CN109841422A - Co3O4/Co2P coaxial heterogeneous structure material and its preparation method and application - Google Patents
Co3O4/Co2P coaxial heterogeneous structure material and its preparation method and application Download PDFInfo
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Abstract
The present invention relates to a kind of Co3O4/Co2P coaxial heterogeneous structure material and preparation method thereof, includes following steps: 1) cobalt hydroxide nano wire being obtained phosphatization cobalt nanowire using hydrogen phosphide atmosphere sintering;2) phosphatization cobalt nanowire is handled by short annealing, aoxidizes superficial layer, obtains Co3O4/Co2P coaxial heterogeneous structure micro super capacitor electrode material.The beneficial effects of the present invention are: for Co3O4/Co2P coaxial heterogeneous structure, the Co of outer layer3O4Fake capacitance capacity will be provided, and the Co of internal layer2P has high conductivity;Meanwhile because electrochemical reaction occurs over just material surface or near surface, due to internal layer Co under higher reaction potential2P can not direct Contact-sorption solion, water decomposition can't be catalyzed.Therefore, which maintains higher capacity and cyclical stability, it may have preferable electronic conduction ability, high rate performance are improved.
Description
Technical field
The invention belongs to material preparations and micro super capacitor crossing domain, and in particular to a kind of Co3O4/Co2P is coaxial
Heterogeneous structure material and preparation method thereof.
Background technique
With scientific and technological progress and development, human society has been entered the age of information, has been developed based on semiconductor technology
The modern electronic equipment come and technology great convenience daily life, wearable intelligent electronic device and Internet of Things go out
Now with the universal demand for further increasing people to energy storage device micromation, portability.It is miniature super in miniature energy storage device
Grade capacitor (Microsupercpacitors, MSCs) is because its power density is high, the charge and discharge time is fast and has extended cycle life
Advantage and have received widespread attention, and have good application prospect in microelectronic field, medical field and machinery field.But at present
The main reason for energy density of MSCs is low, is insufficient for small electronic equipment demand, this is limitation MSCs development.
Summary of the invention
The present invention proposes a kind of Co3O4/Co2P coaxial heterogeneous structure micro super capacitor electrode material and its preparation,
Preparation process is simple, resulting Co3O4/Co2P coaxial heterogeneous structure has higher as the positive electrode of micro super capacitor
Theoretical capacity, and maintain good cyclical stability and high rate performance.
The technical proposal adopted by the invention to solve the above technical problems is that: Co3O4/Co2P coaxial heterogeneous structure material,
For coaxial heterogeneous structure, diameter is between 70 nanometers to 300 nanometers, and length is 600 nanometers to 2 microns, nano wire coaxial heterogeneous
The internal layer of structure is Co2P, outer layer Co3O4, outer layer Co3O4Oxidated layer thickness is 1.2 to 2 nanometers.
The Co3O4/Co2The preparation method of P coaxial heterogeneous structure material, includes following steps:
1) cobalt hydroxide nano wire is obtained into phosphatization cobalt nanowire using hydrogen phosphide atmosphere sintering;
2) phosphatization cobalt nanowire is handled by short annealing, aoxidizes superficial layer, obtains Co3O4/Co2P coaxial heterojunction
Structure micro super capacitor electrode material.
According to the above scheme, the cobalt hydroxide nano wire be using cobalt chloride hexahydrate, ammonium fluoride and urea as raw material, with
Nickel foam is substrate, is prepared using hydro-thermal method.
According to the above scheme, the molar ratio of the cobalt chloride hexahydrate, ammonium fluoride and urea is 2:1:4.
According to the above scheme, step 1) is using sodium hypophosphite pyrolytic as phosphine gas source.
According to the above scheme, sintering described in step 1) is that 300 DEG C are warming up to 2 DEG C/min rate, keeps the temperature 3 hours.
According to the above scheme, short annealing described in step 2) is to be warming up in quick anneal oven using 5 DEG C/min rate
250 DEG C, keep the temperature 3 minutes.
The Co3O4/Co2Application of the P coaxial heterogeneous structure material as micro super capacitor electrode anode material.
With Co3O4/Co2P coaxial heterogeneous structure is as positive electrode, with Fe2O3Nanowire structure is negative electrode material, using receiving
Rice indentation, prepares microelectrode, is assembled into asymmetric miniature ultracapacitor device.
