparticles.Traditionally, before growing nano-tube, in the reduction phase of growth cycle, remove oxide compound with hydrogen.Yet this must carry out before carbon nano-tube immediately, and depended on CNT growing technology and the processing condition that adopted, and for example hot phase article on plasma strengthens, reactive gas is formed and gas temperature, and not every oxide compound all is removed.This has caused the reduction of catalyst activity and reducing of active sites density, grows on catalyzer as expectation thereby cause having hindered carbon nanotube.Embodiment disclosed by the invention is used diamond-like carbon (DLC) layer catalyst deactivation before being included in process of growth, compares with the catalyzer of known technology, and this can increase catalyst activity and selectivity, and produces better carbon nanotube.
Correspondingly, be desirable to provide the method that a kind of preparation is used for the rugged catalyst of carbon nano tube growth.In addition, from detailed description of the Invention and appended claims subsequently, and in conjunction with the accompanying drawings with this background of the present invention, it is obvious that the feature of other expectation of the present invention and characteristic will become.
Summary of the invention
A kind of method for preparing catalyzer is provided.Above substrate, form catalyzer.Apply the gas that comprises hydrogen and carbon to catalyzer, wherein on catalyzer, form the carbon inculating crystal layer.Carbon nanotube can have on the catalyzer of carbon inculating crystal layer then from it grows.
Description of drawings
Below in conjunction with accompanying drawing the present invention is described, the key element that wherein identical numeral is identical,
Fig. 1 is the cross-sectional view of former known catalyst structure;
Fig. 2 is a cross-sectional view of just using the former known catalyst structure of gas processing according to the preferred method of the present invention;
Fig. 3 is the cross-sectional view of the preferred embodiments of the invention;
Fig. 4 is the schema that the step in one embodiment of the invention is shown; With
Fig. 5 illustrates according to the field emission performance of preferred embodiment of the invention carbon nanotubes grown and the graphic representation of the field emission performance of using the prior art carbon nanotubes grown.
Embodiment
On the following detailed description original idea of the present invention only is exemplary, and is not intended to limit the present invention or purposes of the present invention and application.In addition, be not intended to be subjected in the aforesaid background technology of the present invention and the constraint of any theory of following the present invention in describing in detail.
With reference to known before 1, one in the figure, and the method that can use with the present invention, be included in metal refining 16 on the dielectric layer 14, described dielectric layer 14 for example in ambient air in substrate 12 growth or the silicon-dioxide or the silicon nitride that form.Substrate 12 comprises silicon; Yet alternative material for example silicon, glass, pottery, metal, semiconductor material or organic materials all is that content disclosed by the invention is predicted.Substrate 12 can comprise control electronics or other circuit, and for simplicity, it is not illustrated in this embodiment.Metal 16 is molybdenums, but can comprise any metal.With being deposited upon on the metal 16 of metal 18 with supported catalyst 20 thereon.Metal 18 is an aluminium, but can be to be the interactional any solid support material of inertia with catalyzer 20.
Catalyzer 20 preferred package are nickeliferous, comprise in the material of cobalt, iron and transition metal or its oxide compound and alloy any but can comprise a lot of other.Can form catalyzer 20 by industrial known many methods.A preferable methods is to form level and smooth relatively film and provide more coarse surface or catalyzer 40 with this film of after etching.
As used herein, carbon nanotube comprises the carbon structure of any elongation.Before carbon nano-tube 28, the structure 10 that has catalyzer 20 on it can be exposed to the some time in the surrounding environment.This exposure can allow ambient contaminants by physical absorption or chemical absorption to catalyzer 20, one of them effect can be to form oxide skin 22 to be formed on catalyzer 20.When will installing 10 when being placed into the nanotube growth chamber (not shown), in the matting catalyst surface, helping out, and promote to comprise the reduction of the surface contaminant of oxidized catalyst layer to indoor importing hydrogen or hydrogen-containing gas.The matting efficient of catalyzer increases along with the rising of temperature, thereby, being used for low temperature method efficient step-down when the matting catalyzer of carbon nano-tube 28, it can cause the catalytic activity of difference, thereby causes less carbon nanotube 28.
