CN102953150B - Preparation of fullerene micro-nano fiber in volatilization and diffusion ways - Google Patents
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- XMWRBQBLMFGWIX-UHFFFAOYSA-N C60 fullerene Chemical compound C12=C3C(C4=C56)=C7C8=C5C5=C9C%10=C6C6=C4C1=C1C4=C6C6=C%10C%10=C9C9=C%11C5=C8C5=C8C7=C3C3=C7C2=C1C1=C2C4=C6C4=C%10C6=C9C9=C%11C5=C5C8=C3C3=C7C1=C1C2=C4C6=C2C9=C5C3=C12 XMWRBQBLMFGWIX-UHFFFAOYSA-N 0.000 title claims abstract description 98
- 229910003472 fullerene Inorganic materials 0.000 title claims abstract description 97
- 238000009792 diffusion process Methods 0.000 title claims abstract description 11
- 238000002360 preparation method Methods 0.000 title abstract description 19
- 239000002121 nanofiber Substances 0.000 title abstract 5
- 239000002904 solvent Substances 0.000 claims abstract description 23
- 239000000463 material Substances 0.000 claims abstract description 11
- 239000000835 fiber Substances 0.000 claims description 32
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Natural products CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 19
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical group CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 15
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 12
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 6
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 5
- 239000012046 mixed solvent Substances 0.000 claims description 5
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 4
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 4
- QGJOPFRUJISHPQ-NJFSPNSNSA-N carbon disulfide-14c Chemical compound S=[14C]=S QGJOPFRUJISHPQ-NJFSPNSNSA-N 0.000 claims description 3
- 239000002707 nanocrystalline material Substances 0.000 claims description 3
- 239000002131 composite material Substances 0.000 claims description 2
- 238000002425 crystallisation Methods 0.000 claims description 2
- 230000008025 crystallization Effects 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims description 2
- 238000007789 sealing Methods 0.000 claims description 2
- 125000003944 tolyl group Chemical group 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 238000005411 Van der Waals force Methods 0.000 claims 1
- 210000003298 dental enamel Anatomy 0.000 claims 1
- -1 enamel Substances 0.000 claims 1
- 239000011521 glass Substances 0.000 claims 1
- 229910001220 stainless steel Inorganic materials 0.000 claims 1
- 239000010935 stainless steel Substances 0.000 claims 1
- 238000001132 ultrasonic dispersion Methods 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 14
- 239000002994 raw material Substances 0.000 abstract description 5
- 239000003054 catalyst Substances 0.000 abstract description 4
- 239000002086 nanomaterial Substances 0.000 abstract description 3
- 238000009776 industrial production Methods 0.000 abstract description 2
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- 230000003287 optical effect Effects 0.000 description 6
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- 238000011161 development Methods 0.000 description 3
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- 239000004570 mortar (masonry) Substances 0.000 description 3
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- 238000000151 deposition Methods 0.000 description 2
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- 238000005516 engineering process Methods 0.000 description 2
- 238000011534 incubation Methods 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 239000002071 nanotube Substances 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 230000010355 oscillation Effects 0.000 description 2
- 238000010526 radical polymerization reaction Methods 0.000 description 2
- 230000003252 repetitive effect Effects 0.000 description 2
- 238000012827 research and development Methods 0.000 description 2
- XINQFOMFQFGGCQ-UHFFFAOYSA-L (2-dodecoxy-2-oxoethyl)-[6-[(2-dodecoxy-2-oxoethyl)-dimethylazaniumyl]hexyl]-dimethylazanium;dichloride Chemical group [Cl-].[Cl-].CCCCCCCCCCCCOC(=O)C[N+](C)(C)CCCCCC[N+](C)(C)CC(=O)OCCCCCCCCCCCC XINQFOMFQFGGCQ-UHFFFAOYSA-L 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 229940088710 antibiotic agent Drugs 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
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- 238000002848 electrochemical method Methods 0.000 description 1
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- 230000009881 electrostatic interaction Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 229920001002 functional polymer Polymers 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
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Abstract
The invention relates to a preparation method for a fullerene micro-nano fiber. The fullerene micro-nano fiber refers to a one-dimensional fullerene micro-nano material formed by connecting fullerene molecules through intermolecular acting force. According to the method, the fullerene micro-nano fiber is prepared by standing a fullerene solution and a poor solvent in a closed system and utilizing the volatilization and diffusion function of the solvent. The method is simple, easy, high in repetition rate and suitable for industrial production, and raw materials can be recycled. The fullerene micro-nano fiber has potential wide application value in the fields of material science, electronics, optics, biomedicine, catalysts, energy resources, environments and the like.
