CN1935638A - Method for preparing carbon nano fiber - Google Patents
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- CN1935638A CN1935638A CN 200510094531 CN200510094531A CN1935638A CN 1935638 A CN1935638 A CN 1935638A CN 200510094531 CN200510094531 CN 200510094531 CN 200510094531 A CN200510094531 A CN 200510094531A CN 1935638 A CN1935638 A CN 1935638A
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Abstract
The invention is a method of preparing carbon nano fibers, characterized in adopting hydrazine hydrate and high molecular surface active agnet polyvinylpyrrolidone to hydrothermally synthesize nano lines of semiconductor Te at 160-200DEG C; then adopting the nano lines as template and adopting carbohydrate to react at 160-220DEG C for 4-20 h and synthesizing carbon-coated Te nano cables as intermediate for preparing carbon nano fiber; and oxidizing to remove Te cores from the nano cables and obtaining the carbon nano fibers. And it avoids production of carbon balls in the carbonizing course, and the surfaces of the obtained carbon-coated Te nano cables and carbon nano fibers all have large numbers of functional groups. And it is relatively suitable for industrialized production.
Description
Technical field:
The invention belongs to the preparation method of nano material technical field, relate to the low-temperature hydrothermal carbonization of sugary carbohydrates, particularly carbon coats the preparation method of tellurium nano-cable and carbon nanofiber.
Background technology:
Britain's " nature material " (Nature Materials,, the 1st volume, 165-168 page or leaf in 2002) has reported and used plasma-catalytic cracking methane under the situation that transition-metal catalyst exists, and can obtain carbon nano fiber in room temperature.The problem for preparing carbon nanofiber to methods such as adopting laser ablation, chemical vapour deposition and plasma enhanced chemical vapor deposition in the past is similar, because reaction is finished under High Temperature High Pressure, the product surface is difficult to functionalization.
Germany " advanced material " (Advanced materials, 2004, the 16th volume, the 1636-1640 page or leaf) reported under 160-200 ℃, silver ions katalysis, carbon source carbonizations such as starch, glucose are formed carbon contracted payment nano-cable, this method unavoidably has a large amount of carbon balls to generate because the reduction of silver and the carbonization of carbon source are carried out simultaneously, and the carbon contracted payment nano-cable product that obtains is fewer.
U.S.'s " carbon " (Carbon, 1998, the 36th volume, 937-942 page or leaf) reported that the carbonization Paraformaldehyde 96 has obtained carbon nanofiber under high temperature (700-850 ℃) high pressure (10 megapascal (MPa)), owing to be to react under comparatively high temps also, its product surface is difficult to functionalization.
Britain's " new chemistry " (New Journal of Chemistry, 2003, the 27th volume, the 1748-1752 page or leaf) reported nano wire and the nanotube of in pure water mixed system, in the different medium of soda acid, having prepared tellurium respectively, because reaction is (＜140 ℃) reaction under the lower temperature of alcohol-water system neutralization, what obtain is that diameter is the tellurium nano-wire of tens nanometers, and diameter is thicker.
Germany's " advanced material " (Advanced materials,, the 16th volume, 1629-1632 page or leaf in 2004) has reported with Lalgine and has reduced HTeO
42H
2O prepares the nano wire of the tellurium of outlet footpath 80nm, because a little less than the reductibility of reductive agent Lalgine, the line footpath that obtains is bigger.
Summary of the invention:
The present invention proposes a kind of method for preparing carbon nanofiber at a lower temperature, to overcome the above-mentioned shortcoming that prior art exists.
