CN108751158A - A kind of preparation method of phosphoric acid ferrisodium nano wire - Google Patents
A kind of preparation method of phosphoric acid ferrisodium nano wire Download PDFInfo
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- CN108751158A CN108751158A CN201810533676.5A CN201810533676A CN108751158A CN 108751158 A CN108751158 A CN 108751158A CN 201810533676 A CN201810533676 A CN 201810533676A CN 108751158 A CN108751158 A CN 108751158A
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- phosphoric acid
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- acid ferrisodium
- iron phosphate
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/45—Phosphates containing plural metal, or metal and ammonium
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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
- H01M4/36—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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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/54—Particles characterised by their aspect ratio, i.e. the ratio of sizes in the longest to the shortest dimension
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- 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 is realized in this way this method includes mainly two steps, the first step first prepares lithium iron phosphate nano line；Lithium iron phosphate nano line prepared by the first step is changed into phosphoric acid ferrisodium nano wire by second step by way of ion exchange；The present invention successfully prepares phosphoric acid ferrisodium nano wire for the first time, and draw ratio is up to 600 or so, has good pattern expansion；Secondly, the present invention after first preparing lithium iron phosphate nano line again by ion exchange by way of the phosphoric acid ferrisodium nano wire for preparing, maintain original olivine-type structure rather than ferrophosphorus sodium mine type well；Finally, which is used for battery testing, it is found that it is showed with good chemical property.
Description
Technical field
The present invention relates to a kind of preparation fields of function nano material, and in particular to a kind of preparation of phosphoric acid ferrisodium nano wire
Method.
Background technology
With the continuous development of economic society, the energy becomes ever more important, and having become today's society can stablize
The foundation stone of development.Wherein, it is the leading role of current energy source use using coal, oil, natural gas as the fossil fuel of representative, accounts for the energy
80% or more of total quantity consumed is generated since these energy have in use after certain non-renewable and use
A large amount of pollutants, this, which to develop a kind of effective energy of cleaning sustainable use, is particularly important.
In this process, the concept of power battery is applied and is given birth to, wherein using lithium ion battery as the power of Typical Representative
Battery has been achieved for certain commercialization successful application at present, and such as the Roaster 2 of tesla, most fast speed per hour reaches 400
Kilometer, course continuation mileage reach 1000 kilometers, this explanation has very wide application by the power battery of representative of lithium ion battery
Foreground, still, lithium source in lithium ion battery is in recent years also with the extensive use of lithium battery, and also increasingly water rises ship price
Height, this aspect are attributed to the great demand amount in market, another side, and essence is also most importantly the lithium because from the point of view of with regard to the whole world
Mine is relatively fewer, and global lithium reserves are also few.
Development one kind can substitute anode material for lithium-ion batteries and be of great significance as a result,.Sodium-ion battery and lithium from
Sub- battery is similar, is all a kind of novel secondary ion battery, all has a wide range of applications, compare in large-scale energy storage field
Lithium mine, sodium mine not only have extensive distribution, and its content higher；Moreover, sodium-ion battery compares lithium ion battery, have
Higher potential, this makes the electrolyte range of choice of sodium-ion battery more extensively, which means that being replaced using sodium-ion battery
There is very strong feasibility for lithium ion battery.
About the research of sodium-ion battery, many progress are also achieved at present, as Chinese patent CN105006548A is public
A kind of method of microwave method synthesis sodium-ion battery positive material NaFePO4 has been opened, it is directly simple and quick using the method for microwave
Synthesize required product, its advantage is that：Energy saving, heating speed is fast, pollution-free, and sample crystal grain refinement, structure are uniform, can be with
It accurately controls.Also such as Chinese patent CN106587000A discloses a kind of preparation method of phosphoric acid ferrisodium nanometer rods, will be anti-
After answering solution to prepare, phosphoric acid ferrisodium nanometer rods have directly been prepared by microwave one-step method, its advantage is that operation it is simple,
Reaction temperature is low, short preparation period, without post-processing and environmentally friendly.For another example Chun Li et al. people exists《Journal of
Materials Chemistry A》On entitled " the Hollow amorphous NaFePO4 nanospheres as a that deliver
High-capacity and high-rate cathode for sodiumion batteries " are about phosphoric acid ferrisodium nanometer
The preparation method of ball has prepared the phosphoric acid ferrisodium nanosphere with excellent electric property by a kind of method of hard template,
The electrode material still has good cyclical stability after the circle of cycle charging 300；In addition, the Seung- of South Korea's Han Yang University
Entitled " the Reversible NaFePO4 electrode for sodium secondary that Min Oh et al. are delivered
The electrode material is used for sodium by the phosphoric acid ferrisodium for preparing olivine-type in batteries " articles by way of ion exchange
When ion battery, it is found that it still has good cyclical stability after the cycle of 50 circles, and its specific capacitance reaches
125mAh/g.These all illustrate that phosphoric acid ferrisodium is used to substitute lithium ion battery with very strong as sodium-ion battery positive material
Feasibility, and the research at present about phosphoric acid ferrisodium is relatively fewer, and further investigation is more a lack of for the controlledly synthesis of its pattern.
