CN106935807A - A kind of ammonium vanadate/nickel foam sodium-ion battery preparation method of self-supporting positive pole - Google Patents
A kind of ammonium vanadate/nickel foam sodium-ion battery preparation method of self-supporting positive pole Download PDFInfo
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
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Abstract
The invention discloses a kind of ammonium vanadate/nickel foam sodium-ion battery preparation method of self-supporting positive pole, foam nickel sheet is cleaned with acetone and with clean dry after hydrogen peroxide treatment, electrode material matrix is obtained；Then certain density ammonium metavanadate solution is configured, solution pH value is adjusted, required solution is obtained；Resulting solution and nickel sheet are put into water heating kettle again, using hydro-thermal induction heating equipment heating and thermal insulation certain hour, the ammonium vanadate with three-dimensional porous connectivity structure/nickel foam sodium-ion battery anode composite material is obtained final product.The present invention can prepare the nanostructured with three-dimensional porous connection, larger specific surface area and the small sodium-ion battery self-supporting material of itself internal resistance.
Description
Technical field
The invention belongs to sodium-ion battery positive material preparation field, and in particular to a kind of ammonium vanadate/nickel foam sodium ion
The battery preparation method of self-supporting positive pole.
Background technology
Lithium ion battery has the advantages that energy density is big, has extended cycle life, memory-less effect and be widely used in just
Take formula electronic market.But with the aggravation that the industries such as the vehicles and large-scale power system are relied on lithium ion battery, the whole world
Lithium resource will be unable to effectively meet the great demand of power lithium-ion battery, so as to will further raise and lithium associated materials
Price, increases battery cost, the development of final obstruction New Energy Industry.Therefore, other cheap alternative lithium ion batteries are developed
Related energy storage technology it is very crucial.Sodium reserves in the earth 4~5 order of magnitude higher than lithium, and it is widely distributed, therefore use
Sodium-ion battery can alleviate the shortage of resources problem of lithium instead of lithium ion battery.Meanwhile, sodium element and elemental lithium are located at element week
The same main group of phase table, with similar physicochemical properties, and sodium-ion battery has the work similar with lithium ion battery
Make principle so that be possibly realized as electrode material with similar compound in the two systems.But due to sodium ion
Radius ratio lithium ion it is big, cause reversible capacity and high rate performance reduction.What sodium-ion battery was studied it is critical only that new height
The exploitation of performance electrode material, the successful experience based on lithium ion battery, current research is concentrated mainly on negative material, such as
Research of the fruit lifting to positive electrode will greatly improve the performance of sodium-ion battery.
Ammonium vanadate has the advantages that capacity high, easy preparation, abundant raw materials and has a safety feature, simultaneously because NH4+'s
Introduce, its interlamellar spacing bigger, structure is also more stable, is a kind of very promising positive electrode.Prepare at present
NH4V3O8Method mainly have：The precipitation method and hydro-thermal method.Wherein, hydro-thermal method is a kind of effectively route of synthesis.The shape of synthesis
Looks also have fusiform, flower-shaped and banding etc..But the precipitation method synthesize NH4V3O8There is course of reaction to be difficult to control, there is side reaction to send out
Raw, the low shortcoming of product purity, hydro-thermal method synthesis NH4V3O8There is the shortcomings of reaction temperature is of a relatively high, the reaction time is more long.
And ammonium vanadate is small due to itself electrical conductivity, cause its electric conductivity poor.
The content of the invention
It is an object of the invention to provide a kind of ammonium vanadate/nickel foam sodium-ion battery preparation side of self-supporting positive pole
Method, with the defect for overcoming above-mentioned prior art to exist, the present invention can prepare the nanostructured with three-dimensional porous connection, compared with
Big specific surface area and the small sodium-ion battery positive material of itself internal resistance.
