CN109809485A - A kind of height ratio capacity hydration vanadic acid magnesium and the preparation method and application thereof - Google Patents
A kind of height ratio capacity hydration vanadic acid magnesium and the preparation method and application thereof Download PDFInfo
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- CN109809485A CN109809485A CN201910080523.4A CN201910080523A CN109809485A CN 109809485 A CN109809485 A CN 109809485A CN 201910080523 A CN201910080523 A CN 201910080523A CN 109809485 A CN109809485 A CN 109809485A
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Abstract
The invention discloses a kind of height ratio capacity hydration vanadic acid magnesium and the preparation method and application thereof, by vanadic anhydride and magnesium nitrate dispersion and it is dissolved in deionized water, in 160~180 DEG C of hydro-thermal reactions 12~for 24 hours after being dispersed with stirring uniformly, it staticly settles, precipitating be washed with deionized after 80 DEG C of dry 12h to get.Obtained hydration vanadic acid magnesium structural formula is MgxV2O5·nH2O, wherein x is that 0.17~0.2, n is 1.26~1.38.The hydration vanadic acid magnesium, Super P conductive black and the Kynoar that are prepared are prepared by mixing into slurry, it is then coated in anode is made on titanium foil, Zinc ion battery is formed with zinc metal sheet cathode, fibreglass diaphragm and aqueous electrolyte containing zinc ion, the highest specific discharge capacity under 100mA/g current density is up to 410.8mAh/g.
Description
Technical field
The present invention relates to battery material technical fields, and in particular to a kind of MgxV2O5·nH2The preparation method and application of O.
Background technique
As environmental pollution and fossil resource exhaustion are got worse, the cleaning such as exploitation solar energy, wind energy, tide energy is renewable
The energy is very urgent.However, these new energy have the characteristics that intermittent, mating energy storage device is needed.In numerous energy
It stores in equipment, lithium ion battery occupies leading position, has been widely used in mobile electronic device and electric car field.
Regrettably, lithium ion battery is faced with three major issues: (1) reserves of lithium minerals at the earth's surface are low, lead to lithium cost of material
It is expensive；(2) organic solvent in lithium-ion battery electrolytes is at high price, and inflammable and explosive, Frequent Accidents；(3) lithium-ion electric
The assembling in pond needs to carry out in the conditionity of anhydrous and oxygen-free, further increases cost.Problem above pacifies lithium ion battery
Full property is low, at high cost, is not particularly suited for large-scale energy storage device in fact.For example, in July, 2018 South Korea's Lingyan Crag wind-force is sent out
Lithium ion battery explosion accident occurs for power plant, causes fire disaster, has burnt more than 700m3The battery of scale is built and is more than
3500 pieces of lithium ion batteries, suffer heavy losses.Thus, it is necessary to develop water system battery.Using water as electrolyte solvent, not only
Cost can be greatly reduced, additionally it is possible to significantly improve safety.Wherein, water system Zinc ion battery has uniqueness because of following advantages
Advantage: (1) zinc mineral rich reserves, it is cheap；(2) redox potential of zinc metal is suitable (- 0.76V vs.SHE),
And liberation of hydrogen overpotential is high, is just used as the cathode of water system battery；(3) zinc theoretical metal capacity height (820mAh/g, 5851mAh/
cm3), and chemical stability can be kept in water and air.Therefore, water system Zinc ion battery is expected in massive energy memory
It yields unusually brilliant results in the fields such as part, smart grid, electric car.
