CN109755032A - A kind of more shell CuCo2O4The preparation and its application of hollow nano-sphere - Google Patents
A kind of more shell CuCo2O4The preparation and its application of hollow nano-sphere Download PDFInfo
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- CN109755032A CN109755032A CN201910131076.0A CN201910131076A CN109755032A CN 109755032 A CN109755032 A CN 109755032A CN 201910131076 A CN201910131076 A CN 201910131076A CN 109755032 A CN109755032 A CN 109755032A
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention discloses a kind of more shell CuCo2O4The preparation and its application of hollow nano-sphere, the alkoxide hollow nanospheres of copper are prepared as presoma first with one step of hydro-thermal method, adjusting hydrothermal reaction time available nucleocapsid, bivalve, three shells presoma, presoma is sintered in air obtains the CuCo of hollow structure later2O4.CuCo prepared by the present invention2O4Hollow nano-sphere has the characteristics that high-specific surface area, regulatable hull number and active site abundant, to effectively improve the specific capacity of supercapacitor.In addition, stable shell and cavity structure can effectively alleviate the collapsing of supercapacitor electrode material structure in charge and discharge process, and then significant the cyclical stability for improving supercapacitor.The preparation method is easy to operate, and favorable reproducibility is easy to large-scale production.
Description
Technical field
The present invention relates to supercapacitor technologies fields, and in particular to a kind of more shell CuCo2O4The preparation of hollow nano-sphere and
It is applied.
Background technique
With the continuous growth of energy demand, the mankind while constantly developing various new energy, how more efficiently,
Low cost, environmental protection storage and convert these energy and be particularly important.In recent years, lithium ion battery and supercapacitor are recognized
To be the very potential power supply of electric car and mobile device, because having high-energy, high power, high efficiency and environment
The advantages that friendly.For energy storage device, key is exactly electrode material.Therefore the electrode material haveing excellent performance is designed and developed
As researcher's urgent problem.
Transition metal oxide becomes the important electrode material in energy storage field based on itself excellent physics, chemical property
Material.CuCo2O4As one kind of transition metal oxide, the oxide being made of two kinds of transition metal, it compares single metal oxide
Object has higher activity, to have higher capacity, too fast, the structural instability but its charge and discharge process is decayed is conductive
Property is bad, limits application.Hollow structure is often to possess biggish specific surface area, can provide more active sites, is increased
Add redox reaction ability.In addition, internal wide cavity can provide additional delay also for the volume expansion in reaction process
Space is rushed, the stability of structure is kept, meanwhile, compared to the hollow structure of single layer, multi-layer hollow structure can be further increased
Space utilization rate.Therefore, chemical property of the metal oxide electrode material for raising material of more shell hollow structures is obtained
It is very important.
Summary of the invention
Technical problem: in order to overcome the deficiencies in the prior art, the present invention provides a kind of more shell CuCo2O4It is hollow to receive
The preparation and its application of rice ball, the first object of the present invention are to provide a kind of high performance based on more shell CuCo2O4Hollow nano-sphere
Electrode material is used for supercapacitor；The second object of the present invention is to provide more shell CuCo2O4Hollow nano-sphere preparation method.
Technical solution: to achieve the above object, the present invention is made using the alkoxide hollow nanospheres that one step of hydro-thermal method prepares copper
For presoma, presoma is sintered in air obtains the CuCo of hollow structure later2O4, wherein control the hydro-thermal reaction time can
To obtain the presoma of nucleocapsid, bivalve, three shells, and then realize to hollow CuCo2O4The regulation of shell.
The present invention is achieved through the following technical solutions, and step includes:
A. by Cu (NO3)2·6H2O and Co (NO3)2·6H2O is dissolved in the mixed solution of isopropanol and glycerol, 160 DEG C-
Hydro-thermal reaction at 180 DEG C, is cooled to room temperature after reaction, washs drying, obtains Cu-Co presoma；
B. Cu-Co presoma is calcined in air atmosphere, obtains more shell CuCo2O4Hollow nano-sphere.
In the step a, Cu (NO3)2·6H2O and Co (NO3)2·6H2The molar ratio of O is 1:(2-4), isopropanol and sweet
The volume ratio of oil is (4-6): 1.
