CN103594707A - High-temperature solid-phase synthesis method of one-dimensional nano-sodion cell anode material NaxMnO2 - Google Patents

High-temperature solid-phase synthesis method of one-dimensional nano-sodion cell anode material NaxMnO2 Download PDF

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CN103594707A
CN103594707A CN201310633362.XA CN201310633362A CN103594707A CN 103594707 A CN103594707 A CN 103594707A CN 201310633362 A CN201310633362 A CN 201310633362A CN 103594707 A CN103594707 A CN 103594707A
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sodium
powder
manganese
mno
phase synthesis
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徐茂文
牛玉斌
李长明
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Southwest University
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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
    • 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
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G45/00—Compounds of manganese
    • C01G45/12—Manganates manganites or permanganates
    • 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
    • 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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Abstract

The invention discloses a high-temperature solid-phase synthesis method of a one-dimensional nano-sodion cell anode material NaxMnO2. The high-temperature solid-phase synthesis method comprises the following steps of 1, dissolving a sodium salt and a manganese salt in water according to a mole ratio of sodium to manganese of 0.44-0.56 to obtain a solution I, 2, dissolving citric acid in water to obtain a solution II, wherein a mole ratio of citric acid to the total metal ions is in a range 0.5-1, 3, dropwisely adding the solution I into the solution II and carrying out stirring for 10-60min, 4, carrying out heating evaporation on the mixed solution at a temperature of 60-90 DEG C to remove a solvent, heating the residues at a temperature of 120 DEG C for 6-24h, cooling the heated residues to a temperature of 10-30 DEG C, and grinding the cooled residues into powder, 5, heating the powder at a temperature of 350-500 DEG C for 3-10h, cooling the powder to a temperature of 10-30 DEG C, and grinding the cooled powder into fine powder, and 6, heating the fine powder at a temperature of 800-950 DEG C for 10-45h, and carrying out cooling to obtain the one-dimensional nano-sodion cell anode material NaxMnO2. The high-temperature solid-phase synthesis method has short synthesis time and a high yield in unit time. The one-dimensional nano-sodion cell anode material NaxMnO2 has uniform, dispersive, thin and long product morphology and good electrochemical properties (of a specific discharge capacity of 114mA.h/g at 0.1C charging-discharging multiplying power).

