CN100482582C - Carbon nano-tube preparation method and apparatus - Google Patents
Carbon nano-tube preparation method and apparatus Download PDFInfo
- Publication number
- CN100482582C CN100482582C CNB2005100364390A CN200510036439A CN100482582C CN 100482582 C CN100482582 C CN 100482582C CN B2005100364390 A CNB2005100364390 A CN B2005100364390A CN 200510036439 A CN200510036439 A CN 200510036439A CN 100482582 C CN100482582 C CN 100482582C
- Authority
- CN
- China
- Prior art keywords
- granules
- catalyst
- carbon nanotube
- tube
- electrode
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Images
Abstract
This invention relates to a preparation method for carbon nanotube. Said method comprises providing a substrate having a surface, forming a catalyst particles array, a electrode opposite to the array and a groove on the surface of the substrate, wherein the array and the electrode are on both sides of the position opposite to the groove, inputting current to the electrode and forming magnetic field, growing carbon nanotubes on the catalyst particles array along the direction to the electrode. This invention also provide a device for carbon nanotube preparation. Carbon nanotubes with uniform length can be prepared by the method and the device.
Description
[technical field]
The present invention relates to a kind of preparation method of carbon nano-tube and device.
[background technology]
Carbon nanotube is a kind of new carbon, is found in 1991 by Japanology personnel Iijima, sees also ＂ Helical microtubules of graphitic carbon ＂, S Iijima, Nature, vol.354, p56 (1991).Carbon nanotube has extremely excellent conductivity, and it has almost, and long-pending (tip end surface is long-pending littler near the tip end surface of theoretical limit, its internal field more concentrates), so carbon nanotube is one of known best field emmision material, it has extremely low field emission voltage, can transmit great current density, and the electric current stabilizer pole, thereby be fit to very much do the field emmision material of Field Emission Display.
At present, the carbon nanotube that Field Emission Display is commonly used is earlier by behind the preliminary synthesizing carbon nanotubes of arc discharge method, passes through purifying, grinding again, is applied on the conductive glass at last.
But the length of carbon nanotube that this kind method makes differs, thereby causes the characteristic of emitting electrons of carbon nanotube inconsistent.If this carbon nanotube is applied to Field Emission Display, may cause the brightness uniformity of this Field Emission Display not good.
In view of this, be necessary to provide a kind of preparation method of carbon nano-tube and device, it can reach the purpose of obtaining length homogeneous carbon nanotube.
[summary of the invention]
To a kind of preparation method of carbon nano-tube and device be described with specific embodiment below, its realization has the preparation of the carbon nanotube of homogeneous length.
For realizing foregoing, a kind of preparation method of carbon nano-tube is provided, it may further comprise the steps:
One substrate is provided, and it has a surface;
On this substrate surface, form a granules of catalyst array;
The relative position of this granules of catalyst array on this substrate surface forms an electrode;
Form a groove on this substrate surface, this granules of catalyst array lays respectively at the relative both sides of this groove with electrode;
On this electrode, feed electric current with generation magnetic field, carbon nano-tube on this granules of catalyst array, this carbon nanotube will be grown up to electrode direction.
Preferably, this preparation method of carbon nano-tube also further comprises this carbon nanotube of equidistant cutting, obtaining the carbon nanotube fragment of length homogeneous, and then improves the utilising efficiency of carbon nanotube.
Preferred, the cutting of described carbon nanotube can be passed through direct electronic beam writing technology, the focused ion beam direct writing technology, or laser direct-writing technology etc. is finished.
Preferably, the granules of catalyst in the described granules of catalyst array linearly shape arrange.
Preferably, the formation method of described granules of catalyst array may further comprise the steps: form a catalyst nano line in this substrate; This catalyst nano line is heated to 300 ℃～600 ℃, and annealing makes this catalyst nano line be transformed into the granules of catalyst array.
Preferred, the live width of described catalyst nano line is 10nm～1 μ m.
The formation method of described groove comprises method for plasma etching and reactive ion etching method.
Preferably, described magnetic field is 10 in the magnetic induction density B of this granules of catalyst array position
-5T≤B≤1T.
And, a kind of carbon nanotube preparing apparatus is provided, it comprises:
One substrate, it has a surface;
One is positioned at the groove of this substrate surface;
One is positioned at the granules of catalyst array on this substrate surface of this groove one side; And
One is positioned at the electrode on this substrate surface of the relative opposite side of this groove, and this electrode and this granules of catalyst array are oppositely arranged.
