CN105244181B - Spinel-type metal oxide of high specific capacitance characteristic and the preparation method and application thereof - Google Patents

Spinel-type metal oxide of high specific capacitance characteristic and the preparation method and application thereof Download PDF

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CN105244181B
CN105244181B CN201510524161.5A CN201510524161A CN105244181B CN 105244181 B CN105244181 B CN 105244181B CN 201510524161 A CN201510524161 A CN 201510524161A CN 105244181 B CN105244181 B CN 105244181B
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mixed solution
spinel
burning
type metal
specific capacitance
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CN105244181A (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

Abstract

A kind of spinel-type metal oxide of high specific capacitance characteristic, its chemical general formula is MnxCo2O3+x, wherein the value of x is 1≤x≤6；Its preparation method includes the following steps: 1mol/L Co (NO3)2·6H2O, 0.5 ~ 1.5mol/L Mn (NO3)2Solution is mixed and is sufficiently stirred, it adds organic-fuel and the molar ratio for controlling metal ion and organic-fuel is 0.4 ~ 4.0,20 ~ 60min of stirring forms it into homogeneous mixture solotion, mixed solution is placed in 300 ~ 450 DEG C of batch-type furnace makes its burning, continue 1.5 ~ 4h of heat preservation, sample is taken out, spinel-type metal-oxide powder has just been obtained.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, good cycling stability.

Description

Spinel-type metal oxide of high specific capacitance characteristic and the preparation method and application thereof
Technical field
The invention belongs to the preparations of spinel-type metal oxide and its application in chemical field and Material Field, specifically A kind of spinel-type metal-oxide powder and the preparation method and application thereof with high specific capacitance characteristic.
Background technique
From the point of view of new energy technology development and application, with the rapid development of electronics and information industry in recent years, people couple The requirement of power supply energy density and cycle performance is higher and higher, promotes the electrochemical power source of high capacity and high circulation stability Development.The conversion that energy passes through electrochemical system is considered as replaces highly beneficial to one kind of nature fossil fuel energy sources In generation, becomes the important channel for alleviating world energy sources and environmental pressure.In this context, supercapacitor is come into being, it again quilt Referred to as electrochemical capacitor or capacitor with super capacity are a kind of novel storages between conventional electrostatic capacitor and battery Energy device, has the characteristics that high-power output, high charge-discharge efficiencies, long circulation life, very well compensates for conventional electrostatic electricity Container energy storage density is small and the low density disadvantage of battery power, especially supercapacitor are more suitable for high current discharge/charge electric field Close, mobile communication, in terms of have broad application prospects.
Supercapacitor is a kind of energy-storage travelling wave tube using electrode/solution surface electrochemical process storage charge.Double electricity Layer capacitor makees the capacitor of electrode using high-specific surface area carbon material, is based on positive and negative ion in carbon electrode and electrolyte circle It is adsorbed respectively on surface between face, causes the potential difference between two electrodes to realize a kind of energy storage device of energy storage, but Because it stores charge mainly from electric double layer capacitance, therefore specific capacity is lower, and the raising of chemical property is extremely restricted.Method Drawing pseudocapacitor is the capacitor that electrode is done using transition metal oxide or conducting polymer, is in electrode surface and nearly table Face occurs quick and reversible oxidation/reduction reaction and generates capacitor to realize energy storage device, and transition metal oxide is logical It crosses and reversible faraday's reaction occurs in Cathode/Solution Interface, can produce the counterfeit electricity of faraday much larger than carbon material electric double layer capacitance Hold.
