CN109817905A - A kind of ZnMn2O4/Mn2O3The preparation of composite material and its test method of chemical property - Google Patents
A kind of ZnMn2O4/Mn2O3The preparation of composite material and its test method of chemical property Download PDFInfo
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- CN109817905A CN109817905A CN201811631105.1A CN201811631105A CN109817905A CN 109817905 A CN109817905 A CN 109817905A CN 201811631105 A CN201811631105 A CN 201811631105A CN 109817905 A CN109817905 A CN 109817905A
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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
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- 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
- Y02E60/10—Energy storage using batteries
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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
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Abstract
The invention belongs to technical field of composite preparation, disclose a kind of ZnMn2O4/Mn2O3The preparation of composite material and its test method of chemical property；Composite material the preparation method comprises the following steps: by KOH and NaOH deionized water dissolving, wiring solution-forming A；By the Zn (CH of 0.5mol/L3COO)2Solution pours into the Mn (CH of 1.0mol/L3COO)2Wiring solution-forming B in solution；Solution B is added dropwise in solution A；Mixed solution is transferred in autoclave, reacts for 24 hours under the conditions of 180 DEG C, is centrifugated product after cooled to room temperature；Substance after centrifugation is placed in tube furnace, in air atmosphere 500 DEG C of calcining 5h, natural cooling.The present invention can be seen that the material is with good stability by the impedance curve of material before and after comparison charge and discharge, by electro-chemical test it can be seen that the material has good high rate performance and cycle performance.
Description
Technical field
The invention belongs to technical field of composite preparation more particularly to a kind of ZnMn2O4/Mn2O3The preparation of composite material
And its test method of chemical property.
Background technique
Currently, the prior art commonly used in the trade is such that
In recent years, as the development of new energy materials, lithium ion battery and supercapacitor more attract attention.Super electricity
Container is a kind of novel energy storage device, also referred to as electrochemical capacitor.In terms of energy storage, compared to other energy storage devices,
With higher specific capacitance and specific power, and in terms of all have significant advantage.At present for super
Its electrode material and electrolyte are mainly studied in the research of grade capacitor.There is charcoal as the common material of electrode of super capacitor
Material, conducting polymer, metal hydroxides, metal oxide, metal sulfide, metal nitride and metal phosphide and its
Composite material etc..
ZnMn2O4Electrode material as supercapacitor have specific capacity is high, raw material sources are abundant, it is cheap, pacify
The advantages that Atoxic, but volume expansion occurs when transformation reaction during circulating battery and shrinks that larger, conductivity is low for it, leads
Cause the decaying of its capacity circulating very fast, high rate capability is insufficient.Synthesis ZnMn at present2O4Common method has ball-milling method, hydro-thermal
Method, coprecipitation, method of electrostatic spinning etc..
In conclusion problem of the existing technology is:
(1) existing technology synthesizes zinc manganate composite material generally by two steps, and 80 DEG C of stirrings are anti-before this for such method
8h is answered, then by sediment washing, drying to constant weight, as composite material precursor, presoma is obtained in 900 DEG C of calcining 6h
Final composite material.This method operating process is more complicated, and required temperature is higher, consumes energy more.
(2) prior art due to calcination temperature it is higher, obtained material be it is blocky, need just to can be used after crushing, powder
Particle after broken is larger, small as electrode material specific capacitance.
Solve the difficulty and meaning of above-mentioned technical problem: zinc manganate composite material is synthesized by two-step process in existing technology,
Such method was stirred to react 8h for 80 DEG C before this, preceding as composite material precursor then by sediment washing, drying to constant weight
Body is driven in 900 DEG C of calcining 6h, obtains final material.It solves the disadvantage that the prior art while obtaining the higher material of specific capacitance,
Need to invent new synthetic route.The present invention can prepare ZnMn by the method that hydro-thermal method and solid phase method combine2O4/Mn2O3It is multiple
Condensation material, compare the prior art, and calcination temperature is lower, and what is obtained is a kind of composite material, specific capacity with higher.