Currently, the key technology of Zinc ion battery is storage zinc positive electrode.On the one hand, suitable storage zinc current potential is needed,
Guarantee is not only able to achieve high voltage, but also is not influenced by water decomposition.On the other hand, although the diameter of zinc ionLower than lithium
IonThe dynamics that the bigger quality of zinc ion and higher valence state cause it to be subjected to when transmitting in electrode material
It hinders more serious than lithium ion.Therefore, alternative high-performance storage zinc positive electrode and few.Prussian blue similar object is more early
Ground has been investigated as storage zinc positive electrode, but specific capacity is too low, does not have practicability.Mn oxide is used for by a large amount of reports
Zinc positive electrode is stored up, but cyclical stability and high rate performance are all not ideal enough.Nearly 2 years, vanadium-based materials with its height ratio capacity with
And excellent high rate performance and cyclical stability and be increasingly interested by researchers.It is generally believed that the storage zinc of vanadium-based materials
Mechanism is the reversible insertion and abjection of zinc ion.For MxV2O5·nH2O (M Li+、Na+、K+、Ca2+、Mg2+Deng) it is this kind of sun from
The radius of the pre- intercalated layered barium oxide of son, hydration M ion directly affects the interlamellar spacing of material.Before other parameters are identical
It puts, interlamellar spacing is bigger, and zinc ion is easier in MxV2O5·nH2The migration of O interlayer and storage.In view of Mg2+Hydrated ion half
DiameterIt is larger, MgxV2O5·nH2O is expected to become high performance storage zinc positive electrode.
In fact, for MgxV2O5·nH2The research of O, worldwide all seldom.Chinese patent CN106784738A
One kind is disclosed using polymethylacrylic acid as template and carbon source, magnesium is prepared by sol-gal process and adulterates vanadic anhydride
(MgxV2O5The method of)/carbon porous microsphere composite material, for the positive electrode of lithium ion battery, specific capacity is up to
250mAh/g.Chinese patent CN107170967A discloses one kind using vanadic anhydride, hydrogen peroxide and magnesium chloride as raw material, passes through
Hydro-thermal method prepares MgxV2O5·nH2The method of O；Material liquid needs long agitation that pre-reaction occurs, and can put with violent
Thermal response is easy to cause material liquid to splash cruelly so that hydrogen peroxide acutely decomposes；The hydrothermal temperature of this method is higher by (180~200
DEG C), the hydro-thermal time is longer (2~6 days), and product drying has used freeze-drying, these are all unfavorable to industrialized production；
In addition, gained MgxV2O5·nH2Positive electrode capacity of the O for water system Zinc ion battery is relatively low, in 100mA/g current density
Under highest specific capacity less than 230mAh/g.United States Patent (USP) US20180205068A1 discloses one kind to synthesize MgV2O6For original
Material prepares Mg using collosol and gel ion exchange0.1V2O5Method, the positive electrode for Magnesium ion battery under C/10 most
Big specific capacity about 300mAh/g.
Summary of the invention
Goal of the invention: in order to solve existing MgxV2O5·nH2O preparation condition is harsh, complex process and specific capacity are low etc. asks
Topic, a kind of method that the present invention provides simplicity prepare the Mg of height ratio capacityxV2O5·nH2O electrode material.
In order to solve the above-mentioned technical problem, the technical solution adopted by the present invention is as follows:
A kind of hydration vanadic acid magnesium, its structural formula are MgxV2O5·nH2O, wherein x be 0.17~0.2, n be 1.26~
1.38。
The preparation method of above-mentioned hydration vanadic acid magnesium, includes the following steps:
(1) vanadic anhydride and magnesium nitrate are dispersed and are dissolved in deionized water, be dispersed with stirring uniformly；
(2) dispersion liquid for obtaining step (1) is staticly settled in 160~180 DEG C of hydro-thermal reactions 12~for 24 hours；
(3) after the precipitating that step (2) obtains being washed with deionized 80 DEG C of dry 12h to get.
Wherein, the molar ratio of the vanadic anhydride and magnesium nitrate is 1:1~3, the vanadic anhydride and deionized water
Ratio be 1mmoL:60mL.
The above-mentioned hydration vanadic acid magnesium being prepared is also claimed in Zinc ion battery as positive electrode in the present invention
Using.
In the application, Zinc ion battery includes anode, cathode, fibreglass diaphragm and the water system containing zinc ion
Electrolyte composition；Anode hydration vanadic acid magnesium, Super P conductive black as described in claim 1 and Kynoar mixing
It is prepared into slurry, is then coated in being made on titanium foil；Highest electric discharge specific volume of the Zinc ion battery under 100mA/g current density
It measures up to 410.8mAh/g.
Wherein, the hydration vanadic acid magnesium, Super P conductive black and Kynoar are mixed according to mass ratio 70:20:10
It closes, is then dispersed using N-Methyl pyrrolidone, be mixed into after slurry and N-Methyl pyrrolidone is evaporated by baking oven.
