CN110085862A - A kind of sode cell electrode material Na1+xFexTi2-x(PO4)3And its preparation method and application - Google Patents
A kind of sode cell electrode material Na1+xFexTi2-x(PO4)3And its preparation method and application Download PDFInfo
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- CN110085862A CN110085862A CN201910343155.8A CN201910343155A CN110085862A CN 110085862 A CN110085862 A CN 110085862A CN 201910343155 A CN201910343155 A CN 201910343155A CN 110085862 A CN110085862 A CN 110085862A
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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
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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
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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- 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
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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- H—ELECTRICITY
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- 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
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Abstract
The present invention relates to a kind of sode cell electrode material Na1+ xFexTi2‑x(PO4)3And its preparation method and application.The sode cell electrode material, chemical formula Na1+xFexTi2‑x(PO4)3, wherein 0 < x≤0.9.The present invention provides a kind of synthesis in solid state Na simultaneously1+xFexTi2‑x(PO4)3Method: using titanium source, sodium source and phosphorus source as raw material, mixed with source of iron, ball milling, it is dry, be made after sintering.The preparation method is simple, is suitable for industrial production.Gained sodium ion electrode material is for specific capacity with higher in water system sodium-ion battery and cyclical stability.
Description
Technical field
The invention belongs to new energy materials fields, are related to a kind of sodium ion superconductor, in particular to a kind of Na1+ xFexTi2-x(PO4)3, its solid phase synthesis process and its application in water system sodium-ion battery.
Background technique
For water system sodium-ion battery because its is cheap, has a safety feature, becoming a new generation has development and application prospect
Energy storage device, be expected to extensive energy storage, intelligent micro-grid, off-network power station, communication iron tower and in terms of play
Huge effect.
Being currently used primarily in water system sode cell electrode material has: transition-metal oxide, Prussian blue similar object, fluorophosphoric acid
Salt and material with sodium ion superconducting structure, such as Na3Ti2(PO4)3、NaFePO4、NaTi2(PO4)3, wherein NaTi2
(PO4)3It can be used as negative electrode material and a series of positive electrode Na0.44MnO2、Na2NiFe(CN)6、Na3V2(PO4)3、 Na2CuFe
(CN)6、NaMnO2Assemble full battery.
But negative electrode material NaTi2(PO4)3Ionic conductivity it is poor, specific capacity is lower, and cyclical stability is bad,
It needs to be modified it in practical application, but production process is more complex.In addition, Na3Ti2(PO4)3Embedding sodium ability it is limited, lead
Cause its capacity lower.
Summary of the invention
Existing water system sode cell material there are aiming at the problem that, the present invention provides a kind of sode cell electrode material, has
The characteristics of specific capacity is high, good cycling stability.Simultaneously the present invention also provides the preparation method of the electrode material and its in water
It is the application in sodium-ion battery.
Technical scheme is as follows:
A kind of sode cell electrode material, chemical formula Na1+xFexTi2-x(PO4)3, wherein 0 < x≤0.9.
Preferably, the x is 0.3,0.4,0.8.
The present invention also provides sode cell electrode material Na1+xFexTi2-x(PO4)3Suitable industrial mass preparation method, packet
It includes: titanium source, sodium source, phosphorus source, source of iron is mixed, ball milling is dry, and Na is made in sintering1+xFexTi2-x(PO4)3, x is as defined above.
Further, the titanium source is at least one of titanium dioxide, titanium tetrachloride or butyl titanate, preferably dioxy
Change titanium, further preferred titanium dioxide P25.The titanium dioxide P25 is the anatase crystalline substance and golden red that average grain diameter is 25 nanometers
The titanium dioxide of stone crystalline substance mixed phase.
Further, the sodium source is at least one of sodium bicarbonate, sodium carbonate, sodium acetate, sodium citrate.
Further, phosphorus source is at least one of diammonium hydrogen phosphate, ammonium dihydrogen phosphate, ammonium phosphate, phosphoric acid.
Further, the source of iron is di-iron trioxide, ferric trichloride, ferric nitrate, at least one in iron chloride hexahydrate
Kind.