Summary of the invention
In view of the problems of the existing technology, the present invention provides a kind of ZnMn2O4/Mn2O3The preparation of composite material and its
The test method of chemical property.
The invention is realized in this way a kind of ZnMn with outstanding high rate performance2O4/Mn2O3Composite material, this is compound
Material is compared to single ZnMn2O4Material, there are holes and defect between lattice for the composite material, and ion can be improved
Insertion and abjection quantity and migration rate between lattice, improve the capacity and high rate performance of material.ZnMn2O4/Mn2O3It is compound
Material also has application generally as the electrode material of Zinc ion battery in supercapacitor.The preparation method of the composite material
Are as follows:
Step 1: by 3.00gKOH and 1.50gNaOH 20mL deionized water dissolving, wiring solution-forming A；
Step 2: by the Zn (CH of 5mL0.5mol/L3COO)2Solution pours into the Mn (CH of 5mL1.0mol/L3COO)2Solution
Middle wiring solution-forming B；
Step 3: under agitation, solution B is added dropwise in solution A；
Step 4: after being added dropwise to complete, mixed solution being transferred in autoclave, is reacted for 24 hours under the conditions of 180 DEG C,
Product is centrifugated after cooled to room temperature；
Step 5: the substance after centrifugation is placed in tube furnace, in air atmosphere 500 DEG C of calcining 5h, natural cooling
?.
Further, the ZnMn2O4/Mn2O3The physical property of composite material carries out test characterization, XRD using XRD and SEM
Test uses Empyrean x-ray diffractometer, and pipe presses 40kV, the Cu target K alpha ray of Guan Liu 40mA, λ=0.15406nm；SEM
Test uses acceleration voltage for the JSM-6360LV scanning electron microscope of 25kV.
Another object of the present invention is to provide ZnMn2O4/Mn2O3The electrochemical property test method of composite material, the party
Method are as follows:
Step 1: with the ZnMn of preparation2O4/Mn2O3As a positive electrode active material, acetylene black is as conductive agent, PTFE for material
As binder, it is uniformly mixed according to the ratio of mass ratio 8:1:1, anode electrode piece is made；
Step 2: using capacitor active carbon as negative electrode active material, acetylene black as conductive agent, PTFE as binder,
It is uniformly mixed also according to the ratio of mass ratio 8:1:1, negative electricity pole piece is made；
Step 3: to be saturated KNO3Solution is assembled into water system button cell as electrolyte；
Step 4: using the prepared button cell of LANHE battery test system measurement, electrochemical workstation measurement circulation
The AC impedance of volt-ampere curve and material before and after charge and discharge.
In conclusion advantages of the present invention and good effect are as follows:
In the prior art, single ZnMn2O4Material preparation is first stirred to react 8h for 80 DEG C, then washs sediment, is dry
It is dry to constant weight, as composite material precursor, presoma obtains final material in 900 DEG C of calcining 6h, but the calcining of the method
Temperature is higher, and energy consumption is larger.The present invention passed through hydro-thermal reaction before this and is prepared for presoma, then 500 DEG C of calcining 5h, being prepared for property
ZnMn that can be more excellent2O4/Mn2O3Composite material.
The present invention is regulated and controled using potassium hydroxide and sodium hydroxide as raw material using zinc acetate dihydrate and four water acetic acid manganese as raw material
Alkaline environment is successively prepared for ZnMn by hydrothermal synthesis and the method for high-temperature calcination2O4/Mn2O3Composite material, the material exist
Maximum specific discharge capacity under the conditions of 0.1A/g has reached 120.6F/g.The charge and discharge cycles under the current density of 0.2A/g
After 1000 times, ZnMn2O4/Mn2O3The specific discharge capacity of composite material is reduced to 91.1F/g from 109.5F/g, by 1000 times
Charge and discharge cycles after the capacity retention ratio of material be initial 83%；The charge and discharge cycles under the current density of 0.8A/g
After 500 times, ZnMn2O4/Mn2O3The specific discharge capacity of composite material is reduced to 75.7F/g from 94.1F/g, through 500 times fill
The capacity retention ratio of material is initial 80% after discharge cycles, can be with by the impedance curve of material before and after comparison charge and discharge
Find out that the impedance of the material does not change significantly, so even if the material can also be protected after multiple charge and discharge cycles
Good stability is held, by electro-chemical test it can be seen that the material has good high rate performance and cycle performance.
