CN105540567A - Single multi-wall carbon nanotube dispersion liquid and preparation method thereof - Google Patents
Single multi-wall carbon nanotube dispersion liquid and preparation method thereof Download PDFInfo
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- CN105540567A CN105540567A CN201610104571.9A CN201610104571A CN105540567A CN 105540567 A CN105540567 A CN 105540567A CN 201610104571 A CN201610104571 A CN 201610104571A CN 105540567 A CN105540567 A CN 105540567A
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- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/13—Nanotubes
- C01P2004/133—Multiwall nanotubes
Abstract
The invention relates to the fields of nano electronic devices and nano composite materials, belongs to the field of carbon nanotube materials and provides single multi-wall carbon nanotube dispersion liquid and a preparation method thereof. The single multi-wall carbon nanotube dispersion liquid is composed of multi-wall carbon nanotubes with the concentration being 1g/L, fullerol with the concentration being 0.4g/L and a polar solvent with the pH larger than or equal to 7. According to the method, fullerol serves as a surfactant to disperse the purified multi-wall carbon nanotubes, and the uniform and stable single multi-wall carbon nanotube dispersion liquid is prepared through the procedures of mixing, ultrasonic processing and centrifugation. The application field of the carbon nanotubes is further expanded, and the single multi-wall carbon nanotube dispersion liquid particularly plays an important role in development of fields such as nano electronic devices and nano composite materials.
Description
Technical field
The present invention relates to nano electron device, field of nanocomposite materials, specifically belong to carbon nano-tube material field, is a kind of single multi-walled carbon nano-tubes dispersion liquid and preparation method thereof.
Background technology
Carbon nanotube (CNTs), as a kind of novel monodimension nanometer material, has unique structure, excellent physics and chemistry characteristic.In recent years, related application field is fast-developing, scientists successively have developed transistor (see Nature such as TansS, 1998,393:49 52.), sensor (see AdvancedMaterials such as ChenPC, 2010,22:1900-1904.), vibrator is (see Nature such as SazonovaV, 2004,431:284-287.) etc. based on the high performance device of single-root carbon nano-tube, the monodispersity of carbon nanotube is had higher requirement.At present, containing impurity such as catalyst metal particles, carbon nano-particle and decolorizing carbon in the carbon nanotube using the methods such as chemical vapour deposition, arc-over, laser evaporation to prepare; Meanwhile, the effect of Van der Waals force easily makes single-root carbon nano-tube attract each other and forms large coacervate.Therefore, improve purity and the dispersing property of carbon nanotube, significant to the development in the field such as nano electron device, nano composite material.
At present in carbon nanotube method of purification, Physical is complicated, time-consuming and efficiency is low.Chemical method can be purified by selective oxidation, the method of general employing directly carries out liquid-phase oxidation by nitric acid, hydrogen peroxide, concentrated nitric acid/vitriol oil (volume ratio 1:3) mixed acid solution etc., but the experiment parameter that these methods obtain is inconsistent, there is no unified comparison, and larger to the destruction of carbon nanotube structure.In carbon nanotube dispersed Journal of Sex Research, existing experiment is by using Sodium dodecylbenzene sulfonate (see NANOLETTERS such as M.F.Islam, 2003,3(2): 269-273.) and polyvinylpyrrolidone (see ChemicalPhysicsLetters such as MichaelJ.O'Connell, 2001, the dispersing property of carbon nanotube 342(3-4): 265-271.) is relatively improved as tensio-active agent, but still cannot obtain the single-root carbon nano-tube of dispersion, and the tensio-active agent in dispersion liquid is not easily removed.
Summary of the invention
The present invention in order to the single-root carbon nano-tube that solves currently available technology and cannot obtain disperseing and the problem not easily removed of tensio-active agent in dispersion liquid, provides a kind of single multi-walled carbon nano-tubes dispersion liquid and preparation method thereof.
