CN111584849B - Nano zinc oxide composite material applied to secondary battery - Google Patents
Nano zinc oxide composite material applied to secondary battery Download PDFInfo
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- H01—ELECTRIC ELEMENTS
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
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- B—PERFORMING OPERATIONS; TRANSPORTING
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Abstract
The invention relates to the technical field of new material processing, and discloses a nano zinc oxide composite material applied to a secondary battery, wherein the prepared composite material formed by nano zinc oxide and silicon has excellent conductivity and mechanical strength, and the composite material is applied to the preparation of a secondary battery cathode material, is used as a battery cathode to improve the cycle performance of the secondary battery, has larger charge and discharge performance and excellent reversibility, and solves corresponding problems caused by silicon expansion and the like in the charge and discharge process; the negative electrode material prepared from the nano zinc oxide-silicon composite material prepared by the invention has the effects of increasing the conductivity of silicon, buffering the expansion of silicon in the charging and discharging processes, and performing charging and discharging and cycle performance tests, wherein the retention rate reaches 64-66% after 100 times of charging and discharging cycles under the current density of 0.5A/g.
Description
Technical Field
The invention belongs to the technical field of new material processing, and particularly relates to a nano zinc oxide composite material applied to a secondary battery.
Background
The nano zinc oxide refers to zinc oxide particles with the grain size of below 100 nanometers, and as a high-performance semiconductor material, the nano zinc oxide shows a plurality of special properties such as non-toxicity, non-migration, fluorescence, piezoelectricity, ultraviolet absorption and scattering capacity and the like due to the unique small-size effect, surface effect, quantum size effect, macroscopic quantum tunneling effect and dielectric confinement effect. Therefore, the nano-material has wide application prospect in the fields of antibacterial materials, luminescent materials, piezoelectric materials, ultraviolet shielding materials, self-cleaning materials, cell calibration materials, nano-catalysts and the like. The characteristics of the zinc oxide nanoparticles are closely related to the physical characteristics of the zinc oxide nanoparticles. How to select a proper surface modifier, prepare the nano zinc oxide material with controllable size and shape by a solution chemical method, expand the application field of the nano zinc oxide material, and obtain a nano product with excellent application performance is one of the hot problems in the research of the nano zinc oxide material at present.
Due to synergistic effect and other effects in the preparation of the nano composite material, the composite material shows one or more new functions which are often not possessed by the original substance, and the appearance of the new functions opens up a new application field of the nano material. Due to its superior performance and wide application prospect, it is one of the hot spots in the current scientific research of nano materials. At present, the research on the nano zinc oxide in the technical field of electrochemical functions is not yet mature, the nano zinc oxide is not applied well basically, and a huge development space exists.
Disclosure of Invention
The invention aims to solve the existing problems and provides a nano zinc oxide composite material applied to a secondary battery, and the prepared composite material formed by nano zinc oxide and silicon is used as a battery cathode to improve the cycle performance of the secondary battery.
The invention is realized by the following technical scheme:
the nanometer zinc oxide composite material for secondary battery has optimized scheme,
(1) weighing 2.5-2.7 g of nano silicon powder, adding the nano silicon powder into 15-20 ml of 20-30% polyethylene glycol aqueous solution under stirring, stirring the mixture for 10-15 minutes at the speed of 300-350 revolutions per minute, and performing ultrasonic dispersion for 10-20 minutes to obtain nano silicon dispersion liquid; the polyethylene glycol aqueous solution is prepared from polyethylene glycol with the molecular weight of 600;
(2) weighing 17.5-18.0 g of zinc nitrate, placing the zinc nitrate into a beaker, adding deionized water into the beaker under stirring at the speed of 200-240 r/min, continuously stirring until the zinc nitrate is dissolved, preparing a zinc nitrate solution with the molar concentration of 0.42-0.45 mol/l, dropwise adding a sodium hydroxide solution with the molar concentration of 2.6-2.8 mol/l into the beaker at the temperature of 48-50 ℃, adjusting the pH value of the system to be 8.2-8.3, and stirring for 25-30 minutes under a magnetic stirrer to obtain a solid-liquid mixture;
(3) adding the nano-silicon dispersion liquid into the prepared solid-liquid mixture, quickly stirring for 8-10 minutes at 900 revolutions per minute of 800-.
The grain size of the nano silicon powder is between 22 and 28 nanometers.
The grain size of the prepared nano zinc oxide composite material is between 45 and 55 nanometers.
