CN101221886A - Double-walled carbon nano-tube electric bulb and method for producing the same - Google Patents

Double-walled carbon nano-tube electric bulb and method for producing the same Download PDF

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Publication number
CN101221886A
CN101221886A CNA2008100565228A CN200810056522A CN101221886A CN 101221886 A CN101221886 A CN 101221886A CN A2008100565228 A CNA2008100565228 A CN A2008100565228A CN 200810056522 A CN200810056522 A CN 200810056522A CN 101221886 A CN101221886 A CN 101221886A
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carbon nano
walled carbon
tube
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CN100557765C (en
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舒勤科
韦进全
王昆林
李昕明
陈曦
王志诚
骆建彬
吴德海
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Tsinghua University
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Abstract

The invention provides a double-wall carbon nanotube bulb and a method for preparing the same, which belongs to the electroluminescence and nano material application technical field. In order to solve the problems of low luminous efficiency of the double-wall carbon nanotube bulb in prior art, the invention discloses a double-wall carbon nanotube bulb which comprises a double-wall carbon nanotube filament, a stem, a nickel plate, a glass blister and a lamp cap, wherein, the double-wall carbon nanotube bulb filament is a double-wall carbon nanotube bulb long filament loaded with Y2O3:Eu<3+> particles. The invention also discloses a method for preparing the double-wall carbon nanotube bulb. The double-wall carbon nanotube bulb of the invention utilizes Y2O3:Eu<3+> to allow the double-wall carbon nanotube bulb filament to achieve a higher temperature when electrifying and to exhibit the fluorescent property of Y2O3:Eu<3+>, thereby achieving higher luminous efficiency.

Description

Double-walled carbon nano-tube electric bulb and preparation method thereof
Technical field
The present invention relates to a kind of double-walled carbon nano-tube electric bulb and preparation method thereof, belong to electroluminescence and technical field of nano material application.
Background technology
At present, the whole world is being faced with energy crisis, and the competition of various countries on the energy grows in intensity.Recent years, because power tense, many cities of China and area the power cuts to limit consumption phenomenon all occurred in peak times of power consumption.Therefore, the luminous efficiency of raising electric light source just becomes the vital task of electric light source research with energy savings.Since the bright incandescent lamp of self-love enlightening hair tonic, on illuminating incandescent lamps wire material, do not had too big improvement, still continue to use tungsten filament as filament material, luminous by black body radiation.In order to improve the luminous efficiency of incandescent lamp, just need to improve the temperature of filament, make spectrum generation blue shift, but meanwhile the heating of incandescent lamp need consume more electric energy, and because the fusing point of tungsten filament is limited, the luminous efficiency of incandescent lamp is near the end.European Union, Australia and the U.S. respectively will be in 2009,2010 and the superseded in the past incandescent lamps of the year two thousand twenty.
The work in research and development new type electro source is being carried out always in the world.The mankind have developed the electric light source that is applied to different occasions so far, as are mainly used in the iodine-tungsten lamp of building site and plaza lighting, are used for the fluorescent lamp of normal lighting, are used for the sodium vapor lamp of road lighting.Though these electric light sources have the luminous efficiency higher than incandescent lamp, human eyes are their spectrum of sending of incompatibility but.Scientists utilizes semiconductor EL to make diode lights recently.Because the optical efficiency of diode lights is very high, for energy savings with improve environmental pollution and bring glad tidings.But the light-emitting semiconducting material of diode lights is mainly synthetic by the molecular beam epitaxial growth mode, remain in manufacture craft and require high, problems such as the speed of growth is slow, cost height, so the application of diode lights and popularization needs time.
(Nature 1991 for Iijima S, et al., 354:56-58) found carbon nano-tube under Electronic Speculum for people such as Japan Electronic Speculum scholar Iijima S.2004, people (Wei JQ, et al., Appl.Phys.Lett.2004 such as Wei JQ, 84:4869-4871) published about the Primary Study result of carbon nano-tube, proposed the carbon nano-tube electric bulb notion as filament in USA Magazine " Applied Physics Letters "." Nature " editorial office says that this is a kind of " recurrence " of Edison's osram lamp." Science " editorial office estimates that then this may become " the clearly visible example that first carbon nanotube technology is applied ".
