CN110120306A - A kind of Co-Mo-O-S spherical shape flowers structural composite material and its preparation method and application - Google Patents
A kind of Co-Mo-O-S spherical shape flowers structural composite material and its preparation method and application Download PDFInfo
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- CN110120306A CN110120306A CN201910438330.1A CN201910438330A CN110120306A CN 110120306 A CN110120306 A CN 110120306A CN 201910438330 A CN201910438330 A CN 201910438330A CN 110120306 A CN110120306 A CN 110120306A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/46—Metal oxides
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
The invention discloses a kind of Co-Mo-O-S spherical shape flowers structural composite material, microstructure is that spherical flowers structure covers with petal based on ball on ball；The ingredient of the ball is CoS and MoS2, the ingredient of the petal is Mo8O23.Preparation method includes the following steps: 1) preparation of Co-Mo-O presoma；2) preparation of Co-Mo-O-S spherical shape flowers composite material.As the application of electrode material for super capacitor, the charge and discharge within the scope of 0-0.35V, when discharge current density is 1A/g, specific capacitance is 1100-1200 F/g.The present invention avoids introducing the carbon material of low specific capacitance, comprising: and 1, only need hydro-thermal method, without being sintered carbonization, preparation process is simple, and low energy consumption；2, specific capacitance with higher.Meanwhile by vulcanisation operation, realizes spherical flowers structure, greatly improve the cyclical stability of material.
Description
Technical field
The present invention relates to the preparation technical fields of sulfide composite material, and in particular to a kind of Co-Mo-O-S spherical shape flowers
Structural composite material and its preparation method and application.
Background technique
Supercapacitor is as a kind of efficient energy storage device that prospect is bright and clear, because its power density is high, charge and discharge
Rate is fast, the advantages that having extended cycle life, and has caused the extensive research interest of researcher.Core, that is, electrode of supercapacitor
Material will have a direct impact on the main performance index of supercapacitor, and at present, the Main way point of supercapacitor research is
Find even more ideal and low-cost electrode material.
Electrode material for electric double layer capacitor, such as carbon material have the characteristics that stability is good, still, due to its specific capacitance compared with
It is low, and it is unable to satisfy application requirement；In contrast, faraday's capacitance electrode material, such as transition metal oxide and transition metal
Sulfide has the specific capacitance performance much higher than double layer capacity material.
But the prior art is when preparing faraday's capacitance electrode material, it is electric as faraday using single metallic element
Hold electrode material, there is a problem of that material microstructure is unstable and causes super capacitor material cyclicity poor.In order to
Solve the problems, such as this, transition metal oxide or transient metal sulfide is are loaded to microstructure by the method that the prior art uses
On stable carbon material.
The prior art of transition metal oxide class, and Pan Chao et al. (Hi-Tech Fiber Application, 2017
Year 01 phase, ISSN:1007-9815) by the metal oxide nanoparticles of modified in conjunction with graphene, obtained a kind of graphite
The material that alkene wraps up metal oxide is used for supercapacitor.The specific capacitance of the material only has when discharge current density is 1A/g
411 F/g；After having recycled 3000 circles, cycle life is held only in the 70% of original capacitance；After hydro-thermal reaction, by material
Final sample can just be prepared by being sintered.
The prior art of transient metal sulfide class, Gaoyang et al. (" preparation of multi-element metal sulfide electrode material and its
The research of performance of the supercapacitor ", Zhengzhou University, classification number: TM53) using the functional form complex of Co as presoma, it adopts
With simple solvent thermal reaction, synthesize the CoS of a large amount of three-dimensional graded structure1.097Micro-flowers, the CoS finally obtained1.097
Electrode material of the micro-flowers as supercapacitor.Its chemical property is the result shows that monometallic CoS1.097Micro-flowers specific capacity
Only 533F/g, forthright again is 84%.Specific capacitance and cycle performance are in reduced levels, and therefore, the technology is by CoS1.097Micron
Flower is supported on carbon material graphene oxide further to promote material property, is finally obtained the specific capacitance of 810 F/g and is up to
90% high rate performance.
