CN104167295A - Carbon nano tube surface loaded nano cobaltosic oxide composite material and preparation method thereof - Google Patents
Carbon nano tube surface loaded nano cobaltosic oxide composite material and preparation method thereof Download PDFInfo
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- CN104167295A CN104167295A CN201410134471.1A CN201410134471A CN104167295A CN 104167295 A CN104167295 A CN 104167295A CN 201410134471 A CN201410134471 A CN 201410134471A CN 104167295 A CN104167295 A CN 104167295A
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Abstract
The embodiment of the invention discloses a carbon nano tube surface loaded nano cobaltosic oxide composite material and a preparation method thereof. The preparation method comprises the following steps: deionized water and DMF are weighed according to a ratio of 1:1 to 1:9 to obtain a mixed solvent; purified carbon nano tube and the mixed solvent are weighed according to the compounding concentration of 0.1-1g/L, and ultrasonic processing is performed for 10-60min; cobalt(II) acetate tetrahydrate of which the concentration is 10-60g/L relative to carbon nano tube dispersion liquid is weighed, and cobalt(II) acetate tetrahydrate is dispersed in the carbon nano tube dispersion liquid and stirred evenly; the obtained mixed solution is put in a hydrothermal tank with a tetrafluoroethylene liner and then cooled along with a furnace; after the solution is cooled to room temperature, black deposits are cleaned by a centrifuge; and baking is performed until a sample is dried. Co3O4 particles of the carbon nano tube surface loaded nano cobaltosic oxide composite material prepared by the method are cubic and uniform in size, have a side length smaller than 7nm, and are uniformly distributed on the surface of the carbon nano tube.
Description
Technical field
The invention belongs to field of nanocomposite materials, relate to a kind of CNT (carbon nano-tube) area load nano-cobaltic-cobaltous oxide (Co
3o
4) composite material and preparation method thereof, this composite material can be used for catalysis, ultracapacitor or lithium ion cell electrode.
Background technology
Cobaltosic oxide Co
3o
4be a kind of important inorganic material, have huge application prospect in fields such as electrochemistry, catalyst, magnetic fluid, biomedicines.By preparation nano Co
3o
4can significantly improve Co
3o
4activity, thereby improve Co
3o
4in the performance in each field.But nano Co
3o
4easily produce and reunite, conventionally all need nano material to be coated on specific carrier material, thereby reach the object such as activity and stability thereof that improves nano material.Carbon nano-tube (CNT) stable chemical nature, has excellent electricity, calorifics, mechanics, optics, magnetic performance, has high-specific surface area as monodimension nanometer material, and limiting proportion surface area can reach 2630m
2/ g, becomes comparatively desirable support materials.Preparation not only can effectively disperse Co with carbon nano-tube is compound
3o
4, and be more conducive to improve the ability of material conduction electron, improve the electric conductivity of material, thereby can improve its application performance in fields such as catalysis, ultracapacitor or lithium ion batteries.
The existing Co preparing in CNT (carbon nano-tube)
3o
4nano particle exists that distribution density is low, nanoparticle size is excessive, distribution of sizes is inhomogeneous, in carbon nano-tube skewness or have the problem of agglomeration, thereby affect carbon nano-tube/Co
3o
4the performance of composite material.The shape of oxide and size are very large on the impact of performance, at present, and the Co preparing in carbon nano-tube
3o
4and other oxide is mainly taking spherical as main, and cube Co
3o
4under identical volume, have than spherical larger specific area, will likely obtain more excellent performance.The present invention prepared on CNT (carbon nano-tube) surface mutual dispersion, size evenly, be evenly distributed, nano cubic Co that particle is tiny
3o
4.
Summary of the invention
For addressing the above problem, the object of the present invention is to provide a kind of CNT (carbon nano-tube) area load nano-cobaltic-cobaltous oxide composite material and preparation method thereof, the Co of the CNT (carbon nano-tube) area load nano-cobaltic-cobaltous oxide composite material of preparing by the method
3o
4particle is cube, and evenly, the length of side is less than 7nm to size, has each other certain space, is about 1-10nm, is evenly distributed on CNT (carbon nano-tube) surface.
