CN105244181A - Spinel type metal oxide of high specific capacitance and preparation and application of metal oxide - Google Patents

Spinel type metal oxide of high specific capacitance and preparation and application of metal oxide Download PDF

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CN105244181A
CN105244181A CN201510524161.5A CN201510524161A CN105244181A CN 105244181 A CN105244181 A CN 105244181A CN 201510524161 A CN201510524161 A CN 201510524161A CN 105244181 A CN105244181 A CN 105244181A
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metal oxide
spinel
type metal
specific capacitance
solution
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CN105244181B (en
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轩海成
张永庆
李慧
康利涛
韩培德
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Taiyuan University of Technology
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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
    • 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
    • Y02E60/13—Energy storage using capacitors

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Abstract

The invention relates to a spinel type metal oxide of high specific capacitance. A general chemical formula of the metal oxide is MnxCo2O<3+x>, and x is greater than or equivalent to 1 and lower than or equivalent to 6. A preparation method of the metal oxide comprises the following steps that a Co(NO3)2.6H2O solution of 1mol/L and a Mn(NO3)2 solution of 0.5-1.5mol/L are mixed and fully stirred, an organic fuel is added while the mol ratio of metal ions to the organic fuel is controlled between 0.4 and 4.0, the solution is stirred for 20-60 min so that a uniform mixed solution is formed, the mixed solution is arranged in box type furnace of 300 to 450 DEG C and burned, thermal insulation is kept for 1.5 to 4h, and a sample is removed to obtain spinel type metal oxide powder. The metal oxide can be used as an electrode material of a super capacitor, raw materials are abundant, easy to take and low in the cost, the super capacitor made of the metal oxide is excellent in performance, high in the specific capacitance, high in the power multiplying performance and high in circulation stability.