Compared with the prior art, the invention has the following advantages: in order to solve the problems that the research on the existing nano zinc oxide in the technical field of electrochemical functions, particularly on secondary batteries is still immature and better application is not achieved, the invention provides a nano zinc oxide composite material applied to the secondary batteries, the prepared nano zinc oxide and silicon composite material has excellent conductivity and mechanical strength, and the nano zinc oxide and silicon composite material is applied to the preparation of a secondary battery cathode material and used as a battery cathode to improve the cycle performance of the secondary batteries, has larger charge and discharge performance and excellent reversibility, and solves the corresponding problems caused by the expansion of silicon and the like in the charge and discharge process; the negative electrode material prepared from the nano zinc oxide-silicon composite material prepared by the invention has the effects of increasing the conductivity of silicon, buffering the expansion of silicon in the charging and discharging processes, and performing charging and discharging and cycle performance tests, wherein the retention rate reaches 64-66% after 100 times of charging and discharging cycles under the current density of 0.5A/g; the invention can obviously improve the electrochemical activity of the nano zinc oxide composite material and solve the problem of poor application effect of the existing nano zinc oxide in the field of electrochemical functions, and the composite material has the characteristics of high conductivity, thermal stability, long cycle life, easily obtained preparation raw materials, simple synthesis mode, low cost, stable chemical performance, high mechanical strength and the like. The nano zinc oxide-silicon composite material prepared by the invention has very excellent cycle performance, can be applied to the aspects of solar cells, secondary cells and the like by combining with the electronic structure of the semiconductor catalyst of the nano zinc oxide-silicon composite material, becomes a multifunctional material with huge potential, is beneficial to improving the application value of the nano zinc oxide composite material in the electrochemical field, and is a technical scheme which is extremely worthy of popularization and use.
Detailed Description
In order to make the objects, technical solutions and effects of the present invention clearer and clearer, the present invention is further described with reference to specific embodiments, and it should be understood that the specific embodiments described herein are only used for explaining the present invention and are not used for limiting the technical solutions provided by the present invention.
Example 1
The prepared nano zinc oxide composite material is applied to a secondary battery, and specifically comprises the following process steps:
s1: weighing 2.5 g of nano silicon powder, adding the nano silicon powder into 15 ml of polyethylene glycol aqueous solution with the mass concentration of 20% under stirring, stirring the nano silicon powder for 10 minutes at the speed of 300 revolutions per minute, and performing ultrasonic dispersion for 10 minutes to obtain nano silicon dispersion liquid; the polyethylene glycol aqueous solution is prepared from polyethylene glycol with the molecular weight of 600; the grain size of the nano silicon powder is between 22 and 28 nanometers;
s2: weighing 17.5 g of zinc nitrate, placing the zinc nitrate in a beaker, adding deionized water into the beaker under stirring at the speed of 200 revolutions per minute, continuously stirring until the zinc nitrate is dissolved, preparing a zinc nitrate solution with the molar concentration of 0.42 mol/liter, dropwise adding a sodium hydroxide solution with the molar concentration of 2.6 mol/liter into the beaker at 48 ℃, adjusting the pH value of the system to be between 8.2 and 8.3, and stirring for 25 minutes under a magnetic stirrer to obtain a solid-liquid mixture;
s3: adding the nano-silicon dispersion liquid into the prepared solid-liquid mixture, quickly stirring for 8 minutes at 800 r/min, then transferring to a hydrothermal reaction kettle, setting the reaction temperature to 225 ℃, the reaction time to 13 hours, taking out the reaction kettle after the reaction is finished, placing the reaction kettle in a fume hood, naturally cooling to room temperature, pouring out supernatant liquid, respectively washing the obtained precipitate for 4 times by using ethanol and deionized water, placing the obtained precipitate in a 70 ℃ drying oven for drying for 6 hours, then placing the obtained precipitate in a muffle furnace preheated to 170 ℃ for calcining for 65 minutes at the calcining temperature of 500 ℃, and obtaining the nano-zinc oxide composite material; the grain size of the prepared nano zinc oxide composite material is between 45 and 55 nanometers.
S4: the nano zinc oxide composite material prepared in the example 1 is mixed with acetylene black and CMC according to the mass ratio of 7:1.5:1.5, the mixture is fully and uniformly ground in a mortar, a pole piece is coated, and a negative electrode is prepared and used for a secondary lithium ion battery, a metal Li piece is used as a positive electrode, and 1M LiPF6Assembling a CR2025 type button cell as an electrolyte, carrying out charge and discharge tests by using blue electricity, carrying out constant-current charge and discharge tests by using C/20 current at the constant temperature of 25 ℃, carrying out electrochemical tests with the current density of 0.5mA/g, wherein the electrochemical test results show that: the initial discharge specific capacity is 957mAh/g, and the retention rate reaches 64 percent after 100 charge-discharge cycles under the current density of 0.5A/g.
