CN106684435B - A kind of NaFePO4The preparation method of/C nano piece - Google Patents

A kind of NaFePO4The preparation method of/C nano piece Download PDF

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CN106684435B
CN106684435B CN201611229825.6A CN201611229825A CN106684435B CN 106684435 B CN106684435 B CN 106684435B CN 201611229825 A CN201611229825 A CN 201611229825A CN 106684435 B CN106684435 B CN 106684435B
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nafepo
solution
preparation
nano piece
concentration
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CN106684435A (en
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曹丽云
胡海玲
黄剑锋
许占位
李嘉胤
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Shaanxi University of Science and Technology
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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
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • 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
    • 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
    • C01B25/37—Phosphates of heavy metals
    • C01B25/375—Phosphates of heavy metals of iron
    • 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
    • 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
    • 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 discloses a kind of NaFePO4The preparation method of/C nano piece, 1) by Fe2+Soluble salt solutions and phosphatic aqueous solution in molar ratio Fe: P=1: 1 ratio mix, be denoted as solution A；2) sodium oleate solution is instilled in solution A, so that molar ratio Fe: P:Na=1: 1:(1-3), and adjusting pH value is 3-9, obtains suspension；3) mixture is obtained by suspension that step 2) obtains is freeze-dried, and by mixture grind into powder；4) powder for obtaining step 3) carries out calcination processing under an inert atmosphere, it is cooled to room temperature after calcining, products therefrom is filtered after salt acid soak, is then washed till neutrality with water and ethyl alcohol, then vacuum drying treatment is carried out, the NaFePO of nanometer sheet is obtained4/ C-material.The product homogeneity of lithium iron phosphate positive material prepared by the present invention is good, and particle diameter distribution is uniform, stable structure, preferable with compatibility of electrolyte, has good recycling performance.

