CN107732223A - Water system sodium-ion battery positive electrode and preparation method thereof and battery - Google Patents
Water system sodium-ion battery positive electrode and preparation method thereof and battery Download PDFInfo
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- CN107732223A CN107732223A CN201710817470.0A CN201710817470A CN107732223A CN 107732223 A CN107732223 A CN 107732223A CN 201710817470 A CN201710817470 A CN 201710817470A CN 107732223 A CN107732223 A CN 107732223A
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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
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G45/00—Compounds of manganese
- C01G45/12—Manganates manganites or permanganates
- C01G45/1221—Manganates or manganites with a manganese oxidation state of Mn(III), Mn(IV) or mixtures thereof
- C01G45/1228—Manganates or manganites with a manganese oxidation state of Mn(III), Mn(IV) or mixtures thereof of the type [MnO2]n-, e.g. LiMnO2, Li[MxMn1-x]O2
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/36—Accumulators not provided for in groups H01M10/05-H01M10/34
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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
- 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
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
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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
- Y02E60/10—Energy storage using batteries
Abstract
The present invention relates to water system sodium-ion battery positive electrode and preparation method thereof and battery, the positive electrode chemical formula is Na0.66Mn0.66Ti0.34O2, synthetic method is solid phase method, and process comprises the following steps：It is first according to certain proportion and weighs source chemicals respectively：Sodium carbonate (Na2CO3), manganese dioxide (MnO2) and titanium dioxide (TiO2)；Again the source chemicals weighed sufficiently mix and grind, carry out the calcining of certain time under certain heating schedule and calcination procedure by Muffle furnace；Grounds travel is carried out after calcining terminates sample cooling；Obtain target product.The beneficial effects of the invention are as follows：A kind of water system sodium-ion battery positive electrode is synthesized using inexpensive, simple and easy method, raw materials used cheap, synthetic method is simple, and high degree reduces synthesis cost, and industrialization degree is high, the characteristics of synthesized material structure and high stability.
Description
Technical field
The present invention relates to the positive electrode and preparation method of field of batteries, specifically battery, belong to electrochemical material
Field.
Background technology
The rapid development of society increasingly increases the demand of the energy, and the non-renewable energy resources such as limited coal oil of reserves
It has been difficult to meet.The development of the renewable new energies such as water energy, wind energy, solar energy serves huge alleviation to energy crisis and made
With, but energy storage is one of critical limiting factor of renewable new energy large-scale development.
At present, lithium-ion energy storage equipment has obtained widely studied development and application, but the reserves of lithium resource in many fields
It significantly limit its application in terms of extensive energy storage.Congeners of the sodium as elemental lithium, property is similar to lithium, and provides
Source is enriched, and development technique is ripe, and therefore, room temperature sodium-ion battery has obtained the extensive research and development of researchers.Sodium ion
Battery operation principle is similar to lithium ion battery, is a kind of process of reversible rocking chair type deintercalation sodium ion, is existed by both positive and negative polarity
The reversible deintercalation sodium ion of redox reaction in charge and discharge process reaches the charge and discharge electro ultrafiltration of battery.Organic system sodium ion electricity
Organic electrolyte low boiling point used in pond, it is inflammable and explosive, easily there is safety problem, significantly limit organic system sodium ion
The scale of battery.
Water system sodium-ion battery, as electrolyte, is had the characteristics of cost is low, safe, is using the aqueous solution of sodium salt
The splendid selection of extensive energy storage.But the conventional positive electrode of current water system sodium-ion battery mainly includes λ-MnO2、
Na0.44MnO2Deng manganese-base oxide and prussian blue iron cyanogen compound.But λ-MnO2Preparation be confined to pickling LiMn at present2O4
Method, it is impossible to avoid the use of lithium resource；Na0.44MnO2Charging and discharging capacity is low (45mAh/g)；Prussian blue iron cyaniding
Compound specific capacity low (60mAh/g) and contain cyanogen root and safety issue etc. be present and limit it as water system sodium-ion battery positive pole
The application of material.And the manganese-base oxide positive electrode Na of another dopingxMn(1-y-z)AyTizO2-δWith higher specific volume
(76mAh/g) and excellent cyclical stability are measured, but its building-up process uses expensive raw material Mn2O3, cost is high, limitation
It is large-scale to produce.
