CN110498454A - A kind of spinel type nanometer crystalline substance material and its preparation method and application - Google Patents
A kind of spinel type nanometer crystalline substance material and its preparation method and application Download PDFInfo
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- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
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- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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Abstract
The invention belongs to chemical material technical field, specially a kind of spinel type nanometer crystalline substance material and its preparation method and application.The method of the present invention includes: to prepare spinel type nanometer crystalline substance by chemical liquid phase synthesis and solvent-thermal process technique, obtains powder by washing and drying and processing.Spinel type nanometer obtained is brilliant, having a size of 4-10 nm, general formula AB2O4, wherein one of A Mn, Co, Zn, Ni；B is one of Mn, Co.Present invention process is easy, has universality, and nanocrystalline pattern obtained is uniform controllable, has huge application prospect in the fields such as unit price and multivalent ion battery, supercapacitor and photocatalysis.The present invention is used to prepare the secondary Zinc ion battery of water system that spinel type nanometer crystalline substance assembles for positive electrode, the zinc ion storage performance high with specific capacity, high rate performance is excellent.
Description
Technical field
The invention belongs to chemical materials synthesis technical fields, and in particular to spinel type nanometer crystalline substance and preparation method thereof, and
Application in the secondary Zinc ion battery of water system.
Background technique
It is increasingly prominent the problem of in terms of the utilization of resources and environmental pollution with the high speed development of social economy and science and technology
Out.The development and utilization of all kinds of new energy become to be increasingly urgent to, and corresponding energy storage material and energy storage device also become research hotspot.It is high
Effect storage can greatly improve the utilization rate of the energy, monovalention battery (such as lithium, sodium, potassium), multivalent ion battery (such as magnesium,
Zinc, aluminium) and supercapacitor be common a few class high-efficiency energy-storage devices.It is more due to the shortage of lithium resource and the problems such as safety
Valence ion battery gradually causes the concern of researchers in recent years.Wherein, the secondary Zinc ion battery of water system overcomes disposable zinc
Recovery processing and problem of resource waste, there is very big application potential caused by manganese dry cell.
The electrode material of zinc ion secondary cell largely affects battery performance, it is therefore desirable to develop capacity
The electrode material high, power is big, stability is good.Transition metal oxide is common a kind of Zinc ion battery electrode material,
In spinel oxides within 10 nanometers again because of high active specific surface, short ion diffusion length and fast ion diffusion
Rate can speed up the dynamics of ion storage and improve comprehensive performance.Currently, in the preparation process of spinel type nanometer material
In, common method has (the Chen Liqin lithium manganate having spinel structure such as solid phase method, the precipitation method, sol-gel method, hydrothermal/solvent heat
Preparation method patented technology symposium [J] science and technology visual field, 2015,29,324-325.).Nano material is made in the above method
Structure include nano wire, nanometer sheet, nano flower etc., size usually at 20 nanometers or more, even up to arrives micron order
(Yuan, C. Z., Wu. H. B., et al. Mixed Transition-Metal Oxides:Design,
Synthesis, and Energy-Related Applications[J]. Angew. Chem. Int. Ed. 2014,
53,1488-1504), spinel oxides preparation of the size within 10 nanometers is still difficult point.
The present invention provides a kind of simple process, the spinel type nanometer crystal preparation method with certain universality, nanocrystalline
Pattern it is uniform controllable, size is in 10 nm hereinafter, in monovalention battery, multivalent ion battery, supercapacitor and photocatalysis
Equal fields have big application prospect.Use the water system that spinel type nanometer crystalline substance is assembled into the present invention for positive electrode secondary
Zinc ion battery shows the zinc ion storage performance that specific capacity is high, high rate performance is excellent.
Summary of the invention
The present invention for deficiency present in existing zero dimension spinel type materials synthetic technology, propose one kind it is easy to operate,
Spinel type nanometer crystalline substance material of safety and environmental protection and preparation method thereof, and the application in the secondary Zinc ion battery of water system.