The present invention is achieved by the following technical solutions: single multi-walled carbon nano-tubes dispersion liquid, is to strangle by the multi-walled carbon nano-tubes of 1g/L, the richness of 0.4g/L the polar solvent that alcohol and pH be more than or equal to 7 to form.
The tensio-active agent that the present invention adopts is that the richness with polar group strangles alcohol, because compared with non-polar solvent, the soccerballene with polar group is more easily dissolved in polar solvent (such as, water or alcohol).Richness strangles the polyhydroxy derivates of alcohol as soccerballene, is used as tensio-active agent in the present invention, mainly because richness strangles the soluble in water and alcohol polar solvent of alcohol.Simultaneously, the electron adsorption ability that its cage structure is very strong, can be interacted by π-π with multi-walled carbon nano-tubes sidewall and produce physical property and adsorb, weakening the Van der Waals force between multi-walled carbon nano-tubes, therefore effectively can improve dispersiveness and the stability of multi-walled carbon nano-tubes.
Wherein, the pH of polar solvent will be equal to or greater than 7.Reason mainly contains following two aspects: 1) purified multi-wall carbon nano-tube tube-surface can introduce the oxy radical such as hydroxyl, carboxyl, the solution defection of acid ion improves the dispersing property of multi-walled carbon nano-tubes, but acidic conditions can suppress dissociating of multi-walled carbon nano-tubes surface acid group particle.2) compare with sour environment, under alkaline environment, high energy barrier is not existed to the oxidation that richness strangles alcohol, at room temperature easily can realize, be convenient to obtain the oxy radicals such as hydroxyl.Simultaneously richly strangle the character that alcohol has weak acid, therefore alkaline environment can promote its dissociating in the solution, increases rich solvability of strangling alcohol, thus improves the dispersing property of carbon pipe.Further, described polar solvent is sodium hydrate methanol solution, and wherein the concentration of sodium hydroxide is 0.01g/L.
In addition, in order to more detailed explanation the present invention, provide the preparation method of described single multi-walled carbon nano-tubes dispersion liquid,
Operation I: multi-walled carbon nano-tubes is added in alkaline pretreating reagent solution, 40 DEG C of reflux 12h; Then pretreated multi-walled carbon nano-tubes is joined ultrasonic 30min in concentrated nitric acid/vitriol oil mixed acid solution that volume ratio is 1:3, filter after neutral with deionized water wash, dry, reclaim the multi-walled carbon nano-tubes obtaining purifying;
Operation II: the multi-walled carbon nano-tubes of purifying, richness strangle alcohol and polar solvent mixes, adopts ultrasonic vibration dispersion, obtains multi-walled carbon nano-tubes dispersion liquid;
Operation III: carry out centrifugation 30min to the multi-walled carbon nano-tubes dispersion liquid that operation II obtains, rotating speed is 4000 ~ 6000r/min, reclaims the supernatant liquor after centrifugation, obtains single multi-walled carbon nano-tubes dispersion liquid.
In this preparation method, the reason of multi-walled carbon nano-tubes being carried out to the purification of liquid-phase oxidation substep is: the 1) acting in conjunction of pretreating reagent and mixed acid solution, can catalyst-solvent metallic particles, impurity contained in multi-walled carbon nano-tubes after therefore purifying obviously reduces; 2) adopt the purification of nitration mixture ultrasonic substep and direct nitration mixture to reflux to carry out compared with purification, the former is less to multi-walled carbon nano-tubes structural damage, and can keep the intrinsic property of multi-walled carbon nano-tubes better.
