CN101593626B - Nano nickel oxide/carbon composite material and preparation method and application thereof - Google Patents
Nano nickel oxide/carbon composite material and preparation method and application thereof Download PDFInfo
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- CN101593626B CN101593626B CN2009100628734A CN200910062873A CN101593626B CN 101593626 B CN101593626 B CN 101593626B CN 2009100628734 A CN2009100628734 A CN 2009100628734A CN 200910062873 A CN200910062873 A CN 200910062873A CN 101593626 B CN101593626 B CN 101593626B
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- Y02E60/13—Energy storage using capacitors
Abstract
The invention discloses a nano nickel oxide/carbon composite material and a preparation method and application thereof. The material is a composite material comprises evenly mixed nano nickel oxide and conductive black carbon in percentage by weight: 30 to 90 percent of nickel oxide and 10 to 70 percent of conductive black carbon. The preparation method comprises the following steps: under the condition of ultrasonic vibration, mixing soluble nickel salt with conductive black carbon completely; then, carrying out quick reaction of nickel salt and ammonium hydrocarbonate in a mixed solvent system of organic solvent and water; and finally, preparing a finished product by adopting the steps of solid-liquid separation, washing, drying, calcinations, and the like. The preparation method has simple process and easy operation. The prepared nano nickel oxide/carbon composite material has the advantages of high specific capacity and strong heavy current discharge capability and can be used as an electrode material of super capacitors.
Description
Technical field
The present invention relates to a kind of nano nickel oxide, belong to the nano composite material technical field.
Background technology
Ultracapacitor is a kind of novel energy-storing device between physics electric capacity and storage battery; Have than much higher energy density of traditional capacitor and the power density more much bigger, integrate characteristics such as long-life, high power density, wide serviceability temperature scope, charging rate be fast than storage battery.These good characteristics of ultracapacitor have extremely widely it and use in fields such as traffic, radio communication, military affairs, clean energy resource system.Nickel oxide is because of having characteristics such as specific capacity height, serviceability temperature wide ranges, cost be low, attracts tremendous attention on the electrode material of ultracapacitor being used for.
It is raw material that Chinese patent CN1037957C discloses with nickel salt, carbonic hydroammonium or ammonium carbonate, through calcining the method for preparing nickel oxide down at 400～1000 ℃ after the liquid phase reactor.It is the highly purified spherical nickel oxide product of 5～150nm that this method can make average grain diameter; But this kind nickel oxide product itself is reunited easily; In the ultracapacitor assembling process, be difficult to mix, therefore be not suitable as electrode material for super capacitor and use with conductive agent.
U.S. Pat 7,066,976 have reported that the employing electro-catalytic process prepares the method for nano-nickel oxide; The particle diameter of product is 20～40nm, but should will produce a large amount of waste liquids and harmful substance in the preparation process, and is high to the processing requirements of product; Therefore production cost is high, is not suitable for large-scale production.
Chinese patent CN1887728A has reported the preparation method of a kind of electrochemical capacitor with nickel oxide.This method comes the dispersing nanometer particle to obtain the nickel oxide electrode material of high-ratio surface through adding surfactant.But the intermediate products nickel hydroxide must be through cyclic washing to remove unnecessary surfactant, and technical process is loaded down with trivial details.Face the problem how nickel oxide and conductive agent mate and mix in the electrode production process again equally.
It is the preparation method of the electrochemical capacitor of positive electrode active materials with the active carbon that deposits moisture nickel oxide that Chinese patent CN100416722C discloses a kind of.The moisture nickel oxide content of this method load is low, and the deposition on active carbon also comprises the process of mixing with conductive agent only at 1.0～14.0mg/g in the electrode production process.
Know problem such as the existing method ubiquity for preparing nickel oxide that aftertreatment technology is loaded down with trivial details, nano particle difficulties in dispersion, conductive agent are difficult to mix from above.
Summary of the invention
Technical problem to be solved by this invention is, a kind of nano nickel oxide and preparation method thereof and the electrode material purposes of nano nickel oxide as ultracapacitor are provided; This nano nickel oxide has height ratio capacity, advantage that large current discharging capability is strong, and the preparation method is simple, easy operating.