The preparation method of spinel type nanometer crystalline substance material provided by the invention, specific steps are as follows:
(1) it uses chemical liquid phase synthesis technology to obtain synthetic solvent: being original with the soluble-salt of A, the soluble-salt of B and ammonium hydroxide
The molar ratio of reactant, A and B are 1:(1-6), using ethyl alcohol as synthetic environment, uniformly mix, in 80-90 DEG C of hot oil bath
Middle heating reaction system 2-10 h；Here A is one of Mn, Co, Zn, Ni；B is one of Mn, Co；
(2) solvent-thermal process technique is used, spinel type nanometer crystalline substance is prepared: above-mentioned gained synthetic solvent is transferred to reaction kettle
In polytetrafluoroethylliner liner, liquid fills 75%-85%, in 120-250 DEG C of heating reaction kettle 2-40h；
(3) by washing and drying and processing, spinel type nanometer crystalline substance powder body material is obtained.
In the present invention, the spinel type nanometer is brilliant, having a size of 4-10 nm, general formula AB2O4。
In the present invention, the soluble-salt uses acetate hydrate salt；The ammonium hydroxide is commerical grade ammonium hydroxide (mass fraction 25
~ 28%), usage amount is 1-2 mL；The ethyl alcohol is commerical grade dehydrated alcohol (mass fraction >=99.8%), usage amount 150-
300 mL。
In the present invention, the carrying out washing treatment is that hydro-thermal synthesis process products therefrom is transferred in Buchner funnel, Bu Shi leakage
Bucket is internal to cover organic system miillpore filter, and in the precipitating into funnel plus ethyl alcohol is to funnel internal volume is full of, and filters to pumping and washes
Liquid is washed, this operation 3-6 times is repeated.
The drying and processing is that the product of washed processing is transferred on filter paper, dry in 50-70 DEG C of convection oven
12-24 h。
The present invention also provides a kind of secondary Zinc ion batteries of water system, and the secondary Zinc ion battery of the water system is mainly by anode
Pole piece, cathode pole piece, diaphragm and electrolyte composition, the anode pole piece is by positive electrode active materials, conductive agent acetylene black and bonding
Agent PVDF is formed by the mass ratio of 7:2:1, and the positive electrode active materials are above-mentioned spinel type nanometer crystalline substance material.
Compared with prior art, technical effect of the invention includes:
1, the chemical liquid phase synthesis and solvent-thermal process technique, simple process that the present invention uses have certain universality；
2, the spinel type nanometer that the present invention obtains is brilliant, and for nanocrystalline size in 4-10nm, pattern is uniform controllable, and because size is imitated
It answers and the characteristics such as high-specific surface area, more active sites, in monovalention battery, multivalent ion battery, supercapacitor and light
The fields such as catalysis have huge application prospect；
3, the present invention provides a kind of secondary Zinc ion battery of water system, and the secondary Zinc ion battery of the water system is using point in the present invention
Nanocrystalline spar type is positive electrode, the excellent zinc ion storage performance such as specific capacity height, high rate performance is shown, in electrochemistry
Aspect of performance has certain breakthrough.
Detailed description of the invention
Fig. 1 is the transmission electron microscope photo and corresponding selective electron diffraction for the spinel type nanometer crystalline substance that synthesis obtains
Figure.In figure, (a) CoMn2O4, (b) ZnMn2O4, (c) Mn3O4, (d) Co3O4。
Fig. 2 is the X-ray powder diffraction pattern of spinel type nanometer crystalline substance that synthesis obtains, in figure, (a) CoMn2O4, (b)
ZnMn2O4, (c) Mn3O4, (d) Co3O4。
Fig. 3 is by the perseverance electricity for the secondary Zinc ion battery of water system that the spinel type nanometer crystalline substance is positive electrode and is assembled into
Flow charging and discharging curve.
Specific embodiment
The present invention is further described below by specific embodiment.But the present invention is not limited to these Examples.