The multi-walled carbon nano-tubes of above-mentioned purifying, its surface can the oxy radical such as functionalized hydroxyl, carboxyl.This is because the acting in conjunction of pretreating reagent and mixed acid solution can make the fault location rate initial oxidation of multi-walled carbon nano-tubes, also by decolorizing carbon and carbon nano-particle activation, can make the oxy radical such as functionalisation of surfaces hydroxyl, carboxyl of multi-walled carbon nano-tubes simultaneously.And the dispersing property of multi-walled carbon nano-tubes in polar solvent (water or alcohol) of purifying is improved.This is because the multi-wall carbon nano-tube tube-surface of purifying can introduce the oxy radical such as hydroxyl, carboxyl, the solution defection of contained acid ion makes multi-walled carbon nano-tubes surface band negative charge, strengthen the electrostatic repulsion between multi-walled carbon nano-tubes, and then improve the dispersing property of multi-walled carbon nano-tubes.
During embody rule, wherein operation I is the operation of multi-walled carbon nano-tubes, richness being strangled alcohol and polar solvent mixing.In this operation, multi-walled carbon nano-tubes can be mixed simultaneously, richness strangles alcohol and polar solvent; Also can first obtain after richness strangles alcoholic solution, remix multi-walled carbon nano-tubes; After first multi-walled carbon nano-tubes can also being mixed with polar solvent, then add richness and strangle alcohol.
Wherein, operation II carries out sonic oscillation to the mixed solution obtained in operation I, prepares the operation of dispersion liquid.Ultra-sonic oscillation can use the ultrasonic irradiation device of grooved, also can use other ultrasonic unit.The ultra-sonic oscillation time is relevant to the power stage of instrument, if irradiation time is shorter, makes dispersion become insufficient; Otherwise if irradiation time is longer, then the structure of multi-walled carbon nano-tubes can sustain damage, and affects the intrinsic property of multi-walled carbon nano-tubes.
Wherein, operation III dispersion liquid obtained in operation II is carried out centrifugation and reclaims the operation of supernatant liquor.This is the multi-walled carbon nano-tubes in order to stable dispersion non-in removal step II.And if centrifugation is excessively strong, then dispersed multi-walled carbon nano-tubes is also removed.Otherwise if excessively weak, this can not remove the multi-walled carbon nano-tubes not having to disperse.Therefore, preferably carry out centrifugal with the condition of 4000 ~ 6000rpm.By this operation III, the single multi-walled carbon nano-tubes dispersion liquid that can more uniformly be disperseed.
The present invention adopts richness to strangle alcohol as tensio-active agent, the multi-walled carbon nano-tubes of purifying is disperseed, a kind of uniform and stable single-root carbon nano-tube dispersion liquid is prepared by mixing, ultrasonic, centrifugal three-procedure, this will expand the Application Areas of carbon nanotube further, particularly significant in the development in the field such as nano electron device, nano composite material to it.
Accompanying drawing explanation
Fig. 1 is comparative example 1(a) and embodiment 1(b) multi-walled carbon nano-tubes SEM comparison diagram.As seen from the figure, the carbon tube-surface impurity after substep liquid-phase oxidation process obviously reduces, and dispersiveness also increases simultaneously
Fig. 2 is the multi-walled carbon nano-tubes Raman spectrogram comparison diagram of comparative example 1 and embodiment 1.As seen from the figure, the purity of the multi-walled carbon nano-tubes of purifying promotes to some extent, meets the intensity that 0<(the 1st absorbs) technical requirements of/(the 2nd absorb intensity) <1.
Fig. 3 is the multi-walled carbon nano-tubes infrared spectra comparison diagram of comparative example 1 and embodiment 1.As seen from the figure, the multi-walled carbon nano-tubes functionalisation of surfaces oxy radical such as hydroxyl, carboxyl of purifying.
Fig. 4 is that embodiment 1 is to 4(a to d) multi-walled carbon nano-tubes SEM comparison diagram in dispersion liquid.Use sodium hydroxide solution as pretreating reagent, after coordinating the mixed acid solution of concentrated nitric acid/vitriol oil to carry out distribution purification, then richness is strangled alcohol as tensio-active agent, the dispersing property of the multi-walled carbon nano-tubes obtained is best.
