CN102259936A - Preparation method of nano nickel cobalt oxide - Google Patents
Preparation method of nano nickel cobalt oxide Download PDFInfo
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- CN102259936A CN102259936A CN201110195864XA CN201110195864A CN102259936A CN 102259936 A CN102259936 A CN 102259936A CN 201110195864X A CN201110195864X A CN 201110195864XA CN 201110195864 A CN201110195864 A CN 201110195864A CN 102259936 A CN102259936 A CN 102259936A
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Abstract
The invention provides a preparation method of nano nickel cobalt oxide. In the preparation method, an organic solvent is added during a precursor preparation process, an aqueous and organic mixed phase is used as a solvent, and nano nickel cobalt oxide with high purity, uniform particle size and good crystallinity is acquired by a co-precipitation method. By using the nano nickel cobalt oxide prepared by the preparation method as an electrode material for a supercapacitor, a higher specific capacitance (up to 348-617 F.g<-1>) can be acquired. The preparation method provided by the invention has the advantages that operation is simple, conditions are mild and easy to control and cost is low, is suitable for large-scale preparation, and is suitable for commercial production.
Description
Technical field
The present invention relates to a kind of electrode material for super capacitor: nanometer cobalt acid nickel (NiCo
2O
4) the preparation method.
Background technology
The oxide compound of transition metal Co, Ni (oxyhydroxide) is as Co
3O
4, α-CO (OH)
2, NiO and (Co+Ni) (OH)
2NH
2O is the maximum material of present electrode material for super capacitor research, and with the sour nickel Co of bimetallic oxide nanometer cobalt of spinel structure
2O
4Do electrode material for super capacitor, the people of concern is also few.
Spinel NiCo
2O
4Material has Stability Analysis of Structures, is better than the electroconductibility and the reactive behavior of single metallic nickel, cobalt/cobalt oxide, is the first-selected research material in catalyticing research field, and other physicalies such as its magnetic properties also are one of focuses of research, still, and for spinel NiCo
2O
4The discovering of good electrochemical electrode material, but only 2002 by Hispanic study group report [R.Alc á ntara et al., Chem.Mater.2002,14,2847-2848], they find the NiCo of spinel structure
2O
4On the sodium-ion battery negative material, use, has good electrochemical, and just be it is found that [Te-Yu Wei et al. late to 2009 for its character of ultracapacitor of excellence, Adv.Mater.2009,21,1-5], the NiCo of spinel structure cheaply of the method preparation of human epoxide extensions such as the Hu of Taiwan
2O
4Aerogel, have 1400Fg
-1Ratio electric capacity, become alternative RuO
2One of the most potential material.Spinel NiCo like this
2O
4The ultracapacitor character of material just begins to attract much attention.
For nanometer cobalt acid nickel Co
2O
4The research of synthetic method also a lot, as thermolysis, co-precipitation, spraying thermolysis, co-precipitation, sol-gel etc.For high performance spinel structure NiCo
2O
4Aerogel, it is a kind of super light material, has very low mass density, the successive pore structure, high specific surface area and high electroconductibility, be the material that is rich in potentiality of battery and ultracapacitor, the active electrode material of preparation aerogel state also should be the very effective means that improve the electrode materials electric property.But preparation aerogel technology more complicated, laboratory or industrial operation be difficulty relatively, therefore seeks more easy method and prepares high performance NiCo
2O
4It is one of problem that should solve at present.Afterwards, people such as Vinay Gupta has found the spinel structure NiCo of electro-deposition method preparation
2O
4, can obtain 580F g
-1Ratio electric capacity [Vinay Gupta et al., J.Power Sources, 2010,195,3757-3760], though the operation of this method is simple relatively, power consumption is big, production cost is higher, and the NiCo for preparing of this method
2O
4, more relatively low as electrode material for super capacitor than electric capacity, be unfavorable for large-scale industrialization production.CN 101549890B adopts organic solvent propyl carbinol or n-propyl alcohol and the water mixed solvent dispersion agent as nickel acetate and nickel acetate, adopt solvent thermal method to prepare particle size less than 12nm, uniform nanometer cobalt acid nickel material, owing to used in the reaction, autoclave, on safety, in the handiness of operational condition regulation and control, all bring certain difficulty, make suitability for industrialized production bring certain difficulty.
Summary of the invention
The objective of the invention is to overcome the defective of existing synthetic technology, a kind of cobalt acid nickel (NiCo is provided
2O
4) the co-precipitation synthetic method of nano particle, product purity height of the present invention, particle is thin, the distribution of sizes homogeneous, and crystallinity is good.The prepared NiCo of the inventive method
2O
4Be spinel structure, be of a size of about 10nm.Product nanometer cobalt acid nickel material of the present invention is used for electrode material for super capacitor, and the ratio electric capacity of product can reach 348～617Fg
-1
Coprecipitation method can obtain that specific surface area is bigger, particle diameter is littler, more high conductivity, single phase spinel NiCo
2O
4Material, and simple to operate obtains easily, and the present invention plays a positive role by adding organic complexing agent/tensio-active agent aspect such as growth of can reuniting in particle size uniformity, the restriction of product, thereby obtains better electrode material for super capacitor.
The present invention adopts the coprecipitation method under water and the organic phase mixed phase, adds organic solvent in the process of preparation presoma.
