CN100595141C - Method for preparing indium tin oxide assembled carbon nano-tube composite material - Google Patents
Method for preparing indium tin oxide assembled carbon nano-tube composite material Download PDFInfo
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- CN100595141C CN100595141C CN200810038658A CN200810038658A CN100595141C CN 100595141 C CN100595141 C CN 100595141C CN 200810038658 A CN200810038658 A CN 200810038658A CN 200810038658 A CN200810038658 A CN 200810038658A CN 100595141 C CN100595141 C CN 100595141C
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Abstract
The invention relates to a preparation method for assembling carbon nano-tube composite materials by indium tin oxides, which includes: (1) under room temperature, the carbon nano-tube is cleaned by using hydrofluoric acid and nitric acid, the carbon nano-tube after being dried is ultrasonically dispersed, washed and dried in a surfactant, and a carbon nano-tube modified by the surfactant is obtained; (2) under room temperature, indium and tin salt are dissolved in organic solvent which is added in the carbon nano-tube to be stirred and mixed, then sodium salt and additive are added, after being dispersed uniformly the mixture is transferred into a hydrothermal reaction caldron to react for a period of time, then being cooled down to the room temperature, and a carbon nano-tube assembled by indium tin oxide precursors is obtained after washed, filtered and dried; (3) the carbon nano-tube obtained in step (2) is placed at an inert atmosphere to calcine for a period of time, then being cooled down to the room temperature, and the carbon nano-tube composite materials assembled by the indium tin oxides are obtained. The method has the advantages of simplicity and convenience, simple production equipment, being easy to realize industrial production, little damage on the structure of the carbon nano-tube, and being beneficial for assembled carbon nano-tube composite materials to be further applied.
Description
Technical field
The invention belongs to the preparation field of nano composite material, particularly relate to a kind of preparation method of indium tin oxide assembled carbon nano-tube composite material.
Background technology
Carbon nanotube has the characteristic of a lot of novelties, has caused that scientist payes attention to greatly.Studies show that the metal oxide assembled carbon nano-tube composite material shows excellent more physics and chemical property, comprises better catalysis, conduction, optics, absorption property and microwave absorbing property etc., has more wide application prospect.
The method about the metal oxide assembled carbon nano-tube of report mainly contains liquid-phase chemistry deposition technique, pickling process, hydrothermal method etc. both at home and abroad at present.Liquid-phase chemistry deposition technique is that the carbon nanotube that modification is handled is distributed in the metal salt solution that contains active ingredient, add precipitation agent, reaction generates or separates out and is deposited on the carbon nanotube in liquid phase, make the product precursor, the presoma calcination processing is promptly obtained carbon nanotube loaded metal oxide carbon nanotube, this method is simple, with low cost, but generally need to use strong acid that carbon nanotube is carried out oxide treatment, a large amount of defectives of utilizing oxide treatment to produce then in carbon nano tube surface, further introduce metal oxide, but the structure of strong acid oxide treatment meeting destroying carbon nanometer tube, cause its mechanical property, declines such as electrical and thermal conductivity performance, the further use after being unfavorable for modifying.Pickling process is that carbon nanotube is immersed in the metal salt solution that contains active ingredient, thorough mixing, and to reach the method for active constituent loading on carbon nanotube, this method is simple to operate, but load efficiency is not high usually.Hydrothermal method is to utilize High Temperature High Pressure to make metal oxide separate out, be deposited on carbon nano tube surface, and this method is simple, and with low cost and suitable metal oxide a wider range is convenient to practical application.
Lupo etc. have described the method for Hydrothermal Preparation zirconium white/carbon mano-tube composite on Carbon 42 (2004) 1995, but the combination of zirconium white and carbon nanotube is restive, all have zirconium white to generate in carbon nanotube tube wall, the tube chamber.Liu etc. have described on Carbon 43 (2005) 47 carbon nanotube have been mixed with nickelous nitrate, iron nitrate, after dropping sodium is produced oxyhydroxide, pass through hydrothermal method again, the method for preparing carbon nanotube/Ni ferrite mixture, Ni ferrite parcel carbon nanotube is comparatively abundant, but the acidified processing of carbon nanotube back is blocked, and will cause composite property to descend.The common complex process of the method for metal oxide assembled carbon nano-tube in the past, cost height, and the structure of employing strong acid oxide treatment meeting destroying carbon nanometer tube cause the carbon length of tube to shorten, and have a strong impact on material property, and do not see the bibliographical information of relevant indium tin oxide particle assembled carbon nano-tube.
