CN108539190A - The molybdenum trioxide of a kind of oxygen-containing vacancy and using it as the water system aluminium ion battery of negative electrode active material and their preparation method - Google Patents
The molybdenum trioxide of a kind of oxygen-containing vacancy and using it as the water system aluminium ion battery of negative electrode active material and their preparation method Download PDFInfo
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- CN108539190A CN108539190A CN201810286605.XA CN201810286605A CN108539190A CN 108539190 A CN108539190 A CN 108539190A CN 201810286605 A CN201810286605 A CN 201810286605A CN 108539190 A CN108539190 A CN 108539190A
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- molybdenum trioxide
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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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
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- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The invention discloses a kind of molybdenum trioxide of oxygen-containing vacancy and using it as the water system aluminium ion battery of negative electrode active material and their preparation method.The molybdenum trioxide of oxygen-containing vacancy（MoO3‑x）Preparation method be：Using molybdenum trioxide as presoma, using small molecule alcohols such as ethyl alcohol, ethylene glycol or methanol as reducing agent, hydro-thermal reaction is carried out, obtains MoO3‑x.With MoO3‑xFor negative electrode active material, it is positive electrode active materials that graphene, activated carbon or carbon nanotube etc., which have the carbon material of bigger serface, fibreglass diaphragm, polyethylene or polypropylene fibre diaphragm etc. make diaphragm, electrolyte is done containing aluminum ions aqueous solution, the molybdenum trioxide that can be prepared into oxygen-containing vacancy is the water system aluminium ion battery of negative material.Compared to the molybdenum trioxide of complete oxidation, the molybdenum trioxide of oxygen-containing vacancy has the interlamellar spacing of bigger, is conducive to aluminum ions diffusion, therefore have higher capacity as aluminium ion cell negative electrode material, and prepare it is simple, of low cost, conducive to commercially producing and applying on a large scale.
Description
Technical field
The present invention relates to a kind of water system aluminium ion field of batteries, more particularly to the molybdenum trioxide of a kind of oxygen-containing vacancy and with it
For the water system aluminium ion battery and their preparation method of negative electrode active material.
Background technology
Fossil fuel exploitation becomes the focus of global concern using the resource exhaustion and air pollution that bring, to green energy resource
The development of storage system proposes urgent requirement.The energy storage device that lithium ion battery is born as the early 1990s has energy
Metric density is high, the advantages of having extended cycle life.However, lithium resource reserves are limited and in distribution on global unevenness, organic electrolyte is inflammable
Security risk is formed, these problems all force people to find more cheap, safety novel energy-storing equipment, to meet electronic vapour
The demand of the large size energy storage such as vehicle, intelligent grid.
Compared to organic electrolyte, non-flammable aqueous electrolyte has higher safety coefficient, ionic conductivity ratio
Organic electrolyte is higher by two orders of magnitude, and cheap.
Relative to lithium, bauxite resource is abundant, is the highest metallic element of content in the earth's crust.Aluminium ion radius is small, in charge and discharge
Three electron transfer reactions can occur in the process, theoretical specific capacity is up to 2980 mAhg-1.Therefore, water system aluminium ion battery has good
Good application potential.Gonzalez etc. reports vanadic anhydride in 1mol L-1 AlCl3Electrolyte, 200 mA g-1When, electric discharge
Specific capacity is 20 mAh g-1, have apparent aluminium ion embedded and abjection platform (Gonz á lez JR, Nacimiento F,
Cabello M, Alcántara R, et al. Reversible intercalation of aluminium into
vanadium pentoxide xerogel for aqueous rechargeable batteries[J]. Rsc
Advances. 2016)；Liu et al. reports iron copper cyanider in 0.5 mol L-1Al 2(SO 4)3Electrolyte, 400mA g-1Under, just
Beginning specific capacity is 46.9 mAh g-1, after recycling 1000 times, specific capacity is reduced to 22.5 mAh g-1(Liu S, Pan GL, et
al. Copper hexacyanoferrate nanoparticles as cathode material for aqueous Al-
ion batteries[J]. Journal of Materials Chemistry A. 2015)；Wang etc. reports polypyrrole packet
Molybdenum trioxide nano pipe is covered in 0.5 mol L-1Al 2(SO 4)3Electrolyte, 2 A g-1Under, MoO3@Ppy//AC initial specific capacities
For 31.2 mAh g-1, after recycling 1800 times, specific capacity conservation rate is 93%（Wang F, Liu Z, Wang X, et al. A
conductive polymer coated MoO3anode enables an Al-ion capacitor with high
performance[J]. J Mater Chem A. 2016）.These materials can reversible storage aluminium ion, but capacity and follow
Ring performance needs to be further improved, and there has been no the molybdenum trioxides of patent and document report oxygen-containing vacancy as water so far
It is aluminium ion battery cathode.
