CN106865562A - A kind of Na3V2(BO3)3Compound and its preparation and application - Google Patents
A kind of Na3V2(BO3)3Compound and its preparation and application Download PDFInfo
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- CN106865562A CN106865562A CN201510924800.7A CN201510924800A CN106865562A CN 106865562 A CN106865562 A CN 106865562A CN 201510924800 A CN201510924800 A CN 201510924800A CN 106865562 A CN106865562 A CN 106865562A
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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
- C01B35/00—Boron; Compounds thereof
- C01B35/08—Compounds containing boron and nitrogen, phosphorus, oxygen, sulfur, selenium or tellurium
- C01B35/10—Compounds containing boron and oxygen
- C01B35/12—Borates
- C01B35/128—Borates containing plural metal or metal and ammonium
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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
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
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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
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Abstract
The present invention relates to Na3V2(BO3)3Compound and preparation method thereof, Na3V2(BO3)3/ C sodium-ion battery positive materials and its preparation method.Na can be prepared using high-temperature solid phase reaction method and sol-gal process3V2(BO3)3Compound and Na3V2(BO3)3/ C sodium-ion battery positive materials；With preferable sodium-ion battery charge-discharge performance, cyclical stability is good, and operating voltage is suitable, can be used as sodium-ion battery positive material.
Description
Technical field
It is Na the present invention relates to chemical formula3V2(BO3)3Compound, sodium-ion battery positive material, preparation method and profit
Sodium-ion battery is made with the material.
Background technology
With increasingly serious, the increasingly scarcity of non-renewable resources of energy problem, and people are to environmentally friendly understanding of importance
Continuous enhancing, society increasingly strengthens the demand of new energy, and energy storage plays more and more important work in energy system
With.Before, numerous resourcess for research have been attracted as the lithium ion battery of important energy storage device in new energy, it is contemplated that
The less and its higher price of lithium reserves on earth, recently to reserves more abundant, more cheap Na ion-conductances
The research in pond has retrieved the attention of researcher.
The positive electrode for being applied to sodium-ion battery at present mainly has Na3V2(PO4)3、NaVPO4F、Na3V2(PO4)2F3With
NaTiFeO3、NaCoO3And NaMnO3Deng.However, these materials are still present many problems：Specific capacity and operating voltage
It is relatively low, cyclical stability difference and preparation difficulty etc., this severely limits the practical application of these materials.Compared to phosphate,
Sulfate and silicate, borate have specific capacity and specific energy higher due to relatively low molal weight[15].In addition,
BO3And BO4With multiple combination mode, B can be formed3O6, B3O7, B5O12Deng different structure group, this kind of compound tool
Have abundant from zero dimension to one-dimensional, two and three dimensions structures, so that for the transmission of Na ions provides larger passage.
In addition, BO3And BO4Group also has inductive effect, can improve the operating voltage of positive electrode.And at present on boric acid
The research of salt sodium-ion battery positive material does not almost have, and is worth further investigation.
The content of the invention
The present invention is directed to technical problem set forth above, and purpose is to provide a kind of Na3V2(BO3)3Compound and preparation method,
And Na3V2(BO3)3/ C sodium-ion battery positive materials.
To achieve the above object, the concrete technical scheme of use is as follows：
A kind of Na3V2(BO3)3Compound.Its preparation process is as follows：Na compounds, compound containing V and chemical combination containing B will be contained
Thing Na in molar ratio：V：B=3:2:After 3 ratio is well mixed, chemosynthesis reaction is carried out, Na is obtained3V2(BO3)3
Compound；
The compound containing Na is the oxalates of oxide, the carbonate of Na, the nitrate of R or the Na of Na；
The compound containing V is the oxide of V or/and the borate of V；
The boride alloy is H3BO3Or/and B2O3。
The Na that the present invention is provided3V2(BO3)3/ C sodium-ion battery positive materials.
