Sodium-ion battery negative electrode material and preparation method thereof

Abstract

The application provides a kind of sodium ion battery negative material and its preparation method, it is related to battery technical field.The application is in the suspension of graphene oxide is added NiSn (OH) 6 nanosphere, cobalt nitrate and urea, stirring to obtain mixed solution after;The mixed solution is heated to 50~80 DEG C and is kept for 2-3h, after reaction is completed, cooling to room temperature, obtain suspension liquid;The suspension liquid is carried out solid-liquid separation, and the precipitate is obtained;Finally, the precipitate is washed, dried and carbonized, and the sodium ion battery negative material is obtained after cooling.The sodium ion battery prepared by the sodium ion battery negative material of the application can significantly improve the capacity and cycle life of the sodium ion battery.The preparation method of the sodium ion battery negative material is simple and low in cost.

Description

Technical Field

[0001] This invention provides a sodium-ion battery anode material and its preparation method, belonging to the field of battery technology. Background Technology

[0002] Sodium-ion batteries are rechargeable batteries that use sodium ions as charge carriers. Their working principle is similar to that of lithium-ion batteries, storing and releasing electrical energy through the insertion and extraction of sodium ions between the positive and negative electrodes. Compared to lithium-ion batteries, sodium batteries exhibit unique advantages in terms of resources, cost, and safety.

[0003] The electrode materials of sodium-ion batteries are the core factors that determine their performance. Among them, the negative electrode material of sodium-ion batteries directly determines the battery's capacity, cycle life, rate performance, and cost. Summary of the Invention

[0004] Based on this, the present invention provides a sodium-ion battery anode material and its preparation method.

[0005] The present invention is specifically implemented using the following technical solutions:

[0006] A method for preparing a sodium-ion battery anode material includes the following steps:

[0007] (1) Disperse graphene oxide in a solvent to form a uniform graphene oxide suspension.

[0008] (2) Add NiSn(OH)6 nanospheres, cobalt nitrate and urea to the graphene oxide suspension and stir until a mixed solution is obtained;

[0009] (3) Heat the mixed solution to 50~80℃ and keep it at that temperature for 2-3 hours. After the reaction is complete, cool it to room temperature to obtain a suspension.

[0010] (4) The suspension is subjected to solid-liquid separation to obtain a precipitate;

[0011] (5) The precipitate is washed, dried and then carbonized, and cooled to obtain a sodium-ion battery negative electrode material, wherein the carbonization is carried out at 700~800℃ for 3~5h in an inert atmosphere.

[0012] Preferably, the solvent in step (1) is deionized water.

[0013] Preferably, the mass percentages of each component in the mixed solution in step (2) are as follows:

[0014] Graphene oxide 10-30%,

[0015] NiSn(OH)6 nanospheres 1~5%,

[0016] Cobalt nitrate 3~10%,

[0017] Urea 0.1~0.2%.

[0018] Preferably, in step (2), the stirring speed is 500~800 rpm and the stirring time is 10~30 min.

[0019] Preferably, the heating temperature in step (3) is 60~70℃.

[0020] Preferably, the washing in step (5) involves rinsing with deionized water and ethanol in sequence.

[0021] Preferably, the drying temperature in step (5) is 60~80℃.

[0022] Preferably, the drying time in step (5) is 10~24h.

[0023] This invention also protects a sodium-ion battery anode material prepared using the above method.

[0024] Compared with the prior art, the present invention has the following beneficial effects:

[0025] The sodium-ion battery anode material of this invention can be used to prepare sodium-ion batteries, which can significantly improve the capacity and cycle life of sodium-ion batteries. The preparation method of the sodium-ion battery anode material of this invention is simple and low in cost. Attached Figure Description

[0026] Figure 1 SEM image of the sodium-ion battery anode material prepared in Example 1;

[0027] Figure 2 This is a SEM image of the sodium-ion battery anode material prepared in Example 2. Detailed Implementation

[0028] To make the objectives, technical solutions, and advantages of this invention clearer, the preferred embodiments of this invention will be described in further detail below with reference to the examples. All other embodiments obtained by those skilled in the art based on the embodiments of this invention without inventive effort are within the scope of protection of this invention. The NiSn(OH)6 nanospheres of this invention are prepared according to the scheme described in Example 1 of CN111987306 B.

[0029] Example 1

[0030] A method for preparing a sodium-ion battery anode material includes the following steps:

[0031] (1) Graphene oxide is dispersed in deionized water to form a uniform graphene oxide suspension.

[0032] (2) NiSn(OH)6 nanospheres, cobalt nitrate, and urea were added to the graphene oxide suspension, and then stirred at 600 rpm for 20 min to obtain a mixed solution; the mass percentage of each component in the mixed solution is as follows:

[0033] 25% graphene oxide

[0034] 2% NiSn(OH)6 nanospheres

[0035] Cobalt nitrate 7%,

[0036] Urea 0.1%.