The metal oxide electrode material reported at present can be divided into metal oxide containing precious metals (RuO2) and based on Ni, Co, Mn, V The oxide and its hydrate electrode material of equal transition metal.RuO2It is the representative of noble metal oxide electrodes material, conductance Rate is higher than carbon material, and in H2SO4Stable in water solution system, capacity height, internal resistance are small, are a kind of super capacitors haveing excellent performance Device electrode material.Although RuO2Have many advantages, such as electrode material for super capacitor, as conductivity is high, specific capacity is high, follows The ring service life is long and high rate performance is excellent etc., is presently found ideal oxide electrode material.Due to RuO2Price and It is expensive, it is difficult to realize that large-scale commercial uses.There are a variety of oxidation states, the oxide species of manganese due to Mn element Class is various.In transition metal oxide, the oxide and its hydrate of Mn, Ni, Co element have optimal fake capacitance performance. When as electrode material for super capacitor, the most common Mn oxide is MnO2, NiO possesses height ratio capacity, but high rate performance It is poor with cyclical stability, Co3O4Although specific capacity is lower, there is good high rate performance and cyclical stability.And point is brilliant Stone-type metal composite oxide is the complex oxide being combined by two or more metal oxides, and chemical formula can be write as AB2O4Or ABCO4, wherein A is a kind of metallic element, and B is another metallic element；It is provided simultaneously with corresponding various metals sometimes The characteristic of oxide.
The method for preparing metal oxide materials at present mainly has hydro-thermal method, liquid-phase precipitation method, sol-gel method, electrification Sedimentation and low-temperature solid-phase method etc. are learned, but the material that most methods are prepared is as super capacitor material poor performance.
Summary of the invention
The purpose of the invention is to provide with good high rate performance and cyclical stability and have high specific capacitance characteristic A kind of spinel-type metal oxide.
Technical solution of the present invention:
One kind containing spinel-type metal oxide, it is characterized in that: its chemical general formula is MnxCo2O3+x, wherein x takes Value is 1≤x≤6.
It is described containing spinel-type metal oxide the preparation method is as follows: by 1mol/L Co (NO3)2·6H2O, 0.5~ 1.5mol/L Mn(NO3)2Solution is mixed and is sufficiently stirred, and is added organic-fuel and is controlled rubbing for metal ion and organic-fuel , than being 0.4~4.0,20~60min of stirring forms it into homogeneous mixture solotion for you, and mixed solution is placed in 300~450 DEG C of case Make its burning in formula furnace, continues 1.5~4h of heat preservation instant since burning, take out sample, just obtained spinel-type metal Nm-class oxide powder.
The organic-fuel includes glycine, citric acid, urea.
It is described to be applied to supercapacitor or lithium ion battery and other high currents containing spinel-type metal oxide The battery of demand and electric appliance original part field.
Spinel-type metal oxide of the invention specific capacitance characteristic with higher, raw materials for production are cheap, make For process, simple, high production efficiency, feature low for equipment requirements, widely used.
Spinel-type metallic oxide nano powder prepared by the present invention reachable 497F/g under 0.5A/g current density, can It is widely used applied to fields such as supercapacitor, lithium ion and sodium-ion batteries.
Detailed description of the invention
Fig. 1 is the MnCo obtained by embodiment 6 to embodiment 102O4Spinel oxides powder XRD curve.
Fig. 2 is that the general formula obtained by embodiment 6 is MnCo2O4Spinel oxides powder typical scan Electronic Speculum shine Piece.
Fig. 3 is that the general formula obtained by embodiment 13 is MnO2/MnCo2O4Spinel oxides powder typical scan Electromicroscopic photograph.
Fig. 4 is that the general formula obtained by embodiment 7 is MnCo2O4Spinel oxides powder cyclic voltammetric relationship it is bent Line.
Fig. 5 is that the general formula obtained by embodiment 11 is MnO2/MnCo2O4Spinel oxides powder constant current charge and discharge Electric relation curve.
Fig. 6 is the MnO obtained by embodiment 112/MnCo2O4Spinel oxides powder specific capacitance-charge and discharge electricity Current density relation curve.
Specific embodiment
One kind containing spinel-type metal oxide, it is characterized in that: its chemical general formula is MnxCo2O3+x, wherein x takes Value is 1≤x≤6.
