CN104766963B - A kind of method preparing metal-oxide carbon fiber nanometer composite material - Google Patents
A kind of method preparing metal-oxide carbon fiber nanometer composite material Download PDFInfo
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Abstract
The invention provides a kind of method preparing metal-oxide carbon fiber nanometer composite material, comprise the following steps：A () weighs absorbent cotton, after deionized water cleans up, stand-by；B () prepares the precursor solution containing respective metal ion；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 standings 12 24 hours, take out absorbent cotton, scrubbed, be dried after obtain and be loaded with the absorbent cotton of metal-oxide；D () is finally placed in the absorbent cotton being loaded with metal-oxide in step (c) in nitrogen furnace, be warming up to 500 600 DEG C and be incubated 25 hours, obtain metal-oxide carbon fiber nanometer composite material.The inventive method, raw material is easy to get, process is simple, preparation efficiency high, low cost, is easy to large-scale production, can be used in preparing many oxide carbon fiber nanometer composite material.
Description
Technical field
The invention belongs to nano material and nano composite material preparing technical field, more particularly to one kind prepares metal oxygen
The method of compound-carbon fiber nanometer composite material.
Background technology
It is special that most of metal oxide materials all have for physical quantitys such as sound, light, electricity, magnetic, power, humidity, temperature
Response characteristic, and it is widely used as air-sensitive, catalysis, battery, luminous, insulation, weaving, biomedical, fire extinguishing material etc..Example
As nano-TiO2、ZnO、Fe2O3There is the activity of good photocatalysis degradation organic contaminant Deng metal oxide semiconductor；Especially
It is nano-TiO2Because oxidability is strong, good, the nontoxic and long-term photochemical stability of photo-induced super-hydrophilicity and in the depollution of environment
Aspect has important application prospect；ZnO, as a kind of important semi-conducting material, is widely used in catalysis, sensing, light
The fields such as electronic material；Nanometer Fe2O3Also it is widely used at aspects such as catalysis, sensor, electrode materials.But metal oxygen
Compound its there is also the easy defect such as occur side reaction, the easy poisoning and deactivation of course of reaction, its nanoparticle easily to reunite, limit its property
The performance of energy.Carbon fiber (CFs) has high intensity, high-moduluss, the low feature of density, and it is high temperature resistant, corrosion-resistant, has well
Conduction and heat conductivility.The advantages of using the catalysis activity of carbon fiber itself, bigger serface and high stability, bear on its surface
Carry functional metal oxide-based nanomaterial and prepare metal oxide-carbon fiber nano composite material, be not only avoided that metal oxygen
The reunion of compound nano-particle it is ensured that material morphologically with structure on stability, it is to avoid metal-oxide occurs further
Other reactions, moreover it is possible to provide substantial amounts of oxygen-enriched group, effectively suppress catalyst poisoning, extend its service life.
At present, the preparation method of metal oxide-carbon fiber nano composite material mainly has liquid phase deposition, vapour deposition
Method, arc discharge method, hydro-thermal method, mechanical attrition method, blending method, sol-gel process, infusion process etc..The big portion of liquid phase deposition process
Dividing is to choose commercially available carbon fiber, 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, it is unsuitable for producing in enormous quantities；Arc discharge method and
Hydro-thermal method severe reaction conditions, power consumption are big；Mechanical attrition method is serious to equipment loss, easy to introduce out-phase impurity；Blending method, molten
Glue-gel method and the biphase easy generation of infusion process preparation process separate, and lead to nanoparticle to be reunited, the granule dispersion of metal-oxide
Degree and size control difficulty are larger, and the advantage of synthesized composite cannot be realized.
Content of the invention
For above-mentioned technical problem, it is an object of the invention to provide one kind prepares metal oxide-carbon fiber nanometer again
The method of condensation material, is synchronously entered in situ using the further high temperature crystallization of metal oxide nanoparticles and the carbonization of carbon fiber
OK, effectively overcome the nanoparticle existing for carbon fiber-based nano composite material of traditional method preparation and combine between carbon fiber
The shortcomings of poor, biphase easy generation separates.