Summary of the invention
Technical problem to be solved by this invention provides a kind of preparation method of indium tin oxide assembled carbon nano-tube composite material, and this method is easy, and production unit is simple, is easy to suitability for industrialized production, and is little to the destruction of carbon nanotube structure.
The preparation method of a kind of indium tin oxide assembled carbon nano-tube composite material of the present invention comprises:
(1) finishing of carbon nanotube
Under the room temperature, clean carbon nanotube with 1v%～20v% (percent by volume) hydrofluoric acid and 1v%～20v% dilute nitric acid solution respectively, obtain the carbon nanotube of purifying after the drying, with it in the surfactant soln of 0.5wt%～10wt% (weight percentage) behind ultra-sonic dispersion 0.5～8h, cleaning, drying obtain surfactant modified carbon nanotube;
(2) preparation of indium tin hydroxide presoma assembled carbon nano-tube
Under the room temperature, indium, pink salt be dissolved in be made in the organic solvent indium, tin-salt solution, add surfactant modified carbon nanotube again, under 300～800 rev/mins rotating speed, mix, add sodium salt and additives polyethylene glycol then, change in the hydrothermal reaction kettle after being uniformly dispersed, at 100～300 ℃, kept 3～20 hours, and reduced to room temperature, obtain indium tin hydroxide presoma assembled carbon nano-tube after washing, filtration, the drying;
(3) preparation of indium tin oxide assembled carbon nano-tube
Indium tin hydroxide presoma assembled carbon nano-tube is warming up to 400～800 ℃ in inert atmosphere, this temperature lower calcination 0.5～5 hour, be cooled to room temperature under inert atmosphere, is indium tin oxide assembled carbon nano-tube composite material.
Carbon nanotube is single wall or the multi-walled carbon nano-tubes of caliber 10～40nm in the described step (1).
Tensio-active agent is a kind of in Sodium dodecylbenzene sulfonate, tween, class of department or the sodium laurylsulfonate in the described step (1).
Indium, pink salt are selected from muriate, nitrate or the vitriol of indium, tin two kinds in the described step (2), in preferred indium chloride, tin chloride, indium nitrate or the nitric acid tin two kinds, the mol ratio of indium salt and pink salt is 5～10: 1, the concentration of indium, tin-salt solution is 0.1g～100g/L solvent, and the additional proportion of indium tin-salt solution and carbon nanotube is 10～100ml/g.
Organic solvent is a kind of in ethylene glycol, glycerol or the propyl carbinol in the described step (2).
Sodium salt is a kind of in muriate, nitrate, acetate or the vitriol of sodium in the described step (2), and the add-on of sodium salt is 1～300g/L solvent.
The add-on of polyoxyethylene glycol is 0.1～50g/L solvent in the described step (2).
The inert atmosphere of described step (3) is a nitrogen, neon or argon gas atmosphere, and 0.3～5 liter/minute of inert gas flow, heat-up rate are 3～10 ℃/minute.
Room temperature in the described step (1) to (3) is 10～40 ℃.
Ultimate principle of the present invention: the tube wall of carbon nanotube passes through sp by hexagonal carbon atom
2Hydridization forms, and can have a small amount of defect point in the preparation process of carbon nanotube, these defect points active higher, just become the active sites of introducing the indium tin ion, the indium tin ion further generates oxyhydroxide at this, again through calcining, forms the carbon nano tube compound material of indium tin oxide assembling.Concentration by adjusting the indium tin-salt solution and temperature of reaction, reaction times, can obtain the indium tin oxide carbon nano tube compound material of variable grain yardstick.
Beneficial effect
(1) the inventive method is easy, and cost is low, and production unit is simple, is easy to suitability for industrialized production;
(2) little to the destruction of carbon nanotube structure, help the further application of assembled carbon nano-tube composite material.
