CN111807416A - Preparation method of hollow tubular structure FeOOH @ rGO lithium ion battery anode material - Google Patents
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Abstract
A preparation method of a hollow tubular structure FeOOH @ rGO lithium ion battery cathode material belongs to the field of preparation of lithium ion battery cathode materials. The problems of volume expansion and poor insulation of the conventional FeOOH cathode material are solved. The method comprises the following steps: firstly, foam nickel pretreatment; secondly, preparing a graphene oxide aqueous solution; thirdly, preparing foamed nickel-graphene oxide; fourthly, calcining the foamed nickel-graphene oxide; and fifthly, soaking the calcined product in an iron salt solution, washing with water, filtering and drying. According to the lithium ion battery cathode material prepared by the invention, the hollow structure provides sufficient space for volume expansion, and the micron-sized holes increase the diffusion of electrolyte to the electrode material; the three-dimensional mutually cross-linked carbon skeleton provides a conductive network, so that the reaction rate is increased; the method has better cycle stability; the lithium ion transmission path is shortened, and the multiplying power performance is improved. The invention is suitable for being used as the cathode material of the lithium ion battery.
Description
Technical Field
The invention belongs to the field of preparation of lithium ion battery cathode materials, and particularly relates to a preparation method of a hollow tubular structure FeOOH @ rGO lithium ion battery cathode material.
Background
Lithium ion batteries have the advantages of high energy density, long cycle life, and small self-discharge, and have been widely used in the fields of portable electronic devices, such as mobile phones, notebook computers, ipods, and electric vehicles. Since the first development of lithium ion batteries by the company sony, japan, 1990, it has attracted great interest in both academia and industry.
The electrode material is a key factor that limits its performance. The current commercialized negative electrode material adopts graphite materials, which have wide sources and low price, but have certain defects, such as low specific capacity (372mAh/g) and poor rate capability, and can not meet the requirements of people on consumer electronic products. The ferrite compound negative electrode material has high specific capacity, so that the ferrite compound negative electrode material becomes one of hot spots for researching novel negative electrode materials for power lithium ion batteries, in particular to a newly developed FeOOH material in recent years. However, researchers find that FeOOH, as a negative electrode material of a lithium ion battery, also undergoes severe volume expansion during lithium intercalation and has self insulation, which causes problems of electrode material pulverization, active material peeling from a current collector, capacity reduction, poor rate capability and the like, resulting in a sharp drop in battery performance.
Disclosure of Invention
The invention aims to solve the problems of volume expansion and poor insulation of the conventional FeOOH negative electrode material, and provides a preparation method of a hollow tubular structure FeOOH @ rGO lithium ion battery negative electrode material.
A preparation method of a hollow tubular structure FeOOH @ rGO lithium ion battery anode material is realized according to the following steps:
firstly, performing ultrasonic treatment on foamed nickel by using acetone, hydrochloric acid, absolute ethyl alcohol and deionized water in sequence, and drying in a vacuum oven to obtain dried foamed nickel;
secondly, dissolving graphene oxide in deionized water, stirring, and performing ultrasonic treatment to obtain a graphene oxide aqueous solution;
thirdly, soaking the dried foam nickel obtained in the first step into the graphene oxide aqueous solution obtained in the second step, taking out the foam nickel, drying the foam nickel, and repeating the soaking and drying processes for three times to obtain dried foam nickel-graphene oxide;
fourthly, placing the dried foam nickel-graphene oxide in a tubular furnace, and calcining in an inert atmosphere to obtain a product A;
fifthly, dipping the product A obtained in the fourth step into a ferric salt solution, washing with water, filtering and drying to obtain the hollow tubular structure FeOOH @ rGO lithium ion battery cathode material;
wherein the concentration of the graphene oxide aqueous solution in the second step is 2 mg/ml-10 mg/ml;
in the third step, the mass-to-volume ratio of the foam nickel to the graphene oxide aqueous solution is (200-800) mg (20-80) ml;
the calcining temperature is 400-900 ℃, the time is 2-5 h, and the heating rate is 10 ℃/min;
in the fifth step, the ferric salt is ferric trichloride or ferric nitrate;
and in the fifth step, the mass-to-volume ratio of the product A to the ferric salt solution is (10-100) mg:40 mL.
