CN104766963A - Method for preparing metal oxide-carbon fiber nano composite material - Google Patents
Method for preparing metal oxide-carbon fiber nano composite material Download PDFInfo
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- CN104766963A CN104766963A CN201510194163.2A CN201510194163A CN104766963A CN 104766963 A CN104766963 A CN 104766963A CN 201510194163 A CN201510194163 A CN 201510194163A CN 104766963 A CN104766963 A CN 104766963A
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- metal oxide
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- absorbent cotton
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention provides a method for preparing a metal oxide-carbon fiber nano composite material. The method comprises the following steps: (a) measuring degreasing cotton, washing the degreasing cotton by utilizing deionized water for standby use; (b) preparing a precursor solution comprising corresponding metal ions; (c) immersing the washed degreasing cotton in step (a) in the precursor solution of the metal ions in step (b), standing the mixed solution for 12 to 24 hours at the temperature of 80 to 100 DEG C, taking out the degreasing cotton, and obtaining the degreasing cotton loaded with metal oxide after the degreasing cotton is washed and dried; (d) finally placing the degreasing cotton loaded with the metal oxide in step (c) in a nitrogen furnace, heating the nitrogen furnace to 500 to 600 DEG C, preserving the heat for 2 to 5 hours, and obtaining the metal oxide-carbon fiber nano composite material. The method is easy for obtaining raw materials, simple in process, high in preparation efficiency, low in cost, convenient in mass production and capable of preparing various oxide-carbon fiber nano composite material.
Description
Technical field
The invention belongs to nano material and Nano-composite materials technical field, particularly relate to a kind of method preparing metal oxide-carbon fiber nano composite material.
Background technology
Major part metal oxide materials all has special response characteristic for the physical quantity such as sound, optical, electrical, magnetic, power, humidity, temperature, and is widely used as air-sensitive, catalysis, battery, luminescence, insulation, weaving, biomedicine, extinguish material etc.Such as, nano-TiO
2, ZnO, Fe
2o
3the activity of good photocatalysis degradation organic contaminant is had Deng metal oxide semiconductor; Especially nano-TiO
2because oxidability is strong, photo-induced super-hydrophilicity is good, nontoxic and long-term photochemical stability and have important application prospect in the depollution of environment; ZnO, as a kind of important semi-conducting material, is widely used in the fields such as catalysis, sensing, photoelectron material; Nanometer Fe
2o
3also be widely used in catalysis, transducer, electrode material etc.But metal oxide its also there is the defects such as side reaction easily occurs, the easy poisoning and deactivation of course of reaction, its nano particle are easily reunited, limit the performance of its performance.Carbon fiber (CFs) has the features such as high strength, high-modulus, density are low, and it is high temperature resistant, corrosion-resistant, has well conduction and heat conductivility.Utilize the advantage such as the catalytic activity of carbon fiber itself, Large ratio surface sum high stability, metal oxide-carbon fiber nano composite material is prepared at its area load functional metal oxide-based nanomaterial, the reunion of metal oxide nanoparticles can not only be avoided, ensure material morphologically with structural stability, avoid metal oxide that other reactions occur further, a large amount of oxygen enrichment groups can also be provided, effectively suppress catalyst poisoning, extend its useful life.
At present, the preparation method of metal oxide-carbon fiber nano composite material mainly contains liquid phase deposition, vapour deposition process, arc discharge method, hydro thermal method, mechanical attrition method, blending method, sol-gel process, infusion process etc.Liquid phase deposition process major part chooses the carbon fiber that business buys, and due to surface chemistry inertia, poor with the combination of oxide nano-particles after deposition, easily come off, area load is uneven; Vapour deposition process apparatus expensive, complex operation, is unsuitable for producing in enormous quantities; Arc discharge method and hydro thermal method severe reaction conditions, power consumption are large; Mechanical attrition method is serious to equipment loss, easy introduces out-phase impurity; Blending method, sol-gel process is easily separated with infusion process preparation process two-phase, causes nano particle to be reunited, and it is comparatively large that the particle dispersion of metal oxide and particle size control difficulty, and the advantage of synthesized composite material cannot realize.
