CN112018379B - Iron oxide composite graphene oxide nano material containing temperature-sensitive material and preparation method and application thereof - Google Patents
Iron oxide composite graphene oxide nano material containing temperature-sensitive material and preparation method and application thereof Download PDFInfo
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Abstract
The invention provides temperature-sensitive Fe with good electrochemical performance2O3The preparation method of the composite graphene oxide nano material comprises the step of preparing the temperature-sensitive Fe with the controllable shape by using a temperature-sensitive material poly N-isopropylacrylamide (PNIPAAm) as a template and using graphene oxide as a carrier2O3The composite graphene oxide nano-particles have the characteristics of effectively enhancing the conductivity of the material, accelerating the diffusion speed of lithium ions, enabling the lithium desorption and intercalation effect to be stronger, enabling the performance of the battery to be more superior and the like due to large specific surface area and higher carbon and nitrogen content. Meanwhile, the invention also provides a preparation method and application of the material.
Description
Technical Field
The invention belongs to the technical field of nano materials, and particularly relates to an iron oxide composite graphene oxide nano material containing a temperature-sensitive material, and a preparation method and application thereof.
Background
Transition metal oxides are a class of negative electrode materials with high theoretical capacity, such as iron oxide (Fe)2O3) The theoretical capacity of the energy storage device can reach 1008mAh/g, and the energy storage device shows excellent energy storage effect. In addition, the iron element reserves are abundant, easy to be mined and the application prospect is wide. However, the conductivity is poor, and the volume expansion during charge and discharge is large, which leads to a shortened battery life and poor stability.
Graphite electrodes have been dominant in commercial lithium ion batteries. Although the redox energy of graphite is higher than that of the organic electrolysis usedThe Lowest Unoccupied Molecular Orbital (LUMO) in the stroma. The graphite surface reacts with the electrolyte solvent to form a stable solid electrolyte membrane (SEI), providing stability to its operation with a longer lifetime. However, since its operating voltage is close to Li/Li+Particularly under rapid charging and low temperature conditions, lithium dendrites and internal shorts form on the graphite surface, causing catastrophic safety hazards.
In order to solve the above problems, researchers have conducted a great deal of research on various types of electrode materials, and found that graphene sheets are thin and flexible, and can well fix nanoparticles to uniformly disperse the nanoparticles, prevent nanoparticle aggregation to a certain extent, and alleviate volume change of active materials in the charging and discharging processes. In turn, nanoparticles of metal oxides immobilized on graphene lamellae can also prevent the graphene lamellae from agglomerating to some extent. The synergistic effect improves the lithium ion storage performance and cycle performance of the composite material.
The temperature-sensitive material poly-N-isopropyl acrylamide (PNIPAAm) is an amphiphilic substance, mainly consists of C, N, O three elements, and has good solubility in water and organic solvent. The temperature sensitive material can form a solution similar to a gel in water, and therefore, the dispersion performance of the metal oxide can be improved. And the graphene is oxidized to ensure that the surface of the graphene contains rich oxygen-containing functional groups to form graphene oxide, so that the graphene oxide can be uniformly dispersed in water.