The invention has the advantages that:
the hollow tubular FeOOH @ rGO lithium ion battery cathode material prepared by the invention has the hollow structure with the size of 2-10 um, provides sufficient space for the volume expansion of FeOOH in the process of lithium intercalation and deintercalation, and the micron-sized holes also effectively increase the diffusion of electrolyte to the electrode material; meanwhile, the three-dimensional mutually-crosslinked carbon skeleton provides a conductive network, which is beneficial to the transmission of electrons and increases the reaction rate.
The invention utilizes the excellent conductivity of graphene to combine graphene with grapheneFeOOH is compounded to obtain the lithium ion battery cathode material with excellent cycle and rate performance; the doped Ni can further increase the conductivity of the cathode material; high capacity is shown, up to 912mAh g–1And has better cycle stability; the hollow tubular FeOOH @ rGO lithium ion battery cathode material prepared by the invention shortens the lithium ion transmission path and improves the rate capability.
The invention is suitable for being used as the cathode material of the lithium ion battery.
Drawings
FIG. 1 is an XRD spectrum of a hollow tubular structure FeOOH @ rGO lithium ion battery anode material in an example;
FIG. 2 is an SEM spectrogram of the hollow tubular structure FeOOH @ rGO lithium ion battery anode material in the embodiment;
FIG. 3 is a 0.2A/g cycle performance test curve diagram of the hollow tubular structure FeOOH @ rGO lithium ion battery negative electrode material in the embodiment, wherein- ● -represents the specific discharge capacity, and-O-represents the specific charge capacity;
FIG. 4 is a graph of the rate performance test curve of the hollow tubular structure FeOOH @ rGO lithium ion battery negative electrode material in the embodiment, wherein- ● -represents the specific discharge capacity, and-O-represents the specific charge capacity.
Detailed Description
The technical solution of the present invention is not limited to the following specific embodiments, but includes any combination of the specific embodiments.
The first embodiment is as follows: the embodiment of the invention relates to a preparation method of a hollow tubular structure FeOOH @ rGO lithium ion battery anode material, which is realized by the following steps:
firstly, performing ultrasonic treatment on foamed nickel by using acetone, hydrochloric acid, absolute ethyl alcohol and deionized water in sequence, and drying in a vacuum oven to obtain dried foamed nickel;
secondly, dissolving graphene oxide in deionized water, stirring, and performing ultrasonic treatment to obtain a graphene oxide aqueous solution;
thirdly, soaking the dried foam nickel obtained in the first step into the graphene oxide aqueous solution obtained in the second step, taking out the foam nickel, drying the foam nickel, and repeating the soaking and drying processes for three times to obtain dried foam nickel-graphene oxide;
fourthly, placing the dried foam nickel-graphene oxide in a tubular furnace, and calcining in an inert atmosphere to obtain a product A;
fifthly, dipping the product A obtained in the fourth step into a ferric salt solution, washing with water, filtering and drying to obtain the hollow tubular structure FeOOH @ rGO lithium ion battery cathode material;
wherein the concentration of the graphene oxide aqueous solution in the second step is 2 mg/ml-10 mg/ml;
in the third step, the mass-to-volume ratio of the foam nickel to the graphene oxide aqueous solution is (200-800) mg (20-80) ml;
the calcining temperature is 400-900 ℃, the time is 2-5 h, and the heating rate is 10 ℃/min;
in the fifth step, the ferric salt is ferric trichloride or ferric nitrate;
and in the fifth step, the mass-to-volume ratio of the product A to the ferric salt solution is (10-100) mg:40 mL.
The second embodiment is as follows: the difference between the first embodiment and the second embodiment is that the hydrochloric acid concentration in the first step is 1 mol/L-5 mol/L. Other steps and parameters are the same as those in the first embodiment.
The third concrete implementation mode: the difference between the first embodiment and the second embodiment is that the ultrasonic treatment time in the first step is 5min to 30 min. Other steps and parameters are the same as those in the first or second embodiment.
The fourth concrete implementation mode: the difference between the first embodiment and the third embodiment is that the drying temperature in the first step is 40-80 ℃ and the drying time is 1-5 h. Other steps and parameters are the same as those in one of the first to third embodiments.
The fifth concrete implementation mode: the difference between the present embodiment and one of the first to fourth embodiments is that the rotation speed of the stirring in the second step is 500rpm to 2000rpm, and the time is 60min to 180 min. Other steps and parameters are the same as in one of the first to fourth embodiments.