Further, the sodium source, source of iron, titanium source and phosphorus source are (1.1~2) according to the molar ratio of Na:Fe:Ti:P:
(0.1~0.9): (1.9~1.1): 3.
Further, the condition of the ball milling are as follows: ball material mass ratio is (5~20): 1, preferably (8-10): 1；Revolving speed is
500~1000r/min, preferably 800~1000r/min, Ball-milling Time are 0.5~48h, preferably 4-5h.
Further, the ball milling carries out in organic solvent medium, the organic solvent be preferably ethyl alcohol, ethylene glycol,
At least one of propyl alcohol, isopropanol, acetone.
Further, the sintering is divided into two stages: first in 350~500 DEG C of sintering 1h~12h, then 600~
1500 DEG C of 5~48h of sintering；Preferably, it is first sintered at 390-410 DEG C, is then sintered at 890-910 DEG C.The heating of the sintering
Rate be 0.5~20 DEG C/min, preferably 2.5-5 DEG C/min.
The present invention synthesizes Na by simple solid-phase synthesis1+xFexTi2-x(PO4)3Electrode material, the preparation method technique
Simply, yield is higher, is suitable for industrial production.
The present invention also provides above-mentioned sodium ion superconductor Na1+xFexTi2-x(PO4)3Answering in water system sodium-ion battery
With.
The application is specifically, a kind of water system sodium-ion battery, negative electrode material Na1+xFexTi2-x(PO4)3。
Using sodium ion superconductor Na of the present invention1+xFexTi2-x(PO4)3As negative electrode material, can make water system sodium from
Sub- battery specific capacity with higher and preferable cyclical stability.
Detailed description of the invention
Fig. 1 is Na prepared by the embodiment of the present invention 11.3Fe0.3Ti1.7(PO4)3X-ray diffractogram.
Fig. 2 is Na prepared by the embodiment of the present invention 11.3Fe0.3Ti1.7(PO4)3Scanning electron microscope (SEM) photograph.
Fig. 3 is Na prepared by the embodiment of the present invention 11.3Fe0.3Ti1.7(PO4)3Constant current charge-discharge curve graph.
Fig. 4 is Na prepared by the embodiment of the present invention 11.3Fe0.3Ti1.7(PO4)3Cycle performance figure.
Fig. 5 is Na prepared by the embodiment of the present invention 21.4Fe0.4Ti1.6(PO4)3Cycle performance figure.
Fig. 6 is Na prepared by the embodiment of the present invention 31.5Fe0.5Ti1.5(PO4)3Cycle performance figure.
Fig. 7 is Na prepared by the embodiment of the present invention 41.6Fe0.6Ti1.4(PO4)3Cycle performance figure.
Fig. 8 is Na prepared by the embodiment of the present invention 51.8Fe0.8Ti1.2(PO4)3Cycle performance figure.
Fig. 9 is NaTi prepared by comparative example 1 of the present invention2(PO4)3Cycle performance figure.
Specific embodiment
The following examples are used to illustrate the present invention, but are not intended to limit the scope of the present invention..
Embodiment 1
By sodium carbonate, titanium dioxide, diammonium hydrogen phosphate and di-iron trioxide according to material molar ratio 0.65:1.7:3:
0.15 is uniformly mixed, and using isopropanol as organic solvent, ball material mass ratio is 8:1, after engine speed 1000r/min, ball milling 4h.
Resulting material is placed in Muffle furnace, 2h is first sintered at 400 DEG C with the heating rate of 5 DEG C/min, then heats to 900 DEG C
It is sintered 10h, is further mechanically pulverized, obtains Na1.3Fe0.3Ti1.7(PO4)3。
Gained Na1.3Fe0.3Ti1.7(PO4)3Crystal form is good, with NaTi2(PO4)3Diffraction peak match it is good, show Al3+Portion
Divide substitution Ti4+(see Fig. 1).
As seen from Figure 2, gained Na1.3Fe0.3Ti1.7(PO4)3For nano particle, partial size is 300 nm-1 μm, and crystal form is good
It is good, and distribution of particles is relatively uniform.