Description
Technical field
The present invention relates to the preparation method of fullerene micro nanometer fiber.
Background technology
Low-dimensional micro-nano carbon cellulosic material is the size of physical property and the ideal systems of latitude effect such as the behavior of research electric transmission, optical characteristics and mechanical property, by serving as key player in the process constructing the integrated circuits such as micro-nano electronics and opto-electronic device and functional element, become forward position and the focus of current micro Nano material scientific domain.
Fullerene refers to the ball-type of the hollow being comprised of carbon, spheroid shape, the general name of cylindricality or tracheary element.Broader definition can comprise the fullerene molecule of embed fullerene or other functional group modification.Fullerene micro nanometer fiber is a kind of in the micro-nano crystal of fullerene, refers in particular to and by fullerene molecule, by intermolecular force, is interconnected the fullerene micro Nano material of the one dimension forming.
Kroto equals successfully to have confirmed for 1985 the first fullerene, i.e. the existence of [60] fullerene molecule, and inferred in theory C
60football shaped carbon basket structure.Fullerene molecule has the symmetry of height and the pi-electron conjugated system of spherical delocalization, makes its physicochemical properties unique.The unusual optical physics of fullerene, electric conductivity, photoconductivity and light are restricted driving as causing the very big interest of scientists.Through the research of two more than ten years, risen the new subjects such as organic fullerene chemistry, fullerene supramolecular chemistry, TXEndohedral Metallofullerenes, fullerene pharmaceutical chemistry, fullerene photoelectricity magnetics, and in continuous development.
Fullerene micro nanometer fiber, not only has C
60the character of monomer, the size of its micro/nano level and the pattern of one dimension, make also have high specific area, and the feature such as quantum limitation effect.In mechanical property, fullerene micro nanometer fiber and original C
60crystal is compared, and has had higher Young's modulus.On optical properties, they have shown extremely strong photoluminescence property, and have the phenomenon that shows blue shift along with diameter is reduced.On electrical properties, Takeya etc. are by K element is inlaid in fullerene micro nanometer fiber, and have prepared the material with superconducting property, etc.Its many special nature makes it at material, electronics, and optics, biological medicine, catalyst, there is potential application widely in the fields such as the energy and environment.
Because fullerene micro nanometer fiber character is special, application potential is huge, and the research and development of its preparation method have also caused that people study interest widely.About the preparation research of the micro-nano crystal of fullerene, can review from nineteen ninety the earliest (W.Kratschmer, L.D.Lamb, K.Fostiropoulos and D.R.Huffman, the Solid C such as Kratschmer
60: a new form of carbon, Nature, 1990,347:354), just by the method for single vaporization fullerene-benzole soln, prepared the micro-nano stub of fullerene and wafer.It is simple that evaporation is prepared the micro-nano crystal of fullerene, before reprecipitation method exploitation, is the unique method of preparing the micro-nano crystal of fullerene, and obtains people's extensive concern.In addition, because the method can be for the optical property of research fullerene, therefore use till today always, (the M.G.Yao such as Liu, B.M.Andersson, P.Stenmark, B.Sundqvist, B.B.Liu, T.Wagberg, Carbon, 2009,47:1181) by simple evaporation, pass through to use different solvents, different evaporating temperatures is prepared the fullerene nano and micro materials of different dimensions.