For achieving the above object, technical scheme of the present invention is:
A preparation method for CNT (carbon nano-tube) area load nano-cobaltic-cobaltous oxide composite material, comprises the following steps:
The ratio of taking is 1: 1-1: 9 deionized water and dimethyl formamide DMF, obtain mixed solvent after mixing and stirring;
Take purified CNT (carbon nano-tube) after treatment and mixed solvent by the matched proportion density of 0.1-1g/L, CNT (carbon nano-tube) is put into mixed solvent and carry out ultrasonic 10-60 minute, obtain CNT (carbon nano-tube) dispersion liquid;
Take four hydration cobalt acetates, cobalt is II valency, and wherein four hydration cobalt acetates are 10-60g/L with respect to the concentration of CNT (carbon nano-tube) dispersion liquid, and four hydration cobalt acetates are dissolved in to CNT (carbon nano-tube) dispersion liquid, stirs;
Above mixed solution is put into the hydro-thermal tank with tetrafluoroethene liner, wherein the filling volume ratio of hydro-thermal tank is 1/5-1/2, is warmed up to 100-150 DEG C with the programming rate of 1 DEG C/min-10 DEG C/min, and temperature retention time is 1.5h-10h, after cooling with stove;
After cool to room temperature, solution is poured out, black deposit is cleaned with centrifuge, cleaning fluid adopts alcoholic solution, and the number of times of cleaning is at 3-5 time;
The black deposit having cleaned is baked to sample drying at 40-80 DEG C, obtains CNT (carbon nano-tube) area load nano-cobaltic-cobaltous oxide composite material.
Preferably, the concrete purification step of purified CNT (carbon nano-tube) after treatment is: the carbon nano-tube that 0.5g chemical vapour deposition (CVD) CVD method is prepared joins in 100ml red fuming nitric acid (RFNA), first ultrasonic dispersion 30min, after add hot reflux 4h, remove the catalyst granules in carbon nano-tube and connect corresponding functional group in carbon nano tube surface, mixture cooled and filtered, cleans until filtrate is neutral dry 6h at 100 DEG C in air repeatedly with deionized water.
And, a kind of CNT (carbon nano-tube) area load nano-cobaltic-cobaltous oxide composite material, described CNT (carbon nano-tube) area load nano-cobaltic-cobaltous oxide composite material is prepared by method as previously discussed, and cobaltosic oxide material becomes nano cubic even structure to be attached to the surface of CNT (carbon nano-tube).
Preferably, the size of described nano cubic structure is less than 7nm, Co
3o
4gap between nano cubic particle is 1-10nm.
Compared with prior art, beneficial effect of the present invention is as follows:
(1) Co of carbon nano tube surface
3o
4nano particle is evenly distributed, this Co
3o
4particle advantages of good crystallization, is isometric particle, and evenly, the length of side is less than 7nm to size, has each other even space, is about 1-10nm, is evenly distributed on the surface of CNT (carbon nano-tube);
(2) CNT (carbon nano-tube) has larger specific area, good conductivity and thermal conduction characteristic, carbon nano-tube and Co
3o
4particle close contact, is conducive to the fast transport of electronics.
(3) CNT (carbon nano-tube) and cobaltosic oxide nano Interaction between particles, has avoided the accumulation again of carbon pipe and the reunion of oxide nano particles.
(4) this method preparation process is simple and controlled and repeatable good, is suitable for volume production.