Description

1-dimention nano sodium-ion battery positive electrode Na xmnO 2high temperature solid phase synthesis
Technical field
The invention belongs to battery material field, be specifically related to a kind of synthetic method of cell positive material.
Background technology
Sodium-ion battery and lithium ion battery have many similarities, and compare with lithium ion battery, and sodium-ion battery has some obvious advantages, and for example cost of material is low and the electrolyte system of the lower decomposition potential of use.Up to the present, for the NaVPO that mainly contains of sodium-ion battery positive electrode 4f, Na xcoO 2, Na xmnO 2laminated crystalline compound and their doped compound.
Na xmnO 2the preparation method of material mainly contains solid phase method, hydro thermal method, sol-gal process etc. at present.Wherein, the manganese source that solid phase method is mainly used is MnCO 3and Mn 2o 3, sodium source is Na 2cO 3reaction temperature is 800-900 ℃, reaction time is less than 12h, but its product pattern all presents inhomogeneous thick club shaped structure and is adhered to one another, particle is too large, easily causes the distance not good and sodium ion diffusion of particle Contact to increase, under 0.1C charge-discharge magnification, product specific discharge capacity is 80mAh/g only, adds only 113mAh/g of specific discharge capacity after carbon nano-tube.And hydro thermal method, in reaction temperature more than 200 ℃, the reaction time can obtain sodium manganese oxygen nano wire and have good chemical property while being 72h, but the reaction time of 72h is oversize, yielding poorly of unit interval, and consumption sodium amount is large (sodium manganese is than being generally greater than 150), be not suitable for industrialized production, in addition, the manganese source Mn that hydro thermal method is used 2o 3and Mn 3o 4also be required to be fine particulate, even if otherwise reaction 72h is also difficult to obtain nano wire.
Summary of the invention
In view of this, the object of the present invention is to provide a kind of high temperature solid-state synthesizing one-dimensional nanometer sodium-ion battery positive electrode Na xmnO 2method, raw material is cheap and easy to get, easy and simple to handle, generated time is short, output is high, cost is low, product chemical property is good, is applicable to large-scale industrialization and produces.
After deliberation, the invention provides following technical scheme:
1. 1-dimention nano sodium-ion battery positive electrode Na xmnO 2high temperature solid phase synthesis, comprise the following steps:
A. by sodium salt and manganese salt, by the mol ratio of sodium and manganese, be 0.44～0.56 soluble in water, obtain I liquid;
B. citric acid is soluble in water, obtain II liquid; Described citric acid is 0.5～1 with the mol ratio of total metal ion;
C. I drop is entered in II liquid, stir 10～60min;
D. step C gained solution is removed to desolventizing in 60 ℃～90 ℃ heating evaporations, residue, in 120 ℃ of heat treated 6～24h, is cooled to 10 ℃～30 ℃, grind into powder;
E. by step D gained powder in 350 ℃～500 ℃ heat treated 3～10h, be cooled to 10 ℃～30 ℃, grind into powder;
F. by step e gained powder in 800 ℃～950 ℃ heat treated 10～45h, cooling, make 1-dimention nano sodium-ion battery positive electrode Na xmnO 2.
The prerequisite that manganese salt and sodium salt are selected is melting or decomposition within the scope of 1000 ℃.Preferably, the salt of manganese described in steps A is manganese nitrate or manganese chloride; Described sodium salt is sodium nitrate, NaOH, sodium acetate or sodium carbonate.Preferred, the salt of manganese described in steps A is manganese nitrate; Described sodium salt is sodium nitrate.
Preferably, in steps A, the mol ratio of sodium and manganese is 0.45～0.54.
Preferably, the consumption of citric acid described in step B is 1 with the mol ratio of total metal ion.
In steps A, in I liquid and step B, the concentration of II liquid, without specific (special) requirements, is dissolved as long as all reagent is whole.
In step D, by residue, in 120 ℃ of heat treated, be in order to prepare desiccant gel presoma; In step e, by powder, in 350 ℃～500 ℃ heat treated, be in order to remove the chelating agent in presoma, and the impulse force that utilizes chelating agent gasification to produce that system is mixed to get is more even; In step F, by powder, in 800 ℃～950 ℃ heat treated, be in order to obtain required phase, because cannot obtain at low temperatures 1-dimention nano sodium-ion battery positive electrode Na xmnO 2.
Preferably, in step F by step e gained powder in 850 ℃～900 ℃ heat treated 15h.
As the preferred technical solution of the present invention one, 1-dimention nano sodium-ion battery positive electrode Na xmnO 2high temperature solid phase synthesis comprise the following steps:
A. by sodium salt and manganese salt, by the mol ratio of sodium and manganese, be 0.45 soluble in water, obtain I liquid;
B. citric acid is soluble in water, obtain II liquid; Described citric acid is 1 with the mol ratio of total metal ion;
C. I drop is entered in II liquid, stir 10min;
D. step C gained solution is removed to desolventizing in 90 ℃ of heating evaporations, residue, in 120 ℃ of heat treated 24h, is cooled to 10 ℃～30 ℃, grind into powder;
E. by step D gained powder in 450 ℃ of heat treated 6h, be cooled to 10 ℃～30 ℃, grind into powder;
F. by step e gained powder in 900 ℃ of heat treated 15h, cooling, make 1-dimention nano sodium-ion battery positive electrode Na xmnO 2.
As the preferred technical solution of the present invention two, 1-dimention nano sodium-ion battery positive electrode Na xmnO 2high temperature solid phase synthesis comprise the following steps:
A. by sodium salt and manganese salt, by the mol ratio of sodium and manganese, be 0.54 soluble in water, obtain I liquid;
B. citric acid is soluble in water, obtain II liquid; Described citric acid is 1 with the mol ratio of total metal ion;
