CN114725382A - Mg-doped sodium ferric phosphate fluoride material for sodium ion battery and preparation method thereof - Google Patents
Mg-doped sodium ferric phosphate fluoride material for sodium ion battery and preparation method thereof Download PDFInfo
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- CN114725382A CN114725382A CN202110005297.0A CN202110005297A CN114725382A CN 114725382 A CN114725382 A CN 114725382A CN 202110005297 A CN202110005297 A CN 202110005297A CN 114725382 A CN114725382 A CN 114725382A
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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
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
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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
- 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
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—Positive electrodes
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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 invention relates to the technical field of novel energy storage materials, and discloses a Mg-doped sodium ferric phosphate fluoride material for a sodium ion battery and a preparation method thereof, 1) mixing sodium bicarbonate, ferrous oxalate, sodium fluoride, ammonium dihydrogen phosphate and a magnesium source; 2) ball-milling the mixture A with absolute ethyl alcohol or deionized water to obtain a material B, and ball-milling for 18-36 h; putting the ball-milled product into a high-temperature furnace, wherein the ball-milling container is selected from one of an agate ball-milling tank and a polyurethane ball-milling tank; 3) the Mg-doped sodium iron phosphate fluoride material for the sodium ion battery and the preparation method thereof are mixed and prepared according to various proportions, and high-temperature sintering and low-temperature cooling are carried out according to corresponding, so that the high-rate performance is obtained, the solid-phase reaction is adopted, the preparation process is simple, and the material B is suitable for large-scale industrial production.
Description
Technical Field
The invention relates to the technical field of novel energy storage materials, in particular to an Mg-doped sodium iron phosphate fluoride material for a sodium ion battery and a preparation method thereof.
Background
The energy economy based on traditional energy sources presents serious problems such as: the resource is in short supply, the environment is polluted, and the like, so that more new energy sources such as: wind energy, solar energy, biomass energy, geothermal energy, and the like; but factors such as time, space and climate limit the large-scale development and utilization of renewable energy sources, and the novel energy sources have the problems of uneven efficiency distribution, storage and the like. There is therefore a need for new renewable energy utilization by means of more efficient energy conversion and storage devices. In all electrochemical systems, the lithium ion battery in the secondary battery can perform efficient energy conversion and storage, can provide stable power supply, meets the high requirements of electric equipment and the like, and thus realizes sustainable development and utilization of renewable energy. However, in nature, the content of lithium element is very small, only 0.006% of earth element is contained, and the price is continuously increased, while the content of sodium element can reach 2.74%, and the price is low, so that the realization of industrialization of high-performance sodium-ion batteries has great strategic significance.
The preparation of the positive electrode material of the sodium ion battery is particularly important, but the radius of sodium ions is large, and the migration speed of the sodium ions in the charging and discharging process is slow, so that the preparation becomes one of the factors restricting the development of the sodium ion battery; in the sodium iron phosphate fluoride, fluorine ions have a strong induction effect, so that electron cloud forming bonds can be deviated, molecules can be polarized, although the voltage of an active redox pair can be increased by the induction effect, the migration rate of sodium ions is limited, therefore, the rate capability of the sodium iron phosphate fluoride is poor, the Mg-doped sodium iron phosphate fluoride weakens the induction effect through a lattice structure, the migration resistance of sodium ions is reduced, and the rate capability of the sodium iron phosphate fluoride is improved, so that the intrinsic defect of the sodium iron phosphate fluoride material is improved, the Mg-doped sodium iron phosphate fluoride material has a chemical formula of Na X Fe Y Z PO 4F, wherein X is more than or equal to 1.8 and less than or equal to 2.5, and Y + Z is more than or equal to 0.9 and less than or equal to 1.1; the material has good rate performance, and has the other remarkable advantage of being synthesized by solid-phase reaction, simple in synthesis process and suitable for batch production.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides the Mg-doped sodium iron phosphate fluoride material for the sodium ion battery and the preparation method thereof, which have the advantages of good rate performance and cycle performance and solve the problem of reducing the migration resistance of sodium ions.
(II) technical scheme
In order to achieve the purpose of thoroughly driving off formaldehyde, the invention provides the following technical scheme: a Mg-doped sodium ferric phosphate fluoride material for a sodium ion battery and a preparation method thereof are disclosed, wherein the molecular formula of the material is Na X Fe Y Mg Z PO 4F, wherein X is more than or equal to 1.8 and less than or equal to 2.5, and Y + Z is more than or equal to 0.9 and less than or equal to 1.1.