The technical scheme of nano nickel oxide of the present invention is: it is a kind of nano-nickel oxide and the mixed uniformly composite material of conductive carbon black; Wherein the weight percent content of nickel oxide is 30%～90%, and the weight percent content of conductive carbon black is 10%～70%.
Further technical scheme with additional technical feature is:
Described nano nickel oxide, the weight percent content of its nickel oxide are 50%～90%, and the weight percent content of conductive carbon black is 10%～50%.
Described nano nickel oxide, the weight percent content of its nickel oxide are 30%, and the weight percent content of conductive carbon black is 70%.
Described nano nickel oxide, the weight percent content of its nickel oxide are 90%, and the weight percent content of conductive carbon black is 10%.
Described nano nickel oxide, the weight percent content of its nickel oxide are 50%, and the weight percent content of conductive carbon black is 50%.
A kind of preparation method of above-mentioned nano nickel oxide; It is that soluble nickel salt is fully mixed with conductive carbon black; Nickel salt and carbonic hydroammonium are reacted rapidly; Thereby obtain the mixed uniformly composite material of a kind of nano-nickel oxide and conductive carbon black, may further comprise the steps:
(a) press the weight percent of conductive carbon black in the middle of composite material; Taking by weighing an amount of conductive carbon black powder joins in the middle of the aqueous solution of certain density nickel salt; Adding volume simultaneously is a certain proportion of organic solvent of above-mentioned liquor capacity, and the suspension-turbid liquid that forms is obtained mixed solution A with ultrasonic vibration;
(b) in the mixed solvent of organic solvent and water, add carbonic hydroammonium configuration mixed solution B, the kind of organic solvent and proportion and mixed solution A are consistent;
(c) above-mentioned solution A is stirred at a certain temperature, promptly add solution B subsequently, control nickel salt and the mol ratio of carbonic hydroammonium and the pH value of solution;
(d) Separation of Solid and Liquid is carried out to slurry in the back that reacts completely, and sediment is dry after with water washing, at last products therefrom is calcined, and promptly makes nano nickel oxide.
Further technical scheme with additional technical feature is:
The preparation method of described nano nickel oxide, its used nickel salt is at least a in Nickel dichloride hexahydrate, Nickelous nitrate hexahydrate, the six hydration nickel sulfate.
The preparation method of described nano nickel oxide, its used organic solvent is one or more the mixing in methyl alcohol, ethanol, isopropyl alcohol or the acetone.
The preparation method of described nano nickel oxide, it specifically may further comprise the steps:
(a) in the percentage by weight of conductive carbon black in the middle of composite material be 10%～50% ratio; Taking by weighing an amount of conductive carbon black powder joins in the middle of the aqueous solution of nickel salt that concentration is 0.01～1mol/L; Add volume simultaneously and be 10%～400% organic solvent of above-mentioned liquor capacity, it is that the ultrasonic vibration of 20～50KHz obtains mixed solution A that the suspension-turbid liquid that forms is used supersonic frequency;
(b) in the mixed solvent of organic solvent and water, add carbonic hydroammonium configuration mixed solution B, wherein the concentration of carbonic hydroammonium is 0.01～1mol/L, and the kind of organic solvent and proportion and mixed solution A are consistent;
(c) above-mentioned solution A is stirred under 15～35 ℃ temperature, add solution B subsequently, the mol ratio of control nickel salt and carbonic hydroammonium is 1: 2～7, and the pH value of solution is 7～9;
(d) Separation of Solid and Liquid is carried out to slurry in the back that reacts completely, and will precipitate and use water washing, after 50～150 ℃ of dryings, products therefrom 250～450 ℃ of following calcinings, is promptly made nano nickel oxide.
Above-mentioned nano nickel oxide is as the application of the electrode material of ultracapacitor.