Na3V2(BO3)3The preparation method of/C sodium-ion battery positive materials, material preparation is carried out using high temperature solid-state method, its
Step is as follows：
1) dispensing：By Na2CO3、V2O3And H3BO3By Na:V:B is 3:2:3 mol ratio, while adding Na3V2(BO3)3
The sucrose dispensing of quality 20% is simultaneously pre-processed；
2) control parameters carry out materials synthesis：The crucible that above-mentioned dispensing will be filled is placed in and is connected with inert protective atmosphere
In tube furnace；600-1000 DEG C is risen to 1-5 DEG C of speed；Insulation 10-40 hours；After question response is abundant, to be less than
The speed of 50 DEG C/h is down to room temperature, obtains Na3V2(BO3)3/ C-material；
The pretreatment of the pretreated raw material is to be poured into corundum crucible after the raw material that will have been configured is well mixed, in horse
Not be to slowly warm up in stove 300 DEG C heat more than 10 hours, after be cooled to room temperature；
The Na2CO3Replaced with the oxalates of the oxide of Na, the nitrate of Na or Na；
The V2O3With the borate of V, the oxalates or NH of V4VO3Instead of；
Described B2O3Use H3BO3Instead of.
The Na that the present invention is provided3V2(BO3)3The preparation method of/C sodium-ion battery positive materials, is prepared using sol-gal process
Na3V2(BO3)3/ C sodium-ion battery positive materials, its step is as follows：
1) dispensing：Na will be contained2CO3、V2O5、H3BO3Na is pressed with oxalic acid:V:B:Oxalic acid is 30:10:30:(10-30's)
Stirred to uniform blue solution is formed in the deionized water of 80 DEG C of mol ratio addition, be heated to forming colloidal sol；
2) colloidal sol is transferred in 120 DEG C of baking oven, is dried to gel, gel abrasive is transferred in porcelain boat into powder, entered
Row pretreatment；
3) control parameters carry out materials synthesis：The porcelain boat that above-mentioned dispensing will be filled is placed in and is connected with inert protective atmosphere
In tube furnace；600-1000 DEG C is risen to 1-5 DEG C of speed；Insulation 10-40 hours；After question response is abundant, to be less than
The speed of 50 DEG C/h is down to room temperature, obtains Na3V2(BO3)3/ C-material；
The pretreatment of the pretreated raw material is to be poured into porcelain boat after the raw material that will have been configured is well mixed, in Muffle furnace
In be to slowly warm up to 300 DEG C heat more than 5 hours, after be cooled to room temperature；
The Na2CO3Replaced with the oxalates of the oxide of Na, the nitrate of Na or Na；
The V2O3With the borate of V, the oxalates or NH of V4VO3Instead of；
Described B2O3Use H3BO3Instead of.
Typically Na is can obtain the following is several3V2(BO3)3The chemical reaction of compound：
(1)3Na2CO3+2V2O3+3B2O3=2Na3V2(BO3)3+3CO2↑
(2)12NaNO3+4V2O3+6B2O3=4Na3V2(BO3)3+12NO2↑+3O2↑
(3)3Na2CO3+4VOC2O4+6H3BO3=2Na3V2(BO3)3+9CO2↑+2CO↑+9H2O↑
(4)12NaNO3+8VOC2O4+12H3BO3=4Na3V2(BO3)3+12NO2↑+16CO2↑+O2↑+18H2O↑
The advantage of the invention is that：Obtained positive electrode has specific capacity and operating voltage higher, larger stable circulation
Property.Na3V2(BO3)3There is/C sodium-ion battery positive materials specific capacity higher to reach 230mAh/g；Its operating voltage
Between 3.0-4.3V, specific capacity remains to keep more than 95% after 25 circulations.
Brief description of the drawings
Fig. 1 is Na of the present invention3V2(BO3)3The SEM pictures of/C sodium-ion battery positive materials.
Fig. 2 is Na of the present invention3V2(BO3)3The polycrystal powder X ray diffracting spectrum of/C.
Fig. 3 is Na of the present invention3V2(BO3)3Crystal structure figure.
Fig. 4 is Na of the present invention3V2(BO3)3Charging and discharging curve in the range of/C positive electrode material 0.2C multiplying powers, 3-4.3V.
Fig. 5 is Na of the present invention3V2(BO3)3The stable circulation linearity curve of/C positive electrode material in 0.2C.
