CN106024412B - Have carbon nanotube/metal oxide composite and the preparation of high specific capacitance characteristic - Google Patents

Have carbon nanotube/metal oxide composite and the preparation of high specific capacitance characteristic Download PDF

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CN106024412B
CN106024412B CN201610528574.5A CN201610528574A CN106024412B CN 106024412 B CN106024412 B CN 106024412B CN 201610528574 A CN201610528574 A CN 201610528574A CN 106024412 B CN106024412 B CN 106024412B
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carbon nanotube
metal oxide
specific capacitance
mixed solution
oxide composite
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轩海成
徐曰魁
何宏伟
张永庆
张拓
吴亚飞
陈峰华
李慧
韩培德
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Taiyuan University of Technology
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Abstract

It is a kind of have high specific capacitance characteristic carbon nanotube/metal oxide composite and preparation, belong to new material, the chemical general formula of the metal oxide is NixMoO3+x, the value of x is 1≤x≤3；Preparation method: by metal salt Ni (NO3)2·6H2O and (NH4)6Mo7O24·4H2O is mixed to form solution and is sufficiently stirred, it adds organic-fuel and the molar ratio for controlling metal ion and organic-fuel is 0.4 ~ 10.0, stir 30 min, form homogeneous mixture solotion, add acidification carbon nanotube, ultrasonic disperse 40min forms mixed solution, and mixed solution is placed in full combustion in 200 ~ 450 DEG C of batch-type furnace, continues 0.5 ~ 2h of heat preservation.Electrode material of the present invention as supercapacitor, not only raw material rich reserves are easy to get, cheap, and super capacitor performance is excellent, and specific capacitance is big, and high rate performance is high, and cyclical stability is preferable.