The outstanding beneficial effect that the present invention compared with prior art has is:
(1) the nickel oxide nano powder body material just mixes with conductive carbon black in building-up process, has formed unimpeded conductive network in composite inner so on the one hand, makes it have high conductivity; The adding of material with carbon element has hindered intercrystalline collision of adjacent nickel oxide and fused process on the other hand, and it is dispersed preferably that the nickel oxide active material is had.
(2) this technical scheme has also been saved the blend step that nickel oxide electrode prepares active material and conductive agent in the process, the process of sizing mixing is simplified greatly, thereby has been reduced production cost.The result of charge-discharge test shows that the specific capacity of nano nickel oxide is high, large current discharging capability is strong.
Embodiment
A kind of nano nickel oxide is the mixed uniformly Powdered composite material of a kind of nano-nickel oxide and conductive carbon black, and wherein the weight percent content of nickel oxide is 30%～90%, and the weight percent content of conductive carbon black is 10%～70%.Specific embodiment is following:
Embodiment 1: described nano nickel oxide, the weight percent content of its nickel oxide are 50%～90%, and the weight percent content of conductive carbon black is 10%～50%.
Embodiment 2: described nano nickel oxide, the weight percent content of its nickel oxide are 30%, and the weight percent content of conductive carbon black is 70%.
Embodiment 3: described nano nickel oxide, the weight percent content of its nickel oxide are 90%, and the weight percent content of conductive carbon black is 10%.
Embodiment 4: described nano nickel oxide, the weight percent content of its nickel oxide are 50%, and the weight percent content of conductive carbon black is 50%.
A kind of preparation method of above-mentioned nano nickel oxide; It is that soluble nickel salt is fully mixed with conductive carbon black; Nickel salt and carbonic hydroammonium are reacted rapidly, thereby obtain a kind of nano-nickel oxide and the mixed uniformly composite material of conductive carbon black; The mixed uniformly Powdered composite material of nano-nickel oxide and conductive carbon black, wherein the weight percent content of nickel oxide is 30%～90%, the weight percent content of conductive carbon black is 10%～70%.
Its concrete steps are following:
(a) in the percentage by weight of conductive carbon black in the middle of composite material be 10%～50% ratio; Taking by weighing an amount of conductive carbon black powder joins in the middle of the aqueous solution of nickel salt that concentration is 0.01～1mol/L; Add volume simultaneously and be 10%～400% organic solvent of above-mentioned liquor capacity; It is 20～50KHz that the suspension-turbid liquid that forms is used supersonic frequency, ultrasonic vibration obtain mixed solution A;
(b) in the mixed solvent of organic solvent and water, add carbonic hydroammonium configuration mixed solution B, wherein the concentration of carbonic hydroammonium is 0.01～1mol/L, and the kind of organic solvent and proportion and mixed solution A are consistent;
(c) above-mentioned solution A is stirred under 15～35 ℃ temperature, add solution B subsequently, the mol ratio of control nickel salt and carbonic hydroammonium is 1: 2～7, and the pH value of solution is 7～9;
(d) Separation of Solid and Liquid is carried out to slurry in the back that reacts completely, and will precipitate and use water washing, after 50～150 ℃ of dryings, products therefrom 250～450 ℃ of following calcinings, is promptly made nano nickel oxide.
The preparation method of described nano nickel oxide, its used nickel salt is at least a in Nickel dichloride hexahydrate, Nickelous nitrate hexahydrate, the six hydration nickel sulfate.The preparation method of described nano nickel oxide, its used organic solvent is one or more the mixing in methyl alcohol, ethanol, isopropyl alcohol or the acetone.
