CN106698527A - Hydrothermal method for preparing nanometer nickel cobaltate by taking ethylene glycol and water as solvent system - Google Patents
Hydrothermal method for preparing nanometer nickel cobaltate by taking ethylene glycol and water as solvent system Download PDFInfo
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
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Abstract
The invention belongs to the field of nanometer materials and discloses a hydrothermal method for preparing nanometer nickel cobaltate by taking ethylene glycol and water as a solvent system. The method comprises the following steps: taking the ethylene glycol and water as the solvent system, taking nickel nitrate hexahydrate, cobalt nitrate hexahydrate and urea as raw materials, and preparing the nanometer nickel cobaltate by utilizing a hydrothermal method. The nickel cobaltate prepared by taking the ethylene glycol and water as the solvent system has a layered micro-porous structure and a relatively small size, contributes to enabling active materials and electrolyte to be in fully contact, and has better conductivity and higher electrochemical activity and stability. The nickel cobaltate of a nanometer spinel structure is prepared by the hydrothermal method, the potential application of the nickel cobaltate serving as an advanced super-capacitor electrode is proved, the research of taking binary metal oxides as energy conversion materials is stimulated, a novel route is provided for producing high-performance super-capacitor electrodes on a large scale, and industrialization is easily realized.
Description
Technical field
The invention belongs to field of nanometer material technology, a kind of method for being related to hydro-thermal method to prepare nano nickel cobalt oxide, more particularly to
The method that ethylene glycol and water prepare nano nickel cobalt oxide for dicyandiamide solution.
Background technology
Energy and environment turn into the theme of China Today sustainable development, in recent years due to excessively using fossil fuel, ring
Pollute the growing interest that people are caused with energy storage shortage in border.High performance power supply, such as ultracapacitor and lithium-ion electric
Pond, it has also become many researcher field of special interest.Ultracapacitor, also referred to as electrochemical capacitor, tool
Just like high-energy-density, fast charging and discharging rate has extended cycle life, the low advantage of maintenance cost.Many work all concentrate on negative pole
Material, particularly transition metal oxide, such as cobaltosic oxide, nickel oxide, di-iron trioxide, manganese dioxide, zinc oxide, cobalt acid
Nickel etc. has been caused great concern due to its theoretical specific capacity higher.
Bimetallic oxide cobalt acid nickel, with low cost, stability is high, aboundresources, the feature of environmental protection, excellent microwave absorption
Performance, the advantage of controllable size and shape, it is well known that the size and pattern of material can influence its chemical property.It is different
The cobalt acid nickel of pattern, such as nanometer sheet, nanosphere, nano particle, nanometer rods, nanoneedle and nano wire etc., are widely used in super electricity
The fields such as container, electrochemical sensor, medicine delivery and lithium ion battery.The cobalt acid nickel of spinel structure is due to a cobalt original
Son is replaced by nickle atom, is compared with nickel oxide or cobalt/cobalt oxide, the electro-chemical activity with more preferable electric conductivity and Geng Gao.Mesh
Before, the preparation method of nano nickel cobalt oxide mainly has mainly includes colloidal sol-gel method, Hydrothermal Synthesiss and electrodeposition process.Wherein,
Hydro-thermal method extensive use because equipment is simple, easily operated.Using hydro-thermal method can prepare that other methods cannot synthesize it is new
Material, noval chemical compound, are characterized in that product good dispersion, purity be high, particle is relatively easy to control.The performance of the electrochemistry of electrode material
It is highly dependent on the structure of electrode, including form, the condition on size and surface etc..Therefore, prepared not using hydro-thermal method herein
With the cobalt acid nickel of pattern, operating process is simple, and cost is relatively low, and products therefrom particle is uniform, and function admirable, reunion degree is smaller,
Pattern is preferable, it is easy to accomplish industrialization.