In the step a, the hydro-thermal reaction time 2-3h.Obtain nucleocapsid structure presoma.
In the step a, the hydro-thermal reaction time 4-5h obtains double-shell structure presoma.
In the step a, the hydro-thermal reaction time 7-8h obtains three-shell structure presomas.
In the step b, the calcination temperature is 300-400 DEG C, time 1-3h, and heating rate is 2 DEG C/min.
Preparation method preparation of the present invention has more shell CuCo2O4Hollow nano-sphere is applied to prepare super capacitor
Device electrode.
More shell CuCo2O4Hollow nano-sphere powder and Kynoar and acetylene black are with mass ratio (6-8): 1:1 is equal
Even mixing forms slurry, is applied in the nickel foam pre-processed, 2-3mg/cm2；The foam nickel electrode completed is smeared to be applied to
When supercapacitor, the memory device of high capacity and long circulation life is realized.
The utility model has the advantages that the present invention provides a kind of more shell CuCo2O4The preparation and its application of hollow nano-sphere, and it is existing
Technology compare the present invention has the advantages that
1.)CuCo2O4Zonal structure has stable skeleton and cavity structure, can slow down supercapacitor in charge and discharge
Electrode material structure collapses in the process, to significantly improve the cyclical stability of supercapacitor.
2.) more shell CuCo2O4Hollow nano-sphere has the characteristics that large specific surface area, active site are more, makes it have superior
Chemical property.
3.) hollow nano-sphere preparation method provided by the invention does not need to add any mould material, and reaction condition is mild
Controllably, experimental facilities requires simple, strong operability.
Detailed description of the invention
Fig. 1 is the alkoxide transmission electron microscope picture of copper prepared by embodiment 1；
Fig. 2 is CuCo prepared by embodiment 12O4Transmission electron microscope picture；
Fig. 3 is the alkoxide transmission electron microscope picture of copper prepared by embodiment 2；
Fig. 4 is CuCo prepared by embodiment 22O4Transmission electron microscope picture；
Fig. 5 is the alkoxide transmission electron microscope picture of copper prepared by embodiment 3；
Fig. 6 is CuCo prepared by embodiment 32O4Transmission electron microscope picture；
Fig. 7 is the CuCo that embodiment 1,2,3 obtains2O4Constant current charge-discharge curve graph；
Fig. 8 is the CuCo that embodiment 3 obtains2O4The circulation volume figure of active material.
Specific embodiment
The present invention is achieved through the following technical solutions, and step includes:
A. the alkoxide of copper is prepared；
By Cu (NO3)2·6H2O and Co (NO3)2·6H2O is dissolved in the mixed solution of isopropanol and glycerol, and hydro-thermal is anti-
It answers, is cooled to room temperature after reaction, wash drying, obtain Cu-Co presoma.
B. CuCo is prepared2O4；
Cu-Co presoma is placed in Muffle furnace, is calcined in air atmosphere, more shell CuCo are obtained2O4Hollow nano-sphere.
C. it assembles
By CuCo2O4Powder is applied in the nickel foam pre-processed, as electrode for assembling supercapacitor.
Embodiment
Invention is further explained combined with specific embodiments below.
Embodiment 1
1 mM of Co (NO3)2·6H2O and 0.5 mM of Cu (NO3)2·6H2O is dissolved in 33.5 milliliters of isopropyl
In alcohol, 6.5 milliliters of glycerol is added drop-wise in above-mentioned solution and is stirred 30 minutes；Then, obtained mixed liquor is transferred to 50 millis
It rises in stainless steel autoclave, is reacted 2 hours under the conditions of 180 DEG C.By obtained sediment by being collected by centrifugation, washed with dehydrated alcohol
It washs completely, it is 6 hours dry in 80 DEG C of baking ovens, obtain the alkoxide of copper.The alkoxide of copper is finally placed in 300 DEG C of calcinings in Muffle furnace
2 hours, heating rate was 2 DEG C/min, finally obtained CuCo2O4Hollow nucleocapsid ball material.By CuCo2O4Powdered, PVDF and second
Acetylene black is uniformly mixed with mass ratio 8:1:1, is applied in the nickel foam pre-processed, and active material quality is 2mg/cm2.It smears
The nickel foam of completion is as electrode for assembling supercapacitor.