Sequence of process steps of the present invention is as follows:
1, weighing purity is 98.0% Ni (NO
3)
26H
2O and purity are 99.0%Co (NO
3)
26H
2O, described Ni (NO
3)
26H
2O and Co (NO
3)
26H
2The ratio of the amount of O is 1: 2.With described Ni (NO
3)
26H
2O and Co (NO
3)
26H
2O is dissolved in the mixed solvent of organic reagent and deionized water jointly, and organic reagent is any ratio with deionized water in the described mixed solvent, is mixed with to contain Ni
2+And Co
2+Mixed salt solution A, among the described mixed salt solution A, Ni
2+Concentration be 0.01～1molL
-1, Co
2+Concentration be 0.02～2molL
-1Described organic reagent is that purity is that 96.0% ethylene glycol or purity are 99.5% dimethyl formamide;
2, be that 96.0% sodium hydroxide is dissolved in the organic reagent with purity, preparation amount of substance concentration is 0.05～5molL
-1The solution B of NaOH, metal-salt Ni (NO among the mixed salt solution A described in NaOH amount of substance and the step 1 in the described solution B
3)
2And Co (NO
3)
2The ratio of total amount of substance is greater than 2, and described organic reagent is that purity is that 96.0% ethylene glycol or purity are 99.5% dimethyl formamide;
3, the described mixed salt solution A that under 0～80 ℃ step 1 is prepared is by dripping in the solution B of all transferring to step 2 preparation, stir while dripping, dropwise, continuation is stirred 0.5～48h down at 0～80 ℃, obtain precursor solution, in the described precursor solution, the volume ratio of organic reagent ethylene glycol or dimethyl formamide and deionized water is 1～10: 1;
4, the described precursor solution that step 3 is obtained separates with the rotating speed of whizzer with 8O00 rev/min, uses deionized water wash three times, makes presoma;
5, the described presoma that step 4 is made dry 2～48h in 20～100 ℃ of following air dry ovens;
6, the dry precursor that step 4 is made is under 300～400 ℃, and sintering 2～24h obtains nanometer cobalt acid nickel under the atmosphere in retort furnace.
The inventive method is simple to operate, and mild condition and control easily are suitable for preparation in enormous quantities, and cost is low, is suitable for commercially producing.
Description of drawings
Fig. 1 is the XRD figure spectrum of the cobalt acid nickel nano material of embodiment 1 and embodiment 2 preparations;
Fig. 2 is HRTEM (high-resolution-ration transmission electric-lens) collection of illustrative plates of the cobalt acid nickel nano material of embodiment 1 preparation;
Fig. 3 is the discharge and recharge collection of illustrative plates of the cobalt acid nickel nano material of embodiment 1 preparation as electrode materials.
Embodiment
Below knot and drawings and Examples are done the present invention and are described in further detail.
1, weighing 0.004mol purity is 98.0% Ni (NO respectively
3)
26H
2O and 0.008mol purity are 99.0%Co (NO
3)
26H
2O, described Ni (NO
3)
26H
2O and Co (NO
3)
26H
2The ratio of the amount of O is 1: 2.With described Ni (NO
3)
26H
2O and Co (NO
3)
26H
2O is dissolved in the mixed solvent of 20ml organic reagent ethylene glycol and 80ml deionized water jointly, is mixed with to contain Ni
2+And Co
2+Mixed salt solution A 100ml, among the described mixed salt solution A, Ni
2+And Co
2+Concentration is respectively 0.04molL
-1And 0.08molL
-1Described organic reagent is that purity is 96.0% ethylene glycol;
2, be that 96.0% sodium hydroxide is dissolved in the 270ml organic reagent ethylene glycol with 0.026mol purity, preparation amount of substance concentration is 0.096molL
-1The solution B 270ml of NaOH, described organic reagent is the ethylene glycol of purity 96.0%;
3, the 100ml mixed salt solution A that at room temperature step 1 is prepared is added drop-wise in the solution B of 270ml step 2 preparation, stir while dripping, dropwise, continue at room temperature to stir 18h, the volume ratio that obtains ethylene glycol and deionized water is 3.625: 1 a precursor solution;
4, the precursor solution that step 3 is obtained separates with the rotating speed of whizzer with 8000 rev/mins, uses deionized water wash three times, makes presoma;
5, the presoma that step 4 is made dry 48h in 80 ℃ of following air dry ovens;
6, will be under 375 ℃ through step 4 dry precursor, sintering 8h under the atmosphere in retort furnace obtains nanometer cobalt acid nickel.The XRD figure spectrum of products therefrom as shown in Figure 1, the generation of the nanometer cobalt of the spinel structure of single phase acid nickel as can be seen from the collection of illustrative plates, HRTEM collection of illustrative plates as shown in Figure 2, from the collection of illustrative plates as can be seen, good, the distribution of sizes homogeneous of nanometer cobalt acid nickel material crystallinity that generates, particle diameter is about 10nm.The gained material is made electrode material for super capacitor and is done charge-discharge test, can reach 671Fg than electric capacity
-1
Embodiment 2
1, weighing 0.004mol purity is 98.0% Ni (NO respectively
3)
26H
2O and 0.008mol purity are 99.0%Co (NO
3)
26H
2O, described Ni (NO
3)
26H
2O and Co (NO
3)
26H
2The ratio of the amount of O is 1: 2.With described Ni (NO
3)
26H
2O and Co (NO
3)
26H
2O is dissolved in the mixed solvent of 20ml organic reagent ethylene glycol and 80ml deionized water jointly, is mixed with Ni
2+And Co
2+Mixed salt solution A 100ml, among the mixed salt solution A, Ni
2+And Co
2+Concentration is respectively 0.04molL
-1And 0.08molL
-1Described organic reagent is that purity is 96.0% ethylene glycol;
2, be that 96.0% sodium hydroxide is dissolved in the 270ml organic reagent ethylene glycol with 0.026mol purity, preparation amount of substance concentration is 0.096molL
-1The solution B 270ml of NaOH, described organic reagent is that purity is 96.0% ethylene glycol;
3, the 100ml mixed salt solution A that at room temperature step 1 is prepared is added drop-wise in the 270ml solution B of step 2 preparation, stir while dripping, dropwise, continue to stir 18h under the room temperature, the volume ratio that obtains ethylene glycol and deionized water is 3.625: 1 a precursor solution;