Described substrate comprises Silicon Wafer, or the compound wafer of III-V family.
The material of described granules of catalyst comprises iron, cobalt, nickel or its alloy.
With respect to prior art, preparation method of carbon nano-tube that the technical program provided and device, it is provided with an electrode at carbon nano-tube with the relative position of granules of catalyst array, and the substrate surface between this electrode and granules of catalyst array is provided with a groove, and this granules of catalyst array and electrode lay respectively at the relative both sides of this groove; Feed electric current to this electrode and can produce a magnetic field, this magnetic field is drawn carbon nanotube and is grown to electrode direction in the carbon nano tube growth process; It can obtain the carbon nanotube of length homogeneous.
[description of drawings]
Fig. 1 is the synoptic diagram that is formed with the granules of catalyst array in the first embodiment of the invention substrate.
Fig. 2 is first embodiment of the invention is formed with electrode at granules of catalyst array relative position a synoptic diagram.
Fig. 3 is that first embodiment of the invention forms reeded synoptic diagram between electrode and granules of catalyst array.
Fig. 4 is the synoptic diagram of first embodiment of the invention carbon nano-tube on the granules of catalyst array.
Fig. 5 is the synoptic diagram of first embodiment of the invention along the equidistant cutting carbon nanotubes of a line of cut.
[embodiment]
To be described in further detail the embodiment of the invention below in conjunction with accompanying drawing.
First embodiment
Referring to Fig. 1 to Fig. 4, first embodiment of the invention provides a kind of preparation method of carbon nano-tube, and it may further comprise the steps:
(1) referring to Fig. 1, a substrate 10 is provided, in this substrate 10, form a granules of catalyst array 20.This substrate 10 can be selected Silicon Wafer for use, semiconductor materials such as the compound wafer of III-V family.A plurality of granules of catalyst in this granules of catalyst array 20 are preferably, and linearly shape is arranged.Certainly, arranging of a plurality of granules of catalyst can make it equate substantially all can with the distance of the electrode of follow-up formation in this granules of catalyst array 20.The material of granules of catalyst can be selected iron, cobalt, nickel for use, or its alloy.This granules of catalyst array 20 will be as the catalyst of follow-up carbon nano tube growth.Wherein, the formation method of this granules of catalyst array 20 can adopt silk screen print method; Also can adopt following method: at first form a catalyst nano line in substrate 10, the live width of this nano wire can be 10nm～1 μ m; The substrate that then this is formed with the catalyst nano line is heated to 300 ℃～600 ℃, and annealing makes this catalyst nano line change the granules of catalyst array into.
(2), in substrate 10, and form an electrode 30 at the relative a certain distance and position place of granules of catalyst array 20 referring to Fig. 2 and Fig. 3; And 10 surfaces of the substrate between electrode 30 and granules of catalyst array 20 form a groove 12.Granules of catalyst array 20 is positioned on substrate 10 surfaces of groove 10 1 sides; Electrode 30 is positioned on substrate 10 surfaces of relative opposite side of groove 10.The shape of this electrode 30 and the setting of size equate for good to the distance of electrode 30 substantially to guarantee a plurality of granules of catalyst in the granules of catalyst array 20.Generally speaking, the chemical Vapor deposition process growth length for preparing carbon nanotube can be several nanometers to several microns; Therefore, electrode 30 can be set to the number nanometer with the distance of granules of catalyst array 20 in the present embodiment, even is several microns.In the present embodiment,, make the carbon nanotube of subsequent growth be parallel to substrate 10 surfaces substantially via the size of granules of catalyst array 20 and electrode 30 and the setting of shape; Being provided with of the size of groove 12 and shape can make carbon nanotube overcome itself and the bigger model ylid bloom action power (Van der Waals force) of substrate surface substantially, and can align along the vertical magnetic field direction.Generally speaking, the degree of depth of groove 12 is good with it greater than 1 μ m.In addition, electrode 30 can adopt sedimentation to cooperate a mask to form.The formation of groove 12 can be selected method for plasma etching and reactive ion etching method etc. for use.