(Science 2002 for Bachilo SM, et al., find that 298:2361-2366) carbon nano-tube has photoluminescence property for people such as Bachilo SM; (Phys.Rev.Lett.1998 81:1441-1444) finds that carbon nano-tube has electroluminescence characters to people such as Bonard JM for Bonard JM, et al.; (Opt.Mater. 2003 for Kim JY, et al., find that 21:147-151) the carbon nano-tube current capacity is up to 10 for people such as Kim JY 9A/cm 2, exceed 1000 times than the good copper of conduction, and under very high current carrying density, still keep higher thermal stability.The carbon nano-tube flexibility is good, and modulus of elasticity is very high, and density is low, can carry out macrotechnique easily.People such as Cheng HM (Cheng HM, et al., J.Appl.Phys.2005,98:044306) the luminous blackbody radiation characteristic that do not belong to of proof Single Walled Carbon Nanotube; People such as Bonard (Bonard JM, et al., Phys.Rev.Lett.1998,81:1441) the luminous of report multi-walled carbon nano-tubes is not because black body radiation or the thermoluminescence that caused by electric current; People such as Wei JQ (Wei JQ, et al., Appl.Phys.Lett.2004,84:4869-4871) the luminous black body radiation that not exclusively is equal to of proof double-walled carbon nano-tube makes carbon nano-tube can reach higher light efficiency.And, carbon nano-tube can be prepared into have different capacity bulb to adapt to different needs, the element of its filament material is a carbon, can not cause environmental pollution.In addition, because people (Li YL such as Li YL, et al., Science2004 304:276-278) realizes that carbon nano-tube grows continuously, and people (Motta M such as Motta M, et al., Nano lett.2005,5:1529-1533) the proof carbon nano-tube has good hot strength, makes carbon nano-tube electric bulb have the possibility that is generalized to market rapidly.People (Shu QK such as present Shu QK, et al., J.Appl.Phys.2007, the light efficiency of the double-walled carbon nano-tube electric bulb of 101:084306) having developed are 2.2 times of incandescent lamp, but also have suitable gap with respect to electricity-saving lamps such as fluorescent lamps, do not have enough market competitivenesss.
Successfully produce the double-walled carbon nano-tube long filament and the film (patent No.: ZL 03 143102.X of excellent performance at present in the prior art; Wei JQ et al., J Phys Chem B, 2004,108:8844-8847), large-area ultrathin carbon nano-tube film (number of patent application: 200510123986.2, publication number: CN1803594) with carbon nano-tube filament (number of patent application: 200310103042.X, publication number: CN1540713).
Summary of the invention
The objective of the invention is provides a kind of load that Y is arranged at the not high enough problem of double-walled carbon nano-tube electric bulb light efficiency that exists in the prior art 2O 3: Eu 3+Double-walled carbon nano-tube electric bulb of particle and preparation method thereof is intended to utilize Y 2O 3: Eu 3+Make the double-walled carbon nano-tube filament when energising, reach higher colour temperature, bring into play Y simultaneously 2O 3: Eu 3+Fluorescent characteristic, realize higher luminous efficiency with this, to reach purpose of energy saving.
Double-walled carbon nano-tube electric bulb of the present invention comprises double-walled carbon nano-tube filament, stem stem, nickel sheet, glass cell-shell and lamp holder, and described double-walled carbon nano-tube filament is that load has Y 2O 3: Eu 3+The double-walled carbon nano-tube long filament of particle.
In the present invention, the Y of institute's load 2O 3: Eu 3+Particle is attached on the double-walled carbon nano-tube tube wall, keeps the arrangement of double-walled carbon nano-tube surface atom.
In the present invention, the Y of institute's load 2O 3: Eu 3+Particle grain size is 5～30nm.