Fig. 5 is comparative example 2 and 3(a and multi-walled carbon nano-tubes SEM comparison diagram b).Known, use richness to strangle under alcohol will be better than same case greatly as the dispersing property of the carbon pipe dispersion liquid prepared by tensio-active agent and use Sodium dodecylbenzene sulfonate and polyvinylpyrrolidone as the dispersion liquid obtained by tensio-active agent.
Embodiment
embodiment 1
The preparation of single multi-walled carbon nano-tubes dispersion liquid:
Operation I: get 0.05g nitrating multi-walled carbon nano-tube and add in 2MNaOH solution, 40 DEG C of reflux 12h; Then pretreated multi-walled carbon nano-tubes is joined ultrasonic 30min in concentrated nitric acid/vitriol oil (volume ratio 1:3) mixed acid solution, filter after neutral with deionized water wash, dry, reclaim the multi-walled carbon nano-tubes obtaining purifying; The scanning electronic microscope result of the multi-walled carbon nano-tubes of this purifying is shown in Fig. 1 (b).In addition, Raman mensuration (INVIA-Reflex, Reinshaw 514.5nmAr are carried out to the multi-walled carbon nano-tubes of purifying
+the burnt micro-Raman spectroscopy of ion laser copolymerization), result shows that ID/IG is that 0.83(is with reference to Fig. 2).And carry out infrared measurement (TENSOR27, Brooker Fourier infrared spectrograph) to the multi-walled carbon nano-tubes of purifying, result shows at the carbon tube-surface oxy radical such as functionalized hydroxyl, carboxyl (with reference to Fig. 3).
Operation II: by the multi-walled carbon nano-tubes 10mg of the purifying as above obtained, richness strangles alcohol 4mg, sodium hydroxide 0.1mg, methyl alcohol 10ml mixes (or not adding sodium hydroxide, other same aforementioned base materials).
Use ultrasonic unit (KQ-500DE, Kunshan Ultrasonic Instruments Co., Ltd.), ultrasonic wave dispersion is carried out to the mixed solution obtained through above-mentioned operation I.Thus, multi-walled carbon nano-tubes dispersion liquid is obtained.
Operation III: use centrifuge separator (TG16-WGS, Xiang Zhi centrifugal apparatus company limited), implements centrifugation operation to the single multi-walled carbon nano-tubes dispersion liquid obtained in above-mentioned operation 2.The condition of centrifugation is 5000rpm(or 4000,6000rpm) under carry out 30min.Then, the supernatant liquor after centrifugation is reclaimed; Scanning electronic microscope sign is carried out to it, the results are shown in Fig. 4 (a).From its result, obtain the single multi-walled carbon nano-tubes of dispersion.
comparative example 1
Compared with embodiment 1, except operation I being become 0.05g nitrating multi-walled carbon nano-tube directly and except 10ml methanol mixed, other are with embodiment 1, obtain single multi-walled carbon nano-tubes dispersion liquid.Further, the scanning electronic microscope characterization result of single multi-walled carbon nano-tubes dispersion liquid is as shown in Fig. 1 (a), and Raman measures as shown in Figure 2, and infrared measurement as shown in Figure 3.
embodiment 2
Compared with embodiment 1, except the salpeter solution that alkaline pretreating reagent is become 2.6M from the sodium hydroxide solution of 2M, other are with embodiment 1, obtain single multi-walled carbon nano-tubes dispersion liquid.Further, the scanning electronic microscope characterization result of single multi-walled carbon nano-tubes dispersion liquid as shown in Figure 4 (b).
embodiment 3
Compared with embodiment 1, except the hydrochloric acid soln that alkaline pretreating reagent is become 4M from the sodium hydroxide solution of 2M, other are with embodiment 1, obtain single multi-walled carbon nano-tubes dispersion liquid.Further, the scanning electronic microscope characterization result of single multi-walled carbon nano-tubes dispersion liquid as shown in Figure 4 (c).
