CN1305106C - Filament made from Nano carbon tupe and fabricating method - Google Patents
Filament made from Nano carbon tupe and fabricating method Download PDFInfo
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- CN1305106C CN1305106C CNB200310103042XA CN200310103042A CN1305106C CN 1305106 C CN1305106 C CN 1305106C CN B200310103042X A CNB200310103042X A CN B200310103042XA CN 200310103042 A CN200310103042 A CN 200310103042A CN 1305106 C CN1305106 C CN 1305106C
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- filament
- walled carbon
- tube
- carbon nano
- carbon nanometer
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- 238000000034 method Methods 0.000 title claims abstract description 8
- 229910021392 nanocarbon Inorganic materials 0.000 title 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 43
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 32
- 238000002360 preparation method Methods 0.000 claims abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000000746 purification Methods 0.000 claims abstract description 5
- 239000002079 double walled nanotube Substances 0.000 claims description 60
- 239000002109 single walled nanotube Substances 0.000 claims description 44
- 239000002041 carbon nanotube Substances 0.000 claims description 24
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 24
- 230000001476 alcoholic effect Effects 0.000 claims description 4
- 230000000694 effects Effects 0.000 claims description 3
- 238000000280 densification Methods 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 abstract description 18
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 abstract description 5
- 229910052721 tungsten Inorganic materials 0.000 abstract description 5
- 239000010937 tungsten Substances 0.000 abstract description 5
- 230000003287 optical effect Effects 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract 1
- 238000001228 spectrum Methods 0.000 description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 10
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 10
- 230000005457 Black-body radiation Effects 0.000 description 9
- 238000005516 engineering process Methods 0.000 description 5
- 238000007598 dipping method Methods 0.000 description 3
- 239000012153 distilled water Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 229910003481 amorphous carbon Inorganic materials 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 230000000994 depressogenic effect Effects 0.000 description 2
- 239000006210 lotion Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002048 multi walled nanotube Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
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Abstract
The present invention relates to a carbon nanometer tube filament and a preparing method thereof, which belongs to the application technical field of carbon nanometer material. In order to develop the excellent performance of a carbon nanometer tube on the electrical and optical aspects, propel a practicable process of the carbon nanometer tube and solve the problem of lower luminous efficiency of a tungsten filament, the present invention discloses the carbon nanometer tube filament which is prepared by single wall or double wall carbon nanometer tubes. The filament has the preparation method that the method comprises a preorder purification processing step, then a single wall carbon nanometer tube filament or a double wall carbon nanometer tube film is put in acetone or an alcohol solution to be sufficiently infiltrated, the single wall carbon nanometer tube filament or the double wall carbon nanometer tube film is taken out from the acetone or the alcohol solution, the double wall carbon nanometer tube film is naturally formed into a bundle of compact carbon nanometer tube filament after the acetone or alcohol is volatilized, the thickness of a single wall or a double wall carbon nanometer tube filament can be uniform along the length direction under the action of external force, and the filament can be obtained after the single wall or the double wall carbon nanometer tube filament is baked. The carbon nanometer tube filament prepared by the present invention has the advantages of low threshold voltage, high luminous efficiency and high brightness.
Description
Technical field
The invention belongs to the carbon nanomaterial applied technical field.
Background technology
In recent years, carrying out rapidly based on the application study of carbon nano-tube, is the flat-panel monitor of raw material and two achievements that ultracapacitor is considered to can access practical application with the carbon nano-tube.Here the inventor provides another kind and can make carbon nano-tube obtain the achievement in research of very fast application.Carbon nano-tube has very high conductive capability, and for single-root carbon nano-tube, its current capacity can reach 10
9A/cm
2, be 1000 times of copper.Carbon nano-tube has superior optical property, O ' Connell, M.J. wait the people (O ' Connell M.J.et al., Science, 2002,297:593-596) and Bachilo, people such as S.M (Bachilo S.M.et al., Science, 2002,298:2361-2366) reported that respectively carbon nano-tube under the laser pumping of a certain wavelength fluorescent effect can take place.People such as the Wang Peng of Tsing-Hua University (Wang P.et al., Applied Physics Letters, 2003,82:1763-1765) when a branch of length was added an electric current for the 0.6mm thickness is about 20 microns multi-wall carbon nanometer tube bundle, carbon nano-tube can be sent the incandescent light of polarization.
