CN108417798B - ZnO nanosheet/carbon sponge flexible composite negative electrode material and preparation method thereof - Google Patents
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Abstract
The invention belongs to the technical field of electrochemistry, and particularly relates to a ZnO nanosheet/carbon sponge flexible composite negative electrode material and a preparation method thereof. The flexible composite negative electrode material is a composite material which is composed of porous self-supporting carbon sponge as a carrier and zinc oxide (ZnO) two-dimensional nanosheets as a negative electrode active material of a lithium battery, wherein ZnO is high in loading amount, and is stable in circulation under high current density. The preparation method comprises the following steps: depositing ZnO on the surface atomic layer of the porous polyurethane template, removing the organic template at high temperature to obtain ZnO nanosheets, and preparing ZnO nanosheet dispersion liquid; carbonizing melamine sponge at high temperature to obtain carbon sponge, immersing the carbon sponge into ZnO nanosheet dispersion liquid, drying, and carrying out high-temperature heat treatment in an inert atmosphere to obtain a ZnO nanosheet/carbon sponge flexible composite material; the flexible composite material can be directly used for preparing a lithium battery cathode without a conductive agent and a binding agent.
Description
Technical Field
The invention belongs to the technical field of electrochemistry, and particularly relates to a negative electrode material for a lithium ion battery and a preparation method thereof.
Background
Improving the capacity and cycling stability of the negative electrode material is critical to meeting the application of lithium ion batteries in fields including portable electronic devices, electric vehicles, smart grids, and the like (m.v. Reddy, et al,Chem. Rev. 2013, 113, 5364). However, the capacity of the graphite negative electrode material which accounts for the largest market proportion at present is only 372 mAh g-1Low energy density, which limits the development of high-energy lithium batteriesThe steps are applied. The transition metal oxide has high theoretical capacity, and is one of hot cathode materials researched in the field of lithium ion batteries at present. Zinc oxide (ZnO) is used as the negative electrode material of the lithium battery, and the theoretical capacity is high (978 mAh g)-1) The reserve is rich, and is one of lithium battery cathode materials with development prospect (S. Shilpa, et al,J. Mater. Chem.A2015, 3,5344). However, ZnO undergoes volume expansion during charging and discharging, which causes phenomena such as particle breakage and SEI film transition growth, resulting in capacity degradation, and thus it is particularly important to improve the cycle stability. The construction of nanostructures or composites with carbon materials (including surface coating of carbon materials or composites with carbon materials having a three-dimensional network structure) is currently the main method for improving the cycling stability (g.l. Xu, et al,Nano Energy2015, 18, 253). In which the ZnO nanosheet with a two-dimensional structure can release stress generated by lithium intercalation and deintercalation through deformation such as wrinkling and bending, and can effectively relieve pulverization of the material, thereby improving the cycle stability of ZnO (J.H. Liu, et al.,Adv. Mater.2012, 24, 4097.)。
however, the loading of the metal oxide electrode active material is reported so far<1 mg cm-2Flour volume< 2 mAhg-1And the practical application requirements cannot be met. The capacity of the electrode surface can be improved by increasing the loading of the electrode material, but for the electrode taking the metal copper foil as a current collector, the electrode is thickened due to the large loading of the electrode material, and the electrochemical process is limited by the resistance of charge transfer. And an excessively thick electrode is liable to peel off from the current collector upon charging of lithium, causing electrical contact deactivation (h.j. Peng, et al,Adv. Energy Mater. 2017, 1700260). The nano-structured zinc oxide is contained in the conductive carbon material with the porous structure, so that the electrode can show good stability and rate capability under high ZnO loading (G.M. Zhou, et al, Nano Energy2015, 11, 356.). This is mainly because: firstly, the porous material has a large specific surface and can be loaded with more active substances; secondly, electrons can be directly conducted to ZnO loaded on the surface from the porous structure, and the porous structure is also Li+The transfer of (2) provides a channel, reducing charge transfer resistance; in addition, it is porousThe structure may mitigate volume expansion. However, most porous carbon materials, which do not have lithium storage capacity but occupy more than 50% of the total electrode mass, as a current collector, and the use of a binder and a conductive agent further increases the proportion of inactive materials, which greatly limits the increase in the energy density of the battery. Therefore, it is especially important to find a novel porous carbon material which can load more ZnO nano-sheets with high capacity and has lithium storage capacity to obtain a stable composite electrode with high energy.