The content of the invention
The present invention is, and it is an object of the present invention to provide new water system sodium-ion battery is with just in order to solving the above problems and carry out
Pole material, preparation method and the battery using the material.
The invention provides a kind of water system sodium-ion battery positive electrode, it is characterised in that：Chemical formula is expressed as
Na0.66Mn0.66Ti0.34O2, use Cu-KαRadiation, uses Cu-KαRadiation, the XRD powder diffractions represented with 2 θ angles are 13.861
±0.1、16.473±0.1、19.283±0.1、19.500±0.1、22.286±0.1、33.775±0.1、35.605±
0.1st, 36.908 ± 0.1,48.449 ± 0.1,50.833 ± 0.1 have characteristic peak.
The present invention a kind of preparation method of water system sodium-ion battery positive electrode is also provided, it is characterised in that including with
Lower step：
Step 1: according to atomic molar ratio Na:Mn:Ti is (0.67~0.72):0.66:0.34 weighs sodium carbonate
(Na2CO3), manganese dioxide (MnO2) and titanium dioxide (TiO2), it is standby；
Step 2: the initiation material weighed in step 1 to be sufficiently mixed and grind, it is fully mixed to add appropriate organic solvent
Merging is ground to organic solvent evaporating completely, obtains the tiny well mixed precursor powder of particle；
Step 3: the precursor powder obtained in step 2 is poured into high-temperature resistant container, and jolt ramming；
Step 4: the high-temperature resistant container that precursor powder is contained with step 3 is calcined：3~5 DEG C/min heats up
The first temperature T is warming up under speed1Calcining a period of time, and it is continuously heating to second temperature under 3~5 DEG C/min heating rates
T2Calcining a period of time, after the completion of be cooled to room temperature, target product is obtained after grinding.
The preparation method of water system sodium-ion battery positive electrode provided by the invention, can also have the feature that：
Wherein, the organic solvent is anhydrous alcohols solvent.
The preparation method of water system sodium-ion battery positive electrode provided by the invention, can also have the feature that：
Wherein, the alcohols solvent is absolute ethyl alcohol.
The preparation method of water system sodium-ion battery positive electrode provided by the invention, can also have the feature that：
Wherein, the first temperature T1For 700~800 DEG C, second temperature T2For 900~1000 DEG C.
The preparation method of water system sodium-ion battery positive electrode provided by the invention, can also have the feature that：
Wherein, the first temperature T1The time of calcining is 3~6h, second temperature T2The time of calcining is 8~16h.
The preparation method of water system sodium-ion battery positive electrode provided by the invention, can also have the feature that：
Wherein, it is air Muffle furnace that the equipment used is calcined in step 4.
The preparation method of water system sodium-ion battery positive electrode provided by the invention, can also have the feature that：
Wherein, the high-temperature resistant container is corundum crucible.
The present invention also provides a kind of battery, it is characterised in that：The positive electrode of the battery contains above-mentioned water system sodium ion
Positive electrode for battery material.
Battery provided by the invention, it can also have the feature that, it is characterised in that：Wherein, the negative pole material of the battery
Expect that for metallic sodium, the battery be button cell.
The effect of invention and effect
The present invention prepares water system sodium-ion battery positive electrode using method inexpensive, simple to operation：Used
Method in, the raw material sodium carbonate Na that uses2CO3, manganese dioxide MnO2, titanium dioxide TiO2It is cheap, and producer
Calcining and grinding steps in method step require low to Preparation equipment, and whole preparation process is without specific condition requirement, production technology
Simple easily manipulation, industrialization degree is high, and production method does not produce harmful substance, environment-friendly.