Summary of the invention
For above-mentioned technical problem, the object of the present invention is to provide a kind of method preparing metal oxide-carbon fiber nano composite material, adopt the further high temperature crystallization of metal oxide nanoparticles and the synchronous original position of carbonization of carbon fiber to carry out, effectively overcome the nano particle existing for carbon fiber-based nano composite material prepared by conventional method with between carbon fiber in conjunction with the shortcoming such as poor, two-phase is easily separated.
The technical solution used in the present invention is:
Prepare a method for metal oxide-carbon fiber nano composite material, comprise the following steps:
A () takes absorbent cotton, after clean by washed with de-ionized water, stand-by;
B () takes slaine and is dissolved in deionized water, the precursor solution of preparation containing respective metal ion, and wherein concentration of metal ions is within the scope of 0.05 ~ 0.1mol/L;
C () is immersed in the described absorbent cotton after cleaning in step (a) in the precursor solution of metal ion described in step (b), after 80-100 DEG C of standing 12-24 hour, take out absorbent cotton, after washing, drying, obtain the absorbent cotton that load has metal oxide;
D () finally has the absorbent cotton of metal oxide to be placed in nitrogen furnace load in step (c), be warming up to 500-600 DEG C of insulation 2-5 hour, obtain metal oxide-carbon fiber nano composite material.
The method preparing metal oxide-carbon fiber nano composite material of the present invention, wherein, described slaine is the one in titanium potassium oxalate, two acetate hydrate zinc, Iron(III) chloride hexahydrate.
The method preparing metal oxide-carbon fiber nano composite material of the present invention, wherein, metal oxide described in step (d) is TiO
2, ZnO, Fe
2o
3in one.
The method preparing metal oxide-carbon fiber nano composite material of the present invention, wherein, in step (d), the pattern of metal oxide has needle-like cluster arranged in a uniform, platy particle or the spheroidal particle be evenly distributed.
The method preparing metal oxide-carbon fiber nano composite material of the present invention, wherein, the mass fraction of the nano composite material containing metal oxide obtained in step (d) is in 20% ~ 50% scope.
The method preparing metal oxide-carbon fiber nano composite material of the present invention, wherein, load described in step (d) has the absorbent cotton of metal oxide to be placed in nitrogen furnace, and heating rate is 2 DEG C/min, and slower heating rate can avoid the pattern of composite material to change.
The method preparing metal oxide-carbon fiber nano composite material of the present invention, wherein, absorbent cotton described in step (a) is business absorbent cotton, utilizes the homemade absorbent cotton of natural cotton or polymer fiber material.
Beneficial effect of the present invention:
The method preparing metal oxide-carbon fiber nano composite material of the present invention, select absorbent cotton as the raw material forming carbon fiber, first on degreasing cotton fiber, the corresponding metal oxide nanoparticles of liquid phase reactor load is passed through, then be placed in nitrogen atmosphere stove to calcine, fiber is carbonized, finally obtain the metal oxide-carbon fiber nano composite material be made up of on carbon fiber surface the metal oxide nanoparticles homoepitaxial with special appearance, raw material is easy to get, technique is simple, preparation efficiency is high, cost is low, be convenient to large-scale production, can be used in preparing many oxide-carbon fiber nanometer composite material.Metal oxide-carbon fiber nano composite material prepared by the present invention can be widely used in the fields such as catalysis, photocatalysis, fuel cell, lithium ion battery, ultracapacitor, gas sensor.