Specific embodiment further is following:
Embodiment 5:
The weight percent content of nickel oxide is that the preparation process of 30% nano nickel oxide is following:
(a) in the percentage by weight of conductive carbon black in the middle of composite material be 10% ratio, take by weighing an amount of conductive carbon black powder and join in the middle of the aqueous solution of nickel salt that concentration is 0.01mol/L that nickel salt is a Nickel dichloride hexahydrate; Add volume simultaneously and be 10% organic solvent of above-mentioned liquor capacity, organic solvent is that ethanol, propyl alcohol mix; Use supersonic frequency to be 20KHz the suspension-turbid liquid that forms, ultrasonic power 2W/cm
2Ultrasonic vibration obtained mixed solution A in 5 minutes;
(b) in the mixed solvent of organic solvent and water, add carbonic hydroammonium configuration mixed solution B, wherein the concentration of carbonic hydroammonium is 0.01mol/L, and the kind of organic solvent and proportion and mixed solution A are consistent;
(c) above-mentioned solution A was stirred 10 minutes under 15 ℃ temperature, in 30 seconds time, add solution B subsequently fast, the mol ratio of control nickel salt and carbonic hydroammonium was at 1: 2, and the pH value of solution is 7;
(d) Separation of Solid and Liquid is carried out to slurry in the back that reacts completely, and will precipitate with water washing 2 times, in 100 ℃ of dryings after 5 hours, products therefrom 250 ℃ of following calcinings 2 hours, is promptly made nano nickel oxide.
Embodiment 6:
The weight percent content of nickel oxide is that the preparation process of 75% nano nickel oxide is following:
(a) in the percentage by weight of conductive carbon black in the middle of composite material be 40% ratio, take by weighing an amount of conductive carbon black powder and join in the middle of the aqueous solution of nickel salt that concentration is 0.05mol/L that nickel salt is a Nickelous nitrate hexahydrate; Add volume simultaneously and be 100% organic solvent of above-mentioned liquor capacity, organic solvent is an acetone; Use supersonic frequency to be 30KHz the suspension-turbid liquid that forms, ultrasonic power 3W/cm
2Ultrasonic vibration obtained mixed solution A in 100 minutes;
(b) in the mixed solvent of organic solvent and water, add carbonic hydroammonium configuration mixed solution B, wherein the concentration of carbonic hydroammonium is 0.05mol/L, and the kind of organic solvent and proportion and mixed solution A are consistent;
(c) above-mentioned solution A was stirred 80 minutes under 25 ℃ temperature, in 300 seconds time, add solution B subsequently fast, the mol ratio of control nickel salt and carbonic hydroammonium was at 1: 5, and the pH value of solution is 8;
(d) Separation of Solid and Liquid is carried out to slurry in the back that reacts completely, and will precipitate with water washing 4 times, in 100 ℃ of dryings after 8 hours, products therefrom 300 ℃ of following calcinings 4 hours, is promptly made nano nickel oxide.
Embodiment 7:
The weight percent content of nickel oxide is that the preparation process of 90% nano nickel oxide is following:
(a) in the percentage by weight of conductive carbon black in the middle of composite material be 50% ratio, take by weighing an amount of conductive carbon black powder and join in the middle of the aqueous solution of nickel salt that concentration is 1mol/L that nickel salt is a six hydration nickel sulfate; Add volume simultaneously and be 400% organic solvent of above-mentioned liquor capacity, organic solvent is the mixing of methyl alcohol, isopropyl alcohol, acetone; Use supersonic frequency to be 50KHz the suspension-turbid liquid that forms, ultrasonic power 10W/cm
2Ultrasonic vibration obtained mixed solution A in 180 minutes;
(b) in the mixed solvent of organic solvent and water, add carbonic hydroammonium configuration mixed solution B, wherein the concentration of carbonic hydroammonium is 1mol/L, and the kind of organic solvent and proportion and mixed solution A are consistent;
(c) above-mentioned solution A was stirred 180 minutes under 35 ℃ temperature, in 600 seconds time, add solution B subsequently fast, the mol ratio of control nickel salt and carbonic hydroammonium was at 1: 7, and the pH value of solution is 9;
(d) Separation of Solid and Liquid is carried out to slurry in the back that reacts completely, and will precipitate with water washing 5 times, in 150 ℃ of dryings after 24 hours, products therefrom 450 ℃ of following calcinings 6 hours, is promptly made nano nickel oxide.