Disclosure of Invention
The invention aims to solve the technical problem of providing temperature-sensitive Fe with good electrochemical performance2O3The preparation method of the composite graphene oxide nano material comprises the step of preparing temperature-sensitive Fe with a temperature-sensitive material poly N-isopropylacrylamide (PNIPAAm) as a template and graphene oxide as a carrier, wherein the shape of the temperature-sensitive Fe is controllable2O3The composite graphene oxide nano-particles have the characteristics of effectively enhancing the conductivity of the material, accelerating the diffusion speed of lithium ions, enabling the lithium desorption and intercalation effect to be stronger, enabling the performance of the battery to be more superior and the like due to large specific surface area and higher carbon and nitrogen content. In addition, such a knotOn one hand, the volume expansion of the iron oxide in the charging and discharging processes can be relieved; on the other hand, graphene sheets are prevented from being tightly stacked to a certain extent, the electrochemical performance of the lithium battery is better than that of a single material of iron oxide and graphene, and the lithium battery is provided with longer cycle life and stronger safety performance. In conclusion, Fe2O3The application and development of the nano material in the lithium ion battery are worth researching and discussing. Therefore, the development and preparation process is simple, the conditions are mild, the conductivity of the material can be enhanced, and the performance of the lithium battery can be effectively enhanced by the temperature-sensitive Fe2O3The composite graphene oxide nano material has important scientific significance and application prospect.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: a preparation method of an iron oxide composite graphene oxide nano material containing a temperature-sensitive material comprises the following steps:
1) dissolving the temperature-sensitive material in deionized water, and uniformly stirring;
2) dispersing graphene oxide in the solution obtained in the step 1) to obtain a temperature-sensitive material aqueous solution with dispersed graphene oxide;
3) dissolving soluble ferric salt in the temperature-sensitive material aqueous solution with the graphene oxide dispersed in the step 2), adding Polyacrylonitrile (PAN), fully dissolving, and adjusting the pH value of the solution to 7 by using sodium dihydrogen phosphate;
4) and (3) placing the solution obtained in the step 3) at the temperature of 100-180 ℃ for carrying out microwave hydrothermal reaction for 8-12 h to obtain the iron oxide composite graphene oxide nano material with the solid containing the temperature-sensitive material.
On the basis of the technical scheme, the invention can further have the following specific selection or optimized selection.
Specifically, in the step 1), the temperature-sensitive material is poly-N-isopropylacrylamide, and the concentration of the poly-N-isopropylacrylamide in the deionized water is 1 × 10-2～50×10-2mmol/L。
Specifically, in the step 2), the mass ratio of the temperature-sensitive material to the graphene oxide is 1: 1-1: 2. the graphene oxide is prepared by a Hummer method.
Specifically, in the step 3), the mass ratio of the temperature-sensitive material to the soluble iron salt is 1: 20-1: 100. wherein the metal iron salt is soluble iron salt, such as ferric sulfate, ferric nitrate, ferric chloride, etc. The sufficient dissolution is ultrasonic dispersion for 0.5-2 h. The mass ratio of Polyacrylonitrile (PAN) to soluble iron salt is 1: 100-1: 200. The graphene oxide: the mass ratio of the metal iron salt is 1: 10-1: 100.
specifically, in the step 4), the temperature in the microwave hydrothermal reaction technology is 120-180 ℃, and the reaction time is preferably 10-12 h.
Preferably, the method further comprises a step 5), in the step 5), the iron oxide composite graphene oxide nano material containing the temperature-sensitive material obtained in the step 4) is washed by normal hexane and dried, and then annealing treatment is performed under the protection of inert gas.
Specifically, in the step 5), after washing by using anhydrous n-hexane, centrifuging to obtain a solid precipitate, repeating the operation for more than three times, and finally drying the obtained solid in a vacuum drying oven at the drying temperature of 60-80 ℃ for 18-24 hours; the temperature of the annealing treatment is 350-600 ℃, and the time of the annealing treatment is 1-3 h.
The second aspect of the invention also provides an iron oxide composite graphene oxide nano material containing the temperature-sensitive material, which is prepared by adopting the method.
The third aspect of the invention provides an application of the iron oxide composite graphene oxide nano material containing the temperature-sensitive material in a lithium ion battery negative electrode material.
Compared with the prior art for preparing the iron oxide, the invention has the following outstanding advantages:
(1) in the process of preparing the ferric oxide composite material, the temperature-sensitive material is adopted as the template, so that the compatibility of various substances can be enhanced on one hand, and the template effect is provided for the smooth growth of the nano ferric oxide on the other hand.
(2) The nano iron oxide prepared by the method is of a spherical structure, the particle size is less than 50nm, and the nano structure is more favorable for electron transmission and current stability.
(3) Compared with the traditional iron oxide material, the iron oxide composite graphene oxide containing the temperature-sensitive material prepared by the invention has higher specific capacity, and concretely shows that the charging and discharging specific capacity is stabilized at 880mAh/g, the circulation lasts for 50 weeks, and the efficiency is still maintained at 93%.
