CN111029553A - Sodium-ion battery positive electrode material and preparation method and application thereof - Google Patents
Sodium-ion battery positive electrode material and preparation method and application thereof Download PDFInfo
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Abstract
The embodiment of the invention discloses a sodium-ion battery positive electrode material and a preparation method and application thereof. According to the invention, the polyanion compound is added into the oxide containing the transition metal element, so that the polyanion compound is uniformly filled among particles of the oxide containing the transition metal element, and the volume change of sodium ions in the de-intercalation process is resisted by combining the stable sodium storage structure of the polyanion compound, thereby buffering the expansion of the volume of the anode material in the charging and discharging processes, reducing the contact area of the anode material and the electrolyte and improving the cycle stability of the anode material.
Description
Technical Field
The embodiment of the invention relates to the technical field of sodium-ion battery materials, in particular to a sodium-ion battery positive electrode material and a preparation method and application thereof.
Background
Sodium ion batteries have the characteristics of low cost and high safety compared to lithium ion batteries. However, sodium ion batteries also have certain limitations in use compared to lithium ion batteries, for example, as for their positive electrode materials, the following are the main limiting factors: 1) the radius of sodium ion is larger than that of lithium ion (
vs.
) The influence on the material structure is larger in the charging and discharging process, so that the capacity is attenuated more quickly compared with the lithium ion battery; 2) the kinetics of the sodium-ion battery are slow, so that the rate performance of the sodium-ion battery is poor (chemical development, 2018, 37 and 8).
Although the transition metal oxide cathode material containing manganese and/or nickel elements has high specific capacity in the prior art, the problem of electrochemical performance attenuation of the material is more and more serious along with the increase of charging and discharging times due to higher surface activity and poorer structure stability (especially, the material is more obvious in a sodium ion battery) of the electrode material. In the existing improvement method, the surface of the material is coated, although the problem is alleviated to a certain extent, because the coating material has no electrochemical activity, the increase of the coating amount can cause the reduction of the charge-discharge specific capacity of the battery in hand, and the reduction of the discharge capacity of the material (such as CN 109524649A).
Disclosure of Invention
The polyanion compound is added into the oxide containing the transition metal element, so that the polyanion compound is uniformly filled among particles of the oxide containing the transition metal element, and the volume change of sodium ions in the de-intercalation process is resisted by combining the sodium storage performance of the polyanion compound, so that the expansion of the volume of the positive electrode material in the charge-discharge process is buffered, the contact area of the positive electrode material and the electrolyte is reduced, and the cycle stability of the positive electrode material is improved.
In order to achieve the above object, an embodiment of the present invention provides the following:
in one aspect of an embodiment of the present invention, there is provided a positive electrode material for a sodium ion battery, including an oxide containing a transition metal element, and a polyanion compound.
In a preferred embodiment of the present invention, the transition metal element-containing oxide is NaxMyOzSaid polyanion compound is NaaMbVc(PO4)dFe(ii) a Wherein the content of the first and second substances,
NaxMyOzwherein M comprises at least Mn, and optionally one or more of Ni, Li, Mg, Cu, Zn, Co, Ca, Ba, Sr, Al, B, Cr, Zr, Ti, Sn, V, Mo, Ru, Nb, Sb and Nb, and 0.5<x<1.5，y≥1，z≥1；
NaaMbVc(PO4)dFeWherein M is selected from one or more of O, Ti, Fe and Mn, a is more than or equal to 1, b is more than or equal to 0, c is more than or equal to 0, d is more than or equal to 1, and e is more than or equal to 0.
As a preferable embodiment of the present invention, Na is mentionedxMyOzIs NafCugFehMniM(1-g-h-i)O2And NafCugFehMniM(1-g-h-i)O2Wherein M is one or more selected from Li, Ni, Mg, Al, Cr, Ti, Mo, Nb and V, and 0.5<f≤1.5。
In a preferred embodiment of the present invention, the weight ratio of the oxide containing a transition metal element to the polyanion compound is 1:0.001 to 2.
As a preferred aspect of the present invention, the polyanionic compound is a polyanionic compound nanoparticle, or is provided by a polyanionic compound nanoparticle complex containing a conductive material.
In another aspect of the embodiment of the present invention, there is also provided a preparation method of the positive electrode material for a sodium-ion battery, including ball-milling and mixing an oxide containing a transition metal element and a polyanion compound to prepare the positive electrode material for a sodium-ion battery.