Embodiment 2
1 mM of Co (NO3)2·6H2O and 0.5 mM of Cu (NO3)2·6H2O is dissolved in 33.5 milliliters of isopropyl
In alcohol, 6.5 milliliters of glycerol is added drop-wise in above-mentioned solution and is stirred 30 minutes；Then, obtained mixed liquor is transferred to 50 millis
It rises in stainless steel autoclave, is reacted 4 hours under the conditions of 160 DEG C.By obtained sediment by being collected by centrifugation, washed with dehydrated alcohol
It washs completely, it is 6 hours dry in 80 DEG C of baking ovens, obtain the alkoxide of copper.The alkoxide of copper is finally placed in 300 DEG C of calcinings in Muffle furnace
2 hours, heating rate was 2 DEG C/min, finally obtained CuCo2O4Hollow bivalve ball material.By CuCo2O4Powdered, PVDF and second
Acetylene black is uniformly mixed with mass ratio 8:1:1, is applied in the nickel foam pre-processed, and active material quality is 2mg/cm2.It smears
The nickel foam of completion is as electrode for assembling supercapacitor.
Embodiment 3
1 mM of Co (NO3)2·6H2O and 0.5 mM of Cu (NO3)2·6H2O is dissolved in 33.5 milliliters of isopropyl
In alcohol, 6.5 milliliters of glycerol is added drop-wise in above-mentioned solution and is stirred 30 minutes；Then, obtained mixed liquor is transferred to 50 millis
It rises in stainless steel autoclave, is reacted 8 hours under the conditions of 170 DEG C.By obtained sediment by being collected by centrifugation, washed with dehydrated alcohol
It washs completely, it is 6 hours dry in 80 DEG C of baking ovens, obtain the alkoxide of copper.The alkoxide of copper is finally placed in 300 DEG C of calcinings in Muffle furnace
2 hours, heating rate was 2 DEG C/min, finally obtained CuCo2O4Hollow three shells ball material.By CuCo2O4Powdered, PVDF and second
Acetylene black is uniformly mixed with mass ratio 8:1:1, is applied in the nickel foam pre-processed, and active material quality is 2mg/cm2.It smears
The nickel foam of completion is as electrode for assembling supercapacitor.
Embodiment 4
1 mM of Co (NO3)2·6H2O and 0.5 mM of Cu (NO3)2·6H2O is dissolved in 33.5 milliliters of isopropyl
In alcohol, 6.5 milliliters of glycerol is added drop-wise in above-mentioned solution and is stirred 30 minutes；Then, obtained mixed liquor is transferred to 50 millis
It rises in stainless steel autoclave, is reacted 7 hours under the conditions of 180 DEG C.By obtained sediment by being collected by centrifugation, washed with dehydrated alcohol
It washs completely, it is 6 hours dry in 80 DEG C of baking ovens, obtain the alkoxide of copper.The alkoxide of copper is finally placed in 350 DEG C of calcinings in Muffle furnace
2 hours, heating rate was 2 DEG C/min, finally obtained CuCo2O4Hollow three shells ball material.By CuCo2O4Powdered, PVDF and second
Acetylene black is uniformly mixed with mass ratio 8:1:1, is applied in the nickel foam pre-processed, and active material quality is 3mg/cm2.It smears
The nickel foam of completion is as electrode for assembling supercapacitor.
Embodiment 5
2 mMs of Co (NO3)2·6H2O and 0.5 mM of Cu (NO3)2·6H2O is dissolved in 26 milliliters of isopropanol
In, 6.5 milliliters of glycerol is added drop-wise in above-mentioned solution and is stirred 30 minutes；Then, obtained mixed liquor is transferred to 50 milliliters
In stainless steel autoclave, reacted 3 hours under the conditions of 180 DEG C.By obtained sediment by being collected by centrifugation, washed with dehydrated alcohol
Completely, 6 hours dry in 80 DEG C of baking ovens, obtain the alkoxide of copper.The alkoxide of copper is finally placed in 350 DEG C of calcinings 1 in Muffle furnace
Hour, heating rate is 2 DEG C/min, finally obtains CuCo2O4Hollow nucleocapsid ball material.By CuCo2O4Powdered, PVDF and second
Acetylene black is uniformly mixed with mass ratio 7:1:1, is applied in the nickel foam pre-processed, and active material quality is 2mg/cm2.It smears
The nickel foam of completion is as electrode for assembling supercapacitor.