Equally, Dai Jie et al. (" MoS of different-shape2And MoS2Application of the composite material in supercapacitor ", Lanzhou
University, classification number: TM53, TB33) only prepare transient metal sulfide MoS2It is also only real as the electrode material of supercapacitor
Show under the current density of 0.5A/g, MoS2The specific capacity having is 145 F/g, after 1000 circulations, the electricity that measures
Capacity is 65% technical effect of initial capacitance.The solution that the prior art provides be also with carbon material carbon fiber into
Row is compound, and specific capacitance is promoted to 400 F/g, forthright again to be also promoted to 74% by 65%.
By analyze the above-mentioned prior art it is found that only with single transition metal oxide or transient metal sulfide without
Method solves the problems, such as cyclical stability, it is necessary to by being loaded carbon material come Xie Wenti.
And there is following technical problem in the method for loading this kind of prior art of carbon material:
Although 1, the stability of supercapacitor can be improved in carbon material, since the specific capacitance that it is provided is smaller, a large amount of
Carbon material is added, the effect for improving supercapacitor stability is realized, necessarily causes super capacitor material entirety specific capacitance big
Width decline；
2, the preparation process of carbon material can just be prepared after needing (after hydro-thermal reaction) use to be sintered carbonization to carbonaceous material
Final electrode material out, it is clear that there are the cumbersome technical problems of energy consumption height, preparation process.
Summary of the invention
The object of the present invention is to provide a kind of Co-Mo-O-S spherical shape flowers structural composite materials and preparation method thereof.
Using faraday's capacitance electrode material of a variety of high specific capacitances, transition metal oxide and transient metal sulfide into
Row is compound instead of carbon material supported method.This method is due to being not necessarily to complex carbon material, thus the process for the sintering carbonization cut down,
Realize the technical effect for simplifying preparation process, reducing energy consumption；Simultaneously as composite material is faraday's capacitor of high specific capacitance
Electrode material can improve super in the case where keeping without carbon material supported and improving supercapacitor cycle performance
The specific capacitance of grade capacitor.
It is simply that two kinds of transition metal oxides and transient metal sulfide progress are compound but with the prior art, it can not
Realize the raising and improvement of chemical property, specific embodiment described content can confirm this case through the invention.
Therefore, it is necessary to just be able to achieve foregoing invention purpose using the bimetallic synergy generated between transition metal.
The prior art use multi-element metal sulfide coprecipitation method the problem is that, be unable to control two kinds or two kinds with
On inorganic salts settling rate, lead to prepare that material granule is uneven, pattern is uncontrollable, i.e. inhomogeneity.On overcoming
Technical problem is stated, the present invention uses two one-step hydrothermals, effectively controls the granular size and microscopic appearance of material, obtains spherical flowers
Structure improves the specific capacitance and cyclical stability of material.
In order to achieve the above-mentioned object of the invention, the technical solution adopted by the present invention are as follows:
Co-Mo-O-S spherical shape flowers structural composite material, with Co (NO3)2·6H2O、(NH4)6Mo7O24·4H2O、CO(NH2)2、
NH4F and dissolvable sulfide are starting material, are made through hydro-thermal reaction.Its microstructure is spherical flowers structure, is with ball
Main body covers with petal on ball；The ingredient of the ball is CoS and MoS2, the ingredient of the petal is Mo8O23。
The preparation method of Co-Mo-O-S spherical shape flowers structural composite material, comprising the following steps:
1) preparation of Co-Mo-O presoma, Co (NO3)2·6H2O、(NH4)6Mo7O24·4H2O、CO(NH2)2、NH4F presses (2-
4): the ratio between amount of substance of 0.4:6:4 weighs and soluble in water, and magnetic agitation 15-25min is transferred the solution into autoclave,
And 4-6 h is kept at 120-140 DEG C, it is cooled to room temperature, filters, is dried to obtain Co-Mo-O presoma；
2) preparation of Co-Mo-O-S spherical shape flowers composite material, Co-Mo-O presoma and dissolvable sulfide press 3:(10-30)
The ratio between the amount of substance, first weigh Co-Mo-O presoma and be dissolved in water and ultrasound, after pour into dissolvable sulfide aqueous solution, obtain
It is transferred in autoclave after mixed solution, and keeps 11-13 h at 100-120 DEG C, be cooled to room temperature, filter, be dried to obtain
Co-Mo-O-S composite material.
Application of the Co-Mo-O-S spherical shape flowers structural composite material as electrode material for super capacitor, it is characterised in that:
The charge and discharge within the scope of 0-0.35V, when discharge current density is 1A/g, specific capacitance is 1100-1200 F/g.