The content of the invention
The purpose of the present invention is that to use ethylene glycol and water be dicyandiamide solution, and with six water nickel nitrates, cobalt nitrate hexahydrate and urea are original
Material, nano nickel cobalt oxide is prepared using hydro-thermal method.Method is simple, and raw material is easier to obtain, and preparation cost is relatively low, of reduced contamination, fits
For industrialized production.
Technical scheme is as follows:
In the method that ethylene glycol and water prepare nano nickel cobalt oxide as dicyandiamide solution hydro-thermal method, comprise the following steps:
(1)A certain amount of nickel salt and cobalt salt are weighed, is dissolved under the conditions of magnetic agitation in the mixed solvent of water and ethylene glycol, obtained
Mixed liquor A;
(2)In step(1)In the mixed liquor A of gained, a certain amount of precipitating reagent is added, stirred under the conditions of magnetic agitation and form equal
Even mixture B;;
(3)By step(2)The mixture B of gained is transferred in reactor, and 12h, natural cooling are reacted at a temperature of 120 ~ 160 DEG C
To room temperature, products therefrom centrifugation, respectively with deionized water and washes of absolute alcohol 3 times, the solid after separation is put
Enter drying in thermostatic drying chamber;Obtain cobalt acid nickel presoma;
(4)By Muffle furnace temperature programming to calcining heat, then by step(3)The cobalt acid nickel presoma of gained is placed in Muffle furnace
Calcining, calcining end obtains final product cobalt acid nickel.
Step(1)In, the nickel salt and cobalt salt are respectively Nickelous nitrate hexahydrate and cabaltous nitrate hexahydrate, Nickelous nitrate hexahydrate
It is 1 with the ratio between the amount of cabaltous nitrate hexahydrate material:2.
Step(1)In, in the mixed solvent of water and ethylene glycol, the volume ratio of water and ethylene glycol is 1:1.
Step(2)In, the precipitating reagent is urea,
The step(1)The amount summation and step of middle nickel salt and cobalt salt material(2)The ratio between amount of material of middle urea is 1:3.
Step(2)In, the time of the magnetic agitation is 0.5 hour.
Step(3)In, the temperature of the freeze-day with constant temperature is 60 DEG C, and the time is 12h.
Step(4)In, the calcining heat is 300 ~ 350 DEG C, and calcination time is 2h;The speed of the Muffle furnace temperature programming
Rate is 2 DEG C/min.
This experiment reagent used is all analyzes pure, is commercially available.
Beneficial effects of the present invention:
With ethylene glycol and water as dicyandiamide solution, with six water nickel nitrates, cobalt nitrate hexahydrate and urea are raw material to the present invention, using hydro-thermal
Method prepares nano nickel cobalt oxide.Method is simple, and raw material is easier to obtain, and preparation cost is relatively low, of reduced contamination, and products therefrom particle is equal
Even, function admirable, reunion degree is smaller, it is adaptable to industrialized production.
Brief description of the drawings
The X ray diffracting spectrum of Fig. 1 samples(XRD), a is the XRD spectrum of the sample of embodiment 1 in figure, and b is embodiment in figure
The XRD spectrum of 2 samples, c is the XRD spectrum of the sample of embodiment 3 in figure, and d is the XRD spectrum of the sample of embodiment 4 in figure, in figure
E is the XRD spectrum of the sample of embodiment 5;
The SEM of the sample of Fig. 2 embodiments 1(SEM)Collection of illustrative plates;
The transmission electron microscope of the sample of Fig. 3 embodiments 1(TEM)Collection of illustrative plates.
Specific embodiment
With reference to Figure of description and specific implementation example, the present invention will be further described, so that those skilled in the art are more
The present invention is understood well, but the invention is not limited in following examples.