Description

Have carbon nanotube/metal oxide composite and the preparation of high specific capacitance characteristic
Technical field
The invention belongs in chemical field and Material Field spinel-type metal oxide and Nano carbon tube-metal aoxidize The preparation and its application of object composite material, carbon nanotube/metal oxide composite wood of specifically a kind of tool high specific capacitance characteristic Material and preparation.
Background technique
With the rapid development of social economy, the demand to nonrenewable resources such as petroleum, coals is increasing and has withered The trend exhausted.At the same time, exhaust gas caused by the use of these energy, caused greenhouse effects are so that global warming has become Undisputable fact, this is both the hot spot of global concern, and increasingly deep Problems of Socialization.
Since entry into 21st century, economize on resources with environmental protection have become society focus, people to green energy resource with And the demand of practicable environmental protection measure is more more and more intense.Develop as a result, renewable green energy resource become solve these problems Effective selection.Wherein, the conversion that energy passes through electrochemical system is considered as one kind ten to nature fossil fuel energy sources Divide advantageous substitution.
From the point of view of new energy technology development and application, with the fast development of automobile, electronics and information industry in recent years, people Demand to energy density and power density it is higher and higher, promote the development of high-capacity power supply system.With new energy Research and development reach its maturity, and new energy is successfully applied on automobile, become the research focus of utilization of new energy resources.Supercapacitor goes out Now solves the problems, such as this, it is a kind of a kind of novel energy storage apparatus between conventional electrostatic capacitor and secondary cell. The capacity of supercapacitor has reached farad rank, and compared to conventional electrostatic capacitor, its capacity has risen to 3 to 4 quantity Grade, power density is higher by battery an order of magnitude, and it is small and store very well to compensate for conventional electrostatic capacitor energy storage density The low disadvantage of cell power density, especially supercapacitor are more suitable for high current charge/discharge occasion.It is in national economy, section It is widely used in technology and daily life, has to alleviating energy and environment crisis, improving human living standard Great influence, it has also become a new hot spot of global economic development.
Storage device of the electrochemical capacitor as energy, storage electricity number show as the size of capacitor, such as fill The capacitor generated when electric include: pass through at electrode/solution/interface it is double caused by the aligning of electronics and ion or dipole Electric layer capacitor；On the two-dimensional space or quasi- two-dimensional space in electrode surface or body phase, electroactive material carries out underpotential deposition, The chemisorption and redox reaction of high reversible occurs, generates faraday's (counterfeit) capacitor related with electrode charge current potential. In the case where identical electrode area, the capacity of the latter is the former 10-100 times.Fake capacitance electrode mainly uses transition golden Category and its compound or the conducting polymer of doping, late nineteen eighties have developed with RuO2For the pseudo-capacitance capacitor of electrode, However because Ru's is expensive, this kind of capacitor is difficult to realize civilian commercialization, only first in aerospace, military etc. at present It is used on into equipment.The oxide of other transient metal Mns of cheaper, Ni, Co, V etc. becomes the effective of research and development pseudocapacitors Selection, and because its stable voltage window is small, the more low factor of energy density prepares the bimetal composite oxygen of high specific capacitance performance Compound, the shared property for making it have the two and its above element is current research hotspot.
Summary of the invention
The present invention is proposed with high specific capacitance and good high rate performance and with a kind of tool high specific capacitance of good stability Carbon nanotube/metal oxide composite of characteristic and preparation.
Technical solution of the present invention:
A kind of carbon nanotube/metal oxide composite having high specific capacitance characteristic, the chemistry of the metal oxide General formula is NixMoO3+x, wherein the value of x is 1≤x≤3.
A kind of preparation method of high specific capacitance characteristic spinel-type metal oxide composite, include the following steps: by Ni(NO3)2·6H2O(nickel nitrate)；(NH4)6Mo7O24·4H2O(ammonium molybdate) it is mixed to form solution and is sufficiently stirred；It has added Machine fuel and the molar ratio for controlling metal ion and organic-fuel are 0.4 ~ 10.0,20 ~ 60 min of stirring formed uniformly mix it is molten Liquid；Acidification carbon nanotube (CNT) is added, the concentration of carbon nanotube is 0.5 ~ 4mg/ in the solution after acidification carbon nanotube is added Ml, ultrasonic disperse handle 20 ~ 60min and form mixed solution；Mixed solution is placed in 200 ~ 450 DEG C of batch-type furnace and is sufficiently fired It burns, keeps the temperature 0.5 ~ 2h, obtain the spinel-type metal-oxide powder containing carbon nanotube.
It is described acidification carbon nanotube refer to carbon nanotube by 10% nitric acid solution 70 ~ 90 DEG C at a temperature of carry out 6 ~ The processing of 12 h ultrasonic disperses.
The organic-fuel includes glycine, citric acid, urea.
The spinel-type metal oxide and Nano carbon tube-metal oxide composite be applied to supercapacitor or The battery and electric appliance original part field of lithium ion battery and other high current demands.
Spinel-type metal oxide containing carbon nanotube specific capacitance characteristic with higher of the invention, production are former Expect that cheap, preparation process is simple, high production efficiency, feature low for equipment requirements, is widely used.
Spinel-type metal-oxide powder prepared by the present invention containing carbon nanotube can under 1 A/g current density Up to 1037 F/g, it can be applied to the fields such as supercapacitor, lithium ion and sodium-ion battery, it is widely used.
Detailed description of the invention
Fig. 1 is the NiMoO obtained by embodiment 1 ~ 54Spinel oxides powder XRD curve.
Fig. 2 is that the general formula obtained by embodiment 3 is CNT/ NiMoO4Nano carbon tube-metal oxide composite powder The typical scan electromicroscopic photograph of body.
Fig. 3 is that the general formula obtained by embodiment 6 is CNT/ NiMoO4Nano carbon tube-metal oxide composite powder The cyclic voltammetric relation curve of body.
Fig. 4 is that the general formula obtained by embodiment 6 is CNT/ NiMoO4Nano carbon tube-metal oxide composite powder The constant current charge-discharge relation curve of body.