Specific embodiment
The Na of embodiment 13V2(BO3)3It is prepared by the high temperature solid-state of compound
By the Na of 0.03mol2CO3, 0.02mol V2O3With the H of 0.06mol3BO3It is put into agate mortar, grinds
Half an hour.Right hand is transferred in crucible, and crucible is put into the tube furnace of inert gas Ar protections.With 1-10 DEG C/min
Programming rate stove is risen to 200-400 DEG C, be incubated 3-10 hours, room temperature is finally down to the speed of 1-10 DEG C/min.
The material that will synthesize takes out, and is transferred again into crucible after pulverizing, and is put into the tube furnace of inert gas Ar protections.
Stove is risen to 600-900 DEG C with the programming rate of 1-10 DEG C/min, 10-40 hours is incubated, finally with 1-10 DEG C/min
Speed be down to room temperature.Product taking-up grinding composition will be obtained and obtain final product Na3V2(BO3)3Compound.
As shown in figure 1, it is celadon powder, tap density 1.5g/cm3, 930 DEG C of fusing point.Its X-ray diffractogram
Spectrum is as shown in Fig. 2 its crystal structure figure is as shown in Figure 3.It can be seen in figure 3 that its basic construction unit is
BO3Triangle, Na and V occupy same position, by BO3Triangle is interconnected to form three-dimensional net structure.
The Na of embodiment 23V2(BO3)3It is prepared by the sol-gel of compound
By the dissolving oxalic acid of 0.03mol in the beaker equipped with deionized water, the VBO of 0.02mol is subsequently adding3,
Stirring is subsequently adding the H of 0.01mol to being in blue solution in 70-80 DEG C of water bath with thermostatic control3BO3, 0.015mol
Na2CO3, continue stirring and form glaucous boric acid vanadium sodium colloidal sol.The colloidal sol is placed in into baking 10h or so in 80 DEG C of baking ovens to obtain
To blue puffy presoma, by presoma grinding in being placed in crucible after powder, crucible is put into inert gas Ar
In the tube furnace of protection.Stove is risen to 200-400 DEG C with the programming rate of 1-10 DEG C/min, 3-10 hours is incubated, most
Room temperature is down to the speed of 1-10 DEG C/min afterwards.The material that will synthesize takes out, and is transferred again into crucible after pulverizing,
It is put into the tube furnace of inert gas Ar protections.Stove is risen to 600-900 DEG C with the programming rate of 1-10 DEG C/min, is protected
It is warm 10-40 hours, room temperature is finally down to the speed of 1-10 DEG C/min.Product taking-up grinding composition will be obtained to obtain final product
Na3V2(BO3)3Compound.
The Na of embodiment 33V2(BO3)3It is prepared by the high temperature solid-state of/C positive electrode material
By the Na of 0.03mol2CO3, 0.02mol V2O3, 0.06mol H3BO3And Na3V2(BO3)3Quality 20%
Sucrose is put into agate mortar, grinds half an hour.Right hand is transferred in crucible, and crucible is put into inert gas Ar protections
Tube furnace in.Stove is risen to 200-400 DEG C with the programming rate of 1-10 DEG C/min, 3-10 hours is incubated, finally with
The speed of 1-10 DEG C/min is down to room temperature.The material that will synthesize takes out, and is transferred again into crucible after pulverizing, and is put into
In the tube furnace of inert gas Ar protections.Stove is risen to by 600-900 DEG C, insulation with the programming rate of 1-10 DEG C/min
10-40 hours, room temperature is finally down to the speed of 1-10 DEG C/min.Product taking-up grinding composition will be obtained to obtain final product
Na3V2(BO3)3/ C positive electrode material.