Also have a lot of other methods of preparing fullerene micro nanometer fiber to be researched and developed, as (V.Georgakilas such as Prato, V.F.Pellarini, M.Prato, D.M.Guldi, M.Melle-Franco and F.Zerbetto, Proc.Natl.Acad.Sci.U.S.A., 2002,99:5075) reported a kind of Ionized C containing porphyrin unit
60derivative can form nanotube, and think that this is that π due to fullerene and porphyrin-π interacts, due to self assembly and electrostatic interaction.Chinese patent: CN 1195103; CN 1215973 discloses and has utilized electrochemical method to make the aggregation electrophoresis of fullerene in the nano-void of foraminous die plate, thereby forms orderly micro-nano mitron and the method for micro-nano whisker.Chinese patent: CN1267342C discloses the C being obtained by template contral radical polymerization
60the C that intermolecular covalent bond connects
60one dimension condensate nanotube, its radical polymerization is that absorption is had to monomer C
60the template of molecule maintains 2-4 hour, 1 kilowatt of ultraviolet lighting 0.5-1 hour in 400-550 ℃ under inert gas shielding.Japanese laid-open patent: 2005-254393A, 2006-124266A is near room temperature C
60saturated organic solution and the liquid-liquid interface deposition method of isopropyl alcohol successfully prepared the fullerene C with mono-crystalline structures
60micro-nano whisker and micro-nano mitron.101148256 pairs of liquid-liquid interface deposition methods of Chinese patent: CN have carried out further exploitation, and its repetitive rate is improved greatly.
But it should be noted that the micro-nano crystal amount of fullerene prepared by evaporation is few, and have and be difficult to wash out and do not destroy the shortcoming of its pattern from substrate surface, and only can be applicable to scientific research, be not suitable for large-scale production.And there is the problems such as complicated process of preparation in electrochemical process and template rule.Liquid-liquid interface rule is serious to organic solvent waste, and these organic solvents are to human health, and the harm of living environment is serious.In order better to adapt to the demand of more diversified fullerene crystal material, the nanocrystal novel preparation method that more can cater to the strategy of sustainable development is provided, extremely urgent for new fullerene micro nanometer fiber preparation method's research and development.
Summary of the invention
The object of the invention is to expand the preparation method of fullerene micro nanometer fiber, and the nanocrystal novel preparation method that more can cater to the strategy of sustainable development is provided, and through inventor, is engaged in for a long time C
60developmental research and market demand investigation, develop a kind of simple, reproducible, raw material can reuse, be applicable to preparing in a large number fullerene micro nanometer fiber without template novel preparation method.
With, be applicable to preparing in a large number fullerene micro nanometer fiber without template novel preparation method.
The preparation method of fullerene nano micron fibre provided by the invention, comprises the steps:
1) prepare fullerene solution: by fullerene material in mortar for example in agate mortar, be ground to metallic luster, with a small amount of fullerene good solvent, as adding in mortar, toluene, benzene, dimethylbenzene, carbon disulfide, carbon tetrachloride, dichlorotoleune etc. or its mixed solvent dissolve after fullerene, move in vial, then, after using ultrasonic wave as 50-500W ultrasonic oscillation, under room temperature, filter to obtain fullerene solution.
2) step 1) open-top receptacle of the fullerene solution prepared is statically placed in the larger container that fills fullerene poor solvent, and keep the height of poor solvent liquid level low compared with the open-top receptacle mouth of fullerene solution, in case poor solvent flows in open-top receptacle.
3) then, step 2) in standing cultivation under larger container sealing, constant temperature.After standing a couple of days, the fullerene micro nanometer fiber of crystallization micron order or grade length in fullerene solution.
In the preparation method of fullerene micro nanometer fiber provided by the invention, described fullerene is C
60, C
70(C
60, C
70purity is 98-99.9%), C
60/ C
70mixture and derivative thereof are (as C
60[C (OOC
2h
5)
2]) and high carbon number fullerene (as C
82, C
84, C
100, C
110... C
540).Described fullerene micro nanometer fiber is the micro-nano crystalline material of fullerene that above-mentioned fullerene monomer connects into by intermolecular force.