Fig. 5 is the CNT/ NiMoO obtained by embodiment 2,6,74Spinel oxides powder specific capacitance-charge and discharge Electric current density relation curve.
Specific embodiment
Has carbon nanotube/metal oxide composite of high specific capacitance characteristic, the chemical general formula of metal oxide is NixMoO3+x, wherein the value of x is 1≤x≤6.
A kind of preparation method of the spinel-type metal oxide composite of high specific capacitance characteristic include the following steps: by Ni(NO3)2·6H2O, (NH4)6Mo7O24·4H2O metal salt is mixed to form solution and is sufficiently stirred；It adds organic-fuel and controls The molar ratio of metal ion and organic-fuel processed is 0.5 ~ 10.0, and 30 min of stirring form it into homogeneous mixture solotion；Acid is added Carbon nano tube, the concentration that carbon nanotube in the solution after being acidified carbon nanotube is added is 0.5 ~ 4mg/ ml, ultrasonic disperse 40min forms mixed solution；Mixed solution is placed in 200 ~ 450 DEG C of batch-type furnace makes its full combustion, and keeps the temperature 0.5 ~ 3 H obtains composite spinelle type metal-oxide powder.
Acidification carbon nanotube refers to 6 ~ 12h ultrasound point at a temperature of nitric acid solution and 70 ~ 90 DEG C of the carbon nanotube Jing Guo 10% Dissipate processing.
The organic-fuel includes glycine, citric acid, urea.
When organic-fuel is citric acid, the chemical equation in above-mentioned preparation process is:
7Ni(NO3)2+(NH4)6Mo7O24+xC6H8O7 +(x-13)O2→7NiMoO4+6xCO2↑+10N2↑+(12+4x) H2O
0.5<X<10；
The spinel-type metal oxide and Nano carbon tube-metal oxide composite be applied to supercapacitor or The battery and electric elements field of lithium ion battery and other high current demands.
Below with reference to specific embodiment, the present invention is further described.
Embodiment 1
Configure Ni (NO3)2(NH4)6Mo7O24Mixed solution, control solution in Ni2+/Mo2+Ratio is 1:1.To mixing Citric acid (C is added in solution6H8O7), chemical equation is
7Ni(NO3)2+(NH4)6Mo7O24+xC6H8O7 +(x-13)O2→7NiMoO4+6xCO2↑+10N2↑+(12+4x) H2O；
As x=6.5 ÷ 9,30 min of magnetic agitation；Acidification carbon nanotube is added, makes carbon nanotube concentration in mixed solution For 0.5mg/ml, ultrasonic disperse, which handles 40min, becomes precursor liquid, and then precursor liquid is placed in batch-type furnace (Muffle furnace) 300 Heat preservation makes its burning at DEG C, and the subsequent continuation of insurance temperature 30min of full combustion takes out and naturally cools to room temperature and collects product.
Embodiment 2
Configure Ni (NO3)2(NH4)6Mo7O24Mixed solution, control solution in Ni2+/Mo2+Ratio is 1:1.
Citric acid (C is added into mixed solution6H8O7), chemical equation is
7Ni(NO3)2+(NH4)6Mo7O24+xC6H8O7 +(x-13)O2→7NiMoO4+6xCO2↑+10N2↑+(12+4x) H2O；
As x=13 ÷ 9,30 min of magnetic agitation；Acidification carbon nanotube is added, makes carbon nanotube concentration in mixed solution For 0.5mg/ml, ultrasonic disperse, which handles 40min, becomes precursor liquid, and then precursor liquid is placed in batch-type furnace (Muffle furnace) 300 Heat preservation makes its burning at DEG C, and the subsequent continuation of insurance temperature 30min of full combustion takes out and naturally cools to room temperature and collects product.
Embodiment 3
Configure Ni (NO3)2(NH4)6Mo7O24Mixed solution, control solution in Ni2+/Mo2+Ratio is 1:1.To mixing Citric acid (C is added in solution6H8O7), chemical equation is
7Ni(NO3)2+(NH4)6Mo7O24+xC6H8O7 +(x-13)O2→7NiMoO4+6xCO2↑+10N2↑+(12+4x) H2O；
As x=26 ÷ 9,30 min of magnetic agitation；Acidification carbon nanotube is added, makes carbon nanotube concentration in mixed solution For 0.5mg/ml, ultrasonic disperse, which handles 40min, becomes precursor liquid, and then precursor liquid is placed in batch-type furnace (Muffle furnace) 300 Heat preservation makes its burning at DEG C, and the subsequent continuation of insurance temperature 30min of full combustion takes out and naturally cools to room temperature and collects product.
Embodiment 4
Configure Ni (NO3)2(NH4)6Mo7O24Mixed solution, control solution in Ni2+/Mo2+Ratio is 1:1.To mixing Citric acid (C is added in solution6H8O7), chemical equation is
7Ni(NO3)2+(NH4)6Mo7O24+xC6H8O7 +(x-13)O2→7NiMoO4+6xCO2↑+10N2↑+(12+4x) H2O；
As x=39 ÷ 9,30 min of magnetic agitation;Acidification carbon nanotube is added, keeps carbon nanotube in mixed solution dense Degree is 0.5mg/ml, and ultrasonic disperse, which handles 40min, becomes precursor liquid, and then precursor liquid is placed in batch-type furnace (Muffle furnace) Heat preservation makes its burning at 300 DEG C, and the subsequent continuation of insurance temperature 30min of full combustion takes out and naturally cools to room temperature and collects product.
Embodiment 5
Configure Ni (NO3)2(NH4)6Mo7O24Mixed solution, control solution in Ni2+/Mo2+Ratio is 1:1.To mixing Citric acid (C is added in solution6H8O7), chemical equation is
7Ni(NO3)2+(NH4)6Mo7O24+xC6H8O7 +(x-13)O2→7NiMoO4+6xCO2↑+10N2↑+(12+4x) H2O；
As x=52 ÷ 9,30 min of magnetic agitation；Acidification carbon nanotube is added, makes carbon nanotube concentration in mixed solution For 0.5mg/ml, ultrasonic disperse, which handles 40min, becomes precursor liquid, and then precursor liquid is placed in batch-type furnace (Muffle furnace) 300 Heat preservation makes its burning at DEG C, and the subsequent continuation of insurance temperature 30min of full combustion takes out and naturally cools to room temperature and collects product.
Embodiment 6
Configure Ni (NO3)2(NH4)6Mo7O24Mixed solution, control solution in Ni2+/Mo2+Ratio is 1:1.
Citric acid (C is added into mixed solution6H8O7), chemical equation is
7Ni(NO3)2+(NH4)6Mo7O24+xC6H8O7 +(x-13)O2→7NiMoO4+6xCO2↑+10N2↑+(12+4x) H2O；
As x=13 ÷ 9,30 min of magnetic agitation;Acidification carbon nanotube is added, keeps carbon nanotube in mixed solution dense Degree is 1mg/ml, and ultrasonic disperse, which handles 40min, becomes precursor liquid, and then precursor liquid is placed in batch-type furnace (Muffle furnace) 300 Heat preservation makes its burning at DEG C, and the subsequent continuation of insurance temperature 30min of full combustion takes out and naturally cools to room temperature and collects product.
Embodiment 7
Configure Ni (NO3)2(NH4)6Mo7O24Mixed solution, control solution in Ni2+/Mo2+Ratio is 1:1.
Citric acid (C is added into mixed solution6H8O7), chemical equation is 7Ni (NO3)2+(NH4)6Mo7O24+xC6H8O7 +(x-13)O2→7NiMoO4+6xCO2↑+10N2↑+(12+4x)H2O；
As x=13 ÷ 9,30 min of magnetic agitation；Acidification carbon nanotube is added, makes carbon nanotube concentration in mixed solution For 2mg/ml, ultrasonic disperse, which handles 40min, becomes precursor liquid, and then precursor liquid is placed in batch-type furnace (Muffle furnace) at 300 DEG C Lower heat preservation makes its burning, and the subsequent continuation of insurance temperature 30min of full combustion takes out and naturally cools to room temperature and collects product.
Illustrate: after " precursor liquid " described in above-described embodiment refers to that all salt are completely dissolved, preparation is put into batch-type furnace Solution.