Description

A kind of NaFePO4The preparation method of/C nano piece
Technical field
The present invention relates to lithium ion battery fields, and in particular to a kind of NaFePO4The preparation method of/C nano piece.
Background technique
Currently, lithium ion battery is development prospect high-energy battery system the brightest and the clearest, but with industries such as number, traffic Lithium ion battery is relied on and is aggravated, limited lithium resource will face shortage problem.The research and development of sodium-ion battery are certain The battery caused by lithium resource shortage can be mitigated in degree develops limitation problem.
Sodium-ion battery has three big outstanding advantages compared with lithium ion battery: 1. raw material resources are abundant, low in cost, distribution Extensively；2. the half-cell potential of sodium-ion battery 0.3~0.4V high compared with lithium ion potential can utilize the lower electricity of decomposition potential It solves matter solvent and electrolytic salt, the range of choice of electrolyte is wider；3. sode cell has metastable chemical property, using more Add safety.
In sodium-ion battery positive material, phosphate material is due to high voltage capability and thermal stability, it is likely that The positive electrode optimal as sodium-ion battery.Preparation NaFePO at present4The method of material has solid-phase synthesis, coprecipitation Deng.But the Solid phase synthesis time is long, particle is uneven and impurity phase easily occurs, and the Co deposited synthesis period is longer.
Summary of the invention
The purpose of the present invention is to provide a kind of NaFePO4The preparation method of/C nano piece, to overcome the above-mentioned prior art Existing defect, the present invention prepared by lithium iron phosphate positive material product homogeneity it is good, particle diameter distribution is uniform, and structure is steady It is fixed, it is preferable with compatibility of electrolyte, there is good recycling performance.
In order to achieve the above objectives, the present invention adopts the following technical scheme:
A kind of NaFePO4The preparation method of/C nano piece, comprising the following steps:
1) by Fe2+Soluble salt solutions and phosphatic aqueous solution in molar ratio Fe: P=1: 1 ratio mix, be denoted as Solution A；
2) sodium oleate solution is instilled in solution A, so that molar ratio Fe: P:Na=1: 1:(1-3), and adjusting pH value is 3- 9, obtain suspension；
3) mixture is obtained by suspension that step 2) obtains is freeze-dried, and by mixture grind into powder；
4) powder for obtaining step 3) carries out calcination processing under an inert atmosphere, is cooled to room temperature after calcining, will Products therefrom filters after salt acid soak, is then washed till neutrality with water and ethyl alcohol, then carries out vacuum drying treatment, obtains nanometer The NaFePO of piece4/ C-material.
Further, the Fe in step 1)2+Soluble-salt be FeC2O4、FeCl2Or FeSO4。
Further, the Fe in step 1)2+Soluble salt solutions concentration and the concentration of phosphate aqueous solution be 1- 10mol/L。
Further, the phosphate in step 1) is ammonium phosphate, ammonium hydrogen phosphate or ammonium dihydrogen phosphate.
Further, the concentration of sodium oleate solution is 1-3mol/L in step 2).
Further, pH is adjusted using ammonium hydroxide in step 2), and ammonia concn is 2-4mol/L.
Further, sublimation drying is 8h in step 3).
Further, inert atmosphere is Ar or N in step 4)2Atmosphere.
Further, calcination temperature is 500-800 DEG C in step 4), calcination time 2-12h.
Further, in step 4) vacuum drying treatment be under the conditions of temperature is 60~100 DEG C, vacuum drying 6~ 12h。
Compared with prior art, the invention has the following beneficial technical effects:
The method for preparing phosphoric acid ferrisodium positive electrode of the invention has following outstanding feature: (1) original used Material source is extensive, cheap, at low cost, and substitute is more；(2) enuatrol not only there is soft template to make in the present invention With, and carbon source is provided, and can effectively prevent Fe in product2+It is oxidized to Fe3+, simple process is easy to control and operates, and pacifies Full property and stability are good, Yi Shixian industrial-scale production.
Further, the present invention is by control reaction condition, and obtained phosphoric acid ferrisodium positive electrode product purity is high, tool There are good chemical property and processing performance, and the product homogeneity of prepared lithium iron phosphate positive material is good, partial size It is evenly distributed, stable structure is preferable with compatibility of electrolyte, has good recycling performance.