It is described containing spinel-type metal oxide the preparation method is as follows: by 1mol/L Co (NO3)2·6H2O, 0.5~ 1.5mol/L Mn(NO3)2Solution is mixed and is sufficiently stirred, and is added certain organic-fuel and is controlled metal ion and organic combustion The molar ratio of material is 0.4~4.0, and 20~60min of stirring forms it into homogeneous mixture solotion, and mixed solution is placed in 300~450 DEG C batch-type furnace in make its burning, rising at once for beginning of burning continues 1.5~4h of heat preservation, take out sample, just obtained spinelle Type metal-oxide powder.
The organic-fuel is glycine, citric acid or urea.
When organic-fuel is glycine, the chemical equation in above-mentioned preparation process is:
It is described to be applied to supercapacitor or lithium ion battery containing spinel-type metal oxide
And battery and the electric elements field of other high current demands.
Below with reference to specific embodiment, the present invention is further described.
Embodiment 1
Configure Mn (NO3)2With Co (NO3)2Mixed solution, control solution in Mn2+/Co2+Ratio is 1:2.To mixed solution Middle addition citric acid (C6H8O7), so that (Mn2++Co2+)/C6H8O7Molar ratio is 1.92.Magnetic agitation 30min, then by forerunner Liquid, which is placed in batch-type furnace (Muffle furnace) heat preservation at 300 DEG C, makes its burning, and rising at once for beginning of burning continues to keep the temperature 2h, takes out simultaneously It naturally cools to room temperature and collects product.
Embodiment 2
Configure Mn (NO3)2With Co (NO3)2Mixed solution, control solution in Mn2+/Co2+Ratio is 1:2.To mixed solution Middle addition citric acid (C6H8O7), so that (Mn2++Co2+)/C6H8O7Molar ratio is 1.0.Magnetic agitation 30min, then by forerunner Liquid, which is placed in batch-type furnace the heat preservation at 350 DEG C, makes its burning, and rising at once for beginning of burning continues to keep the temperature 2h, takes out and is cooled to room Temperature collects product.
Embodiment 3
Configure Mn (NO3)2With Co (NO3)2Mixed solution, control solution in Mn2+/Co2+Ratio is 1:2.To mixed solution Middle addition citric acid (C6H8O7), so that (Mn2++Co2+)/C6H8O7Molar ratio is 0.65.Magnetic agitation 30min, then by forerunner Liquid, which is placed in batch-type furnace the heat preservation at 400 DEG C, makes its burning, and rising at once for beginning of burning continues to keep the temperature 2h, takes out and is cooled to room Temperature collects product.
Embodiment 4
Configure Mn (NO3)2With Co (NO3)2Mixed solution, control solution in Mn2+/Co2+Ratio is 1:2.To mixed solution Middle addition urea (CO (NH2)2), so that (Mn2++Co2+)/CO(NH2)2Molar ratio is 0.65.Magnetic agitation 30min, then will before Driving liquid and being placed in batch-type furnace to keep the temperature at 350 DEG C makes its burning, and rising at once for beginning of burning continues to keep the temperature 2h, takes out and is cooled to Room temperature collects product.
Embodiment 5
Configure Mn (NO3)2With Co (NO3)2Mixed solution, control solution in Mn2+/Co2+Ratio is 1:2.To mixed solution Middle addition urea (CO (NH2)2), so that (Mn2++Co2+)/CO(NH2)2Molar ratio is 1.29.Magnetic agitation 30min, then will before Driving liquid and being placed in batch-type furnace to keep the temperature at 400 DEG C makes its burning, and rising at once for beginning of burning continues to keep the temperature 2h, takes out and is cooled to Room temperature collects product.
Embodiment 6
Configure Mn (NO3)2With Co (NO3)2Mixed solution, control solution in Mn2+/Co2+Ratio is 1:2.To mixed solution Middle addition glycine (C2H5NO2), so that (Mn2++Co2+)/C2H5NO2Molar ratio is 3.86.Magnetic agitation 30min, then will before Driving liquid and being placed in batch-type furnace to keep the temperature at 300 DEG C makes its burning, and rising at once for beginning of burning continues to keep the temperature 2h, takes out and is cooled to Room temperature collects product.