The technical solution used in the present invention is：
A kind of method preparing metal oxide-carbon fiber nano composite material, comprises the following steps：
A () weighs absorbent cotton, after deionized water cleans up, stand-by；
B () weighs slaine and is dissolved in deionized water, prepare the precursor solution containing respective metal ion, wherein metal
Ion concentration is in the range of 0.05～0.1mol/L；
C presoma that () is immersed in metal ion described in step (b) the described absorbent cotton after cleaning in step (a) is molten
In liquid, 80-100 DEG C standing 12-24 hour after, take out absorbent cotton, scrubbed, be dried after obtain be loaded with metal-oxide
Absorbent cotton；
D () is finally placed in the absorbent cotton being loaded with metal-oxide in step (c) in nitrogen furnace, be warming up to 500-600
DEG C 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
One of 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, institute in step (d)
Stating metal-oxide is TiO2、ZnO、Fe2O3One of.
The method preparing metal oxide-carbon fiber nano composite material of the present invention, wherein, gold in step (d)
The pattern belonging to oxide has needle-like cluster arranged in a uniform, platy particle or the spheroidal particle being evenly distributed.
The method preparing metal oxide-carbon fiber nano composite material of the present invention, wherein, institute in step (d)
The mass fraction of the nano composite material containing metal oxide obtaining is in the range of 20%～50%.
The method preparing metal oxide-carbon fiber nano composite material of the present invention, wherein, institute in step (d)
State and be loaded with the absorbent cotton of metal-oxide and be placed in nitrogen furnace, heating rate is 2 DEG C/min, and slower heating rate can avoid
The pattern of composite changes.
The method preparing metal oxide-carbon fiber nano composite material of the present invention, wherein, institute in step (a)
State absorbent cotton to be business absorbent cotton, utilize 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, from absorbent cotton as shape
Become the raw material of carbon fiber, first on degreasing cotton fiber, corresponding metal oxide nanoparticles are loaded by liquid phase reactor, so
After be placed in nitrogen atmosphere stove calcining, fiber is carried out carbonization, finally obtains by the metal oxide nano with special appearance
The metal oxide-carbon fiber nano composite material that granule homoepitaxial is constituted on carbon fiber surface, raw material is easy to get, technique
Simply, preparation efficiency height, low cost, are easy to large-scale production, can be used in preparing many oxide-carbon fiber nanometer composite wood
Material.The metal oxide-carbon fiber nano composite material of present invention preparation can be widely used for catalysis, photocatalysis, fuel cell, lithium
The fields such as ion battery, ultracapacitor, gas sensor.
Brief description
Fig. 1 a is the TiO of embodiment 1 preparation2Powder X-ray diffraction (XRD) figure of-carbon fibre composite；
Fig. 1 b is the XRD figure of the ZnO- carbon fibre composite of embodiment 2 preparation；
Fig. 1 c is the Fe of embodiment 3 preparation2O3The XRD figure of-carbon fibre composite；
Fig. 2 a is the TiO of embodiment 1 preparation2- carbon fibre composite amplifies 2000 times of scanning electron microscope (SEM)
Figure；
Fig. 2 b is the TiO of embodiment 1 preparation2- carbon fibre composite amplifies 20000 times of SEM figure；
Fig. 2 c is the SEM figure of 5000 times of the ZnO- carbon fibre composite amplification of embodiment 2 preparation；
Fig. 2 d is the SEM figure of 10000 times of the ZnO- carbon fibre composite amplification of embodiment 2 preparation；
Fig. 2 e is the Fe of embodiment 3 preparation2O3- carbon fibre composite amplifies 1000 times of SEM figure；
Fig. 2 f is the Fe of embodiment 3 preparation2O3- carbon fibre composite amplifies 20000 times of SEM figure；
Fig. 3 is the TiO of embodiment 1 preparation2Thermogravimetric analysiss (TGA) curve chart of-carbon fibre composite；
Fig. 4 is thermogravimetric analysiss (TGA) curve chart of the ZnO- carbon fibre composite of embodiment 2 preparation；
Fig. 5 is the Fe of embodiment 3 preparation2O3Thermogravimetric analysiss (TGA) curve chart of-carbon fibre composite.
Below in conjunction with specific embodiment and accompanying drawing, the invention will be further described.
Specific embodiment
In following examples, the SEM of gained oxide-carbon fiber nanometer composite material schemes all using model Sirion200
Field emission scanning electron microscope characterized；XRD figure all using the x-ray powder diffraction instrument of Japanese Shimadzu Corporation XRD-6000 type,
Record under the conditions of Cu target, voltage 40.0KV, electric current 30.0mA, 10 °/min of scanning speed, 10 °～80 ° of sweep limitss；TGA is bent
Line chart all measures as follows and obtains：Using the thermal analyzer of 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 determination sample.