[0037] (3) Heat the mixed solution to 70°C and keep it at that temperature for 2 hours. After the reaction is complete, cool it to room temperature to obtain a suspension.

[0038] (4) The suspension is subjected to solid-liquid separation to obtain a precipitate;

[0039] (5) The precipitate was washed three times with deionized water and ethanol, then dried at 80°C for 24 hours and carbonized (the carbonization was carried out at 800°C for 3 hours under nitrogen atmosphere), and then cooled to obtain sodium-ion battery anode material.

[0040] Example 2

[0041] A method for preparing a sodium-ion battery anode material includes the following steps:

[0042] (1) Graphene oxide is dispersed in deionized water to form a uniform graphene oxide suspension.

[0043] (2) NiSn(OH)6 nanospheres, cobalt nitrate, and urea were added to the graphene oxide suspension, and then stirred at 500 rpm for 30 min to obtain a mixed solution; the mass percentage of each component in the mixed solution is as follows:

[0044] 25% graphene oxide

[0045] 2% NiSn(OH)6 nanospheres

[0046] Cobalt nitrate 5%,

[0047] Urea 0.1%.

[0048] (3) Heat the mixed solution to 60°C and keep it at that temperature for 2 hours. After the reaction is complete, cool it to room temperature to obtain a suspension.

[0049] (4) The suspension is subjected to solid-liquid separation to obtain a precipitate;

[0050] (5) The precipitate was washed three times with deionized water and ethanol, then dried at 60°C for 24 hours and carbonized (the carbonization was carried out at 800°C for 3 hours under nitrogen atmosphere), and cooled to obtain sodium-ion battery anode material.

[0051] Example 3

[0052] A method for preparing a sodium-ion battery anode material includes the following steps:

[0053] (1) Graphene oxide is dispersed in deionized water to form a uniform graphene oxide suspension.

[0054] (2) NiSn(OH)6 nanospheres, cobalt nitrate, and urea were added to the graphene oxide suspension, and then stirred at 800 rpm for 30 min to obtain a mixed solution; the mass percentage of each component in the mixed solution is as follows:

[0055] 15% graphene oxide

[0056] 1% NiSn(OH)6 nanospheres

[0057] Cobalt nitrate 3%,

[0058] Urea 0.2%.

[0059] (3) The mixed solution was heated to 80°C and kept at that temperature for 3 hours. After the reaction was completed, it was cooled to room temperature to obtain a suspension.

[0060] (4) The suspension is subjected to solid-liquid separation to obtain a precipitate;

[0061] (5) The precipitate was washed three times with deionized water and ethanol, then dried at 80°C for 24 hours and carbonized (the carbonization was carried out at 800°C for 3 hours under nitrogen atmosphere), and then cooled to obtain sodium-ion battery anode material.

[0062] Example 4

[0063] A method for preparing a sodium-ion battery anode material includes the following steps:

[0064] (1) Graphene oxide is dispersed in deionized water to form a uniform graphene oxide suspension.

[0065] (2) NiSn(OH)6 nanospheres, cobalt nitrate, and urea were added to the graphene oxide suspension, and then stirred at 800 rpm for 10 min to obtain a mixed solution; the mass percentage of each component in the mixed solution is as follows:

[0066] 30% graphene oxide

[0067] 1% NiSn(OH)6 nanospheres

[0068] Cobalt nitrate 10%,

[0069] Urea 0.2%.

[0070] (3) Heat the mixed solution to 60°C and keep it at that temperature for 3 hours. After the reaction is complete, cool it to room temperature to obtain a suspension.

[0071] (4) The suspension is subjected to solid-liquid separation to obtain a precipitate;

[0072] (5) The precipitate was washed three times with deionized water and ethanol, then dried at 80°C for 24 hours and carbonized (the carbonization was carried out at 800°C for 3 hours under nitrogen atmosphere), and then cooled to obtain sodium-ion battery anode material.

[0073] Example 5

[0074] A method for preparing a sodium-ion battery anode material includes the following steps:

[0075] (1) Graphene oxide is dispersed in deionized water to form a uniform graphene oxide suspension.

[0076] (2) NiSn(OH)6 nanospheres, cobalt nitrate, and urea were added to the graphene oxide suspension, and then stirred at 600 rpm for 30 min to obtain a mixed solution; the mass percentage of each component in the mixed solution is as follows:

[0077] 10% graphene oxide

[0078] NiSn(OH)6 nanospheres 5%,

[0079] Cobalt nitrate 5%,

[0080] Urea 0.1%.

[0081] (3) Heat the mixed solution to 60°C and keep it at that temperature for 2 hours. After the reaction is complete, cool it to room temperature to obtain a suspension.

[0082] (4) The suspension is subjected to solid-liquid separation to obtain a precipitate;

[0083] (5) The precipitate was washed three times with deionized water and ethanol, then dried at 60°C for 24 hours and carbonized (the carbonization was carried out at 800°C for 3 hours under nitrogen atmosphere), and cooled to obtain sodium-ion battery anode material.