The Na of embodiment 43V2(BO3)3The preparation of/C positive electrode material
By the dissolving oxalic acid of 0.03mol in the beaker equipped with deionized water, the vanadic anhydride of 0.01mol is subsequently adding,
Stirring is subsequently adding the H of 0.03mol to being in blue solution in 70-80 DEG C of water bath with thermostatic control3BO3, mass percent be
20% sucrose, the Na of 0.015mol2CO3, continue stirring and form glaucous boric acid vanadium sodium colloidal sol.The colloidal sol is placed in
10h or so is dried in 80 DEG C of baking ovens and obtains blue puffy presoma, by presoma grinding in being placed in crucible after powder,
Crucible is put into the tube furnace of inert gas Ar protections.Stove is risen to the programming rate of 1-10 DEG C/min
200-400 DEG C, 3-10 hours is incubated, room temperature is finally down to the speed of 1-10 DEG C/min.The material that will synthesize takes out,
It is transferred again into crucible after pulverizing, is put into the tube furnace of inert gas Ar protections.With the liter of 1-10 DEG C/min
Stove is risen to 600-900 DEG C by warm speed, is incubated 10-40 hours, is finally down to room temperature with the speed of 1-10 DEG C/min.
Product taking-up grinding composition will be obtained and obtain final product Na3V2(BO3)3/ C positive electrode material.
By the gained composite of embodiment 3 and 4, according to active material, conductive black, binding agent three mass ratio
It is 8:1:1 is dissolved in appropriate 1-METHYLPYRROLIDONE and being well mixed, and it is 0.15mm's to be coated into thickness with wet film maker
Electrode film, is cut into the electrode slice of a diameter of 12mm with slicer after vacuum drying, weigh and calculate the quality of active material.
Simultaneously using lithium piece as positive pole, using Celgard 2500 as barrier film, the NaPF of 1mol/L6EC+DMC (volume ratios
It is 1:1) solution is electrolyte, and button cell is dressed up in the glove box full of argon gas.Then the battery of assembling is entered
Row electro-chemical test, tests under 3-4.3V constant current conditions respectively.Test result is as shown in Figures 4 and 5, it can be seen that
Na3V2(BO3)3With specific discharge capacity higher, 230mAh/g is reached, and with good cyclical stability, 25
Do not decay significantly after circulation.
Claims (8)
1. a kind of Na3V2(BO3)3Compound.
2. Na described in a kind of claim 13V2(BO3)3The preparation method of compound, it is characterised in that：Preparation process
It is as follows, Na compounds, the compounds of V containing trivalent and boride alloy Na in molar ratio will be contained:V:B=3:2:3 ratio
After example is well mixed, chemosynthesis reaction is carried out, Na is obtained3V2(BO3)3Compound.
3. according to the preparation method described in claim 2, it is characterised in that：
The compound containing Na is the oxide of Na, the carbonate of Na, the borate of Na, the nitrate of Na or
One or two or more kinds in the oxalates of Na；
The compounds of V containing trivalent are the oxide of trivalent V or/and the borate of V；
The boride alloy is H3BO3Or/and B2O3。
4. according to the preparation method described in Claims 2 or 3, it is characterised in that：Prepared using solid phase reaction
Na3V2(BO3)3Compound, its step is as follows：
1) dispensing：Na compounds, the compounds of V containing trivalent and boride alloy will be contained by Na:V:B is 3：2:3
Molar ratio ingredient pre-processed；
The pretreatment of the pretreated raw material is to be poured into corundum crucible after the raw material that will have been configured is well mixed,
In Muffle furnace from room temperature to 200-500 DEG C heat more than 2-10 hours, after be cooled to room temperature；
2) control parameters carry out materials synthesis：The crucible that above-mentioned dispensing will be filled is placed in and is connected with inert protective atmosphere
Tube furnace in；With 1-5 DEG C of speed 600-1000 DEG C is risen to from room temperature；Insulation 10-40 hours；Question response fills
After point, room temperature is down to the speed of 1-50 DEG C/h, obtains Na3V2(BO3)3Material.