Disclosure of Invention
The invention aims to provide a negative electrode material for a lithium ion battery with high ZnO loading and good cycling stability and a preparation method thereof.
The invention provides a negative electrode material for a lithium ion battery, which is a composite material formed by using porous self-supporting carbon sponge as a carrier and using zinc oxide (ZnO) two-dimensional nanosheets as negative electrode active materials of the lithium battery, and is called as a ZnO nanosheet/carbon sponge flexible composite negative electrode material. The composite material relieves the problem of capacity attenuation of ZnO as a negative electrode, and ensures the cycling stability and rate capability under high ZnO loading capacity.
The preparation method of the ZnO nanosheet/carbon sponge flexible composite negative electrode material provided by the invention has the flow shown in figure 1, and comprises the following specific steps:
(1) preparing ZnO nanosheets: porous polyurethane is taken as a template, diethyl zinc (DEZ) is taken as a zinc source, deionized water (DIW) is taken as an oxygen source, and N2Atomic Layer Deposition (ALD) of ZnO thin film on the surface of the template for carrier gas and pulse gas; placing ZnO-coated polyurethane into O2Removing the polyurethane template at high temperature in the atmosphere to obtain ZnO nanosheets; then, the ZnO nano-sheet is ultrasonically dispersed in an alcohol solution to prepare the ZnO nano-sheet with the concentration of 5-30 mg mL-1The ZnO nanosheet dispersion of (a);
(2) preparation of carbon sponge: placing the melamine sponge in a high-temperature tubular furnace, introducing inert gas, heating to a carbonization temperature at a heating rate of 5-10 ℃/min, keeping for 1-3h, cooling and taking out to obtain carbon sponge;
(3) preparing a ZnO nanosheet/carbon sponge flexible composite negative electrode material: and (3) immersing the carbon sponge prepared in the step (2) into the ZnO nanosheet dispersion liquid prepared in the step (1), taking out and drying, placing in a tubular furnace again, introducing inert gas, and carrying out heat treatment to obtain the ZnO nanosheet/carbon sponge flexible composite negative electrode material.
In the step (1), the temperature for removing the polyurethane template is 650-750 ℃, the time is 2-4h, the preferred temperature is 700 ℃, and the time is 3 h.
In the step (1), the thickness of the prepared ZnO nanosheet can be regulated and controlled by adjusting the cycle number of atomic layer deposition.
In step (1), each ALD cycle comprises: DEZ pulse 30 ms, wait 2s, N2Cleaning for 20s, DIW pulsing for 20ms, waiting for 2s, N2And (5) cleaning for 20 s.
In the step (2), the prepared carbon sponge has a self-supporting structure and can be bent, folded and compressed to deform.
In the step (3), the loading capacity of the ZnO nanosheets in the prepared composite material is controlled by adjusting the dipping times or the concentration of the ZnO dispersion liquid. The ZnO loading capacity can reach 3-4 mg cm-2。
In the step (3), the heat treatment temperature is 650-750 ℃, the heat treatment time is 1-2h, preferably the heat treatment temperature is 700 ℃, and the heat treatment time is 1 h.