Gained Co-Mo-O-S spherical shape flowers structural composite material experiment detection of the invention, as a result as follows:
It, should by sem test in order to prove the size and particle diameter distribution of Co-Mo-O-S spherical shape flowers structural composite material
The partial size of material is 2-5 μm.
In order to prove the structure feature of Co-Mo-O-S spherical shape flowers structural composite material, pass through transmissioning electric mirror test, the material
The structure of material is spherical flowers structure.
The electrochemical property test of Co-Mo-O-S spherical shape flowers structural composite material detects the charge and discharge within the scope of 0-0.35V
Electricity, when discharge current density is 1 A/g, Co-Mo-O-S spherical shape flowers structural composite material electrode of super capacitor specific capacitance
Range shows that Co-Mo-O-S spherical shape flowers structural composite material has good super capacitor performance in 1100-1200F/g.
Co-Mo-O-S spherical shape flowers structural composite material of the invention has the advantage that the prior art
1. the present invention is using Co (NO3)2·6H2O、(NH4)6Mo7O24·4H2O、CO(NH2)2、NH4F and dissolvable sulfide are made
For reaction reagent, Co-Mo-O-S spherical shape flowers structural composite material, which is made, to be realized and mentions in the case where not adding carbon material
The effect of high supercapacitor stability, and specific capacitance is 1100-1200F/g；
2.Co-Mo-O-S spherical shape flowers structural composite material is synthesized using two one-step hydrothermals, and first step hydro-thermal obtains oxide, the
Two step hydro-thermals obtain sulfide, for a step hydro-thermal, can be effectively controlled the granular size and microscopic appearance of material, obtain spherical
Flowers structure improves the specific capacitance and cyclical stability of material；And resulting materials, without being sintered carbonization, low energy consumption.
3. Co-Mo-O-S spherical shape flowers structural composite material of the present invention, treatment process is understandable, is suitble to be prepared on a large scale.
Therefore, the present invention has broad application prospects in super capacitor material field.
Detailed description of the invention:
Fig. 1 is the scanning electron microscope that embodiment 1 prepares the Co-Mo-O-S spherical shape flowers structural composite material that sulphion concentration is 2 M
Figure；
Fig. 2 is the scanning electron microscope that comparative example 2 prepares the Co-Mo-O-S spherical shape flowers structural composite material that sulphion concentration is 3 M
Figure；
Fig. 3 is the scanning electron microscope that comparative example 2 prepares the Co-Mo-O-S spherical shape flowers structural composite material that sulphion concentration is 4 M
Figure；
Fig. 4 is the transmission electron microscope picture that embodiment 1 prepares Co-Mo-O-S spherical shape flowers structural composite material；
Fig. 5 is that Co-Mo-O-S spherical shape flowers composite material prepared by embodiment 1 and Co-Ni-O-S prepared by its comparative example 1 are compound
The discharge curve of material；
Fig. 6 is the Co-Mo-O-S spherical shape flowers composite material that sulphion concentration prepared by embodiment 1 is 2M and its comparative example 2 system
The Co-Mo-O-S composite material that Co-Mo-O-S composite material that standby sulphion concentration is 3M, sulphion concentration are 4M is put
Electric curve graph；
Fig. 7 is the Co-Mo-O-S spherical shape flowers composite material and its 3 one step hydro-thermal system of comparative example of 1 liang of embodiment step hydro-thermal preparation
The discharge curve of standby Co-Mo-O-S composite material；
Fig. 8 is the XRD of Co-Mo-O presoma prepared by embodiment 1 and Co-Mo-O-S spherical shape flowers composite material；
Fig. 9 is the cycle life curve of Co-Mo-O-S spherical shape flowers composite material prepared by embodiment 1.
Specific embodiment
The present invention is described in further detail the content of present invention in conjunction with Figure of description, but be not pair by embodiment
Restriction of the invention.