Detailed description of the invention
Fig. 1 is that ferric phosphate prepared by the embodiment of the present invention 1 receives the XRD diagram of material；
Fig. 2 be the embodiment of the present invention 1 prepare ferric phosphate receive material SEM figure；
Fig. 3 be the embodiment of the present invention 1 prepare ferric phosphate receive material assembling half-cell cycle performance figure.
Specific embodiment
The invention will be described in further detail below:
A kind of NaFePO4The preparation method of/C nano piece, comprising the following steps:
1) be by concentration 1-10mol/L Fe2+Soluble salt solutions and phosphatic aqueous solution in molar ratio Fe: P =1: 1 ratio mixing, is denoted as solution A, wherein Fe2+Soluble-salt be FeC2O4、 FeCl2Or FeSO4, phosphate is phosphorus Sour ammonium, ammonium hydrogen phosphate or ammonium dihydrogen phosphate；
2) sodium oleate solution that concentration is 1-3mol/L is instilled in solution A, so that molar ratio Fe: P:Na=1: 1:(1- 3), and use concentration for 2-4mol/L ammonium hydroxide adjust pH value be 3-9, obtain suspension；
3) the freeze-dried 8h of suspension that step 2) obtains is obtained into mixture, and by mixture grind into powder；
4) powder for obtaining step 3) is in Ar or N2Calcination processing is carried out under atmosphere, calcination temperature is 500-800 DEG C, Calcination time is 2-12h, is cooled to room temperature after calcining, products therefrom is filtered after the salt acid soak 2h of 2mol/L, so It is washed till neutrality with water and ethyl alcohol afterwards, 6~12h of vacuum drying treatment is then carried out under the conditions of 60~100 DEG C, obtains nanometer sheet NaFePO4/ C-material.
Below with reference to embodiment, the invention will be described in further detail:
Embodiment 1
1) FeC for being 2mol/L by concentration2O4Solution and concentration are the aqueous solution in molar ratio Fe: P of the ammonium phosphate of 2mol/L =1: 1 ratio mixing, is denoted as solution A；
2) sodium oleate solution that concentration is 2mol/L is instilled in solution A, so that molar ratio Fe: P:Na=1: 1:2, and Using concentration to adjust pH value for the ammonium hydroxide of 3mol/L is 6, obtains suspension；
3) the freeze-dried 8h of suspension that step 2) obtains is obtained into mixture, and by mixture grind into powder；
4) powder for obtaining step 3) is in N2Calcination processing is carried out under atmosphere, calcination temperature is 600 DEG C, and calcination time is 8h is cooled to room temperature after calcining, and products therefrom is filtered after the salt acid soak 2h of 2mol/L, then uses water and ethyl alcohol It is washed till neutrality, vacuum drying treatment 8h is then carried out under the conditions of 80 DEG C, obtains the NaFePO of nanometer sheet4/ C-material.
It can be seen from figure 1 that prepared material meets NaFePO well4The standard card of/C, illustrates NaFePO4/C For pure phase, no other impurities.As can be seen from Figure 2, NaFePO4The pattern of/C is the laminated structure with a thickness of 50-80nm, structure tool There is biggish specific surface, the contact area with electrolyte can be increased, reduces ion diffusion path.As can be seen from Figure 3, in 100mAg-1 When, discharge capacity is 153mAh g for the first time-1, recycle 100 descendants and remain at 130mAh g-1, sheet NaFePO4/ C table Reveal excellent chemical property.
Embodiment 2
1) FeCl for being 1mol/L by concentration2Solution and concentration are the aqueous solution Fe in molar ratio of the ammonium hydrogen phosphate of 1mol/L : P=1: 1 ratio mixing is denoted as solution A；
2) sodium oleate solution that concentration is 1mol/L is instilled in solution A, so that molar ratio Fe: P:Na=1: 1:1, and Using concentration to adjust pH value for the ammonium hydroxide of 2mol/L is 3, obtains suspension；
3) the freeze-dried 8h of suspension that step 2) obtains is obtained into mixture, and by mixture grind into powder；
4) powder for obtaining step 3) carries out calcination processing under an ar atmosphere, and calcination temperature is 800 DEG C, and calcination time is 2h is cooled to room temperature after calcining, and products therefrom is filtered after the salt acid soak 2h of 2mol/L, then uses water and ethyl alcohol It is washed till neutrality, vacuum drying treatment 6h is then carried out under the conditions of 60 DEG C, obtains the NaFePO of nanometer sheet4/ C-material.
Embodiment 3
1) FeSO for being 10mol/L by concentration4Solution and concentration be the ammonium dihydrogen phosphate of 10mol/L aqueous solution by mole Ratio mixing than Fe: P=1: 1, is denoted as solution A；
2) sodium oleate solution that concentration is 3mol/L is instilled in solution A, so that molar ratio Fe: P:Na=1: 1:3, and Using concentration to adjust pH value for the ammonium hydroxide of 4mol/L is 9, obtains suspension；