[0084] Example 6

[0085] A method for preparing a sodium-ion battery anode material includes the following steps:

[0086] (1) Graphene oxide is dispersed in deionized water to form a uniform graphene oxide suspension.

[0087] (2) NiSn(OH)6 nanospheres, cobalt nitrate, and urea were added to the graphene oxide suspension, and then stirred at 700 rpm for 20 min to obtain a mixed solution; the mass percentage of each component in the mixed solution is as follows:

[0088] 18% graphene oxide

[0089] NiSn(OH)6 nanospheres 3%,

[0090] Cobalt nitrate 4%,

[0091] Urea 0.1%.

[0092] (3) The mixed solution was heated to 80°C and kept at that temperature for 3 hours. After the reaction was completed, it was cooled to room temperature to obtain a suspension.

[0093] (4) The suspension is subjected to solid-liquid separation to obtain a precipitate;

[0094] (5) The precipitate was washed three times with deionized water and ethanol, then dried at 80°C for 24 hours and carbonized (the carbonization was carried out at 800°C for 3 hours under nitrogen atmosphere), and then cooled to obtain sodium-ion battery anode material.

[0095] Example 7

[0096] A method for preparing a sodium-ion battery anode material includes the following steps:

[0097] (1) Graphene oxide is dispersed in deionized water to form a uniform graphene oxide suspension.

[0098] (2) NiSn(OH)6 nanospheres, cobalt nitrate, and urea were added to the graphene oxide suspension, and then stirred at 800 rpm for 30 min to obtain a mixed solution; the mass percentage of each component in the mixed solution is as follows:

[0099] Graphene oxide 22%,

[0100] NiSn(OH)6 nanospheres 3%,

[0101] Cobalt nitrate 10%,

[0102] Urea 0.2%.

[0103] (3) The mixed solution was heated to 80°C and kept at that temperature for 3 hours. After the reaction was completed, it was cooled to room temperature to obtain a suspension.

[0104] (4) The suspension is subjected to solid-liquid separation to obtain a precipitate;

[0105] (5) The precipitate was washed three times with deionized water and ethanol, then dried at 80°C for 24 hours and carbonized (the carbonization was carried out at 800°C for 3 hours under nitrogen atmosphere), and then cooled to obtain sodium-ion battery anode material.

[0106] The sodium-ion battery anode materials prepared in Examples 1-7 were used to prepare sodium-ion battery anode sheets and assembled into coin cells. The cells were tested at a current density of 100 mAg. -1 The tests were conducted within a voltage range of 0.4-2.6V, and the results are shown in Table 1.

[0107] Table 1

[0108]

[0109] As can be seen from Table 1, the sodium-ion battery prepared using the sodium-ion battery anode material of the present invention can significantly improve the capacity and cycle life of the sodium-ion battery.

[0110] The embodiments described above are some, but not all, embodiments of the present invention. The detailed description of the embodiments of the present invention is not intended to limit the scope of the claimed invention, but merely to illustrate selected embodiments. All other embodiments obtained by those skilled in the art based on the embodiments of the present invention without inventive effort are within the scope of protection of the present invention.

Claims

1. A method for preparing a sodium-ion battery anode material, characterized in that, Includes the following steps: (1) Graphene oxide is dispersed in deionized water to form a uniform graphene oxide suspension. (2) NiSn(OH)6 nanospheres, cobalt nitrate, and urea were added to the graphene oxide suspension and stirred until a mixed solution was obtained. The mass percentages of each component in the mixed solution were as follows: graphene oxide 10-30%, NiSn(OH)6 nanospheres 1-5%, cobalt nitrate 3-10%, and urea 0.1-0.2%. (3) Heat the mixed solution to 50~80℃ and keep it at that temperature for 2-3 hours. After the reaction is complete, cool it to room temperature to obtain a suspension. (4) The suspension is subjected to solid-liquid separation to obtain a precipitate; (5) The precipitate is washed, dried and carbonized, and then cooled to obtain a sodium-ion battery anode material.

2. The method for preparing the sodium-ion battery negative electrode material according to claim 1, characterized in that, In step (2), the stirring speed is 500~800 rpm and the stirring time is 10~30 min.

3. The method for preparing the sodium-ion battery negative electrode material according to claim 1, characterized in that, The heating temperature in step (3) is 60~70℃.

4. The method for preparing the sodium-ion battery negative electrode material according to claim 1, characterized in that, The washing process in step (5) involves rinsing with deionized water and ethanol in sequence.

5. The method for preparing the sodium-ion battery negative electrode material according to claim 1, characterized in that, The drying temperature in step (5) is 60~80℃.

6. The method for preparing the sodium-ion battery negative electrode material according to claim 1, characterized in that, The drying time in step (5) is 10~24 h.

7. A sodium-ion battery anode material, characterized in that, It is prepared using any one of the methods described in claims 1 to 6.

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