C. I drop is entered in II liquid, stir 10min;
D. step C gained solution is removed to desolventizing in 80 ℃ of heating evaporations, residue, in 120 ℃ of heat treated 12h, is cooled to 10 ℃～30 ℃, grind into powder;
E. by step D gained powder in 400 ℃ of heat treated 3h, be cooled to 10 ℃～30 ℃, grind into powder;
F. by step e gained powder in 850 ℃ of heat treated 15h, cooling, make 1-dimention nano sodium-ion battery positive electrode Na xmnO 2.
Beneficial effect of the present invention is: the present invention is using citric acid as chelating agent first for the synthesis of 1-dimention nano sodium-ion battery positive electrode Na xmnO 2, by the chelating of citric acid and metal ion, realize system in the even mixing of atomic level.With respect to traditional solid phase method and sol-gal process, adopt the synthetic 1-dimention nano sodium-ion battery positive electrode Na of the inventive method xmnO 2pattern more evenly, dispersion, thin, long, do not need can obtain good chemical property (under 0.1C charge-discharge magnification, specific discharge capacity is 114mAh/g) with carbon nano-tube is compound; With respect to hydro thermal method, the generated time of the inventive method shortens greatly, and the output of unit interval is high, and consumption sodium amount obviously declines.
Accompanying drawing explanation
In order to make object of the present invention, technical scheme and beneficial effect clearer, the invention provides following accompanying drawing and describe:
Fig. 1 is the scanning electron microscope (SEM) photograph of embodiment 1 products obtained therefrom, and upper right corner block diagram is partial enlarged drawing.
Fig. 2 is the scanning electron microscope (SEM) photograph of embodiment 2 products obtained therefroms, and upper right corner block diagram is partial enlarged drawing.
Fig. 3 is embodiment 1(dotted line) and embodiment 2(solid line) X-ray diffractogram of products obtained therefrom.
Fig. 4 is the charging and discharging curves of embodiment 2 products obtained therefroms under 0.1C constant current.
Embodiment
Below in conjunction with accompanying drawing, the preferred embodiments of the present invention are described in detail.The experimental technique of unreceipted actual conditions in preferred embodiment, conventionally according to normal condition, or the condition of advising according to reagent manufacturer is carried out.
Embodiment 1,1-dimention nano sodium-ion battery positive electrode Na xmnO 2synthetic
Get 11.6ml50% (w/w) Mn (NO 3) 2solution and 2.295g NaNO 3be dissolved in 18ml deionized water, stir and make abundant dissolving, obtain I liquid; Get 14.795g citric acid and be dissolved in 24.6ml deionized water, obtain II liquid; I liquid is slowly splashed in II liquid, stir 10min, 90 ℃ of heating evaporations are except desolventizing, and residue goes to heat treated 24h in 120 ℃ of baking ovens, be cooled to room temperature, grind into powder, gained powder continues at 450 ℃ of heat treated 6h, is cooled to room temperature, grind into powder, again by gained powder in 900 ℃ of heat treated 15h, be cooled to room temperature, obtain final products.
As shown in Figure 1, degree of crystallinity is very high for the pattern of final products, is laminar, can see the existence of nano wire; Component analysis result as shown in Fig. 3 (dotted line), Na xmnO 2in x be 0.44.
Embodiment 2,1-dimention nano sodium-ion battery positive electrode Na xmnO 2synthetic
Get 11.6ml50% (w/w) Mn (NO 3) 2solution and 1.912g NaNO 3be dissolved in 15ml deionized water, stir and make abundant dissolving, obtain I liquid; Get 13.930g citric acid and be dissolved in 23ml deionized water, obtain II liquid; I liquid is slowly splashed in II liquid, stir 10min, 80 ℃ of heating evaporations are except desolventizing, and residue goes to heat treated 12h in 120 ℃ of baking ovens, be cooled to room temperature, grind into powder, gained powder continues at 400 ℃ of heat treated 3h, is cooled to room temperature, grind into powder, again gained powder is processed to 15h in 850 ℃, be cooled to room temperature, obtain final products.
The pattern of final products as shown in Figure 2, is uniform super-thin sheet-shaped; Component analysis result as shown in Fig. 3 (solid line), Na xmnO 2in x be 0.44.
The preparation of embodiment 3, battery and 1-dimention nano sodium-ion battery positive electrode Na xmnO 2electrochemical property test
Get embodiment 2 products obtained therefroms and conductive black, PVDF binding agent mixes with mass ratio 80:10:10, add a certain amount of 1-Methyl-2-Pyrrolidone (NMP), with agate mortar, grind to form pasty state, be coated in again on the aluminium foil that diameter is 12mm, the every about 1mg of active material load capacity left and right, put dry 12h in 120 ℃ of vacuum drying chambers, be cooled to 40 ℃ of following rear taking-ups and weigh, be transferred in argon gas glove box and wait to assemble.Button cell model is CR2025, and negative pole is sodium sheet, and barrier film is Celgard2325, and electrolyte is 1M NaClO 4solution (solvent is EC and the DMC of volume ratio 1:1).It is above to be measured that the battery of having assembled is placed 6h.Electro-chemical test carries out on Land test macro.Voltage range is 2～4V, and size of current is 0.1C.As shown in Figure 4, under 0.1C charge-discharge magnification, the specific discharge capacity of battery is 114mAh/g to result, illustrates and adopts the synthetic 1-dimention nano sodium-ion battery positive electrode Na of the inventive method xmnO 2there is good chemical property.
Finally explanation is, above preferred embodiment is only unrestricted in order to technical scheme of the present invention to be described, although the present invention is described in detail by above preferred embodiment, but those skilled in the art are to be understood that, can to it, make various changes in the form and details, and not depart from the claims in the present invention book limited range.