3) the freeze-dried 8h of suspension that step 2) obtains is obtained into mixture, and by mixture grind into powder；
4) powder for obtaining step 3) is in N2Calcination processing is carried out under atmosphere, calcination temperature is 500 DEG C, and calcination time is 12h is cooled to room temperature after calcining, and products therefrom is filtered after the salt acid soak 2h of 2mol/L, then uses water and ethyl alcohol It is washed till neutrality, vacuum drying treatment 12h is then carried out under the conditions of 100 DEG C, obtains the NaFePO of nanometer sheet4/ C-material.
Embodiment 4
1) FeCl for being 5mol/L by concentration2Solution and concentration are the aqueous solution in molar ratio Fe: P of the ammonium phosphate of 5mol/L =1: 1 ratio mixing, is denoted as solution A；
2) sodium oleate solution that concentration is 1mol/L is instilled in solution A, so that molar ratio Fe: P:Na=1: 1:1.5, And using concentration to adjust pH value for the ammonium hydroxide of 4mol/L is 5, obtains suspension；
3) the freeze-dried 8h of suspension that step 2) obtains is obtained into mixture, and by mixture grind into powder；
4) powder for obtaining step 3) is in N2Calcination processing is carried out under atmosphere, calcination temperature is 700 DEG C, and calcination time is 10h is cooled to room temperature after calcining, and products therefrom is filtered after the salt acid soak 2h of 2mol/L, then uses water and ethyl alcohol It is washed till neutrality, vacuum drying treatment 12h is then carried out under the conditions of 80 DEG C, obtains the NaFePO of nanometer sheet4/ C-material.
Embodiment 5
1) FeSO for being 3mol/L by concentration4The aqueous solution for the ammonium dihydrogen phosphate that solution and concentration are 5mol/L is in molar ratio Fe: P=1: 1 ratio mixing, is denoted as solution A；
2) sodium oleate solution that concentration is 2mol/L is instilled in solution A, so that molar ratio Fe: P:Na=1: 1:1.5, And using concentration to adjust pH value for the ammonium hydroxide of 2mol/L is 8, obtains suspension；
3) the freeze-dried 8h of suspension that step 2) obtains is obtained into mixture, and by mixture grind into powder；
4) powder for obtaining step 3) carries out calcination processing under an ar atmosphere, and calcination temperature is 700 DEG C, and calcination time is 8h is cooled to room temperature after calcining, and products therefrom is filtered after the salt acid soak 2h of 2mol/L, then uses water and ethyl alcohol It is washed till neutrality, vacuum drying treatment 10h is then carried out under the conditions of 70 DEG C, obtains the NaFePO of nanometer sheet4/ C-material.
Embodiment 6
1) FeCl for being 8mol/L by concentration2The aqueous solution for the ammonium dihydrogen phosphate that solution and concentration are 5mol/L is in molar ratio Fe: P=1: 1 ratio mixing, is denoted as solution A；
2) sodium oleate solution that concentration is 2mol/L is instilled in solution A, so that molar ratio Fe: P:Na=1: 1:1.5, And using concentration to adjust pH value for the ammonium hydroxide of 4mol/L is 8, obtains suspension；
3) the freeze-dried 8h of suspension that step 2) obtains is obtained into mixture, and by mixture grind into powder；
4) powder for obtaining step 3) carries out calcination processing under an ar atmosphere, and calcination temperature is 600 DEG C, and calcination time is 8h is cooled to room temperature after calcining, and products therefrom is filtered after the salt acid soak 2h of 2mol/L, then uses water and ethyl alcohol It is washed till neutrality, vacuum drying treatment 10h is then carried out under the conditions of 80 DEG C, obtains the NaFePO of nanometer sheet4/ C-material.
Embodiment 7
1) FeCl for being 8mol/L by concentration2Solution and concentration are the aqueous solution Fe in molar ratio of the ammonium hydrogen phosphate of 5mol/L : P=1: 1 ratio mixing is denoted as solution A；
2) sodium oleate solution that concentration is 2mol/L is instilled in solution A, so that molar ratio Fe: P:Na=1: 1:2, and Using concentration to adjust pH value for the ammonium hydroxide of 3mol/L is 8, obtains suspension；
3) the freeze-dried 8h of suspension that step 2) obtains is obtained into mixture, and by mixture grind into powder；
4) powder for obtaining step 3) carries out calcination processing under an ar atmosphere, and calcination temperature is 600 DEG C, and calcination time is 8h is cooled to room temperature after calcining, and products therefrom is filtered after the salt acid soak 2h of 2mol/L, then uses water and ethyl alcohol It is washed till neutrality, vacuum drying treatment 10h is then carried out under the conditions of 90 DEG C, obtains the NaFePO of nanometer sheet4/ C-material.