As a preferred scheme of the invention, the ball milling process is carried out in an inert atmosphere environment, the rotating speed of the ball milling process is 200-300 r/min, and the ball milling time is 12-36 h.
As a preferable scheme of the invention, the material-ball ratio in ball milling is 1: 15-25.
In another aspect of the embodiment of the invention, the application of the positive electrode material of the sodium-ion battery in the sodium-ion battery is also provided.
The embodiment of the invention has the following advantages:
1) according to the invention, the polyanion compound is mixed and filled among the particles of the oxide containing the transition metal element, so that the volume change of sodium ions in the de-intercalation process can be relieved to a certain extent by virtue of the stable structure of the polyanion compound, thereby effectively reducing the contact area between the anode material and the electrolyte and reducing the side reaction between the electrode materials;
2) the polyanion compound has stable structure and can provide capacity, so that a certain capacity can be provided for the whole battery cathode material, the structural stability of the cathode material is maintained, and the cycle stability of the cathode material is further improved.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below. It should be apparent that the drawings in the following description are merely exemplary, and that other embodiments can be derived from the drawings provided by those of ordinary skill in the art without inventive effort.
The structures, ratios, sizes, and the like shown in the present specification are only used for matching with the contents disclosed in the specification, so as to be understood and read by those skilled in the art, and are not used to limit the conditions that the present invention can be implemented, so that the present invention has no technical significance, and any structural modifications, changes in the ratio relationship, or adjustments of the sizes, without affecting the effects and the achievable by the present invention, should still fall within the range that the technical contents disclosed in the present invention can cover.
Fig. 1 is an SEM image of a positive electrode material a3 of a battery produced in example 3 of the present invention;
fig. 2 is an SEM image of a positive electrode material D1 of the battery prepared in comparative example 1 of the present invention;
fig. 3 is a graph showing cycle characteristics of a battery applied with the battery positive electrode material a3 obtained in example 3 of the present invention;
fig. 4 is a graph showing cycle characteristics of a battery applied to a battery using the battery cathode material D1 prepared in comparative example 1 of the present invention.
Detailed Description
The present invention is described in terms of particular embodiments, other advantages and features of the invention will become apparent to those skilled in the art from the following disclosure, and it is to be understood that the described embodiments are merely exemplary of the invention and that it is not intended to limit the invention to the particular embodiments disclosed. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a positive electrode material of a sodium-ion battery, which comprises an oxide containing a transition metal element and a polyanion compound.
In a preferred embodiment of the invention, in order to make the prepared cathode material have better cycle stability in the application of the cathode material in a sodium ion battery, the cycle stability is further reducedThe degree of the electrochemical performance degradation occurring during the cycle of the method is that the oxide containing the transition metal element is NaxMyOzSaid polyanion compound is NaaMbVc(PO4)dFe(ii) a Wherein the content of the first and second substances,
NaxMyOzwherein M comprises at least Mn, and optionally one or more of Ni, Li, Mg, Cu, Zn, Co, Ca, Ba, Sr, Al, B, Cr, Zr, Ti, Sn, V, Mo, Ru, Nb, Sb and Nb, and 0.5<x<1.5，y≥1，z≥1；
NaaMbVc(PO4)dFeWherein M is selected from one or more of O, Ti, Fe and Mn, a is more than or equal to 1, b is more than or equal to 0, c is more than or equal to 0, d is more than or equal to 1, and e is more than or equal to 0. Of course, a, b, c, d and e herein may be further selected as integers. Meanwhile, it is to be noted that Na herexMyOzX, y and z in (A) are required so that the respective elements in the entire chemical formula satisfy charge balance, and likewise, NaaMbVc(PO4)dFeA, b, c, d and e in (a), (b), (c), (d) and (e) also need to be such that each element in the entire formula satisfies charge balance. Of course, the specific determination of the charge balance value can be determined according to the positive and negative ions and their valence states, which can be understood by those skilled in the art. Meanwhile, here, M may be further selected to include at least Mn, or at least two types of Mn and Ni.
In a more specific and preferred embodiment of the invention, the Na isxMyOzIs NafCugFehMniM(1-g-h-i)O2And NafCugFehMniM(1-g-h-i)O2Wherein M is one or more selected from Li, Ni, Mg, Al, Cr, Ti, Mo, Nb and V, and 0.5<f≤1.5。
The content ratio of the above-mentioned raw materials can be selected within a wide range, and it is a matter of course that in a more preferred embodiment of the present invention, the weight ratio of the oxide containing the transition metal element to the polyanion compound is 1:0.001 to 2.