Detailed description of the invention
Fig. 1 is ZnMn provided in an embodiment of the present invention2O4/Mn2O3The preparation method flow chart of composite material；
Fig. 2 is ZnMn provided in an embodiment of the present invention2O4/Mn2O3The electrochemical property test method flow of composite material
Figure；
Fig. 3 is ZnMn provided in an embodiment of the present invention2O4/Mn2O3The XRD diagram of composite material；
Fig. 4 is ZnMn provided in an embodiment of the present invention2O4/Mn2O3The SEM of composite material schemes；
Fig. 5 is ZnMn provided in an embodiment of the present invention2O4/Mn2O3Cyclic voltammetric of the composite material under different scanning rates
Curve graph；
Fig. 6 is the specific capacity schematic diagram of CV curve under different scanning rates provided in an embodiment of the present invention；
Fig. 7 is ZnMn provided in an embodiment of the present invention2O4/Mn2O3Head of the composite material under different charging and discharging currents density
Secondary charging and discharging curve figure；
Fig. 8 is ZnMn provided in an embodiment of the present invention2O4/Mn2O3Electric discharge specific volume of the composite material under different current densities
Spirogram；
Fig. 9 is ZnMn provided in an embodiment of the present invention2O4/Mn2O3Charge and discharge of the composite material under different current densities follow
Ring figure；
Figure 10 (a) is ZnMn provided in an embodiment of the present invention2O4/Mn2O3Composite material recycles under 0.2A/g current density
1000 specific capacities and efficiency charts；
Figure 10 (b) is ZnMn provided in an embodiment of the present invention2O4/Mn2O3Composite material recycles under 0.8A/g current density
500 specific capacities and efficiency charts；
Figure 11 is ZnMn provided in an embodiment of the present invention2O4/Mn2O3AC impedance of the composite material before and after charge and discharge.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.
Application principle of the invention is described in detail with reference to the accompanying drawing.
As shown in Figure 1, ZnMn provided in an embodiment of the present invention2O4/Mn2O3Composite material the preparation method comprises the following steps:
S101: by KOH and NaOH deionized water dissolving, wiring solution-forming A；
S102: by the Zn (CH of 0.5mol/L3COO)2Solution pours into the Mn (CH of 1.0mol/L3COO)2It is made into solution molten
Liquid B；
S103: under agitation, solution B is added dropwise in solution A；
S104: after being added dropwise to complete, mixed solution being transferred in autoclave, is reacted for 24 hours under the conditions of 180 DEG C, from
Product is centrifugated after being so cooled to room temperature；
S105: the substance after centrifugation is placed in tube furnace, and 500 DEG C of calcining 5h, natural cooling are in air atmosphere
It can.
In step s101 by 3.00gKOH and 1.50gNaOH 20mL deionized water dissolving, wiring solution-forming A；
In step s 102 by the Zn (CH of 5mL0.5mol/L3COO)2Solution pours into the Mn of 5mL1.0mol/L
(CH3COO)2Wiring solution-forming B in solution；
ZnMn provided in an embodiment of the present invention2O4/Mn2O3The physical property of composite material is tested using XRD and SEM
Characterization, XRD test use Empyrean x-ray diffractometer, and pipe presses 40kV, the Cu target K α of Guan Liu 40mA, λ=0.15406nm
Ray；SEM test uses acceleration voltage for the JSM-6360LV scanning electron microscope of 25kV.