Embodiment 1
The present embodiment prepares TiO2The method of-carbon fiber nanometer composite material, comprises the following steps：
A () first, weighs 0.1g business absorbent cotton, deionized water cleans up, stand-by；
(b) and then, weigh 0.70g titanium potassium oxalate (K2TiO(C2O4)2) be dissolved in 30mL deionized water, stirring and dissolving, then
Slowly instill 1mL hydrogen peroxide solution (H2O2, 30wt.%), finally using dilute hydrochloric acid (HCl, 1mol/L), solution ph is transferred to 1-
In the range of 2, as prepare contains Ti4+The precursor solution of ion；
C () is immersed in Ti in step (b) the absorbent cotton cleaning up in step (a)4+In the precursor solution of ion, close
Be enclosed in glass jar, 80 DEG C standing 24 hours after, take out absorbent cotton, scrubbed, be dried after obtain be loaded with TiO2's
Absorbent cotton；
D () is finally being loaded with TiO2Absorbent cotton be placed in N2In atmosphere furnace, it is increased to 500 with the heating rate of 2 DEG C/min
DEG C, insulation obtains TiO in 3 hours2- carbon fiber nanometer composite material.
As shown in Figure 1a, the TiO of embodiment 1 preparation2The XRD figure of-carbon fiber nanometer composite material and Anatase TiO2's
Standard diffraction peak (JCPDS No.21-1272) is consistent it was demonstrated that wherein oxide is the TiO of Anatase2Material.Fig. 2 a and
Fig. 2 b is respectively the TiO of embodiment 1 preparation2- carbon fiber nanometer composite material amplifies 2000 and 20000 times of SEM figure, shows this
The microstructure of sample is nano-TiO2Homoepitaxial is in carbon fiber surface, wherein nano-TiO2Pattern be pin arranged in a uniform
Shape cluster, about 10 microns of carbon fiber diameter, up to～0.5cm, carbon fiber surface assumes many gullies.Fig. 3 is prepared for embodiment 1
TiO2The TGA curve chart of-carbon fiber nanometer composite material, is warmed up to 350 DEG C in air atmosphere, and sample starts substantially to lose
Weight, this is because, caused by the carbon fiber burning in composite, up to 498.2 DEG C, carbon fiber burns completely, remaining TiO2
Account for the 41.76% of sample gross mass, the TiO prepared by embodiment 1 is described2TiO is contained in-carbon fiber nanometer composite material2For
41.76wt%.
Embodiment 2
The method that the present embodiment prepares ZnO- carbon fiber nanometer composite material, comprises the following steps：
A () first, weighs 0.1g business absorbent cotton, deionized water cleans up, stand-by；
(b) and then, weigh 0.44g bis- acetate hydrate zinc (Zn (Ac)2·2H2O) it is dissolved in 30mL deionized water, stirring is molten
Solution, then it is slowly added into 0.40g sodium hydroxide (NaOH), continue stirring and be allowed to be completely dissolved, as prepare contains Zn2+Ion
Precursor solution；
C () is immersed in Zn in step (b) the absorbent cotton cleaning up2+In the precursor solution of ion, it is sealed in glass
In wide mouthed bottle, after 80 DEG C of standings 24 hours, take out absorbent cotton, scrubbed, be dried after obtain and be loaded with the absorbent cotton of ZnO；
D () is finally placed in N the absorbent cotton being loaded with ZnO2In atmosphere furnace, it is increased to 500 with the heating rate of 2 DEG C/min
DEG C, insulation obtains ZnO- carbon fiber nanometer composite material in 3 hours.
As shown in Figure 1 b, the XRD figure of the ZnO- carbon fiber nanometer composite material of embodiment 2 preparation, the mark with hexagonal phase ZnO
Quasi- diffraction maximum (JCPDS No.79-0205) is consistent it was demonstrated that wherein oxide is the ZnO material of hexagonal phase.Fig. 2 c and Fig. 2 d divides
Not Wei embodiment 2 preparation ZnO- carbon fiber nanometer composite material amplify 5000 and 10000 times SEM figure, show this sample
Microstructure is that nano-ZnO is grown in the groove of carbon fiber surface, and the pattern of wherein nano-ZnO is platy particle.Fig. 4 is real
Apply the TGA curve chart of the ZnO- carbon fiber nanometer composite material of example 2 preparation, be warmed up to 340 DEG C in air atmosphere, sample starts
Substantially weightless, this is because, caused by the carbon fiber burning in composite, up to 478.7 DEG C, carbon fiber burns completely, remaining
Lower ZnO accounts for the 36.34wt% of sample gross mass, illustrates to contain ZnO in the ZnO- carbon fiber nanometer composite material prepared by embodiment 2
For 36.34wt%.