Brief description of the drawings
Fig. 1 is the preparation method's of the CNT (carbon nano-tube) area load nano-cobaltic-cobaltous oxide composite material of the embodiment of the present invention flow chart of steps;
Fig. 2 is the one scan Electronic Speculum figure of the CNT (carbon nano-tube) area load nano-cobaltic-cobaltous oxide composite material of the embodiment of the present invention;
Fig. 3 is the another scanning electron microscope (SEM) photograph of the CNT (carbon nano-tube) area load nano-cobaltic-cobaltous oxide composite material of the embodiment of the present invention;
Fig. 4 is the transmission electron microscope picture through the CNT (carbon nano-tube) area load nano-cobaltic-cobaltous oxide composite material of the embodiment of the present invention;
Fig. 5 is through the XRD of the CNT (carbon nano-tube) area load nano-cobaltic-cobaltous oxide composite material of embodiment of the present invention figure.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearer, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein, only in order to explain the present invention, is not intended to limit the present invention.
On the contrary, the present invention contain any defined by claim in marrow of the present invention and scope, make substitute, amendment, equivalent method and scheme.Further, for the public is had a better understanding to the present invention, in below details of the present invention being described, detailed some specific detail sections of having described.Do not have for a person skilled in the art the description of these detail sections can understand the present invention completely yet.
Referring to Fig. 1, be depicted as the preparation method's of a kind of CNT (carbon nano-tube) area load nano-cobaltic-cobaltous oxide composite material of the embodiment of the present invention flow chart of steps, it comprises the following steps:
S10, the ratio of taking is 1: 1-1: 9 deionized water and dimethyl formamide DMF, obtain mixed solvent after mixing and stirring;
S20, takes purified CNT (carbon nano-tube) after treatment and mixed solvent by the matched proportion density of 0.1-1g/L, CNT (carbon nano-tube) is put into mixed solvent and carry out ultrasonic 10-60 minute, obtains CNT (carbon nano-tube) dispersion liquid;
Wherein, in concrete application example, the concrete purification step of CNT (carbon nano-tube) can be, the carbon nano-tube that 0.5g chemical vapour deposition (CVD) CVD method is prepared joins in 100ml red fuming nitric acid (RFNA), first ultrasonic dispersion 30min, after add hot reflux 4h, remove the catalyst granules in carbon nano-tube and connect corresponding functional group in carbon nano tube surface, mixture cooled and filtered, cleans until filtrate is neutral dry 6h at 100 DEG C in air repeatedly with deionized water.
S30, takes four hydration cobalt acetates, and cobalt is II valency, and wherein four hydration cobalt acetates are 10-60g/L with respect to the concentration of CNT (carbon nano-tube) dispersion liquid, and four hydration cobalt acetates are dissolved in to CNT (carbon nano-tube) dispersion liquid, stirs;
In concrete application example below, be that four hydration cobalt acetates of II valency are referred to as four hydration cobalt acetates (II) by cobalt.
S40, above mixed solution is put into the hydro-thermal tank with tetrafluoroethene liner, wherein the filling volume ratio of hydro-thermal tank is 1/5-1/2, be the 20%-50% that reaction solution volume accounts for hydro-thermal tank cumulative volume, programming rate with 1 DEG C/min-10 DEG C/min is warmed up to 100-150 DEG C, temperature retention time is 1.5h-10h, after cooling with stove;
S50, after cool to room temperature, pours out solution, black deposit is cleaned with centrifuge, and cleaning fluid adopts alcoholic solution, and the number of times of cleaning is at 3-5 time;
S60 is baked to sample drying by the black deposit having cleaned at 40-80 DEG C, obtains CNT (carbon nano-tube) area load nano-cobaltic-cobaltous oxide composite material.
Known by above preparation process explanation, the present invention adopts above method to prepare carbon nano tube surface loaded with nano cobaltosic oxide composite material, and preparation process is simple and controlled and repeatable good, is suitable for volume production.