The ZnO nanosheet/carbon sponge flexible composite negative electrode material prepared by the invention has the following advantages and characteristics:
(1) the ZnO two-dimensional nanosheet obtained in the step 2 is characterized in that the size of the nanosheet is micron-sized, the thickness of the nanosheet is nano-sized, the nanosheet is flexible (as shown in figure 2), stress can be released by deformation such as wrinkling, bending and curling under stress, and the problem of powdering of ZnO under stress when lithium is filled and embedded can be solved;
(2) the carbon sponge obtained in the step 2 of the invention (as shown in figure 3) is characterized in that the obtained carbon sponge has a cross-linked porous structure (as shown in figure 4);
(3) according to the ZnO nanosheet/carbon sponge flexible composite negative electrode material obtained in the step 3, the dipping times are increased or the ZnO nanosheet fraction is increasedThe concentration of the dispersion can improve the content of ZnO nano-sheets in the composite material, and the carbon sponge has a porous structure and a large specific surface (50 m)2 g-1) Can improve the ZnO loading capacity to 3-4 mg cm-2；
(4) According to the composite electrode obtained in the step 3 (shown in figure 4), the composite material can be directly used for manufacturing the electrode without a binder or a conductive agent;
(5) the method for preparing the carbon sponge in the step 2 is also suitable for compounding various metal oxide nanosheets and the carbon sponge.
Drawings
Fig. 1 is a schematic diagram of a preparation process of the ZnO nanosheet/carbon sponge flexible composite anode material of the present invention. Wherein, 1, the melamine sponge block body; 2. carbonized carbon sponge; 3. the ZnO nanosheet is attached to the surface of the carbon sponge to form the ZnO nanosheet/carbon sponge flexible composite negative electrode material.
Fig. 2 is a SEM image of ZnO nanosheets. Has flexibility.
Fig. 3 is a block-shaped carbon sponge.
Fig. 4 is an SEM image of a carbon sponge having a cross-linked porous structure.
Fig. 5 is an SEM image of the ZnO nanosheet/carbon sponge flexible composite anode material.
FIG. 6 shows that the ZnO nanosheet/carbon sponge flexible composite negative electrode material is at 640 mA g-1And 2000 mA g-1Cycling performance at current density. The ZnO nanosheet is compounded with the carbon sponge, so that the stability of the electrode can be improved.
Detailed Description
The present invention is further illustrated by the following examples, which are intended to be illustrative only and are not to be construed as limiting the scope of the invention.
Example 1
(1) Growing a ZnO nano film on the porous polyurethane template by utilizing an atomic layer deposition method;
the atomic layer deposition method takes diethyl zinc (Diethylzinc) and deionized water (DIW) as precursors, and the source heating temperature is controlled to be room temperature. Setting the reaction temperature, namely the cavity temperature, to be 150 ℃, and taking out after 200 ALD cycles to obtain ZnO-coated polyurethane;
(2) and (3) placing the ZnO-coated polyurethane in a tubular furnace, and introducing oxygen for heat treatment. Heating at a heating rate of 10 ℃/min, wherein the burning temperature is 650 ℃, the heat preservation time is 4 hours, and taking out the sample after the sample is naturally cooled;
(3) ultrasonically dispersing the sample in alcohol solution for 30min to obtain the concentration of 30mg mL-1A solution in which ZnO is uniformly dispersed;
(4) putting the melamine sponge into a tube furnace, and introducing N2Heating to 700 ℃ at the temperature rising rate of 10 ℃/min, keeping for 1 time, cooling and taking out to obtain carbon sponge;
(5) carbon sponge was immersed in 30mg mL-1Taking out the uniform dispersion liquid of the ZnO nanosheet, drying, putting the ZnO nanosheet into a tubular furnace again, and introducing N2And carrying out heat treatment for 2 hours at 700 ℃ to obtain the ZnO nanosheet/carbon sponge flexible composite negative electrode material.
