CN102953150A - Preparation of fullerene micro-nano fiber in volatilization and diffusion ways - Google Patents
Preparation of fullerene micro-nano fiber in volatilization and diffusion ways Download PDFInfo
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- CN102953150A CN102953150A CN2012104554036A CN201210455403A CN102953150A CN 102953150 A CN102953150 A CN 102953150A CN 2012104554036 A CN2012104554036 A CN 2012104554036A CN 201210455403 A CN201210455403 A CN 201210455403A CN 102953150 A CN102953150 A CN 102953150A
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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 94
- 229910003472 fullerene Inorganic materials 0.000 title claims abstract description 93
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 238000009792 diffusion process Methods 0.000 title claims abstract description 7
- 239000002121 nanofiber Substances 0.000 title abstract 5
- 239000002904 solvent Substances 0.000 claims abstract description 24
- 239000000463 material Substances 0.000 claims abstract description 10
- 239000000835 fiber Substances 0.000 claims description 28
- 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
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- -1 enamel Substances 0.000 claims description 2
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- 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
- 239000011521 glass Substances 0.000 claims 1
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- 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
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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 the physical propertys such as the behavior of research electric transmission, optical characteristics and mechanical property and the ideal system of latitude effect, to in the process of constructing the integrated circuits such as micro-nano electronics and opto-electronic device and functional element, serve as the key player, become forward position and the focus of current micro Nano material scientific domain.
Fullerene refers to the ball-type of the hollow that is comprised of carbon, spheroid shape, the general name of cylindricality or tracheary element.Broader definition then can comprise the fullerene molecule of embed fullerene or other functional group modification.The fullerene micro nanometer fiber is a kind of in the micro-nano crystal of fullerene, refers in particular to the fullerene micro Nano material that is interconnected the one dimension that forms by fullerene molecule by intermolecular force.
Kroto has equaled successful confirmation in 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.
The 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 to have high specific area, and the characteristics such as quantum limitation effect.On mechanical property, fullerene micro nanometer fiber and original C
60Crystal is compared, and has had higher Young's modulus.On optical properties, they have showed extremely strong photoluminescence property, and the phenomenon that shows blue shift along with diameter is reduced is arranged.On electrical properties, Takeya etc. are by being inlaid into the K element in the 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 widely potential application 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 caused that also 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 prepares the micro-nano crystal of fullerene, before the reprecipitation method exploitation, is the unique method of the micro-nano crystal of preparation fullerene, and obtains people's extensive concern.In addition, because the method can be used for the optical property of research fullerene, so 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) pass through to use different solvents with simple evaporation, different evaporating temperatures is prepared the fullerene nano and micro materials of different dimensions.
Also have a lot of other methods that prepare the fullerene micro nanometer fiber to obtain research and development, such 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 that contains the porphyrin unit
60Derivative can form nanotube, and think that this is because the π of fullerene and porphyrin-π interacts, due to self assembly and electrostatic interaction.Chinese patent: CN 1195103; CN 1215973 disclose utilize electrochemical method to make fullerene the aggregation electrophoresis in the nano-void of foraminous die plate, thereby form orderly micro-nano mitron and the method for micro-nano whisker.Chinese patent: CN1267342C discloses the C that is obtained by template contral radical polymerization
60The C that intermolecular covalent bond connects
60One dimension condensate nanotube, its radical polymerization are that absorption is had monomer C
60The template of molecule was kept 2-4 hour in 400-550 ℃ under inert gas shielding, 1 kilowatt ultraviolet lighting 0.5-1 hour.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 the micro-nano crystal amount of fullerene that it should be noted that evaporation preparation is few, and has 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, is not suitable for large-scale production.And there are the problems such as complicated process of preparation in electrochemical process and template rule.The 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 that more can cater to strategy of sustainable development novel preparation method 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 that more can cater to strategy of sustainable development novel preparation method is provided, and is engaged in for a long time C through the inventor
60Developmental research and market demand investigation, develop a kind of simple, good reproducibility, raw material can reuse, be fit to a large amount of preparation fullerene micro nanometer fibers without the template novel preparation method.
The preparation method of fullerene nano micron fibre provided by the invention comprises the steps:
1) preparation fullerene solution: with the fullerene material in mortar for example in the agate mortar, be ground to metallic luster, add in mortar behind the dissolving fullerene with a small amount of fullerene good solvent such as toluene, benzene, dimethylbenzene, carbon disulfide, carbon tetrachloride, dichlorotoleune etc. or its mixed solvent, move in the vial, then after using ultrasonic wave such as 50-500W ultrasonic oscillation, filter to get fullerene solution under the room temperature.
2) step 1) open-top receptacle of the fullerene solution prepared is statically placed in the larger container that fills the fullerene poor solvent, and keep the height of poor solvent liquid level low than the open-top receptacle mouth of fullerene solution, in case poor solvent flows in the open-top receptacle.