Invention content
In order to overcome the disadvantages mentioned above and deficiency of the prior art, the purpose of the present invention is to provide the three of a kind of oxygen-containing vacancy
Molybdenum oxide and using it as the water system aluminium ion battery of negative electrode active material and their preparation method.Three oxygen of this oxygen-containing vacancy
Changing molybdenum has the advantages that prepare water system aluminium ion battery appearance simple, of low cost, being assembled as negative electrode active material using the material
Amount is high, cycle performance is good.
The purpose of the present invention can be realized by following technical solution：
A kind of preparation method of the molybdenum trioxide of oxygen-containing vacancy, specifically includes following steps, molybdenum trioxide is distributed in water, add
Enter reducing agent, mixture is put into high-temperature high-pressure reaction kettle after being uniformly dispersed, after hydro-thermal reaction, obtains three oxidations of oxygen-containing vacancy
Molybdenum, that is, MoO3-x, ranging from the 0 ~ 1 of x.
Further, the reducing agent is at least one of small molecule alcohols such as ethyl alcohol, ethylene glycol or methanol.
Further, the hydrothermal temperature is 80 ~ 150 DEG C, and the time is 1 ~ 12h.
The molybdenum trioxide of oxygen-containing vacancy can be made by above-described preparation method.
It is a kind of using the molybdenum trioxide of oxygen-containing vacancy as the water system aluminium ion battery of negative electrode active material, cathode, anode, diaphragm
And electrolyte, which is characterized in that the cathode includes：Negative electrode active material, collector, binder and conductive agent, wherein afflux
Body is the coating matrix of negative electrode active material, binder, conductive agent composition；The anode includes：Positive electrode active materials, afflux
Body, binder and conductive agent, wherein collector is the coating matrix of positive electrode active materials, binder, conductive agent composition；Every
Film is glass fibre, polyethylene or polypropylene fibre diaphragm etc.；Electrolyte is aqueous electrolyte containing aluminium ion；The negative electrode active
Material is the molybdenum trioxide of oxygen-containing vacancy.
Further, the negative electrode active material is the molybdenum trioxide of oxygen-containing vacancy；Positive electrode active materials are graphene, work
Property charcoal or carbon nanotube etc. there is one or more of carbon material mixing of bigger serface；Collector is steady in the electrolytic solution
One kind in fixed carbon paper, stainless steel, titanium sheet, tantalum piece etc.；Binder is polytetrafluoroethylene (PTFE), Kynoar, carboxymethyl cellulose
At least one of plain sodium or butadiene-styrene rubber；Conductive agent is at least one in acetylene black, Super-P, Ketjen black or graphene
Kind.
Further, the aqueous electrolyte containing aluminium ion by aluminium chloride, aluminum sulfate, aluminum nitrate, aluminium acetate etc. it is a kind of or
Two or more solution compositions.
The method for preparing above-mentioned water system aluminium ion battery, includes the following steps：
1）MoO3-x, conductive agent and binder are mixed, are coated uniformly on collector after slurry is made, then at 60 ~ 120 DEG C
It is dried in vacuum drying chamber, cathode pole piece is made；
2）With reference to step 1）Anode pole piece is made in positive electrode by the process；
3）By step 1）With 2）Obtained cathode pole piece, anode pole piece and diaphragm is assembled, and the electrolysis of water system containing aluminium ion is added
Liquid obtains soft-package battery or button cell to get the water system aluminium to a kind of molybdenum trioxide of oxygen-containing vacancy for negative electrode active material
Ion battery.