Embodiment 1
0.4351 gram of Nickelous nitrate hexahydrate and 0.8739 gram of cabaltous nitrate hexahydrate are weighed, 40 millis are dissolved under the conditions of magnetic agitation
In the solvent for rising(20 milliliters of water and 20 milliliters of ethylene glycol);0.8106 gram of urea is subsequently added, is stirred under the conditions of magnetic agitation
Mix 0.5 hour and form uniform mixture;Above-mentioned mixed solution is transferred in reactor, 12h is reacted at a temperature of 160 DEG C,
After naturally cooling to room temperature, by products therefrom centrifugation, respectively with deionized water and washes of absolute alcohol 3 times, after separation
Solid be put into 60 DEG C of thermostatic drying chamber in dry 12h;Then gained cobalt acid nickel presoma is forged in 350 DEG C of Muffle furnace
Burn 2 hours, Muffle furnace is heated up with 2 DEG C per minute of condition, obtain final product cobalt acid nickel, XRD such as Fig. 1 a of sample.
Embodiment 2
0.4357 gram of Nickelous nitrate hexahydrate and 0.8736 gram of cabaltous nitrate hexahydrate are weighed, 40 millis are dissolved under the conditions of magnetic agitation
In the solvent for rising(40 ml deionized waters);0.8096 gram of urea is subsequently added, is stirred 0.5 hour under the conditions of magnetic agitation
Form uniform mixture;Above-mentioned mixed solution is transferred in reactor, 12h is reacted at a temperature of 160 DEG C, naturally cooled to
After room temperature, products therefrom centrifugation, respectively with deionized water and washes of absolute alcohol 3 times, the solid after separation is put into
12h is dried in 60 DEG C of thermostatic drying chamber;Then gained cobalt acid nickel presoma is calcined into 2 hours, horse in 350 DEG C of Muffle furnace
Not stove is heated up with 2 DEG C per minute of condition, obtains final product cobalt acid nickel, XRD such as Fig. 1 b of sample.
Embodiment 3
0.4359 gram of Nickelous nitrate hexahydrate and 0.8741 gram of cabaltous nitrate hexahydrate are weighed, 40 millis are dissolved under the conditions of magnetic agitation
In the solvent for rising(40 milliliters of ethylene glycol);0.8102 gram of urea is subsequently added, is stirred under the conditions of magnetic agitation 0.5 hour and is formed
Uniform mixture;Above-mentioned mixed solution is transferred in reactor, 12h is reacted at a temperature of 160 DEG C, naturally cool to room temperature
Afterwards, by products therefrom centrifugation, respectively with deionized water and washes of absolute alcohol 3 times, the solid after separation is put into 60 DEG C
Thermostatic drying chamber in dry 12h;Then gained cobalt acid nickel presoma is calcined into 2 hours, Muffle furnace in 350 DEG C of Muffle furnace
Heated up with 2 DEG C per minute of condition, obtained final product cobalt acid nickel, XRD such as Fig. 1 c of sample.
Embodiment 4
0.4351 gram of Nickelous nitrate hexahydrate and 0.8732 gram of cabaltous nitrate hexahydrate are weighed, 40 millis are dissolved under the conditions of magnetic agitation
In the solvent for rising(Water and ethylene glycol ratio are 1:1);0.8112 gram of urea is subsequently added, 0.5 is stirred under the conditions of magnetic agitation
Hour forms uniform mixture;Above-mentioned mixed solution is transferred in reactor, 12h is reacted at a temperature of 120 DEG C, it is naturally cold
But to after room temperature, by products therefrom centrifugation, respectively with deionized water and washes of absolute alcohol 3 times, by the solid after separation
It is put into 60 DEG C of thermostatic drying chamber and dries 12h;Then gained cobalt acid nickel presoma is calcined 2 in 300 DEG C of Muffle furnace small
When, Muffle furnace is heated up with 2 DEG C per minute of condition, obtains final product cobalt acid nickel, XRD such as Fig. 1 d of sample.