The preparation method comprises the following steps:
1) mixing sodium bicarbonate, ferrous oxalate, sodium fluoride, ammonium dihydrogen phosphate and a magnesium source until the molar ratio of the sodium bicarbonate, the ferrous oxalate, the sodium fluoride, the ammonium dihydrogen phosphate and the doped magnesium source is respectively 0.8-1.5: 0.8-0.98: 1: 1: 0.005-0.15; keeping the stirring direction clockwise in the mixing process, and stirring for 10-15 min by using a special glass rod to stir uniformly;
2) ball-milling the mixed material A and absolute ethyl alcohol or deionized water to obtain a material B, and ball-milling for 18-36 h; putting the ball-milled product into a high-temperature furnace, wherein the ball-milling container is selected from one of an agate ball-milling tank and a polyurethane ball-milling tank, and the balance and stability of the material B are kept in the sintering process to prevent sintering errors caused by inclination caused by shaking;
3) and after vacuum drying the material B, placing the material B in an atmosphere furnace, sintering the material B for 4-6 hours at 550-700 ℃ in an inert atmosphere, cooling the material B to obtain Mg-doped sodium ferric phosphate fluoride, wherein the cooling is carried out in a sealed cold control chamber, so that the instability caused by air flow can be effectively prevented.
Further, in the step 1), the type of the magnesium source is MgO, Mg (OH)2、Mg2(OH)2CO3、MgCO3、Mg(NO3)2、MgCl2、Mg(HCO3)2、Mg(ClO)2、MgC2O4One or more of them.
Further, sintering in the step 3) under an inert atmosphere, heating at a heating rate of 10-30 ℃/min, and baking at a constant temperature of 450-750 ℃ for 10-60min, wherein a container made of porcelain is selected for storage in the sintering process.
Further, in the step 3), the inert gas is one or a mixture of several of nitrogen, argon and hydrogen, and is cooled to room temperature at a cooling rate of 10-30 ℃/min, and the nitrogen, argon and hydrogen are inactive in chemical properties and can only be reacted at high temperature.
Further, the Mg-doped sodium iron phosphate fluoride material obtained by the preparation method of any one of claims 1 to 4 is prepared, and each step is strictly operated according to standard dosage.
(III) advantageous effects
Compared with the prior art, the invention provides the Mg-doped sodium ferric phosphate fluoride material for the sodium ion battery and the preparation method thereof, and the Mg-doped sodium ferric phosphate fluoride material has the following beneficial effects:
1. the Mg-doped sodium ferric phosphate fluoride material for the sodium ion battery and the preparation method thereof are prepared by mixing in various proportions and sintering at high temperature and cooling at low temperature correspondingly, so that the material has good rate capability, adopts solid-phase reaction, has simple preparation process and is suitable for large-scale industrial production.
2. The Mg-doped ferric sodium phosphate fluoride material for the sodium ion battery weakens the induction effect through a lattice structure, reduces the migration resistance of sodium ions and further improves the rate capability of the ferric sodium phosphate fluoride.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, rather than all embodiments, and all other embodiments obtained by a person of ordinary skill in the art without creative efforts based on the embodiments of the present invention belong to the protection scope of the present invention.
The first embodiment is as follows:
a Mg-doped sodium ferric phosphate fluoride material for a sodium ion battery and a preparation method thereof are disclosed, wherein the molecular formula of the material is Na X Fe Y Mg Z PO 4F, wherein X is more than or equal to 1.8 and less than or equal to 2.5, and Y + Z is more than or equal to 0.9 and less than or equal to 1.1.
The preparation method comprises the following steps:
1) and mixing sodium bicarbonate, ferrous oxalate, sodium fluoride, ammonium dihydrogen phosphate and a magnesium source until the molar ratio of the sodium bicarbonate, the ferrous oxalate, the sodium fluoride, the ammonium dihydrogen phosphate and the doped magnesium source is respectively 0.8: 0.8: 1: 1: 0.005; keeping the stirring direction clockwise in the mixing process, and stirring for 10-15 min by using a special glass rod to stir uniformly;
2) ball-milling the mixed material A with absolute ethyl alcohol or deionized water to obtain a material B, and ball-milling for 18 hours; putting the ball-milled product into a high-temperature furnace, wherein the ball-milling container is selected from one of an agate ball-milling tank and a polyurethane ball-milling tank, and the balance and stability of the material B are kept in the sintering process to prevent sintering errors caused by inclination caused by shaking;
3) after the material B is dried in vacuum, the material B is placed in an atmosphere furnace, and is sintered for 4 hours at 550 ℃ under inert atmosphere, Mg-doped sodium ferric phosphate fluoride is obtained after cooling, and cooling needs to be carried out in a sealed cold control chamber, so that instability caused by air flow can be effectively prevented.