Invention content
The purpose of the present invention is to provide a kind of preparation methods of phosphoric acid ferrisodium nano wire, to realize for phosphoric acid ferrisodium shape
The controllable research of looks, the present invention used in reagent it is relatively simple, nontoxic, preparation method is simple, it is easy to accomplish, do not need spy
Different processing, and there is the sodium phosphate Fe nanowire prepared the pattern of expansion and uniform size, draw ratio to be up to 600 left sides
The right side is applied to sodium-ion battery and achieves good chemical property.
In order to achieve the object of the present invention, the invention is realized in this way, this method includes mainly two steps, and the first step is first
Prepare lithium iron phosphate nano line；Second step, lithium iron phosphate nano line prepared by the first step are turned by way of ion exchange
Become phosphoric acid ferrisodium nano wire.
In order to more clearly show that technical scheme of the present invention, the present invention specifically include following steps,
The raw material for preparing LiFePO4 is uniformly mixed by the first step, and the raw material includes source of iron, lithium source, phosphorus source and template；
It is dissolved in solvent specifically, weighing suitable source of iron, lithium source, phosphorus source and template, then carries out hydro-thermal reaction so that described
Reactant carries out well-regulated growth along the hole of template；After growth, by lithium iron phosphate nano line composite mould plate agent
Removed template method operation is carried out, removed template method operation refers to dissolving template using particular agent, obtains target production
Object lithium iron phosphate nano line；After obtaining lithium iron phosphate nano line, alternately washed using a large amount of ethyl alcohol and deionized water, with
The template solvent on surface is removed, the lithium iron phosphate nano line being purified is carried out high temperature sintering in turn, with further
The crystal property of LiFePO4 is improved, and then is conducive to the performance of its chemical property.
Aforementioned obtained lithium iron phosphate nano line is obtained final product phosphoric acid by second step by way of ion exchange
Ferrisodium nano wire, wherein the ion exchange refers to that the lithium iron phosphate nano line being prepared first is prepared into electrode material
Material, is then assembled into battery, is charged to the battery so that the lithium in lithium iron phosphate nano line is all deviate from, and waits for lithium
After abjection, battery is dismantled, by obtained anode electrode piece under argon atmosphere, uses methyl ethyl carbonate（EMC）It is washed, it
Carry out drying and processing under vacuum afterwards；Dry powder is prepared into electrode slice, using metallic sodium as cathode, after battery is made
By can be obtained final product-phosphoric acid ferrisodium nano wire after embedding sodium.
Further, the source of iron in the first step refers to one or more in ferrous sulfate, frerrous chloride or ferrous nitrate；
Lithium source is one or more in lithium carbonate, lithium hydroxide, lithium oxalate or lithium chloride；Phosphorus source refer to phosphoric acid, ammonium dihydrogen phosphate or
One or more of ammonium hydrogen phosphate.
Further, lithium source in the first step：Source of iron：The molar ratio of phosphorus source is 0.5-5:1-2:1.
Further, template refers to anodised aluminium in the first step（AAO）, one kind in SBA-15, ZSM-5.
Further, particular agent refers to one or more of LiOH, NaOH, KOH in the first step.
Further, hydrothermal condition is 150-300 DEG C in the first step, react 5-24h, the high temperature sintering refer to
It is sintered 4-12h at 500-1200 DEG C.
Further, second step intermediate ion exchange in electrode slice prepare refer to using this field routine preparation method into
It is prepared by row.