To reach above-mentioned purpose, the present invention is adopted the following technical scheme that：
A kind of ammonium vanadate/nickel foam sodium-ion battery the preparation method of self-supporting positive pole, comprises the following steps：
1) electrode material matrix sheet nickel foam is cut to the foam nickel sheet A of rectangle；
2) A is immersed in acetone and is cleaned by ultrasonic, then take out A, then B is obtained with deionized water rinsing；
3) B is immersed in hydrogenperoxide steam generator and the treatment in ultrasound environments, then takes out B and rinsed with absolute ethyl alcohol,
Place into oven drying and obtain C；
4) ammonium metavanadate is dissolved in deionized water, heating, stirring are obtained NH4VO3Solution D；
5) pH value of D is adjusted to 1~5, obtains solution E；
6) E is transferred in hydro-thermal sensing kettle, is put into C, wherein 0.25-0.50g C are added in per 50mLE, after kettle is sealed,
It is placed in hydro-thermal induction heating equipment, with the induction frequencies of 400~800KHz by room temperature to 70~180 DEG C, and it is incubated 1~
4h, obtains nickel foam/ammonium vanadate composite F；
7) F is used into deionized water and the soft washing of absolute ethyl alcohol respectively, is then dried to obtain with three-dimensional porous connection knot
The nickel foam of structure/ammonium vanadate sodium-ion battery positive material.
Further, step 1) in the Ni-based body thickness of sheet-formed foam be 1mm, cut A a length of 3cm, a width of 2cm.
Further, step 2) used in acetone for analysis it is pure, ultrasonics cleaning frequency be 40KHz, ultrasonic cleaning the time
It is 0.5~1h.
Further, step 3) in hydrogen peroxide mass concentration be 30%, supersonic frequency be 40K Hz, when ultrasonically treated
Between be 0.5~1h.
Further, step 3) in drying temperature be 60~90 DEG C, the time be 1~3h.
Further, step 4) in NH4VO3Solution molar concentration is 0.05~0.20mol/L.
Further, step 4) in ammonium metavanadate is dissolved in deionized water, be heated to 30~60 DEG C, use magnetic agitation
Device is stirred, and speed is 500~800 revs/min, and the time is 0.5~1h.
Further, step 5) the middle nitric acid regulation pH value of solution using 2mol/L.
Further, step 6) in C induction coils in hydro-thermal induction heating equipment magnetic induction line place.
Further, step 7) in F is washed using deionized water and absolute ethyl alcohol at room temperature, absolute ethyl alcohol is dense
Spend for analysis is pure, drying temperature is 50~70 DEG C in drying process, the time is 6~12h.
Compared with prior art, the present invention has following beneficial technique effect：
The thinking that the present invention is combined using ammonium vanadate/nickel foam.On the one hand, foam nickel electrode substrate has hole higher
Rate, good electric conductivity, preferable pliability and extensibility and larger specific surface area, play collector and conducting matrix grain
Effect, not only improves the high density filling of ammonium vanadate, does not again allow the crystallization of ammonium vanadate nano particle easy to fall off, and also good leads
Electric network structure, improves the influence of ammonium vanadate poorly conductive, and nickel foam also has certain free space to bear the swollen of electrode
It is swollen, greatly improve the high rate performance and cycle performance of electrode material.On the other hand, the compound method of ammonium vanadate/nickel foam is exempted from
The step of having removed conventional electrode materials film, and binding agent, conductive agent are not used, the capacity of electrode material is not influenceed, not only subtract
Few production process, it is also cost-effective.
Additionally, the present invention uses hydro-thermal induction heating technique, it is former on its surface with three-dimensional porous nickel foam as supporter
Two-dimensional nano thin slice has been constructed in position.By controlling the thickness of nickel foam, size and by induction area, realization it is carried out it is in situ
Even heating, makes its surface temperature raise rapidly, there is provided substantial amounts of active nucleation site, active material is more easy to and supporter formationization
Key is learned, adhesion is strong；By the speed of growth of the controllable crystal of the size, frequency and the mixing speed that change alternating current, realize
To the accuracy controlling of active material crystal structure.Compared with self-supporting electrode prepared by common technique, prepared using the technology
Self-supporting two-dimensional nanostructure electrode is used to show capacity higher in sodium-ion battery, and excellent stable circulation and times
Rate performance.
Nano combined self-supporting electrode with excellent interface binding ability prepared by the present invention, has given full play to supporter
Synergy between active material, due to the electrode prepared using the method, interface cohesion stabilization, nanosizing degree is high,
Even aperture distribution, overcomes the defect of easy reunion, and former capital shows capacity higher, the cycle performance of stabilization and excellent times
Rate performance.
