CN109244414B - Bundle-shaped MoO3@ NC lithium ion battery electrode material and preparation method thereof - Google Patents

Bundle-shaped MoO3@ NC lithium ion battery electrode material and preparation method thereof Download PDF

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CN109244414B
CN109244414B CN201811139013.1A CN201811139013A CN109244414B CN 109244414 B CN109244414 B CN 109244414B CN 201811139013 A CN201811139013 A CN 201811139013A CN 109244414 B CN109244414 B CN 109244414B
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曹丽云
贺菊菊
李嘉胤
黄剑锋
贺慧
张宁
李倩颖
党欢
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Shaanxi University of Science and Technology
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Abstract

本发明提供了一种束状MoO3@NC锂离子电池电极材料，具有由纳米纤维状结构规整排列形成的束状形貌，由如下步骤得到：浓缩含有壳聚糖、及钼源的均匀溶液，得到悬浊液；冷冻干燥前述悬浊液，得到MoO3@NC前驱体；在惰性气氛下载入水蒸气对MoO3@NC前驱体进行水蒸气活化热处理，得到MoO3@NC。该MoO3@NC材料兼具容量高，导电性好，离子扩散率高，结构稳定的特点，于锂离子电池电极材料应用而言具有极大地潜力。该方法不仅操作简单，且对其他过渡金属氧化物形貌的调控具有很好的指导意义。

Figure 201811139013

The invention provides a bundled MoO3@NC lithium ion battery electrode material, which has a bundled shape formed by regular arrangement of nanofibrous structures, and is obtained by the following steps: concentrating a uniform solution containing chitosan and a molybdenum source , to obtain a suspension; freeze-dry the aforementioned suspension to obtain MoO 3 @NC precursor; add water vapor in an inert atmosphere to perform water vapor activation heat treatment on the MoO 3 @NC precursor to obtain MoO 3 @NC. The MoO 3 @NC material has the characteristics of high capacity, good conductivity, high ion diffusivity, and stable structure, and has great potential for the application of lithium-ion battery electrode materials. This method is not only simple to operate, but also has good guiding significance for the regulation of the morphology of other transition metal oxides.