Compared with prior art, the invention has the advantages that and technique effect：The present invention provides a kind of oxygen-containing vacancies
Molybdenum trioxide and preparation method thereof and the application in water system aluminium ion battery.Relative to organic electrolyte, aqueous electrolyte
Ionic conductivity is high, safe and non-toxic, cheap.Since aluminium is more abundanter than lithium resource, aluminium ion battery is relative to lithium
Ion battery has more advantage in price.Relative to the molybdenum trioxide of complete oxidation, (020) of the molybdenum trioxide of oxygen-containing vacancy is brilliant
Face interlamellar spacing becomes larger, and is conducive to aluminum ions diffusion, therefore have higher capacity as aluminium ion cell negative electrode material.And it should
Material preparation is simple, of low cost, conducive to commercially producing and applying on a large scale.Electrode material preparation method in the present invention
Simply, capacity is high, electrolyte Environmental Safety, cheap, the water system aluminium ion battery that assembling gained provides have high power capacity and
The characteristics of good cycle, can be used for the multiple fields such as large-scale energy-accumulating power station.
Description of the drawings
Fig. 1 is MoO prepared by present example 13-xWith MoO3XRD diagram.
Fig. 2 is that water system aluminium ion battery prepared by present example 1 in current density is 5A g-1When cycle charge-discharge it is bent
Line chart.
Specific implementation method
The present invention will be described in more detail by the following specific embodiments.
【Embodiment 1】
By 8mL H2O2（30wt %）It is added dropwise in 0.96g molybdenum powders, waits for that molybdenum powder is completely dissolved, deionized water is added to be diluted to 70
ML, is then transferred to 100 mL reaction kettles, and 180oC reacts 24 h, is filtered, washed and dries, obtains molybdenum trioxide.By 300
Ethanol water is added in mg molybdenum trioxides（15 mL water, 15 mL absolute ethyl alcohols）In, it is evenly dispersed, 50 mL reaction kettles are transferred to,
110oC reacts 6h, is filtered, washed and dries, obtain the molybdenum trioxide of oxygen-containing vacancy, Fig. 1 show MoO3- x and MoO3XRD
Figure, as seen from the figure,（020）The corresponding diffraction maximum left avertence of crystal face, calculates according to Bragg equation, and lattice constant b is from MoO3's
13.80 increasing to MoO3The 13.86 of-x, explanation（020）The interlamellar spacing of crystal face increases, that is, proves the presence of Lacking oxygen.It should
Material and conductive agent acetylene black, binder polyvinylidene fluoride（PVDF）According to mass ratio 8:1.5:0.5 mixing, instills N- methyl
Pyrrolidones（NMP）Uniform sizing material is stirred into, is coated on carbon paper, 80 in vacuum drying chamberoC is dried to get cathode pole piece.It will
Graphene is fabricated to anode pole piece with identical method.The cathode pole piece, anode pole piece and fibreglass diaphragm that prepare are set
In Soft Roll, AlCl is added3Aqueous solution（1mol L-1）Make electrolyte, encapsulates up to water system aluminium ion soft-package battery.By the battery
Constant current charge-discharge test is carried out, charging and discharging curve is as shown in Fig. 2, as seen from the figure, when current density is 1A g-1When, cycle the 50th
Secondary and 300 times specific capacities are up to 36.5 mAh g-1（It is calculated by positive and negative pole material gross mass）.
【Embodiment 2】
By 8mL H2O2（30wt %）It is added dropwise in 0.96g molybdenum powders, waits for that molybdenum powder is completely dissolved, deionized water is added to be diluted to 70
ML, is then transferred to 100 mL reaction kettles, and 180oC reacts 24 h, is filtered, washed and dries, obtains molybdenum trioxide.By 300
Glycol water is added in mg molybdenum trioxides（20 mL water, 10 mL ethylene glycol）In, it is evenly dispersed, 50 mL reaction kettles are transferred to,
120 oC reacts 6 h, is filtered, washed and dries, obtains the molybdenum trioxide of oxygen-containing vacancy.By the material and conductive agent Super P,
Binder polyvinylidene fluoride（PVDF）According to mass ratio 8:1.5:0.5 mixing, instills N-Methyl pyrrolidone（NMP）It stirs into
Uniform sizing material is coated on carbon paper, 80 in vacuum drying chamberoC is dried to get cathode pole piece.By the identical method of activated carbon
It is fabricated to anode pole piece.The cathode pole piece, anode pole piece and polypropylene fibre diaphragm that prepare are placed in Soft Roll, Al is added2
(SO4)3Aqueous solution（0.5mol L-1）Make electrolyte, encapsulates up to water system aluminium ion soft-package battery.