This method for preparing carbon nanofiber is characterized in that: the polyvinylpyrrolidone and the 2.2-6.6g/L Na that will contain 8-48g/L earlier
2TeO
3The aqueous solution, with hydrazine hydrate that accounts for reaction system weight 2-4% and the ammoniacal liquor of 1-4%, be sealed in the reaction vessel, in 160-200 ℃ of reaction 4-10 hour, obtain the nano wire of semi-conductor tellurium;
This tellurium nano-wire is enclosed in 160-220 ℃ of reaction 4-20 hour by the 0.1-2.5g/L aqueous solution and saccharide compound 12.5-312.5g/L, and cool to room temperature obtains carbon and coats the tellurium nano-cable;
Carbon is coated the tellurium nano-cable by the 0.1-2.5g/L aqueous solution, add the 0.02-2M/L oxygenant, promptly obtain carbon nanofiber.
Described saccharide compound comprises starch, glucose, beta-cyclodextrin, fructose, maltose or sucrose.
Described oxygenant can be chosen from hydrogen peroxide, nitric acid, potassium bromate, potassium permanganate, Potcrate, sodium borohydride, POTASSIUM BOROHYDRIDE or inferior sodium phosphate oxygenant.
The present invention prepares the intermediate product carbon that obtains in the procedure of carbon nanofiber and coats the tellurium nano-cable, and it is characterized in that: the core of cable is the semi-conductor tellurium of diameter 4-9 nanometer, and what the tellurium core coated outward is that thickness is the amorphous carbon of 6-68 nanometer.
The size of the final product carbon nanofiber that the inventive method prepares is the size decision that is coated the tellurium nano-cable by intermediate product carbon, so can control the size of prepared final product carbon nanofiber by the size of controlling prepared intermediate product carbon bag tellurium nano-cable.
Because the nano wire that the present invention has adopted the semi-conductor tellurium as template, adopts sugary carbohydrates as reaction raw materials, realized that under lower temperature a large amount of synthetic carbon coat the nano-cable of tellurium, have avoided the generation of carbon ball in the carbonization process; The tellurium core that coats the nano-cable of tellurium owing to this carbon is easy to oxidized removing, thereby can be by preparation intermediate product carbon coats the tellurium nano-cable earlier, the tellurium core of nano-cable is removed in oxidation then, obtains carbon nanofiber easily; Because the reaction among the present invention is to carry out under lower temperature (160-220 ℃), saccharide compound charing fully, therefore the surface that prepared carbon coats tellurium nano-cable and carbon nanofiber all has a large amount of functional groups, can carry out functionalization to nano-cable or the carbon nanofiber that carbon coats tellurium according to different application needs, particularly aspect the heterocatalysis, has very high using value at catalytic field as: the catalytic nanometer particle of modifying precious metal; If it is complete at high temperature to continue charing, also having broad application prospects aspect field emission source and the electrode materials; The present invention adopts the sugary carbohydrates be easy to get as raw material, and preparation condition gentleness, operation are simple and easy, and processing requirement is simple, relatively is fit to industrialization and amplifies.
Description of drawings:
Fig. 1 is the stereoscan photograph that carbon coats the tellurium nano-cable;
Fig. 2 is the transmission electron microscope photo that carbon coats the tellurium nano-cable;
Fig. 3 is the stereoscan photograph of carbon nanofiber;
Fig. 4 is the transmission electron microscope photo of carbon nanofiber.
The specific examples mode:
Below in conjunction with embodiment the preparation method of carbon nanofiber of the present invention is done specific description.
Embodiment 1:
The line footpath of prior art synthetic tellurium nano-wire is all bigger, and specific surface area is little.In the present invention, we adopt strong reductive agent (hydrazine hydrate), in the presence of relatively higher temperature of reaction (160-200 ℃) and polymeric surface active agent polyvinylpyrrolidone, first hydro-thermal synthesizes that to have higher specific surface area, line directly be the nano wire of the semi-conductor tellurium of 4-9nm; The nano wire that adopts this semi-conductor tellurium then adopts sugary carbohydrates as template, and synthetic carbon coats the nano-cable of tellurium under lower temperature, as the intermediate product of preparation carbon nanofiber; Reoxidize the tellurium core of removing semi-conductor tellurium nano-cable, finally obtain carbon nanofiber.