Present invention combination Co3O4With Co2The different characteristics and synthesis preparation method of P innovatively propose design synthesis
Co3O4/Co2P coaxial heterogeneous structure.By the Co with coaxial heterogeneous structure3O4/Co2When P is applied to high load amount MSCs, surface layer
Co3O4It can provide high capacitance by electrochemical reaction, and Co2It is vertical to meet device that P provides quick electron transport channel
Demand is conducted to electronics, so that the specific energy density of MSCs can be effectively improved in material structure angle, is avoided through complexity
The electronics conducting networks of produced by micro processing process optimization MSCs, to realize that MSCs energy density and the effective of high rate performance mention
It rises, provides a kind of effective, simple, feasible new way for the further development of MSCs.
The beneficial effects of the present invention are: for Co3O4/Co2P coaxial heterogeneous structure, the Co of outer layer3O4Fake capacitance appearance will be provided
Amount, and the Co of internal layer2P has high conductivity;Meanwhile because electrochemical reaction occurs over just material surface or near surface, higher
Reaction potential under due to internal layer Co2P can not direct Contact-sorption solion, water decomposition can't be catalyzed.Therefore, this is coaxial
Heterojunction structure maintains higher capacity and cyclical stability, it may have preferable electronic conduction ability, high rate performance are mentioned
It is high.
Detailed description of the invention
Fig. 1 is the Co of the embodiment of the present invention3O4/Co2The preparation of P coaxial heterogeneous structure micro super capacitor electrode material
Flow chart;
Fig. 2 is the SEM figure of the embodiment of the present invention 1, and wherein Fig. 2 a is the SEM of phosphatization cobalt nanowire in the embodiment of the present invention 1
Figure;Fig. 2 b is Co in the embodiment of the present invention 13O4/Co2The SEM of P coaxial heterogeneous structure schemes;Fig. 2 c is the embodiment of the present invention 1, implements
The SEM figure of di-iron trioxide nano wire in example 2, embodiment 3;
Fig. 3 is the Co in the embodiment of the present invention 13O4/Co2The energy of P coaxial heterogeneous structure micro super capacitor electrode material
Spectrogram;
Fig. 4 is the cyclic voltammogram (figure a) of the phosphatization cobalt nanowire for preparing in the embodiment of the present invention 1 in the case where 5mV/s sweeps speed
With Co3O4/Co2Cyclic voltammogram (figure b) of the P coaxial heterogeneous structure in the case where 5mV/s sweeps speed;
Fig. 5 is the high rate performance figure (figure a) and Co of the cobaltosic oxide nano line prepared in the embodiment of the present invention 13O4/
Co2The high rate performance figure (figure b) of P coaxial heterogeneous structure.
Specific embodiment
For a better understanding of the present invention, below with reference to the embodiment content that the present invention is furture elucidated, but it is of the invention
Content is not limited solely to the following examples.
Embodiment 1:
A kind of Co3O4/Co2The preparation process of P coaxial heterogeneous structure micro super capacitor electrode material, such as Fig. 1, including
Following steps:
1) hydro-thermal method is used, cobalt hydroxide nano wire is prepared:
1a) nickel foam is cleaned: clip nickel foam first passes sequentially through hydrochloric acid, deionized water, acetone, EtOH Sonicate 15 and divides
Clock, it is 12 hours dry in 60 DEG C of baking ovens, it takes out and weighs dried foam nickel quality;
1b) 2mmol cobalt chloride hexahydrate, 1mmol ammonium fluoride, 4mmol urea will be added in 70mL deionized water respectively,
Stirring is allowed to be uniformly dissolved for 15 minutes;
1c) solution is added in ptfe autoclave, be put into cleaning after load weighted nickel foam, 120 DEG C into
Row hydro-thermal 8-12 hours, after cooling, with deionized water and ethyl alcohol centrifuge washing, being put into oven drying and obtaining loading had cobalt hydroxide
The nickel foam of nano wire;
2) using sodium hypophosphite pyrolytic as hydrogen phosphide source, by cobalt hydroxide nano wire and sodium hypophosphite according to
The mass ratio of 1:10 is placed in two porcelain boats, is put into tube furnace jointly, is warming up to 300 DEG C with 2 DEG C/min, is kept the temperature 3 hours, obtain
Phosphatization cobalt nanowire.