Brief description of the drawings
Fig. 1 is X-ray diffraction (XRD) collection of illustrative plates of sodium-ion battery positive material prepared by the embodiment of the present invention 1；
Fig. 2 is that ESEM (SEM) photo of sodium-ion battery positive material prepared by the embodiment of the present invention 1 (amplifies 20,000
Times)；
Fig. 3 is the cycle performance figure of sodium-ion battery positive material prepared by the embodiment of the present invention 1,3,5.
Specific embodiment
Embodiments of the present invention are described in further detail below：
A kind of ammonium vanadate/nickel foam sodium-ion battery the preparation method of self-supporting positive pole, comprises the following steps：
1) by thickness for 1mm electrode material matrix sheet nickel foam cut rectangle foam nickel sheet A, make its a length of
3cm, a width of 2cm；
2) 0.25~0.50g (i.e. 1-2 pieces) A is immersed in the analytically pure acetone of 40~70mL super with the frequency of 40KHz
Sound cleans 0.5~1h, then takes out A, then obtain B with deionized water rinsing；
3) 0.25~0.50g (i.e. 1-2 pieces) B is immersed in 40~70mL, the hydrogenperoxide steam generator of mass concentration 30% is simultaneously
0.5~1h is processed in frequency is for the ultrasound environments of 40K Hz, B is then taken out and is rinsed with absolute ethyl alcohol, place into baking oven,
1~3h is dried in 60~90 DEG C of temperature and obtains C；
4) ammonium metavanadate is dissolved in deionized water, be heated to 30~60 DEG C, using magnetic stirring apparatus with 500~800 turns/
The speed of minute stirs 0.5~1h and the NH that molar concentration is 0.05~0.20mol/L is obtained4VO3Solution D；
5) pH value of D is adjusted to 1~5 using the nitric acid of 2mol/L and obtains solution E；
6) 50mLE is transferred in hydro-thermal sensing kettle, then by 0.25~0.50g (i.e. 1-2 pieces) C perpendicular to hydro-thermal sensing heating
The magnetic induction line of induction coil is put into equipment, after kettle is sealed, is placed in hydro-thermal induction heating equipment, with 400~800KHz's
Induction frequencies are incubated 1~4h by room temperature to 70~180 DEG C, obtain ammonium vanadate/foam nickel composite material F；
7) by F respectively with the deionized water and the soft washing of analytically pure absolute ethyl alcohol that temperature is room temperature, then 50~
6~12h is dried in 70 DEG C of temperature and obtains the ammonium vanadate with three-dimensional porous connectivity structure/nickel foam sodium-ion battery positive pole material
Material.
The present invention is described in further detail with reference to embodiment：
Embodiment 1
(1) by thickness for 1mm electrode material matrix sheet nickel foam cut rectangle foam nickel sheet A, make its a length of
3cm, a width of 2cm；
(2) 0.25g A are immersed in the analytically pure acetone of 40ml and 0.5h, Ran Houqu is cleaned with the frequency ultrasound of 40KHz
Go out A, then B is obtained with deionized water rinsing；
(3) 0.25g B are immersed in 40ml, the hydrogenperoxide steam generator of 30% mass concentration and the surpassing for 40K Hz in frequency
0.5h is processed in acoustic environment, B is then taken out and is rinsed with absolute ethyl alcohol, place into baking oven, drying 1h in 60 DEG C of temperature obtains
C；
(4) ammonium metavanadate is dissolved in deionized water, be heated to 30 DEG C, using magnetic stirring apparatus with 500 revs/min of speed
It is the NH of 0.05mol/L that degree stirring 0.5h is obtained molar concentration4VO3Solution D；
(5) pH value of D is adjusted to 1 using the nitric acid of 2mol/L and obtains solution E；
(6) 50mL E are transferred in hydro-thermal sensing kettle, then 0.25gg C is sensed in hydro-thermal induction heating equipment
The magnetic induction line of coil is put into, and after kettle is sealed, is placed in hydro-thermal induction heating equipment, with the induction frequencies of 400KHz by room temperature liter
Temperature is incubated 1h to 70 DEG C, obtains ammonium vanadate/foam nickel composite material F；
(7) by F respectively with the deionized water and the soft washing of analytically pure absolute ethyl alcohol that temperature is room temperature, then at 50 DEG C
Temperature in dry 6h and obtain the ammonium vanadate with three-dimensional porous connectivity structure/nickel foam sodium-ion battery positive material.