Claims (8)

1. 1-dimention nano sodium-ion battery positive electrode Na xmnO 2high temperature solid phase synthesis, it is characterized in that, comprise the following steps:
A. by sodium salt and manganese salt, by the mol ratio of sodium and manganese, be 0.44～0.56 soluble in water, obtain I liquid;
B. citric acid is soluble in water, obtain II liquid; Described citric acid is 0.5～1 with the mol ratio of total metal ion;
C. I drop is entered in II liquid, stir 10～60min;
D. step C gained solution is removed to desolventizing in 60 ℃～90 ℃ heating evaporations, residue, in 120 ℃ of heat treated 6～24h, is cooled to 10 ℃～30 ℃, grind into powder;
E. by step D gained powder in 350 ℃～500 ℃ heat treated 3～10h, be cooled to 10 ℃～30 ℃, grind into powder;
F. by step e gained powder in 800 ℃～950 ℃ heat treated 10～45h, cooling, obtain 1-dimention nano sodium-ion battery positive electrode Na xmnO 2.
2. 1-dimention nano sodium-ion battery positive electrode Na as claimed in claim 1 xmnO 2high temperature solid phase synthesis, it is characterized in that, the salt of manganese described in steps A is manganese nitrate or manganese chloride; Described sodium salt is sodium nitrate, NaOH, sodium acetate or sodium carbonate.
3. 1-dimention nano sodium-ion battery positive electrode Na as claimed in claim 2 xmnO 2high temperature solid phase synthesis, it is characterized in that, the salt of manganese described in steps A is manganese nitrate; Described sodium salt is sodium nitrate.
4. 1-dimention nano sodium-ion battery positive electrode Na as claimed in claim 1 xmnO 2high temperature solid phase synthesis, it is characterized in that, in steps A, the mol ratio of sodium and manganese is 0.45～0.54.
5. 1-dimention nano sodium-ion battery positive electrode Na as claimed in claim 1 xmnO 2high temperature solid phase synthesis, it is characterized in that, the consumption of citric acid described in step B is 1 with the mol ratio of total metal ion.
6. 1-dimention nano sodium-ion battery positive electrode Na as claimed in claim 1 xmnO 2high temperature solid phase synthesis, it is characterized in that, in step F by step e gained powder in 850 ℃～900 ℃ heat treated 15h.
7. the 1-dimention nano sodium-ion battery positive electrode Na as described in claim 1 to 6 any one xmnO 2high temperature solid phase synthesis, it is characterized in that, comprise the following steps:
A. by sodium salt and manganese salt, by the mol ratio of sodium and manganese, be 0.45 soluble in water, obtain I liquid;
B. citric acid is soluble in water, obtain II liquid; Described citric acid is 1 with the mol ratio of total metal ion;
C. I drop is entered in II liquid, stir 10min;
D. step C gained solution is removed to desolventizing in 90 ℃ of heating evaporations, residue, in 120 ℃ of heat treated 24h, is cooled to 10 ℃～30 ℃, grind into powder;
E. by step D gained powder in 450 ℃ of heat treated 6h, be cooled to 10 ℃～30 ℃, grind into powder;
F. by step e gained powder in 900 ℃ of heat treated 15h, cooling, obtain 1-dimention nano sodium-ion battery positive electrode Na xmnO 2.
8. the 1-dimention nano sodium-ion battery positive electrode Na as described in claim 1 to 6 any one xmnO 2high temperature solid phase synthesis, it is characterized in that, comprise the following steps:
A. by sodium salt and manganese salt, by the mol ratio of sodium and manganese, be 0.54 soluble in water, obtain I liquid;
B. citric acid is soluble in water, obtain II liquid; Described citric acid is 1 with the mol ratio of total metal ion;
C. I drop is entered in II liquid, stir 10min;
D. step C gained solution is removed to desolventizing in 80 ℃ of heating evaporations, residue, in 120 ℃ of heat treated 12h, is cooled to 10 ℃～30 ℃, grind into powder;
E. by step D gained powder in 400 ℃ of heat treated 3h, be cooled to 10 ℃～30 ℃, grind into powder;
F. by step e gained powder in 850 ℃ of heat treated 15h, cooling, obtain 1-dimention nano sodium-ion battery positive electrode Na xmnO 2.
CN201310633362.XA 2013-11-29 2013-11-29 High-temperature solid-phase synthesis method of one-dimensional nano-sodion cell anode material NaxMnO2 Pending CN103594707A (en)