Double-walled carbon nano-tube is the one-dimensional nano structure that is curled and form according to certain helical angle by two-layer graphite synusia, is the simplest multi-walled carbon nano-tubes.Because the diameter and the Single Walled Carbon Nanotube of double-walled carbon nano-tube are approaching, and its interlamellar spacing big (between 0.34～0.41nm), so, the performance of double-walled carbon nano-tube near or be better than Single Walled Carbon Nanotube, the inventor's result of study shows, double-walled carbon nano-tube have the electric resistance changing temperature lower than Single Walled Carbon Nanotube (Wei J.Q.et al.Carbon, 2003,41:2495-2500).Because the preparation technology of Single Walled Carbon Nanotube limits, the Single Walled Carbon Nanotube that obtains relatively large highly purified macro-size is also relatively more difficult, thereby has limited its application study.But because the length of carbon nano-tube is powdered form usually in tens of micron dimensions, these carbon nanotube powders have limited its application.On June 9th, 2003, the patent of invention " synthetic method of double-walled carbon nano-tube " of inventor's application (number of patent application: the method that discloses preparation gram double-walled carbon nano-tube film magnitude, that have macro-size 03143102.X).
Above-mentioned double-walled carbon nano-tube film is used hydrogen peroxide dipping 72 hours, add concentrated hydrochloric acid then, can obtain purity after cleaning through distilled water is the above double-walled carbon nano-tube of 90wt%, and double-walled carbon nano-tube still keeps macroscopical membrane structure.These technology make the inventor to carry out macrotechnique to carbon nano-tube easily, and the macro property of research double-walled carbon nano-tube is prepared practical device.
Summary of the invention
The present invention is intended to develop the excellent properties of the electricity and the optics aspect of carbon nano-tube, thereby advances the practicalization of carbon nano-tube, solves the lower problem of tungsten filament luminous efficiency.
The invention provides a kind of carbon nano-tube filament, it is characterized in that: described filament is made by single wall or double-walled carbon nano-tube long filament.
The present invention also provides the preparation method of above-mentioned carbon nano-tube filament, comprises the preorder purification step of Single Walled Carbon Nanotube long filament or double-walled carbon nano-tube film, it is characterized in that this method also comprises the steps:
1) with the Single Walled Carbon Nanotube long filament after the purified processing or the double-walled carbon nano-tube film is put into acetone or alcoholic solution fully soaks into;
2) described Single Walled Carbon Nanotube long filament or double-walled carbon nano-tube film are taken out from acetone or alcoholic solution, treat acetone or alcohol the volatilization after, the double-walled carbon nano-tube film forms the carbon nano-tube long filament of a branch of densification naturally;
3) under the effect of external force, make the thickness of described single wall or double-walled carbon nano-tube long filament alongst even;
4) described single wall of oven dry or double-walled carbon nano-tube long filament obtain the filament of being made by single wall or double-walled carbon nano-tube.
It is low that the carbon nano-tube filament of the present invention preparation has a threshold voltage, luminous efficiency height, the high advantage of safe bulb of the 40W that the brightness ratio same electrical is depressed.
Description of drawings
Fig. 1 be contain the double-walled carbon nano-tube filament bulb under different temperature at the luminescent spectrum figure of visible region.The luminescent spectrum that curve 1 calculates under 1600K for black body radiation among the figure; Curve 2 is the luminescent spectrum of double-walled carbon nano-tube filament under 1560K; Curve 3 is the luminescent spectrum of double-walled carbon nano-tube filament under 1420K; Curve 4 is the luminescent spectrum of double-walled carbon nano-tube under 1340K; The luminescent spectrum that curve 5 calculates under 1350K for black body radiation.
Fig. 2 be contain the Single Walled Carbon Nanotube filament bulb under different temperatures at the luminescent spectrum figure of visible region.The luminescent spectrum that curve 1 calculates under 2000K for black body radiation among the figure; Curve 2 is the luminescent spectrum of Single Walled Carbon Nanotube filament under 1900K; Curve 3 is the luminescent spectrum of Single Walled Carbon Nanotube filament under 1800K; Curve 4 is the luminescent spectrum of Single Walled Carbon Nanotube under 1700K; The luminescent spectrum that curve 5 calculates under 1700K for black body radiation.
Fig. 3 is double-walled carbon nano-tube filament (8.2 Ω), Single Walled Carbon Nanotube filament (18.2 Ω) and common safe bulb (tungsten filament, 36V, brightness 40W) and the graph of relation of voltage.The brightness of curve 1 expression double-walled carbon nano-tube filament and the relation curve of voltage among the figure; The brightness of curve 2 expression Single Walled Carbon Nanotube filaments and the relation curve of voltage; The brightness of curve 3 expression tungsten filaments and the relation curve of voltage.
Embodiment
Describe the present invention in detail below in conjunction with accompanying drawing.