Compared with prior art, the present invention has following advantageous effects：
First, the present invention successfully prepares phosphoric acid ferrisodium nano wire for the first time, and draw ratio is up to 600 or so, has good shape
Looks expansion；Secondly, the present invention after first preparing lithium iron phosphate nano line again by ion exchange by way of the phosphoric acid for preparing
Ferrisodium nano wire maintains original olivine-type structure rather than ferrophosphorus sodium mine type well；Finally, which is received
Rice noodles are used for battery testing, it is found that it is showed with good chemical property.
Description of the drawings
The low power transmitted electron photo of phosphoric acid ferrisodium nano wire prepared by Fig. 1 present invention；
The high power transmitted electron photo of phosphoric acid ferrisodium nano wire prepared by Fig. 2 present invention.
Specific implementation mode
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings, it is to be understood that described herein
Specific implementation method be not restriction to the application, all technical solutions for not departing from inventive concept of the present invention are in the present invention
Protection domain in.
Embodiment 1
According to Li：Fe：The molar ratio of P is 1：1：1 metering ratio weighs lithium carbonate, ferrous sulfate and phosphoric acid respectively, will weigh
Substance be add to deionized water, form uniform solution, add account for the template SBA-15 of total solution weight 0.5% into
Row is sufficiently stirred, and after mixing, adjusts pH to 9 using pH regulators, then above-mentioned mixed solution is fitted into reaction kettle,
15h is reacted at 180 DEG C, after reaction, cooled to room temperature handles product to remove after filtration washing product with the NaOH of 1M
Template is removed, obtained product is fully washed with deionization and ethyl alcohol, is dried overnight at 80 DEG C later, dry
To powder be sintered 3h at 800 DEG C and obtain lithium iron phosphate nano line；Obtained lithium iron phosphate nano line is first prepared
At electrode slice, it is assembled into after battery and first carries out de- lithium operation, and then carry out embedding sodium operation, you can obtain final product-
Phosphoric acid ferrisodium nano wire.
Embodiment 2
According to Li：Fe：The molar ratio of P is 1：1：1 metering ratio weighs lithium oxalate, frerrous chloride and phosphoric acid respectively, will weigh
Substance be add to deionized water, form uniform solution, add account for the template SBA-15 of total solution weight 1.0% into
Row is sufficiently stirred, and after mixing, adjusts pH to 9 using pH regulators, then above-mentioned mixed solution is fitted into reaction kettle,
12h is reacted at 160 DEG C, after reaction, cooled to room temperature handles product to remove after filtration washing product with the NaOH of 1M
Template is removed, obtained product is fully washed with deionization and ethyl alcohol, is dried overnight at 80 DEG C later, dry
To powder be sintered 3h at 800 DEG C and obtain lithium iron phosphate nano line；Obtained lithium iron phosphate nano line is first prepared
At electrode slice, it is assembled into after battery and first carries out de- lithium operation, and then carry out embedding sodium operation, you can obtain final product-
Phosphoric acid ferrisodium nano wire.
Embodiment 3
According to Li：Fe：The molar ratio of P is 0.8：1：1 metering ratio weighs lithium carbonate, frerrous chloride and ammonium hydrogen phosphate respectively, will
Load weighted substance is add to deionized water, and forms uniform solution, adds the template AAO for accounting for total solution weight 0.5%
It is sufficiently stirred, after mixing, adjusts pH to 10 using pH regulators, above-mentioned mixed solution is then packed into reaction kettle
In, 12h is reacted at 160 DEG C, after reaction, cooled to room temperature, with the NaOH of 1M processing productions after filtration washing product
Object is fully washed to remove template, by obtained product with deionization and ethyl alcohol, is dried overnight at 80 DEG C later,
The powder being dried to obtain is sintered 3h at 800 DEG C and obtains lithium iron phosphate nano line；The lithium iron phosphate nano line that will be obtained
It is first prepared into electrode slice, is assembled into after battery and first carries out de- lithium operation, and then carry out embedding sodium operation, you can obtain final
Product-phosphoric acid ferrisodium nano wire.