Accompanying drawing explanation
Fig. 1 a is TiO prepared by embodiment 1
2powder x-ray diffraction (XRD) figure of-carbon fibre composite;
Fig. 1 b is the XRD figure of ZnO-carbon fibre composite prepared by embodiment 2;
Fig. 1 c is Fe prepared by embodiment 3
2o
3the XRD figure of-carbon fibre composite;
Fig. 2 a is TiO prepared by embodiment 1
2-carbon fibre composite amplifies scanning electron microscopy (SEM) figure of 2000 times;
Fig. 2 b is TiO prepared by embodiment 1
2-carbon fibre composite amplifies the SEM figure of 20000 times;
Fig. 2 c is the SEM figure that the ZnO-carbon fibre composite of embodiment 2 preparation amplifies 5000 times;
Fig. 2 d is the SEM figure that the ZnO-carbon fibre composite of embodiment 2 preparation amplifies 10000 times;
Fig. 2 e is Fe prepared by embodiment 3
2o
3-carbon fibre composite amplifies the SEM figure of 1000 times;
Fig. 2 f is Fe prepared by embodiment 3
2o
3-carbon fibre composite amplifies the SEM figure of 20000 times;
Fig. 3 is TiO prepared by embodiment 1
2thermogravimetric analysis (TGA) curve chart of-carbon fibre composite;
Fig. 4 is thermogravimetric analysis (TGA) curve chart of ZnO-carbon fibre composite prepared by embodiment 2;
Fig. 5 is Fe prepared by embodiment 3
2o
3thermogravimetric analysis (TGA) curve chart of-carbon fibre composite.
Below in conjunction with specific embodiment and accompanying drawing, the invention will be further described.
Embodiment
In following examples, the SEM figure of gained oxide-carbon fiber nanometer composite material all adopts model to be that the field emission scanning electron microscope of Sirion200 characterizes; XRD figure all adopts the x-ray powder diffraction instrument of Japanese Shimadzu Corporation XRD-6000 type, records under Cu target, voltage 40.0KV, electric current 30.0mA, sweep speed 10 °/min, sweep limits 10 ° ~ 80 ° conditions; TGA curve chart measures all as follows and obtains: the thermal analyzer using Japanese Shimadzu Corporation model TA-50, in air atmosphere, with the rate of heat addition of 10 DEG C/min, 5mg sample is heated to 600 DEG C from room temperature, the weight change of working sample.
Embodiment 1
The present embodiment prepares TiO
2the method of-carbon fiber nanometer composite material, comprises the following steps:
A () first, weighs 0.1g business absorbent cotton, clean by washed with de-ionized water, stand-by;
B () then, weighs 0.70g titanium potassium oxalate (K
2tiO (C
2o
4)
2) be dissolved in 30mL deionized water, stirring and dissolving, more slowly instill 1mL hydrogen peroxide solution (H
2o
2, 30wt.%), finally use watery hydrochloric acid (HCl, 1mol/L) that solution ph is transferred within the scope of 1-2, be prepare containing Ti
4+the precursor solution of ion;
C () is immersed in Ti in step (b) the absorbent cotton cleaned up in step (a)
4+in the precursor solution of ion, be sealed in glass jar, after leaving standstill 24 hours at 80 DEG C, take out absorbent cotton, after washing, drying, obtain load has TiO
2absorbent cotton;
D () finally has TiO load
2absorbent cotton be placed in N
2in atmosphere furnace, be elevated to 500 DEG C with the heating rate of 2 DEG C/min, be incubated and namely obtain TiO in 3 hours
2-carbon fiber nanometer composite material.
As shown in Figure 1a, the TiO of embodiment 1 preparation
2xRD figure and the Anatase TiO of-carbon fiber nanometer composite material
2standard diffraction peak (JCPDS No.21-1272) consistent, prove that wherein oxide is the TiO of Anatase
2material.Fig. 2 a and Fig. 2 b is respectively TiO prepared by embodiment 1
2-carbon fiber nanometer composite material amplifies the SEM figure of 2000 and 20000 times, shows that the microstructure of this sample is nano-TiO
2homoepitaxial in carbon fiber surface, wherein nano-TiO
2pattern be needle-like cluster arranged in a uniform, carbon fiber diameter about 10 microns, reach ~ 0.5cm, carbon fiber surface presents many gullies.Fig. 3 is TiO prepared by embodiment 1
2the TGA curve chart of-carbon fiber nanometer composite material, is warmed up to 350 DEG C in air atmosphere, and sample starts obvious weightlessness, and this is that until 498.2 DEG C, carbon fiber burns completely, remaining TiO because the carbon fiber burning in composite material causes
2account for 41.76% of sample gross mass, the TiO prepared by embodiment 1 is described
2containing TiO in-carbon fiber nanometer composite material
2for 41.76wt%.