Description of drawings
Fig. 1 is the transmission electron microscope photo of carbon nanometer tube material;
Fig. 2 is the X-ray diffractogram of indium tin oxide assembled carbon nano-tube;
Fig. 3 is the transmission electron microscope photo of indium tin oxide assembled carbon nano-tube;
Fig. 4 is the high-resolution-ration transmission electric-lens photo of indium tin oxide assembled carbon nano-tube.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Embodiment 1
Under the room temperature, clean carbon nanotube with the hydrofluoric acid of 10v% and the nitric acid of 20v% respectively, obtain the carbon nanotube of purifying after the drying, the carbon nanotube of purifying is dispersed in the Sodium dodecylbenzene sulfonate solution of 4wt%, after ultrasonic 4 hours, cleaning, drying obtain surfactant modified carbon nanotube.
Under the room temperature, 0.2g five nitric hydrate indiums (analytical pure) and 0.02g five hydration tin chlorides (analytical pure) are dissolved in the 40mL ethylene glycol, obtain the ethylene glycol solution of indium pink salt.
(average caliber is the multi-walled carbon nano-tubes of 30nm to the carbon nanotube that 2.0g is surfactant modified, decompose preparation by hydrocarbon oxidation catalyst) put into beaker, the ethylene glycol solution that then adds 40ml indium pink salt under (600 rev/mins of the rotating speeds) condition of stirring, adds 3.6g sodium-acetate and 1.0g polyoxyethylene glycol, after being uniformly dispersed, change in the hydrothermal reaction kettle,, kept 8 hours at 200 ℃, reduce to room temperature, obtain indium tin hydroxide presoma assembled carbon nano-tube after washing, filtration, the drying.
With the indium tin hydroxide presoma assembled carbon nano-tube that obtains; put into quartz boat; the tubular type of packing into atmosphere furnace; feed nitrogen, 0.6 liter/minute of gas flow, heat-up rate are 10 ℃/minute; be warming up to 600 ℃; and under 600 ℃, kept 1.0 hours, under nitrogen protection, naturally cool to room temperature then, obtaining black powder shape sample is indium tin oxide assembled carbon nano-tube.
Fig. 1 is the transmission electron microscope photo of carbon nanometer tube material.The caliber of carbon nanotube is about 30nm, and middle bright part is a carbon nanotubes lumen, and the part of darker in color is the nanotube tube wall, and the thickness of tube wall is approximately 6nm (caliber 1/3rd), and the outside surface of carbon nanotube is very smooth, does not see to be attached with other material.
Fig. 2 is the X-ray diffractogram of the indium tin oxide assembled carbon nano-tube of present embodiment preparation.A ° diffraction peak of locating is the characteristic peak of carbon nanotube in 2 θ=26.8, show with JCPDS card 06-0416 contrast: indium tin oxide is a cubic, diffraction peaks all among the figure is all corresponding with the cubic Indium sesquioxide, wherein the diffraction peak of five corresponding Indium sesquioxide (211) crystal faces of stronger diffraction peak, (222) crystal face, (400) crystal face, (440) crystal face, (622) crystal face.
Fig. 3 is the transmission electron microscope photo of indium tin oxide assembled carbon nano-tube, can see that the carbon nano tube surface coated pellet is comparatively even, and particle diameter is in 10～30nm scope.At a place is individual particle, and the b place has small quantities of particles to assemble.
Fig. 4 is the high-resolution-ration transmission electric-lens photo of indium tin oxide assembled carbon nano-tube.The c place is a carbon nanotube, and the d place is the indium tin oxide particle, and the indium tin oxide grain diameter is comparatively even as can be seen, and in 15～20nm scope, spacing is about 0.4nm, corresponding to (211) crystal face of tin indium oxide.
Embodiment 2
Under the room temperature, clean carbon nanotube, obtain the carbon nanotube of purifying after the drying with the hydrofluoric acid of 5v% and the nitric acid of 10v%, the carbon nanotube of purifying is dispersed in 2wt%) sodium dodecyl sulfate solution in, after ultrasonic 6 hours, cleaning, drying obtain surfactant modified carbon nanotube.