It will be seen from figure 1 that positive electrode good crystallinity manufactured in the present embodiment, purity is higher；Figure it is seen that
Nickel foam/the ammonium vanadate prepared in step (7) is the vanadic acid of the three-dimensional framework framework of porous connection and surface with laminated structure
Ammonium；From figure 3, it can be seen that nickel foam manufactured in the present embodiment/ammonium vanadate positive electrode capacity is high, stable cycle performance.
Embodiment 2
(1) by thickness for 1mm electrode material matrix sheet nickel foam cut rectangle foam nickel sheet A, make its a length of
3cm, a width of 2cm；
(2) 0.50g A are immersed in the analytically pure acetone of 70ml and 1h is cleaned with the frequency ultrasound of 40KHz, then taken out
A, then obtain B with deionized water rinsing；
(3) 0.50g B are immersed in 70ml, the hydrogenperoxide steam generator of 30% mass concentration and the surpassing for 40K Hz in frequency
1h is processed in acoustic environment, B is then taken out and is rinsed with absolute ethyl alcohol, place into baking oven, drying 3h in 90 DEG C of temperature obtains C；
(4) ammonium metavanadate is dissolved in deionized water, be heated to 60 DEG C, using magnetic stirring apparatus with 800 revs/min of speed
It is the NH of 0.20mol/L that degree stirring 1h is obtained molar concentration4VO3Solution D；
(5) pH value of D is adjusted to 5 using the nitric acid of 2mol/L and obtains solution E；
(6) by 50mL E be transferred to hydro-thermal sensing kettle in, then by 0.50g C in hydro-thermal induction heating equipment the line of induction
The magnetic induction line of circle is put into, and after kettle is sealed, is placed in hydro-thermal induction heating equipment, with the induction frequencies of 800KHz by room temperature
To 180 DEG C, and 4h is incubated, obtains ammonium vanadate/foam nickel composite material F；
(7) by F respectively with the deionized water and the soft washing of analytically pure absolute ethyl alcohol that temperature is room temperature, then at 70 DEG C
Temperature in dry 12h and obtain the ammonium vanadate with three-dimensional porous connectivity structure/nickel foam sodium-ion battery positive material.
Embodiment 3
(1) by thickness for 1mm electrode material matrix sheet nickel foam cut rectangle foam nickel sheet A, make its a length of
3cm, a width of 2cm；
(2) 0.25g A are immersed in the analytically pure acetone of 55ml and 0.75h, Ran Houqu is cleaned with the frequency ultrasound of 40KHz
Go out A, then B is obtained with deionized water rinsing；
(3) 0.25g B are immersed in 55ml, the hydrogenperoxide steam generator of 30% mass concentration and the surpassing for 40K Hz in frequency
0.75h is processed in acoustic environment, B is then taken out and is rinsed with absolute ethyl alcohol, place into baking oven, drying 2h in 75 DEG C of temperature obtains
C；
(4) ammonium metavanadate is dissolved in deionized water, be heated to 45 DEG C, using magnetic stirring apparatus with 650 revs/min of speed
It is the NH of 0.125mol/L that degree stirring 0.75h is obtained molar concentration4VO3Solution D；
(5) pH value of D is adjusted to 3 using the nitric acid of 2mol/L and obtains solution E；
(6) by 50mL E be transferred to hydro-thermal sensing kettle in, then by 0.25g C in hydro-thermal induction heating equipment the line of induction
The magnetic induction line of circle is put into, and after kettle is sealed, is placed in hydro-thermal induction heating equipment, with the induction frequencies of 600KHz by room temperature
To 110 DEG C, and 2.5h is incubated, obtains ammonium vanadate/foam nickel composite material F；
(7) by F respectively with the deionized water and the soft washing of analytically pure absolute ethyl alcohol that temperature is room temperature, then at 60 DEG C
Temperature in dry 9h and obtain the ammonium vanadate with three-dimensional porous connectivity structure/nickel foam sodium-ion battery positive material.