The utility model has the advantages that
The present invention is using easy one step hydro thermal method, and only with vanadic anhydride and magnesium nitrate as raw material, and hydro-thermal is anti-
Without pretreatment or pre-reaction before answering, process flow is simple, and condition is relatively mild, time-consuming relatively short；Gained MgxV2O5·
nH2It is reachable that O is used for highest specific discharge capacity of the positive electrode of water system Zinc ion battery under 100mA/g current density
410.8mAh/g。
Detailed description of the invention
The present invention is done with reference to the accompanying drawings and detailed description and is further illustrated, of the invention is above-mentioned
And/or otherwise advantage will become apparent.
Fig. 1 is 1 gained Mg of the embodiment of the present invention0.20V2O5·1.38H2The XRD spectrum of O；
Fig. 2 is 1 gained Mg of the embodiment of the present invention0.20V2O5·1.38H2The TGA curve of O；
Fig. 3 is 1 gained Mg of the embodiment of the present invention0.20V2O5·1.38H2The SEM of O schemes；
Fig. 4 is 1 gained Mg of the embodiment of the present invention0.20V2O5·1.38H2The storage zinc high rate performance of O；
Fig. 5 is 2 gained Mg of the embodiment of the present invention0.17V2O5·1.26H2The XRD spectrum of O；
Fig. 6 is 2 gained Mg of the embodiment of the present invention0.17V2O5·1.26H2The TGA curve of O；
Fig. 7 is 2 gained Mg of the embodiment of the present invention0.17V2O5·1.26H2The SEM of O schemes；
Fig. 8 is 2 gained Mg of the embodiment of the present invention0.17V2O5·1.26H2The storage zinc high rate performance of O.
Specific embodiment
According to following embodiments, the present invention may be better understood.
Embodiment 1
(1) 1/3mmoL vanadic anhydride and 1mmoL magnesium nitrate are dispersed and are dissolved in 20mL deionized water, stirring is equal
After even for 24 hours in 160 DEG C of hydro-thermal reactions；
(2) it is obtained in air dry oven in 80 DEG C of dry 12h after precipitating obtained by step (1) being washed with deionized
MgxV2O5·nH2O。
The assembling and test of Zinc ion battery: the resulting Mg of the present embodiment is takenxV2O5·nH2O and Super P conductive black,
Kynoar (PVDF) is mixed by the mass ratio of 70:20:10, with N-Methyl pyrrolidone (NMP) for dispersing agent, is stirred evenly
It is configured to slurry；Then slurry is coated on titanium foil, is struck off, is placed in 80 DEG C of baking ovens and is evaporated NMP；It is compacted at 10MPa, so
Above-mentioned titanium foil is cut into slicer the circular electric pole piece of diameter 12mm afterwards；Using above-mentioned electrode slice, metal zinc metal sheet, Whatman
Glass fibre membrane (GF/A) and 3M trifluoromethayl sulfonic acid zinc (Zn (CF3SO3)2) aqueous solution as working electrode (anode), to electricity
Pole, diaphragm and electrolyte are assembled into 2016 type button batteries in air.The constant current charge-discharge test of battery uses LAND
CT2001A tester, blanking voltage 0.2-1.6V.
Mg manufactured in the present embodimentxV2O5·nH2The XRD spectrum of O as shown in Figure 1, be similar to CN107170967A and
Testing result in US20180205068A1 shows significant (001) diffraction maximum, corresponds to layer structure.According to Prague
Equation is it is found that its interlamellar spacing is up to
According to ICP-OES result it is found that Mg manufactured in the present embodimentxV2O5·nH2X=0.20 in O；It is tested further accordance with TGA
As a result (Fig. 2) can derive Mg0.20V2O5·nH2N=1.38 in O.Therefore, the molecular formula of gained hydration vanadic acid magnesium is
Mg0.20V2O5·1.38H2O。
Mg manufactured in the present embodiment0.20V2O5·1.38H2The SEM of O schemes as shown in figure 3, primary structure pattern is nanobelt,
Secondary structure pattern is micron-sized random particle.