Described step 1) in, good solvent is toluene, benzene, dimethylbenzene, carbon disulfide, carbon tetrachloride, pyridine etc. or its mixed solvent.
Described step 2) in, poor solvent is isopropyl alcohol, methyl alcohol, ethanol, acetone, water etc. or its mixed solvent.
The preparation method of fullerene micro nanometer fiber provided by the invention is according to needs, regulate concentration and the consumption of fullerene solution, the consumption of poor solvent, container volume size, standing incubation time, the process conditions such as temperature, prepare the fullerene micro nanometer fiber of different draw ratios and the micro-nano crystalline material of fullerene of other dimensions.
Preparation method's difference with the prior art of fullerene micro nanometer fiber provided by the invention is: preparation technology is simple, and repetitive rate is high, and raw material can reuse, and fiber pattern controllability is strong, can be used for large-scale industrial production.
1. the advantages such as device required for the present invention is only two containers, belongs to without method for preparing template, has simple economy, easy to operate, reliable and stable.
In raw material of the present invention the good solvent that uses and poor solvent can recycle, reduce largely the wasting of resources and environmental pollution.
3. the present invention relates to regulate and control many factors, as the concentration of fullerene solution and consumption, the consumption of poor solvent, container volume size, standing incubation time, the process conditions such as temperature, though develop at present limitedly, can be applicable to the preparation of different size fullerene micro nanometer fiber.
4. the prepared product of the present invention is to have the fullerene material of conjugated pi electron structure as the new aggregated structure of fullerene family, both the structure and the character that had kept fullerene molecule, the feature again with one-dimensional material, its excellent properties makes it in fields such as micro-nano device, a transmitter, catalyst or catalyst carrier, fuel cell electrode, solar cell, limited chemical reaction field, high frequency filter, functional polymer composites, anti-biotic materials, will have potential widely application prospect.
Accompanying drawing explanation
Fig. 1 is that volatilization diffusion method is prepared fullerene micro nanometer fiber experimental provision schematic diagram;
Fig. 2 is the optical microscope photograph of the fullerene micro nanometer fiber prepared of volatilization diffusion method;
Fig. 3 is the electron scanning micrograph of the fullerene micro nanometer fiber prepared of volatilization diffusion method, and wherein b figure is the partial enlarged drawing of a figure.
The specific embodiment
The present invention further illustrates technical characterictic of the present invention with the following example, but protection scope of the present invention is not limited to the following example.
Embodiment 1
1. take 3mg C
60powder is in 15ml vial, and purity is 99.9%, and commercially available prod is got 6ml toluene with graduated cylinder and added in vial.
2. by above-mentioned C
60-toluene solution is put into ultrasonic container, at ambient temperature with 50W power ultrasonic concussion 10min, to make C
60be well dispersed in toluene solution.
3. after ultrasonic oscillation, by above-mentioned C
60-toluene solution and vial in unsealing situation, are put into the 100ml vial that fills 25ml isopropyl alcohol in the lump, and assurance isopropyl alcohol can not overflow into and fill C
60in the vial of-toluene.Experimental provision schematic diagram, is shown in Fig. 1.
4. standing in room temperature (25 ℃) environment, after a couple of days, in the suspension of upper strata, can obtain length in micron-sized fiber, its optical microscope photograph is shown in Fig. 2, electron scanning micrograph is shown in Fig. 3.
Embodiment 2
Embodiment 2 is identical with embodiment 1 step, but difference is preparation C
60in solution, the amount of toluene is 7ml.
Embodiment 3
Embodiment 3 is identical with embodiment 1 step, but difference is poor solvent, selects 1-propyl alcohol.
Embodiment 4
Embodiment 4 is identical with embodiment 1 step, but difference is poor solvent consumption, is 30ml.
Embodiment 5
Embodiment 5 is identical with embodiment 1 step, but difference is the C that is used for preparation
60the good solvent of solution is selected as benzene.
Embodiment 6
Embodiment 6 is identical with embodiment 1 step, but difference is to disperse C
60solution is not used ultrasonic, and uses the mode of manually rocking to disperse.