Description

Spinel-type metal oxide of high specific capacitance characteristic and preparation method thereof and application
Technical field
The spinel-type metal oxide that the invention belongs in chemical field and Material Field is prepared and is applied, specifically a kind of spinel-type metal-oxide powder with high specific capacitance characteristic and preparation method thereof and application.
Background technology
From new energy technology development and should being used for, along with developing rapidly of electronics and information industry in recent years, the requirement of people to power supply energy density and cycle performance is more and more higher, facilitates the development of the electrochemical power source of high power capacity and high cyclical stability.Energy is considered to, to a kind of very favourable the substituting of nature fossil fuel energy sources, become the important channel alleviating world energy sources and ambient pressure by the conversion of electrochemical system.In this context, ultracapacitor arises at the historic moment, it is otherwise known as electrochemical capacitor or capacitor with super capacity, it is a kind of Novel energy storage apparatus between conventional electrostatic capacitor and storage battery, there is the features such as high-power output, high charge-discharge efficiencies, long circulation life, very well compensate for the shortcoming that conventional electrostatic capacitor energy storage density is little and storage battery power density is low, especially ultracapacitor is more suitable for big current charge/discharge occasion, has broad application prospects in mobile communication, electric automobile etc.
Ultracapacitor is a kind of energy-storage travelling wave tube utilizing the electrochemical process of electrode/solution surface to store electric charge.Double electric layer capacitor adopts high-specific surface area material with carbon element to make the capacitor of electrode, adsorb respectively based on the surface of positive and negative ion between carbon electrode and electrolyte interface, cause the electrical potential difference between two electrodes thus realize a kind of energy storage device of energy storage, but because it stores electric charge mainly from electric double layer capacitance, therefore specific capacity is lower, and the raising of chemical property is extremely restricted.Faradic pseudo-capacitor is the capacitor adopting transition metal oxide or conducting polymer to do electrode, quick and reversible oxidation/reduction reaction occurs at electrode surface and nearly surface and produces electric capacity thus realize energy storage device, and transition metal oxide is by reversible faraday reaction occurs at Cathode/Solution Interface, the Faraday pseudo-capacitance much larger than material with carbon element electric double layer capacitance can be produced.
The metal oxide electrode material of current report can be divided into metal oxide containing precious metals (RuO 2) and based on the oxide of the transition metal such as Ni, Co, Mn, V and hydrate electrode material thereof.RuO 2the representative of noble metal oxide electrodes material, its conductivity higher than material with carbon element, and at H 2sO 4stablize in water solution system, capacity is high, internal resistance is little, is a kind of electrode material for super capacitor of excellent performance.Although RuO 2as electrode material for super capacitor, there is plurality of advantages, as high in conductivity, specific capacity is high, have extended cycle life and high rate performance excellent etc., be the ideal oxide electrode material found at present.Due to RuO 2price and costliness thereof, be difficult to realize large-scale commercial and use.Have multiple oxidation state due to Mn element, therefore the oxide of manganese is of a great variety.In transition metal oxide, the oxide of Mn, Ni, Co element and hydrate thereof have optimum fake capacitance performance.When as electrode material for super capacitor, modal Mn oxide is MnO 2, NiO has height ratio capacity, but high rate performance and cyclical stability poor, Co 3o 4although specific capacity is lower, there is good high rate performance and cyclical stability.And spinel type composite metal oxide is the complex oxide be composited by two or more metal oxides, chemical formula can be write as AB 2o 4or ABCO 4, wherein A is a kind of metallic element, and B is another kind of metallic element; Possesses the characteristic of corresponding various metal oxide sometimes simultaneously.
The method preparing metal oxide materials at present mainly contains hydro thermal method, liquid-phase precipitation method, sol-gel process, electrochemical deposition method and low-temperature solid-phase method etc., but the material that most methods prepares is as super capacitor material poor performance.
Summary of the invention