Obtained Na0.66Mn0.66Ti0.34O2Positive electrode, constituent structure is stable, stable in the air can exist, beneficial to letter
Change the packaging of material, reduce storage, the cost of transport.
The water system sodium-ion battery of preparation holds specific capacity with the charge discharge of positive electrode and is up to 73mAh/g, charge and discharge
Electricity has stable average voltage (3.0V, Na+/ Na), good cycling stability, overall chemical property is high, is suitable as water system
Sodium-ion battery positive material.
Moreover, the positive electrode nontoxic pollution-free, environment-friendly.
Brief description of the drawings
Fig. 1 is water system sodium-ion battery positive electrode Na prepared by embodiments of the invention method0.66Mn0.66Ti0.34O2
X-ray powder diffraction pattern；
Fig. 2 is the water system sodium-ion battery positive electrode prepared using embodiments of the invention method
Na0.66Mn0.66Ti0.34O2In the charge-discharge performance test result using metallic sodium as the button cell to electrode assembling.
Embodiment
In order that the technical means, the inventive features, the objects and the advantages of the present invention are easy to understand, it is real below
Apply the performance for the electrode material that example is obtained to the water system sodium-ion battery of the present invention with the preparation method and making of positive electrode
It is specifically addressed.
Building-up process comprises the following steps：
Step 1: 1.2242g sodium carbonate Na is weighed respectively2CO3(11.55mmol), 1.9127g manganese dioxide MnO2
(22.00mmol), 0.9052g titanium dioxide TiO2(11.34mmol), (i.e. atomic molar ratio Na:Mn:Ti is 23.10：
22.10：11.34) standby.
Step 2: the initiation material weighed in step 1 to be sufficiently mixed and be ground with agate mortar, it is anhydrous to add 10ml
Ethanol is sufficiently mixed, and is ground to absolute ethyl alcohol evaporating completely, obtains drying, the tiny well mixed precursor powder of particle.
Step 3: the precursor powder obtained in step 2 is poured into corundum crucible, and jolt ramming.
Calcined, calcined Step 4: the crucible that precursor powder is contained with step 3 is placed in air Muffle furnace
Technique includes two stages：
1. low temperature presintering stage, concrete operations are as follows：Precursor powder is heated up by 3 DEG C/min of Muffle furnace heating rate
To 750 DEG C, 5h low temperature calcination is carried out at such a temperature；
2. the high-temperature calcination stage, low temperature calcination process with 3 DEG C/min heating rate is continuously heating to 950 DEG C after terminating,
12h high-temperature calcination is carried out at such a temperature.Room temperature is cooled to after the completion of two above calcination stage, is obtained after grinding
Target product Na0.66Mn0.66Ti0.34O2。
Analysis test
In order to characterize the chemical composition of obtained powder, appropriate progress elementary analysis is taken, the target product prepared
Chemical formula is expressed as Na0.66Mn0.66Ti0.34O2。
Further, XRD powder diffraction experiments are carried out to the material of preparation.Experimental result is as shown in figure 1, use Cu-KαSpoke
Penetrate, with the XRD powder diffractions that 2 θ angles represent 13.861 ± 0.1,16.473 ± 0.1,19.283 ± 0.1,19.500 ±
0.1st, 22.286 ± 0.1,33.775 ± 0.1,35.605 ± 0.1,36.908 ± 0.1,48.449 ± 0.1,50.833 ± 0.1 have
Characteristic peak.Data above illustrates that synthesized positive electrode belongs to the Pbam space groups of rhombic system, corresponding cell parameter a, b, c
Respectively(130) that above diffraction maximum is corresponded respectively in crystal,
(140), (200), (150), (160), (350), (360), (211), (291), (401) crystal face.