As shown in Fig. 2, ZnMn provided in an embodiment of the present invention2O4/Mn2O3The electrochemical property test method of composite material
Are as follows:
S201: with the ZnMn of preparation2O4/Mn2O3Material as a positive electrode active material, make as conductive agent, PTFE by acetylene black
For binder, it is uniformly mixed according to the ratio of mass ratio 8:1:1, anode electrode piece is made；
S202: using capacitor active carbon as negative electrode active material, acetylene black is as conductive agent, and PTFE is as binder, together
Sample is uniformly mixed according to the ratio of mass ratio 8:1:1, and negative electricity pole piece is made；
S203: to be saturated KNO3Solution is assembled into water system button cell as electrolyte；
S204: using the prepared button cell of LANHE battery test system measurement, electrochemical workstation measurement circulation volt
Pacify the AC impedance of curve and material before and after charge and discharge.
The invention will be further described combined with specific embodiments below.
XRD analysis
The material is ZnMn as can be seen from Figure 32O4/Mn2O3Composite material, 211 in XRD diagram, 222,321,332,
134, peak corresponding to 440,622 and standard card PDF#03-065-7467 match, and are Mn2O3Diffraction maximum；Other peaks
It is ZnMn2O4Diffraction maximum, match with standard card PDF#01-071-2499.The peak shape at each peak is sharp in figure, and without it
His miscellaneous peak, the structure of material are the Mn by cubic system2O3With the ZnMn of tetragonal crystal system2O4What interaction rearranged.
Sem analysis
As can be seen from Figure 4 prepared ZnMn2O4/Mn2O3Composite material is random small particles, and is had bright
Aobvious agglomeration.Presoma had been synthesized by hydro-thermal method before this in the preparation process of material, had been obtained further through high-temperature calcination
Final product.Due to there is hot stage during the preparation process, so material has agglomeration.
Electrochemical property test
Fig. 5 is ZnMn2O4/Mn2O3The CV curve that composite material measures under different scanning rates.Fig. 6 is different scanning
The specific capacity of CV curve under rate, can calculate in 1mV/s, 3mV/s, 5mV/s, 10mV/s, 30mV/ according to the following formula
S, the specific capacity under 50mV/s, 100mV/s sweep speed be respectively 121.5F/g, 82.6F/g, 72.9F/g, 63.2F/g,
51.9F/g、45.7F/g、39.8F/g。
Wherein C is specific capacity；Q is discharge electricity amount, i.e. the ratio between CV curve integral area half and sweep speed；M is activity
The quality of substance；Δ V is potential region.
Fig. 7 is ZnMn2O4/Mn2O3First charge-discharge curve graph of the composite material under different charging and discharging currents density；Fig. 8
It is ZnMn2O4/Mn2O3Specific discharge capacity figure of the composite material under different current densities.As can be seen from Figure 8, in 0.1A/
G, the specific discharge capacity under 0.2A/g, 0.4A/g, 0.8A/g, 1.0A/g, 2.0A/g, 4.0A/g current density is respectively
120.6F/g,108.7F/g,99.0F/g,94.2F/g,91.8F/g,85.0F/g,74.9F/g.The number that charge-discharge test measures
According to compared with the data that CV curve is calculated, it can be found that the size of specific capacity very close to.
Fig. 9 is ZnMn2O4/Mn2O3Charge and discharge cycles figure of the composite material under different current densities.It can from figure
Out with the increase of current density, the specific capacity of material is sequentially reduced.And specific capacity and Fig. 7, Fig. 8 survey under each multiplying power
The data obtained are consistent.As can be seen from the figure the material has good high rate performance.
Figure 10 is ZnMn2O4/Mn2O3The cycle performance figure of composite material.It can find out from Figure 10 (a) 0.2A/g's
Under current density after charge and discharge cycles 1000 times, ZnMn2O4/Mn2O3The specific discharge capacity of composite material is dropped from 109.5F/g
As low as 91.1F/g, the capacity retention ratio of material is initial 83% after 1000 charge and discharge cycles.It can be from Figure 10
(b) after finding out under the current density of 0.8A/g charge and discharge cycles 500 times in, ZnMn2O4/Mn2O3The electric discharge of composite material
Specific capacity is reduced to 75.7F/g from 94.1F/g, and the capacity retention ratio of material is initial after 500 charge and discharge cycles
80%.