With reference to figure 2 and according to the present invention, structure 10 is put into the chamber (not shown) and handle with gas 24.Gas 24 preferably comprises methane (CH
4), but can comprise the arbitrary combination of hydrogen and carbon.Energizing gas 24 is to form plasma body then, and it produces the free radical and the ion of carbon and hydrogen.For given condition, gas 24 can form to be contained from hydrogen-rich decolorizing carbon (base polymer) to the film that has than the fine and close more decolorizing carbon of low hydrogen content, and it is commonly referred to as diamond-like carbon (DLC) film.The treatment temp that is used for the DLC film can be in 15 ℃ to 600 ℃ scope, and can comprise the pressure range of several millitorrs (Torr) to hundreds of holders.For the present invention, gas 24 must comprise enough hydrogen so that any oxide compound that chemical reduction forms on catalyzer 22, go back the decolorizing carbon (DLC) 26 of deposition compact simultaneously or by DLC bunch that loads in the amorphous carbon layer 26 DLC matrix of forming, wherein amorphous carbon layer 26 has the thickness that is enough to complete catalyst deactivation, is generally 5nm or bigger.This DLC passivation layer 26 becomes inculating crystal layer subsequently and has improved catalytic activity significantly in the carbon nano tube growth process.
Further specify this method by the flow process Figure 40 among Fig. 4, wherein (42) form conducting stratum 16,18 above substrate 12, and (44) form catalyzer 20 on conducting stratum 16,18 then.(46) gas 24 that will comprise carbon and hydrogen is applied on the catalyzer 20 to form inculating crystal layer 26 on catalyzer 20.(48) carbon nanotube 28 can have growth on the catalyzer 20 of carbon inculating crystal layer 26 from it then.
With reference to figure 5, this diagram shows with respect to the improved emission of the present invention of known technology.Except data and curves 52 and 54, make in an identical manner and specimen, before carrying out HF-CVD, described sample has experienced the pre-deposition of DLC inculating crystal layer above catalyzer 20.During HF-CVD, with the independent hydrogen reducing step process sample relevant with curve 56 and 58 to remove any oxide compound.Results reported shows by catalyzer 20 samples 52 and the 54 field emissioies that drawn that adopt the present invention to handle among Fig. 5, and its magnitude is better than prior art catalyst sample 56 and 58." improvement " that catalyzer of the present invention produced is main owing to longer carbon nanotube, thinner carbon nanotube, higher carbon nanotube density and defective carbon nanotube still less.Because use catalyzer 20 and carbon inculating crystal layer 26, the high current density that records for catalyst sample 52 and 54 reflects higher density and more consistent carbon nano tube growth.In addition, the acutance of the I-V characteristic that is shown by curve 52 and 54 and their low threshold of emission current are the signs with carbon nano tube growth of better shape factor (longer and thinner), and this is the better activity owing to carbon inculating crystal layer 26 inactive catalyst.
Though provided at least one exemplary in the detailed description of the present invention in front, should be appreciated that very many changing form of existence.Should be appreciated that also exemplary only is embodiment, and be not intended to limit the scope of the invention by any way, practicality or structure.But, preceding detailed description can be the indication easily that those skilled in the art are provided for implementing illustrative embodiments of the invention, should be appreciated that, can do various changes to the function and the layout of key element described in the exemplary, and not deviate from the defined scope of the present invention of claims.
Claims (21)
1. method for preparing the catalyzer that is used for carbon nano tube growth, it comprises:
With the gas processing catalyst that comprises hydrogen and carbon, be included in and form the carbon inculating crystal layer on the catalyzer.
2. method as claimed in claim 1, wherein treatment step comprises and applies methane.
3. method as claimed in claim 1, wherein treatment step is included in 15 ℃ to 600 ℃ the temperature range and applies gas.
4. method as claimed in claim 1, wherein treatment step is included under about 200 ℃ temperature and applies gas.
5. method as claimed in claim 1 wherein forms step and comprises the carbon inculating crystal layer of formation thickness at least 5 nanometers.
6. method as claimed in claim 1 wherein forms step and comprises that forming thickness is the carbon inculating crystal layer of about 10 nanometers.
7. method as claimed in claim 1, wherein treatment step further comprises from catalyzer reduction and falls oxide skin.
8. method for preparing the substrate that is used for carbon nano-tube, it comprises:
In substrate, form catalyzer;
Apply the gas that comprises hydrogen and carbon to catalyzer, wherein on catalyzer, form the carbon inculating crystal layer;
Has carbon nano-tube on the catalyzer of carbon inculating crystal layer from it.
9. method as claimed in claim 8 wherein applies step and comprises and apply methane.
10. method as claimed in claim 8 wherein applies in the temperature range that step is included in 15 ℃ to 600 ℃ and applies gas.
11. method as claimed in claim 8 wherein applies step and is included under about 200 ℃ temperature and applies gas.
12. method as claimed in claim 8 wherein forms step and comprises the carbon inculating crystal layer of formation thickness at least 5 nanometers.
13. method as claimed in claim 8 wherein forms step and comprises that forming thickness is the carbon inculating crystal layer of about 10 nanometers.
14. method as claimed in claim 8, wherein treatment step further comprises from catalyzer reduction and falls oxide skin.
