CN108793254A - A kind of Na0.7ZnxMnyO2The preparation method of stratified material - Google Patents

A kind of Na0.7ZnxMnyO2The preparation method of stratified material Download PDF

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CN108793254A
CN108793254A CN201810581549.2A CN201810581549A CN108793254A CN 108793254 A CN108793254 A CN 108793254A CN 201810581549 A CN201810581549 A CN 201810581549A CN 108793254 A CN108793254 A CN 108793254A
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sodium
preparation
stratified material
stratified
ion battery
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刘国强
张竟
张竟一
于晗
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Northeastern University China
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G45/00—Compounds of manganese
    • C01G45/006—Compounds containing, besides manganese, two or more other elements, with the exception of oxygen or hydrogen
    • 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
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
    • 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
    • H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
    • 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
    • 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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • 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
    • 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
    • H01M2004/021—Physical characteristics, e.g. porosity, surface area
    • 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
    • H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/028—Positive electrodes
    • 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

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  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
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  • Engineering & Computer Science (AREA)
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  • Manufacturing & Machinery (AREA)
  • Battery Electrode And Active Subsutance (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

The present invention relates to a kind of Na0.7ZnxMnyO2The preparation method of stratified material, belongs to field of new energy technologies.A kind of Na0.7ZnxMnyO2The preparation method of stratified material, by sodium carbonate, zinc oxide, manganese dioxide in molar ratio 0.35:0.1~0.2:0.775~0.725 using absolute ethyl alcohol as medium mixing and ball milling, dry, obtains persursor material；Persursor material is placed in corundum crucible, crucible is placed in Muffle furnace, heating rate is 4~5 DEG C/min, and 8~12h is calcined at 800~900 DEG C of air atmosphere；It is cooled to room temperature with the speed of 2~3 DEG C/min, after grinding both.It is provided by the invention that preparation method is simple；Stratified material is made using this method and can be used as sodium-ion battery material.When using the stratified material as when the positive electrode of sodium-ion battery, first three specific discharge capacity enclosed of the battery increases, the grain size of material is more uniform.