Embodiment 4
According to Li：Fe：The molar ratio of P is 1：1：1 metering ratio weighs lithium carbonate, frerrous chloride and ammonium hydrogen phosphate respectively, will claim
Measured substance is add to deionized water, and forms uniform solution, add account for the template AAO of total solution weight 0.8% into
Row is sufficiently stirred, and after mixing, adjusts pH to 10 using pH regulators, then above-mentioned mixed solution is fitted into reaction kettle,
10h is reacted at 200 DEG C, after reaction, cooled to room temperature, after filtration washing product with the NaOH of 1M processing products with
Template is removed, obtained product is fully washed with deionization and ethyl alcohol, is dried overnight at 80 DEG C later, it is dry
Obtained powder is sintered 5h at 700 DEG C and obtains lithium iron phosphate nano line；Obtained lithium iron phosphate nano line is first made
De- lithium operation is first carried out at electrode slice, being assembled into after battery, and then carries out embedding sodium operation, you can obtains final production
Object-phosphoric acid ferrisodium nano wire.
Embodiment 5
According to Li：Fe：The molar ratio of P is 1：1.2：1 metering ratio weighs lithium carbonate, frerrous chloride and ammonium hydrogen phosphate respectively, will
Load weighted substance is add to deionized water, and forms uniform solution, adds the template AAO for accounting for total solution weight 1.0%
It is sufficiently stirred, after mixing, adjusts pH to 10 using pH regulators, above-mentioned mixed solution is then packed into reaction kettle
In, 12h is reacted at 160 DEG C, after reaction, cooled to room temperature, with the NaOH of 1M processing productions after filtration washing product
Object is fully washed to remove template, by obtained product with deionization and ethyl alcohol, is dried overnight at 80 DEG C later,
The powder being dried to obtain is sintered 5h at 700 DEG C and obtains lithium iron phosphate nano line；The lithium iron phosphate nano line that will be obtained
It is first prepared into electrode slice, is assembled into after battery and first carries out de- lithium operation, and then carry out embedding sodium operation, you can obtain final
Product-phosphoric acid ferrisodium nano wire.
Embodiment 6
According to Li：Fe：The molar ratio of P is 1：1：1 metering ratio weighs lithium carbonate, frerrous chloride and ammonium hydrogen phosphate respectively, will claim
Measured substance is add to deionized water, and forms uniform solution, adds the template SBA- for accounting for total solution weight 0.5%
15 are sufficiently stirred, and after mixing, adjust pH to 10 using pH regulators, above-mentioned mixed solution is then packed into reaction kettle
In, 12h is reacted at 160 DEG C, after reaction, cooled to room temperature, with the LiOH of 1M processing productions after filtration washing product
Object is fully washed to remove template, by obtained product with deionization and ethyl alcohol, is dried overnight at 80 DEG C later,
The powder being dried to obtain is sintered 3h at 800 DEG C and obtains lithium iron phosphate nano line；The lithium iron phosphate nano line that will be obtained
It is first prepared into electrode slice, is assembled into after battery and first carries out de- lithium operation, and then carry out embedding sodium operation, you can obtain final
Product-phosphoric acid ferrisodium nano wire.
Embodiment 7
According to Li：Fe：The molar ratio of P is 1：1：1 metering ratio weighs lithium carbonate, frerrous chloride and ammonium hydrogen phosphate respectively, will claim
Measured substance is add to deionized water, and forms uniform solution, adds the template SBA- for accounting for total solution weight 0.5%
15 are sufficiently stirred, and after mixing, adjust pH to 10 using pH regulators, above-mentioned mixed solution is then packed into reaction kettle
In, 12h is reacted at 160 DEG C, after reaction, cooled to room temperature, with the NaOH of 1M processing productions after filtration washing product
Object is fully washed to remove template, by obtained product with deionization and ethyl alcohol, is dried overnight at 80 DEG C later,
The powder being dried to obtain is sintered 3h at 1000 DEG C and obtains lithium iron phosphate nano line；The lithium iron phosphate nano line that will be obtained
It is first prepared into electrode slice, is assembled into after battery and first carries out de- lithium operation, and then carry out embedding sodium operation, you can obtain final
Product-phosphoric acid ferrisodium nano wire.
Claims (7)
1. a kind of preparation method of phosphoric acid ferrisodium nano wire, it is characterised in that：This method includes mainly two steps, and the first step first makes
Lithium iron phosphate nano line is prepared with hydro-thermal method；Lithium iron phosphate nano line prepared by the first step is passed through ion exchange by second step
Mode be changed into phosphoric acid ferrisodium nano wire.