4, the precursor solution that step 3 is obtained separates with the rotating speed of whizzer with 8000 rev/mins, uses deionized water wash three times, makes presoma;
5, the presoma that step 4 is made dry 48h in 80 ℃ of following air dry ovens;
6, will be under 375 ℃ through step 4 dry precursor, sintering 2h under the atmosphere in retort furnace obtains nanometer cobalt acid nickel.The XRD figure of products therefrom spectrum as shown in Figure 1, the generation of the nanometer cobalt acid nickel of the spinel structure of single phase as can be seen from the collection of illustrative plates, good, the distribution of sizes homogeneous of nanometer cobalt acid nickel material crystallinity of generation, particle diameter is about 10nm.The gained material is made electrode material for super capacitor and is done charge-discharge test, can reach 348Fg than electric capacity
-1
Embodiment 3
1, weighing 0.004mol purity is 98.0% Ni (NO respectively
3)
26H
2O and 0.008mol purity are 99.0%Co (NO
3)
26H
2O, described Ni (NO
3)
26H
2O and Co (NO
3)
26H
2The ratio of the amount of O is 1: 2.With described Ni (NO
3)
26H
2O and Co (NO
3)
26H
2O is dissolved in the mixed solvent of 10ml organic reagent ethylene glycol and 40ml deionized water jointly, is mixed with Ni
2+And Co
2+Mixed salt solution A50ml, Ni among the mixed salt solution A
2+And Co
2+Concentration be respectively 0.08molL
-1And 0.16molL
-1Described organic reagent is that purity is 96.0% ethylene glycol;
2, be that 96.0% sodium hydroxide is dissolved in the 60ml organic reagent ethylene glycol with 0.03mol purity, preparation amount of substance concentration is 0.5molL
-1The solution B 60ml of NaOH, described organic reagent is that purity is 96.0% ethylene glycol;
3, the mixed salt solution A50ml that under 0 ℃ step 1 is prepared is added drop-wise among the solution B 60ml of step 2 preparation, stir while dripping, dropwise, continue to stir 48h down at 0 ℃, the volume ratio that obtains ethylene glycol and deionized water is 1.75: 1 a precursor solution;
4, the precursor solution that step 3 is obtained separates with the rotating speed of whizzer with 8000 rev/mins, uses deionized water wash three times, makes presoma;
5, the presoma that step 4 is made dry 48h in 80 ℃ of following air dry ovens;
6, will be under 350 ℃ of step 4 dry precursor, sintering 2h obtains nanometer cobalt acid nickel under the atmosphere in retort furnace.Good, the distribution of sizes homogeneous of nanometer cobalt acid nickel material crystallinity that generates, particle diameter is about 10nm.
Embodiment 4
1, weighing 0.04mol purity is 98.0% Ni (NO respectively
3)
26H
2O and 0.08mol purity are 99.0%Co (NO
3)
26H
2O, described Ni (NO
3)
26H
2O and Co (NO
3)
26H
2The ratio of the amount of O is 1: 2.With described Ni (NO
3)
26H
2O and Co (NO
3)
26H
2O is dissolved in the mixed solvent of 20ml organic reagent dimethyl formamide and 80ml deionized water jointly, is mixed with to contain Ni
2+And Co
2+Mixed salt solution A100ml, Ni among the mixed salt solution A
2+And Co
2+Concentration be respectively 0.4molL
-1And 0.8molL
-1Described organic reagent is that purity is 99.5% dimethyl formamide;
2, be that 96.0% sodium hydroxide is dissolved in the 270ml organic reagent ethylene glycol with 0.27mol purity, preparation amount of substance concentration is 1molL
-1The solution B 270ml of NaOH, described organic reagent is that purity is 99.5% dimethyl formamide;
3, the mixed salt solution A100ml that at room temperature step 1 is prepared is added drop-wise among the solution B 270ml of step 2 preparation, stir while dripping, dropwise, continue at room temperature to stir 18h, the volume ratio that obtains dimethyl formamide and deionized water is 3.625: 1 a precursor solution;
4, the precursor solution that step 3 is obtained separates with the rotating speed of whizzer with 8000 rev/mins, uses deionized water wash three times, makes presoma;
5, the presoma that step 4 is made dry 24h in 60 ℃ of following air dry ovens;
6, will be under 375 ℃ of step 4 dry precursor, sintering 8h under the atmosphere in retort furnace obtains nanometer cobalt acid nickel.Good, the distribution of sizes homogeneous of nanometer cobalt acid nickel material crystallinity that generates, particle diameter is about 10nm.The gained material is made electrode material for super capacitor and is done charge-discharge test, can reach 374Fg than electric capacity
-1
Embodiment 5
1, weighing 0.001mol purity is 98.0% Ni (NO respectively
3)
26H
2O and 0.002mol purity are 99.0%Co (NO
3)
26H
2O, described Ni (NO
3)
26H
2O and Co (NO
3)
26H
2The ratio of the amount of O is 1: 2.With described Ni (NO
3)
26H
2O and Co (NO
3)
26H
2O is dissolved in the mixed solvent of 25ml organic reagent dimethyl formamide and 25ml deionized water jointly, is mixed with Ni
2+And Co
2+Mixed salt solution A50ml, Ni among the mixed salt solution A
2+And Co
2+Concentration be respectively 0.02molL
-1And 0.04molL
-1Described organic reagent is that purity is 99.5% dimethyl formamide;
2, be that 96.0% sodium hydroxide is dissolved in the 200ml organic reagent dimethyl formamide with 0.12mol purity, preparation amount of substance concentration is 0.6molL
-1The solution B 200ml of NaOH, described organic reagent is that purity is 99.5% dimethyl formamide;
3, the mixed salt solution A50ml that under 40 ℃ step 1 is prepared is added drop-wise among the solution B 200ml of step 2 preparation, stir while dripping, dropwise, continue to stir 24h down at 40 ℃, the volume ratio that obtains dimethyl formamide and deionized water is 9: 1 a precursor solution;
4, the precursor solution that step 3 is obtained separates with the rotating speed of whizzer with 8000 rev/mins, uses deionized water wash three times, makes presoma;
5, the presoma that step 4 is made dry 24h in 50 ℃ of following air dry ovens;
6, will be under 350 ℃ of step 4 dry precursor, sintering 12h under the atmosphere in retort furnace obtains nanometer cobalt acid nickel.Good, the distribution of sizes homogeneous of nanometer cobalt acid nickel material crystallinity that generates, particle diameter is about 10nm.