In order to prove that the present embodiment prepares performance of the electrode material as the positive electrode of battery, embodiments of the invention are used
Water system sodium-ion battery positive electrode prepared by method, button cell is assembled by negative electrode of metallic sodium, to the battery
Charge-discharge performance is tested, as a result as shown in Fig. 2 experiment surface material electrochemical charge and discharge electric capacity specific capacity height (reaches
73mAh/g), discharge and recharge average voltage 3.0V (vs Na+/ Na), good cycling stability, overall chemical property is high, is suitable as
Water system sodium-ion battery positive material.
The effect of embodiment and effect
The present embodiment prepares water system sodium-ion battery positive electrode using method inexpensive, simple to operation：Adopted
In method, the raw material sodium carbonate Na that uses2CO3, manganese dioxide MnO2, titanium dioxide T iO2It is cheap, Er Qiesheng
Produce the calcining in method and step and grinding steps and low is required to Preparation equipment, whole preparation process is without specific condition requirement, production
Technique simply easily manipulates, and industrialization degree is high, and production method does not produce harmful substance, environment-friendly.
In preparation process, according to atomic molar ratio Na:Mn:Ti is (0.67~0.72):0.66:0.34 weighs sodium carbonate
(Na2CO3), manganese dioxide (MnO2) and titanium dioxide (TiO2), such proportioning cause Na it is somewhat excessive (compared to
Na0.66Mn0.66Ti0.34O2For) so that whole calcined crystalline process reaction is more abundant, improves manganese dioxide (MnO2) and two
Titanium oxide (TiO2) raw material utilization rate.
Mixed grinding raw material is come by using absolute ethyl alcohol and prepares precursor powder, is on the one hand mixed by liquid dispersion
Close evenly, the addition of another aspect liquid make it that the particle that grinding obtains is more tiny, and size distribution is evenly.
Obtained Na0.66Mn0.66Ti0.34O2Positive electrode, constituent structure is stable, stable in the air can exist, beneficial to letter
Change the packaging of material, reduce storage, the cost of transport.
The water system sodium-ion battery of preparation holds specific capacity with the charge discharge of positive electrode and is up to 73mAh/g, charge and discharge
Electricity has stable average voltage (3.0V, Na+/ Na), good cycling stability, overall chemical property is high, is suitable as water system
Sodium-ion battery positive material.
Moreover, the positive electrode nontoxic pollution-free, environment-friendly.
Extended as one kind, the solvent that absolute ethyl alcohol is prepared as presoma is used in above-described embodiment, as a kind of generation
Replace, be all possible using other organic solvents such as petroleum ether, dioxane or low-alcohol solution, be from ethanol because
Consider cost and environment, toxicity considerations, can also be according to circumstances using the organic solvent of other greens, safety.
Extended as one kind, 3 DEG C/min heating rate is warming up to 750 DEG C in above-described embodiment, carries out at such a temperature
5h low temperature calcination；950 DEG C are continuously heating to 3 DEG C/min heating rate afterwards, the high temperature for carrying out 12h at such a temperature is forged
Burn, obtain electrode material, it is also possible that the regulation heating rate in 3-5 DEG C/min, while in the first temperature T1For 700~
800 DEG C, second temperature T2For 900~1000 DEG C and the first temperature T1The time of calcining is 3~6h, second temperature T2Calcining
Time is to be adjusted in 8~16h, and simply in the case of temperature height, corresponding calcination time suitably shortens, and makes in the case that temperature is low
Calcination time must be extended.
Above-described embodiment is that one embodiment that the effect of selection is relatively good is used as explanation in numerous experimental examples, real
The heating rate summarized on border in Summary, calcines problem, and calcination time is possible to the invention mesh of the present invention
.
Claims (10)
- A kind of 1. water system sodium-ion battery positive electrode, it is characterised in that：Chemical formula is expressed as Na0.66Mn0.66Ti0.34O2,Use Cu-KαRadiation, with the XRD powder diffractions that 2 θ angles represent 13.861 ± 0.1,16.473 ± 0.1,19.283 ± 0.1、19.500±0.1、22.286±0.1、33.775±0.1、35.605±0.1、36.908±0.1、48.449±0.1、 50.833 ± 0.1 has characteristic peak.