At room temperature, 0.3g four hydration indium chlorides (analytical pure) and 0.06g five hydration tin chlorides (analytical pure) are dissolved in the 20mL glycerol, obtain the glycerol solution of indium pink salt.Then that 0.5g is surfactant modified carbon nanotube is put into beaker, the glycerol solution that then adds 20ml indium pink salt under whipped state, adds 3.0g SODIUMNITRATE and 0.5g polyoxyethylene glycol, after being uniformly dispersed, change in the hydrothermal reaction kettle,, kept 12 hours at 160 ℃, reduce to room temperature, washing is filtered, and obtains indium tin hydroxide presoma assembled carbon nano-tube after the drying.
Following step is pressed embodiment 1 described method preparation.X-ray diffraction, TEM (transmission electron microscope) analysis show that gained black sample is an indium tin oxide assembled carbon nano-tube.
Embodiment 3
Under the room temperature, clean carbon nanotube, obtain the carbon nanotube of purifying after the drying with the hydrofluoric acid of 5v% and the nitric acid of 20v%, the carbon nanotube of purifying is dispersed in class of the department solution of 2wt%, after ultrasonic 6 hours, cleaning, drying obtain surfactant modified carbon nanotube.
At room temperature, 0.2g nine hydration tin sulphates (analytical pure) and 0.04g five hydration tin chlorides (analytical pure) are dissolved in the 20mL propyl carbinol, obtain the butanol solution of indium pink salt.
The carbon nanotube that 0.3g is surfactant modified is put into beaker; the butanol solution that then adds 20ml indium pink salt; under whipped state; add 3.0g sodium-chlor and 1.0g polyoxyethylene glycol, after being uniformly dispersed, change in the hydrothermal reaction kettle; at 180 ℃; kept 12 hours, and reduced to room temperature, washing; filter; obtain indium tin hydroxide presoma assembled carbon nano-tube after the drying, put into quartz boat, the tubular type of packing into atmosphere furnace; feed argon gas; 0.3 liter/minute of gas flow, heat-up rate is 5 ℃/minute, is warming up to 500 ℃; and under 500 ℃, kept 2 hours; naturally cool to room temperature under argon shield after, obtain black powder shape sample, X-ray diffraction and TEM (transmission electron microscope) analysis show that sample is an indium tin oxide assembled carbon nano-tube.
Embodiment 4
Under the room temperature, clean carbon nanotube, obtain the carbon nanotube of purifying after the drying with the hydrofluoric acid of 5v% and the nitric acid of 15v%, the carbon nanotube of purifying is dispersed in the sodium dodecyl sulfate solution of 1wt%, after ultrasonic 2 hours, cleaning, drying obtain surfactant modified carbon nanotube.
At room temperature, 0.4g four hydration indium chlorides (analytical pure) and 0.08g five hydration tin chlorides (analytical pure) are dissolved in the 40mL glycerol, obtain the glycerol solution of indium pink salt.
The carbon nanotube that 0.5g is surfactant modified (source is with embodiment 1) is put into beaker; the glycerol solution that then adds 15ml indium pink salt; under whipped state; add 2.0g SODIUMNITRATE and 0.5g polyoxyethylene glycol, after being uniformly dispersed, change in the hydrothermal reaction kettle; at 130 ℃; kept 10 hours, and reduced to room temperature, washing; filter; obtain indium tin hydroxide presoma assembled carbon nano-tube after the drying, put into quartz boat, the tubular type of packing into atmosphere furnace; feed argon gas; 0.6 liter/minute of gas flow, heat-up rate is 10 ℃/minute, is warming up to 600 ℃; and under 600 ℃, kept 1.5 hours; naturally cool to room temperature under argon shield after, obtain black powder shape sample, X-ray diffraction and TEM (transmission electron microscope) analysis show that sample is an indium tin oxide assembled carbon nano-tube.