Figure 201811139013

Description

Bundle-shaped MoO3@ NC lithium ion battery electrode material and preparation method thereof
Technical Field
The invention belongs to the technical field of transition metal oxide electrode materials, and particularly relates to a bundle-shaped MoO3@ NC lithium ion battery electrode material and a preparation method thereof.
Background
Lithium ion batteries have been widely used in aerospace, hybrid electric vehicles, portable electronic devices, and other fields because of their significant advantages of high specific capacity, light weight, long life, no memory, and the like. At present, the commercial graphite cathode has low energy density, and has huge potential safety hazard due to easy precipitation of lithium dendrite and action with electrolyte, thereby greatly limiting the development and application of the lithium dendrite.
Molybdenum trioxide, a transition metal oxide, has a layered structure and a framework in which extensive channels exist, and can be used as a flow channel and an intercalation site for ions. Theoretically every unit of molybdenum trioxide can be mixed with 6 units of Li+The conversion reaction occurs, so the method has higher theoretical specific capacity. However, in the process of charging and discharging, the molybdenum oxide has obvious volume effect, is easy to expand in volume, and has obvious capacity attenuation and low capacity retention rate.
In response to the above deficiency, researchers mainly studied the following aspects: (1) the shape of the material is regulated by different methods, and the material with a special structure is prepared to slow down the volume effect caused by the ion disintercalation process, such as the thermal evaporation method [ Lili Cai, Pratap M. Rao, Xiaoolin Zheng. Morphology-controlled flame synthesis of single, branched, and flow-like alpha-MoO3 nanobelt arrays[J]. Nano Letters, 2011, 11(2):872-7. ]Solvothermal method [ Sakaushi K, Thomas J, Kaskel S, et al. Aqueous solution process for the synthesis and analysis of nanostructured one-dimensional alpha-MoO3 electrode materials[J]. Chemistry of Materials, 2013, 25(12):2557-2563. ]Template-assisted method [ Zhiming Cui, Weiying Yuan, Chang Ming Li. Template-mediated growth of microspheres, microbelt and nano alpha-MoO3structures and their high pseudo-capacitances[J]. J. Mater. Chem:a, 2013, 1(41):12926-12931. ]. (2) Coating a structurally stable material, such as a single-walled carbon nanotube [ Mendoza-S ] n P S. Charge storage properties of a α-MoO3/carboxyl-functionalized single-walled carbon nanotube composite electrode in a Li ion electrolyte[J]. Electrochimica Acta, 2013, 98:294-302. ]。[ Wang Q, Sun J, Wang Q, et al. Electrochemical performance of α-MoO3–In2O3 core–shell nanorods as anode materials for lithium-ion batteries[J]. Journal of Materials Chemistry A, 2015, 3(9):5083-5091. ]。
However, the following problems are common to the above-mentioned various modification methods: (1) the synthesis process needs the auxiliary action of surfactant and the like [ dyeing Cui, wetting Yuan, Chang Ming Li. Template-modified growth of microsphere, microsphere and nano alpha-MoO3 structures and their high pseudo-capacitances[J]. J. Mater. Chem:a, 2013, 1(41):12926-12931. ](2) The cycling stability of the prepared pure-phase molybdenum oxide electrode material still needs to be improved, and after multiple cycles, the cycling stability is lower than 80% [ Wang Q, Sun J, Wang Q, et al, Electrochemical performance of alpha-MoO3–In2O3 core–shell nanorods as anode materials for lithium-ion batteries[J]. Journal of Materials Chemistry A, 2015, 3(9):5083-5091. ]。
The high-efficiency freeze drying-heat treatment method is adopted to prepare MoO with special morphology3@ NC (NC, i.e. nitrogen-doped carbon), MoO3The @ NC material has the characteristics of high capacity, good conductivity, high ion diffusivity and stable structure.
Disclosure of Invention
The invention aims to provide MoO with a special morphology3@ NC and application in preparation of lithium ion battery cathode materials. The MoO3The @ NC material has the characteristics of high capacity, good conductivity, high ion diffusivity and stable structure, and has great potential in the application of lithium ion battery electrode materials. The method is simple to operate, and has good guiding significance for regulating and controlling the shapes of other transition metal oxides.
The specific technical scheme is as follows: bundle-shaped MoO3@ NC lithium ion battery electrode materialThe preparation method comprises the following steps:
(1) weighing a certain amount of chitosan, dissolving the chitosan in 30 mL of acid solutions with different concentrations, and magnetically stirring for 30-60 min to obtain a solution A;
(2) weighing a certain amount of molybdenum source, dissolving the molybdenum source in 30 mL of deionized water, and magnetically stirring for 30-60 min to obtain a solution B;
(3) slowly adding the obtained solution B into the solution A, and continuously magnetically stirring for 1-4 hours to obtain a solution C;
(4) heating the solution C to evaporate the solvent until the volume of the solution is 0.01-0.1 time of the volume of the initial solution, so as to obtain a suspension D;
(5) freeze-drying the suspension D, and collecting a dried product as a precursor E;
(6) and (3) putting a certain amount of the precursor E into a crucible and placing the precursor E into a tube furnace, carrying out heat treatment in an inert atmosphere Ar, and simultaneously carrying water vapor through Ar to synchronously realize water vapor activation-heat treatment. The heat treatment temperature is 350-550 ℃, the time is 0.5-3 h, the heating rate is 3-20 ℃/min, the Ar flow rate is 50-200 sccm, and the target product MoO is obtained3@NC。
The amount of the chitosan in the step (1) is 0.1-1 g.
The types of the acid in the step (1) are acetic acid and hydrochloric acid.
The concentration range of the acid in the step (1) is 3-12 mol/L.
The molybdenum source in the step (2) is ammonium molybdate tetrahydrate ((NH)4)6Mo7O24·4H2O）。
0.1-1 g of the certain amount of molybdenum source in the step (2).
And (3) heating the mixed solution at 50-80 ℃ by using an electric heating sleeve to evaporate the solvent.
And (4) carrying out freeze drying at-50 to-40 ℃.
Weighing a certain amount of the freeze-dried product E in the step (5) to be 1-4 g.
Compared with the prior art, the invention can obtain the following beneficial effects:
(1) the invention adopts an efficient freeze drying-heat treatment method to prepare MoO with special morphology3@NC。
(2) MoO prepared by the invention3The @ NC material has the characteristics of high capacity, good conductivity, high ion diffusivity and stable structure, and the method has good guiding significance for regulating and controlling the shapes of other transition metal oxides.
Drawings
FIG. 1 is an X-ray diffraction analysis of the product of example 1;
FIG. 2 is an SEM image of the product of example 1 at 7.0K;
FIG. 3 is an SEM image of the product of example 1 at 40.0K.
Detailed Description
The present invention will be further illustrated with reference to the following examples, but the present invention is not limited to the following examples.
Example 1
(1) Weighing 0.5 g of chitosan, dissolving the chitosan in 30 mL of acetic acid solution with the concentration of 6 mol/L, and magnetically stirring for 30 min to obtain a solution A;
(2) 1 g of ammonium molybdate tetrahydrate ((NH) was weighed4)6Mo7O24·4H2O) is dissolved in 30 mL of deionized water, and the solution B is obtained after magnetic stirring for 30 min;
(3) slowly adding the obtained solution B into the solution A, and continuously magnetically stirring for 4 hours to obtain a solution C;
(4) heating the solution C at 60 ℃ to evaporate the solvent until the volume of the solution is 0.1 time of the volume of the initial solution, thereby obtaining a suspension D;
(5) freeze-drying the suspension D at-45 ℃, and collecting a dried product as a precursor E;
(6) 1 g of the precursor E is placed in a crucible and placed in a tube furnace, heat treatment is carried out in an inert atmosphere Ar, and meanwhile water vapor is loaded through Ar, so that water vapor activation-heat treatment is synchronously realized. The heat treatment temperature is 450 ℃, the time is 1h, the heating rate is 10 ℃/min, the Ar flow rate is 100 sccm, and the target product MoO is obtained3@NC。
FIG. 1 is an X-ray diffraction analysis chart of the product of this example. XRD characteristic peak and MoO of product in figure 13The characteristic peaks are consistent, which shows that the MoO is obtained by the molybdenum source of the invention through the water vapor activation heat treatment3. Since chitosan is a nitrogen-containing carbon source, nitrogen-doped carbon, i.e., NC, is obtained after heat treatment. The analysis shows that the invention successfully prepares the target product MoO3@NC。
FIG. 2 is an SEM image of the product of example 1 at 7.0K, and FIG. 3 is an SEM image of the product of example 1 at 40.0K. FIGS. 2 and 3 show that MoO prepared by the invention3@ NC, having a bundle-like regular morphology formed by the assembly of a plurality of nanofibrous structures.
Example 2
(1) Weighing 1 g of chitosan, dissolving the chitosan in 30 mL of 12 mol/L acetic acid solution, and magnetically stirring for 60 min to obtain a solution A;