2. a kind of preparation method of phosphoric acid ferrisodium nano wire according to claim 1, it is characterised in that：The first step is that will make
The raw material of standby LiFePO4 is uniformly mixed, and the raw material includes source of iron, lithium source, phosphorus source and template；Specifically, weighing appropriate
Source of iron, lithium source, phosphorus source and template be dissolved in solvent, hydro-thermal reaction is then carried out, after growth, by lithium iron phosphate nano
Line composite mould plate agent carries out removed template method operation, and removed template method operation refers to dissolving template using particular agent
Agent obtains target product lithium iron phosphate nano line.
3. a kind of preparation method of phosphoric acid ferrisodium nano wire according to claim 1, it is characterised in that：Second step be will before
The lithium iron phosphate nano line stated obtains final product phosphoric acid ferrisodium nano wire by way of ion exchange；Wherein, institute
The ion exchange stated refers to that the lithium iron phosphate nano line being prepared first is prepared into electrode material, is then assembled into electricity
It charges to the battery in pond so that the lithium in lithium iron phosphate nano line is all deviate from, and after lithium abjection, battery is dismantled, will
Obtained anode electrode piece uses methyl ethyl carbonate under argon atmosphere（EMC）It is washed, is dried under vacuum later
Dry-cure；Dry powder being prepared into electrode slice, using metallic sodium as cathode, being made after battery by can be obtained most after embedding sodium
Whole product-phosphoric acid ferrisodium nano wire.
4. a kind of preparation method of phosphoric acid ferrisodium nano wire according to claim 1, it is characterised in that：In the first step
Lithium source：Source of iron：The molar ratio of phosphorus source is 0.5-5:1-2:1.
5. a kind of preparation method of phosphoric acid ferrisodium nano wire according to claim 1, it is characterised in that：In the first step
Template refers to anodised aluminium（AAO）, one kind in SBA-15, ZSM-5.
6. a kind of preparation method of phosphoric acid ferrisodium nano wire according to claim 1, it is characterised in that：In the first step
Particular agent refers to one or more of LiOH, NaOH, KOH.
7. a kind of preparation method of phosphoric acid ferrisodium nano wire according to claim 1, it is characterised in that：In the first step
Hydrothermal condition is 150-300 DEG C, reacts 5-24h, the high temperature sintering refers to being sintered 4-12h at 500-1200 DEG C.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114249312A (en) * | 2021-11-26 | 2022-03-29 | 广东邦普循环科技有限公司 | Rod-shaped sodium ion positive electrode material and preparation method and application thereof |
| CN114368736A (en) * | 2022-01-28 | 2022-04-19 | 中南大学 | Preparation method of olivine type sodium iron phosphate cathode material |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106784744A (en) * | 2017-03-02 | 2017-05-31 | 欣旺达电子股份有限公司 | LiFePO4 and preparation method thereof |
-
2018
- 2018-05-29 CN CN201810533676.5A patent/CN108751158A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106784744A (en) * | 2017-03-02 | 2017-05-31 | 欣旺达电子股份有限公司 | LiFePO4 and preparation method thereof |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114249312A (en) * | 2021-11-26 | 2022-03-29 | 广东邦普循环科技有限公司 | Rod-shaped sodium ion positive electrode material and preparation method and application thereof |
| CN114249312B (en) * | 2021-11-26 | 2023-02-14 | 广东邦普循环科技有限公司 | Rod-shaped sodium ion positive electrode material and preparation method and application thereof |
| WO2023093181A1 (en) * | 2021-11-26 | 2023-06-01 | 广东邦普循环科技有限公司 | Rod-shaped sodium ion positive electrode material, preparation method therefor and application thereof |
| GB2621031A (en) * | 2021-11-26 | 2024-01-31 | Guangdong Brunp Recycling Technology Co Ltd | Rod-shaped sodium ion positive electrode material, preparation method therefor and application thereof |
| US11984596B2 (en) | 2021-11-26 | 2024-05-14 | Guangdong Brunp Recycling Technology Co., Ltd | Rod-shaped sodium ion positive electrode material, preparation method therefor and application thereof |
| CN114368736A (en) * | 2022-01-28 | 2022-04-19 | 中南大学 | Preparation method of olivine type sodium iron phosphate cathode material |
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