With 0.6g polyvinylpyrrolidone and 0.1107g Na
2TeO
3, placing capacity is the reactor of 30ml, adds the 21ml dissolved in distilled water, adds 1ml hydrazine hydrate and 2ml ammoniacal liquor then successively, stirs, and after the reactor sealing, places 160 ℃ of baking ovens, keeps 10 hours; Naturally cool to room temperature, the product that obtains comes out with the 40ml acetone precipitation, cleans multipass with distilled water and dehydrated alcohol successively, obtains the nano wire of semi-conductor tellurium.
Get nano wire 0.01 gram of above-mentioned tellurium, be dispersed in the water of 24ml, add 1.5 gram sucrose, after the stirring and dissolving, transfer in the reactor of 30ml; After the reactor sealing, place 160 ℃ of baking ovens to keep 20 hours; Naturally cool to room temperature; Product is used distilled water and absolute ethanol washing respectively three times, after the drying, obtains the nano-cable that carbon coats tellurium.
The carbon of getting above-mentioned acquisition coats tellurium nano-cable 0.01 gram, is distributed in the 20ml water, adds the 1ml hydrogen peroxide, stirring at room 2 hours.After centrifugation goes out product, use distilled water wash three times, drying promptly obtains carbon nano fiber.
Employed oxidants hydrogen peroxide in the foregoing description also can select for use nitric acid, potassium bromate, potassium permanganate, Potcrate, sodium borohydride, POTASSIUM BOROHYDRIDE or inferior sodium phosphate oxygenant to replace.
Adopt Philip X ' Pert PRO SUPER X-ray diffractometer respectively, field emission scanning electron microscope, the H-8010 of Hitachi transmission electron microscope, fourier transform infrared spectra, Raman spectrum and and x-ray photoelectron spectroscopy sample is characterized.
Show that by transmission electron microscope is observed the nano wire of tellurium the line of the nano wire of tellurium directly is 4-9nm, length can reach tens microns, even up to a hundred microns.
By field emission scanning electron microscope and transmission electron microscope the carbon that obtains in the present embodiment being coated the tellurium nano-cable observes.The stereoscan photograph that the carbon that provides from Fig. 1 coats the tellurium nano-cable is as seen: the diameter that carbon coats tellurium nano-cable sample is 50-80nm, and length can reach tens microns, even up to a hundred microns, and not finding does not have the carbon ball to generate.The transmission electron microscope photo that the carbon that Fig. 2 provides coats the tellurium nano-cable shows: it is the core-shell nano structure that the carbon that is obtained coats tellurium nano-cable sample, the diameter 4-9 nanometer of nuclear, and the end of nuclear all is wrapped and goes up thick carbon-coating, and the thickness of carbon-coating is the 20-38 nanometer.
Adopt photoelectron spectrograph that the result of study that carbon coats the tellurium nano-cable is shown, very weak at the peak of the bonded energy 573eV of Te3d5, almost detect not come out, illustrate that the nano wire of tellurium has been wrapped.
The carbon nanofiber that present embodiment is prepared carries out field emission scanning electron microscope and transmission electron microscope observation, the stereoscan photograph of the carbon nanofiber that Fig. 3 provides shows: the diameter of the carbon nanofiber sample that obtains in the present embodiment is 50-80nm, length can reach tens microns, even up to a hundred microns, do not find the existence of carbon ball; The transmission electron microscope photo of carbon nanofiber shown in Figure 4 shows: the tellurium core that former intermediate product carbon coats the tellurium nano-cable has been fallen the carbon nanofiber diameter 50-80nm of acquisition, tens microns of length by chemical treatment.
Raman study to this carbon nanofiber shows, at 1589cm
-1A tangible peak is arranged, and this is because the C-C stretching vibration of typical graphite-structure causes, shows that sample is that part is graphited; At 1360cm
-1Have one not to be clearly peak, very weak, this is because the C-C stretching vibration of agraphitic carbon causes.Sample is that part is graphited as from the foregoing.