Embodiment 7
Embodiment 7 is identical with embodiment 1 step, does not select room temperature, and select 50 ℃ but difference is dwell temperature.
Embodiment 8
Embodiment 8 is identical with embodiment 1 step, but difference be raw materials used be not C
60, and make C
60/ C
70mixed-powder.
Claims (5)
1. volatilization diffusion method is prepared fullerene micro nanometer fiber, it is characterized in that comprising the following steps:
1) prepare fullerene solution: after fullerene material is ground, be dissolved in the good solvent of fullerene, through ultrasonic dispersion, form fullerene solution; The concentration of its fullerene solution is fullerene material: good solvent=3mg:6 or 7mL;
2) step 1) made fullerene solution injects in open-top receptacle;
3) step 2) open-top receptacle of the fullerene solution prepared is statically placed in the larger container that fills fullerene poor solvent, and keep poor solvent liquid level low compared with the open-top receptacle mouth of fullerene solution, in case poor solvent flows in open-top receptacle;
4) then, step 3) in larger container sealing, under-5 ℃ of-60 ℃ of constant temperature after standing cultivation a couple of days, the fullerene micro nanometer fiber of crystallization micron order or grade length in fullerene solution.
2. volatilization diffusion method according to claim 1 is prepared fullerene micro nanometer fiber, it is characterized in that described fullerene is C
60, C
70, C
60/ C
70mixture and derivative thereof, embed fullerene and high carbon number fullerene; Described fullerene micro nanometer fiber refers to that above-mentioned fullerene molecule is by covalent bond, the micro-nano crystalline material of one dimension fullerene that ionic bond or Van der Waals force are interconnected to.
3. volatilization diffusion method according to claim 1 is prepared fullerene micro nanometer fiber, it is characterized in that described good solvent is toluene, benzene, dimethylbenzene, carbon disulfide, carbon tetrachloride, pyridine or its mixed solvent.
4. volatilization diffusion method according to claim 1 is prepared fullerene micro nanometer fiber, it is characterized in that described poor solvent is isopropyl alcohol, 1-propyl alcohol, methyl alcohol, ethanol, acetone, water or its mixed solvent.
5. volatilization diffusion method according to claim 1 is prepared fullerene micro nanometer fiber, it is characterized in that described container is glass, enamel, stainless steel, composite material vessel.
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| CN103147155A (en) * | 2013-04-08 | 2013-06-12 | 福建师范大学 | Preparation method of conjugated polymer nanofiber with crosslinking group |
| CN103408931B (en) * | 2013-05-29 | 2015-07-01 | 青岛科技大学 | Preparation method of hybrid material compounded from fullerene micro-nano material and conjugated polymer |
| CN103879984A (en) * | 2014-02-19 | 2014-06-25 | 东华大学 | Method for preparing fullerene self-assemble structure through solvent atmosphere control |
| CN107236223A (en) * | 2017-07-20 | 2017-10-10 | 太仓市格雷得五金有限公司 | A kind of corrosion-resistant biodegradable polymer of antibacterial and preparation method thereof |
| CN108889291B (en) * | 2018-06-13 | 2020-10-23 | 中国科学院化学研究所 | SnO2Modified fullerene composite material with micro-nano structure and preparation method and application thereof |
| CN109111714A (en) * | 2018-07-25 | 2019-01-01 | 四川龙华光电薄膜股份有限公司 | Silver nanowires modified fullerenes micro/nano-fibre, preparation method and applications |
| CN110016712B (en) * | 2019-04-25 | 2020-07-28 | 大连民族大学 | Fullerene C70-calixarene host-guest composite nanocrystalline material and preparation method thereof |
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| JP4595110B2 (en) * | 2004-03-23 | 2010-12-08 | 独立行政法人物質・材料研究機構 | Needle-like crystal having a hollow structure composed of fullerene molecules and method for producing the same |
| CN100581998C (en) * | 2007-08-30 | 2010-01-20 | 青岛科技大学 | Method for preparing fullerenes nano micron fibre |
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