Description

A kind of Na0.7ZnxMnyO2The preparation method of stratified material
Technical field
The present invention relates to a kind of Na0.7ZnxMnyO2The preparation method of stratified material, belongs to field of new energy technologies.
Background technology
Compared with lithium ion battery, sodium-ion battery has advantage more outstanding, and especially in terms of cost, sodium resource is rich Richness is distributed than wide；In addition, sodium-ion battery selects electrolyte range bigger, there is metastable chemical property, make With safer.Sodium-ion battery positive material is to influence sodium-ion battery to develop a very important part, studies ratio at present More electrode material is Na0.44MnO2, but Na+Radius is bigger, and the material of the preparation structure in charge and discharge process is easy to collapse It collapses, cycle performance is bad；Additionally, due to Jahn-Teller effects, this effect can cause the dissolving of Mn, limit Mn-based material Practical application, and it is less for the study on the modification of sodium ion battery electrode material at present.
Invention content
In order to improve the reversible capacity of sodium-ion battery, improve sodium-ion battery performance, the present invention provides a kind of sodium from Sub- cell positive material Na0.7ZnxMnyO2Preparation method, utilize cell positive material Na made from this method0.7ZnxMnyO2For The stratified material of zinc is adulterated, which has higher reversible capacity between 2~4.4V.
A kind of Na0.7ZnxMnyO2The preparation method of stratified material, in molar ratio by sodium carbonate, zinc oxide, manganese dioxide 0.35:0.1~0.2:0.775~0.725 using absolute ethyl alcohol as medium mixing and ball milling, and ball milling 4 under 400~500rad/min~ 5h, it is dry, obtain persursor material；Persursor material is placed in corundum crucible, crucible is placed in Muffle furnace, heating rate is 4~5 DEG C/min, 8~12h is calcined at 800~900 DEG C of air atmosphere；It is cooled to room temperature with the speed of 2~3 DEG C/min, after grinding Both Na is obtained0.7ZnxMnyO2Stratified material, wherein x=0.1~0.2, y=0.775~0.725.
In above-mentioned technical proposal, the Na0.7ZnxMnyO2In stratified material, x, y meet in Na0.7ZnxMnyO2In chemical formula The criterion that chemical valence algebraical sum is zero.
In above-mentioned technical proposal, the drying preferably operates as follows：Mixture after ball milling is placed on constant temperature to do Dry 4~6h obtains persursor material in dry case.
A preferred technical solution of the invention is：By sodium carbonate, zinc oxide, manganese dioxide in molar ratio 0.35:0.1: 0.775,0.35:0.15:0.75 or 0.35:0.2:0.725 using absolute ethyl alcohol as medium mixing and ball milling, 400~500rad/min 4~5h of lower ball milling, it is dry, obtain persursor material；Persursor material is placed in corundum crucible, crucible is placed in Muffle furnace, Heating rate is 4~5 DEG C/min, and 8~12h is calcined at 800~900 DEG C of air atmosphere；It is cooled to the speed of 2~3 DEG C/min Room temperature both obtains Na after grinding0.7ZnxMnyO2Stratified material.
The Na obtained using above-mentioned preferred preparation method0.7ZnxMnyO2Stratified material, chemical formula Na0.7ZnxMnyO2 In, x=0.1, y=0.775 or x=0.15, y=0.75 or x=0.2, y=0.725.
It is a further object of the present invention to provide the Na made from the above method0.7ZnxMnyO2Stratified material, should Na0.7ZnxMnyO2Stratified material is made as follows：By sodium carbonate, zinc oxide, manganese dioxide in molar ratio 0.35:0.1~ 0.2:0.775~0.725 using absolute ethyl alcohol as medium mixing and ball milling, 4~5h of ball milling under 400~500rad/min, dry, before obtaining Drive body material；Persursor material is placed in corundum crucible, crucible is placed in Muffle furnace, heating rate is 4~5 DEG C/min, 8~12h is calcined at 800~900 DEG C of air atmosphere；It is cooled to room temperature with the speed of 2~3 DEG C/min, after grinding both Na0.7ZnxMnyO2Stratified material, wherein x=0.1~0.2, y=0.775~0.725.
A further object of the present invention provides above-mentioned Na0.7ZnxMnyO2Stratified material is answered as sodium-ion battery positive material With.
Beneficial effects of the present invention are：Preparation Na provided by the invention0.7ZnxMnyThe method of O is simple and practicable；Utilize the party Legal system obtains Na0.7ZnxMnyO2Stratified material can be used as sodium-ion battery material.When utilizing Na0.7ZnxMnyO2Stratified material is as sodium When the positive electrode of ion battery, first three specific discharge capacity enclosed of the battery increases, the grain size of material is more uniform.
Description of the drawings