The preparation technology of double-walled carbon nano-tube filament of the present invention is as follows: the double-walled carbon nano-tube film that will prepare attitude was with 30% hydrogen peroxide dipping 24～72 hours, add 37% concentrated hydrochloric acid then, to remove amorphous carbon and the metal catalyst particles on the double-walled carbon nano-tube film, clean the double-walled carbon nano-tube film with distilled water then and be neutral up to washing lotion.Purity through the double-walled carbon nano-tube after hydrogen peroxide and the concentrated hydrochloric acid processing can reach more than 90%, and double-walled carbon nano-tube still keeps macroscopic view membranaceous after handling.Then the double-walled carbon nano-tube film after the purification process is immersed in the acetone, it is fully soaked into, with tweezers the double-walled carbon nano-tube film is taken out from acetone soln after 1～10 minute.After treating the acetone volatilization, the double-walled carbon nano-tube film forms the comparatively fine and close long filament of a structure.With two planes (as wave carrier piece etc.) the double-walled carbon nano-tube long filament is pushed along diametric(al), alongst size is even to make its thickness, just made the double-walled carbon nano-tube filament after the oven dry.
The preparation technology of Single Walled Carbon Nanotube filament of the present invention is as follows: the Single Walled Carbon Nanotube long filament that will prepare attitude was with 30% hydrogen peroxide dipping 24～72 hours, add 37% concentrated hydrochloric acid then, to remove amorphous carbon and the metal catalyst particles on the Single Walled Carbon Nanotube long filament, clean the Single Walled Carbon Nanotube long filament with distilled water then and be neutral up to washing lotion.Purity through the Single Walled Carbon Nanotube long filament after hydrogen peroxide and the concentrated hydrochloric acid processing can reach more than 85%.Then the Single Walled Carbon Nanotube long filament after the purification process is immersed in the acetone, it is fully soaked into, with tweezers the Single Walled Carbon Nanotube long filament is taken out from acetone soln after 1～10 minute.After treating acetone volatilization, with two planes (as wave carrier piece etc.) the Single Walled Carbon Nanotube long filament is pushed along diametric(al), alongst size is even to make its thickness, just made the Single Walled Carbon Nanotube filament after the oven dry.
Use alcohol to replace acetone, can realize the present invention equally.
The Single Walled Carbon Nanotube filament that method for preparing is come out or the length of double-walled carbon nano-tube filament are more than the 10mm, and Single Walled Carbon Nanotube filament or double-walled carbon nano-tube filament have certain intensity and toughness.With the carbon nano-tube filament thickness for preparing is the pure nickel paper tinsel clamping of 0.05～0.15mm, makes electrode and connects, and is installed in after the oven dry in the bulb, is evacuated to vacuum degree and is higher than 10
-5Pa charges into 0.5 atmospheric argon gas or nitrogen and bromize hydrogen gas mixture then, encapsulates in quartz glass tube, has just prepared Single Walled Carbon Nanotube bulb or double-walled carbon nano-tube bulb.
To including the Single Walled Carbon Nanotube filament, the bulb of double-walled carbon nano-tube filament carries out test shows: the bulb that contains the Single Walled Carbon Nanotube filament has similar performance with the bulb that contains the double-walled carbon nano-tube filament.As shown in Figure 1, the brightness ratio black body radiation of double-walled carbon nano-tube filament partly has more superior performance at visible light, and wavelength be 407 and the purple light of 417nm and the ruddiness place that wavelength is 655nm the peak is arranged, and peak value raises along with voltage and increases, and illustrates that double-walled carbon nano-tube can launch the cold light of some.Under the lower condition of temperature, the spoke intensity of double-walled carbon nano-tube filament and black body radiation close, and at high temperature (＞1350K), the spoke intensity of double-walled carbon nano-tube filament is at the height of visible light part than black body radiation, and low at the spoke strength ratio black body radiation of infrared part double-walled carbon nano-tube filament, this has shown that the double-walled carbon nano-tube filament has higher luminous efficiency at visible region.
As shown in Figure 2, also has similar characteristic for the Single Walled Carbon Nanotube filament.The Single Walled Carbon Nanotube filament wavelength be 407,417 and the 655nm place peak value is arranged, show that Single Walled Carbon Nanotube excites the cold light that can launch some down at certain electric field.Similar with the double-walled carbon nano-tube filament, the intensity height of Single Walled Carbon Nanotube filament black body radiation under the strength ratio uniform temp of visible light part, and at infrared region, the spoke intensity of the identical black matrix of spoke strength ratio of Single Walled Carbon Nanotube filament is low, has shown that the Single Walled Carbon Nanotube filament has higher luminous efficiency at visible region.