15. the method for a carbon nano-tube, it comprises:
Substrate is provided;
Depositing metal layers in substrate;
On metal level, form catalyzer; With
Apply the gas that comprises hydrogen and carbon, thereby on catalyzer, form the carbon inculating crystal layer.
16., wherein apply step and comprise and apply methane as the method for claim 15.
17., wherein apply in the temperature range that step is included in 15 ℃ to 600 ℃ and apply gas as the method for claim 15.
18., wherein apply step and be included under about 200 ℃ temperature and apply gas as the method for claim 15.
19., wherein form step and comprise the carbon inculating crystal layer of formation thickness at least 5 nanometers as the method for claim 15.
20. as the method for claim 15, wherein said formation carbon inculating crystal layer comprises that forming thickness is the carbon inculating crystal layer of about 10 nanometers.
21., wherein apply step and further comprise from catalyzer getting on except that the oxide compound inculating crystal layer as the method for claim 15.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US11/082,437 | 2005-03-17 | ||
| US11/082,437 US20060210467A1 (en) | 2005-03-17 | 2005-03-17 | Producing a stable catalyst for nanotube growth |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101133190A true CN101133190A (en) | 2008-02-27 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA200680004863XA Pending CN101133190A (en) | 2005-03-17 | 2006-02-17 | Producing a stable catalyst for nanotube growth |
Country Status (5)
| Country | Link |
|---|---|
| US (1) | US20060210467A1 (en) |
| EP (1) | EP1859084A2 (en) |
| JP (1) | JP2008525183A (en) |
| CN (1) | CN101133190A (en) |
| WO (1) | WO2006101637A2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107601458A (en) * | 2017-09-12 | 2018-01-19 | 刘云芳 | A kind of preparation method of single-walled carbon nanotube |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5089898B2 (en) * | 2006-03-20 | 2012-12-05 | 株式会社アルバック | Carbon nanotube growth method |
| US7678672B2 (en) * | 2007-01-16 | 2010-03-16 | Northrop Grumman Space & Mission Systems Corp. | Carbon nanotube fabrication from crystallography oriented catalyst |
| JP5293126B2 (en) * | 2008-12-01 | 2013-09-18 | 富士通株式会社 | Manufacturing method of semiconductor device |
| JP4799623B2 (en) * | 2009-01-19 | 2011-10-26 | 株式会社東芝 | Carbon nanotube growth method |
| JP5780704B2 (en) * | 2010-01-19 | 2015-09-16 | 株式会社リケン | Hydrogen-containing amorphous hard carbon coated member |
Family Cites Families (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6087765A (en) * | 1997-12-03 | 2000-07-11 | Motorola, Inc. | Electron emissive film |
| US6346189B1 (en) * | 1998-08-14 | 2002-02-12 | The Board Of Trustees Of The Leland Stanford Junior University | Carbon nanotube structures made using catalyst islands |
| US6475573B1 (en) * | 1999-05-03 | 2002-11-05 | Guardian Industries Corp. | Method of depositing DLC inclusive coating on substrate |
| US6261693B1 (en) * | 1999-05-03 | 2001-07-17 | Guardian Industries Corporation | Highly tetrahedral amorphous carbon coating on glass |
| US6548313B1 (en) * | 2002-05-31 | 2003-04-15 | Intel Corporation | Amorphous carbon insulation and carbon nanotube wires |
| US6841002B2 (en) * | 2002-11-22 | 2005-01-11 | Cdream Display Corporation | Method for forming carbon nanotubes with post-treatment step |
| CN1286716C (en) * | 2003-03-19 | 2006-11-29 | 清华大学 | Method for growing carbon nano tube |
| JP3973662B2 (en) * | 2003-03-31 | 2007-09-12 | 富士通株式会社 | Carbon nanotube manufacturing method |
-
2005
- 2005-03-17 US US11/082,437 patent/US20060210467A1/en not_active Abandoned
-
2006
- 2006-02-17 WO PCT/US2006/005838 patent/WO2006101637A2/en active Application Filing
- 2006-02-17 CN CNA200680004863XA patent/CN101133190A/en active Pending
- 2006-02-17 JP JP2007548626A patent/JP2008525183A/en not_active Withdrawn
- 2006-02-17 EP EP06735485A patent/EP1859084A2/en not_active Withdrawn
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107601458A (en) * | 2017-09-12 | 2018-01-19 | 刘云芳 | A kind of preparation method of single-walled carbon nanotube |
Also Published As
| Publication number | Publication date |
|---|---|
| WO2006101637A2 (en) | 2006-09-28 |
| EP1859084A2 (en) | 2007-11-28 |
| US20060210467A1 (en) | 2006-09-21 |
| WO2006101637A3 (en) | 2007-11-15 |
| JP2008525183A (en) | 2008-07-17 |
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Open date: 20080227 |