Figure 11 is ZnMn2O4/Mn2O3AC impedance curve of the composite material before and after charge and discharge compares EIS figure medium-high frequency
The semicircle diameter in area and the straight slope of low frequency range, it can be seen that after it have passed through charge and discharge cycles, ZnMn2O4/
Mn2O3Although the impedance of composite material increased, but be consistent substantially or with the impedance before circulation.So this can also
To find out ZnMn2O4/Mn2O3Composite material has fine stability.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (6)
1. a kind of ZnMn2O4/Mn2O3The preparation method of composite material, which is characterized in that the ZnMn2O4/Mn2O3Composite material
The preparation method comprises the following steps:
Step 1: by 3.00gKOH and 1.50gNaOH 20mL deionized water dissolving, wiring solution-forming A；
Step 2: by the Zn (CH of 5mL0.5mol/L3COO)2Solution pours into the Mn (CH of 5mL1.0mol/L3COO)2It is made into solution
Solution B；
Step 3: under agitation, solution B is added dropwise in solution A；
Step 4: after being added dropwise to complete, mixed solution being transferred in autoclave, is reacted for 24 hours under the conditions of 180 DEG C, natural
Product is centrifugated after being cooled to room temperature；
Step 5: the substance after centrifugation is placed in tube furnace, in air atmosphere 500 DEG C of calcining 5h, natural cooling.
2. ZnMn as described in claim 12O4/Mn2O3The preparation method of composite material, which is characterized in that the ZnMn2O4/
Mn2O3The physical property of composite material carries out test characterization using XRD and SEM, and XRD test uses Empyrean X-ray diffraction
Instrument, pipe press 40kV, the Cu target K alpha ray of Guan Liu 40mA, λ=0.15406nm；SEM test uses acceleration voltage for the JSM- of 25kV
6360LV scanning electron microscope.
3. one kind ZnMn as described in claim 1~2 any one2O4/Mn2O3The preparation method preparation of composite material
ZnMn2O4/Mn2O3Composite material.
4. a kind of ZnMn as claimed in claim 32O4/Mn2O3The test method of the chemical property of composite material, feature exist
In the ZnMn2O4/Mn2O3The electrochemical property test method of composite material are as follows:
Step 1: with the ZnMn of preparation2O4/Mn2O3As a positive electrode active material, acetylene black is as conductive agent, PTFE conduct for material
Binder is uniformly mixed according to the ratio of mass ratio 8:1:1, anode electrode piece is made；
Step 2: using capacitor active carbon as negative electrode active material, acetylene black is as conductive agent, and PTFE is as binder, equally
It is uniformly mixed according to the ratio of mass ratio 8:1:1, negative electricity pole piece is made；
Step 3: to be saturated KNO3Solution is assembled into water system button cell as electrolyte；
Step 4: using the prepared button cell of LANHE battery test system measurement, electrochemical workstation measures cyclic voltammetric
The AC impedance of curve and material before and after charge and discharge.
5. one kind includes ZnMn described in claim 32O4/Mn2O3The lithium ion battery of composite material.
6. one kind includes ZnMn described in claim 32O4/Mn2O3The supercapacitor of composite material.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110190272A (en) * | 2019-07-09 | 2019-08-30 | 齐鲁工业大学 | A kind of preparation method of the nanocomposite for water system Zinc ion battery anode |
| CN110474017A (en) * | 2019-08-29 | 2019-11-19 | 瑞海泊有限公司 | The preparation method and applications of mangaic acid zinc electrode |
-
2018
- 2018-12-29 CN CN201811631105.1A patent/CN109817905A/en not_active Withdrawn
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110190272A (en) * | 2019-07-09 | 2019-08-30 | 齐鲁工业大学 | A kind of preparation method of the nanocomposite for water system Zinc ion battery anode |
| CN110474017A (en) * | 2019-08-29 | 2019-11-19 | 瑞海泊有限公司 | The preparation method and applications of mangaic acid zinc electrode |
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Application publication date: 20190528 |