Further, the polyanion compound can be any existing form of polyanion compound, and in a preferred embodiment of the invention, in order to enable the polyanion compound to be better inserted into sodium oxide, and to better effectively reduce the change of the volume of the polyanion compound in the process of sodium extraction, and the like, the stability of the whole cathode material is further improved, the polyanion compound is a polyanion compound nanoparticle, and in another mode, the polyanion compound can also be a polyanion compound nanoparticle compound containing a conductive material. Of course, the conductive material may be any suitable material, such as carbon, or other conductive material.
The invention also provides a preparation method of the positive electrode material of the sodium-ion battery, which comprises the step of ball-milling and mixing the oxide containing the transition metal element and the polyanion compound to prepare the positive electrode material of the sodium-ion battery.
In a preferred embodiment of the present invention, the ball milling process is performed under an inert atmosphere, the rotation speed of the ball milling process is 200 to 300r/min, and the ball milling time is 12 to 36 hours.
In a further preferred embodiment, the ratio of material balls in the ball milling is 1: 15-25.
The invention also provides an application of the positive electrode material of the sodium-ion battery in the sodium-ion battery. Of course, the specific application field can be adjusted according to the actual situation, and any field capable of using the sodium ion battery can be applied, for example, the wind power field, the electric device and other fields.
The following is a further description by way of specific examples.
The NFM, the NCFM and the CFM are synthesized by a high-temperature solid phase method, and the specific preparation method comprises the following steps:
NFM preparation: refer to the description of J Alloy company 794(2019) page 509-2CO3、Fe2O3、MnO2NiO is mixed evenly according to a certain proportion, and thenPlacing the mixture in a tube furnace to be roasted for 10-24h at the temperature of 800-1000 ℃ to obtain NFM;
NCFM preparation steps: referring to the records of "science and technology of energy storage", Vol.5, No.3, 2016, 5 months, Na2CO3、CuO、Fe2O3、MnO2And NiO are uniformly mixed according to a certain proportion, and then the mixture is placed in a tube furnace to be roasted for 10 to 24 hours at the temperature of 800-;
and (3) CFM preparation steps: with reference to the description in Chin. Phys. B, Vol.24, No.3(2015)038202, Na2CO3、CuO、Fe2O3、MnO2Uniformly mixing according to a certain proportion, and then placing the mixture in a tube furnace to be roasted for 10-24h at the temperature of 800-;
the specific preparation method of NOVPF comprises the following steps: with reference to the description of Joule 2, 2348-3Followed by the addition of an amount of NaH2PO4And NaF, stirring for 6-12h, and centrifuging and drying to obtain the NOVPF.
Example 1
Under inert atmosphere, NaNi0.34Fe0.33Mn0.33O2(abbreviated as NFM) and Na3O2V2(PO4)2F (abbreviated NOVPF) was as follows: a weight ratio of 0.002 was placed in a stainless steel ball mill jar. The mass ratio of the material balls is 1: 20. And carrying out ball milling for 12-36 h under the condition that the rotating speed is 250r/min to obtain the battery anode material A1.
Example 2
The preparation was carried out as in example 1, except that the weight ratio of NFM to NOVPF was 1: 0.008, and obtaining a battery cathode material A2.
Example 3
The preparation was carried out as in example 1, except that the weight ratio of NFM to NOVPF was 1:0.01, a battery positive electrode material A3 was obtained. The resulting SEM image is shown in FIG. 1.
Example 4
The preparation was carried out as in example 1, except that the weight ratio of NFM to NOVPF was 1: 0.02, a battery positive electrode material A4 was obtained.
Example 5
Under inert atmosphere, NaNi0.23Cu0.11Fe0.33Mn0.33O2(abbreviated as NCFM) and Na3O2V2(PO4)2F is placed in a stainless steel ball milling tank according to the weight ratio of 1: 0.01. The mass ratio of the material balls is 1: 20. And carrying out ball milling for 12-36 h under the condition that the rotating speed is 250r/min to obtain the battery anode material A5.
Example 6
Adding Na under inert atmosphere0.9Cu0.22Fe0.30Mn0.48O2(abbreviated CFM) and Na3O2V2(PO4)2F is placed in a stainless steel ball milling tank according to the weight ratio of 1: 0.01. The mass ratio of the material balls is 1: 20. And carrying out ball milling for 12-36 h under the condition that the rotating speed is 250r/min to obtain the battery anode material A6.
Comparative example 1
The NFM in example 1 was directly used as a battery positive electrode material D1. The resulting SEM image is shown in FIG. 2.