Example 2
(1) Growing a ZnO nano film on the porous polyurethane template by utilizing an atomic layer deposition method;
the atomic layer deposition method takes diethyl zinc (Diethylzinc) and deionized water (DIW) as precursors, and the source heating temperature is controlled to be room temperature. Setting the reaction temperature, namely the cavity temperature, to be 150 ℃, and taking out after 200 ALD cycles to obtain ZnO-coated polyurethane;
(2) and (3) placing the ZnO-coated polyurethane in a tubular furnace, and introducing oxygen for heat treatment. Heating at a heating rate of 10 ℃/min, wherein the burning temperature is 700 ℃, the heat preservation time is 3 hours, and taking out the sample after the sample is naturally cooled;
(3) ultrasonically dispersing the sample in alcohol solution for 30min to obtain the concentration of 30mg mL-1A solution in which ZnO is uniformly dispersed;
(4) putting the melamine sponge into a tube furnace, and introducing N2Heating to 700 ℃ at the temperature rising rate of 10 ℃/min, keeping for 1h, cooling and taking out to obtain carbon sponge;
(5) immersing carbon sponge to a concentrationIs 30mg mL-1Taking out the uniform dispersion liquid of the ZnO nanosheet, drying, soaking again into the ZnO dispersion liquid, taking out, drying, placing in a tubular furnace, introducing N2Carrying out heat treatment at 700 ℃ for 1 hour to obtain the ZnO nanosheet/carbon sponge flexible composite negative electrode material;
(6) cutting the obtained ZnO nanosheet/carbon sponge flexible composite negative electrode material into a circular sheet with the diameter of 12mm, directly using the circular sheet as a negative electrode plate, assembling the circular sheet into a button cell (CR 2032) in a glove box (under argon), using a metal lithium sheet as a counter electrode and using 1 mol/L LiPF as electrolyte6Ethylene Carbonate (EC)/dimethyl carbonate (DMC) (volume ratio 1: 1) solution. Button cell charge-discharge test conditions: the battery is put at 640 mA g-1And 2000 mA g-1Charging and discharging are carried out, the cycle performance is observed, and the experimental result is recorded and listed in the attached figure 6.
Example 3
(1) Growing a ZnO nano film on the porous polyurethane template by utilizing an atomic layer deposition method;
the atomic layer deposition method takes diethyl zinc (Diethylzinc) and deionized water (DIW) as precursors, and the source heating temperature is controlled to be room temperature. Setting the reaction temperature, namely the cavity temperature, to be 150 ℃, and taking out after 200 ALD cycles to obtain ZnO-coated polyurethane;
(2) and (3) placing the ZnO-coated polyurethane in a tubular furnace, and introducing oxygen for heat treatment. Heating at a heating rate of 10 ℃/min, wherein the burning temperature is 750 ℃, the heat preservation time is 2 hours, and taking out the sample after the sample is naturally cooled;
(3) ultrasonically dispersing the sample in alcohol solution for 30min to obtain the concentration of 20mg mL-1A solution in which ZnO is uniformly dispersed;
(4) putting the melamine sponge into a tube furnace, and introducing N2Heating to 700 ℃ at the temperature rising rate of 10 ℃/min, keeping for 1 time, cooling and taking out to obtain carbon sponge;
(5) carbon sponge was immersed in a concentration of 20mg mL-1Taking out the uniform dispersion liquid of ZnO nanosheet, drying, taking out, drying, placing in a tube furnace, and introducing N2，650℃And carrying out heat treatment for 3 hours to obtain the ZnO nanosheet/carbon sponge flexible composite negative electrode material.
Example 4
(1) Growing a ZnO nano film on the porous polyurethane template by utilizing an atomic layer deposition method;
the atomic layer deposition method takes diethyl zinc (Diethylzinc) and deionized water (DIW) as precursors, and the source heating temperature is controlled to be room temperature. Setting the reaction temperature, namely the cavity temperature, to be 150 ℃, and taking out after 200 ALD cycles to obtain ZnO-coated polyurethane;
(2) and (3) placing the ZnO-coated polyurethane in a tubular furnace, and introducing oxygen for heat treatment. Heating at a heating rate of 10 ℃/min, wherein the burning temperature is 700 ℃, the heat preservation time is 3 hours, and taking out the sample after the sample is naturally cooled;
(3) ultrasonically dispersing the sample in alcohol solution for 30min to obtain the concentration of 20mg mL-1A solution in which ZnO is uniformly dispersed;
(4) putting the melamine sponge into a tube furnace, and introducing N2Heating to 700 ℃ at the temperature rising rate of 10 ℃/min, keeping for 1 time, cooling and taking out to obtain carbon sponge;
(5) carbon sponge was immersed in a concentration of 20mg mL-1Taking out the uniform dispersion liquid of the ZnO nanosheet, drying, dipping again, drying, placing in a tube furnace, and introducing N2And carrying out heat treatment for 2 hours at 700 ℃ to obtain the ZnO nanosheet/carbon sponge flexible composite negative electrode material.