Drawings
FIG. 1 shows the hydrothermal preparation of pure Fe2O3SEM characterization of nanospheres;
FIG. 2 shows that pure Fe is prepared by a hydrothermal method after adding a temperature-sensitive material as a template2O3SEM characterization of nanospheres;
FIG. 3 shows Fe containing a temperature sensitive material2O3A TEM representation of the composite graphene oxide nanomaterial;
FIG. 4 shows pure Fe2O3The composite graphene oxide nano material is used as a battery negative electrode material cyclic voltammogram;
FIG. 5 shows Fe containing a temperature sensitive material2O3The composite graphene oxide nano material is used as a battery negative electrode material cyclic voltammogram;
fig. 6 is a schematic diagram of a lithium ion battery assembly process.
Detailed Description
For a better understanding of the present invention, the following further illustrates the present invention with reference to the accompanying drawings and specific examples, but the present invention is not limited to the following examples.
Example 1:
hydrothermal synthesis of pure Fe2O3The nano material comprises the following specific implementation flows: the specific operation process is as follows: 1.0g FeCl was weighed3·6H2And completely dissolving O in 30mL of deionized water, weighing 10mg of PAN (polyacrylonitrile), adding the solution, and stirring at constant temperature until the solution is clear and transparent. The pH value of the mixed solution is adjusted to 7. And adjusting the pH value of the solution, then putting the solution into an ultrasonic instrument for mixing and oscillating, eliminating bubbles, pouring the solution into a polytetrafluoroethylene high-pressure reaction kettle with the capacity of 50mL, and heating and reacting for 12 hours at 180 ℃. Washing the product with deionized water, washing with anhydrous ethanol, centrifuging, and repeating the above steps for several times. Finally, the mixture is placed in a vacuum drying oven to be dried for 24 hours at the temperature of 80 ℃ to obtain Fe2O3Nanosphere particles.
Example 2:
hydrothermal synthesis of Fe2O3The composite graphene oxide nano material comprises the following specific operation processes: weighing 0.050g of graphene oxide and 1.0g of FeCl3·6H2O, 10mg of polyacrylonitrile are dissolved in 30mL of deionized water, the pH value of the solution is adjusted to 7 by using 0.1mol/mL sodium dihydrogen phosphate solution, and the mixed solution is shaken for 30min by using an ultrasonic instrument to eliminate bubbles. Then pouring the mixture into a polytetrafluoroethylene reaction kettle with the capacity of 50mL, and heating and reacting for 12h at 180 ℃. Washing with anhydrous ethanol, centrifuging, repeating the above steps for several times, and drying in a vacuum drying oven at 120 deg.C for 24 hr. Taking out the solid particles and cooling.
Example 3
Synthesizing temperature-sensitive Fe by hydrothermal method by taking the prepared temperature-sensitive material as a template2O3The composite graphene oxide nano material comprises the following specific operation processes: weighing 0.050g of temperature-sensitive material PNIPAAm, dissolving in 10mL of deionized water, weighing 0.050g of graphene oxide, adding into the solution after fully dissolving, performing ultrasonic dispersion until a uniform solution is formed, and adding 1.0g of FeCl3·6H2Dissolving O and 10mg polyacrylonitrile in 30mL of deionized water, mixing the two solutions, adjusting the pH of the mixed solution to about 7 by using 0.1mol/mL sodium dihydrogen phosphate solution, and shaking the mixed solution for 30min by using an ultrasonic instrument to eliminate bubbles. Then pouring the mixture into a polytetrafluoroethylene reaction kettle with the capacity of 100mL, and heating and reacting for 12h at 180 ℃. Washing the hydrothermal reaction product with anhydrous n-hexane, centrifuging, repeating the operation for more than three times, and finally drying in a vacuum drying oven at the drying temperature of 60-80 ℃ for 18-24 hours. Finally, annealing treatment is carried out at 500 ℃, and the annealing treatment time is 2 h.