Claims (8)

1. a kind of NaFePO4The preparation method of/C nano piece, which comprises the following steps:
1) by Fe2+Soluble salt solutions and phosphatic aqueous solution in molar ratio Fe: P=1: 1 ratio mix, be denoted as solution A, wherein Fe2+Soluble salt solutions concentration and the concentration of phosphate aqueous solution be 1-10mol/L；
2) sodium oleate solution is instilled in solution A, wherein the concentration of sodium oleate solution is 1-3mol/L, so that molar ratio Fe: P: Na=1: 1:(1-3), and pH value is adjusted as 3-9, obtain suspension；
3) mixture is obtained by suspension that step 2) obtains is freeze-dried, and by mixture grind into powder；
4) powder for obtaining step 3) carries out calcination processing under an inert atmosphere, is cooled to room temperature after calcining, by gained Product filters after salt acid soak, is then washed till neutrality with water and ethyl alcohol, then carries out vacuum drying treatment, obtains nanometer sheet NaFePO4/ C-material.
2. a kind of NaFePO according to claim 14The preparation method of/C nano piece, which is characterized in that in step 1) Fe2+Soluble-salt be FeC2O4、FeCl2Or FeSO4。
3. a kind of NaFePO according to claim 14The preparation method of/C nano piece, which is characterized in that the phosphorus in step 1) Hydrochlorate is ammonium phosphate, ammonium hydrogen phosphate or ammonium dihydrogen phosphate.
4. a kind of NaFePO according to claim 14The preparation method of/C nano piece, which is characterized in that used in step 2) Ammonium hydroxide adjusts pH, and ammonia concn is 2-4mol/L.
5. a kind of NaFePO according to claim 14The preparation method of/C nano piece, which is characterized in that freezing in step 3) Drying time is 8h.
6. a kind of NaFePO according to claim 14The preparation method of/C nano piece, which is characterized in that inertia in step 4) Atmosphere is Ar or N2Atmosphere.
7. a kind of NaFePO according to claim 14The preparation method of/C nano piece, which is characterized in that calcining in step 4) Temperature is 500-800 DEG C, calcination time 2-12h.
8. a kind of NaFePO according to claim 14The preparation method of/C nano piece, which is characterized in that vacuum in step 4) It is dried to be dried in vacuo 6~12h under the conditions of temperature is 60~100 DEG C.
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CN113526483B (en) * 2021-07-13 2022-12-30 内蒙古大学 Ferro-phosphorus sodalite type cathode material and preparation method and application thereof
CN115050934B (en) * 2022-05-31 2024-01-30 四川大学 Hydrophobic and oleophilic Na 2 Fe 2 （SO 4 ） 3 C positive electrode material and preparation method thereof

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103227327A (en) * 2013-04-26 2013-07-31 天津大学 Pyrolysis preparation method of two-dimensional nano-sheet-layer lithium ion battery negative electrode material
CN105140489A (en) * 2015-09-25 2015-12-09 中南大学 Titanium-doped carbon-coated sodium ferric phosphate material and preparation method thereof
CN105161688A (en) * 2015-09-25 2015-12-16 中南大学 Carbon-coated iron phosphate sodium-vanadium phosphate sodium composite material and preparation method thereof
CN105280899A (en) * 2015-09-22 2016-01-27 中南大学 Method for preparing carbon-coated sodium ferric phosphate material
CN105399073A (en) * 2015-11-06 2016-03-16 成都理工大学 Preparation method of hollow amorphous state NaFePO4 nanospheres
CN105810910A (en) * 2016-04-20 2016-07-27 中南大学 Na<2-2x>Fe<1+x>P<2>O<7>/carbon composite material and preparation method and application thereof
CN105845974A (en) * 2016-06-06 2016-08-10 四川国润新材料有限公司 Preparation method for positive electrode material NaFePO4/C of sodium ion battery
CN105938904A (en) * 2016-05-31 2016-09-14 中南大学 Composite positive electrode material for sodium-ion battery and preparation method of composite positive electrode material

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103227327A (en) * 2013-04-26 2013-07-31 天津大学 Pyrolysis preparation method of two-dimensional nano-sheet-layer lithium ion battery negative electrode material
CN105280899A (en) * 2015-09-22 2016-01-27 中南大学 Method for preparing carbon-coated sodium ferric phosphate material
CN105140489A (en) * 2015-09-25 2015-12-09 中南大学 Titanium-doped carbon-coated sodium ferric phosphate material and preparation method thereof
CN105161688A (en) * 2015-09-25 2015-12-16 中南大学 Carbon-coated iron phosphate sodium-vanadium phosphate sodium composite material and preparation method thereof
CN105399073A (en) * 2015-11-06 2016-03-16 成都理工大学 Preparation method of hollow amorphous state NaFePO4 nanospheres
CN105810910A (en) * 2016-04-20 2016-07-27 中南大学 Na<2-2x>Fe<1+x>P<2>O<7>/carbon composite material and preparation method and application thereof
CN105938904A (en) * 2016-05-31 2016-09-14 中南大学 Composite positive electrode material for sodium-ion battery and preparation method of composite positive electrode material
CN105845974A (en) * 2016-06-06 2016-08-10 四川国润新材料有限公司 Preparation method for positive electrode material NaFePO4/C of sodium ion battery

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