Embodiment 3
The present embodiment prepares Fe2O3The method of-carbon fiber nanometer composite material, comprises the following steps：
A () first, weighs 0.1g business absorbent cotton, deionized water cleans up, stand-by；
(b) and then, weigh 0.54g Iron(III) chloride hexahydrate (FeCl3·6H2O) it is dissolved in 30mL deionized water, stirring is molten
Solution, as prepare contains Fe3+The precursor solution of ion；
C () is immersed in Fe in step (b) the absorbent cotton cleaning up3+In the precursor solution of ion, it is sealed in glass
In wide mouthed bottle, 90 DEG C standing 24 hours after, take out absorbent cotton, scrubbed, be dried after obtain be loaded with Fe2O3Absorbent cotton；
D () is finally being loaded with Fe2O3Absorbent cotton be placed in N2In atmosphere furnace, it is increased to the heating rate of 2 DEG C/min
500 DEG C, insulation obtains Fe in 3 hours2O3- carbon fiber nanometer composite material.
As illustrated in figure 1 c, the Fe of embodiment 3 preparation2O3The XRD figure of-carbon fiber nanometer composite material, with Emission in Cubic γ-
Fe2O3Standard diffraction peak (JCPDS No.4-755) consistent it was demonstrated that wherein oxide is the γ-Fe of Emission in Cubic2O3Material.
Fig. 2 e and Fig. 2 f is respectively the Fe of embodiment 3 preparation2O3- carbon fiber nanometer composite material amplifies 1000 and 20000 times of SEM figure,
The microstructure showing this sample is nanometer Fe2O3Homoepitaxial is in carbon fiber surface, wherein nanometer Fe2O3Pattern be distribution
Uniform spheroidal particle.Fig. 5 is the Fe of embodiment 3 preparation2O3The TGA curve chart of-carbon fiber nanometer composite material, in air gas
It is warmed up to 330 DEG C, sample starts obvious weightlessness, this is because the carbon fiber burning in composite is caused under atmosphere, until
487.8 DEG C, carbon fiber burns completely, remaining Fe2O3Account for the 27.43wt% of sample gross mass, illustrate prepared by embodiment 3
Fe2O3Fe is contained in-carbon fiber nanometer composite material2O3For 27.43wt%.
Metal oxide precursor in above-described embodiment 1, embodiment 2 and embodiment 3 is replaced with other solubility gold
Belong to salt such as zinc nitrate, ferric nitrate, cobaltous chloride, Nickel dichloride., butter of tin, titanous chloride., or homemade de- using natural cotton
Fat cotton, macromolecular fibre replace the business absorbent cotton in above-described embodiment, also can get other similar to above-described embodiment
Metal oxide-carbon fiber nano composite material.
Embodiment described above is only that the preferred embodiment of the present invention is described, the not model to the present invention
Enclose and be defined, on the premise of without departing from design spirit of the present invention, the technical side to the present invention for the those of ordinary skill in the art
Various modifications and improvement that case is made, all should fall in the protection domain of claims of the present invention determination.
Claims (5)
1. a kind of method preparing metal oxide-carbon fiber nano composite material it is characterised in that：Comprise the following steps：
A () weighs absorbent cotton, after deionized water cleans up, stand-by；
B () weighs slaine and is dissolved in deionized water, prepare the precursor solution containing respective metal ion, wherein metal ion
Concentration in the range of 0.05～0.1mol/L, described slaine is titanium potassium oxalate, two acetate hydrate zinc, in Iron(III) chloride hexahydrate
One kind；
C () is immersed in the precursor solution of metal ion described in step (b) the described absorbent cotton after cleaning in step (a)
In, after 80-100 DEG C of standing 12-24 hour, take out absorbent cotton, scrubbed, be dried after obtain and be loaded with the de- of metal-oxide
Fat cotton；
D () is finally placed in the absorbent cotton being loaded with metal-oxide in step (c) in nitrogen furnace, be warming up to 500-600 DEG C of guarantor
Warm 2-5 hour, obtains metal oxide-carbon fiber nano composite material；
Metal-oxide described in step (d) is TiO2、ZnO、Fe2O3One of.
2. the method preparing metal oxide-carbon fiber nano composite material according to claim 1 it is characterised in that：
In step (d), the pattern of metal-oxide has needle-like cluster arranged in a uniform, platy particle or the spheroidal particle being evenly distributed.