【Embodiment 3】
Methanol aqueous solution is added in 300 mg molybdenum trioxides（20 mL water, 10 mL methanol）In, it is evenly dispersed, it is transferred to 50 mL
Reaction kettle, 100oC reacts 6 h, is filtered, washed and dries, obtains the molybdenum trioxide of oxygen-containing vacancy.By the material and conductive agent
Ketjen black, polyfluortetraethylene of binding element lotion（PTFE）According to mass ratio 8:1:1 mixing, instillation deionized water, which stirs into, to be homogenized
Material is coated on carbon paper, and 80 DEG C of drying are to get cathode pole piece in vacuum drying chamber.The identical method of carbon nanotube is made
At anode pole piece.The cathode pole piece, anode pole piece and polyethylene diagrams that prepare are placed in Soft Roll, Al (NO are added3)3It is water-soluble
Liquid（1 mol L-1）Make electrolyte, encapsulates up to water system aluminium ion soft-package battery.
It should be appreciated that the technical concepts and features of above-described embodiment only to illustrate the invention, be not intended to limit the invention,
In the case of all conception and scopes described in the appended claims of the present invention and its equivalent, various repair can be made to it
Change and replaces.
Claims (8)
1. a kind of preparation method of the molybdenum trioxide of oxygen-containing vacancy, which is characterized in that molybdenum trioxide is distributed in water, is added also
Mixture is put into high-temperature high-pressure reaction kettle by former agent after being uniformly dispersed, and after hydro-thermal reaction, obtains the molybdenum trioxide of oxygen-containing vacancy i.e.
MoO3-x, ranging from the 0 ~ 1 of x.
2. a kind of preparation method of the molybdenum trioxide of oxygen-containing vacancy as described in claim 1, which is characterized in that the reduction
Agent is at least one of small molecule alcohols such as ethyl alcohol, ethylene glycol or methanol.
3. a kind of preparation method of the molybdenum trioxide of oxygen-containing vacancy as described in claim 1, which is characterized in that the hydro-thermal is anti-
It is 80 ~ 150 DEG C to answer temperature, and the time is 1 ~ 12h.
4. the molybdenum trioxide of oxygen-containing vacancy made from claim 1--3 any one of them preparation methods.
5. a kind of using the molybdenum trioxide of oxygen-containing vacancy as the water system aluminium ion battery of negative electrode active material, including cathode, anode, every
Film and electrolyte, which is characterized in that the cathode includes：Negative electrode active material, collector, binder and conductive agent, wherein collection
Fluid is the coating matrix of negative electrode active material, binder, conductive agent composition；The anode includes：Positive electrode active materials, collection
Fluid, binder and conductive agent, wherein collector is the coating matrix of positive electrode active materials, binder, conductive agent composition；
Diaphragm is glass fibre, polyethylene or polypropylene fibre diaphragm etc.；Electrolyte is aqueous electrolyte containing aluminium ion；The cathode is lived
Property material be oxygen-containing vacancy molybdenum trioxide.
6. as claimed in claim 5 a kind of using the molybdenum trioxide of oxygen-containing vacancy as the water system aluminium ion electricity of negative electrode active material
Pond, which is characterized in that positive electrode active materials are in the carbon material with bigger serface such as graphene, activated carbon or carbon nanotube
One or more of mixing；Collector is one kind in stable in the electrolytic solution carbon paper, stainless steel, titanium sheet, tantalum piece etc.；It bonds
Agent is at least one of polytetrafluoroethylene (PTFE), Kynoar, sodium carboxymethylcellulose or butadiene-styrene rubber；Conductive agent is acetylene
At least one of black, Super-P, Ketjen black or graphene.
7. as claimed in claim 5 a kind of using the molybdenum trioxide of oxygen-containing vacancy as the water system aluminium ion electricity of negative electrode active material
Pond, which is characterized in that aqueous electrolyte containing aluminium ion is by one or more such as aluminium chloride, aluminum sulfate, aluminum nitrate, aluminium acetates
Solution composition.