Embodiment 2
Sodium acetate, P25, diammonium hydrogen phosphate and iron oxide are uniformly mixed according to molar ratio 0.7:1.6:3:0.2, with second
Alcohol is organic solvent, and ball material mass ratio is 8:1, after engine speed 1000r/min, ball milling 4h.Resulting material is placed in Muffle
In furnace, 2h is first sintered at 400 DEG C with the heating rate of 5 DEG C/min, then heats to 900 DEG C of sintering 10h, further machinery powder
It is broken to obtain Na1.4Fe0.4Ti1.6(PO4)3。
Embodiment 3
Sodium acetate, P25, diammonium hydrogen phosphate and iron oxide are uniformly mixed according to molar ratio 0.75:1.5:3:0.25, with
Acetone is organic solvent, and ball material mass ratio is 10:1, after engine speed 800r/min, ball milling 5h.Resulting material is placed in horse
Not in furnace, 2h is first sintered at 400 DEG C with the heating rate of 5 DEG C/min, then heats to 900 DEG C of sintering 10h, it is further mechanical
Crushing obtains Na1.5Fe0.5Ti1.5(PO4)3。
Embodiment 4
Sodium citrate, P25, diammonium hydrogen phosphate and iron oxide are uniformly mixed according to molar ratio 0.8:1.4:3:0.3, with
Ethyl alcohol is organic solvent, and ball material mass ratio is 8:1, after engine speed 1000r/min, ball milling 4h.Resulting material is placed in horse
Not in furnace, 5h is first sintered at 400 DEG C with the heating rate of 5 DEG C/min, then heats to 900 DEG C of sintering 10h, it is further mechanical
Crushing obtains Na1.6Fe0.6Ti1.4(PO4)3。
Embodiment 5
Sodium carbonate, titanium dioxide, diammonium hydrogen phosphate and iron oxide are uniformly mixed according to molar ratio 0.9:1.2:3:0.4,
Using ethyl alcohol as organic solvent, ball material mass ratio is 10:1, after engine speed 1000r/min, ball milling 4h.Resulting material is placed in
In Muffle furnace, 5h is first sintered at 400 DEG C with the heating rate of 2.5 DEG C/min, then heats to 900 DEG C of sintering 10h, further
Mechanical crushing obtains Na1.8Fe0.8Ti1.2(PO4)3。
Comparative example 1
Sodium carbonate, titanium dioxide and diammonium hydrogen phosphate are uniformly mixed according to molar ratio 0.5:1:3, are organic molten with ethyl alcohol
Agent, ball material mass ratio is 10:1, after engine speed 1000r/min, ball milling 4h.Resulting material is placed in Muffle furnace, first with
The heating rate of 2.5 DEG C/min is sintered 5h at 400 DEG C, then heats to 900 DEG C of sintering 10h, is further mechanically pulverized and obtains
NaTi2(PO4)3。
Compliance test result Na1+xFexTi2-x(PO4)3The specific capacity and cyclical stability of sodium-ion battery as negative electrode material
Test
1, the test result of 1 gained negative electrode material of embodiment:
By 1 gained Na of embodiment1.3Fe0.3Ti1.7(PO4)3With conductive black, polyfluortetraethylene of binding element according to mass ratio
80:10:10 mixing, is sized mixing with N-Methyl pyrrolidone, is then coated on stainless (steel) wire, 12 hours dry.
Na1.3Fe0.3Ti1.7(PO4)3The quality of electrode material is about 20 mg/cm2.Then using 1M aqueous sodium persulfate solution as electrolyte, warp
It crosses carbon-coated manganese dioxide and carries out constant current charge-discharge and cycle performance test for anode, charging and discharging currents density is 0.5A/g.
Fig. 3 is the constant current charge-discharge curve graph under current density 0.5A/g, and the voltage of battery reaches 1.45V, puts for the first time
Electric specific capacity is 45mAh/g.
Fig. 4 is cycle performance curve graph, its specific capacity remains to reach 40 mAh/g or more, specific capacity after recycling 150 times
Conservation rate is 89%.