Studies show that through Fourier transform infrared spectroscopy sample contains hydroxyl and aldehyde radical, confirmed the functional of this carbon nanofiber carbon nanofiber.
Embodiment 2:
With 0.2g polyvinylpyrrolidone and 0.1584gNa
2TeO
3, placing capacity is the reactor of 30ml, adds the 21ml dissolved in distilled water, add 1ml hydrazine hydrate and 2ml ammoniacal liquor then successively, stir, after the reactor sealing, place 180 ℃ of baking ovens, kept 8 hours, naturally cool to room temperature, the product that obtains comes out with the 40ml acetone precipitation, cleans multipass with distilled water and dehydrated alcohol successively, remove impurity, obtain the nano wire of semi-conductor tellurium.
Get nano wire 0.06 gram of this tellurium, be dispersed in the water of 24ml, add 0.3 gram beta-cyclodextrin then, after the stirring and dissolving, transfer in the reactor of 30ml, closed reactor places 180 ℃ of baking ovens to keep 4 hours, naturally cools to room temperature; Product repeatedly washs with distilled water and dehydrated alcohol, after the drying, promptly obtains carbon and coats the tellurium nano-cable.
Get this carbon and coat tellurium nano-cable 0.02 gram, in the 20ml water, add the 0.2g inferior sodium phosphate, stirring at room 2 hours in the dispersion.Centrifugation goes out product, uses distilled water wash three times, promptly obtains carbon nano fiber.
By this nano-cable is carried out field emission scanning electron microscope and transmission electron microscope observation as can be known, the diameter of nano-cable sample is 20-40nm, and length can reach tens microns, even micron up to a hundred; Transmission electron microscope observation shows that the sample that is obtained is the core-shell nano structure, the diameter 4-9 nanometer of nuclear, and the end of nuclear all is wrapped and goes up thick carbon-coating, and the thickness of carbon-coating is the 6-18 nanometer.
Resulting nano-cable is carried out the photoelectron spectrograph result of study show, very weak at the peak of the bonded energy 573eV of Te3d5, almost detect not come out, illustrate that the nano wire of tellurium has been wrapped.
The carbon nanofiber that obtains in the present embodiment is carried out the field emission scanning electron microscope observation show that the diameter of this carbon nanofiber sample is 20-40nm, length can reach tens microns even micron up to a hundred; Carbon nanofiber shows that through transmission electron microscope observation the tellurium core that former carbon coats the tellurium nano-cable has been fallen by chemical treatment, and the carbon nanofiber diameter is 20-40nm, tens microns of length.
The raman study that carbon nanofiber is carried out shows, at 1592cm
-1A tangible peak is arranged, and this is because the C-C stretching vibration of typical graphite-structure causes, shows that the sample part is graphited, at 1361cm
-1Have one not to be clearly peak, very weak, this is because the C-C stretching vibration of agraphitic carbon causes.So it is graphited that sample is a part.
Studies show that through carbon nanofiber is carried out Fourier transform infrared spectroscopy sample contains hydroxyl and aldehyde radical, it is functional to have confirmed that this carbon nanofiber has.
Embodiment 3:
With 1.2g polyvinylpyrrolidone and 0.0528gNa
2TeO
3, placing capacity is the reactor of 30ml, adds the 21ml dissolved in distilled water, adds 1ml hydrazine hydrate and 2ml ammoniacal liquor then successively, stirs, and after the reactor sealing, places 190 ℃ of baking ovens, keeps 6 hours, naturally cools to room temperature then; The product that obtains comes out with the 40ml acetone precipitation, cleans multipass with distilled water and dehydrated alcohol successively, removes impurity, obtains the nano wire of semi-conductor tellurium.
Get 2.4 milligrams of the nano wires of above-mentioned tellurium, be dispersed in the water of 24ml, add 7.5 gram glucose, after the stirring and dissolving, transfer in the reactor of 30ml, closed reactor places 190 ℃ of baking ovens to keep 8 hours, naturally cools to room temperature; Product repeatedly washs with distilled water and dehydrated alcohol, and is dry then, obtains carbon and coats the tellurium nano-cable.
