CN102965766A - New method for synthesizing nanometal particle-loaded carbon nanofiber - Google Patents
New method for synthesizing nanometal particle-loaded carbon nanofiber Download PDFInfo
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Abstract
The invention relates to a new method for synthesizing nanometal particle-loaded carbon nanofiber. According to the method, an iron-containing compound and a high molecular polymer are taken as reaction precursors and the method comprises the following steps of: mixing the reaction precursors, absolute ethyl alcohol and dimethylformamide (DMF) to obtain a uniform solution; preparing pre-composite nanofiber by an electrostatic spinning device, and drying; transferring the nanofiber into a tube furnace; heating to 500-700 DEG C in oxygen-free condition; and keeping the temperature for a certain period of time to obtain the nanometal particle-loaded carbon nanofiber. Compared with the prior art, the method provided by the invention takes short time and has simple steps.
Description
Technical field
The invention belongs to technical field of nano material, relate to a kind of new method of synthesis of nano metallic particles load carbon nano-fiber.
Background technology
Carbon nano-fiber (CNF) has to CNT as one-dimensional nano structure material and has similar surface chemistry, high mechanical strength, good electric conductivity and large specific area, it not only has the skin effect that common nano material has, quantum size effect and small-size effect etc., also has excellent heat endurance, mechanical property, electronics and photon transmission, optical property and photoconductivity can wait, make its basic construction unit that can be used as material, at nanometer electricity and optics, sensor, the aspects such as nanometer biotechnology demonstrate important using value.The method of constructing monodimension nanometer material mainly contains template (template-assisted), gas-liquid-solid reaction method (vapaor-liquid-solid), vapor-solid growth method (apaor--solid), hydro-thermal method (hydrothermal synthesis), method of electrostatic spinning (elctrospinnning) etc.In these methods, method of electrostatic spinning is simple with its manufacturing installation, spinning is with low cost, can spin the advantages such as substance classes is various, technique is controlled, has become one of main path of effective preparation nano-fiber material.Electrostatic spinning technique has been successfully applied to preparation polymer, pottery, metal and inorganic/organic composite fiber.
Iron is the active metal, has reducibility.Nanometer metallic iron is because it in high magnetic recording density material, magnetic material, catalyst material, electric conductor and the increasingly extensive application in field such as electromagnetic wave absorbent material and biomedical carrier material, more and more is subject to researcher's attention in recent years to the research of nanometer metallic iron.The carbon-coated magnetic nano particle as Fe, Co, Ni, because the protection of carbon is arranged, makes it aspect magnetic data storage, xerography, magnetic ink, magnetic fluid and the bioengineering (administration, magnetic resonance etc.) application arranged.
This paper adopts method of electrostatic spinning to prepare carbon nano-fiber (Fe/CNF) composite of Fe nano particle load.Have about the method for preparing Fe@C composite in the disclosed document of prior art: chemical vapour deposition technique, arc discharge method, high-temperature catalytic decomposition method etc.Jiao J etc. utilizes arc discharge method to prepare Fe@C core shell structure compound, but the method yields poorly, temperature high.Song H H utilizes chemical vapour deposition technique also to prepare Fe@C compound, but the method needs independently carbon source, catalyst, catalyst difficulty and separation of products.In the Fe@C compound that these methods are synthesized, iron nano-particle all is coated on the material with carbon element the inside and is not fully used.
Summary of the invention
Purpose of the present invention is exactly the defective that exists in order to overcome existing technology of preparing, and provides a kind of new electrospinning process to prepare nano-metal particle load carbon nano-fiber.
Purpose of the present invention can be achieved through the following technical solutions:
The present invention relates to a kind of new method of synthesis of nano metallic particles load carbon nano-fiber, it is characterized in that, the method with ferrocene and high molecular polymer as pre-reaction material, pre-reaction material, absolute ethyl alcohol and dimethyl formamide (DMF) three is mixed the formation homogeneous solution, adopt electrostatic spinning apparatus to make the composite nano fiber in early stage, drying, nanofiber changes in the tube furnace, under the condition of anaerobic, be heated to 500-700 ℃, and under this temperature, be incubated the carbon nano-fiber that a period of time can make the nano-metal particle load.
The reaction system of the simple raw material of above-mentioned utilization, simple mechanism and easy steps, the method specifically may further comprise the steps:
(1) ferrocene and high molecular polymer are dissolved in the mixed solvent of a certain proportion of absolute ethyl alcohol and dimethyl formamide and are mixed with certain density solution, this solution needs magnetic agitation a few hours to form uniform solution, wherein the mass ratio of ferrocene and high molecular polymer is 9:25--5:6, the volume ratio of absolute ethyl alcohol and dimethyl formamide is 1:1--0:1, and the mass ratio of high molecular polymer and mixed solvent is 2:17--2:31.
(2) mixed solution that step (1) is obtained moves in the syringe, carries out electrostatic spinning with certain voltage, spinning speed and receiving range, and setting syringe pump, high pressure generator control program make whole spinning process continue some hours.After spinning finished, the gained fiber was dry under 55--65 ℃ of condition, and this product is the composite nano fiber in early stage.