Embodiment 7
Configure Mn (NO3)2With Co (NO3)2Mixed solution, control solution in Mn2+/Co2+Ratio is 1:2.To mixed solution Middle addition glycine (C2H5NO2), so that (Mn2++Co2+)/C2H5NO2Molar ratio is 1.92.Magnetic agitation 30min, then will before Driving liquid and being placed in batch-type furnace to keep the temperature at 300 DEG C makes its burning, and rising at once for beginning of burning continues to keep the temperature 3h, takes out and is cooled to Room temperature collects product.
Embodiment 8
Configure Mn (NO3)2With Co (NO3)2Mixed solution, control solution in Mn2+/Co2+Ratio is 1:2.To mixed solution Middle addition glycine (C2H5NO2), so that (Mn2++Co2+)/C2H5NO2Molar ratio is 0.96.Magnetic agitation 30min, then will before Driving liquid and being placed in batch-type furnace to keep the temperature at 300 DEG C makes its burning, and rising at once for beginning of burning continues to keep the temperature 2h, takes out and is cooled to Room temperature collects product.
Embodiment 9
Configure Mn (NO3)2With Co (NO3)2Mixed solution, control solution in Mn2+/Co2+Ratio is 1:2.To mixed solution Middle addition glycine (C2H5NO2), so that (Mn2++Co2+)/C2H5NO2Molar ratio is 0.64.Magnetic agitation 30min, then will before Driving liquid and being placed in batch-type furnace to keep the temperature at 400 DEG C makes its burning, and rising at once for beginning of burning continues to keep the temperature 4h, takes out and is cooled to Room temperature collects product.
Embodiment 10
Configure Mn (NO3)2With Co (NO3)2Mixed solution, control solution in Mn2+/Co2+Ratio is 1:2.To mixed solution Middle addition glycine (C2H5NO2), so that (Mn2++Co2+)/C2H5NO2Molar ratio is 0.48.Magnetic agitation 30min, then will before Driving liquid and being placed in batch-type furnace to keep the temperature at 300 DEG C makes its burning, and rising at once for beginning of burning continues to keep the temperature 4h, takes out and is cooled to Room temperature collects product.
Embodiment 11
Configure Mn (NO3)2With Co (NO3)2Mixed solution, control solution in Mn2+/Co2+Ratio is 3:4.To mixed solution Middle addition glycine (C2H5NO2), so that (Mn2++Co2+)/C2H5NO2Molar ratio is 2.0.Magnetic agitation 30min, then will before Driving liquid and being placed in batch-type furnace to keep the temperature at 300 DEG C makes its burning, and rising at once for beginning of burning continues to keep the temperature 2h, takes out and is cooled to Room temperature collects product.
Embodiment 12
Configure Mn (NO3)2With Co (NO3)2Mixed solution, control solution in Mn2+/Co2+Ratio is 4:4.To mixed solution Middle addition glycine (C2H5NO2), so that (Mn2++Co2+)/C2H5NO2Molar ratio is 2.0.Magnetic agitation 30min, then will before Driving liquid and being placed in batch-type furnace to keep the temperature at 300 DEG C makes its burning, and rising at once for beginning of burning continues to keep the temperature 2h, takes out and is cooled to Room temperature collects product.
Embodiment 13
Configure Mn (NO3)2With Co (NO3)2Mixed solution, control solution in Mn2+/Co2+Ratio is 5:4.To mixed solution Middle addition glycine (C2H5NO2), so that (Mn2++Co2+)/C2H5NO2Molar ratio is 2.1.Magnetic agitation 30min, then will before Driving liquid and being placed in batch-type furnace to keep the temperature at 300 DEG C makes its burning, and rising at once for beginning of burning continues to keep the temperature 2h, takes out and is cooled to Room temperature collects product.