3. the method preparing metal oxide-carbon fiber nano composite material according to claim 1 it is characterised in that：
The mass fraction of the nano composite material containing metal oxide obtained in step (d) is in the range of 20%～50%.
4. the method preparing metal oxide-carbon fiber nano composite material according to claim 1 it is characterised in that：
The absorbent cotton being loaded with metal-oxide described in step (d) is placed in nitrogen furnace, and heating rate is 2 DEG C/min.
5. the method preparing metal oxide-carbon fiber nano composite material according to claim 1-4 any one, its
It is characterised by：Absorbent cotton described in step (a) is business absorbent cotton, utilizes the homemade absorbent cotton of natural cotton.
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| CN105413672A (en) * | 2015-11-25 | 2016-03-23 | 天津中材工程研究中心有限公司 | Nano-zinc oxide and carbon fiber composite material and preparation method thereof |
| CN106057486B (en) * | 2016-05-11 | 2018-08-24 | 温州大学 | A kind of carbon ball-silicon/iron oxide composite material and preparation method thereof and purposes |
| CN106207188A (en) * | 2016-08-16 | 2016-12-07 | 安徽师范大学 | Three-dimensional ultra-thin C-base composte material and its preparation method and application |
| CN106206060A (en) * | 2016-09-25 | 2016-12-07 | 桂林理工大学 | The preparation of cobalt hydroxide@carbon fiber nanometer composite material and electrode material for super capacitor application |
| CN107331854B (en) * | 2017-08-23 | 2020-02-11 | 吉林大学 | Composite electrode material with multi-stage nanostructure and prepared by coating carbon fiber loaded with metal nanoparticles with transition metal oxide |
| CN109216036A (en) * | 2017-12-25 | 2019-01-15 | 南京大学 | The preparation method of carbon fibre cloth load iron oxide nano-wire flexible electrode |
| CN108686649B (en) * | 2018-05-09 | 2020-09-29 | 济南大学 | Mn based on absorbent cotton biological form3O4/ZnO/ACFs micromotor photocatalyst and application thereof |
| CN108640165B (en) * | 2018-05-15 | 2020-07-03 | 武汉中科先进技术研究院有限公司 | Metal oxide nano-structure composite material and preparation method thereof |
| CN108565132B (en) * | 2018-05-15 | 2019-09-27 | 中国科学院深圳先进技术研究院 | A kind of fibrous material and preparation method thereof with metal oxide nanostructure |
| CN108993506A (en) * | 2018-08-10 | 2018-12-14 | 张家港市汇鼎新材料科技有限公司 | A kind of preparation method of Fe2O3 doping titanium dioxide-carbon fibre composite |
| CN109768288B (en) * | 2018-12-27 | 2021-10-29 | 浙江工业大学 | Biomorphic Ni-Li/C catalyst and preparation method and application thereof |
| CN110429247A (en) * | 2019-07-05 | 2019-11-08 | 合肥国轩高科动力能源有限公司 | A kind of lithium ion battery three-dimensional ZnO/C composite negative pole material and preparation method thereof |
| CN110950302B (en) * | 2019-12-16 | 2021-05-11 | 中盈志合吉林科技股份有限公司 | Hydrogen storage alloy containing cobalt oxide and cobalt boron of carbon fiber micron tube and preparation method thereof |
| CN113470981B (en) * | 2021-05-28 | 2022-08-16 | 湖南大学 | Preparation method of porous carbon fiber/metal oxide composite material and graphene-based conductive ink and application of porous carbon fiber/metal oxide composite material and graphene-based conductive ink in supercapacitor |
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| CN103066294B (en) * | 2013-01-28 | 2015-02-04 | 福州大学 | Method for preparing lithium battery material by using plant fibers |
| CN103730645B (en) * | 2014-01-17 | 2015-11-18 | 江苏华盛精化工股份有限公司 | Coated carbon fiber nanometer composite material of a kind of silicon and its preparation method and application |
| CN103746099B (en) * | 2014-01-17 | 2015-10-28 | 江苏华盛精化工股份有限公司 | The preparation method of the carbon fibre material of a kind of tin ash parcel, product and application |
| CN104014302B (en) * | 2014-07-11 | 2016-06-29 | 上海大学 | The preparation method of magnesium oxide-mesoporous carbon composite material |
| CN104157832B (en) * | 2014-09-04 | 2016-09-28 | 湖北工程学院 | A kind of preparation method of ferroferric oxide/carbon composite lithium ion battery material |
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