Embodiment 4
(1) by thickness for 1mm electrode material matrix sheet nickel foam cut rectangle foam nickel sheet A, make its a length of
3cm, a width of 2cm；
(2) 0.25g A are immersed in the analytically pure acetone of 50ml and 0.6h, Ran Houqu is cleaned with the frequency ultrasound of 40KHz
Go out A, then B is obtained with deionized water rinsing；
(3) 0.25g B are immersed in 50ml, the hydrogenperoxide steam generator of 30% mass concentration and the surpassing for 40K Hz in frequency
0.6h is processed in acoustic environment, B is then taken out and is rinsed with absolute ethyl alcohol, place into baking oven, 1.5h is dried in 70 DEG C of temperature
Obtain C；
(4) ammonium metavanadate is dissolved in deionized water, be heated to 40 DEG C, using magnetic stirring apparatus with 600 revs/min of speed
It is the NH of 0.10mol/L that degree stirring 0.6h is obtained molar concentration4VO3Solution D；
(5) pH value of D is adjusted to 2 using the nitric acid of 2mol/L and obtains solution E；
(6) by 50mL E be transferred to hydro-thermal sensing kettle in, then by 0.25g C in hydro-thermal induction heating equipment the line of induction
The magnetic induction line of circle is put into, and after kettle is sealed, is placed in hydro-thermal induction heating equipment, with the induction frequencies of 500KHz by room temperature
To 130 DEG C, and 2h is incubated, obtains ammonium vanadate/foam nickel composite material F；
(7) by F respectively with the deionized water and the soft washing of analytically pure absolute ethyl alcohol that temperature is room temperature, then at 55 DEG C
Temperature in dry 8h and obtain the ammonium vanadate with three-dimensional porous connectivity structure/nickel foam sodium-ion battery positive material.
Embodiment 5
(1) by thickness for 1mm electrode material matrix sheet nickel foam cut rectangle foam nickel sheet A, make its a length of
3cm, a width of 2cm；
(2) 0.50g A are immersed in the analytically pure acetone of 60ml and 0.8h, Ran Houqu is cleaned with the frequency ultrasound of 40KHz
Go out A, then B is obtained with deionized water rinsing；
(3) 0.50g B are immersed in 60ml, the hydrogenperoxide steam generator of 30% mass concentration and the surpassing for 40K Hz in frequency
0.8h is processed in acoustic environment, B is then taken out and is rinsed with absolute ethyl alcohol, place into baking oven, 2.5h is dried in 80 DEG C of temperature
Obtain C；
(4) ammonium metavanadate is dissolved in deionized water, be heated to 50 DEG C, using magnetic stirring apparatus with 700 revs/min of speed
It is the NH of 0.15mol/L that degree stirring 0.8h is obtained molar concentration4VO3Solution D；
(5) pH value of D is adjusted to 4 using the nitric acid of 2mol/L and obtains solution E；
(6) by 50mL E be transferred to hydro-thermal sensing kettle in, then by 0.50g C in hydro-thermal induction heating equipment the line of induction
The magnetic induction line of circle is put into, and after kettle is sealed, is placed in hydro-thermal induction heating equipment, with the induction frequencies of 700KHz by room temperature
To 150 DEG C, and 3h is incubated, obtains ammonium vanadate/foam nickel composite material F；
(7) by F respectively with the deionized water and the soft washing of analytically pure absolute ethyl alcohol that temperature is room temperature, then at 65 DEG C
Temperature in dry 10h and obtain the ammonium vanadate with three-dimensional porous connectivity structure/nickel foam sodium-ion battery positive material.