Example 4
The two materials in the embodiments 2 and 3 are respectively prepared into button lithium ion batteries, and then the lithium ion batteries are subjected to constant current charge and discharge tests to test the electrochemical performance of the lithium ion batteries. The specific implementation steps are as follows: grinding and sieving the materials in the embodiments 2 and 3, respectively mixing the materials with Super-P-Li and PVDF according to the mass ratio of 8:1:1, adding NMP, stirring the materials in a disc turbine stirrer to be viscous, pouring the slurry on a current collector copper foil for coating, placing the current collector copper foil in a vacuum drying box for drying at 60 ℃ for 24 hours, slicing the current collector copper foil to prepare a lithium ion battery electrode, and finally assembling and sealing the current collector copper foil in a glove box filled with argon to prepare the button type lithium ion battery. The flow diagram is shown in FIG. 6.
The prepared material is tested by a blue-electricity battery testing system, the experimental voltage range is 0.05-3V, the current density is 100mA/g, and the cyclic voltammetry curve of the obtained material is tested.
As shown in FIGS. 4 and 5, two different types of Fe2O3The cycle curve of the nano material shows that the cycle efficiency of the two materials is about 93 percent, and the nano material has better stability. FIG. 4 is a hydrothermal process for preparing Fe2O3The composite graphene oxide material is a cycle curve of a battery cathode, and the charge-discharge specific capacity is about 550 mAh/g. FIG. 5 shows Fe prepared from temperature-sensitive material as template2O3The specific capacity of the composite graphene oxide nano material can reach 880mAh/g, and is greatly improved compared with a material without a temperature-sensitive material. The iron oxide composite graphene oxide nanomaterial containing the temperature-sensitive material provided by the invention has excellent cycling stability and specific capacity value.
In conclusion, the temperature-sensitive material is used as the template, and the temperature-sensitive iron oxide composite graphene oxide nano material is prepared by a microwave hydrothermal method. The graphite is used as a battery cathode for performance test, shows more excellent charge and discharge performance 880mAh/g than the prior art, is greatly higher than the theoretical capacity (350mAh/g) of graphite, and has the cycle stability of 93 percent.
In addition, the negative electrode material prepared by the invention adopts the temperature-sensitive material as the substrate, so that the conductivity and flexibility of the negative electrode material can be more effectively improved, and further, the conductivity of the iron oxide as the negative electrode material is improved. In addition, the layered structure of the graphene oxide can improve the porosity of the electrode material, so that the charge and discharge performance of the material is improved.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. A preparation method of an iron oxide composite graphene oxide nano material containing a temperature-sensitive material is characterized by comprising the following steps:
1) dissolving the temperature-sensitive material in deionized water, and uniformly stirring;
2) dispersing graphene oxide in the solution obtained in the step 1) to obtain a temperature-sensitive material aqueous solution with dispersed graphene oxide;
3) dissolving soluble ferric salt in the temperature-sensitive material aqueous solution with the dispersed graphene oxide in the step 2), adding polyacrylonitrile, and adjusting the pH value of the solution to 7 by using sodium dihydrogen phosphate after the solution is fully dissolved;
4) placing the solution obtained in the step 3) at the temperature of 100-180 ℃ for microwave hydrothermal reaction for 8-12 h to obtain the iron oxide composite graphene oxide nano material with the solid containing the temperature-sensitive material,
wherein the temperature-sensitive material is poly N-isopropyl acrylamide.
2. The preparation method of the iron oxide composite graphene oxide nanomaterial containing the temperature-sensitive material according to claim 1, characterized in that: in the step 1), the concentration of the temperature-sensitive material in the deionized water is 1 multiplied by 102～50×10- 2mmol/L。
3. The preparation method of the iron oxide composite graphene oxide nanomaterial containing the temperature-sensitive material according to claim 1, characterized in that: in the step 2), the mass ratio of the temperature-sensitive material to the graphene oxide is 1: 1-1: 2.