2, the test result of 2 gained negative electrode material of embodiment:
The Na prepared with embodiment 21.4Fe0.4Ti1.6(PO4)3For raw material, pressed with conductive black and polyfluortetraethylene of binding element
It is mixed according to mass ratio 80:10:10, is sized mixing with N-Methyl pyrrolidone, be then coated on stainless (steel) wire, it is 12 hours dry.
Na1.4Fe0.4Ti1.6(PO4)3The quality of electrode material is about 20mg/cm2.Then using 1M aqueous sodium persulfate solution as electrolyte, pass through
Carbon-coated manganese dioxide is that anode carries out constant current charge-discharge and cycle performance test, and charging and discharging currents density is 0.5A/g.
Fig. 5 is the cycle performance curve graph of the material, its specific capacity remains to reach 34mAh/g, capacity after recycling 150 times
Conservation rate is 79%, coulombic efficiency 99%.
3, the test result of 3 gained negative electrode material of embodiment:
Na prepared with embodiment 31.5Fe0.5Ti1.5(PO4)3For raw material, pressed with conductive black and polyfluortetraethylene of binding element
It is mixed according to mass ratio 80:10:10, is sized mixing with N-Methyl pyrrolidone, be then coated on stainless (steel) wire, it is 12 hours dry.
Na1.5Fe0.5Ti1.5(PO4)3The quality of electrode material is about 20mg/cm2.Then using 1M aqueous sodium persulfate solution as electrolyte, pass through
Carbon-coated manganese dioxide is that anode carries out constant current charge-discharge and cycle performance test, and charging and discharging currents density is 0.5A/g.
Fig. 6 is the cycle performance curve graph of the material, its specific capacity remains to reach 35mAh/g, capacity after recycling 150 times
Conservation rate is 81.4%, and coulombic efficiency is close to 100%.
4, the test result of 4 gained negative electrode material of embodiment:
The Na prepared with embodiment 41.6Fe0.6Ti1.4(PO4)3For raw material, pressed with conductive black and polyfluortetraethylene of binding element
It is mixed according to mass ratio 80:10:10, is sized mixing with N-Methyl pyrrolidone, be then coated on stainless (steel) wire, it is 12 hours dry.
Na1.6Fe0.6Ti1.4(PO4)3The quality of electrode material is about 20mg/cm2.Then using 1M aqueous sodium persulfate solution as electrolyte, pass through
Carbon-coated manganese dioxide is that anode carries out constant current charge-discharge and cycle performance test, and charging and discharging currents density is 0.5A/g.
Fig. 7 is the cycle performance curve graph of the material, its specific capacity remains to reach 34mAh/g, capacity after recycling 150 times
Conservation rate is 78.7%, and coulombic efficiency is close to 100%.
5, the test result of 5 gained negative electrode material of embodiment:
The Na prepared with embodiment 51.8Fe0.2Ti1.8(PO4)3For raw material, pressed with conductive black and polyfluortetraethylene of binding element
It is mixed according to mass ratio 80:10:10, is sized mixing with N-Methyl pyrrolidone, be then coated on stainless (steel) wire, it is 12 hours dry.
Na1.8Fe0.2Ti1.2(PO4)3The quality of electrode material is about 20mg/cm2.Then using 1M aqueous sodium persulfate solution as electrolyte, pass through
Carbon-coated manganese dioxide is that anode carries out constant current charge-discharge and cycle performance test, and charging and discharging currents density is 0.5A/g.
Fig. 8 is the cycle performance curve graph of the material, its specific capacity remains to reach 35.4mAh/g after recycling 150 times, is held
Measuring conservation rate is 85.6%, and coulombic efficiency is close to 100%.
6, the test result of 1 gained negative electrode material of comparative example:
The NaTi prepared with comparative example 12(PO4)3For raw material, with conductive black and polyfluortetraethylene of binding element according to quality
It is mixed than 80:10:10, is sized mixing with N-Methyl pyrrolidone, be then coated on stainless (steel) wire, it is 12 hours dry.NaTi2
(PO4)3The quality of electrode material is about 20 mg/cm2.Then using 1M aqueous sodium persulfate solution as electrolyte, by carbon-coated two
Manganese oxide is that anode carries out constant current charge-discharge and cycle performance test, and charging and discharging currents density is 0.5A/g.