Embodiment 14
Configure Mn (NO3)2With Co (NO3)2Mixed solution, control solution in Mn2+/Co2+Ratio is 6:4.To mixed solution Middle addition glycine (C2H5NO2), so that (Mn2++Co2+)/C2H5NO2Molar ratio is 2.1.Magnetic agitation 30min, then will before Driving liquid and being placed in batch-type furnace to keep the temperature at 300 DEG C makes its burning, and rising at once for beginning of burning continues to keep the temperature 2h, takes out and is cooled to Room temperature collects product.

Claims (6)

1. a kind of spinel-type metal oxide of high specific capacitance characteristic, its chemical general formula is MnCo2O4；It is characterized in that: it Preparation method includes the following steps: 1 mol/L Co (NO3)2·6H2O, 0.5 ~ 1.5 mol/L Mn (NO3)2Solution mixes simultaneously It is sufficiently stirred, adds glycine and the molar ratio for controlling metal ion and glycine is 0.4 ~ 4.0, stir 20 ~ 60 min Homogeneous mixture solotion is formed it into, mixed solution is placed in 300 ~ 450 DEG C of batch-type furnace makes its burning, continues heat preservation 1.5 ~ 4 H takes out sample, has just obtained in 0.5 A/g electric current lower density being the spinel-type metal-oxide powder of 497 F/g MnCo2O4；Its chemical equation is:
。
2. a kind of spinel-type metal oxide of high specific capacitance characteristic according to claim 1, it is characterized in that described MnCo2O4Preparation method be: configuration Mn (NO3)2With Co (NO3)2Mixed solution, control mixed solution in Mn2+/Co2+Ratio For 1:2；Citric acid is added into mixed solution, so that (Mn2++Co2+)/C6H8O7Molar ratio is 1.92；Magnetic agitation 30 Min, being then placed in Muffle furnace the heat preservation at 300 DEG C makes its burning, and rising at once for beginning of burning continues to keep the temperature 2 h, takes Out and naturally cool to room temperature collection product.
3. a kind of spinel-type metal oxide of high specific capacitance characteristic according to claim 1, it is characterized in that described MnCo2O4Preparation method be: configuration Mn (NO3)2With Co (NO3)2Mixed solution, control mixed solution in Mn2+/Co2+Ratio For 1:2；Urea is added into mixed solution, so that (Mn2++Co2+)/CO (NH2)2Molar ratio is 0.65；Magnetic agitation 30 Min, being subsequently placed in batch-type furnace the heat preservation at 350 DEG C makes its burning, and rising at once for beginning of burning continues to keep the temperature 2 h, takes out And it is cooled to room temperature and collects product.
4. a kind of spinel-type metal oxide of high specific capacitance characteristic according to claim 1, it is characterized in that described MnCo2O4Preparation method be: configuration Mn (NO3)2With Co (NO3)2Mixed solution, control mixed solution in Mn2+/Co2+Ratio For 1:2；Glycine (C is added into mixed solution2H5NO2), so that (Mn2++Co2+)/C2H5NO2Molar ratio is 3.86；Magnetic force 30 min are stirred, and the heat preservation at 300 DEG C, which is subsequently placed in batch-type furnace, makes its burning, and rising at once for beginning of burning continues heat preservation 2 H takes out and is cooled to room temperature and collects product.
5. such as a kind of described in any item spinel-type metal oxides of high specific capacitance characteristic of claim 1 ~ 4, it is characterized in that It is applied to supercapacitor or field of lithium ion battery.
6. such as a kind of described in any item spinel-type metal oxides of high specific capacitance characteristic of claim 1 ~ 4, it is characterized in that It is applied to electric elements field.
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CN108238648B (en) * 2018-03-26 2019-12-24 淮北师范大学 Preparation method of lithium ion battery negative electrode material
CN109003829B (en) * 2018-08-07 2020-08-11 东北大学秦皇岛分校 Controllable capacitance material under electric field and preparation method and application thereof
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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