The present invention also provides the preparation method of described double-walled carbon nano-tube electric bulb, comprises the double-walled carbon nano-tube film for preparing in advance behind the purifying, and this method also comprises the steps:
1) preparation contains Y (NO 3) 3And Eu (NO 3) 3Solution, both molar concentration rates are (5～40): 1, and Y (NO 3) 3Concentration be less than or equal to 0.02mol/L;
2) the double-walled carbon nano-tube film behind the described purifying is put into above-mentioned solution, slowly splash into OH -Concentration is no more than the alkaline solution of 0.01mol/L, and constantly stirs, and obtaining load has Y 2O 3: Eu 3+The double-walled carbon nano-tube film of particle; The speed that wherein splashes into alkaline solution meets the following conditions: promptly add OH -Amount of substance with contain Y (NO 3) 3And Eu (NO 3) 3The increment of ratio of liquor capacity per hour be no more than 0.001mol/L; When splashing into the end of alkaline solution process, add OH -Amount of substance with contain Y (NO 3) 3And Eu (NO 3) 3The ratio of liquor capacity still be no more than 0.005mol/L;
3) water has Y to load 2O 3: Eu 3+The double-walled carbon nano-tube film of particle carries out rinsing, is 7 until the pH of washing lotion value;
4) load there is Y 2O 3: Eu 3+The double-walled carbon nano-tube film of particle takes out from water, and making it be shrunk to load has Y 2O 3: Eu 3+The double-walled carbon nano-tube long filament of particle;
5) load there is Y 2O 3: Eu 3+The double-walled carbon nano-tube long filament be fixed on the stem stem by the nickel sheet, be encapsulated in the cell-shell then, and load onto lamp holder.
The present invention has Y with load 2O 3: Eu 3+The double-walled carbon nano-tube film preparation of particle becomes filament, and the preparation method is simple, and raw material are organic substances, has reduced the use of tungsten with respect to osram lamp, and therefore, it is cheap for manufacturing cost.The Y of deposition 2O 3: Eu 3+Particle has strengthened the cold light composition on pure double-walled carbon nano-tube electric bulb basis, can reach higher light efficiency when lower input power.In addition, the bulb that the present invention proposes has been inherited incandescent lamp is not had stroboscopic, to the human eye close friend, helps preventing advantages such as eye fatigue, is applicable to the illumination in high-speed rotating component workshop, as the lathe illumination etc.The load that the present invention proposes has Y 2O 3: Eu 3+The double-walled carbon nano-tube electric bulb of particle can also be as novel energy-saving electric light source.
Description of drawings
Fig. 1 is the structural representation of double-walled carbon nano-tube electric bulb of the present invention.
Fig. 2 is that the load that is used for the filament preparation has Y 2O 3: Eu 3+The transmission electron microscope photo of the double-walled carbon nano-tube film of particle.
Embodiment
The present invention is described further below in conjunction with the drawings and specific embodiments.
Fig. 1 is the structural representation of double-walled carbon nano-tube electric bulb of the present invention.This double-walled carbon nano-tube electric bulb comprises double-walled carbon nano-tube filament, stem stem 2, nickel sheet 3, glass cell-shell 4 and lamp holder 5, and the double-walled carbon nano-tube filament is that load has Y 2O 3: Eu 3+The double-walled carbon nano-tube long filament 1 of particle.Load has Y 2O 3: Eu 3+The double-walled carbon nano-tube long filament 1 of particle is fixed on the stem stem 2 by nickel sheet 3, and stem stem 2 and glass cell-shell 4 at high temperature are fused to together, lamp holder 5 be installed in glass cell-shell 4 below.The Y of institute's load wherein 2O 3: Eu 3+Particle is attached on the double-walled carbon nano-tube tube wall, keeps the arrangement of double-walled carbon nano-tube surface atom.The Y of institute's load 2O 3: Eu 3+Particle grain size is 5～30nm.
The preparation method of above-mentioned double-walled carbon nano-tube electric bulb is as follows:
At first, preparation double-walled carbon nano-tube film: according to the existing patent (patent No.: the technology of being introduced ZL 03143102.X), with the n-hexane is carbon source, ferrocene is a catalyst precursor, the mist of argon gas and hydrogen is carrier gas, sulphur is as additive, with chemical vapour deposition technique synthetic double-walled carbon nano-tube on horizontal electric resistance furnace; Then according to existing patent (number of patent application: 200510123986.2, publication number: the CN1803594) technology of being introduced, double-walled carbon nano-tube oxidation in air that back is synthetic, be immersed in the hydrogen peroxide then, then add strong acid, rinsing to rinsing liquid is neutral then, last alcohol or the acetone of dripping in the aqueous solution of double-walled carbon nano-tube, double-walled carbon nano-tube is emerged, launch to form the double-walled carbon nano-tube film.