5. according to the preparation method described in Claims 2 or 3, it is characterised in that prepared using sol-gal process
Na3V2(BO3)3Compound, its step is as follows：
1) dispensing：Na compounds, the compounds of V containing trivalent and boride alloy will be contained by Na:V:B is 3:2:3
Mol ratio added and stir in 50-100 DEG C of deionized water to forming uniform solution；
2) solution is transferred in 100-150 DEG C of baking oven, pulverizes and be transferred in porcelain boat, pre-processed；
The pretreatment of the pretreated raw material is to be poured into porcelain boat after the raw material that will have been configured is well mixed, in horse
Not in stove from room temperature to 200-500 DEG C heat more than 2-10 hours, after be cooled to room temperature；
3) control parameters carry out materials synthesis：The porcelain boat that above-mentioned dispensing will be filled is placed in and is connected with inert protective atmosphere
Tube furnace in；600-1000 DEG C is risen to 1-5 DEG C of speed；Insulation 10-40 hours；After question response is abundant,
Room temperature, Na are down to the speed of 1-50 DEG C/h3V2(BO3)3Compound.
6. Na described in a kind of claim 13V2(BO3)3Compound is as active material in sodium-ion battery positive material
In application, it is characterised in that：The sodium-ion battery positive material is Na3V2(BO3)3/ C-material, C mass contents
It is 10-50%.
7. according to the application described in claim 6, it is characterised in that：Na is prepared using solid reaction process3V2(BO3)3/C
Sodium-ion battery positive material, its step is as follows：
1) dispensing：Na compounds, compound containing V and boride alloy will be contained by Na:V:B is 3:2:3 mole
Than while adding Na3V2(BO3)3The sucrose dispensing of quality 10-50% is simultaneously pre-processed；
The pretreatment of the pretreated raw material is to be poured into corundum crucible after the raw material that will have been configured is well mixed,
In Muffle furnace from room temperature to 200-500 DEG C heat more than 2-10 hours, after be cooled to room temperature；
2) control parameters carry out materials synthesis：The crucible that above-mentioned dispensing will be filled is placed in and is connected with inert protective atmosphere
Tube furnace in；With 1-5 DEG C of speed 600-1000 DEG C is risen to from room temperature；Insulation 10-40 hours；Question response fills
After point, room temperature is down to the speed of 1-50 DEG C/h, obtains Na3V2(BO3)3/ C-material；
The compound containing Na is the oxide of Na, the carbonate of Na, the borate of Na, the nitrate of Na or
One or two or more kinds in the oxalates of Na；
The compound containing V is oxide, the borate of V, the oxalates of V or the NH of V4VO3In one kind or two
More than kind；
The boride alloy is H3BO3Or/and B2O3。
8. according to the application described in claim 6, it is characterised in that prepare Na using sol-gal process3V2(BO3)3/C
Sodium-ion battery positive material, its step is as follows：
1) dispensing：Na compounds, the compounds of V containing trivalent and boride alloy will be contained by Na:V:B is 3:2:3
Stirred in the deionized water of 50-100 DEG C of mol ratio addition to uniform blue solution is formed, while adding Na3V2(BO3)3
The sucrose of quality 10-50% continues to stir to formation colloidal sol；
2) colloidal sol is transferred in 100-150 DEG C of baking oven, is dried to gel, gel abrasive is transferred to porcelain into powder
In boat, pre-processed；
The pretreatment of the pretreated raw material is to be poured into porcelain boat after the raw material that will have been configured is well mixed, in horse
Not in stove from room temperature to 200-500 DEG C heat more than 2-10 hours, after be cooled to room temperature；
3) control parameters carry out materials synthesis：The porcelain boat that above-mentioned dispensing will be filled is placed in and is connected with inert protective atmosphere
Tube furnace in；600-1000 DEG C is risen to 1-5 DEG C of speed；Insulation 10-40 hours；After question response is abundant,
Room temperature is down to the speed of 1-50 DEG C/h, Na is obtained3V2(BO3)3/ C-material；
The compound containing Na is the oxide of Na, the carbonate of Na, the borate of Na, the nitrate of Na or
One or two or more kinds in the oxalates of Na；
The compound containing V is oxide, the borate of V, the oxalates of V or the NH of V4VO3In one kind or two
More than kind；
The boride alloy is H3BO3Or/and B2O3In.
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Cited By (1)
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| CN115133002A (en) * | 2022-07-29 | 2022-09-30 | 湖北万润新能源科技股份有限公司 | Sodium battery positive electrode material and preparation method and application thereof |
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