(3) product that step (2) obtained moves in the tube furnace, is heated to 500-700 ℃ with certain heating rate in argon atmosphere, and keeps a period of time under this temperature.After reaction stops, naturally cooling, obtaining end product is black nano metallic particles load carbon nano-fiber.
Preferably, described pbz polymer polymer is polyvinylpyrrolidone or polyacrylonitrile.
Preferably, the certain spinning condition described in the step (2) is the voltage of 10-13Kv, the flow velocity of 0.5-1ml/h and the receiving range of 10-20cm.
Preferably, the heating rate described in the step (3) and temperature retention time are respectively 1-2 ℃/min and 1-2h.
Mechanism of the present invention: have the organo-metallic compound ferrocene in the precursor that uses in this invention, this material not only can be used as the catalyst of carbon nano-fiber preparation, simultaneously itself can also be as carbon source, that is: adopt electrostatic spinning technique, ferrocene is dispersed in the nanofiber of high molecular polymer uniformly, improved the high molecular polymer catalytic effect, again in conjunction with the high-temperature heating under the follow-up oxygen free condition, high molecular polymer is carbonized, ferrocene is decomposed simultaneously, luxuriant ring wherein also forms carbon nano-fiber as carbon source, and ferro element is assembled the formation nano iron particles at carbon fiber surface.
The bright method of electrostatic spinning of we is not only simplified synthesis step, do not have simultaneously separating of product and catalyst, and the Fe@C compound that obtains is the one dimension size.Compared with prior art, the inventive method is simple, raw material is easy to get, equipment is simple, easy to operate, can prepare the nano-metal particle load carbon nano-fiber of size homogeneous, and preparation cost reduces greatly.
The present invention adopts that nano iron particles is to load on the carbon nano-fiber surface in carbon nano-fiber (Fe/CNF) composite of Fe nano particle load of method of electrostatic spinning preparation, rather than being coated on the material with carbon element the inside, such combining structure is so that the character of Fe@C compound is more suitable for being applied to the fields such as catalyst material, electrode material.
Description of drawings
Fig. 1 be embodiment 1 early stage combination product scanning electron microscope (SEM) photograph.
Fig. 2 is the scanning electron microscope (SEM) photograph of the end product of embodiment 1.
Fig. 3 is end product transmission electron microscope picture among the embodiment 1.
Fig. 4 is end product transmission electron microscope picture among the embodiment 1.
Fig. 5 is the scanning electron microscope (SEM) photograph of the end product of embodiment 2.
Fig. 6 is the scanning electron microscope (SEM) photograph of the end product of embodiment 3
The specific embodiment
The present invention is described in detail below in conjunction with the drawings and specific embodiments.All raw materials that participate in reaction system among the embodiment are commercially available, and polyvinylpyrrolidone (MW=1300000) is bought in Aldrich, and polyacrylonitrile (MW=150000) is bought in J﹠amp; K Science and Technology Ltd., ferrocene is purchased from Shanghai green grass or young crops and analyses Chemical Industry Science Co., Ltd, dimethyl formamide and ethanol all are purchased from Solution on Chemical Reagents in Shanghai company of Chinese Medicine group, above chemical reagent be analyze pure, not purified direct use.
Embodiment 1
The first step takes by weighing the 2.0g polyvinylpyrrolidone and the 0.9g ferrocene is dissolved in the beaker, adds 11ml absolute ethyl alcohol and 9ml solvent dimethylformamide, places the interior magnetic agitation of beaker to form even crocus solution.
Second step changes the solution for preparing in the syringe over to, connects electrostatic spinning apparatus, and spinning condition is set, and voltage is 13Kv, and injection rate is that the 1ml/h receiving range is 15cm.Start high pressure generator, spinning process continues 5 hours, and is then that the composite nano fiber that makes is dry under 60 ° of C.Peel off from aluminium foil general combination product in early stage with tweezers, by field emission scanning electron microscope (Philips company, XL-30E, SEM), set scanning voltage 3KV, can find out under 60,000 times of (Fig. 1) conditions of multiplication factor that early stage, combination product was the one dimension linear structure, but the surface there is no particulate load.
The 3rd step changed the second step product in the tube furnace over to, and directly the speed with 2 ° of C/min is heated to 500 ° of C in argon atmosphere, and is incubated 1h under these 500 ° of C temperature, then naturally cools to room temperature.This moment, the product of gained was nano-metal particle load carbon nano-fiber.And sample analyzed:
(1) by field emission scanning electron microscope (Philips company, XL-30E, SEM), set scanning voltage 3KV, can find out that product is the one dimension linear structure under 20,000 times of (Fig. 2) conditions of multiplication factor, and have metallic particles to load on fiber surface.A indication ferrous metal particle among the figure, b indicates carbon nano-fiber.
(2) by transmission electron microscope (JEOL company, JEM-2100, TEM), (Fig. 3) can find out that metallic particles evenly is embedded in the carbon nano-fiber surface under the setting scale 100nm condition, and particle is not easy to split away off like this.