Embodiment 5
0.4362 gram of Nickelous nitrate hexahydrate and 0.8728 gram of cabaltous nitrate hexahydrate are weighed, 40 millis are dissolved under the conditions of magnetic agitation
In the solvent for rising(Water and ethylene glycol ratio are 1:1);0.8102 gram of urea is subsequently added, 0.5 is stirred under the conditions of magnetic agitation
Hour forms uniform mixture;Above-mentioned mixed solution is transferred in reactor, 12h is reacted at a temperature of 140 DEG C, it is naturally cold
But to after room temperature, by products therefrom centrifugation, respectively with deionized water and washes of absolute alcohol 3 times, by the solid after separation
It is put into 60 DEG C of thermostatic drying chamber and dries 12h;Then gained cobalt acid nickel presoma is calcined 2 in 300 DEG C of Muffle furnace small
When, Muffle furnace is heated up with 2 DEG C per minute of condition, obtains final product cobalt acid nickel, XRD such as Fig. 1 e of sample.
Fig. 1 illustrates that cobalt acid nickel has pure Emission in Cubic, and extra diffraction maximum or other phases is not observed, and shows in letter
The cobalt acid nickel nano material with high-purity is obtained after single annealing process.Product at differential responses temperature and calcining heat
With different crystalline structures.The chemical property of the cobalt acid nickel nano material of different structure is tested in subsequent experimental.
Highdensity cobalt acid nickel nano wire is uniformly distributed after Fig. 2 illustrates to be displayed in simple annealing process, whole nanometer
The average diameter that line has about 20nm, length extends to hundreds of nanometers, and this small crystalline size necessarily causes cobalt acid nickel nanometer
Line has specific surface area higher so that they more effectively can be contacted with electrolyte ion, and this is conducive to active material
Make full use of.
Fig. 3 illustrates that cobalt acid nickel nano wire has the layering central hole structure of well-crystallized, and these layering loose structures are by big
The nanocrystal composition of small about 20nm, this unique layering porous form feature makes electrolyte be easily penetrate into cobalt acid nickel
In nano wire, and the volumetric expansion during effectively adapting to charge and discharge process, so as to improve electrochemical reaction performance.
Claims (7)
1. the method for nano nickel cobalt oxide being prepared as dicyandiamide solution hydro-thermal method with ethylene glycol and water, it is characterised in that including following step
Suddenly:
(1)A certain amount of nickel salt and cobalt salt are weighed, is dissolved under the conditions of magnetic agitation in the mixed solvent of water and ethylene glycol, obtained
Mixed liquor A;
(2)In step(1)In the mixed liquor A of gained, a certain amount of precipitating reagent is added, stirred under the conditions of magnetic agitation and form equal
Even mixture B;
(3)By step(2)The mixture B of gained is transferred in reactor, and 12h, natural cooling are reacted at a temperature of 120 ~ 160 DEG C
To room temperature, products therefrom centrifugation, respectively with deionized water and washes of absolute alcohol 3 times, the solid after separation is put
Enter drying in thermostatic drying chamber;Obtain cobalt acid nickel presoma;
(4)By Muffle furnace temperature programming to calcining heat, then by step(3)The cobalt acid nickel presoma of gained is placed in Muffle furnace
Calcining, calcining end obtains final product cobalt acid nickel.
2. the method that nano nickel cobalt oxide is prepared as dicyandiamide solution hydro-thermal method with ethylene glycol and water according to claim 1, its
It is characterised by, step(1)In, the nickel salt and cobalt salt are respectively Nickelous nitrate hexahydrate and cabaltous nitrate hexahydrate, six nitric hydrates
The ratio between amount of nickel and cabaltous nitrate hexahydrate material is 1:2.
3. the method that nano nickel cobalt oxide is prepared as dicyandiamide solution hydro-thermal method with ethylene glycol and water according to claim 1, its
It is characterised by, step(1)In, in the mixed solvent of water and ethylene glycol, the volume ratio of water and ethylene glycol is 1:1.
4. the method that nano nickel cobalt oxide is prepared as dicyandiamide solution hydro-thermal method with ethylene glycol and water according to claim 1, its
It is characterised by, step(2)In, the precipitating reagent is urea, the step(1)The amount summation and step of middle nickel salt and cobalt salt material
(2)The ratio between amount of material of middle urea is 1:3.