(2) 0.1 g of ammonium molybdate tetrahydrate ((NH) was weighed4)6Mo7O24·4H2O) is dissolved in 30 mL of deionized water, and the solution B is obtained after magnetic stirring for 40 min;
(3) slowly adding the obtained solution B into the solution A, and continuously magnetically stirring for 2 hours to obtain a solution C;
(4) heating the solution C at 80 ℃ to evaporate the solvent until the volume of the solution is 0.05 times of the volume of the initial solution, thereby obtaining a suspension D;
(5) freeze-drying the suspension D at-40 ℃, and collecting a dried product as a precursor E;
(6) 4 g of the precursor E is placed in a crucible and placed in a tube furnace, heat treatment is carried out in an inert atmosphere Ar, and meanwhile water vapor is loaded through Ar, so that water vapor activation-heat treatment is synchronously realized. The heat treatment temperature is 550 ℃, the time is 0.5 h, the heating rate is 20 ℃/min, the Ar flow rate is 200 sccm, and the target product MoO is obtained3@NC。
Example 3
(1) Weighing 0.1 g of chitosan, dissolving the chitosan in 30 mL of hydrochloric acid solution with the concentration of 3 mol/L, and magnetically stirring for 40 min to obtain a solution A;
(2) 0.5 g of ammonium molybdate tetrahydrate ((NH) was weighed4)6Mo7O24·4H2O) is dissolved in 30 mL of deionized water, and the solution B is obtained after magnetic stirring for 50 min;
(3) slowly adding the obtained solution B into the solution A, and continuously magnetically stirring for 1h to obtain a solution C;
(4) heating the solution C at 50 ℃ to evaporate the solvent until the volume of the solution is 0.01 time of the volume of the initial solution, so as to obtain a suspension D;
(5) freeze-drying the suspension D at-45 ℃, and collecting a dried product as a precursor E;
(6) 2 g of the precursor E is placed in a crucible and placed in a tube furnace, heat treatment is carried out in an inert atmosphere Ar, and meanwhile water vapor is loaded through Ar, so that water vapor activation-heat treatment is synchronously realized. The heat treatment temperature is 500 ℃, the time is 1.5 h, the heating rate is 5 ℃/min, the Ar flow rate is 150 sccm, and the target product MoO is obtained3@NC。
Example 4
(1) Weighing 0.2 g of chitosan, dissolving the chitosan in 30 mL of hydrochloric acid solution with the concentration of 12 mol/L, and magnetically stirring for 50 min to obtain a solution A;
(2) 1 g of ammonium molybdate tetrahydrate ((NH) was weighed4)6Mo7O24·4H2O) is dissolved in 30 mL of deionized water, and the mixture is magnetically stirred for 60 min to obtain a solution B;
(3) slowly adding the obtained solution B into the solution A, and continuously magnetically stirring for 4 hours to obtain a solution C;
(4) heating the solution C at 60 ℃ to evaporate the solvent until the volume of the solution is 0.08 times of the volume of the initial solution, so as to obtain a suspension D;
(5) freeze-drying the suspension D at-45 ℃, and collecting a dried product as a precursor E;
(6) 3 g of the precursor E is placed in a crucible and placed in a tube furnace, heat treatment is carried out in an inert atmosphere Ar, and meanwhile water vapor is loaded through Ar, so that water vapor activation-heat treatment is synchronously realized. The heat treatment temperature is 350 DEG CThe time is 3 h, the heating rate is 3 ℃/min, the Ar flow rate is 50 sccm, and the target product MoO is obtained3@NC。
Example 5
(1) Weighing 0.8 g of chitosan, dissolving the chitosan in 30 mL of acetic acid solution with the concentration of 3 mol/L, and magnetically stirring for 45 min to obtain a solution A;
(2) 0.5 g of ammonium molybdate tetrahydrate ((NH) was weighed4)6Mo7O24·4H2O) is dissolved in 30 mL of deionized water, and the solution B is obtained after magnetic stirring for 30 min;
(3) slowly adding the obtained solution B into the solution A, and continuously magnetically stirring for 1h to obtain a solution C;
(4) heating the solution C at 60 ℃ to evaporate the solvent until the volume of the solution is 0.02 times of the volume of the initial solution, thereby obtaining a suspension D;
(5) freeze-drying the suspension D at-45 ℃, and collecting a dried product as a precursor E;
(6) 1 g of the precursor E is placed in a crucible and placed in a tube furnace, heat treatment is carried out in an inert atmosphere Ar, and meanwhile water vapor is loaded through Ar, so that water vapor activation-heat treatment is synchronously realized. The heat treatment temperature is 400 ℃, the time is 2h, the heating rate is 15 ℃/min, the Ar flow rate is 100 sccm, and the target product MoO is obtained3@NC。