The making of nickel oxide electrode and performance test: be active material with the nano nickel oxide that makes in embodiment 5 or 6 or 7 respectively; PTFE (polytetrafluoroethylene) is a binding agent; Active material and binding agent are pressed 15～20: 1 mixed, add to be coated on the nickel foam substrate equably after water stirs into paste.Drying is after 2～5 hours down at 65 ℃, and with the pole piece hydrostatic profile, the lug of burn-oning promptly makes nickel oxide electrode under the pressure of 12～18Mpa.Adopt three-electrode system to carry out charge-discharge test, work electrode is above-mentioned nickel oxide electrode, is platinum electrode to electrode, and reference electrode is the Hg/HgO electrode, and electrolyte is the KOH solution of 6mol/L.Can calculate the specific capacity of nickel oxide active material under the different discharge current densities according to the content of the weight of the result of charge-discharge test, nano nickel oxide and nickel oxide, concrete outcome is seen table 1.
The specific capacity of nickel oxide active material under the different discharge current densities of table 1
Visible by table 1, be suitable for being used as the electrode material of ultracapacitor with the nano nickel oxide of method for preparing.
Claims (7)
1. nano nickel oxide; It is characterized in that: it is that soluble nickel salt is fully mixed with conductive carbon black; Nickel salt and carbonic hydroammonium are reacted rapidly, thereby obtain a kind of nano-nickel oxide and the mixed uniformly composite material of conductive carbon black; The mixed uniformly composite material of said nano-nickel oxide and conductive carbon black, wherein the weight percent content of nickel oxide is 30%～90%, the weight percent content of conductive carbon black is 10%～70%.
2. nano nickel oxide as claimed in claim 1 is characterized in that: the weight percent content of nickel oxide is 50%～90%, and the weight percent content of conductive carbon black is 10%～50%.
3. nano nickel oxide as claimed in claim 1 is characterized in that: the weight percent content of nickel oxide is 30%, and the weight percent content of conductive carbon black is 70%.
4. nano nickel oxide as claimed in claim 1 is characterized in that: the weight percent content of nickel oxide is 90%, and the weight percent content of conductive carbon black is 10%.
5. nano nickel oxide as claimed in claim 1 is characterized in that: the weight percent content of nickel oxide is 50%, and the weight percent content of conductive carbon black is 50%.
6. the preparation method of a nano nickel oxide as claimed in claim 1; It is characterized in that: soluble nickel salt is fully mixed with conductive carbon black; Nickel salt and carbonic hydroammonium are reacted rapidly, thereby obtain a kind of nano-nickel oxide and the mixed uniformly composite material of conductive carbon black; Used nickel salt is at least a in Nickel dichloride hexahydrate, Nickelous nitrate hexahydrate, the six hydration nickel sulfate; Used organic solvent is one or more the mixing in methyl alcohol, ethanol, isopropyl alcohol or the acetone; Specifically may further comprise the steps:
(a) in the percentage by weight of conductive carbon black in the middle of composite material be 10%～50% ratio; Taking by weighing an amount of conductive carbon black powder joins in the middle of the aqueous solution of nickel salt that concentration is 0.01～1mol/L; Add volume simultaneously and be 10%～400% organic solvent of above-mentioned liquor capacity, it is that the ultrasonic vibration of 20～50KHz obtains mixed solution A that the suspension-turbid liquid that forms is used supersonic frequency;
(b) in the mixed solvent of organic solvent and water, add carbonic hydroammonium configuration mixed solution B, wherein the concentration of carbonic hydroammonium is 0.01～1mol/L, and the kind of organic solvent and proportion and mixed solution A are consistent;
(c) above-mentioned solution A is stirred under 15～35 ℃ temperature, add solution B subsequently, the mol ratio of control nickel salt and carbonic hydroammonium is 1: 2～7, and the pH value of solution is 7～9;
(d) Separation of Solid and Liquid is carried out to slurry in the back that reacts completely, and will precipitate and use water washing, after 50～150 ℃ of dryings, products therefrom 250～450 ℃ of following calcinings, is promptly made nano nickel oxide.
7. with the electrode material of the described nano nickel oxide of claim 1 as ultracapacitor.
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