Example 2
The prepared nano zinc oxide composite material is applied to a secondary battery, and specifically comprises the following process steps:
s1: weighing 2.6 g of nano silicon powder, adding the nano silicon powder into 18 ml of 25% polyethylene glycol aqueous solution under stirring, stirring at 330 revolutions per minute for 12 minutes, and performing ultrasonic dispersion for 15 minutes to obtain nano silicon dispersion liquid; the polyethylene glycol aqueous solution is prepared from polyethylene glycol with the molecular weight of 600; the grain size of the nano silicon powder is between 22 and 28 nanometers;
s2: weighing 17.8 g of zinc nitrate, placing the zinc nitrate in a beaker, adding deionized water into the beaker under stirring at a speed of 220 r/min, continuously stirring until the zinc nitrate is dissolved, preparing a zinc nitrate solution with a molar concentration of 0.43 mol/l, dropwise adding a sodium hydroxide solution with a molar concentration of 2.7 mol/l into the beaker at 49 ℃, adjusting the pH value of the system to be between 8.2 and 8.3, and stirring for 28 minutes under a magnetic stirrer to obtain a solid-liquid mixture;
s3: adding the nano-silicon dispersion liquid into the prepared solid-liquid mixture, quickly stirring for 9 minutes at 850 revolutions per minute, then transferring the mixture into a hydrothermal reaction kettle, setting the reaction temperature to 228 ℃, the reaction time to 14 hours, taking the reaction kettle out after the reaction is finished, placing the reaction kettle into a fume hood, naturally cooling to room temperature, pouring out supernatant liquid, respectively washing the obtained precipitate for 5 times by using ethanol and deionized water, placing the obtained precipitate into a 75 ℃ drying oven for drying for 7 hours, then placing the obtained precipitate into a muffle furnace preheated to 180 ℃ for calcining for 68 minutes, and setting the calcining temperature to 510 ℃, thus obtaining the nano-zinc oxide composite material; the grain size of the prepared nano zinc oxide composite material is between 45 and 55 nanometers.
S4: the nano zinc oxide composite material prepared in the example 2 is mixed with acetylene black and CMC according to the mass ratio of 7:1.5:1.5, the mixture is fully and uniformly ground in a mortar, a pole piece is coated, and a negative electrode is prepared and used for a secondary lithium ion battery, a metal Li piece is used as a positive electrode, and 1M LiPF6Assembling a CR2025 type button cell as an electrolyte, carrying out charge and discharge tests by using blue electricity, carrying out constant-current charge and discharge tests by using C/20 current at the constant temperature of 25 ℃, carrying out electrochemical tests with the current density of 0.5mA/g, wherein the electrochemical test results show that: the first discharge specific capacity is 960mAh/g, and the retention rate reaches 66% after 100 charge-discharge cycles under the current density of 0.5A/g.
Example 3
The prepared nano zinc oxide composite material is applied to a secondary battery, and specifically comprises the following process steps:
s1: weighing 2.7 g of nano silicon powder, adding the nano silicon powder into 20 ml of 30% polyethylene glycol aqueous solution under stirring, stirring the mixture at the speed of 350 revolutions per minute for 15 minutes, and performing ultrasonic dispersion for 20 minutes to obtain nano silicon dispersion liquid; the polyethylene glycol aqueous solution is prepared from polyethylene glycol with the molecular weight of 600; the grain size of the nano silicon powder is between 22 and 28 nanometers;
s2: weighing 18.0 g of zinc nitrate, placing the zinc nitrate in a beaker, adding deionized water into the beaker under the stirring at the speed of 240 r/min, continuously stirring until the zinc nitrate is dissolved, preparing a zinc nitrate solution with the molar concentration of 0.45 mol/l, dropwise adding a sodium hydroxide solution with the molar concentration of 2.8 mol/l into the beaker at the temperature of 50 ℃, adjusting the pH value of the system to be between 8.2 and 8.3, and stirring for 30 minutes under a magnetic stirrer to obtain a solid-liquid mixture;
s3: adding the nano-silicon dispersion liquid into the prepared solid-liquid mixture, quickly stirring for 10 minutes at 900 revolutions per minute, transferring the mixture into a hydrothermal reaction kettle, setting the reaction temperature to 230 ℃, setting the reaction time to 16 hours, taking the reaction kettle out after the reaction is finished, placing the reaction kettle into a fume hood, naturally cooling to room temperature, pouring out supernatant liquid, respectively washing the obtained precipitate for 6 times by using ethanol and deionized water, placing the obtained precipitate into an 80 ℃ drying oven for drying for 8 hours, then placing the obtained precipitate into a muffle furnace preheated to 190 ℃ for calcining for 70 minutes, and setting the calcining temperature to 530 ℃, thus obtaining the nano-zinc oxide composite material; the grain size of the prepared nano zinc oxide composite material is between 45 and 55 nanometers.