Further, in the step 1), the type of the magnesium source is MgO, Mg (OH)2、Mg2(OH)2CO3、MgCO3、Mg(NO3)2、MgCl2、Mg(HCO3)2、Mg(ClO)2、MgC2O4One or more of them.
Further, sintering in the step 3) under an inert atmosphere, heating at a heating rate of 10 ℃/min, and baking at a constant temperature of 450 ℃ for 10min, wherein a container made of porcelain is selected for storage in the sintering process.
Further, in the step 3), the inert gas is one or a mixture of several of nitrogen, argon and hydrogen, and is cooled to room temperature at a cooling rate of 10 ℃/min, and the nitrogen, argon and hydrogen are inactive in chemical properties and can only react at high temperature.
Further, the Mg-doped sodium iron phosphate fluoride material obtained by the preparation method of any one of claims 1 to 4 is prepared, and each step is strictly operated according to standard dosage.
Example two:
a Mg-doped sodium ferric phosphate fluoride material for a sodium ion battery and a preparation method thereof are disclosed, wherein the molecular formula of the material is Na X Fe Y Mg Z PO 4F, wherein X is more than or equal to 1.8 and less than or equal to 2.5, and Y + Z is more than or equal to 0.9 and less than or equal to 1.1.
The preparation method comprises the following steps:
1) and mixing sodium bicarbonate, ferrous oxalate, sodium fluoride, ammonium dihydrogen phosphate and a magnesium source until the molar ratio of the sodium bicarbonate, the ferrous oxalate, the sodium fluoride, the ammonium dihydrogen phosphate and the doped magnesium source is 1.2: 0.93: 1: 1: 0.11; keeping the stirring direction clockwise in the mixing process, and stirring for 13min by using a special glass rod to stir uniformly;
2) ball-milling the mixed material A with absolute ethyl alcohol or deionized water to obtain a material B, and ball-milling for 24 hours; putting the ball-milled product into a high-temperature furnace, wherein the ball-milling container is selected from one of an agate ball-milling tank and a polyurethane ball-milling tank, and the balance and stability of the material B are kept in the sintering process to prevent sintering errors caused by inclination caused by shaking;
3) and after the material B is dried in vacuum, placing the material B in an atmosphere furnace, sintering the material B for 5 hours at the temperature of 620 ℃ under the inert atmosphere, cooling the material B to obtain Mg-doped sodium ferric phosphate fluoride, wherein the cooling is carried out in a sealed cold control chamber, so that the instability caused by air flow can be effectively prevented.
Further, in the step 1), the type of the magnesium source is MgO, Mg (OH)2、Mg2(OH)2CO3、MgCO3、Mg(NO3)2、MgCl2、Mg(HCO3)2、Mg(ClO)2、MgC2O4One or more of them.
Further, sintering in the step 3) under an inert atmosphere, heating at a heating rate of 20 ℃/min, and roasting at a constant temperature of 600 ℃ for 30min, wherein a container made of porcelain is selected for storage in the sintering process.
Further, in the step 3), the inert gas is one or a mixture of several of nitrogen, argon and hydrogen, and is cooled to room temperature at a cooling rate of 20 ℃/min, and the nitrogen, argon and hydrogen are inactive in chemical properties and can only react at high temperature.
Further, the Mg-doped sodium iron phosphate fluoride material obtained by the preparation method of any one of claims 1 to 4 is prepared, and each step is strictly operated according to standard dosage.
Example three:
the molecular formula of the material is Na X Fe Y Mg Z PO 4F, wherein X is more than or equal to 1.8 and less than or equal to 2.5, and Y + Z is more than or equal to 0.9 and less than or equal to 1.1.
The preparation method comprises the following steps:
1) mixing sodium bicarbonate, ferrous oxalate, sodium fluoride, ammonium dihydrogen phosphate and a magnesium source until the molar ratio of the sodium bicarbonate, the ferrous oxalate, the sodium fluoride, the ammonium dihydrogen phosphate and the doped magnesium source is 1.5 respectively; 0.98: 1: 1: 0.15; keeping the stirring direction clockwise in the mixing process, and stirring for 15min by using a special glass rod to stir uniformly;
2) ball-milling the mixed material A with absolute ethyl alcohol or deionized water to obtain a material B, and ball-milling for 36 hours; putting the ball-milled product into a high-temperature furnace, wherein the ball-milling container is selected from one of an agate ball-milling tank and a polyurethane ball-milling tank, and the balance and stability of the material B are kept in the sintering process to prevent sintering errors caused by inclination caused by shaking;
3) and after the material B is dried in vacuum, placing the material B in an atmosphere furnace, sintering the material B for 6 hours at 700 ℃ in an inert atmosphere, cooling the material B to obtain Mg-doped sodium ferric phosphate fluoride, wherein the cooling is carried out in a sealed cold control chamber, so that the instability caused by air flow can be effectively prevented.