The object of the invention is to there is good high rate performance and cyclical stability and a kind of spinel-type metal oxide with high specific capacitance characteristic to provide.
Technical scheme of the present invention:
A kind of containing spinel-type metal oxide, it is characterized in that: its chemical general formula is Mn xco 2o 3+x, wherein the value of x is 1≤x≤6.
The described preparation method containing spinel-type metal oxide is as follows: by 1mol/LCo (NO 3) 26H 2o, 0.5 ~ 1.5mol/LMn (NO 3) 2solution mixing is also fully stirred, add organic-fuel again and the mol ratio controlling metal ion and organic-fuel is 0.4 ~ 4.0, stirring 20 ~ 60min makes it form homogeneous mixture solotion, box type furnace mixed solution being placed in 300 ~ 450 DEG C makes it burn, insulation 1.5 ~ 4h is continued from burning starts immediately, take out sample, just obtain spinel-type metallic oxide nano powder.
Described organic-fuel comprises glycine, citric acid, urea.
Described battery and the electrical equipment original paper field being applied to ultracapacitor or lithium ion battery and other big current demands containing spinel-type metal oxide.
Spinel-type metal oxide of the present invention has higher ratio capacitance characteristic, the feature that its raw materials for production are cheap, preparation process is simple, production efficiency is high, low for equipment requirements, of many uses.
Spinel-type metallic oxide nano powder prepared by the present invention can reach 497F/g under 0.5A/g current density, can be applicable to the fields such as ultracapacitor, lithium ion and sodium-ion battery, of many uses.
Accompanying drawing explanation
Fig. 1 is the MnCo obtained by embodiment 6 to embodiment 10 2o 4spinel oxides powder XRD curve.
Fig. 2 is the general formula obtained by embodiment 6 is MnCo 2o 4the typical scan electromicroscopic photograph of spinel oxides powder.
Fig. 3 is the general formula obtained by embodiment 13 is MnO 2/ MnCo 2o 4the typical scan electromicroscopic photograph of spinel oxides powder.
Fig. 4 is the general formula obtained by embodiment 7 is MnCo 2o 4the cyclic voltammetric relation curve of spinel oxides powder.
Fig. 5 is the general formula obtained by embodiment 11 is MnO 2/ MnCo 2o 4the constant current charge-discharge relation curve of spinel oxides powder.
Fig. 6 is the MnO obtained by embodiment 11 2/ MnCo 2o 4the ratio capacitance-charging and discharging currents density relationship curve of spinel oxides powder.
Embodiment
A kind of containing spinel-type metal oxide, it is characterized in that: its chemical general formula is Mn xco 2o 3+x, wherein the value of x is 1≤x≤6.
The described preparation method containing spinel-type metal oxide is as follows: by 1mol/LCo (NO 3) 26H 2o, 0.5 ~ 1.5mol/LMn (NO 3) 2solution mixing is also fully stirred, add certain organic-fuel again and the mol ratio controlling metal ion and organic-fuel is 0.4 ~ 4.0, stirring 20 ~ 60min makes it form homogeneous mixture solotion, box type furnace mixed solution being placed in 300 ~ 450 DEG C makes it burn, what burning started plays continuation insulation 1.5 ~ 4h at once, take out sample, just obtain spinel-type metal-oxide powder.
Described organic-fuel is glycine, citric acid or urea.
When organic-fuel is glycine, the chemical equation in above-mentioned preparation process is:
M n ( NO 3 ) 2 + 2 C o ( NO 3 ) 2 + 2 yC 2 H 5 NO 2 + ( 9 2 y - 7 ) O 2 &RightArrow; MnCo 2 O 4 + ( 3 + y ) N 2 + 4 yCO 2 + 5 yH 2 O , 0.375 &le; y &le; 3.75
The described spinel-type metal oxide that contains is applied to ultracapacitor or lithium ion battery
And the battery of other big current demands and electric elements field.
Below in conjunction with specific embodiment, the present invention is further described.
Embodiment 1
Configuration Mn (NO 3) 2with Co (NO 3) 2mixed solution, control Mn in solution 2+/ Co 2+ratio is 1:2.Citric acid (C is added in mixed solution 6h 8o 7), make (Mn 2++ Co 2+)/C 6h 8o 7mol ratio is 1.92.Magnetic agitation 30min, is then placed in box type furnace (Muffle furnace) and is incubated at 300 DEG C and makes it burn by precursor liquid, what burning started rise at once continues insulation 2h, takes out and naturally cools to room temperature collection product.
Embodiment 2
Configuration Mn (NO 3) 2with Co (NO 3) 2mixed solution, control Mn in solution 2+/ Co 2+ratio is 1:2.Citric acid (C is added in mixed solution 6h 8o 7), make (Mn 2++ Co 2+)/C 6h 8o 7mol ratio is 1.0.Magnetic agitation 30min, is then placed in box type furnace and is incubated at 350 DEG C and makes it burn by precursor liquid, what burning started rise at once continues insulation 2h, takes out and cool to room temperature collects product.
Embodiment 3
Configuration Mn (NO 3) 2with Co (NO 3) 2mixed solution, control Mn in solution 2+/ Co 2+ratio is 1:2.Citric acid (C is added in mixed solution 6h 8o 7), make (Mn 2++ Co 2+)/C 6h 8o 7mol ratio is 0.65.Magnetic agitation 30min, is then placed in box type furnace and is incubated at 400 DEG C and makes it burn by precursor liquid, what burning started rise at once continues insulation 2h, takes out and cool to room temperature collects product.