4. the preparation method of the iron oxide composite graphene oxide nanomaterial containing the temperature-sensitive material according to claim 1, characterized in that: in the step 3), the mass ratio of the temperature-sensitive material to the soluble iron salt is 1: 20-1: 100, respectively; the full dissolution is ultrasonic dispersion for 0.5-2 h; the mass ratio of polyacrylonitrile to soluble iron salt is 1: 100-1: 200.
5. The preparation method of the iron oxide composite graphene oxide nanomaterial containing the temperature-sensitive material according to claim 4, characterized in that: the soluble ferric salt is one of ferric sulfate, ferric nitrate and ferric chloride.
6. The preparation method of the iron oxide composite graphene oxide nanomaterial containing the temperature-sensitive material according to claim 1, characterized in that: in the step 4), the temperature of the microwave hydrothermal reaction is 120-180 ℃, and the reaction time is 10-12 h.
7. The preparation method of the iron oxide composite graphene oxide nanomaterial containing the temperature-sensitive material according to any one of claims 1 to 6, wherein the preparation method comprises the following steps: and 5) washing and drying the iron oxide composite graphene oxide nano material containing the temperature-sensitive material obtained in the step 4) by using n-hexane, and then annealing under the protection of inert gas.
8. The preparation method of the iron oxide composite graphene oxide nanomaterial containing the temperature-sensitive material according to claim 7, characterized in that: in the step 5), after washing with anhydrous n-hexane, centrifuging to obtain a lower-layer solid precipitate, repeating the washing and centrifuging operation for more than three times, and finally drying the obtained solid in a vacuum drying oven at the drying temperature of 60-80 ℃ for 18-24 h; the temperature of the annealing treatment is 350-600 ℃, and the time of the annealing treatment is 1-3 h.
9. The iron oxide composite graphene oxide nano material containing the temperature-sensitive material is characterized by being prepared by the preparation method of the iron oxide composite graphene oxide nano material containing the temperature-sensitive material according to any one of claims 1 to 8.
10. The application of the iron oxide composite graphene oxide nanomaterial containing a temperature-sensitive material according to claim 9 in a lithium ion battery negative electrode material.
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| CN102120787A (en) * | 2011-01-13 | 2011-07-13 | 东华大学 | Preparation method of graphene/N-isopropylacrylamide composite microgel |
| CN103495368A (en) * | 2013-09-17 | 2014-01-08 | 南昌大学 | Preparation method of thermo-magnetic dual responsive mesoporous silicon microspheres |
| CN106076385A (en) * | 2016-06-12 | 2016-11-09 | 江苏大学 | A kind of temperature response type composite and its production and use |
| CN109277091A (en) * | 2018-12-01 | 2019-01-29 | 浙江海洋大学 | A kind of preparation method of the composite material of Thermo-sensitive |
| CN109449390A (en) * | 2018-10-08 | 2019-03-08 | 浙江衡远新能源科技有限公司 | A kind of iron oxide/graphene aerogel composite negative pole material and preparation method thereof |
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| CN105891293B (en) * | 2016-06-01 | 2018-10-16 | 辽宁大学 | A kind of preparation of PNIPAM-RGO graphene composite materials and its application on intelligent response sex modification electrode |
| CN107522825B (en) * | 2017-07-27 | 2019-12-27 | 西北工业大学 | Three-dimensional cell culture device based on temperature-responsive liquid marbles and construction and use methods |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102120787A (en) * | 2011-01-13 | 2011-07-13 | 东华大学 | Preparation method of graphene/N-isopropylacrylamide composite microgel |
| CN103495368A (en) * | 2013-09-17 | 2014-01-08 | 南昌大学 | Preparation method of thermo-magnetic dual responsive mesoporous silicon microspheres |
| CN106076385A (en) * | 2016-06-12 | 2016-11-09 | 江苏大学 | A kind of temperature response type composite and its production and use |
| CN109449390A (en) * | 2018-10-08 | 2019-03-08 | 浙江衡远新能源科技有限公司 | A kind of iron oxide/graphene aerogel composite negative pole material and preparation method thereof |
| CN109277091A (en) * | 2018-12-01 | 2019-01-29 | 浙江海洋大学 | A kind of preparation method of the composite material of Thermo-sensitive |
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