Comparative example 2
The NCFM in example 5 was directly used as a battery positive electrode material D2.
Comparative example 3
CFM in example 5 was used directly as battery positive electrode material D3.
Test example
The sodium ion batteries prepared by respectively assembling the A1-A6 and the D1-D3 serving as battery anode materials are tested for 200 times in a circulating way, and the obtained results are shown in Table 1. Wherein, the cycle performance graphs of A3 and D1 are shown in FIG. 3 and FIG. 4 respectively.
The test results herein were tested for assembly into a CR2032 button cell.
TABLE 1
| Numbering | Capacity retention (%) |
| A1 | 90.1 |
| A2 | 92.1 |
| A3 | 93.5 |
| A4 | 91.8 |
| A5 | 94.2 |
| A6 | 92.8 |
| D1 | 86.2 |
| D2 | 85.4 |
| D3 | 82.0 |
According to the test examples, after the battery is cycled for 200 times, the capacity retention rate of the sodium-ion battery adopting the battery cathode material prepared by the invention can still reach more than 90%, and the capacity retention rate of the sodium-ion battery adopting the common cathode material is obviously greatly reduced and is below 87%.
Although the invention has been described in detail above with reference to a general description and specific examples, it will be apparent to one skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (9)
1. The positive electrode material of the sodium-ion battery is characterized by comprising an oxide containing a transition metal element and a polyanion compound.
2. The positive electrode material for sodium-ion batteries according to claim 1, wherein the transition metal element-containing oxide is NaxMyOzSaid polyanion compound is NaaMbVc(PO4)dFe(ii) a Wherein the content of the first and second substances,
NaxMyOzwherein M comprises at least Mn, and optionally one or more of Ni, Li, Mg, Cu, Zn, Co, Ca, Ba, Sr, Al, B, Cr, Zr, Ti, Sn, V, Mo, Ru, Nb, Sb and Nb, and 0.5<x<1.5，y≥1，z≥1；
NaaMbVc(PO4)dFeWherein M is selected from one or more of O, Ti, Fe and Mn, a is more than or equal to 1, b is more than or equal to 0, c is more than or equal to 0, d is more than or equal to 1, and e is more than or equal to 0.
3. The positive electrode material for sodium-ion battery according to claim 2, wherein the Na isxMyOzIs NafCugFehMniM(1-g-h-i)O2And NafCugFehMniM(1-g-h-i)O2Wherein M is one or more selected from Li, Ni, Mg, Al, Cr, Ti, Mo, Nb and V, and 0.5<f≤1.5。
4. The positive electrode material for a sodium-ion battery according to any one of claims 1 to 3, wherein the weight ratio of the oxide containing a transition metal element to the polyanion compound is 1:0.001 to 2.
5. A sodium-ion battery positive electrode material according to any one of claims 1 to 3, wherein the polyanionic compound is a nanoparticle of a polyanionic compound or is provided by a nanoparticle composite of a polyanionic compound containing a conductive material.
6. A preparation method of the positive electrode material of the sodium-ion battery according to any one of claims 1 to 5, characterized by comprising the step of ball-milling and mixing an oxide containing a transition metal element and a polyanion compound to prepare the positive electrode material of the sodium-ion battery.
7. The preparation method of the sodium-ion battery cathode material as claimed in claim 6, wherein the ball milling process is carried out in an inert atmosphere, the rotation speed of the ball milling process is 200-300 r/min, and the ball milling time is 12-36 h.
8. The preparation method of the positive electrode material of the sodium-ion battery as claimed in claim 6 or 7, wherein the ratio of material to ball in ball milling is 1: 15-25.
9. Use of the positive electrode material for sodium-ion batteries according to any one of claims 1 to 5 in sodium-ion batteries.
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| CN114156452A (en) * | 2021-11-30 | 2022-03-08 | 上海瑞浦青创新能源有限公司 | Sodium ion positive electrode material and preparation method and application thereof |
| CN115000374A (en) * | 2022-06-13 | 2022-09-02 | 星恒电源股份有限公司 | Composite positive electrode material, sodium ion battery positive plate and sodium ion battery |
| CN115241422A (en) * | 2022-06-21 | 2022-10-25 | 上海璞钠能源科技有限公司 | Positive electrode material for sodium ion battery and preparation method thereof |
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| CN115241422A (en) * | 2022-06-21 | 2022-10-25 | 上海璞钠能源科技有限公司 | Positive electrode material for sodium ion battery and preparation method thereof |
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Application publication date: 20200417 |