Embodiment 6
1, weighing 0.004mol purity is 98.0% Ni (NO respectively
3)
26H
2O and 0.008mol purity are 99.0%Co (NO
3)
26H
2O, described Ni (NO
3)
26H
2O and Co (NO
3)
26H
2The ratio of the amount of O is 1: 2.With described Ni (NO
3)
26H
2O and Co (NO
3)
26H
2O is dissolved in the mixed solvent of 5Oml organic reagent ethylene glycol and 50ml deionized water jointly, is mixed with Ni
2+And Co
2+Mixed salt solution A100ml, Ni among the mixed salt solution A
2+And Co
2+Concentration be respectively 0.04molL
-1And 0.08molL
-1Described organic reagent is that purity is 96.0% ethylene glycol;
2, be that 96.0% sodium hydroxide is dissolved in the 100ml organic reagent ethylene glycol with 0.025mol purity, preparation amount of substance concentration is 0.25molL
-1The solution B 100ml of NaOH, described organic reagent is that purity is 96.0% ethylene glycol;
3, the mixed salt solution A100ml that under 35 ℃ step 1 is prepared is added drop-wise among the solution B 100ml of step 2 preparation, stir while dripping, dropwise, continue to stir 20h down at 35 ℃, the volume ratio that obtains ethylene glycol and deionized water is 3: 1 a precursor solution;
4, the precursor solution that step 3 is obtained separates with the rotating speed of whizzer with 8000 rev/mins, uses deionized water wash three times, makes presoma;
5, the presoma that step 4 is made dry 32h in 90 ℃ of following air dry ovens;
6, will be under 350 ℃ of step 4 dry precursor, sintering 10h obtains nanometer cobalt acid nickel under the atmosphere in retort furnace.Good, the distribution of sizes homogeneous of nanometer cobalt acid nickel material crystallinity that generates, particle diameter is about 10nm.
Embodiment 7
1, weighing 0.004mol purity is 98.0% Ni (NO respectively
3)
26H
2O and 0.008mol purity are 99.0%Co (NO
3)
26H
2O, described Ni (NO
3)
26H
2O and Co (NO
3)
26H
2The ratio of the amount of O is 1: 2.With described Ni (NO
3)
26H
2O and Co (NO
3)
26H
2O is dissolved in the mixed solvent of 50ml organic reagent ethylene glycol and 50ml deionized water jointly, is mixed with to contain Ni
2+And Co
2+Mixed salt solution A100ml, Ni among the mixed salt solution A
2+And Co
2+Concentration be respectively 0.04molL
-1And 0.08molL
-1Described organic reagent is that purity is 96.0% ethylene glycol;
2, be that 96.0% sodium hydroxide is dissolved in the 250ml organic reagent ethylene glycol with 0.025mol purity, preparation amount of substance concentration is 0.1molL
-1The solution B 250ml of NaOH, described organic reagent is that purity is 96.0% ethylene glycol;
3, the mixed salt solution A100ml that under 35 ℃ step 1 is prepared is added drop-wise among the solution B 250ml of step 2 preparation, stir while dripping, dropwise, continue 35 ℃ and stir 20h down, the volume ratio that obtains ethylene glycol and deionized water is 6: 1 a precursor solution;
4, the precursor solution that step 3 is obtained separates with the rotating speed of whizzer with 8000 rev/mins, uses deionized water wash three times, makes presoma;
5, the presoma that step 4 is made dry 32h in 90 ℃ of following air dry ovens;
6, will be under 350 ℃ of step 4 dry precursor, sintering 10h obtains nanometer cobalt acid nickel under the atmosphere in retort furnace.Good, the distribution of sizes homogeneous of nanometer cobalt acid nickel material crystallinity that generates, particle diameter is about 10nm.