Get this carbon coating tellurium nano-cable and be distributed in the 20ml water for 1 milligram, add 0.5ml nitric acid, stirring at room 2 hours, the product that centrifugation goes out distilled water wash three times promptly obtain carbon nano fiber.
The carbon that obtains in the present embodiment is coated the tellurium nano-cable carry out field emission scanning electron microscope and transmission electron microscope observation, the diameter of visible nano-cable sample is 60-80nm, and length can reach tens microns, even up to a hundred microns.Tem observation shows that the nano-cable sample is the core-shell nano structure, the diameter 4-9 nanometer of nuclear, and the end of nuclear all is wrapped and goes up thick carbon-coating, and the thickness of carbon-coating is the 25-38 nanometer.
The carbon that obtains in the present embodiment is coated the tellurium nano-cable carry out photoelectron spectrograph research, the result shows, and is very weak at the peak of the bonded energy 573eV of Te3d5, almost detects not come out, and illustrates that the nano wire of tellurium has been wrapped.
The carbon nanofiber that obtains in the present embodiment is carried out field emission scanning electron microscope and transmission electron microscope observation shows, the diameter of this carbon nanofiber sample is 60-80nm, and length can reach tens microns even micron up to a hundred.
This carbon nanofiber is carried out raman study show, at 1586cm
-1A tangible peak is arranged, and this is because the C-C stretching vibration of typical graphite-structure causes, shows that the sample part is graphited, at 1355cm
-1Have one not to be clearly peak, very weak, this is because the C-C stretching vibration of agraphitic carbon causes.So it is graphited that sample is a part.
This carbon nanofiber be studies show that through Fourier transform infrared spectroscopy sample contains hydroxyl and aldehyde radical, confirm the functional of this carbon nanofiber.
Embodiment 4:
With 0.6 gram polyvinylpyrrolidone and 0.1107gNa
2TeO
3, placing capacity is the reactor of 30ml, adds the 21ml dissolved in distilled water, adds 1ml hydrazine hydrate and 2ml ammoniacal liquor then successively, stirs, and after the reactor sealing, places 200 ℃ of baking ovens, keeps 4 hours, naturally cools to room temperature then; The product that obtains comes out with the 40ml acetone precipitation, cleans multipass with distilled water and dehydrated alcohol successively, removes impurity, obtains the nano wire of semi-conductor tellurium.
Get nano wire 0.01 gram of this tellurium, be dispersed in the water of 24ml, add 1.5 gram starch then, after the stirring and dissolving, transfer in the reactor of 30ml, closed reactor places 220 ℃ of baking ovens to keep 4 hours, naturally cools to room temperature; Product repeatedly washs with distilled water and dehydrated alcohol, after the drying, promptly obtains carbon and coats the tellurium nano-cable.
Get this carbon and coat tellurium nano-cable 0.01 gram, in the 20ml water, add 0.3g potassium permanganate, stirring at room 2 hours in the dispersion.Centrifugation goes out product, uses distilled water wash three times, promptly obtains carbon nano fiber.
By this nano-cable is carried out field emission scanning electron microscope and transmission electron microscope observation as can be known, the diameter of nano-cable sample is 100-140 nm, and length can reach tens microns, even micron up to a hundred; Transmission electron microscope observation shows that the sample that is obtained is the core-shell nano structure, the diameter 4-9 nanometer of nuclear, and the end of nuclear all is wrapped and goes up thick carbon-coating, and the thickness of carbon-coating is the 45-68 nanometer.
Resulting nano-cable is carried out the photoelectron spectrograph result of study show, very weak at the peak of the bonded energy 573eV of Te3d5, almost detect not come out, illustrate that the nano wire of tellurium has been wrapped.