(3) referring to Fig. 4, on this electrode 30, feed electric current to produce a magnetic field (figure does not show), utilize chemical Vapor deposition process (as, hot-filament cvd reactor method, plasma auxiliary chemical vapor deposition method, microwave plasma CVD method etc.) carbon nano-tube 40 on granules of catalyst array 20, this carbon nanotube 40 will be along growing perpendicular to this field direction; Also promptly grow to electrode 30 directions.Specific descriptions are:
Above-mentioned substrate 10 is placed in a CVD (Chemical Vapor Deposition, the chemical vapour deposition) reactor (figure does not show), heat 10 to 500 ℃～1000 ℃ of this substrates; And in this CVD reactor, feed carbon source gas (as, ethene, methane, acetylene etc.) carry out carbon nano tube growth.When carbon nanotube 40 grows to electrode 30 positions, make its stopped reaction.
When carbon nano tube growth begins, feed direct current or exchange current to electrode 30, it will be in the magnetic field that granules of catalyst array 20 sides generation one is basically perpendicular to substrate 10 surfaces that has of this electrode 30.This field direction determine to satisfy the right-handed helix rule; And the induction level of a certain position increases with the distance of itself and electrode 30 and reduces.For obtaining effective magnetic field, this magnetic field should be not less than 10 in the magnetic induction density B of granules of catalyst array 30 positions
-5T (tesla); Be preferably 10
-5T≤B≤1T.
Because the setting of groove 12 makes the carbon nanotube 40 and the interaction force on substrate 10 surfaces not have influence substantially to the orientation of carbon nanotube 40; Under the magnetic attraction effect, carbon nanotube will be oriented in the growth of electrode 30 directions, and because a plurality of granules of catalyst in the granules of catalyst array 20 equate substantially that with the distance of electrode 30 therefore, it can obtain and align and a plurality of carbon nanotubes of length homogeneous.
In addition, referring to Fig. 5, for the utilising efficiency that improves carbon nanotube 40 and obtain the carbon nanotube that has more homogeneous length; Can this carbon nanotube 40 of equidistant cutting.Its concrete steps are: adopt direct writing technology equidistantly cutting is above-mentioned aligns and the carbon nanotube 40 of length homogeneous along line of cut 50 at distance substrate 10 certain position places; And then obtain the carbon nanotube fragment of length homogeneous.The setting of this spacing can be decided according to the length of required carbon nanotube fragment.Preferably, this line of cut 50 is basically perpendicular to the axial direction due of carbon nanotube 40.Wherein, this direct writing technology is optional with direct electronic beam writing technology, focused ion beam direct writing technology and laser direct-writing technology.
Step in the present embodiment (1) and (2) can form a kind of carbon nanotube preparing apparatus (as shown in Figure 3).This carbon nanotube preparing apparatus comprises a substrate 10, and it has a surface; One is formed on the groove 12 on these substrate 10 surfaces; One is positioned at the substrate 10 lip-deep granules of catalyst arrays 20 of these groove 12 1 sides; And substrate 10 lip-deep electrodes 30 that are positioned at the relative opposite side of this groove 12.By the step in the present embodiment (3), can adopt this carbon nanotube preparing apparatus to carry out the preparation of length homogeneous carbon nanotube.
Second embodiment
The second embodiment of the invention and first embodiment are basic identical, and its difference is the change to the step of first embodiment (1) and step (2).The preparation method of the carbon nanotube of present embodiment may further comprise the steps:
(1) provide a substrate, it has a surface; Form a groove at this substrate surface.Generally speaking, the chemical Vapor deposition process growth length for preparing carbon nanotube can be several nanometers to several microns; Therefore, the width of present embodiment further groove can be set to the number nanometer, even is several microns; Its length by the subsequent growth carbon nanotube is decided.Generally speaking, the degree of depth of this groove is good with it greater than 1 μ m.
(2) on the substrate surface of above-mentioned groove one side, form a granules of catalyst array, and on the substrate surface of the relative opposite side of this groove, form an electrode.This electrode and granules of catalyst array are oppositely arranged.This granules of catalyst array shape, and the shape of electrode and the setting of size equate to be good to guarantee a plurality of granules of catalyst in the granules of catalyst array substantially to the distance of electrode.
(3) on this electrode, feed electric current to produce a magnetic field, utilize chemical Vapor deposition process (as, hot-filament cvd reactor method, plasma auxiliary chemical vapor deposition method, microwave plasma CVD method etc.) carbon nano-tube on this granules of catalyst array, this carbon nanotube will be along growing perpendicular to this field direction; Also promptly to this electrode direction growth.And then can obtain the carbon nanotube of orientation and length homogeneous.