Claims (3)

1. a kind of carbon nanotube/metal oxide composite for having high specific capacitance characteristic, it is characterized in that configuration Ni (NO3)2With (NH4)6Mo7O24Mixed solution, control solution in Ni2+/Mo2+Ratio is 1:1, and citric acid is added into mixed solution (C6H8O7), chemical equation is
7Ni(NO3)2+(NH4)6Mo7O24+xC6H8O7 +(x-13)O2→7NiMoO4+6xCO2↑+10N2↑+(12+4x)H2O；
30 min of magnetic agitation；Acidification carbon nanotube is added, makes carbon nanotube concentration 0.5mg/ml in mixed solution, ultrasound point Dissipating processing 40min becomes precursor liquid, and precursor liquid, which is then placed in batch-type furnace the heat preservation at 300 DEG C, makes its burning, full combustion Subsequent continuation of insurance temperature 30min takes out and naturally cools to room temperature and collects product NiMoO4；X is following any one numbers:
(1) ÷ of x=6.5 9；
(2) ÷ of x=13 9；
(3) ÷ of x=26 9；
(4) ÷ of x=39 9；
(5) ÷ of x=52 9.
2. a kind of carbon nanotube/metal oxide composite for having high specific capacitance characteristic as described in claim 1, feature It is: is applied to supercapacitor or lithium ion battery.
3. a kind of carbon nanotube/metal oxide composite for having high specific capacitance characteristic as described in claim 1, feature It is: is applied to electric elements field.
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CN101255544A (en) * 2008-03-21 2008-09-03 中国科学院上海硅酸盐研究所 Method for preparing nano metal or metal oxide/carbon nano-tube composite material
CN104752067A (en) * 2015-03-27 2015-07-01 新疆大学 Microwave-assisted method of nickel molybdate graphene composite material used for capacitor

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