Therefore, corresponding with method, further embodiment of this invention provides the carbon nano tube surface loaded with nano cobaltosic oxide of preparing by said method composite material, referring to Fig. 2 to Fig. 5, Fig. 2 and Fig. 3 are respectively the scanning electron microscope (SEM) photograph of carbon nano tube surface loaded with nano cobaltosic oxide composite material prepared by the embodiment of the present invention, Fig. 4 is transmission electron microscope picture, and Fig. 5 is XRD figure.From Fig. 2 to Fig. 4, cobaltosic oxide material becomes nano cubic even structure to be attached to the surface of CNT (carbon nano-tube), and the size of nano cubic structure is less than 7nm, Co
3o
4gap between nano cubic particle is 1-10nm.Referring to Fig. 5, in X-ray diffraction, can obviously see (002) diffraction maximum of CNT (carbon nano-tube).
To the preparation process of CNT (carbon nano-tube) area load nano-cobaltic-cobaltous oxide composite material be described by multiple specific embodiments below.The hydro-thermal tank using in specific embodiment is market and buys, and its typical volume is 20ml, 50ml, 100ml and 250ml.In specific embodiment, the cumulative volume of mixed solution can cover reaction solution volume and account for the 20%-50% of hydro-thermal tank cumulative volume in the adjustment of proportioning ratio.
Embodiment 1
Take DMF8ml, deionized water 2ml, stirs, and obtains mixed solvent.Take the CNT (carbon nano-tube) 4mg after purification process, CNT (carbon nano-tube) is put into mixed solvent and carry out ultrasonic 60 minutes, obtain CNT (carbon nano-tube) dispersion liquid.Take four hydration cobalt acetate (II) 400mg, four hydration cobalt acetates (II) are dissolved in and obtain CNT (carbon nano-tube) dispersion liquid, be stirred to completely and dissolve.Above solution is put into and had the hydro-thermal tank that the volume of tetrafluoroethene liner is 20ml, the cumulative volume that reaction solution accounts for hydro-thermal tank is about 50%, meets the filling volume proportion requirement of hydro-thermal tank, is warmed up to 120 DEG C with the programming rate of 1 DEG C/point, temperature retention time 1.5h, after cooling with stove.Microparticle is cleaned with centrifuge, clean and adopt alcoholic solution, the number of times of cleaning is at 5 times.At 40 DEG C, be baked to sample drying, obtain CNT (carbon nano-tube) area load nano-cobaltic-cobaltous oxide composite material.
Embodiment 2
Take DMF10ml, deionized water 10ml, stirs, and obtains solvent.Take the carbon nano-tube 2mg after purification process, CNT (carbon nano-tube) is put into solvent and carry out ultrasonic 10 minutes, obtain CNT (carbon nano-tube) dispersion liquid.Take four hydration cobalt acetate (II) 200mg, four hydration cobalt acetates (II) are dissolved in to mixed solvent, be stirred to completely and dissolve.Above solution is put into and had the hydro-thermal tank that the volume of tetrafluoroethene liner is 50ml, the cumulative volume that reaction solution accounts for hydro-thermal tank is about 40%, meets the filling volume proportion requirement of hydro-thermal tank, is warmed up to 150 DEG C with the programming rate of 5 DEG C/point, temperature retention time 5h, after cooling with stove.Microparticle is cleaned with centrifuge, clean and adopt alcoholic solution, the number of times of cleaning is at 3 times.At 80 DEG C, be baked to sample drying, obtain CNT (carbon nano-tube) area load nano-cobaltic-cobaltous oxide composite material.
Embodiment 3
Take DMF27ml, deionized water 3ml, stirs, and obtains solvent.Take the carbon nano-tube 30mg after purification process, carbon nano-tube is put into solvent and carry out ultrasonic 40 minutes, obtain CNT (carbon nano-tube) dispersion liquid.Take four hydration cobalt acetate (II) 1800mg, four hydration cobalt acetates (II) are dissolved in to mixed solvent, be stirred to completely and dissolve.Above solution is put into and had the hydro-thermal tank that the volume of tetrafluoroethene liner is 100ml, the cumulative volume that reaction solution accounts for hydro-thermal tank is about 30%, meets the filling volume proportion requirement of hydro-thermal tank, is warmed up to 130 DEG C with the programming rate of 10 DEG C/point, temperature retention time 10h, after cooling with stove.Microparticle is cleaned with centrifuge, clean and adopt alcoholic solution, the number of times of cleaning is at 5 times.At 60 DEG C, be baked to sample drying, obtain CNT (carbon nano-tube) area load nano-cobaltic-cobaltous oxide composite material.