Embodiment 8
1, weighing 0.001mol purity is 98.0% Ni (NO respectively
3)
26H
2O and 0.002mol purity are 99.0%Co (NO
3)
26H
2O, described Ni (NO
3)
26H
2O and Co (NO
3)
26H
2The ratio of the amount of O is 1: 2.With described Ni (NO
3)
26H
2O and Co (NO
3)
26H
2O is dissolved in the mixed solvent of 40ml organic reagent ethylene glycol and 40ml deionized water jointly, is mixed with to contain Ni
2+And Co
2+Mixed salt solution A80ml, Ni among the mixed salt solution A
2+And Co
2+Concentration be respectively 0.0125molL
-1And 0.025molL
-1Described organic reagent is that purity is 96.0% ethylene glycol;
2, be that 96.0% sodium hydroxide is dissolved in the 200ml organic reagent ethylene glycol with 0.0135mol purity, preparation amount of substance concentration is 0.0675molL
-1The solution B 200ml of NaOH, described organic reagent is that purity is 96.0% ethylene glycol;
3, the mixed salt solution A80ml that at room temperature step 1 is prepared is added drop-wise among the solution B 200ml of step 2 preparation, stir while dripping, dropwise, continue at room temperature to stir 48h, the volume ratio that obtains ethylene glycol and deionized water is 6: 1 a precursor solution;
4, the precursor solution that step 3 is obtained separates with the rotating speed of whizzer with 8000 rev/mins, uses deionized water wash three times, makes presoma;
5, the presoma that step 4 is made dry 48h in 20 ℃ of following air dry ovens;
6, will be under 300 ℃ of step 4 dry precursor, sintering 24h obtains nanometer cobalt acid nickel under the atmosphere in retort furnace.Good, the distribution of sizes homogeneous of nanometer cobalt acid nickel material crystallinity that generates, particle diameter is about 10nm.
Embodiment 9
1, weighing 0.001mol purity is 98.0% Ni (NO respectively
3)
26H
2O and 0.002mol purity are 99.0%Co (NO
3)
26H
2O, described Ni (NO
3)
26H
2O and Co (NO
3)
26H
2The ratio of the amount of O is 1: 2.With described Ni (NO
3)
26H
2O and Co (NO
3)
26H
2O is dissolved in the mixed solvent of 20ml organic reagent dimethyl formamide and 80ml deionized water jointly, is mixed with to contain Ni
2+And Co
2+Mixed salt solution A100ml, Ni among the mixed salt solution A
2+And Co
2+Concentration be respectively 1molL
-1And 2molL
-1Described organic reagent is that purity is 99.5% dimethyl formamide;
2, be that 96.0% sodium hydroxide is dissolved in the 120ml organic reagent dimethyl formamide with 0.12mol purity, preparation amount of substance concentration is 1molL
-1The solution B 120ml of NaOH, described organic reagent is that purity is 99.5% dimethyl formamide;
3, the mixed salt solution A100ml that under 80 ℃ step 1 is prepared all is added drop-wise among the solution B 120ml of step 2 preparation, stir while dripping, dropwise, continue to stir 0.5h down at 80 ℃, the volume ratio that obtains dimethyl formamide and deionized water is 10: 1 a precursor solution;
4, the precursor solution that step 3 is obtained separates with the rotating speed of whizzer with 8000 rev/mins, uses deionized water wash three times, makes presoma;
5, the presoma that step 4 is made dry 24h in 60 ℃ of following air dry ovens;
6, will be under 360 ℃ of step 4 dry precursor, sintering 2h under the atmosphere in retort furnace obtains nanometer cobalt acid nickel.Good, the distribution of sizes homogeneous of nanometer cobalt acid nickel material crystallinity that generates, particle diameter is about 10nm.
Embodiment 10
1, weighing 0.003mol purity is 98.0% Ni (NO respectively
3)
26H
2O and 0.006mol purity are 99.0%Co (NO
3)
26H
2O, described Ni (NO
3)
26H
2O and Co (NO
3)
26H
2The ratio of the amount of O is 1: 2.With described Ni (NO
3)
26H
2O and Co (NO
3)
26H
2O is dissolved in the mixed solvent of 60ml organic reagent ethylene glycol and 60ml deionized water jointly, is mixed with to contain Ni
2+And Co
2+Mixed salt solution A120ml, Ni among the mixed salt solution A
2+And Co
2+Concentration be respectively 0.025molL
-1And 0.05molL
-1Described organic reagent is that purity is 96.0% ethylene glycol;
2, be that 96.0% sodium hydroxide is dissolved in the 250ml organic reagent ethylene glycol with 0.025mol purity, preparation amount of substance concentration is 0.1molL
-1The solution B 250ml of NaOH, described organic reagent is that purity is 96.0% ethylene glycol;
3, the mixed salt solution A120ml that under 35 ℃ step 1 is prepared all is added drop-wise among the solution B 250ml of step 2 preparation, stir while dripping, dropwise, continue to stir 20h down at 35 ℃, the volume ratio that obtains ethylene glycol and deionized water is 5.167: 1 a precursor solution;
4, the precursor solution that step 3 is obtained separates with the rotating speed of whizzer with 8000 rev/mins, uses deionized water wash three times, makes presoma;
5, the presoma that step 4 is made dry 32h in 90 ℃ of following air dry ovens;
6, will be under 350 ℃ of step 4 dry precursor, sintering 10h obtains nanometer cobalt acid nickel under the atmosphere in retort furnace.Good, the distribution of sizes homogeneous of nanometer cobalt acid nickel material crystallinity that generates, particle diameter is about 10nm.