Fig. 1 (a) and (b) are respectively Na of the present invention0.7ZnxMnyO2(x=0.15, y=0.75) and Na0.7ZnxMnyO2(x= 0.2, y=0.725) XRD spectrum；
Fig. 2 (a)~(c) is Na of the present invention0.7ZnxMnyO2(x=0.1, y=0.775), Na0.7ZnxMnyO2(x=0.15, y =0.75) and Na0.7ZnxMnyO2The preceding charge and discharge collection of illustrative plates three times of (x=0.2, y=0.725)；
Fig. 3 is Na of the present invention0.7ZnxMnyO2The cycle performance collection of illustrative plates of (x=0.15, y=0.75)；
Fig. 4 is Na of the present invention0.7ZnxMnyO2The high rate performance collection of illustrative plates of (x=0.15, y=0.75)；
Fig. 5 is Na of the present invention0.7ZnxMnyO2The SEM spectrum of (x=0.15, y=0.75)；
Fig. 6 is Na of the present invention0.7ZnxMnyO2The XPS collection of illustrative plates of (x=0.15, y=0.75).
Specific implementation mode
Following non-limiting embodiments can make those skilled in the art be more fully understood the present invention, but not with Any mode limits the present invention.
Test method described in following embodiments is unless otherwise specified conventional method；The reagent and material, such as Without specified otherwise, commercially obtain.
Embodiment 1
Sodium-ion battery anode electrode material Na0.7Zn0.1Mn0.775O2Preparation method, include the following steps：
Step 1, Na is prepared0.7Zn0.1Mn0.775O2Precursor：
(1) sodium carbonate 1.1463g, zinc oxide 0.2515g and manganese dioxide 2.0820g is weighed to be placed in ball grinder；
(2) dispersant absolute ethyl alcohol 10mL is added；
(3) by raw material to be taken out after the rotating speed ball milling 4h of 400rad/min, it is placed in thermostatic drying chamber dry 6h, is obtained Powder is Na0.7Zn0.1Mn0.775O2Precursor.
Step 2, Na is prepared0.7Zn0.1Mn0.775O2Electrode material：
(1) precursor powder of gained in step 1 is put into corundum crucible and in Muffle furnace, with 800 under air atmosphere 10h is calcined at DEG C, heating rate is 5 DEG C/min, is cooled to room temperature with the speed of 3 DEG C/min, finally obtains electrode material Na0.7Zn0.1Mn0.775O2。
The present invention passes through Solid phase synthesis positive electrode Na0.7Zn0.1Mn0.775O2, material structure form is preferable.Battery is existed Charge-discharge test, Na are carried out under 0.1C0.7Zn0.1Mn0.775O2First discharge specific capacity be up to (126.4mAh g-1)。
Embodiment 2
Sodium-ion battery anode Na0.7Zn0.15Mn0.75O2The preparation method of electrode material, includes the following steps：
Step 1, Na is prepared0.7Zn0.15Mn0.75O2Precursor：
(1) sodium carbonate 1.1228g, zinc oxide 0.3695g and manganese dioxide 1.9735g is weighed to be placed in ball grinder；
(2) dispersant absolute ethyl alcohol 10mL is added；
(3) by raw material to be taken out after the rotating speed ball milling 4h of 400rad/min, it is placed in thermostatic drying chamber dry 6h, is obtained Powder is Na0.7Zn0.15Mn0.75O2Precursor.
Step 2, Na is prepared0.7Zn0.15Mn0.75O2Electrode material：
(1) precursor powder of gained in step 1 is put into corundum crucible and in Muffle furnace, with 800 under air atmosphere 10h is calcined at DEG C, heating rate is 5 DEG C/min, is cooled to room temperature with the speed of 3 DEG C/min, finally obtains electrode material Na0.7Zn0.15Mn0.75O2。
The present invention passes through Solid phase synthesis positive electrode Na0.7Zn0.15Mn0.75O2, material structure form is preferable, and battery follows Ring performance is good, and decaying is few, and chemical property obtains different degrees of raising.Battery is subjected to charge and discharge electrical measurement at 0.1C Examination, Na0.7Zn0.15Mn0.75O2Discharge capacity for the first time be up to (158.1mAh g-1)。
Embodiment 3
Sodium-ion battery anode Na0.7Zn0.2Mn0.725O2The preparation method of electrode material, includes the following steps：
Step 1, Na is prepared0.7Zn0.2Mn0.725O2Precursor：
(1) sodium carbonate 1.1018g, zinc oxide 0.4835g and manganese dioxide 1.8720g is weighed to be placed in ball grinder；
(2) dispersant absolute ethyl alcohol 10mL is added；
(3) by raw material to be taken out after the rotating speed ball milling 4h of 400rad/min, it is placed in thermostatic drying chamber dry 6h, is obtained Powder is Na0.7Zn0.2Mn0.725O2Precursor.
Step 2, Na is prepared0.7Zn0.2Mn0.725O2Electrode material：
(1) precursor powder of gained in step 1 is put into corundum crucible and in Muffle furnace, with 800 under air atmosphere 10h is calcined at DEG C, heating rate is 5 DEG C/min, is cooled to room temperature with the speed of 3 DEG C/min, finally obtains electrode material Na0.7Zn0.2Mn0.725O2。
The present invention passes through Solid phase synthesis positive electrode Na0.7Zn0.2Mn0.725O2, material structure form is preferable.Battery is existed Charge-discharge test, Na are carried out under 0.1C0.7Zn0.2Mn0.725O2Discharge capacity for the first time be up to (171.7mAh g-1)。