Embodiment 2
The method of the present embodiment making ZnO-carbon fiber nanometer composite material, comprises the following steps:
A () first, weighs 0.1g business absorbent cotton, clean by washed with de-ionized water, stand-by;
B () then, weighs 0.44g bis-acetate hydrate zinc (Zn (Ac)
22H
2o) be dissolved in 30mL deionized water, stirring and dissolving, more slowly add 0.40g NaOH (NaOH), continue stirring and make it to dissolve completely, be prepare containing Zn
2+the precursor solution of ion;
C () is immersed in Zn in step (b) the absorbent cotton cleaned up
2+in the precursor solution of ion, be sealed in glass jar, after leaving standstill 24 hours at 80 DEG C, take out absorbent cotton, after washing, drying, obtain the absorbent cotton that load has ZnO;
D () finally has the absorbent cotton of ZnO to be placed in N load
2in atmosphere furnace, be elevated to 500 DEG C with the heating rate of 2 DEG C/min, be incubated and namely obtain ZnO-carbon fiber nanometer composite material in 3 hours.
As shown in Figure 1 b, the XRD figure of ZnO-carbon fiber nanometer composite material prepared by embodiment 2, consistent with the standard diffraction peak (JCPDS No.79-0205) of six side phase ZnO, prove that wherein oxide is the ZnO material of six side's phases.Fig. 2 c and Fig. 2 d is respectively the SEM figure of ZnO-carbon fiber nanometer composite material amplification 5000 and 10000 times prepared by embodiment 2, and show that the microstructure of this sample is that nano-ZnO is grown in the groove of carbon fiber surface, wherein the pattern of nano-ZnO is platy particle.Fig. 4 is the TGA curve chart of ZnO-carbon fiber nanometer composite material prepared by embodiment 2, be warmed up to 340 DEG C in air atmosphere, sample starts obvious weightlessness, this is because the carbon fiber burning in composite material causes, until 478.7 DEG C, carbon fiber burns completely, and remaining ZnO accounts for the 36.34wt% of sample gross mass, illustrates that containing ZnO in the ZnO-carbon fiber nanometer composite material prepared by embodiment 2 is 36.34wt%.
Embodiment 3
The present embodiment prepares Fe
2o
3the method of-carbon fiber nanometer composite material, comprises the following steps:
A () first, weighs 0.1g business absorbent cotton, clean by washed with de-ionized water, stand-by;
B () then, weighs 0.54g Iron(III) chloride hexahydrate (FeCl
36H
2o) be dissolved in 30mL deionized water, stirring and dissolving, be prepare containing Fe
3+the precursor solution of ion;
C () is immersed in Fe in step (b) the absorbent cotton cleaned up
3+in the precursor solution of ion, be sealed in glass jar, after leaving standstill 24 hours at 90 DEG C, take out absorbent cotton, after washing, drying, obtain load has Fe
2o
3absorbent cotton;
D () finally has Fe load
2o
3absorbent cotton be placed in N
2in atmosphere furnace, be elevated to 500 DEG C with the heating rate of 2 DEG C/min, be incubated and namely obtain Fe in 3 hours
2o
3-carbon fiber nanometer composite material.