Embodiment 11
1, weighing 0.001mol purity is 98.0% Ni (NO respectively
3)
26H
2O and 0.002mol purity are 99.0%Co (NO
3)
26H
2O, described Ni (NO
3)
26H
2O and Co (NO
3)
26H
2The ratio of the amount of O is 1: 2.With described Ni (NO
3)
26H
2O and Co (NO
3)
26H
2O is dissolved in the mixed solvent of 50ml organic reagent dimethyl formamide and 50ml deionized water jointly, is mixed with to contain Ni
2+And Co
2+Mixed salt solution A100ml, Ni among the mixed salt solution A
2+And Co
2+Concentration be respectively 0.01molL
-1And 0.02molL
-1Described organic reagent is that purity is 99.5% dimethyl formamide;
2, be that 96.0% sodium hydroxide is dissolved in the 200ml organic reagent dimethyl formamide with 0.12mol purity, preparation amount of substance concentration is 0.6molL
-1The solution B 200ml of NaOH, described organic reagent is that purity is 99.5% dimethyl formamide;
3, the mixed salt solution A100ml that under 40 ℃ step 1 is prepared is by dripping among the solution B 200ml that all transfers to step 2 preparation, stir while dripping, dropwise, continuation is stirred 24h down at 40 ℃, and the volume ratio that obtains dimethyl formamide and deionized water is 5: 1 a precursor solution;
4, the precursor solution that step 3 is obtained separates with the rotating speed of whizzer with 8000 rev/mins, uses deionized water wash three times, makes presoma;
5, the presoma that step 4 is made dry 24h in 50 ℃ of following air dry ovens;
6, will be under 350 ℃ of step 4 dry precursor, sintering 12h under the atmosphere in retort furnace obtains nanometer cobalt acid nickel.Good, the distribution of sizes homogeneous of nanometer cobalt acid nickel material crystallinity that generates, particle diameter is about 10nm.
Embodiment 12
1, weighing 0.1mol purity is 98.0% Ni (NO respectively
3)
26H
2O and 0.2mol purity are 99.0%Co (NO
3)
26H
2O, described Ni (NO
3)
26H
2O and Co (NO
3)
26H
2The ratio of the amount of O is 1: 2.With described Ni (NO
3)
26H
2O and Co (NO
3)
26H
2O is dissolved in the mixed solvent of 40ml organic reagent ethylene glycol and 160ml deionized water jointly, is mixed with to contain Ni
2+And Co
2+Mixed salt solution A200ml, Ni among the mixed salt solution A
2+And Co
2+Concentration be respectively 0.05molL
-1And 1molL
-1Described organic reagent is that purity is 96.0% ethylene glycol;
2, be that 96.0% sodium hydroxide is dissolved in the 135ml organic reagent ethylene glycol with 1.35mol purity, preparation amount of substance concentration is 10molL
-1The solution B 135ml of NaOH, described organic reagent is that purity is 96.0% ethylene glycol;
3, the mixed salt solution A200ml that at room temperature step 1 is prepared is by dripping among the solution B 135ml that all transfers to step 2 preparation, stir while dripping, dropwise, continue at room temperature to stir 2h, the volume ratio that obtains ethylene glycol and deionized water is 1.094: 1 a precursor solution;
4, the precursor solution that step 3 is obtained separates with the rotating speed of whizzer with 8000 rev/mins, uses deionized water wash three times, makes presoma;
5, the presoma that step 4 is made dry 2h in 100 ℃ of following air dry ovens;
6, will be under 400 ℃ of step 4 dry precursor, sintering 2h obtains nanometer cobalt acid nickel under the atmosphere in retort furnace.Good, the distribution of sizes homogeneous of nanometer cobalt acid nickel material crystallinity that generates, particle diameter is about 10nm.
Embodiment 13
1, weighing 0.007mol purity is 98.0% Ni (NO respectively
3)
26H
2O and 0.014mol purity are 99.0%Co (NO
3)
26H
2O, described Ni (NO
3)
26H
2O and Co (NO
3)
26H
2The ratio of the amount of O is 1: 2.With described Ni (NO
3)
26H
2O and Co (NO
3)
26H
2O is dissolved in the mixed solvent of 30ml organic reagent dimethyl formamide and 40ml deionized water jointly, is mixed with Ni
2+And Co
2+Mixed salt solution A70ml, Ni among the A
2+And Co
2+Concentration be respectively 1molL
-1And 2molL
-1Described organic reagent is that purity is 99.5% dimethyl formamide;
2, be that 96.0% sodium hydroxide is dissolved in the 200ml organic reagent dimethyl formamide with 0.12mol purity, preparation amount of substance concentration is 0.6molL
-1The solution B 200ml of NaOH, described organic reagent is that purity is 99.5% dimethyl formamide;
3, the mixed salt solution A70ml that under 50 ℃ step 1 is prepared is added drop-wise among the solution B 200ml of step 2 preparation, stir while dripping, dropwise, continue to stir 24h down at 50 ℃, the volume ratio that obtains dimethyl formamide and deionized water is 5.75: 1 a precursor solution;
4, the precursor solution that step 3 is obtained separates with the rotating speed of whizzer with 8000 rev/mins, uses deionized water wash three times, makes presoma;
5, the presoma that step 4 is made dry 24h in 60 ℃ of following air dry ovens;
6, will be under 350 ℃ of step 4 dry precursor, sintering 4h under the atmosphere in retort furnace obtains nanometer cobalt acid nickel.Good, the distribution of sizes homogeneous of nanometer cobalt acid nickel material crystallinity that generates, particle diameter is about 10nm.