S4: the nano zinc oxide composite material prepared in the example 3 is mixed with acetylene black and CMC according to the mass ratio of 7:1.5:1.5, the mixture is fully and uniformly ground in a mortar, a pole piece is coated, and a negative electrode is prepared and used for a secondary lithium ion battery, a metal Li piece is used as a positive electrode, and 1M LiPF6Assembling a CR2025 type button cell as an electrolyte, carrying out charge and discharge tests by using blue electricity, carrying out constant-current charge and discharge tests by using C/20 current at the constant temperature of 25 ℃, carrying out electrochemical tests with the current density of 0.5mA/g, wherein the electrochemical test results show that: the first discharge specific capacity is 958mAh/g, and the retention rate reaches 65% after 100 charge-discharge cycles under the current density of 0.5A/g.
The invention can obviously improve the electrochemical activity of the nano zinc oxide composite material and solve the problem of poor application effect of the existing nano zinc oxide in the field of electrochemical functions, and the composite material has the characteristics of high conductivity, thermal stability, long cycle life, easily obtained preparation raw materials, simple synthesis mode, low cost, stable chemical performance, high mechanical strength and the like. The nano zinc oxide-silicon composite material prepared by the invention has very excellent cycle performance, can be applied to the aspects of solar cells, secondary cells and the like by combining with the electronic structure of the semiconductor catalyst of the nano zinc oxide-silicon composite material, becomes a multifunctional material with huge potential, is beneficial to improving the application value of the nano zinc oxide composite material in the electrochemical field, and is a technical scheme which is extremely worthy of popularization and use.
Claims (3)
1. A nano zinc oxide composite material applied to a secondary battery is characterized by comprising the following steps:
(1) weighing 2.5-2.7 g of nano silicon powder, adding the nano silicon powder into 15-20 ml of 20-30% polyethylene glycol aqueous solution under stirring, stirring the mixture for 10-15 minutes at the speed of 300-350 revolutions per minute, and performing ultrasonic dispersion for 10-20 minutes to obtain nano silicon dispersion liquid; the polyethylene glycol aqueous solution is prepared from polyethylene glycol with the molecular weight of 600;
(2) weighing 17.5-18.0 g of zinc nitrate, placing the zinc nitrate into a beaker, adding deionized water into the beaker under stirring at the speed of 200-240 r/min, continuously stirring until the zinc nitrate is dissolved, preparing a zinc nitrate solution with the molar concentration of 0.42-0.45 mol/l, dropwise adding a sodium hydroxide solution with the molar concentration of 2.6-2.8 mol/l into the beaker at the temperature of 48-50 ℃, adjusting the pH value of the system to be 8.2-8.3, and stirring for 25-30 minutes under a magnetic stirrer to obtain a solid-liquid mixture;
(3) adding the nano silicon dispersion liquid obtained in the step (1) into the solid-liquid mixture obtained in the step (2), rapidly stirring for 8-10 minutes at 900 revolutions per minute of 800-.
2. The nano zinc oxide composite material for secondary batteries according to claim 1, wherein the nano silicon powder of step (1) has a particle size of 22-28 nm.
3. The nano zinc oxide composite material for secondary batteries according to claim 1, wherein the nano zinc oxide composite material prepared in step (3) has a particle size of 45-55 nm.
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Citations (5)
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| CN101580405A (en) * | 2009-06-05 | 2009-11-18 | 华东师范大学 | Semiconductor material with ZnO cone-shaped nano structure compounded on silicon chip and preparation method thereof |
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| CN107235506A (en) * | 2017-07-10 | 2017-10-10 | 安徽锦华氧化锌有限公司 | A kind of preparation method of nano zine oxide heterojunction structure |
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| CN110867565A (en) * | 2019-07-26 | 2020-03-06 | 吉林大学 | Preparation method of carbon-coated silicon and zinc oxide composite electrode material |
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| CN101580405A (en) * | 2009-06-05 | 2009-11-18 | 华东师范大学 | Semiconductor material with ZnO cone-shaped nano structure compounded on silicon chip and preparation method thereof |
| CN104009211A (en) * | 2014-05-13 | 2014-08-27 | 昆明理工大学 | Preparation method for porous silicon nanofiber/carbon composite material |
| CN107235506A (en) * | 2017-07-10 | 2017-10-10 | 安徽锦华氧化锌有限公司 | A kind of preparation method of nano zine oxide heterojunction structure |
| CN110277248A (en) * | 2019-05-27 | 2019-09-24 | 江苏大学 | A kind of zinc oxide-porous silicon composite material and its preparation method and application |
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| "Interfacial stabilizing effect of ZnO on Si anodes for lithium ion battery";Bin Zhu等;《Nano Energy》;20150414;第13卷;第620-625页 * |
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