The carbon nanofiber that obtains in the present embodiment is carried out the field emission scanning electron microscope observation show that the diameter of this carbon nanofiber sample is 100-140nm, length can reach tens microns even micron up to a hundred; The tellurium core that coats the tellurium nano-cable through the former carbon of transmission electron microscope observation has been fallen by chemical treatment, and the carbon nanofiber diameter is 100-140nm, tens microns of length.
The raman study that carbon nanofiber is carried out shows, at 1590cm
-1A tangible peak is arranged, and this is because the C-C stretching vibration of typical graphite-structure causes, shows that the sample part is graphited, at 1359cm
-1Have one not to be clearly peak, very weak, this is because the C-C stretching vibration of agraphitic carbon causes.So it is graphited that sample is a part.
Studies show that through carbon nanofiber is carried out Fourier transform infrared spectroscopy sample contains hydroxyl and aldehyde radical, it is functional to have confirmed that this carbon nanofiber has.
Claims (5)
1, a kind of method for preparing carbon nanofiber is characterized in that: the polyvinylpyrrolidone and the 2.2-6.6g/L Na that will contain 8-48g/L earlier
2TeO
3The aqueous solution, with hydrazine hydrate that accounts for reaction system weight 2-4% and the ammoniacal liquor of 1-4%, be sealed in the reaction vessel, in 160-200 ℃ of reaction 4-10 hour, obtain the nano wire of semi-conductor tellurium;
This tellurium nano-wire is enclosed in 160-220 ℃ of reaction 4-20 hour by the 0.1-2.5g/L aqueous solution and saccharide compound 12.5-312.5g/L, and cool to room temperature obtains carbon and coats the tellurium nano-cable;
Carbon is coated the tellurium nano-cable by the 0.1-2.5g/L aqueous solution, add the 0.02-2M/L oxygenant, promptly obtain carbon nanofiber.
2, the method for preparing carbon nanofiber according to claim 1 is characterised in that described saccharide compound comprises starch, glucose, beta-cyclodextrin, fructose, maltose or sucrose.
3, the method for preparing carbon nanofiber according to claim 1 is characterised in that described oxygenant chooses from hydrogen peroxide, nitric acid, potassium bromate, potassium permanganate, Potcrate, sodium borohydride, POTASSIUM BOROHYDRIDE or inferior sodium phosphate oxygenant.
4, the intermediate product carbon among the described carbon nanofiber preparation method of claim 1 coats the preparation method of tellurium nano-cable, it is characterized in that: the polyvinylpyrrolidone and the 2.2-6.6g/L Na that will contain 8-48g/L earlier
2TeO
3The aqueous solution, with hydrazine hydrate that accounts for reaction system weight 2-4% and the ammoniacal liquor of 1-4%, be sealed in the reaction vessel, in 160-200 ℃ of reaction 4-10 hour, obtain the nano wire of semi-conductor tellurium; This tellurium nano-wire is enclosed in 160-220 ℃ of reaction 4-20 hour by the 0.1-2.5g/L aqueous solution and saccharide compound 12.5-312.5g/L, and cool to room temperature obtains carbon and coats the tellurium nano-cable.
5, the carbon of the described method preparation of claim 4 coats the tellurium nano-cable, and it is characterized in that: the core of cable is the semi-conductor tellurium of diameter 4-9 nanometer, and what the tellurium core coated outward is that thickness is the amorphous carbon of 6-68 nanometer.
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| CN102179182A (en) * | 2011-03-29 | 2011-09-14 | 中国科学技术大学 | Method for preparing carbon nanofiber membrane |
| CN102430387A (en) * | 2011-10-24 | 2012-05-02 | 浙江师范大学 | Method for preparing novel carbon material at low temperature for processing dye waste water |
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| CN103641101A (en) * | 2013-12-19 | 2014-03-19 | 上海交通大学 | Two-dimensional structural carbon nanomaterial and preparation method thereof |
| CN105810446A (en) * | 2016-03-16 | 2016-07-27 | 杭州禹净环境科技有限公司 | Preparation method for molybdenum disulfide nanosheet loaded tellurium nanotube |
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