Embodiment 14
1, weighing 0.001mol purity is 98.0% Ni (NO respectively
3)
26H
2O and 0.002mol purity are 99.0%Co (NO
3)
26H
2O, described Ni (NO
3)
26H
2O and Co (NO
3)
26H
2The ratio of the amount of O is 1: 2.With described Ni (NO
3)
26H
2O and Co (NO
3)
26H
2O is dissolved in the mixed solvent of 50ml organic reagent dimethyl formamide and 50ml deionized water jointly, is mixed with to contain Ni
2+And Co
2+Mixed salt solution A100ml, Ni among the mixed salt solution A
2+And Co
2+Concentration be respectively 0.01molL
-1And 0.02molL
-1Described organic reagent is that purity is 99.5% dimethyl formamide;
2, be that 96.0% sodium hydroxide is dissolved in the 200ml organic reagent dimethyl formamide with 0.12mol purity, preparation amount of substance concentration is 0.6molL
-1The solution B 200ml of NaOH, described organic reagent is that purity is 99.5% dimethyl formamide;
3, the mixed salt solution A100ml that under 50 ℃ step 1 is prepared all is added drop-wise among the solution B 200ml of step 2 preparation, stir while dripping, dropwise, continue to stir 24h down at 50 ℃, the volume ratio that obtains dimethyl formamide and deionized water is 5: 1 a precursor solution;
4, the precursor solution that step 3 is obtained separates with the rotating speed of whizzer with 8000 rev/mins, uses deionized water wash three times, makes presoma;
5, the presoma that step 4 is made dry 24h in 60 ℃ of following air dry ovens;
6, will be under 350 ℃ of step 4 dry precursor, sintering 4h under the atmosphere in retort furnace obtains nanometer cobalt acid nickel.Good, the distribution of sizes homogeneous of nanometer cobalt acid nickel material crystallinity that generates, particle diameter is about 10nm.
Embodiment 15
1, weighing 0.1mol purity is 98.0% Ni (NO respectively
3)
26H
2O and 0.2mol purity are 99.0%Co (NO
3)
26H
2O, described Ni (NO
3)
26H
2O and Co (NO
3)
26H
2The ratio of the amount of O is 1: 2.With described Ni (NO
3)
26H
2O and Co (NO
3)
26H
2O is dissolved in the mixed solvent of 20ml organic reagent ethylene glycol and 80ml deionized water jointly, is mixed with to contain Ni
2+And Co
2+Mixed salt solution A100ml, Ni among the mixed salt solution A
2+And Co
2+Concentration be respectively 1molL
-1And 2molL
-1Described organic reagent is that purity is 96.0% ethylene glycol;
2, be that 96.0% sodium hydroxide is dissolved in the 270ml organic reagent ethylene glycol with 1.35mol purity, preparation amount of substance concentration is 5molL
-1The solution B 270ml of NaOH, described organic reagent is that purity is 96.0% ethylene glycol;
3, the mixed salt solution A100ml that at room temperature step 1 is prepared is by dripping among the solution B 270ml that all transfers to step 2 preparation, stir while dripping, dropwise, continue at room temperature to stir 2h, the volume ratio that obtains ethylene glycol and deionized water is 3.625: 1 a precursor solution;
4, the precursor solution that step 3 is obtained separates with the rotating speed of whizzer with 8000 rev/mins, uses deionized water wash three times, makes presoma;
5, the presoma that step 4 is made dry 2h in 100 ℃ of following air dry ovens;
6, will be under 400 ℃ of step 4 dry precursor, sintering 2h obtains nanometer cobalt acid nickel under the atmosphere in retort furnace.Good, the distribution of sizes homogeneous of nanometer cobalt acid nickel material crystallinity that generates, particle diameter is about 10nm.
Embodiment 16
1, weighing 0.0075mol purity is 98.0% Ni (NO respectively
3)
26H
2O and 0.015mol purity are 99.0%Co (NO
3)
26H
2O, described Ni (NO
3)
26H
2O and Co (NO
3)
26H
2The ratio of the amount of O is 1: 2.With described Ni (NO
3)
26H
2O and Co (NO
3)
26H
2O is dissolved in the mixed solvent of 70ml organic reagent dimethyl formamide and 80ml deionized water jointly, is mixed with to contain Ni
2+And Co
2+Mixed salt solution A150ml, Ni among the mixed salt solution A
2+And Co
2+Concentration be respectively 0.4molL
-1And 0.8molL
-1Described organic reagent is that purity is 99.5% dimethyl formamide;
2, be that 96.0% sodium hydroxide is dissolved in the 50ml organic reagent ethylene glycol with 0.05mol purity, preparation amount of substance concentration is 1molL
-1The solution B 50ml of NaOH, described organic reagent is that purity is 99.5% dimethyl formamide;
3, the mixed salt solution A150ml that at room temperature step 1 is prepared all is added drop-wise among the solution B 50ml of step 2 preparation, stir while dripping, dropwise, continue at room temperature to stir 18h, the volume ratio that obtains dimethyl formamide and deionized water is 1.5: 1 a precursor solution;
4, the precursor solution that step 3 is obtained separates with the rotating speed of whizzer with 8000 rev/mins, uses deionized water wash three times, makes presoma;
5, the presoma that step 4 is made dry 24h in 60 ℃ of following air dry ovens;
6, will be under 375 ℃ of step 4 dry precursor, sintering 8h under the atmosphere in retort furnace obtains nanometer cobalt acid nickel.Good, the distribution of sizes homogeneous of nanometer cobalt acid nickel material crystallinity that generates, particle diameter is about 10nm.The gained material is made electrode material for super capacitor and is done charge-discharge test, can reach 374Fg than electric capacity
-1
Embodiment 17
1, weighing 0.004mol purity is 98.0% Ni (NO respectively
3)
26H
2O and 0.008mol purity are 99.0%Co (NO
3)
26H
2O, described Ni (NO
3)
26H
2O and Co (NO
3)
26H
2The ratio of the amount of O is 1: 2.With described Ni (NO
3)
26H
2O and Co (NO
3)
26H
2O is dissolved in the mixed solvent of 20ml organic reagent ethylene glycol and 80ml deionized water jointly, is mixed with to contain Ni
2+And Co
2+Mixed salt solution mixed salt solution A100ml, Ni among the A
2+And Co
2+Concentration be respectively 0.04molL
-1And 0.08molL
-1Described organic reagent is that purity is 96.0% ethylene glycol;
2, be that 96.0% sodium hydroxide is dissolved in the 60ml organic reagent ethylene glycol with 0.03mol purity, preparation amount of substance concentration is 0.5molL
-1The solution B 60ml of NaOH, described organic reagent is that purity is 96.0% ethylene glycol;
3, the mixed salt solution A100ml that under 0 ℃ step 1 is prepared is by dripping among the solution B 60ml that all transfers to step 2 preparation, stir while dripping, dropwise, continue to stir 48h down at 0 ℃, the volume ratio that obtains ethylene glycol and deionized water is 1: 1 a precursor solution;
4, the precursor solution that step 3 is obtained separates with the rotating speed of whizzer with 8000 rev/mins, uses deionized water wash three times, makes presoma;
5, the presoma that step 4 is made dry 48h in 80 ℃ of following air dry ovens;
6, will be under 350 ℃ of step 4 dry precursor, sintering 2h obtains nanometer cobalt acid nickel under the atmosphere in retort furnace.Good, the distribution of sizes homogeneous of nanometer cobalt acid nickel material crystallinity that generates, particle diameter is about 15nm.