Embodiment 4
Take DMF40ml, deionized water 10ml, stirs, and obtains solvent.Take the carbon nano-tube 30mg after purification process, carbon nano-tube is put into solvent and carry out ultrasonic 30 minutes, obtain CNT (carbon nano-tube) dispersion liquid.Take four hydration cobalt acetate (II) 1000mg, four hydration cobalt acetates (II) are dissolved in to mixed solvent, be stirred to completely and dissolve.Above solution is put into the hydro-thermal tank that volume is 250ml, and the cumulative volume that reaction solution accounts for hydro-thermal tank is about 20%, meets the filling volume proportion requirement of hydro-thermal tank, is warmed up to 140 DEG C with the programming rate of 5 DEG C/point, temperature retention time 4h, after cooling with stove.Microparticle is cleaned with centrifuge, clean and adopt alcoholic solution, the number of times of cleaning is at 4 times.At 40 DEG C, be baked to sample drying, obtain CNT (carbon nano-tube) area load nano-cobaltic-cobaltous oxide composite material.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments of doing within the spirit and principles in the present invention, be equal to and replace and improvement etc., within all should being included in protection scope of the present invention.
Claims (4)
1. a preparation method for CNT (carbon nano-tube) area load nano-cobaltic-cobaltous oxide composite material, is characterized in that, comprises the following steps:
S10, the ratio of taking is 1: 1-1: 9 deionized water and dimethyl formamide DMF, obtain mixed solvent after mixing and stirring;
S20, takes purified CNT (carbon nano-tube) after treatment and mixed solvent by the matched proportion density of 0.1-1g/L, CNT (carbon nano-tube) is put into mixed solvent and carry out ultrasonic 10-60 minute, obtains CNT (carbon nano-tube) dispersion liquid;
S30, takes four hydration cobalt acetates, and cobalt is II valency, and wherein four hydration cobalt acetates are 10-60g/L with respect to the concentration of CNT (carbon nano-tube) dispersion liquid, and four hydration cobalt acetates are dissolved in to CNT (carbon nano-tube) dispersion liquid, stirs;
S40, above mixed solution is put into the hydro-thermal tank with tetrafluoroethene liner, wherein the filling volume ratio of hydro-thermal tank is 1/5-1/2, is warmed up to 100-150 DEG C with the programming rate of 1 DEG C/min-10 DEG C/min, temperature retention time is 1.5h-10h, after cooling with stove;
S50, after cool to room temperature, pours out solution, black deposit is cleaned with centrifuge, and cleaning fluid adopts alcoholic solution, and the number of times of cleaning is at 3-5 time;
S60 is baked to sample drying by the black deposit having cleaned at 40-80 DEG C, obtains CNT (carbon nano-tube) area load nano-cobaltic-cobaltous oxide composite material.
2. the preparation method of CNT (carbon nano-tube) area load nano-cobaltic-cobaltous oxide composite material according to claim 1, it is characterized in that, in S20, the concrete purification step of purified CNT (carbon nano-tube) after treatment is: the carbon nano-tube that 0.5g chemical vapour deposition (CVD) CVD method is prepared joins in 100ml red fuming nitric acid (RFNA), first ultrasonic dispersion 30min, after add hot reflux 4h, remove the catalyst granules in carbon nano-tube and connect corresponding functional group in carbon nano tube surface, mixture cooled and filtered, repeatedly clean until filtrate is neutral with deionized water, dry 6h at 100 DEG C in air.
3. a CNT (carbon nano-tube) area load nano-cobaltic-cobaltous oxide composite material, is characterized in that, described CNT (carbon nano-tube) area load nano-cobaltic-cobaltous oxide composite material is prepared by the method as described in as arbitrary in claim 1-2, cobaltosic oxide Co
3o
4material becomes nano cubic even structure to be attached to the surface of CNT (carbon nano-tube).