Embodiment 4
Configuration Mn (NO 3) 2with Co (NO 3) 2mixed solution, control Mn in solution 2+/ Co 2+ratio is 1:2.Urea (CO (NH is added in mixed solution 2) 2), make (Mn 2++ Co 2+)/CO (NH 2) 2mol ratio is 0.65.Magnetic agitation 30min, is then placed in box type furnace and is incubated at 350 DEG C and makes it burn by precursor liquid, what burning started rise at once continues insulation 2h, takes out and cool to room temperature collects product.
Embodiment 5
Configuration Mn (NO 3) 2with Co (NO 3) 2mixed solution, control Mn in solution 2+/ Co 2+ratio is 1:2.Urea (CO (NH is added in mixed solution 2) 2), make (Mn 2++ Co 2+)/CO (NH 2) 2mol ratio is 1.29.Magnetic agitation 30min, is then placed in box type furnace and is incubated at 400 DEG C and makes it burn by precursor liquid, what burning started rise at once continues insulation 2h, takes out and cool to room temperature collects product.
Embodiment 6
Configuration Mn (NO 3) 2with Co (NO 3) 2mixed solution, control Mn in solution 2+/ Co 2+ratio is 1:2.Glycine (C is added in mixed solution 2h 5nO 2), make (Mn 2++ Co 2+)/C 2h 5nO 2mol ratio is 3.86.Magnetic agitation 30min, is then placed in box type furnace and is incubated at 300 DEG C and makes it burn by precursor liquid, what burning started rise at once continues insulation 2h, takes out and cool to room temperature collects product.
Embodiment 7
Configuration Mn (NO 3) 2with Co (NO 3) 2mixed solution, control Mn in solution 2+/ Co 2+ratio is 1:2.Glycine (C is added in mixed solution 2h 5nO 2), make (Mn 2++ Co 2+)/C 2h 5nO 2mol ratio is 1.92.Magnetic agitation 30min, is then placed in box type furnace and is incubated at 300 DEG C and makes it burn by precursor liquid, what burning started rise at once continues insulation 3h, takes out and cool to room temperature collects product.
Embodiment 8
Configuration Mn (NO 3) 2with Co (NO 3) 2mixed solution, control Mn in solution 2+/ Co 2+ratio is 1:2.Glycine (C is added in mixed solution 2h 5nO 2), make (Mn 2++ Co 2+)/C 2h 5nO 2mol ratio is 0.96.Magnetic agitation 30min, is then placed in box type furnace and is incubated at 300 DEG C and makes it burn by precursor liquid, what burning started rise at once continues insulation 2h, takes out and cool to room temperature collects product.
Embodiment 9
Configuration Mn (NO 3) 2with Co (NO 3) 2mixed solution, control Mn in solution 2+/ Co 2+ratio is 1:2.Glycine (C is added in mixed solution 2h 5nO 2), make (Mn 2++ Co 2+)/C 2h 5nO 2mol ratio is 0.64.Magnetic agitation 30min, is then placed in box type furnace and is incubated at 400 DEG C and makes it burn by precursor liquid, what burning started rise at once continues insulation 4h, takes out and cool to room temperature collects product.
Embodiment 10
Configuration Mn (NO 3) 2with Co (NO 3) 2mixed solution, control Mn in solution 2+/ Co 2+ratio is 1:2.Glycine (C is added in mixed solution 2h 5nO 2), make (Mn 2++ Co 2+)/C 2h 5nO 2mol ratio is 0.48.Magnetic agitation 30min, is then placed in box type furnace and is incubated at 300 DEG C and makes it burn by precursor liquid, what burning started rise at once continues insulation 4h, takes out and cool to room temperature collects product.
Embodiment 11
Configuration Mn (NO 3) 2with Co (NO 3) 2mixed solution, control Mn in solution 2+/ Co 2+ratio is 3:4.Glycine (C is added in mixed solution 2h 5nO 2), make (Mn 2++ Co 2+)/C 2h 5nO 2mol ratio is 2.0.Magnetic agitation 30min, is then placed in box type furnace and is incubated at 300 DEG C and makes it burn by precursor liquid, what burning started rise at once continues insulation 2h, takes out and cool to room temperature collects product.
Embodiment 12
Configuration Mn (NO 3) 2with Co (NO 3) 2mixed solution, control Mn in solution 2+/ Co 2+ratio is 4:4.Glycine (C is added in mixed solution 2h 5nO 2), make (Mn 2++ Co 2+)/C 2h 5nO 2mol ratio is 2.0.Magnetic agitation 30min, is then placed in box type furnace and is incubated at 300 DEG C and makes it burn by precursor liquid, what burning started rise at once continues insulation 2h, takes out and cool to room temperature collects product.
Embodiment 13
Configuration Mn (NO 3) 2with Co (NO 3) 2mixed solution, control Mn in solution 2+/ Co 2+ratio is 5:4.Glycine (C is added in mixed solution 2h 5nO 2), make (Mn 2++ Co 2+)/C 2h 5nO 2mol ratio is 2.1.Magnetic agitation 30min, is then placed in box type furnace and is incubated at 300 DEG C and makes it burn by precursor liquid, what burning started rise at once continues insulation 2h, takes out and cool to room temperature collects product.
Embodiment 14
Configuration Mn (NO 3) 2with Co (NO 3) 2mixed solution, control Mn in solution 2+/ Co 2+ratio is 6:4.Glycine (C is added in mixed solution 2h 5nO 2), make (Mn 2++ Co 2+)/C 2h 5nO 2mol ratio is 2.1.Magnetic agitation 30min, is then placed in box type furnace and is incubated at 300 DEG C and makes it burn by precursor liquid, what burning started rise at once continues insulation 2h, takes out and cool to room temperature collects product.