Embodiment 1:
Four water manganese acetate of four water cobalt acetate of 1.5mmol commerical grade and 3 mmol commerical grade is weighed, 225ml ethyl alcohol and 1.5 mL are added
Ammonium hydroxide is uniformly mixed in 250mL three-neck flask, and 2 h of reaction system is heated in 80 DEG C of hot oil baths.After reaction, to anti-
It answers system to be cooled to room temperature, acquired solution is transferred in the polytetrafluoroethylliner liner of laboratory room small-sized reaction kettle, in 150 DEG C of drums
10 h of reaction kettle is heated in wind baking oven.After reaction, it is cooled to room temperature to reaction system, products therefrom is transferred to Bu Shi leakage
In bucket, covering organic system miillpore filter (aperture is 0.22 μm), adds ethyl alcohol to funnel internal volume is full of, filters extremely inside funnel
Cleaning solution is pumped, is repeated 3 times.Product after washing is transferred on filter paper, dry 12 h, obtain in 60 DEG C of convection ovens
CoMn2O4Nanocrystalline powder, particle size in 4-10 nm, pattern as shown in Fig. 1 (a), X-ray powder diffraction pattern such as Fig. 2
(a) shown in.
Embodiment 2:
4.5 mmol commerical grade, four water manganese acetate is weighed, 225ml ethyl alcohol and 1.5 mL ammonium hydroxide are added, in 250 mL three-neck flasks
It is uniformly mixed, 2 h of reaction system is heated in 80 DEG C of hot oil baths.After reaction, it is cooled to room temperature to reaction system, by institute
It obtains solution to be transferred in the polytetrafluoroethylliner liner of laboratory room small-sized reaction kettle, reaction kettle 10 is heated in 150 DEG C of convection ovens
h.After reaction, it is cooled to room temperature to reaction system, products therefrom is transferred in Buchner funnel, covering is organic inside funnel
It is miillpore filter (aperture is 0.22 μm), adds ethyl alcohol to funnel internal volume is full of, filter to cleaning solution is pumped, be repeated 3 times.It will
Product after washing is transferred on filter paper, and dry 12 h, obtain Mn in 60 DEG C of convection ovens3O4Nanocrystalline powder, particle size exist
Shown in 4-10 nm, pattern such as Fig. 1 (c), X-ray powder diffraction pattern is as shown in Figure 2 (c).
Embodiment 3:
A kind of secondary Zinc ion battery of water system, the secondary Zinc ion battery positive electrode of the water system is using described in embodiment 1
CoMn2O4It is nanocrystalline.Weigh the positive electrode CoMn that mass ratio is 7:2:12O4Nanocrystalline, conductive agent acetylene black and binder
PVDF, by positive electrode Mn3O4Nanocrystalline and conductive agent acetylene black is fully ground in mortar, and PVDF is placed in small beaker, is added
Enter NMP and stirs 1h to being completely dissolved.Mixture after will be ground is added in the PVDF dissolved, and appropriate NMP, which is added, makes viscosity
Suitably, 8h is stirred.Slurry is coated on 10 μm of 304L stainless steel foils or carbon paper, surface density about 2mg/cm2, in 80 DEG C of vacuum
Dry 12h in drying box, is cut into the round anode pole piece that diameter is 15mm after being cooled to room temperature.
Using above-mentioned round pole piece as anode pole piece, using 10 μm of metallic zinc foils that diameter is 15 mm as cathode pole piece, with
The glass fibre that diameter is 19 mm is diaphragm, with 2 mol/L ZnSO4+0.2 mol/L MnSO4Aqueous solution is electrolyte, assembly
At 2032 button cells, constant current charge-discharge curve is as shown by dotted lines in figure 3.
Embodiment 4:
A kind of secondary Zinc ion battery of water system, the secondary Zinc ion battery positive electrode of the water system use Mn described in embodiment 13O4
It is nanocrystalline.Weigh the positive electrode Mn that mass ratio is 7:2:13O4Nanocrystalline, conductive agent acetylene black and binder PVDF, will be positive
Material Mn3O4Nanocrystalline and conductive agent acetylene black is fully ground in mortar, and PVDF is placed in small beaker, and NMP is added and stirs 1h
To being completely dissolved.Mixture after will be ground is added in the PVDF dissolved, and appropriate NMP, which is added, keeps viscosity appropriate, stirs 8h.
Slurry is coated on 10 μm of 304L stainless steel foils or carbon paper, about 2 mg/cm of surface density2, done in 80 DEG C of vacuum ovens
Dry 12 h is cut into the round anode pole piece that diameter is 15 mm after being cooled to room temperature.
Using above-mentioned round pole piece as anode pole piece, using 10 μm of metallic zinc foils that diameter is 15 mm as cathode pole piece, with
The glass fibre that diameter is 19 mm is diaphragm, with 2 mol/L ZnSO4+0.2 mol/L MnSO4Aqueous solution is electrolyte, assembly
At 2032 button cells, constant current charge-discharge curve is as shown in figure 3 by the solid lines.