3) cobalt hydroxide nano wire is put into tube furnace, using argon gas as protective atmosphere, is warming up to 350 with 2 DEG C/min
DEG C, 2 hours are kept the temperature, cobaltosic oxide nano line is obtained.
4) phosphatization cobalt nanowire is put into quick anneal oven, is warming up to 250 DEG C with 5 DEG C/min, keeps the temperature 3 minutes, make table
Face phosphatization cobalt oxidation, and then obtain Co3O4/Co2P coaxial heterogeneous structure.
5) using 1mol/L potassium hydroxide aqueous solution as electrolyte, using mercury-mercury oxide reference electrode, three electrodes is constructed and are surveyed
Examination system carries out electrochemical property test, including cyclic voltammetric, constant current charge-discharge etc..By weighing quality, nickel foam is obtained
Upper active material load capacity, calculates the specific discharge capacity of material.
6) with Co3O4/Co2P coaxial heterogeneous structure is as positive electrode, with Fe2O3Nanowire structure is negative electrode material, is used
Nanoindentation prepares microelectrode, is assembled into asymmetric miniature ultracapacitor device.
The resulting Co of the present embodiment3O4/Co2P coaxial heterogeneous structure micro super capacitor electrode material, internal layer Co2P,
Outer layer is Co3O4.Using this synthetic schemes, phosphatization cobalt nanowire diameter of movement is in 100 rans (as shown in Figure 2 a), length
800 nanometers (as shown in Figure 2 a), nano wire homoepitaxial is in foam nickel base.Co3O4/Co2P coaxial heterogeneous structure outer layer
For Co3O4Oxide layer (as shown in Figure 3), with a thickness of 1.2 to 2 nanometers.The Co being sintered in argon gas3O4Nano wire pattern base
This is consistent with cobalt hydroxide nano wire.Since crystal transfer, Co occurring during the sintering process3O4Nano wire is actually by many
Small nanometer rods are connected with each other, and are arranged as nano wire pattern.The Co obtained through hydrogen phosphide atmosphere sintering2After P surface oxidation most
The Co obtained eventually3O4/Co2P coaxial heterogeneous structure, pattern is consistent with phosphatization cobalt nanowire, is uniformly grown in foam nickel base
(as shown in Figure 2 b).The Fe of synthesis2O3Nanowire diameter is uniformly grown in foam 500 or so in 70 rans, length
In nickel substrate (as shown in Figure 2 c).
With the resulting Co of the present embodiment3O4/Co2P coaxial heterogeneous structure micro super capacitor electrode material, in 1mol/L
It is tested in potassium hydroxide aqueous solution, under the current density of 1A/g, Co3O4Nanowire Quality specific capacity reaches 767F/g, Co2P nanometers
Line mass specific capacity is 446F/g (as shown in fig. 4 a), Co3O4/Co2P coaxial heterogeneous structure specific discharge capacity is 590F/g (as schemed
Shown in 4b).Under the current density of 20A/g, Co3O4Nanowire Quality specific capacity is that its specific discharge capacity can still keep 390F/g,
Capacity attenuation 49.15% (as shown in Figure 5 a);Co3O4/Co2P coaxial heterogeneous structure specific discharge capacity reaches 468F/g, capacity attenuation
Only 20.68% (as shown in Figure 5 b).Co3O4/Co2P coaxial heterogeneous structure as supercapacitor have excellent high rate performance and
Chemical stability.In production capacity-energy storage-function integration device is constructed, due to its high energy density, connect with solar battery
After LED etc. can be lighted in the case where disconnecting solar battery.
Embodiment 2:
A kind of Co3O4/Co2The preparation process of P coaxial heterogeneous structure micro super capacitor electrode material, including walk as follows
It is rapid:
1) hydro-thermal method is used, cobalt hydroxide nano wire is prepared:
1a) nickel foam is cleaned: clip nickel foam first passes sequentially through hydrochloric acid, deionized water, acetone, EtOH Sonicate 15 and divides
Clock, it is 12 hours dry in 60 DEG C of baking ovens, it takes out and weighs dried foam nickel quality;
1b) 70mL deionized water will be added in 5mmol cobalt chloride hexahydrate, 2.5mmol ammonium fluoride, 10mmol urea respectively
In, stirring is allowed to be uniformly dissolved for 20 minutes;
1c) solution is added in ptfe autoclave, be put into cleaning after load weighted nickel foam, 120 DEG C into
Row hydro-thermal 8-12 hours, after cooling, with deionized water and ethyl alcohol centrifuge washing, being put into oven drying and obtaining loading had cobalt hydroxide
The nickel foam of nano wire;
2) using sodium hypophosphite pyrolytic as hydrogen phosphide source, by cobalt hydroxide nano wire and sodium hypophosphite according to
The mass ratio of 1:10 is placed in two porcelain boats, is put into tube furnace jointly, is warming up to 300 DEG C with 2 DEG C/min, is kept the temperature 3 hours, obtain
Phosphatization cobalt nanowire.