3) then, step 2) in leave standstill cultivation under the larger container sealing, constant temperature.After leaving standstill a couple of days, the fullerene micro nanometer fiber of crystallization micron order or grade length in fullerene solution.
Among the preparation method according to 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 (such as C
60[C (OOC
2H
5)
2]) and high carbon number fullerene (such 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) good solvent is toluene, benzene, dimethylbenzene, carbon disulfide, carbon tetrachloride, pyridine etc. or its mixed solvent in.
Described step 2) poor solvent is isopropyl alcohol, methyl alcohol, ethanol, acetone, water etc. or its mixed solvent in.
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, the container volume size, leave standstill 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 only is two containers, belongs to without method for preparing template, has simple economy, and is easy to operate, reliable and stable.
In the 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, such as concentration and the consumption of fullerene solution, the consumption of poor solvent, the container volume size leaves standstill 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, fullerene molecular structures and character had both been kept, the characteristics that have again one-dimensional material, its excellent properties make 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 potential widely application prospect will be arranged.
Description of drawings
Fig. 1 is that the volatilization diffusion method prepares fullerene micro nanometer fiber experimental provision schematic diagram;
Fig. 2 is the optical microscope photograph of the fullerene micro nanometer fiber of volatilization diffusion method preparation;
Fig. 3 is the electron scanning micrograph of the fullerene micro nanometer fiber of volatilization diffusion method preparation, and wherein b figure is the partial enlarged drawing of a figure.
The specific embodiment
The present invention further specifies 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 by weighing 3mgC
60Powder is in the 15ml vial, and purity is 99.9%, and the commercially available prod is got 6ml toluene with graduated cylinder and added in the vial.
2. with above-mentioned C
60-toluene solution is put into ultrasonic container, at ambient temperature with 50W power ultrasonic concussion 10min, in order to make C
60Be well dispersed in the toluene solution.
Ultrasonic oscillation complete after, with above-mentioned C
60-toluene solution and vial in the unsealing situation, are put into the 100ml vial that fills the 25ml isopropyl alcohol in the lump, and the assurance isopropyl alcohol can not overflow into and fill C
60In the vial of-toluene.The experimental provision schematic diagram is seen Fig. 1.
4. leave standstill in room temperature (25 ℃) environment, after a couple of days, can get length in the suspension of upper strata and be in micron-sized fiber, its optical microscope photograph is seen Fig. 2, and electron scanning micrograph is seen Fig. 3.
Embodiment 2
Embodiment 2 is identical with embodiment 1 step, but difference is preparation C
60The amount of toluene is 7ml in the solution.
Embodiment 3
Embodiment 3 is identical with embodiment 1 step, selects the 1-propyl alcohol but difference is poor solvent.
Embodiment 4
Embodiment 4 is identical with embodiment 1 step, is 30ml but difference is the poor solvent consumption.
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 and is benzene.
Embodiment 6
Embodiment 6 is identical with embodiment 1 step, but difference is to disperse C
60Solution does not use 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 but difference is dwell temperature, and selects 50 ℃.
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 (6)
1. the volatilization diffusion method prepares the fullerene micro nanometer fiber, comprises the following steps:
1) preparation fullerene solution: after the grinding of fullerene material, be dissolved in the good solvent of fullerene, form fullerene solution through ultrasonic dispersion.
2) step 1) made fullerene solution injects in the open-top receptacle.
3) step 2) open-top receptacle of the fullerene solution prepared is statically placed in the larger container that fills the fullerene poor solvent, and keep the poor solvent liquid level low than the open-top receptacle mouth of fullerene solution, in case poor solvent flows in the open-top receptacle.
4) then, step 3) in leave standstill cultivation under the larger container sealing, constant temperature.After leaving standstill a couple of days, the fullerene micro nanometer fiber of crystallization micron order or grade length in fullerene solution.
2. fullerene micro nanometer fiber according to claim 1 is characterized in that described fullerene is C
60, C
70, C
60/ C
70Mixture and derivative thereof are (such as C
60[C (OOC
2H
5)
2]), embed fullerene and high carbon number fullerene be (such as C
82, C
84, C
100, C
110... C
540).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. according to claims 1 described fullerene good solvent, it is characterized in that described good solvent is toluene, benzene, dimethylbenzene, carbon disulfide, carbon tetrachloride, pyridine etc. or its mixed solvent.
4. according to claims 1 described fullerene poor solvent, it is characterized in that described poor solvent is isopropyl alcohol, 1-propyl alcohol, methyl alcohol, ethanol, acetone, water etc. or its mixed solvent.
5. according to claims 1 described container, it is characterized in that described container is the containers such as glass, enamel, stainless steel, composite.
6. according to claims 1 described constant temperature, it is characterized in that described constant temperature is that temperature range is at-5 ℃-60 ℃.
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CN103408931A (en) * | 2013-05-29 | 2013-11-27 | 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 |
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