As shown in Figure 3 be the bulb (8.2 Ω) that includes the double-walled carbon nano-tube filament, bulb of Single Walled Carbon Nanotube filament (18.2 Ω) and common safe bulb (2.8 Ω, 36V, illumination 40W) and the relation curve of voltage, as can be seen, the carbon nano-tube bulb have than the lower threshold voltage of safety bulb and under identical voltage the brightness ratio safety bulb of carbon nano-tube bulb higher.The double-walled carbon nano-tube bulb has the threshold voltage lower than tungsten filament, the high advantage of safe bulb of the 40W that its brightness ratio same electrical is depressed.Life-span to the bulb that contains the double-walled carbon nano-tube filament is carried out test shows, and obvious variation does not take place after lighting 360 hours the bulb that contains the double-walled carbon nano-tube filament yet, illustrates with the double-walled carbon nano-tube to be that the bulb of filament has actual application prospect.
Claims (2)
1. carbon nano-tube filament, it is characterized in that: described filament is made by single wall or double-walled carbon nano-tube long filament.
2. the preparation method of carbon nano-tube filament according to claim 1 comprises the preorder purification step of Single Walled Carbon Nanotube long filament or double-walled carbon nano-tube film it is characterized in that this method also comprises the steps:
1) with the Single Walled Carbon Nanotube long filament after the purified processing or the double-walled carbon nano-tube film is put into acetone or alcoholic solution fully soaks into;
2) described Single Walled Carbon Nanotube long filament or double-walled carbon nano-tube film are taken out from acetone or alcoholic solution, treat acetone or alcohol the volatilization after, the double-walled carbon nano-tube film forms the carbon nano-tube long filament of a branch of densification naturally;
3) under the effect of external force, make the thickness of described single wall or double-walled carbon nano-tube long filament alongst even;
4) described single wall of oven dry or double-walled carbon nano-tube long filament obtain the filament of being made by single wall or double-walled carbon nano-tube.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200310103042XA CN1305106C (en) | 2003-10-31 | 2003-10-31 | Filament made from Nano carbon tupe and fabricating method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200310103042XA CN1305106C (en) | 2003-10-31 | 2003-10-31 | Filament made from Nano carbon tupe and fabricating method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1540713A CN1540713A (en) | 2004-10-27 |
| CN1305106C true CN1305106C (en) | 2007-03-14 |
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| Application Number | Title | Priority Date | Filing Date |
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| CNB200310103042XA Expired - Fee Related CN1305106C (en) | 2003-10-31 | 2003-10-31 | Filament made from Nano carbon tupe and fabricating method |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101192490B (en) | 2006-11-24 | 2010-09-29 | 清华大学 | Surface conductive electronic emission element and electronic source applying same |
| CN101192494B (en) * | 2006-11-24 | 2010-09-29 | 清华大学 | Electron emission element preparation method |
| CN103366644B (en) * | 2012-03-30 | 2015-09-30 | 清华大学 | The preparation method of incandescent source and incandescent source display device |
| CN103395240B (en) * | 2013-08-14 | 2015-11-11 | 苏州捷迪纳米科技有限公司 | The preparation method of carbon nano-composite material and corresponding carbon nano-composite material |
| US20220064003A1 (en) * | 2018-12-27 | 2022-03-03 | Sumitomo Electric Industries, Ltd. | Method for manufacturing carbon nanotube, method for manufacturing carbon nanotube assembled wire, method for manufacturing carbon nanotube assembled wire bundle, carbon nanotube manufacturing apparatus, carbon nanotube assembled wire manufacturing apparatus, and carbon nanotube assembled wire bundle manufacturing apparatus |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5494783A (en) * | 1978-01-10 | 1979-07-26 | Toshiba Corp | Incandescent lamp |
| JPH11162333A (en) * | 1997-12-01 | 1999-06-18 | Ise Electronics Corp | Manufacture of fluorescent character display device |
| US20030190278A1 (en) * | 2002-04-08 | 2003-10-09 | Yan Mei Wang | Controlled deposition of nanotubes |
-
2003
- 2003-10-31 CN CNB200310103042XA patent/CN1305106C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5494783A (en) * | 1978-01-10 | 1979-07-26 | Toshiba Corp | Incandescent lamp |
| JPH11162333A (en) * | 1997-12-01 | 1999-06-18 | Ise Electronics Corp | Manufacture of fluorescent character display device |
| US20030190278A1 (en) * | 2002-04-08 | 2003-10-09 | Yan Mei Wang | Controlled deposition of nanotubes |
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| CN1540713A (en) | 2004-10-27 |
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