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CN104112858A (en) * 2014-06-26 2014-10-22 西南大学 Preparation method and application of network structure nano NaVPO4F/C composite material and application thereof
CN106575744A (en) * 2014-08-08 2017-04-19 住友电气工业株式会社 Positive electrode for sodium ion secondary cell, and sodium ion secondary cell
CN108140826A (en) * 2015-05-26 2018-06-08 尤米科尔公司 To cathode material of the sodium manganese oxide doping divalent metal as sodium-ion battery
CN107045948A (en) * 2017-04-11 2017-08-15 南京理工大学 NaxMnO2Positive electrode, preparation method and applications
CN107093739A (en) * 2017-05-08 2017-08-25 东北大学 Kalium ion battery positive electrode potassium Mn oxide and preparation method thereof
CN107093739B (en) * 2017-05-08 2020-07-21 东北大学 Potassium manganese oxide for potassium ion battery anode material and preparation method thereof
CN106946238A (en) * 2017-05-19 2017-07-14 西南大学 A kind of vanadium phosphate manganese sodium electrode material and its preparation method and application
CN106946238B (en) * 2017-05-19 2018-12-28 西南大学 A kind of vanadium phosphate manganese sodium electrode material and its preparation method and application
CN107946564A (en) * 2017-11-16 2018-04-20 武汉理工大学 Rich sodium manganese base Na4Mn2O5/Na0.7MnO2Composite material and its preparation method and application
CN108615932A (en) * 2018-03-30 2018-10-02 南京大学 Negative and positive double ion rocking chair type secondary cell and preparation method thereof
CN109346329A (en) * 2018-10-15 2019-02-15 吉首大学 A kind of water system sodium ion mixed capacitor and preparation method thereof
CN109216039A (en) * 2018-10-15 2019-01-15 吉首大学 A kind of Na2Mn5O10The preparation method and application of nanometer rods
CN109659520A (en) * 2018-12-07 2019-04-19 北京化工大学 A kind of preparation of sodium ion energy storage device positive and negative electrode material and its symmetrical energy storage device
CN109659520B (en) * 2018-12-07 2022-05-10 北京化工大学 Application of battery material in positive electrode and negative electrode of sodium ion battery
CN109638278A (en) * 2018-12-14 2019-04-16 桑顿新能源科技有限公司 Sodium-ion battery positive material and preparation method thereof and sodium-ion battery
CN109638278B (en) * 2018-12-14 2023-08-22 桑顿新能源科技有限公司 Sodium ion battery positive electrode material, preparation method thereof and sodium ion battery
CN110504437A (en) * 2019-08-30 2019-11-26 浙江大学山东工业技术研究院 A kind of coated porous sodium manganate composite material and preparation method of polypyrrole and application
CN111584874A (en) * 2020-05-28 2020-08-25 西安建筑科技大学 Sodium ion battery positive electrode material based on nanofiber framework and preparation method and application thereof
CN114180633A (en) * 2020-09-15 2022-03-15 中国科学院大连化学物理研究所 Preparation method and application of sodium manganate
CN114180633B (en) * 2020-09-15 2022-09-23 中国科学院大连化学物理研究所 Preparation method and application of sodium manganate

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