Then, carry out load as described below and encapsulation step again:
1) preparation contains Y (NO 3) 3And Eu (NO 3) 3Solution, both molar concentration rates are (5～40): 1, and Y (NO 3) 3Concentration be less than or equal to 0.02mol/L;
2) the double-walled carbon nano-tube film behind the described purifying is put into above-mentioned solution, slowly splash into OH -Concentration is no more than the alkaline solution of 0.01mol/L, and constantly stirs, and obtaining load has Y 2O 3: Eu 3+The double-walled carbon nano-tube film of particle; The speed that wherein splashes into alkaline solution meets the following conditions: promptly add OH -Amount of substance with contain Y (NO 3) 3And Eu (NO 3) 3The increment of ratio of liquor capacity per hour be no more than 0.001mol/L; When splashing into the end of alkaline solution process, add OH -Amount of substance with contain Y (NO 3) 3And Eu (NO 3) 3The ratio of liquor capacity still be no more than 0.005mol/L;
3) water has Y to load 2O 3: Eu 3+The double-walled carbon nano-tube film of particle carries out rinsing, is 7 until the pH of washing lotion value;
4) load there is Y 2O 3: Eu 3+The double-walled carbon nano-tube film of particle takes out from water, and making it be shrunk to load has Y 2O 3: EU 3+The double-walled carbon nano-tube long filament of particle;
5) load there is Y 2O 3: Eu 3+The double-walled carbon nano-tube long filament of particle is fixed on the stem stem by the nickel sheet, is encapsulated in the cell-shell then, and loads onto lamp holder.
Provide the specific embodiment of preparation double-walled carbon nano-tube electric bulb below.
Embodiment 1:
At first adopt prior art for preparing double-walled carbon nano-tube film.On this basis, load Y on the double-walled carbon nano-tube film 2O 3: Eu 3+Particle, and preparation filament and encapsulation bulb are specially:
1) solution of configuration 100 mL, Y (NO in this solution 3) 3And Eu (NO 3) 3Molar concentration rate is 20: 1 (Y (NO in this example 3) 3And Eu (NO 3) 3Molar concentration is respectively 0.01mol/L and 0.0005mol/L).
2) double-walled carbon nano-tube is put into wherein, slowly splashed into the KOH solution of 0.005mol/L, the speed that splashes into is 10mL per hour, splashes into altogether 5 hours.In splashing into the alkaline solution process, solution is constantly stirred, obtaining load has Y 2O 3: Eu 3+The double-walled carbon nano-tube film of particle.
3) water has Y to load 2O 3: Eu 3+The double-walled carbon nano-tube film of particle carries out rinsing, is 7 until the pH of washing lotion value.
4) load there is Y 2O 3: Eu 3+The double-walled carbon nano-tube film of particle takes out from water, and making it be shrunk to load has Y 2O 3: Eu 3+Double-walled carbon nano-tube long filament 1.
5) load there is Y 2O 3: Eu 3+The double-walled carbon nano-tube long filament 1 of particle is fixed on the stem stem 2 by nickel sheet 3, is encapsulated in then in the cell-shell 4, and loads onto lamp holder 5.
Preparation has Y based on load by this method 2O 3: Eu 3+The double-walled carbon nano-tube electric bulb of particle can reach higher light efficiency with respect to the bulb based on pure double-walled carbon nano-tube when lower input power.For example when input power is 2.5W, Y is arranged based on load 2O 3: Eu 3+The bulb relative luminous efficiency of the double-walled carbon nano-tube filament of particle is 6.11x/W, is based on 8 times of bulb of pure double-walled carbon nano-tube, can be used as novel energy-saving electric light source.
The Comparative Examples 1 of embodiment 1:
Under the constant situation of other step, make the Y (NO among the embodiment 1 3) 3Molar concentration surpasses 0.02mol/L (Y (NO in this Comparative Examples 3) 3And Eu (NO 3) 3Molar concentration changes 0.03mol/L and 0.0015mol/L respectively into).