embodiment 4
Compared with embodiment 1, except the superoxol that alkaline pretreating reagent is become 30% from the sodium hydroxide solution of 2M, other are with embodiment 1, obtain single multi-walled carbon nano-tubes dispersion liquid.Further, the scanning electronic microscope characterization result of single multi-walled carbon nano-tubes dispersion liquid is as shown in Fig. 4 (d).
comparative example 2
Compared with embodiment 1, become except Sodium dodecylbenzene sulfonate except tensio-active agent is strangled alcohol from richness, other are with embodiment 1, obtain single multi-walled carbon nano-tubes dispersion liquid.Further, the scanning electronic microscope characterization result of single multi-walled carbon nano-tubes dispersion liquid is as shown in Fig. 5 (a).
comparative example 3
Compared with embodiment 1, strangle alcohol from richness become except polyvinylpyrrolidone except being had by tensio-active agent, other are with embodiment 1, obtain single multi-walled carbon nano-tubes dispersion liquid.Further, the scanning electronic microscope characterization result of single multi-walled carbon nano-tubes dispersion liquid is as shown in Fig. 5 (b).
Claims (4)
1. single multi-walled carbon nano-tubes dispersion liquid, is characterized in that, is to strangle by the multi-walled carbon nano-tubes of 1g/L, the richness of 0.4g/L the polar solvent that alcohol and pH be more than or equal to 7 to form.
2. single multi-walled carbon nano-tubes dispersion liquid according to claim 1, is characterized in that, described polar solvent is sodium hydrate methanol solution, and wherein the concentration of sodium hydroxide is 0.01g/L.
3. the preparation method of single multi-walled carbon nano-tubes dispersion liquid described in claim 1 or 2, is characterized in that,
Operation I: multi-walled carbon nano-tubes is added in alkaline pretreating reagent, 40 DEG C of reflux 12h; Then pretreated multi-walled carbon nano-tubes is joined ultrasonic 30min in concentrated nitric acid/vitriol oil mixed acid solution that volume ratio is 1:3, filter after neutral with deionized water wash, dry, reclaim the multi-walled carbon nano-tubes obtaining purifying;
Operation II: the multi-walled carbon nano-tubes of purifying, richness strangle alcohol and polar solvent mixes, adopts ultrasonic vibration dispersion, obtains multi-walled carbon nano-tubes dispersion liquid;
Operation III: carry out centrifugation 30min to the multi-walled carbon nano-tubes dispersion liquid that operation II obtains, rotating speed is 4000 ~ 6000r/min, reclaims the supernatant liquor after centrifugation, obtains single multi-walled carbon nano-tubes dispersion liquid.
4. the preparation method of single multi-walled carbon nano-tubes dispersion liquid according to claim 3, it is characterized in that, preferred alkaline pretreating reagent is the sodium hydroxide solution of 2M.
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CN112126217A (en) * | 2020-10-12 | 2020-12-25 | 广东工业大学 | Fullerene/carbon nanotube/thermoplastic resin composite film, and preparation method and application thereof |
CN113004052A (en) * | 2021-02-07 | 2021-06-22 | 沈阳中钛装备制造有限公司 | Multi-walled carbon nanotube toughened boron carbide-based ceramic material and preparation method and application thereof |
CN113003565A (en) * | 2021-03-31 | 2021-06-22 | 三棵树(上海)新材料研究有限公司 | Preparation method of easily-dispersible micron-sized multi-walled carbon nanotube |
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CN113004052A (en) * | 2021-02-07 | 2021-06-22 | 沈阳中钛装备制造有限公司 | Multi-walled carbon nanotube toughened boron carbide-based ceramic material and preparation method and application thereof |
CN113004052B (en) * | 2021-02-07 | 2022-06-17 | 沈阳中钛装备制造有限公司 | Multi-walled carbon nanotube toughened boron carbide-based ceramic material and preparation method and application thereof |
CN113003565A (en) * | 2021-03-31 | 2021-06-22 | 三棵树(上海)新材料研究有限公司 | Preparation method of easily-dispersible micron-sized multi-walled carbon nanotube |
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