Fig. 9 is the cycle performance curve graph of the material, and initial capacity only has 25.6mAh/g, compared to Fe doping
NaTi2(PO4)3The specific capacity of electrode material is lower, and 50 its specific capacities of circulation rise to after 36.4mAh/g and circulation 150 times
Its specific capacity only has 27.3mAh/g, and capacity retention ratio 75%, coulombic efficiency is lower, and only 94%.
Although above the present invention is described in detail with a general description of the specific embodiments,
On the basis of the present invention, it can be made some modifications or improvements, this will be apparent to those skilled in the art.Cause
This, these modifications or improvements, fall within the scope of the claimed invention without departing from theon the basis of the spirit of the present invention.
Claims (10)
1. a kind of sode cell electrode material, which is characterized in that its chemical formula is Na1+xFexTi2-x(PO4)3, wherein 0 < x≤0.9.
2. sode cell electrode material according to claim 1, which is characterized in that the x is 0.3,0.4,0.8.
3. electrode material Na as claimed in claim 1 or 21+xFexTi2-x(PO4)3Preparation method characterized by comprising by titanium
Source, sodium source, phosphorus source, source of iron mixing, ball milling is dry, and Na is made in sintering1+xFexTi2-x(PO4)3, wherein 0 < x≤0.9.
4. preparation method according to claim 3, which is characterized in that the titanium source is titanium dioxide, titanium tetrachloride or titanium
At least one of sour four butyl esters, preferably titanium dioxide, further preferred titanium dioxide P25；
And/or the sodium source is at least one of sodium bicarbonate, sodium carbonate, sodium acetate, sodium citrate；
And/or phosphorus source is at least one of diammonium hydrogen phosphate, ammonium dihydrogen phosphate, ammonium phosphate, phosphoric acid；
And/or the source of iron is at least one of di-iron trioxide, ferric trichloride, ferric nitrate, iron chloride hexahydrate.
5. preparation method according to claim 3 or 4, which is characterized in that the sodium source, source of iron, titanium source and phosphorus source according to
The molar ratio of Na:Fe:Ti:P is (1.1~2): (0.1~0.9): (1.9~1.1): 3.
6. according to preparation method as claimed in claim 3 to 5, which is characterized in that the condition of the ball milling are as follows: ball material quality
Than for (5~20): 1, preferably (8-10): 1；
And/or revolving speed is 500~1000r/min, preferably 800~1000r/min.
7. according to any preparation method of claim 3-6, which is characterized in that the sintering is divided into two stages: first existing
350~500 DEG C of sintering 1h~12h, then in 600~1500 DEG C of 5~48h of sintering；Preferably, it is first sintered at 390-410 DEG C, so
It is sintered afterwards at 890-910 DEG C.
8. according to any preparation method of claim 3-7, which is characterized in that the heating rate of the sintering is 0.5~
20 DEG C/min, preferably 2.5-5 DEG C/min.
9. sode cell electrode material Na as claimed in claim 1 or 21+xFexTi2-x(PO4)3Application in water system sodium-ion battery.
10. a kind of water system sodium-ion battery, which is characterized in that its negative electrode material is sode cell electrode material as claimed in claim 1 or 2
Expect Na1+xFexTi2-x(PO4)3。
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| CN111477872A (en) * | 2020-03-26 | 2020-07-31 | 合肥国轩电池材料有限公司 | Water-based lithium/sodium ion battery with iron-doped sodium titanium phosphate as negative electrode active material and preparation method thereof |
| CN114068906A (en) * | 2021-10-15 | 2022-02-18 | 广东邦普循环科技有限公司 | Deposition type sodium iron phosphate cathode material and preparation method and application thereof |
| CN115472784A (en) * | 2022-08-16 | 2022-12-13 | 北京航空航天大学 | Na 3 Ti 2 (PO 4 ) 3 Preparation method of positive electrode and application of positive electrode in sodium ion battery |
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