- 2. the preparation method of the water system sodium-ion battery positive electrode described in claim 1, it is characterised in that including following step Suddenly：Step 1: according to atomic molar ratio Na:Mn:Ti is (0.67~0.72):0.66:0.34 weighs sodium carbonate (Na2CO3)、 Manganese dioxide (MnO2) and titanium dioxide (TiO2), it is standby；Step 2: the initiation material weighed in step 1 to be sufficiently mixed and grind, add appropriate organic solvent and be sufficiently mixed simultaneously Organic solvent evaporating completely is ground to, obtains the tiny well mixed precursor powder of particle；Step 3: the precursor powder obtained in step 2 is poured into high-temperature resistant container, and jolt ramming；Step 4: the high-temperature resistant container that precursor powder is contained with step 3 is calcined：3~5 DEG C/min heating rates Under be warming up to the first temperature T1Calcining a period of time, and it is continuously heating to second temperature T under 3~5 DEG C/min heating rates2Forge Burn a period of time, after the completion of be cooled to room temperature, target product is obtained after grinding.
- 3. the preparation method of water system sodium-ion battery positive electrode according to claim 2, it is characterised in that：Wherein, the organic solvent is anhydrous alcohols solvent.
- 4. the preparation method of water system sodium-ion battery positive electrode according to claim 3, it is characterised in that：Wherein, the alcohols solvent is absolute ethyl alcohol.
- 5. the preparation method of water system sodium-ion battery positive electrode according to claim 2, it is characterised in that：Wherein, the first temperature T1For 700~800 DEG C, second temperature T2For 900~1000 DEG C.
- 6. the preparation method of water system sodium-ion battery positive electrode according to claim 2, it is characterised in that its feature It is：Wherein, the first temperature T1The time of calcining is 3~6h, second temperature T2The time of calcining is 8~16h.
- 7. the preparation method of water system sodium-ion battery positive electrode according to claim 2, it is characterised in that its feature It is：Wherein, it is in air Muffle furnace that the equipment used is calcined in step 4.
- 8. the preparation method of water system sodium-ion battery positive electrode according to claim 2, it is characterised in that：Wherein, the high-temperature resistant container is corundum crucible.
- A kind of 9. battery, it is characterised in that：The positive electrode of the battery contains the water system sodium-ion battery positive electrode described in claim 1.
- 10. battery according to claim 9, it is characterised in that：Wherein, the negative material of the battery is metallic sodium,The battery is button cell.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110336026A (en) * | 2019-06-11 | 2019-10-15 | 中国电力科学研究院有限公司 | The preparation method and water system sodium-ion battery of water system sodium-ion battery positive material |
| CN115010182A (en) * | 2022-04-28 | 2022-09-06 | 华南农业大学 | Sodium ion battery iron-manganese-based positive electrode material and preparation and application thereof |
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| CN104795555A (en) * | 2014-07-28 | 2015-07-22 | 中国科学院物理研究所 | Aqueous-solution sodium-ion battery and cathode material, preparation method and application thereof |
| CN107004868A (en) * | 2014-11-26 | 2017-08-01 | 3M创新有限公司 | Anode material for sodium ion battery and preparation method thereof |
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2017
- 2017-09-12 CN CN201710817470.0A patent/CN107732223A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104795555A (en) * | 2014-07-28 | 2015-07-22 | 中国科学院物理研究所 | Aqueous-solution sodium-ion battery and cathode material, preparation method and application thereof |
| CN107004868A (en) * | 2014-11-26 | 2017-08-01 | 3M创新有限公司 | Anode material for sodium ion battery and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110336026A (en) * | 2019-06-11 | 2019-10-15 | 中国电力科学研究院有限公司 | The preparation method and water system sodium-ion battery of water system sodium-ion battery positive material |
| CN115010182A (en) * | 2022-04-28 | 2022-09-06 | 华南农业大学 | Sodium ion battery iron-manganese-based positive electrode material and preparation and application thereof |
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Application publication date: 20180223 |