Embodiment 6
2 mMs of Co (NO3)2·6H2O and 0.5 mM of Cu (NO3)2·6H2O is dissolved in 39 milliliters of isopropanol
In, 6.5 milliliters of glycerol is added drop-wise in above-mentioned solution and is stirred 30 minutes；Then, obtained mixed liquor is transferred to 50 milliliters
In stainless steel autoclave, reacted 5 hours under the conditions of 180 DEG C.By obtained sediment by being collected by centrifugation, washed with dehydrated alcohol
Completely, 6 hours dry in 80 DEG C of baking ovens, obtain the alkoxide of copper.The alkoxide of copper is finally placed in 400 DEG C of calcinings 2 in Muffle furnace
Hour, heating rate is 2 DEG C/min, finally obtains CuCo2O4Hollow bivalve ball material.By CuCo2O4Powdered, PVDF and second
Acetylene black is uniformly mixed with mass ratio 6:1:1, is applied in the nickel foam pre-processed, and active material quality is 2.5mg/cm2.It applies
The nickel foam for smearing completion is used to assemble supercapacitor as electrode.
Embodiment 7
1.5 mMs of Co (NO3)2·6H2O and 0.5 mM of Cu (NO3)2·6H2O is dissolved in 39 milliliters of isopropyl
In alcohol, 6.5 milliliters of glycerol is added drop-wise in above-mentioned solution and is stirred 30 minutes；Then, obtained mixed liquor is transferred to 50 millis
It rises in stainless steel autoclave, is reacted 3 hours under the conditions of 180 DEG C.By obtained sediment by being collected by centrifugation, washed with dehydrated alcohol
It washs completely, it is 6 hours dry in 80 DEG C of baking ovens, obtain the alkoxide of copper.The alkoxide of copper is finally placed in 400 DEG C of calcinings in Muffle furnace
3 hours, heating rate was 2 DEG C/min, finally obtained CuCo2O4Hollow nucleocapsid ball material.By CuCo2O4Powdered, PVDF and second
Acetylene black is uniformly mixed with mass ratio 7:1:1, is applied in the nickel foam pre-processed, and active material quality is 2mg/cm2.It smears
The nickel foam of completion is as electrode for assembling supercapacitor.
Embodiment 8
1 mM of Co (NO3)2·6H2O and 0.5 mM of Cu (NO3)2·6H2O is dissolved in 39 milliliters of isopropanol
In, 6.5 milliliters of glycerol is added drop-wise in above-mentioned solution and is stirred 30 minutes；Then, obtained mixed liquor is transferred to 50 milliliters
In stainless steel autoclave, reacted 8 hours under the conditions of 180 DEG C.By obtained sediment by being collected by centrifugation, washed with dehydrated alcohol
Completely, 6 hours dry in 80 DEG C of baking ovens, obtain the alkoxide of copper.The alkoxide of copper is finally placed in 400 DEG C of calcinings 1 in Muffle furnace
Hour, heating rate is 2 DEG C/min, finally obtains CuCo2O4Hollow three shells ball material.By CuCo2O4Powdered, PVDF and second
Acetylene black is uniformly mixed with mass ratio 8:1:1, is applied in the nickel foam pre-processed, and active material quality is 2mg/cm2.It smears
The nickel foam of completion is as electrode for assembling supercapacitor.The above is only a preferred embodiment of the present invention, should
It points out: for those skilled in the art, without departing from the principle of the present invention, if can also make
Dry improvements and modifications, these modifications and embellishments should also be considered as the scope of protection of the present invention.