Claims (4)

1. a kind of Na0.7ZnxMnyO2The preparation method of stratified material, it is characterised in that：Sodium carbonate, zinc oxide, manganese dioxide are pressed Molar ratio 0.35:0.1~0.2:0.775~0.725 using absolute ethyl alcohol as medium mixing and ball milling, ball under 400~500rad/min 4~5h is ground, it is dry, obtain persursor material；Persursor material is placed in corundum crucible, crucible is placed in Muffle furnace, is heated up Speed is 4~5 DEG C/min, and 8~12h is calcined at 800~900 DEG C of air atmosphere；It is cooled to room temperature with the speed of 2~3 DEG C/min, Both Na is obtained after grinding0.7ZnxMnyO2Stratified material, wherein x=0.1~0.2, y=0.775~0.725.
2. according to the method described in claim 1, it is characterized in that：The sodium carbonate, zinc oxide, manganese dioxide molar ratio be 0.35:0.1:0.775,0.35:0.15:0.75 or 0.35:0.2:0.725；The Na0.7ZnxMnyO2X=0.1, y=in formula 0.775 or x=0.15, y=0.75 or x=0.2, y=0.725.
3. Na made from claim 1 the method0.7ZnxMnyO2Stratified material.
4. Na described in claim 30.7ZnxMnyO2Application of the stratified material as sodium-ion battery positive material.
CN201810581549.2A 2018-06-05 2018-06-05 A kind of Na0.7ZnxMnyO2The preparation method of stratified material Pending CN108793254A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20200083825A (en) * 2018-12-31 2020-07-09 동국대학교 산학협력단 Cathode active material having zinc in sodium atomic layer, preparation method thereof and the sodium secondary battery comprising the same
CN112830521A (en) * 2019-11-22 2021-05-25 南京理工大学 F-doped P2-Na0.7MnO2Electrode material and preparation method thereof
KR20220100261A (en) * 2021-01-08 2022-07-15 고려대학교 산학협력단 Cathode active material
CN115536072A (en) * 2022-10-24 2022-12-30 沈阳国科金能科技有限公司 Ferromanganese-based Na 0.67 Mn 0.9 Fe 0.1 O 2 Modification method of positive electrode material of sodium ion battery
CN117902631A (en) * 2024-03-14 2024-04-19 新乡学院 Layered metal oxide Na0.7MnO2.05And a method for preparing the same

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105633342A (en) * 2014-11-27 2016-06-01 中国科学院长春应用化学研究所 Sodium ion energy storage device positive electrode material and preparation method therefor, and sodium ion energy storage device
CN107834106A (en) * 2017-11-13 2018-03-23 东莞市联洲知识产权运营管理有限公司 A kind of preparation method of flexible water system sodium-ion battery

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105633342A (en) * 2014-11-27 2016-06-01 中国科学院长春应用化学研究所 Sodium ion energy storage device positive electrode material and preparation method therefor, and sodium ion energy storage device
CN107834106A (en) * 2017-11-13 2018-03-23 东莞市联洲知识产权运营管理有限公司 A kind of preparation method of flexible water system sodium-ion battery

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20200083825A (en) * 2018-12-31 2020-07-09 동국대학교 산학협력단 Cathode active material having zinc in sodium atomic layer, preparation method thereof and the sodium secondary battery comprising the same
KR102161900B1 (en) * 2018-12-31 2020-10-06 동국대학교 산학협력단 Cathode active material having zinc in sodium atomic layer, preparation method thereof and the sodium secondary battery comprising the same
CN112830521A (en) * 2019-11-22 2021-05-25 南京理工大学 F-doped P2-Na0.7MnO2Electrode material and preparation method thereof
CN112830521B (en) * 2019-11-22 2022-03-15 南京理工大学 F-doped P2-Na0.7MnO2Electrode material and preparation method thereof
KR20220100261A (en) * 2021-01-08 2022-07-15 고려대학교 산학협력단 Cathode active material
KR102586288B1 (en) 2021-01-08 2023-10-18 고려대학교 산학협력단 Cathode active material
CN115536072A (en) * 2022-10-24 2022-12-30 沈阳国科金能科技有限公司 Ferromanganese-based Na 0.67 Mn 0.9 Fe 0.1 O 2 Modification method of positive electrode material of sodium ion battery
CN115536072B (en) * 2022-10-24 2023-08-11 沈阳国科金能科技有限公司 Ferromanganese based Na 0.67 Mn 0.9 Fe 0.1 O 2 Modification method of sodium ion battery anode material
CN117902631A (en) * 2024-03-14 2024-04-19 新乡学院 Layered metal oxide Na0.7MnO2.05And a method for preparing the same

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Application publication date: 20181113