Embodiment 18
1, weighing 0.001mol purity is 98.0% Ni (NO respectively
3)
26H
2O and 0.002mol purity are 99.0%Co (NO
3)
26H
2O, described Ni (NO
3)
26H
2O and Co (NO
3)
26H
2The ratio of the amount of O is 1: 2.With described Ni (NO
3)
26H
2O and Co (NO
3)
26H
2O is dissolved in the mixed solvent of 20ml organic reagent ethylene glycol and 80ml deionized water jointly, is mixed with to contain Ni
2+And Co
2+Mixed salt solution A100ml, Ni among the molten A of mixed metal salt
2+And Co
2+Concentration be respectively 0.01molL
-1And 0.02molL
-1Described organic reagent is that purity is 96.0% ethylene glycol;
2, be that 96.0% sodium hydroxide is dissolved in the 270ml organic reagent ethylene glycol with 0.0135mol purity, preparation amount of substance concentration is 0.05molL
-1The solution B 270ml of NaOH, described organic reagent is that purity is 96.0% ethylene glycol;
3, the mixed salt solution A100ml that at room temperature step 1 is prepared is by dripping among the solution B 270ml that all transfers to step 2 preparation, stir while dripping, dropwise, continue at room temperature to stir 48h, the volume ratio that obtains ethylene glycol and deionized water is 3.625: 1 a precursor solution;
4, the precursor solution that step 3 is obtained separates with the rotating speed of whizzer with 8000 rev/mins, uses deionized water wash three times, makes presoma;
5, the presoma that step 4 is made dry 48h in 20 ℃ of following air dry ovens;
6, with under 300 ℃ of the dry precursor, sintering 24h obtains nanometer cobalt acid nickel under the atmosphere in retort furnace.Good, the distribution of sizes homogeneous of nanometer cobalt acid nickel material crystallinity that generates, particle diameter is about 10nm.
Claims (7)
1. the preparation method of nanometer cobalt acid nickel is characterized in that described preparation method may further comprise the steps:
(1) with Ni (NO
3)
26H
2O and Co (NO
3)
26H
2O is dissolved in the mixed solvent of organic reagent and deionized water jointly, is mixed with to contain Ni
2+And Co
2+Mixed salt solution A;
(2) sodium hydroxide NaOH is dissolved in the organic reagent solution B of preparation NaOH;
(3) the described mixed salt solution A with step (1) preparation all is added drop-wise in the described solution B of step (2) preparation, stirs while dripping, and dropwises and continues to stir, and obtains precursor solution;
(4) the described precursor solution that step (3) is obtained separates with the rotating speed of whizzer with 8000 rev/mins, uses deionized water wash three times, makes presoma;
(5) the described presoma that step (4) is made is dry in air dry oven;
(6) the described presoma of exsiccant that step (4) is made in retort furnace under atmosphere sintering, obtain described nanometer cobalt acid nickel.
2. the preparation method of nanometer cobalt acid nickel according to claim 1, it is characterized in that, in the mixed solvent of described organic reagent and deionized water, organic reagent is any ratio with the ratio of deionized water, and described organic reagent is that purity is that 96.0% ethylene glycol or purity are 99.5% dimethyl formamide.
3. the preparation method of nanometer cobalt acid nickel according to claim 1 is characterized in that, among the described mixed salt solution A, and Ni
2+And Co
2+The ratio of amount be 1: 2, Ni
2+Concentration be 0.01～1molL
-1, Co
2+Concentration be 0.02～2molL
-1
4. the preparation method of nanometer cobalt acid nickel according to claim 1 is characterized in that, in the described solution B, and Ni (NO among NaOH and the described mixed salt solution A
3)
2And Co (NO
3)
2The ratio of total amount of substance greater than 2, the concentration of NaOH is 0.05～5molL
-1
5. the preparation method of nanometer cobalt acid nickel according to claim 1 is characterized in that in the described precursor solution of acquisition, the volume ratio of organic reagent ethylene glycol or dimethyl formamide and water is 1～10: 1.
6. the preparation method of nanometer cobalt acid nickel according to claim 1 is characterized in that in the presoma preparation process, the temperature of reaction is 0～80 ℃, dropwises the back and continues to stir 0.5～48h, and drying temperature is 20～100 ℃, and the exsiccant time is 2～48h.
7. the preparation method of nanometer cobalt acid nickel according to claim 1 is characterized in that sintering temperature is 300～400 ℃, and the time is 2～24h.
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