Claims (9)
1. the preparation method of an indium tin oxide assembled carbon nano-tube composite material comprises:
(1) finishing of carbon nanotube
Under the room temperature, clean carbon nanotube with 1v%～20v% hydrofluoric acid and 1v%～20v% dilute nitric acid solution respectively, obtain the carbon nanotube of purifying after the drying, with it in the surfactant soln of 0.5wt%～10wt% behind ultra-sonic dispersion 0.5～8h, cleaning, drying obtain surfactant modified carbon nanotube; Wherein, tensio-active agent is a kind of in Sodium dodecylbenzene sulfonate, tween, class of department or the sodium laurylsulfonate;
(2) preparation of indium tin hydroxide presoma assembled carbon nano-tube
Under the room temperature, indium salt and pink salt are dissolved in the composite solution that is made into the indium pink salt in the organic solvent, add surfactant modified carbon nanotube again, under 300～800 rev/mins rotating speed, mix, add sodium salt and additives polyethylene glycol then, change in the hydrothermal reaction kettle after being uniformly dispersed, at 100～300 ℃, kept 3～20 hours, and reduced to room temperature, obtain indium tin hydroxide presoma assembled carbon nano-tube after washing, filtration, the drying;
(3) preparation of indium tin oxide assembled carbon nano-tube
Indium tin hydroxide presoma assembled carbon nano-tube is warming up to 400～800 ℃ in inert atmosphere, this temperature lower calcination 0.5～5 hour, be cooled to room temperature under inert atmosphere, is indium tin oxide assembled carbon nano-tube composite material.
2. the preparation method of indium tin oxide assembled carbon nano-tube composite material according to claim 1 is characterized in that: carbon nanotube is single wall or the multi-walled carbon nano-tubes of caliber 10～40nm in the described step (1).
3. the preparation method of indium tin oxide assembled carbon nano-tube composite material according to claim 1 is characterized in that: indium salt is selected from muriate, nitrate or the vitriol of indium in the described step (2); Pink salt is selected from muriate, nitrate or the vitriol of tin, and the mol ratio of indium salt and pink salt is 5～10: 1, and the concentration of the composite solution of indium pink salt is 0.1g～100g/L solvent, and the additional proportion of indium tin-salt solution and carbon nanotube is 10～100ml/g.
4. the preparation method of indium tin oxide assembled carbon nano-tube composite material according to claim 3 is characterized in that: indium salt is selected from the indium chloride or the indium nitrate of indium in the described step (2); Pink salt is selected from tin chloride or nitric acid tin.
5. the preparation method of indium tin oxide assembled carbon nano-tube composite material according to claim 1 is characterized in that: organic solvent is a kind of in ethylene glycol, glycerol or the propyl carbinol in the described step (2).
6. the preparation method of indium tin oxide assembled carbon nano-tube composite material according to claim 1, it is characterized in that: sodium salt is a kind of in muriate, nitrate, acetate or the vitriol of sodium in the described step (2), and the add-on of sodium salt is 1～300g/L solvent.
7. the preparation method of indium tin oxide assembled carbon nano-tube composite material according to claim 1 is characterized in that: the add-on of polyoxyethylene glycol is 0.1～50g/L solvent in the described step (2).
8. the preparation method of indium tin oxide assembled carbon nano-tube composite material according to claim 1, it is characterized in that: the inert atmosphere of described step (3) is a nitrogen, neon or argon gas atmosphere, 0.3～5 liter/minute of inert gas flow, heat-up rate are 3～10 ℃/minute.
9. the preparation method of indium tin oxide assembled carbon nano-tube composite material according to claim 1, it is characterized in that: the room temperature in the described step (1) to (3) is 10～40 ℃.
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| CN101792119B (en) * | 2010-04-08 | 2012-07-04 | 哈尔滨工业大学 | Method for preparing carbon nano tube composite material loaded with nano indium-tin oxide |
| CN101864316B (en) * | 2010-06-22 | 2013-04-17 | 上海师范大学 | Carbon nanotube/cadmium selenide quantum dot nano composite material and preparation method thereof |
| CN104923095A (en) * | 2015-06-11 | 2015-09-23 | 长沙理工大学 | Physical dispersing method for carbon nano-tube |
| CN106391054B (en) * | 2016-08-10 | 2019-04-02 | 上海交通大学 | A kind of carbon nanotube/indium sulfide heterojunction nano-wire and preparation method thereof |
| CN110320324A (en) * | 2019-04-26 | 2019-10-11 | 河南理工大学 | A kind of In of hollow structure2O3Gas sensitive and preparation method and application |
| CN115104047B (en) * | 2020-02-17 | 2024-06-07 | 三菱综合材料株式会社 | Infrared shielding film and infrared shielding material |
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