Mg manufactured in the present embodiment0.20V2O5·1.38H2The storage zinc high rate performance of O is as shown in figure 4, in 100mA/g electric current
Highest specific discharge capacity under density is up to 410.8mAh/g.When current density is successively increased to 200,500,1000,2000 and
When 5000mA/g, the specific discharge capacity recycled for the last time under each multiplying power is respectively 355.6,275.9,154.2,21.7 and
8.3mAh/g。
Embodiment 2
(1) 1/3mmoL vanadic anhydride and 1/3mmoL magnesium nitrate are dispersed and are dissolved in 20mL deionized water, stirred
In 180 DEG C of hydro-thermal reaction 12h after uniformly；
(2) it is obtained in air dry oven in 80 DEG C of dry 12h after precipitating obtained by step (1) being washed with deionized
MgxV2O5·nH2O。
The assembling and test of Zinc ion battery are referring to embodiment 1.
Mg manufactured in the present embodimentxV2O5·nH2The XRD spectrum of O as shown in figure 5, be similar to CN107170967A and
Testing result in US20180205068A1 shows significant (001) diffraction maximum, corresponds to layer structure.According to Prague
Equation is it is found that its interlamellar spacing is up to
According to ICP-OES result it is found that Mg manufactured in the present embodimentxV2O5·nH2X=0.17 in O；It is tested further accordance with TGA
As a result (Fig. 6) can derive Mg0.17V2O5·nH2N=1.26 in O.Therefore, the molecular formula of gained hydration vanadic acid magnesium is
Mg0.17V2O5·1.26H2O。
Mg manufactured in the present embodiment0.17V2O5·1.26H2The SEM of O schemes as shown in fig. 7, primary structure pattern is nanobelt,
Secondary structure pattern is micron-sized random particle.
Mg manufactured in the present embodiment0.17V2O5·1.26H2The storage zinc high rate performance of O is as shown in figure 8, in 100mA/g electric current
Highest specific discharge capacity under density is up to 375.4mAh/g.When current density is successively increased to 200,500,1000,2000 and
When 5000mA/g, the specific discharge capacity recycled for the last time under each multiplying power is respectively 308.9,193.9,53.3,3.3 and
8.3mAh/g。
The present invention provides the thinkings and method of a kind of height ratio capacity hydration vanadic acid magnesium and the preparation method and application thereof, specifically
Realize that there are many method and the approach of the technical solution, the above is only a preferred embodiment of the present invention, it is noted that for
For those skilled in the art, without departing from the principle of the present invention, can also make it is several improvement and
Retouching, these modifications and embellishments should also be considered as the scope of protection of the present invention.Each component part being not known in the present embodiment
It is realized with the prior art.
Claims (6)
1. a kind of hydration vanadic acid magnesium, which is characterized in that its structural formula is MgxV2O5·nH2O, wherein x is that 0.17~0.2, n is
1.26~1.38.
2. being hydrated the preparation method of vanadic acid magnesium described in claim 1, which comprises the steps of:
(1) vanadic anhydride and magnesium nitrate are dispersed and are dissolved in deionized water, be dispersed with stirring uniformly；
(2) dispersion liquid for obtaining step (1) is staticly settled in 160~180 DEG C of hydro-thermal reactions 12~for 24 hours；
(3) after the precipitating that step (2) obtains being washed with deionized 80 DEG C of dry 12h to get.
3. the preparation method of hydration vanadic acid magnesium according to claim 2, which is characterized in that in step (1), five oxidation
The molar ratio of two vanadium and magnesium nitrate is 1:1~3, and the ratio of the vanadic anhydride and deionized water is 1mmoL:60mL.
4. hydration vanadic acid magnesium is in Zinc ion battery as the application of positive electrode described in claim 1.
5. application according to claim 4, the Zinc ion battery includes anode, cathode, fibreglass diaphragm and contains
The aqueous electrolyte of zinc ion forms；The anode is hydrated vanadic acid magnesium, Super P conductive black and is gathered as described in claim 1
Vinylidene is prepared by mixing into slurry, is then coated in being made on titanium foil；The Zinc ion battery is under 100mA/g current density
Highest specific discharge capacity is up to 410.8mAh/g.
6. application according to claim 5, the hydration vanadic acid magnesium, Super P conductive black and Kynoar according to
Mass ratio 70:20:10 mixing, is then dispersed using N-Methyl pyrrolidone.