Claims (5)

1. a spinel-type metal oxide for high specific capacitance characteristic, is characterized in that: its chemical general formula is Mn xco 2o 3+x, wherein the value of x is 1≤x≤6.
2. the spinel-type metal oxide of a kind of high specific capacitance characteristic as claimed in claim 1, is characterized in that its preparation method comprises the steps: 1mol/LCo (NO 3) 26H 2o, 0.5 ~ 1.5mol/LMn (NO 3) 2solution mixing is also fully stirred, add organic-fuel again and the mol ratio controlling metal ion and organic-fuel is 0.4 ~ 4.0, stirring 20 ~ 60min makes it form homogeneous mixture solotion, box type furnace mixed solution being placed in 300 ~ 450 DEG C makes it burn, continue insulation 1.5 ~ 4h, take out sample, just obtain spinel-type metal-oxide powder.
3. the spinel-type metal oxide of a kind of high specific capacitance characteristic as claimed in claim 2, is characterized in that described above-mentioned organic-fuel comprises glycine, citric acid, urea.
4. the spinel-type metal oxide of a kind of high specific capacitance characteristic as claimed in claim 1, is characterized in that it is applied to ultracapacitor or lithium ion battery and electric elements field.
5. the spinel-type metal oxide of high specific capacitance characteristic as claimed in claim 1, is characterized in that it is applied to electric elements field.
CN201510524161.5A 2015-08-24 2015-08-24 Spinel-type metal oxide of high specific capacitance characteristic and the preparation method and application thereof Active CN105244181B (en)

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CN108238648A (en) * 2018-03-26 2018-07-03 淮北师范大学 A kind of preparation method of lithium ion battery negative material
CN109003829A (en) * 2018-08-07 2018-12-14 东北大学秦皇岛分校 Controlled capacitance material and its preparation method and application under a kind of electric field
CN111029171A (en) * 2019-12-24 2020-04-17 江苏理工学院 Porous AB without adhesive2O4Preparation method of @ M electrode

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Publication number Priority date Publication date Assignee Title
CN108238648A (en) * 2018-03-26 2018-07-03 淮北师范大学 A kind of preparation method of lithium ion battery negative material
CN109003829A (en) * 2018-08-07 2018-12-14 东北大学秦皇岛分校 Controlled capacitance material and its preparation method and application under a kind of electric field
CN111029171A (en) * 2019-12-24 2020-04-17 江苏理工学院 Porous AB without adhesive2O4Preparation method of @ M electrode

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