Embodiment 1
A kind of Co-Mo-O-S spherical shape flowers shape composite material and preparation method thereof:
Preparation Co (the NO of step 1) Co-Mo-O presoma3)2·6H2O、(NH4)6Mo7O24·4H2O、CO(NH2)2、NH4F presses 2:
The ratio between amount of substance of 0.4:6:4 weighs rear soluble in water, and acquired solution is transferred in autoclave by 20 min of magnetic agitation,
And 5 h are kept at 130 DEG C, it is cooled to room temperature, filters, is dried to obtain Co-Mo-O presoma；
The preparation of step 2 Co-Mo-O-S spherical shape flowers composite material takes 0.1g Co-Mo-O presoma to be dissolved in water and ultrasound,
The Na that 30ml sulphion concentration is 2M is poured into afterwards2S aqueous solution, mixed solution is transferred in autoclave, and is kept at 110 DEG C
12 h, are cooled to room temperature, and filter, are dried to obtain Co-Mo-O-S composite material.
In order to prove the size and particle diameter distribution of Co-Mo-O-S spherical shape flowers structural composite material, surveyed by scanning electron microscope
Examination, the partial size of the material as shown in Figure 1 are 2-5 μm.
In order to prove the structure feature of Co-Mo-O-S spherical shape flowers structural composite material, by transmissioning electric mirror test, such as scheme
The structure of the material shown in 4 is spherical flowers structure.
The electrochemical property test of Co-Mo-O-S spherical shape flowers shape composite material, method particularly includes: weigh 0.008 g
Co-Mo-O-S composite material, 0.001 g acetylene black and 0.001 g ptfe micropowder are placed in small agate and grind in alms bowl, be added
0.5 mL ethyl alcohol is ground；The foamed nickel current collector of the sample after grinding and 1 mm thickness is suppressed with the pressure of 10 kPa,
It in air, at room temperature dries, cuts into the cm of 2 cm × 2, electrode of super capacitor is made, tests its specific capacitance.
Testing result is as shown in Figure 5, it is known that: the charge and discharge within the scope of 0-0.35V, when discharge current density is 1 A/g,
Co-Mo-O-S spherical shape flowers shape composite supercapacitor electrode specific capacitance is 1142 F/g.
Comparative example 1
In order to study influence of the bimetallic synergy generated between transition metal to material property, it is prepared for Co-Ni-O-S
Composite material, the preparation method of not specified step and the above-mentioned Co-Mo-O-S composite material of the present embodiment in specific steps
It is identical.
The difference is that: by (NH in the step 14)6Mo7O24·4H2O replaces with Ni (NO3)2·6H2O is made
It is standby.
Obtained Co-Ni-O-S composite material is subjected to electro-chemical test, test method is same as Example 1, detection knot
Fruit is as shown in figure 5, the charge and discharge within the scope of 0-0.35V, and when discharge current density is 1 A/g, specific capacitance is 340 F/g.
Therefore, under same current density, the discharge time of Co-Mo-O-S electrode material is apparently higher than Co-Ni-O-S electricity
Pole material, discharge time improves shows that its specific capacitance is obviously improved compared with the performance of Co-Ni-O-S material more 4 times, table
Bright Co-Mo-O-S composite material has good super capacitor performance.
Comparative example 2
In order to study influence of the microscopic appearance to Co-Mo-O-S composite property, i.e. influence of the experimental technique to material property,
It is identical to control raw material, only changes experimental process parameters, is prepared for the Co-Mo-O-S composite material of different sulphion concentration,
The system for the Co-Mo-O-S composite material that not specified step and the above-mentioned sulphion concentration of the present embodiment are 2M in specific steps
Preparation Method is identical.
The difference is that: sulphion concentration is that have become sulphion concentration be 3M and 4 M to 2 M in the step 3.
By the sulphion concentration prepared in comparative example for 3M, 4M Co-Mo-O-S composite material through sem test institute
Microscopic appearance is as shown in Figure 2 and Figure 3, experimental result show, and the microscopic appearances of comparative example resulting materials is large grained, rather than
Spherical flowers structure.
Electrochemical property test method is same as Example 1, testing result as shown in fig. 6, gained sulphion concentration be 3M,
The Co-Mo-O-S composite material of the large grained (aspherical flowers structure) of 4M is when discharge current density is 1 A/g, specific capacitance
Respectively 733F/g and 210F/g.
Therefore, the microscopic appearance of material influences performance significant, the specific capacitance size point of spherical flowers structural composite material
It is not 1.5 times and 5 times of the composite material for the large grained that sulphion concentration is 3M, 4M, shows the microcosmic of spherical flowers structure
Pattern has directly obtained the technical effect that composite material capacitive property significantly improves.