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Cited By (10)
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|---|---|---|---|---|
| CN111082003A (en) * | 2019-12-05 | 2020-04-28 | 华南理工大学 | Vanadate hydrate electrode material and preparation method and application thereof |
| CN111244422A (en) * | 2020-01-19 | 2020-06-05 | 山东大学 | Organic ion doped vanadium oxide positive electrode material for water-based zinc ion battery and preparation method and application thereof |
| CN111573731A (en) * | 2020-04-26 | 2020-08-25 | 上海大学 | Vanadium-based positive electrode material of water-based zinc ion battery and preparation method and application thereof |
| CN112670502A (en) * | 2021-01-28 | 2021-04-16 | 河南工业大学 | Antimony telluride nanosheet and application thereof in water-based zinc ion battery |
| CN113764661A (en) * | 2020-06-01 | 2021-12-07 | 南京航空航天大学 | Transition metal vanadate zinc ion battery positive electrode material and preparation method thereof |
| CN114497888A (en) * | 2022-01-25 | 2022-05-13 | 郑州大学 | Preparation method and application of lithium-sulfur battery diaphragm modification material |
| CN114566628A (en) * | 2022-03-04 | 2022-05-31 | 合肥工业大学 | Preparation method of anode material of phytic acid doped polypyrrole @ vanadate water-based zinc ion battery |
| CN114956172A (en) * | 2022-05-20 | 2022-08-30 | 广西大学 | Magnesium vanadate adsorbent targeting strontium ions and cesium ions as well as preparation method and application thereof |
| CN115472815A (en) * | 2022-09-23 | 2022-12-13 | 天津大学 | Vanadium-based cathode material and preparation method and application thereof |
| CN116282155A (en) * | 2023-04-13 | 2023-06-23 | 重庆大学 | Magnesium vanadium oxide positive electrode material and preparation method and application thereof |
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| CN111082003A (en) * | 2019-12-05 | 2020-04-28 | 华南理工大学 | Vanadate hydrate electrode material and preparation method and application thereof |
| CN111244422A (en) * | 2020-01-19 | 2020-06-05 | 山东大学 | Organic ion doped vanadium oxide positive electrode material for water-based zinc ion battery and preparation method and application thereof |
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| CN111573731A (en) * | 2020-04-26 | 2020-08-25 | 上海大学 | Vanadium-based positive electrode material of water-based zinc ion battery and preparation method and application thereof |
| CN113764661A (en) * | 2020-06-01 | 2021-12-07 | 南京航空航天大学 | Transition metal vanadate zinc ion battery positive electrode material and preparation method thereof |
| CN112670502A (en) * | 2021-01-28 | 2021-04-16 | 河南工业大学 | Antimony telluride nanosheet and application thereof in water-based zinc ion battery |
| CN114497888A (en) * | 2022-01-25 | 2022-05-13 | 郑州大学 | Preparation method and application of lithium-sulfur battery diaphragm modification material |
| CN114497888B (en) * | 2022-01-25 | 2024-04-05 | 郑州大学 | Preparation method and application of lithium-sulfur battery diaphragm modification material |
| CN114566628A (en) * | 2022-03-04 | 2022-05-31 | 合肥工业大学 | Preparation method of anode material of phytic acid doped polypyrrole @ vanadate water-based zinc ion battery |
| CN114566628B (en) * | 2022-03-04 | 2023-02-24 | 合肥工业大学 | Preparation method of phytic acid doped polypyrrole @ vanadate aqueous zinc ion battery positive electrode material |
| CN114956172A (en) * | 2022-05-20 | 2022-08-30 | 广西大学 | Magnesium vanadate adsorbent targeting strontium ions and cesium ions as well as preparation method and application thereof |
| CN114956172B (en) * | 2022-05-20 | 2023-09-15 | 广西大学 | Magnesium vanadate adsorbent for targeting strontium ions and cesium ions, and preparation method and application thereof |
| CN115472815A (en) * | 2022-09-23 | 2022-12-13 | 天津大学 | Vanadium-based cathode material and preparation method and application thereof |
| CN115472815B (en) * | 2022-09-23 | 2024-04-26 | 天津大学 | Vanadium-based positive electrode material and preparation method and application thereof |
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