As illustrated in figure 1 c, the Fe of embodiment 3 preparation
2o
3the XRD figure of-carbon fiber nanometer composite material, with Emission in Cubic γ-Fe
2o
3standard diffraction peak (JCPDS No.4-755) consistent, prove that wherein oxide is the γ-Fe of Emission in Cubic
2o
3material.Fig. 2 e and Fig. 2 f is respectively Fe prepared by embodiment 3
2o
3-carbon fiber nanometer composite material amplifies the SEM figure of 1000 and 20000 times, shows that the microstructure of this sample is nanometer Fe
2o
3homoepitaxial in carbon fiber surface, wherein nanometer Fe
2o
3pattern be the spheroidal particle be evenly distributed.Fig. 5 is Fe prepared by embodiment 3
2o
3the TGA curve chart of-carbon fiber nanometer composite material, is warmed up to 330 DEG C in air atmosphere, and sample starts obvious weightlessness, and this is that until 487.8 DEG C, carbon fiber burns completely, remaining Fe because the carbon fiber burning in composite material causes
2o
3account for the 27.43wt% of sample gross mass, the Fe prepared by embodiment 3 is described
2o
3containing Fe in-carbon fiber nanometer composite material
2o
3for 27.43wt%.
Metal oxide precursor in above-described embodiment 1, embodiment 2 and embodiment 3 is replaced with other soluble metallic salt as zinc nitrate, ferric nitrate, cobalt chloride, nickel chloride, butter of tin, titanium trichloride, or utilize the homemade absorbent cotton of natural cotton, business absorbent cotton that macromolecular fibre replaces in above-described embodiment, also can obtain other metal oxide-carbon fiber nano composite material similar to above-described embodiment.
Above-described embodiment is only be described the preferred embodiment of the present invention; not scope of the present invention is limited; under not departing from the present invention and designing the prerequisite of spirit; the various distortion that those of ordinary skill in the art make technical scheme of the present invention and improvement, all should fall in protection range that claims of the present invention determines.
Claims (7)
1. prepare a method for metal oxide-carbon fiber nano composite material, it is characterized in that: comprise the following steps:
A () takes absorbent cotton, after clean by washed with de-ionized water, stand-by;
B () takes slaine and is dissolved in deionized water, the precursor solution of preparation containing respective metal ion, and wherein concentration of metal ions is within the scope of 0.05 ~ 0.1mol/L;
C () is immersed in the described absorbent cotton after cleaning in step (a) in the precursor solution of metal ion described in step (b), after 80-100 DEG C of standing 12-24 hour, take out absorbent cotton, after washing, drying, obtain the absorbent cotton that load has metal oxide;
D () finally has the absorbent cotton of metal oxide to be placed in nitrogen furnace load in step (c), be warming up to 500-600 DEG C of insulation 2-5 hour, obtain metal oxide-carbon fiber nano composite material.
2. the method preparing metal oxide-carbon fiber nano composite material according to claim 1, is characterized in that: described slaine is the one in titanium potassium oxalate, two acetate hydrate zinc, Iron(III) chloride hexahydrate.
3. the method preparing metal oxide-carbon fiber nano composite material according to claim 1, is characterized in that: metal oxide described in step (d) is TiO
2, ZnO, Fe
2o
3in one.
4. the method preparing metal oxide-carbon fiber nano composite material according to claim 1, is characterized in that: in step (d), the pattern of metal oxide has needle-like cluster arranged in a uniform, platy particle or the spheroidal particle be evenly distributed.
5. the method preparing metal oxide-carbon fiber nano composite material according to claim 1, is characterized in that: the mass fraction of the nano composite material containing metal oxide obtained in step (d) is in 20% ~ 50% scope.
6. the method preparing metal oxide-carbon fiber nano composite material according to claim 1, is characterized in that: load described in step (d) has the absorbent cotton of metal oxide to be placed in nitrogen furnace, and heating rate is 2 DEG C/min.
7. the method preparing metal oxide-carbon fiber nano composite material according to claim 1-6 any one, is characterized in that: absorbent cotton described in step (a) is business absorbent cotton, utilizes the homemade absorbent cotton of natural cotton or polymer fiber material.
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|---|---|---|---|
| CN201510194163.2A CN104766963B (en) | 2015-04-22 | 2015-04-22 | A kind of method preparing metal-oxide carbon fiber nanometer composite material |
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