4. CNT (carbon nano-tube) area load nano-cobaltic-cobaltous oxide composite material according to claim 3, is characterized in that, the size of described nano cubic structure is less than 7nm, Co
3o
4gap between nano cubic particle is 1-10nm.
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Cited By (7)
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| CN105390700A (en) * | 2015-11-16 | 2016-03-09 | 哈尔滨工业大学 | Method for modifying positive electrode of lithium ion battery by adding metal oxide/carbon composite material |
| CN108269976A (en) * | 2017-12-19 | 2018-07-10 | 中南大学 | Cobalt-based lithium ion battery negative material preparation method |
| CN110993969A (en) * | 2019-12-03 | 2020-04-10 | 哈尔滨工程大学 | Coquassia flower pistil hollow carbonization tube composite Co3O4H of (A) to (B)2O2Electro-reduction catalyst |
| CN111740083A (en) * | 2020-06-12 | 2020-10-02 | 新昌县华发机械股份有限公司 | Carbon-coated porous Co3O4Microsphere lithium ion battery cathode material and preparation method thereof |
| CN112611792A (en) * | 2020-12-01 | 2021-04-06 | 常州大学 | Multi-walled carbon nanotube/transition metal oxide non-enzymatic caffeic acid electrochemical sensor and preparation method thereof |
| CN113224329A (en) * | 2021-04-30 | 2021-08-06 | 南京工业大学 | Co3O4/MXene composite catalyst and preparation method and application thereof |
| CN113634255A (en) * | 2021-08-24 | 2021-11-12 | 武汉理工大学 | Loaded Co3O4Preparation method of granular nano carbon composite catalytic material |
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Cited By (7)
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|---|---|---|---|---|
| CN105390700A (en) * | 2015-11-16 | 2016-03-09 | 哈尔滨工业大学 | Method for modifying positive electrode of lithium ion battery by adding metal oxide/carbon composite material |
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| CN110993969A (en) * | 2019-12-03 | 2020-04-10 | 哈尔滨工程大学 | Coquassia flower pistil hollow carbonization tube composite Co3O4H of (A) to (B)2O2Electro-reduction catalyst |
| CN111740083A (en) * | 2020-06-12 | 2020-10-02 | 新昌县华发机械股份有限公司 | Carbon-coated porous Co3O4Microsphere lithium ion battery cathode material and preparation method thereof |
| CN112611792A (en) * | 2020-12-01 | 2021-04-06 | 常州大学 | Multi-walled carbon nanotube/transition metal oxide non-enzymatic caffeic acid electrochemical sensor and preparation method thereof |
| CN113224329A (en) * | 2021-04-30 | 2021-08-06 | 南京工业大学 | Co3O4/MXene composite catalyst and preparation method and application thereof |
| CN113634255A (en) * | 2021-08-24 | 2021-11-12 | 武汉理工大学 | Loaded Co3O4Preparation method of granular nano carbon composite catalytic material |
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Effective date of registration: 20190418 Address after: Room 2402, Building 1, Ocean International Center, Gongshu District, Hangzhou City, Zhejiang Province Patentee after: Zhejiang Yunmo Green Energy Technology Co., Ltd. Address before: 310018 2 street, Xiasha Higher Education Park, Hangzhou, Zhejiang Patentee before: Hangzhou Electronic Science and Technology Univ |
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Effective date of registration: 20210520 Address after: 310011 room 1202-9, Lantian business center, Gongshu District, Hangzhou City, Zhejiang Province Patentee after: Hangzhou ZhongMeng Intelligent Control Technology Group Co.,Ltd. Address before: Room 2402, Building 1, Ocean International Center, Gongshu District, Hangzhou City, Zhejiang Province Patentee before: ZHEJIANG CLOUD GRAPHENE GREEN ENERGY TECHNOLOGY Co.,Ltd. |