In addition, for the utilising efficiency that improves carbon nanotube and obtain the carbon nanotube that has more homogeneous length, can this carbon nanotube of equidistant cutting, to form the carbon nanotube fragment of length homogeneous.
Step in the present embodiment (1) and (2) can form a kind of carbon nanotube preparing apparatus.This carbon nanotube preparing apparatus comprises a substrate, and it has a surface; One is formed on the groove of this substrate surface; One is positioned at the granules of catalyst array on the substrate surface of this groove one side; An and electrode that is positioned on the substrate surface of the relative opposite side of this groove.By the step in the present embodiment (3), can adopt this carbon nanotube preparing apparatus to carry out the preparation of length homogeneous carbon nanotube.
In addition, those skilled in the art also can do other variation in spirit of the present invention, shape as suitable change electrode and groove, the formation method of granules of catalyst array, the formation order that reaches granules of catalyst array, electrode, groove is to be used for the present invention, as long as it does not depart from technique effect of the present invention and all can.The variation that these are done according to spirit of the present invention all should be included within the present invention's scope required for protection.
Claims (13)
1. preparation method of carbon nano-tube, it may further comprise the steps:
One substrate is provided, and it has a surface;
On this substrate surface, form a granules of catalyst array;
The relative position of this granules of catalyst array on this substrate surface forms an electrode;
Form a groove at this substrate surface, this granules of catalyst array and electrode lay respectively at the relative both sides of this groove;
On this electrode, feed electric current with generation magnetic field, carbon nano-tube on this granules of catalyst array, this carbon nanotube will be grown up to electrode direction.
2. preparation method of carbon nano-tube as claimed in claim 1 is characterized in that also further comprising step:
This carbon nanotube of equidistant cutting is to obtain the carbon nanotube fragment of length homogeneous.
3. preparation method of carbon nano-tube as claimed in claim 2, the cutting that it is characterized in that described carbon nanotube is by direct electronic beam writing technology, the focused ion beam direct writing technology, or the laser direct-writing technology is finished.
4. preparation method of carbon nano-tube as claimed in claim 1, it is characterized in that in the described granules of catalyst array granules of catalyst linearly shape arrange.
5. preparation method of carbon nano-tube as claimed in claim 1 is characterized in that the formation method of described granules of catalyst array may further comprise the steps: form a catalyst nano line in this substrate; This catalyst nano line is heated to 300 ℃～600 ℃, and annealing makes this catalyst nano line be transformed into the granules of catalyst array.
6. preparation method of carbon nano-tube as claimed in claim 5, the live width that it is characterized in that described catalyst nano line are 10nm～1 μ m.
7. preparation method of carbon nano-tube as claimed in claim 1 is characterized in that the formation method of described groove comprises method for plasma etching and reactive ion etching method.
8. preparation method of carbon nano-tube as claimed in claim 1, the growth method that it is characterized in that described carbon nanotube is a chemical Vapor deposition process.
9. preparation method of carbon nano-tube as claimed in claim 8 is characterized in that described chemical Vapor deposition process comprises hot-filament cvd reactor method, plasma auxiliary chemical vapor deposition method and microwave plasma CVD method.
10. preparation method of carbon nano-tube as claimed in claim 1 is characterized in that described magnetic field is 10 in the magnetic induction density B of this granules of catalyst array position
-5T≤B≤1T.
11. a carbon nanotube preparing apparatus, it comprises:
One substrate, it has a surface;
One is positioned at the groove of this substrate surface;
One is positioned at the granules of catalyst array on this substrate surface of this groove one side; And
One is positioned at the electrode on this substrate surface of the relative opposite side of this groove, and this electrode and this granules of catalyst array are oppositely arranged.
12. carbon nanotube preparing apparatus as claimed in claim 11 is characterized in that described substrate comprises Silicon Wafer, or the compound wafer of III-V family.