Further, in the step 1), the magnesium source is of the typeMgO、Mg(OH)2、Mg2(OH)2CO3、MgCO3、Mg(NO3)2、MgCl2、Mg(HCO3)2、Mg(ClO)2、MgC2O4One or more of them.
Further, sintering in the step 3) under an inert atmosphere, heating at a heating rate of 30 ℃/min, and roasting at a constant temperature of 750 ℃ for 60min, wherein a container made of porcelain is selected for storage in the sintering process.
Further, in the step 3), the inert gas is one or a mixture of several of nitrogen, argon and hydrogen, and is cooled to room temperature at a cooling rate of 30 ℃/min, and the nitrogen, argon and hydrogen are inactive in chemical properties and can only be reacted at high temperature.
Further, the Mg-doped sodium iron phosphate fluoride material obtained by the preparation method of any one of claims 1 to 4 is prepared, and each step is strictly operated according to standard dosage.
The invention has the beneficial effects that: an Mg-doped sodium ferric phosphate fluoride material for a sodium ion battery and a preparation method thereof, wherein the material is prepared by mixing in various proportions and sintering at high temperature and cooling at low temperature correspondingly, so that the material has good rate capability, adopts solid-phase reaction, has simple preparation process and is suitable for large-scale industrial production; the Mg-doped ferric sodium phosphate fluoride in the sodium ion battery weakens the induction effect and reduces the migration resistance of sodium ions through a lattice structure, thereby improving the rate capability of the ferric sodium phosphate fluoride.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (5)
1. An Mg-doped sodium ferric phosphate fluoride material for a sodium ion battery and a preparation method thereof are characterized in that: the molecular formula of the material is Na X Fe Y Mg Z PO 4F, wherein X is more than or equal to 1.8 and less than or equal to 2.5, and Y + Z is more than or equal to 0.9 and less than or equal to 1.1;
the preparation method comprises the following steps:
1) mixing sodium bicarbonate, ferrous oxalate, sodium fluoride, ammonium dihydrogen phosphate and a magnesium source to obtain a mixed material A;
2) ball-milling the mixture A with absolute ethyl alcohol or deionized water to obtain a material B, and ball-milling for 18-36 h; putting the ball-milled product into a high-temperature furnace;
3) and after vacuum drying the material B, placing the material B in an atmosphere furnace, sintering for 4-6h at 550-700 ℃ in an inert atmosphere, and cooling to obtain Mg-doped sodium ferric phosphate fluoride.
2. The Mg-doped sodium iron phosphate fluoride material for the sodium-ion battery and the preparation method thereof according to claim 1, wherein the Mg-doped sodium iron phosphate fluoride material comprises the following components in percentage by weight: in the step 1), the type of the magnesium source is MgO and Mg (OH)2、Mg2(OH)2CO3、MgCO3、Mg(NO3)2、MgCl2、Mg(HCO3)2、Mg(ClO)2、MgC2O4One or more of them.
3. The Mg-doped sodium iron phosphate fluoride material for the sodium-ion battery and the preparation method thereof according to claim 1, wherein the Mg-doped sodium iron phosphate fluoride material comprises the following components in percentage by weight: sintering in inert atmosphere in step 3), heating at a heating rate of 10-30 ℃/min, and baking at a constant temperature of 450-750 ℃ for 10-60 min.
4. The Mg-doped sodium iron phosphate fluoride material for the sodium-ion battery and the preparation method thereof according to claim 1, wherein the Mg-doped sodium iron phosphate fluoride material comprises the following components in percentage by weight: in the step 3), the inert gas is one or a mixture of several gases of nitrogen, argon and hydrogen, and is cooled to the room temperature at the cooling speed of 10-30 ℃/min.
5. An Mg-doped sodium ferric phosphate fluoride material for a sodium ion battery and a preparation method thereof are characterized in that: the Mg-doped sodium iron phosphate fluoride material prepared by the preparation method of any one of claims 1 to 4.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115566187A (en) * | 2022-11-11 | 2023-01-03 | 上海领钫新能源科技有限公司 | Positive active material for sodium ion battery and preparation method and application thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115566187A (en) * | 2022-11-11 | 2023-01-03 | 上海领钫新能源科技有限公司 | Positive active material for sodium ion battery and preparation method and application thereof |
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Application publication date: 20220708 |