The Comparative Examples 2 of embodiment 1:
Under the constant situation of other step, make the molar concentration of the KOH solution that is added among the embodiment 1 surpass 0.01mol/L (molar concentration of KOH solution is 0.03mol/L in this Comparative Examples).
The Comparative Examples 3 of embodiment 1:
Under the constant situation of other step, make the excessive velocities of the KOH solution that is added among the embodiment 1, for example change per hour 50mL into.
The Comparative Examples 4 of embodiment 1:
Under the constant situation of other step, in the process that splashes into KOH solution, do not stir.
Above Comparative Examples is resulting result be: containing Y (NO 3) 3And Eu (NO 3) 3Solution in local form a large amount of precipitations, and uneven the loading on the double-walled carbon nano-tube film of these precipitations, after it is prepared into filament and encapsulates bulb, the relative luminous efficiency reduction that bulb can reach.
The Comparative Examples 5 of embodiment 1:
Under the constant situation of other step, change the pH value of washing lotion among the embodiment 1 into 4, the result who obtains is: load has Y 2O 3: Eu 3+Deposit other impurity on the double-walled carbon nano-tube film of particle, after being prepared into filament and encapsulating bulb, its relative luminous efficiency that can reach reduces.
Embodiment 2:
At first adopt prior art for preparing double-walled carbon nano-tube film.On this basis, load Y on the double-walled carbon nano-tube film 2O 3: Eu 3+Particle, and preparation filament and encapsulation bulb are specially:
1) solution of configuration 200mL, Y (NO in this solution 3) 3And Eu (NO 3) 3Molar concentration rate is 40: 1 (Y (NO in this example 3) 3And Eu (NO 3) 3Molar concentration is respectively 0.02mol/L and 0.0005mol/L).
2) double-walled carbon nano-tube is put into wherein, slowly splashed into the NaOH solution of 0.01mol/L, the speed that splashes into is 20mL per hour, splashes into altogether 10 hours.In splashing into the alkaline solution process, solution is constantly stirred, obtaining load has Y 2O 3: Eu 3+The double-walled carbon nano-tube film of particle.
3) water has Y to load 2O 3: Eu 3+The double-walled carbon nano-tube film of particle carries out rinsing, is 7 until the pH of washing lotion value.
4) load there is Y 2O 3: Eu 3+The double-walled carbon nano-tube film of particle takes out from water, and making it be shrunk to load has Y 2O 3: Eu 3+The double-walled carbon nano-tube long filament 1 of particle.
5) load there is Y 2O 3: Eu 3+The double-walled carbon nano-tube long filament 1 of particle is fixed on the stem stem 2 by nickel sheet 3, is encapsulated in then in the cell-shell 4, and loads onto lamp holder 5.
Preparation has Y based on load by this method 2O 3: Eu 3+The double-walled carbon nano-tube electric bulb of particle can reach higher light efficiency, reaches purpose of energy saving.
The Comparative Examples 1 of embodiment 2:
Under the constant situation of other step, make the time lengthening of the NaOH solution that is added among the embodiment 2, for example change 20 hours into, make that having excess NaOH to join contains Y (NO 3) 3And Eu (NO 3) 3Solution in.Consequently contain Y (NO 3) 3And Eu (NO 3) 3Solution in form a large amount of flocculent deposits, these flocculent deposits are a large amount of uneven attached on the double-walled carbon nano-tube film, after being prepared into filament and encapsulating bulb, its relative luminous efficiency that can reach reduction.
Embodiment 3:
At first adopt prior art for preparing double-walled carbon nano-tube film.On this basis, load Y on the double-walled carbon nano-tube film 2O 3: Eu 3+Particle, and preparation filament and encapsulation bulb are specially:
1) solution of configuration 150mL, Y (NO in this solution 3) 3And Eu (NO 3) 3Molar concentration rate is 5: 1 (Y (NO in this example 3) 3And Eu (NO 3) 3Molar concentration is respectively 0.015mol/L and 0.003mol/L).
2) double-walled carbon nano-tube is put into wherein, slowly splashed into the NaOH solution of 0.002mol/L, the speed that splashes into is 20mL per hour, splashes into altogether 15 hours.In splashing into the alkaline solution process, solution is constantly stirred.