13. carbon nanotube preparing apparatus as claimed in claim 11 is characterized in that the material of granules of catalyst comprises iron, cobalt, nickel or its alloy.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100364390A CN100482582C (en) | 2005-08-05 | 2005-08-05 | Carbon nano-tube preparation method and apparatus |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100364390A CN100482582C (en) | 2005-08-05 | 2005-08-05 | Carbon nano-tube preparation method and apparatus |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1907845A CN1907845A (en) | 2007-02-07 |
| CN100482582C true CN100482582C (en) | 2009-04-29 |
Family
ID=37699106
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2005100364390A Expired - Fee Related CN100482582C (en) | 2005-08-05 | 2005-08-05 | Carbon nano-tube preparation method and apparatus |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100482582C (en) |
Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101823687B (en) * | 2009-03-06 | 2013-01-23 | 中国科学院物理研究所 | Method for separating nano-materials and manufacturing nano-electrode |
| CN101811662B (en) * | 2010-03-12 | 2013-05-29 | 北京大学 | Method for preparing small-size optical microcavities |
| CN102074429B (en) * | 2010-12-27 | 2013-11-06 | 清华大学 | Field emission cathode structure and preparation method thereof |
| CN102786023B (en) * | 2011-05-18 | 2015-01-21 | 中国科学院上海微***与信息技术研究所 | Cover plate-free carbon nanotube device structure and manufacturing method thereof |
| 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 |
| CN104787749B (en) * | 2015-04-30 | 2016-07-06 | 西安科技大学 | A kind of preparation method of aligned carbon nanotube |
| CN107128901A (en) * | 2017-05-12 | 2017-09-05 | 长春理工大学 | A kind of oriented and ordered preparation method of carbon nano-tube |
| CN110116987A (en) * | 2019-03-15 | 2019-08-13 | 大连理工大学 | A kind of semiconductor nanowires sensor |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2003053846A2 (en) * | 2001-07-10 | 2003-07-03 | Universities Space Research Association | Spatial localization of dispersed single walled carbon nanotubes into useful structures |
| CN1456497A (en) * | 2002-04-05 | 2003-11-19 | 滝川浩史 | Method and device for producing nano-size carbon particles and monolayer carbon tube |
| JP2004215473A (en) * | 2003-01-06 | 2004-07-29 | Hiroshi Arai | Guidance and control technology and peripheral technologies thereof |
-
2005
- 2005-08-05 CN CNB2005100364390A patent/CN100482582C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2003053846A2 (en) * | 2001-07-10 | 2003-07-03 | Universities Space Research Association | Spatial localization of dispersed single walled carbon nanotubes into useful structures |
| CN1456497A (en) * | 2002-04-05 | 2003-11-19 | 滝川浩史 | Method and device for producing nano-size carbon particles and monolayer carbon tube |
| JP2004215473A (en) * | 2003-01-06 | 2004-07-29 | Hiroshi Arai | Guidance and control technology and peripheral technologies thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1907845A (en) | 2007-02-07 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN100482582C (en) | Carbon nano-tube preparation method and apparatus | |
| Terranova et al. | Nanodiamonds for field emission: state of the art | |
| CN101471211B (en) | Thermal emission electronic component | |
| KR100504971B1 (en) | Electron emissive film and method | |
| CN101471213B (en) | Thermal emission electronic component and method for producing the same | |
| CN101471212B (en) | Thermal emission electronic component | |
| CN101471215B (en) | Production method of thermoelectron source | |
| CN100405519C (en) | Preparation method of field emission element | |
| JP2004512247A (en) | Apparatus for electron cyclotron resonance plasma deposition process and single-walled carbon nanotubes and nanotubes obtained thereby | |
| Chouhan et al. | Field emission from optimized structure of carbon nanotube field emitter array | |
| JP2009231287A (en) | Carbon nanotube needle and manufacturing method of the same | |
| WO2006135094A1 (en) | Diamond electron emission cathode, electron emission source, electron microscope, and electron beam exposure device | |
| TWI386511B (en) | Apparatus and method for producing aligned carbon nanotube arrays | |
| CN101425439B (en) | Producing method for field emission type electron source | |
| JP2002179418A (en) | Method for forming carbon nanotube | |
| US9666400B2 (en) | Field emission electron source and field emission device | |
| WO2010123007A1 (en) | Cold-cathode field-emission electron source including rare-earth hexaboride | |
| US8727827B2 (en) | Method for making field emission electron source | |
| CN101442848B (en) | Method for locally heating object | |
| CN100437876C (en) | Field emission element | |
| US20110056433A1 (en) | Device for forming diamond film | |
| JPWO2008001805A1 (en) | Diamond electron emission cathode, electron source, electron microscope and electron beam exposure machine | |
| US8669696B1 (en) | Field emission electron source array and field emission device | |
| TWI330858B (en) | Thermionic emission device | |
| Shimoi et al. | Nonthermal and selective crystal bridging of ZnO grains by irradiation with electron beam as nonequilibrium reaction field |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20090429 Termination date: 20150805 |
|
| EXPY | Termination of patent right or utility model |