8. the method for preparing any one of claim 5 ~ 7 water system aluminium ion battery, which is characterized in that include the following steps：
1）By MoO3-x, conductive agent and binder mixing, be coated uniformly on collector after slurry is made, then at 60 ~ 120 DEG C
It is dried in vacuum drying chamber, cathode pole piece is made；
2）With step 1）Anode pole piece is made in positive electrode by the method；
3）By step 1）With 2）Obtained cathode pole piece, anode pole piece and diaphragm is assembled, and the electrolysis of water system containing aluminium ion is added
Liquid obtains soft-package battery or button cell to get the water system aluminium ion to a kind of molybdenum trioxide of oxygen-containing vacancy for negative material
Battery.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109375113A (en) * | 2018-09-26 | 2019-02-22 | 山东精工电子科技有限公司 | The method for testing lithium electric material specific discharge capacity |
| CN109546078A (en) * | 2018-12-28 | 2019-03-29 | 银隆新能源股份有限公司 | A kind of preparation method and water system aluminium ion battery of water system aluminium ion battery cathode |
| CN109879320A (en) * | 2019-03-14 | 2019-06-14 | 清华大学深圳研究生院 | α-MoO3-xNanobelt and preparation method thereof, electrode material and energy storage device |
| CN110212182A (en) * | 2019-05-27 | 2019-09-06 | 珠海格力电器股份有限公司 | Cell positive material and the positive plate comprising it, cell negative electrode material and the negative electrode tab comprising it, lithium ion battery and electrode slurry |
| CN110586166A (en) * | 2019-10-13 | 2019-12-20 | 中国科学院福建物质结构研究所 | Preparation of molybdenum oxide nanosheet and application of molybdenum oxide nanosheet in photocatalytic nitrogen fixation |
| CN110767459A (en) * | 2019-10-30 | 2020-02-07 | 东华大学 | High-voltage water system symmetrical super capacitor and preparation method thereof |
| CN111715241A (en) * | 2020-07-31 | 2020-09-29 | 北京师范大学 | Oxygen-deficient molybdenum oxide/nickel sulfide/foamed nickel electrocatalyst and preparation method thereof |
| CN112563575A (en) * | 2020-12-08 | 2021-03-26 | 上海电力大学 | Composite solid electrolyte with transition molybdenum trioxide as filler, preparation method and application |
| CN114149028A (en) * | 2021-11-15 | 2022-03-08 | 大连理工大学 | Method for doping molybdenum disulfide with oxygen induced by ethylene glycol and application of method in lithium-sulfur battery |
| CN114824240A (en) * | 2022-04-01 | 2022-07-29 | 五邑大学 | Modified molybdenum oxide and zinc ion battery based on modified molybdenum oxide |
| CN115744989A (en) * | 2022-11-11 | 2023-03-07 | 华中科技大学 | alpha-MoO 3 Nanobelt, preparation method and energy storage application of nanobelt in proton battery |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109375113A (en) * | 2018-09-26 | 2019-02-22 | 山东精工电子科技有限公司 | The method for testing lithium electric material specific discharge capacity |
| CN109546078A (en) * | 2018-12-28 | 2019-03-29 | 银隆新能源股份有限公司 | A kind of preparation method and water system aluminium ion battery of water system aluminium ion battery cathode |
| CN109879320A (en) * | 2019-03-14 | 2019-06-14 | 清华大学深圳研究生院 | α-MoO3-xNanobelt and preparation method thereof, electrode material and energy storage device |
| CN110212182A (en) * | 2019-05-27 | 2019-09-06 | 珠海格力电器股份有限公司 | Cell positive material and the positive plate comprising it, cell negative electrode material and the negative electrode tab comprising it, lithium ion battery and electrode slurry |
| CN110586166A (en) * | 2019-10-13 | 2019-12-20 | 中国科学院福建物质结构研究所 | Preparation of molybdenum oxide nanosheet and application of molybdenum oxide nanosheet in photocatalytic nitrogen fixation |
| CN110767459A (en) * | 2019-10-30 | 2020-02-07 | 东华大学 | High-voltage water system symmetrical super capacitor and preparation method thereof |
| CN111715241A (en) * | 2020-07-31 | 2020-09-29 | 北京师范大学 | Oxygen-deficient molybdenum oxide/nickel sulfide/foamed nickel electrocatalyst and preparation method thereof |
| CN112563575A (en) * | 2020-12-08 | 2021-03-26 | 上海电力大学 | Composite solid electrolyte with transition molybdenum trioxide as filler, preparation method and application |
| CN114149028A (en) * | 2021-11-15 | 2022-03-08 | 大连理工大学 | Method for doping molybdenum disulfide with oxygen induced by ethylene glycol and application of method in lithium-sulfur battery |
| CN114824240A (en) * | 2022-04-01 | 2022-07-29 | 五邑大学 | Modified molybdenum oxide and zinc ion battery based on modified molybdenum oxide |
| CN115744989A (en) * | 2022-11-11 | 2023-03-07 | 华中科技大学 | alpha-MoO 3 Nanobelt, preparation method and energy storage application of nanobelt in proton battery |
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Application publication date: 20180914 |