Example 5
(1) Growing a ZnO nano film on the porous polyurethane template by utilizing an atomic layer deposition method;
the atomic layer deposition method takes diethyl zinc (Diethylzinc) and deionized water (DIW) as precursors, and the source heating temperature is controlled to be room temperature. Setting the reaction temperature, namely the temperature of the cavity to be 150 ℃, and taking out after 100 ALD cycles to obtain ZnO-coated polyurethane;
(2) and (3) placing the ZnO-coated polyurethane in a tubular furnace, and introducing oxygen for heat treatment. Heating at a heating rate of 10 ℃/min, wherein the burning temperature is 700 ℃, the heat preservation time is 3 hours, and taking out the sample after the sample is naturally cooled;
(3) ultrasonically dispersing the sample in alcohol solution for 30min to obtain the concentration of 30mg mL-1A solution in which ZnO is uniformly dispersed;
(4) putting the melamine sponge into a tube furnace, and introducing N2Heating to 800 ℃ at the temperature rising rate of 20 ℃/min, keeping for 1 time, cooling and taking out to obtain carbon sponge;
(5) carbon sponge was immersed in 30mg mL-1Taking out the uniform dispersion liquid of the ZnO nanosheet, drying, placing in a tubular furnace, and introducing N2And carrying out heat treatment at 750 ℃ for 1 hour to obtain the ZnO nanosheet/carbon sponge flexible composite negative electrode material.
Claims (4)
1. A preparation method of a ZnO nanosheet/carbon sponge flexible composite negative electrode material is characterized by comprising the following specific steps:
(1) preparing ZnO nanosheets: porous polyurethane is taken as a template, diethyl zinc is taken as a zinc source, deionized water is taken as an oxygen source, and N2Depositing a ZnO film on the surface of the template by using an atomic layer as a carrier gas and a pulse gas; placing ZnO-coated polyurethane in O2Removing the polyurethane template at high temperature in the atmosphere to obtain ZnO nanosheets; then, the ZnO nano-sheet is ultrasonically dispersed in an alcohol solution to prepare the ZnO nano-sheet with the concentration of 5-30 mg mL-1The ZnO nanosheet dispersion of (a);
(2) preparation of carbon sponge: placing the melamine sponge in a high-temperature tubular furnace, introducing inert gas, heating to a carbonization temperature at a heating rate of 5-10 ℃/min, keeping for 1-3h, cooling and taking out to obtain carbon sponge;
(3) preparing a ZnO nanosheet/carbon sponge flexible composite negative electrode material: dipping the carbon sponge prepared in the step (2) into the ZnO nanosheet dispersion liquid prepared in the step (1), taking out and drying, putting the obtained product into a tubular furnace again, introducing inert gas, and carrying out heat treatment at the temperature of 650-750 ℃ for 1-2h to obtain a ZnO nanosheet/carbon sponge flexible composite negative electrode material; wherein the loading amount of the ZnO nano-sheet is controlled by adjusting the dipping times or the concentration of the ZnO dispersion liquid.
2. The preparation method according to claim 1, wherein the temperature for removing the polyurethane template in the step (1) is 650 ℃ to 750 ℃ and the time is 2 to 4 hours.
3. The preparation method according to claim 1, wherein the thickness of the ZnO nanosheet prepared in step (1) is controlled by adjusting the number of cycles of atomic layer deposition.
4. The method of claim 1, wherein the carbon sponge prepared in the step (2) has a self-supporting structure and can be bent, folded and compressively deformed.
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| CN113460991A (en) * | 2021-06-17 | 2021-10-01 | 四川启睿克科技有限公司 | Self-supporting porous lithium titanate composite precursor, negative electrode material thereof and preparation method |
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