Therefore, the technology that gained composite material only provides through the invention is made into spherical flowers shape ability
Realize excellent chemical property.
Comparative example 3
It is to use the influence of one-step method or two-step method to Co-Mo-O-S spherical shape flowers composite property to study hydro-thermal,
That is influence of the experimental technique to material property, control raw material is identical, only changes experimental process parameters, is prepared for by a step water
The Co-Mo-O-S composite material that heat obtains, not specified step is obtained with the above-mentioned two steps hydro-thermal of the present embodiment in specific steps
The preparation method of the Co-Mo-O-S spherical shape flowers structural composite material obtained is identical.
The difference is that: the step 3 is removed, by 30ml Na2S aqueous solution directly pours into matched solution in step 1.
XRD by the Co-Mo-O-S spherical shape flowers structural composite material of two step hydro-thermals preparation is as shown in Figure 8, it can be seen that
MoO and CoO are obtained from Co-Mo-O presoma prepared by first step hydro-thermal, from Co-Mo-O presoma and Na2Bis- hydro-thermals of S
MoS has been obtained in the Co-Mo-O-S composite material of preparation2And CoS, and this is step hydro-thermal preparation Co-Mo-O-S composite material
It is unobtainable.
Co-Mo-O-S composite material prepared by a step hydro-thermal in comparative example carries out electro-chemical test, test method and reality
It is identical to apply example 1, testing result is as shown in fig. 7, the charge and discharge within the scope of 0-0.35V, when discharge current density is 1 A/g, than
Capacitor is 302 F/g.
Therefore, material made from two step hydro-thermals influences performance significant, and the specific capacitance of spherical flowers structural composite material is big
Small is 3.5 times of the Co-Mo-O-S composite material of step hydro-thermal preparation, shows the Co-Mo-O-S composite wood of spherical flowers structure
Material performance is obviously improved, and shows that Co-Mo-O-S composite material has good super capacitor performance.
Claims (6)
1. a kind of Co-Mo-O-S spherical shape flowers structural composite material, it is characterised in that: its microstructure is spherical flowers structure,
Based on ball, petal is covered on ball；The ingredient of the ball is CoS and MoS2, the ingredient of the petal is Mo8O23。
2. Co-Mo-O-S spherical shape flowers structural composite material according to claim 1, it is characterised in that: with Co (NO3)2·
6H2O、(NH4)6Mo7O24·4H2O、CO(NH2)2、NH4F and dissolvable sulfide are starting material, are made through hydro-thermal reaction.
3. according to the preparation method of Co-Mo-O-S spherical shape flowers structural composite material described in claim 1, it is characterised in that including
Following steps:
1) preparation of Co-Mo-O presoma weighs Co (NO by the ratio between the amount of certain substance3)2·6H2O、(NH4)6Mo7O24·
4H2O、CO(NH2)2、NH4F is soluble in water, and magnetic agitation 15-25min is transferred the solution into autoclave, and in 120-140
4-6 h is kept at DEG C, is cooled to room temperature, is filtered, is dried to obtain Co-Mo-O presoma；
2) it is molten to weigh Co-Mo-O presoma by the ratio between the amount of certain substance for the preparation of Co-Mo-O-S spherical shape flowers composite material
After water and ultrasound, dissolvable sulfide aqueous solution is poured into, is transferred in autoclave after obtaining mixed solution, and in 100-120
11-13 h is kept at DEG C, is cooled to room temperature, is filtered, is dried to obtain Co-Mo-O-S composite material.
4. preparation method according to claim 3, it is characterised in that: Co (NO used in the step 1)3)2·6H2O、
(NH4)6Mo7O24·4H2O、CO(NH2)2、NH4The ratio between amount of substance of F is (2-4): 0.4:6:4；Used in the step 2
The ratio between amount of substance of Co-Mo-O presoma and dissolvable sulfide is 3:(10-30).
5. preparation method according to claim 3, it is characterised in that: the sulphur of the step 2 dissolvable sulfide aqueous solution
Ion concentration is 0.1-0.2 M.
6. Co-Mo-O-S spherical shape flowers structural composite material is as electrode material for super capacitor according to claim 1
Using, it is characterised in that: the charge and discharge within the scope of 0-0.35V, when discharge current density is 1A/g, specific capacitance 1100-
1200 F/g。
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