3) cobalt hydroxide nano wire is put into tube furnace, using argon gas as protective atmosphere, is warming up to 350 with 2 DEG C/min
DEG C, 2 hours are kept the temperature, cobaltosic oxide nano line is obtained.
4) phosphatization cobalt nanowire is put into quick anneal oven, is warming up to 250 DEG C with 5 DEG C/min, keeps the temperature 3 minutes, make table
Face phosphatization cobalt oxidation, and then obtain Co3O4/Co2P coaxial heterogeneous structure.
5) using 1mol/L potassium hydroxide aqueous solution as electrolyte, using mercury-mercury oxide reference electrode, three electrodes is constructed and are surveyed
Examination system carries out electrochemical property test, including cyclic voltammetric, constant current charge-discharge etc..By weighing quality, nickel foam is obtained
Upper active material load capacity, calculates the specific discharge capacity of material.
6) with Co3O4/Co2P coaxial heterogeneous structure is as positive electrode, with Fe2O3Nanowire structure is negative electrode material, is used
Nanoindentation prepares microelectrode, is assembled into asymmetric miniature ultracapacitor device.
With the resulting Co of the present embodiment3O4/Co2P coaxial heterogeneous structure micro super capacitor electrode material, in 1mol/L
It is tested in potassium hydroxide aqueous solution, under the current density of 1A/g, Co3O4Nanowire Quality specific capacity reaches 700F/g, Co2P nanometers
Line mass specific capacity is 440F/g, Co3O4/Co2P coaxial heterogeneous structure specific discharge capacity is 557F/g.It is close in the electric current of 20A/g
Under degree, Co3O4/Co2P coaxial heterogeneous structure specific discharge capacity reaches 432F/g, capacity attenuation only 22.44%.Co3O4/Co2P is coaxial
Heterojunction structure has excellent high rate performance and chemical stability as supercapacitor.In production capacity-energy storage-function integration device
It, can be in disconnection solar battery in the case where point after being used in conjunction with solar battery due to its high energy density during part is constructed
Bright LED etc..
Embodiment 3:
A kind of Co3O4/Co2The preparation process of P coaxial heterogeneous structure micro super capacitor electrode material, including walk as follows
It is rapid:
1) hydro-thermal method is used, cobalt hydroxide nano wire is prepared:
1a) nickel foam is cleaned: clip nickel foam first passes sequentially through hydrochloric acid, deionized water, acetone, EtOH Sonicate 15 and divides
Clock, it is 12 hours dry in 60 DEG C of baking ovens, it takes out and weighs dried foam nickel quality.
1b) 70mL deionized water will be added in 10mmol cobalt chloride hexahydrate, 5mmol ammonium fluoride, 20mmol urea respectively
In, stirring is allowed to be uniformly dissolved for 30 minutes.
1c) solution is added in ptfe autoclave, be put into cleaning after load weighted nickel foam, 120 DEG C into
Row hydro-thermal 8-12 hours, after cooling, with deionized water and ethyl alcohol centrifuge washing, being put into oven drying and obtaining loading had cobalt hydroxide
The nickel foam of nano wire.
2) using sodium hypophosphite pyrolytic as hydrogen phosphide source, by cobalt hydroxide nano wire and sodium hypophosphite according to
The mass ratio of 1:10 is placed in two porcelain boats, is put into tube furnace jointly, is warming up to 300 DEG C with 2 DEG C/min, is kept the temperature 3 hours, obtain
Phosphatization cobalt nanowire.
3) cobalt hydroxide nano wire is put into tube furnace, using argon gas as protective atmosphere, is warming up to 350 with 2 DEG C/min
DEG C, 2 hours are kept the temperature, cobaltosic oxide nano line is obtained.