Claims (6)
1. a kind of preparation method of spinel type nanometer crystalline substance material, which is characterized in that specific steps are as follows:
(1) it uses chemical liquid phase synthesis technology to obtain synthetic solvent: being original with the soluble-salt of A, the soluble-salt of B and ammonium hydroxide
The molar ratio of reactant, A and B are 1:(1-6), using ethyl alcohol as synthetic environment, uniformly mix, in 80-90 DEG C of hot oil bath
Middle heating reaction system 2-10 h；Here A is one of Mn, Co, Zn, Ni；B is one of Mn, Co；
(2) spinel type nanometer crystalline substance is prepared using solvent-thermal process technique: above-mentioned gained synthetic solvent is transferred to reaction kettle
In polytetrafluoroethylliner liner, liquid fills 75%-85%, in 120-250 DEG C of heating reaction kettle 2-40h；Obtained spinel-type is received
The size of meter Jing is 4-10 nm, general formula AB2O4；
(3) by washing and drying and processing, spinel type nanometer crystalline substance powder body material is obtained.
2. the preparation method of spinel type nanometer crystalline substance material according to claim 1, which is characterized in that the solubility
Salt uses acetate hydrate salt；The ammonium hydroxide is commerical grade ammonium hydroxide, and mass fraction is 25 ~ 28%；The ethyl alcohol is the anhydrous second of commerical grade
Alcohol, mass fraction >=99.8%.
3. the preparation method of spinel type nanometer crystalline substance material according to claim 1, which is characterized in that the washup
Reason, is that hydro-thermal synthesis process products therefrom is transferred in Buchner funnel, and organic system miillpore filter is covered inside Buchner funnel, to
In precipitating in funnel plus ethyl alcohol is to funnel internal volume is full of, and filters to cleaning solution is pumped, repeats this operation 3-6 times；Institute
Drying and processing is stated, is that the resulting product of carrying out washing treatment is transferred on filter paper, the dry 12-24 h in 50-70 DEG C of convection oven.
4. the spinel type nanometer crystalline substance material that the preparation method as described in one of claim 1-3 obtains.
5. spinel type nanometer crystalline substance material as claimed in claim 4 is as positive electrode in the secondary Zinc ion battery of water system
Using.
6. a kind of secondary Zinc ion battery of water system, which is characterized in that with spinel type nanometer crystalline substance material as claimed in claim 4 work
For the positive electrode active materials of anode pole piece.
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| CN111740089A (en) * | 2020-07-06 | 2020-10-02 | 齐鲁工业大学 | Preparation method of anode material for water-based zinc ion battery |
| CN111769276A (en) * | 2020-06-01 | 2020-10-13 | 上海海事大学 | Water-containing leaf-shaped lamellar structure nano material, preparation method thereof and lithium ion energy storage application |
| CN112694131A (en) * | 2020-12-28 | 2021-04-23 | 惠州亿纬锂能股份有限公司 | Zinc manganate negative electrode material, method for preparing same by adopting coprecipitation method and application of zinc manganate negative electrode material |
| CN118335916A (en) * | 2024-04-16 | 2024-07-12 | 常州大学 | Anion step-by-step substitution spinel electrode material for zinc ion battery and preparation method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111769276A (en) * | 2020-06-01 | 2020-10-13 | 上海海事大学 | Water-containing leaf-shaped lamellar structure nano material, preparation method thereof and lithium ion energy storage application |
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| CN112694131A (en) * | 2020-12-28 | 2021-04-23 | 惠州亿纬锂能股份有限公司 | Zinc manganate negative electrode material, method for preparing same by adopting coprecipitation method and application of zinc manganate negative electrode material |
| CN112694131B (en) * | 2020-12-28 | 2023-07-28 | 惠州亿纬锂能股份有限公司 | Zinc manganate negative electrode material, method for preparing same by adopting coprecipitation method and application thereof |
| CN118335916A (en) * | 2024-04-16 | 2024-07-12 | 常州大学 | Anion step-by-step substitution spinel electrode material for zinc ion battery and preparation method thereof |
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