3) water has Y to load 2O 3: Eu 3+The double-walled carbon nano-tube film of particle carries out rinsing, is 7 until the pH of washing lotion value.
4) load there is Y 2O 3: Eu 3+The double-walled carbon nano-tube film of particle takes out from water, and making it be shrunk to load has Y 2O 3: Eu 3+The double-walled carbon nano-tube long filament 1 of particle.
5) load there is Y 2O 3: Eu 3+The double-walled carbon nano-tube long filament 1 of particle is fixed on the stem stem 2 by nickel sheet 3, is encapsulated in then in the cell-shell 4, and loads onto lamp holder 5.
Preparation has Y based on load by this method 2O 3: Eu 3+The double-walled carbon nano-tube electric bulb of particle can reach higher light efficiency, reaches purpose of energy saving.

Claims (4)

1. a double-walled carbon nano-tube electric bulb comprises double-walled carbon nano-tube filament, stem stem, nickel sheet, glass cell-shell and lamp holder, it is characterized in that: described double-walled carbon nano-tube filament is that load has Y 2O 3: Eu 3+The double-walled carbon nano-tube long filament of particle.
2. double-walled carbon nano-tube electric bulb according to claim 1 is characterized in that: the Y of institute's load 2O 3: Eu 3+Particle is attached on the double-walled carbon nano-tube tube wall, keeps the arrangement of double-walled carbon nano-tube surface atom.
3. double-walled carbon nano-tube electric bulb according to claim 1 and 2 is characterized in that: the Y of institute's load 2O 3: Eu 3+Particle grain size is 5～30nm.
4. the preparation method of the described double-walled carbon nano-tube electric bulb of claim 1 comprises the double-walled carbon nano-tube film for preparing in advance behind the purifying, it is characterized in that this method also comprises the steps:
1) preparation contains Y (NO 3) 3And Eu (NO 3) 3Solution, both molar concentration rates are (5～40): 1, and Y (NO 3) 3Concentration be less than or equal to 0.02mol/L;
2) the double-walled carbon nano-tube film behind the described purifying is put into above-mentioned solution, slowly splash into OH -Concentration is no more than the alkaline solution of 0.01mol/L, and constantly stirs, and obtaining load has Y 2O 3: Eu 3+The double-walled carbon nano-tube film of particle; The speed that wherein splashes into alkaline solution meets the following conditions: promptly add OH -Amount of substance with contain Y (NO 3) 3And Eu (NO 3) 3The increment of ratio of liquor capacity per hour be no more than 0.001mol/L; When splashing into the end of alkaline solution process, add OH -Amount of substance with contain Y (NO 3) 3And Eu (NO 3) 3The ratio of liquor capacity still be no more than 0.005mol/L;
3) water has Y to load 2O 3: Eu 3+The double-walled carbon nano-tube film of particle carries out rinsing, is 7 until the pH of washing lotion value;
4) load there is Y 2O 3: Eu 3+The double-walled carbon nano-tube film of particle takes out from water, and making it be shrunk to load has Y 2O 3: Eu 3+The double-walled carbon nano-tube long filament of particle;
5) load there is Y 2O 3: Eu 3+The double-walled carbon nano-tube long filament of particle is fixed on the stem stem by the nickel sheet, is encapsulated in the cell-shell then, and loads onto lamp holder.
CNB2008100565228A 2008-01-21 2008-01-21 Double-walled carbon nano-tube electric bulb and preparation method thereof Expired - Fee Related CN100557765C (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2009184881A (en) * 2008-02-06 2009-08-20 Sumitomo Osaka Cement Co Ltd Sintered compact and manufacturing process of the same
JP2012167015A (en) * 2012-06-11 2012-09-06 Sumitomo Osaka Cement Co Ltd Sintered body, and method for producing the same

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2009184881A (en) * 2008-02-06 2009-08-20 Sumitomo Osaka Cement Co Ltd Sintered compact and manufacturing process of the same
JP2012167015A (en) * 2012-06-11 2012-09-06 Sumitomo Osaka Cement Co Ltd Sintered body, and method for producing the same

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