5. the method that nano nickel cobalt oxide is prepared as dicyandiamide solution hydro-thermal method with ethylene glycol and water according to claim 1, its
It is characterised by, step(2)In, the time of the magnetic agitation is 0.5 hour.
6. the method that nano nickel cobalt oxide is prepared as dicyandiamide solution hydro-thermal method with ethylene glycol and water according to claim 1, its
It is characterised by, step(3)In, the temperature of the freeze-day with constant temperature is 60 DEG C, and the time is 12h.
7. the method that nano nickel cobalt oxide is prepared as dicyandiamide solution hydro-thermal method with ethylene glycol and water according to claim 1, its
It is characterised by, step(4)In, the calcining heat is 300 ~ 350 DEG C, and calcination time is 2h;The Muffle furnace temperature programming
Speed is 2 DEG C/min.
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Cited By (8)
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CN107824172A (en) * | 2017-10-12 | 2018-03-23 | 大连理工大学 | A kind of preparation method of nano oxidized alumina supporter of the surface rich in defective bit |
CN108155271A (en) * | 2017-11-28 | 2018-06-12 | 华灿光电(苏州)有限公司 | The chip and preparation method of a kind of light emitting diode |
CN108910963A (en) * | 2018-06-25 | 2018-11-30 | 青岛大学 | A kind of Fe, Ni replace altogether cobalt-based spinel-type absorbing material and its preparation method and application |
CN108980622A (en) * | 2018-08-20 | 2018-12-11 | 中国石油大学(北京) | A kind of nano combined pour-point depressant and its preparation method and application |
CN110395774A (en) * | 2019-07-19 | 2019-11-01 | 五邑大学 | A kind of preparation method and application of cobalt acid nickel porous material |
CN113649007A (en) * | 2021-08-31 | 2021-11-16 | 广东工业大学 | Nano-structured NiCo spinel catalyst material and preparation method and application thereof |
CN114284082A (en) * | 2021-12-30 | 2022-04-05 | 江西科技师范大学 | Preparation method and application of high-capacitance oxygen vacancy rare earth doped cobaltosic oxide nanosheet |
WO2023019664A1 (en) * | 2021-08-20 | 2023-02-23 | 武汉工程大学 | Method for preparing boron nitride nanotube by means of double-transition metal oxide catalysis |
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Cited By (15)
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CN108910963A (en) * | 2018-06-25 | 2018-11-30 | 青岛大学 | A kind of Fe, Ni replace altogether cobalt-based spinel-type absorbing material and its preparation method and application |
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CN108980622A (en) * | 2018-08-20 | 2018-12-11 | 中国石油大学(北京) | A kind of nano combined pour-point depressant and its preparation method and application |
CN108980622B (en) * | 2018-08-20 | 2020-03-13 | 中国石油大学(北京) | Nano composite pour point depressant, and preparation method and application thereof |
CN110395774A (en) * | 2019-07-19 | 2019-11-01 | 五邑大学 | A kind of preparation method and application of cobalt acid nickel porous material |
WO2021012397A1 (en) * | 2019-07-19 | 2021-01-28 | 五邑大学 | Method for preparing nickel cobaltate porous material, and use thereof |
CN110395774B (en) * | 2019-07-19 | 2022-04-08 | 五邑大学 | Preparation method and application of nickel cobaltate porous material |
WO2023019664A1 (en) * | 2021-08-20 | 2023-02-23 | 武汉工程大学 | Method for preparing boron nitride nanotube by means of double-transition metal oxide catalysis |
CN113649007A (en) * | 2021-08-31 | 2021-11-16 | 广东工业大学 | Nano-structured NiCo spinel catalyst material and preparation method and application thereof |
CN114284082A (en) * | 2021-12-30 | 2022-04-05 | 江西科技师范大学 | Preparation method and application of high-capacitance oxygen vacancy rare earth doped cobaltosic oxide nanosheet |
CN114284082B (en) * | 2021-12-30 | 2023-04-28 | 江西科技师范大学 | Preparation method and application of high-capacitance oxygen vacancy rare earth doped cobaltosic oxide nano-sheet |
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