Claims (8)
1. a kind of more shell CuCo2O4The preparation method of hollow nano-sphere, which is characterized in that the preparation method includes the following steps:
A. by Cu (NO3)2·6H2O and Co (NO3)2·6H2O is dissolved in the mixed solution of isopropanol and glycerol, and 160 DEG C -180
Hydro-thermal reaction at DEG C, is cooled to room temperature after reaction, washs drying, obtains Cu-Co presoma；
B. Cu-Co presoma is calcined in air atmosphere, obtains more shell CuCo2O4Hollow nano-sphere.
2. a kind of more shell CuCo according to claim 12O4The preparation method of hollow nano-sphere, which is characterized in that the step
In a, Cu (NO3)2·6H2O and Co (NO3)2·6H2The molar ratio of O is 1:(2-4), the volume ratio of isopropanol and glycerol is (4-
6): 1.
3. a kind of more shell CuCo according to claim 12O4The preparation method of hollow nano-sphere, which is characterized in that the step
In a, the hydro-thermal reaction time 2-3h obtains nucleocapsid structure presoma.
4. a kind of more shell CuCo according to claim 12O4The preparation method of hollow nano-sphere, which is characterized in that the step
In a, the hydro-thermal reaction time 4-5h obtains double-shell structure presoma.
5. a kind of more shell CuCo according to claim 12O4The preparation method of hollow nano-sphere, which is characterized in that the step
In a, the hydro-thermal reaction time 7-8h obtains three-shell structure presomas.
6. a kind of more shell CuCo according to claim 12O4The preparation method of hollow nano-sphere, which is characterized in that the step
In b, the calcination temperature is 300-400 DEG C, time 1-3h, and heating rate is 2 DEG C/min.
7. a kind of have more shell CuCo using preparation method described in claim 1 preparation2O4The application of hollow nano-sphere,
It is characterized in that, is used to prepare electrode of super capacitor.
8. according to claim 7 have more shell CuCo2O4The application of hollow nano-sphere, which is characterized in that more shells
CuCo2O4Hollow nano-sphere powder is with Kynoar and acetylene black with mass ratio (6-8): 1:1 is uniformly mixed, and forms slurry, is applied
It is put in the nickel foam pre-processed, 2-3mg/cm2；When smearing the foam nickel electrode completed applied to supercapacitor, realize
The memory device of high capacity and long circulation life.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106745326A (en) * | 2017-02-06 | 2017-05-31 | 江苏大学 | ZnCo2O4The preparation method of hollow nuclear shell ball |
| CN108609665A (en) * | 2018-05-31 | 2018-10-02 | 安阳师范学院 | Core-shell structure copolymer hollow-core construction zinc-cobalt sulfide nanosphere electrode material and preparation method thereof |
| CN109663595A (en) * | 2018-12-11 | 2019-04-23 | 中科廊坊过程工程研究院 | A kind of copper based composite metal oxidate hollow microsphere, preparation method and the usage |
-
2019
- 2019-02-21 CN CN201910131076.0A patent/CN109755032A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106745326A (en) * | 2017-02-06 | 2017-05-31 | 江苏大学 | ZnCo2O4The preparation method of hollow nuclear shell ball |
| CN108609665A (en) * | 2018-05-31 | 2018-10-02 | 安阳师范学院 | Core-shell structure copolymer hollow-core construction zinc-cobalt sulfide nanosphere electrode material and preparation method thereof |
| CN109663595A (en) * | 2018-12-11 | 2019-04-23 | 中科廊坊过程工程研究院 | A kind of copper based composite metal oxidate hollow microsphere, preparation method and the usage |
Non-Patent Citations (2)
| Title |
|---|
| GAOFENG LI ET AL.: "Self-templated formation of CuCo2O4triple-shelled hollow microspheres for all-solid-state asymmetric supercapacitors", 《JOURNAL OF ALLOYS AND COMPOUNDS》 * |
| SAEID KAMARI KAVERLAVANI ET AL.: "Self-templated synthesis of uniform nanoporous CuCo2O4 double-shelled hollow spheres for high-performance asymmetric supercapacitors", 《CHEM. COMMUN.》 * |
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Application publication date: 20190514 |