Claims (10)
1. a kind of ammonium vanadate/nickel foam sodium-ion battery preparation method of self-supporting positive pole, it is characterised in that including following step
Suddenly：
1) electrode material matrix sheet nickel foam is cut to the foam nickel sheet A of rectangle；
2) A is immersed in acetone and is cleaned by ultrasonic, then take out A, then B is obtained with deionized water rinsing；
3) B is immersed in hydrogenperoxide steam generator and the treatment in ultrasound environments, then takes out B and rinsed with absolute ethyl alcohol, then put
Enter oven drying and obtain C；
4) ammonium metavanadate is dissolved in deionized water, heating, stirring are obtained NH4VO3Solution D；
5) pH value of D is adjusted to 1~5, obtains solution E；
6) E is transferred in hydro-thermal sensing kettle, is put into C, wherein adding 0.25-0.50gC in per 50mLE, after kettle is sealed, be placed in
In hydro-thermal induction heating equipment, with the induction frequencies of 400~800KHz by room temperature to 70~180 DEG C, and 1~4h is incubated,
Obtain nickel foam/ammonium vanadate composite F；
7) F is used into deionized water and the soft washing of absolute ethyl alcohol respectively, is then dried to obtain with three-dimensional porous connectivity structure
Nickel foam/ammonium vanadate sodium-ion battery positive material.
2. a kind of ammonium vanadate/nickel foam sodium-ion battery according to claim 1 preparation method of self-supporting positive pole, its
Be characterised by, step 1) in the Ni-based body thickness of sheet-formed foam be 1mm, cut A a length of 3cm, a width of 2cm.
3. a kind of ammonium vanadate/nickel foam sodium-ion battery according to claim 1 preparation method of self-supporting positive pole, its
Be characterised by, step 2) used in acetone for analysis is pure, ultrasonics cleaning frequency is 40KHz, be cleaned by ultrasonic the time for 0.5~
1h。
4. a kind of ammonium vanadate/nickel foam sodium-ion battery according to claim 1 preparation method of self-supporting positive pole, its
Be characterised by, step 3) in hydrogen peroxide mass concentration for 30%, supersonic frequency is 40K Hz, and sonication treatment time is 0.5
~1h.
5. a kind of ammonium vanadate/nickel foam sodium-ion battery according to claim 1 preparation method of self-supporting positive pole, its
Be characterised by, step 3) in drying temperature be 60~90 DEG C, the time be 1~3h.
6. a kind of ammonium vanadate/nickel foam sodium-ion battery according to claim 1 preparation method of self-supporting positive pole, its
Be characterised by, step 4) in NH4VO3Solution molar concentration is 0.05~0.20mol/L.
7. a kind of ammonium vanadate/nickel foam sodium-ion battery according to claim 1 preparation method of self-supporting positive pole, its
Be characterised by, step 4) in ammonium metavanadate is dissolved in deionized water, be heated to 30~60 DEG C, stirred using magnetic stirring apparatus
Mix, speed is 500~800 revs/min, the time is 0.5~1h.
8. a kind of ammonium vanadate/nickel foam sodium-ion battery according to claim 1 preparation method of self-supporting positive pole, its
It is characterised by, step 5) the middle nitric acid regulation pH value of solution using 2mol/L.
9. a kind of ammonium vanadate/nickel foam sodium-ion battery according to claim 1 preparation method of self-supporting positive pole, its
Be characterised by, step 6) in C induction coils in hydro-thermal induction heating equipment magnetic induction line place.
10. a kind of ammonium vanadate/nickel foam sodium-ion battery according to claim 1 preparation method of self-supporting positive pole,
Characterized in that, step 7) in F is washed using deionized water and absolute ethyl alcohol at room temperature, absolute ethyl alcohol concentration for point
Analysis is pure, and drying temperature is 50~70 DEG C in drying process, and the time is 6~12h.
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| CN109449394A (en) * | 2018-10-19 | 2019-03-08 | 陕西科技大学 | A kind of flower-shaped (NH4)2V3O8/ foam copper composite material and preparation method and application |
| CN109980198A (en) * | 2019-03-15 | 2019-07-05 | 湖南宸宇富基新能源科技有限公司 | A kind of SiO of self-supportingxBase composite negative pole material and preparation method thereof |
| CN111081983A (en) * | 2019-12-26 | 2020-04-28 | 陕西科技大学 | Co9S8Preparation method of self-supporting cathode of carbon felt sodium ion battery |
| CN114639819A (en) * | 2022-03-24 | 2022-06-17 | 中南大学 | Sodium-rich manganese-based oxide composite substrate metal oxide self-supporting binary anode material and preparation method thereof |
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| CN114639819B (en) * | 2022-03-24 | 2024-01-30 | 中南大学 | Sodium-rich manganese-based oxide composite substrate metal oxide self-supporting binary anode material and preparation method thereof |
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