(3) by transmission electron microscope Electronic Speculum (JEOL company, JEM-2100, TEM), set under the scale 5nm condition (Fig. 4), can see interplanar distance, metallic particles is the good monocrystalline of crystallinity as can be known.
Embodiment 2
The first step takes by weighing the 1.0g polyacrylonitrile and the 0.5g ferrocene is dissolved in the beaker, adds the 10ml solvent dimethylformamide, and magnetic agitation forms even crocus solution.
Second step changes the solution for preparing in the syringe over to, connects electrostatic spinning apparatus, and spinning condition is set, and voltage is 10Kv, and injection rate is that the 0.5ml/h receiving range is 19cm.Start high pressure generator, spinning process was held 5 hours, and is then that the composite nano fiber that makes is dry under 61 ° of C. peel off product and aluminium foil with tweezers.
The 3rd step changed the second step product in the tube furnace over to, and the speed with 2 ° of C/min in air atmosphere encloses is heated to 250 ° of C, and insulation 0.5h. continues to be heated to 700 ° of C again in argon atmosphere under this temperature, and then insulation 1h naturally cools to room temperature.This moment, the product of gained was nano-metal particle load carbon nano-fiber.
The present embodiment sample is analyzed: by field emission scanning electron microscope (Philips company, XL-30E, SEM), the setting scanning voltage is 3KV, multiplication factor is that (Fig. 5) can clearly find out under 30,000 times of conditions, product is the one dimension linear structure, and has metallic particles to load on fiber surface.
Embodiment 3
The first step takes by weighing the 1.5g polyvinylpyrrolidone and the 0.6g ferrocene is dissolved in the beaker, adds 9ml absolute ethyl alcohol and 6ml solvent dimethylformamide, places the interior magnetic agitation of beaker to form even crocus solution.
Second step changes the solution for preparing in the syringe over to, connects electrostatic spinning apparatus, and spinning condition is set, and voltage is 11Kv, and injection rate is that the 0.6ml/h receiving range is 17cm.Start high pressure generator, spinning process continues 10 hours, and is then that the composite nano fiber that makes is dry under 64 ° of C. peel off product and aluminium foil with tweezers.
The 3rd step changed the second step product in the tube furnace over to, and directly the speed with 1 ° of C/min is heated to 600 ° of C in argon atmosphere, and is incubated 2h under this temperature, then naturally cools to room temperature.This moment, the product of gained was nano-metal particle load carbon nano-fiber.
The present embodiment sample is analyzed: by field emission scanning electron microscope (Philips company, XL-30E, SEM), the setting scanning voltage is 3KV, multiplication factor is that (Fig. 6) can clearly find out under 60,000 times of conditions, product presents the one dimension linear structure equally, and has metallic particles to load on the carbon nano-fiber surface.
Claims (5)
1. the new method of a synthesis of nano metallic particles load carbon nano-fiber, it is characterized in that, the method with ferrocene and high molecular polymer as pre-reaction material, pre-reaction material, absolute ethyl alcohol and dimethyl formamide three are mixed the formation homogeneous solution, adopt electrostatic spinning apparatus to make the composite nano fiber in early stage, drying, nanofiber changes in the tube furnace, under the condition of anaerobic, be heated to 500-700 ℃, and under this temperature, be incubated the carbon nano-fiber that a period of time can make the nano-metal particle load.
2. the method for claim 1 is characterized in that, the method specifically may further comprise the steps:
(1) ferrocene and high molecular polymer are dissolved in the mixed solvent of a certain proportion of absolute ethyl alcohol and dimethyl formamide and are mixed with certain density solution, this solution need to stir and form uniform solution, wherein the mass ratio of ferrocene and high molecular polymer is 9:25--5:6, the volume ratio of absolute ethyl alcohol and dimethyl formamide is 1:1--0:1, and the mass ratio of high molecular polymer and mixed solvent is 2:17--2:31;
(2) mixed solution that step (1) is obtained moves in the syringe, carry out electrostatic spinning with certain voltage, spinning speed and receiving range, setting syringe pump, high pressure generator control program make whole spinning process continue some hours, after spinning finishes, the gained fiber is dry under 55--65 ℃ of condition, and this product is the composite nano fiber in early stage;
(3) product that step (2) is obtained moves in the tube furnace, in argon atmosphere, be heated to 500-700 ℃ with certain heating rate, and under this outlet temperature, keep a period of time, after reaction stops, naturally cooling, obtaining end product is black nano metallic particles load carbon nano-fiber.
3. such as claim 1 or 2 described methods, it is characterized in that described pbz polymer polymer is polyvinylpyrrolidone or polyacrylonitrile.
4. method as claimed in claim 2 is characterized in that, the certain spinning condition described in the step (2) is the voltage of 10-13Kv, the flow velocity of 0.5-1ml/h and the receiving range of 10-20cm.
5. method as claimed in claim 2 is characterized in that, the heating rate described in the step (3) and temperature retention time are respectively 1-2 ℃/min and 1-2h.
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