Claims (6)

1.一种束状MoO3@氮掺杂碳锂离子电池电极材料的制备方法，其特征在于，包括如下步骤：1. a preparation method of beam-shaped MoO 3 @ nitrogen-doped carbon lithium ion battery electrode material, is characterized in that, comprises the steps: 浓缩含有质量比为（1~10）：（1~10）的壳聚糖与四水合钼酸铵的均匀溶液，得到悬浊液；冷冻干燥前述悬浊液，得到MoO3@氮掺杂碳前驱体；在惰性气氛下载入水蒸气350~550 ℃对MoO3@氮掺杂碳前驱体进行水蒸气活化热处理，得到MoO3@氮掺杂碳锂离子电池电极材料。Concentrate a homogeneous solution containing chitosan and ammonium molybdate tetrahydrate with a mass ratio of (1~10):(1~10) to obtain a suspension; freeze-dry the aforementioned suspension to obtain MoO 3 @nitrogen-doped carbon Precursor; the MoO 3 @nitrogen-doped carbon precursor is subjected to water vapor activation heat treatment at 350-550 ℃ in an inert atmosphere, and the MoO 3 @nitrogen-doped carbon lithium-ion battery electrode material is obtained. 2.根据权利要求1所述的一种束状MoO3@氮掺杂碳锂离子电池电极材料的制备方法，其特征在于，含有质量比为（1~10）：（1~10）的壳聚糖与四水合钼酸铵的均匀溶液，由包括以下步骤的方法得到：2 . The method for preparing a bundled MoO 3 @nitrogen-doped carbon lithium-ion battery electrode material according to claim 1 , wherein the method comprises a shell with a mass ratio of (1~10):(1~10) The homogeneous solution of polysaccharide and ammonium molybdate tetrahydrate is obtained by a method comprising the following steps: 将壳聚糖溶解在3 mol/L~12 mol/L的酸液中，配制壳聚糖浓度为3.33~33.33mg/ml的溶液，记为溶液A；Dissolve chitosan in 3 mol/L~12 mol/L acid solution to prepare a solution with a chitosan concentration of 3.33~33.33 mg/ml, denoted as solution A; 配制钼源浓度为3.33~33.33mg/ml的溶液，记为溶液B；Prepare a solution with a molybdenum source concentration of 3.33-33.33 mg/ml, denoted as solution B; 将溶液B缓慢加入溶液A中，充分搅拌，含有质量比为（1~10）：（1~10）的壳聚糖与四水合钼酸铵的均匀溶液。Slowly add solution B to solution A, stir well, and contain a homogeneous solution of chitosan and ammonium molybdate tetrahydrate with a mass ratio of (1~10):(1~10). 3.根据权利要求2所述的一种束状MoO3@氮掺杂碳锂离子电池电极材料的制备方法，其特征在于，所述3 mol/L~12 mol/L的酸液为醋酸或盐酸。3. the preparation method of a kind of bundle MoO 3 @Nitrogen-doped carbon lithium ion battery electrode material according to claim 2, is characterized in that, the acid solution of described 3 mol/L～12 mol/L is acetic acid or hydrochloric acid. 4.根据权利要求2所述的一种束状MoO3@氮掺杂碳锂离子电池电极材料的制备方法，其特征在于，浓缩含有质量比为（1~10）：（1~10）的壳聚糖与四水合钼酸铵的均匀溶液时，将该溶液加热蒸发溶剂至溶液体积为初始溶液体积的0.01~0.1倍，得到悬浊液。4 . The method for preparing a bundled MoO 3 @nitrogen-doped carbon lithium-ion battery electrode material according to claim 2 , wherein the concentration contains a mass ratio of (1~10): (1~10) When a uniform solution of chitosan and ammonium molybdate tetrahydrate is obtained, the solution is heated to evaporate the solvent until the volume of the solution is 0.01-0.1 times the volume of the initial solution to obtain a suspension. 5.根据权利要求1所述的一种束状MoO3@氮掺杂碳锂离子电池电极材料的制备方法，其特征在于，浓缩含有质量比为（1~10）：（1~10）的壳聚糖与四水合钼酸铵的均匀溶液时，在50~80℃下加热蒸发溶剂。5 . The method for preparing a bundled MoO 3 @nitrogen-doped carbon lithium-ion battery electrode material according to claim 1 , wherein the concentration contains a mass ratio of (1~10):(1~10) When a homogeneous solution of chitosan and ammonium molybdate tetrahydrate is obtained, the solvent is evaporated by heating at 50~80℃. 6.根据权利要求1所述的一种束状MoO3@氮掺杂碳锂离子电池电极材料的制备方法，其特征在于，对MoO3@氮掺杂碳前驱体进行水蒸气活化热处理采用Ar作为惰性气氛及载气，热处理温度为350~550 ℃，时间为0.5~3 h，升温速率为3~20 ℃/min，Ar流速为50~200 sccm。6. The method for preparing a bundled MoO 3 @nitrogen-doped carbon lithium-ion battery electrode material according to claim 1, wherein the MoO 3 @nitrogen-doped carbon precursor is subjected to water vapor activation heat treatment using Ar As inert atmosphere and carrier gas, the heat treatment temperature was 350-550 °C, the time was 0.5-3 h, the heating rate was 3-20 °C/min, and the Ar flow rate was 50-200 sccm.
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