4) phosphatization cobalt nanowire is put into quick anneal oven, is warming up to 250 DEG C with 5 DEG C/min, keeps the temperature 3 minutes, make table
Face phosphatization cobalt oxidation, and then obtain Co3O4/Co2P coaxial heterogeneous structure.
5) using 1mol/L potassium hydroxide aqueous solution as electrolyte, using mercury-mercury oxide reference electrode, three electrodes is constructed and are surveyed
Examination system carries out electrochemical property test, including cyclic voltammetric, constant current charge-discharge etc..By weighing quality, nickel foam is obtained
Upper active material load capacity, calculates the specific discharge capacity of material.
6) with Co3O4/Co2P coaxial heterogeneous structure is as positive electrode, with Fe2O3Nanowire structure is negative electrode material, is used
Nanoindentation prepares microelectrode, is assembled into asymmetric miniature ultracapacitor device.
With the resulting Co of the present embodiment3O4/Co2P coaxial heterogeneous structure micro super capacitor electrode material, in 1mol/L
It is tested in potassium hydroxide aqueous solution, under the current density of 1A/g, Co3O4Nanowire Quality specific capacity reaches 680F/g, Co2P nanometers
Line mass specific capacity is 423F/g, Co3O4/Co2P coaxial heterogeneous structure specific discharge capacity is 543F/g.It is close in the electric current of 20A/g
Under degree, Co3O4/Co2P coaxial heterogeneous structure specific discharge capacity reaches 416F/g, capacity attenuation only 23.38%.Co3O4/Co2P is coaxial
Heterojunction structure has excellent high rate performance and chemical stability as supercapacitor.In production capacity-energy storage-function integration device
It, can be in disconnection solar battery in the case where point after being used in conjunction with solar battery due to its high energy density during part is constructed
Bright LED etc..
Claims (8)
1.Co3O4/Co2P coaxial heterogeneous structure material, is coaxial heterogeneous structure, and diameter is long between 70 nanometers to 300 nanometers
Degree is 600 nanometers to 2 microns, and the internal layer of nano wire coaxial heterogeneous structure is Co2P, outer layer Co3O4, outer layer Co3O4Aoxidize thickness
Degree is 1.2 to 2 nanometers.
2. Co described in claim 13O4/Co2The preparation method of P coaxial heterogeneous structure material, includes following steps:
1) cobalt hydroxide nano wire is obtained into phosphatization cobalt nanowire using hydrogen phosphide atmosphere sintering;
2) phosphatization cobalt nanowire is handled by short annealing, aoxidizes superficial layer, obtains Co3O4/Co2P coaxial heterogeneous structure is micro-
Type electrode material for super capacitor.
3. Co according to claim 23O4/Co2The preparation method of P coaxial heterogeneous structure material, it is characterized in that the hydrogen
Aoxidizing cobalt nanowire, using nickel foam as substrate, is prepared using hydro-thermal method using cobalt chloride hexahydrate, ammonium fluoride and urea as raw material
And it obtains.
4. Co according to claim 33O4/Co2The preparation method of P coaxial heterogeneous structure material, it is characterized in that described six
The molar ratio of hydrated cobalt chloride, ammonium fluoride and urea is 2:1:4.
5. Co according to claim 23O4/Co2The preparation method of P coaxial heterogeneous structure material, it is characterized in that step 1) with
Sodium hypophosphite pyrolytic is as phosphine gas source.
6. Co according to claim 23O4/Co2The preparation method of P coaxial heterogeneous structure material, it is characterized in that step 1) institute
The sintering stated is that 300 DEG C are warming up to 2 DEG C/min rate, keeps the temperature 3 hours.
7. Co according to claim 23O4/Co2The preparation method of P coaxial heterogeneous structure material, it is characterized in that step 2) institute
The short annealing stated is to be warming up to 250 DEG C using 5 DEG C/min rate in quick anneal oven, keeps the temperature 3 minutes.
8. Co described in claim 13O4/Co2P coaxial heterogeneous structure material is as micro super capacitor electrode anode material
Application.
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CN113697786A (en) * | 2021-09-22 | 2021-11-26 | 中山大学 | Preparation method of needle-shaped cobalt phosphide with phosphorus vacancies and application of needle-shaped cobalt phosphide in seawater electrolysis hydrogen production |
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