The sixth specific implementation mode: the difference between the present embodiment and one of the first to fifth embodiments is that the frequency of the ultrasonic treatment in the second step is 20KHz to 50KHz, and the time is 30min to 60 min. Other steps and parameters are the same as those in one of the first to fifth embodiments.
The seventh embodiment: the difference between this embodiment and one of the first to sixth embodiments is that the immersion time in the third step is 0.5 to 6 hours each time. Other steps and parameters are the same as those in one of the first to sixth embodiments.
The specific implementation mode is eight: the difference between the first and the seventh embodiments is that the first two times of drying in the third step are vacuum-dried for 1 hour at 60 ℃; the third drying adopts freeze drying, the freeze drying temperature is-30 ℃ to-80 ℃, and the freezing time is 20h to 60 h. Other steps and parameters are the same as those in one of the first to seventh embodiments.
The specific implementation method nine: the present embodiment is different from the first to eighth embodiments in that the inert atmosphere in the fourth step is argon or nitrogen. Other steps and parameters are the same as those in one to eight of the embodiments.
The detailed implementation mode is ten: the difference between the present embodiment and one of the first to ninth embodiments is that the concentration of the iron salt solution in the fifth step is 5 to 20 mg/ml. Other steps and parameters are the same as those in one of the first to ninth embodiments.
The concrete implementation mode eleven: the difference between this embodiment and the first to tenth embodiments is that the immersion time in the fifth step is 24 to 48 hours. Other steps and parameters are the same as in one of the first to tenth embodiments.
The specific implementation mode twelve: the difference between this embodiment and the first to the eleventh embodiments is that in the fifth step, the water washing is performed 1 to 3 times by using deionized water. Other steps and parameters are the same as those in one of the first to eleventh embodiments.
The specific implementation mode is thirteen: the difference between the first embodiment and the second embodiment is that the temperature for drying in the fifth step is 50-80 ℃ and the time is 2-4 h. Other steps and parameters are the same as those in one to twelve embodiments.
The beneficial effects of the present invention are demonstrated by the following examples:
example (b):
a preparation method of a hollow tubular structure FeOOH @ rGO lithium ion battery anode material is realized according to the following steps:
firstly, performing ultrasonic treatment on foamed nickel by using acetone, hydrochloric acid, absolute ethyl alcohol and deionized water in sequence, and drying in a vacuum oven to obtain dried foamed nickel;
secondly, dissolving graphene oxide in deionized water, stirring, and performing ultrasonic treatment to obtain a graphene oxide aqueous solution;
thirdly, soaking the dried foam nickel obtained in the first step into the graphene oxide aqueous solution obtained in the second step, taking out the foam nickel, drying the foam nickel, and repeating the soaking and drying processes for three times to obtain dried foam nickel-graphene oxide;
fourthly, placing the dried foam nickel-graphene oxide in a tubular furnace, and calcining in an inert atmosphere to obtain a product A;
fifthly, dipping the product A obtained in the fourth step into a ferric salt solution, washing with water, filtering and drying to obtain the hollow tubular structure FeOOH @ rGO lithium ion battery cathode material;
wherein the concentration of the hydrochloric acid in the step one is 3 mol/L;
the ultrasonic treatment time of the step one is 15 min;
the drying temperature in the step one is 60 ℃, and the drying time is 2 hours;
the rotating speed of the stirring in the second step is 1200rpm, and the time is 120 min;
secondly, the ultrasonic treatment frequency is 30KHz, and the time is 60 min;
secondly, the concentration of the graphene oxide aqueous solution is 5 mg/ml;
the dipping time in the third step is 2 hours each time;
vacuum drying is carried out for 1h at the temperature of 60 ℃ in the first two times of drying in the third step; freeze drying at-80 deg.C for 20 hr;
in the third step, the mass-to-volume ratio of the foamed nickel to the graphene oxide aqueous solution is 500mg:20 ml;
fourthly, the calcining temperature is 800 ℃, the time is 2 hours, and the heating rate is 10 ℃/min;
the inert atmosphere in the step four is argon;
in the fifth step, the ferric salt is ferric trichloride;
in the fifth step, the mass-volume ratio of the product A to the ferric salt solution is 100mg:40 mL;
the concentration of the ferric salt solution in the step five is 5 mg/ml;
the impregnation time in the step five is 24 hours;
washing with deionized water for 2 times in the step five;
and in the fifth step, the drying temperature is 60 ℃ and the drying time is 3 h.
An XRD spectrogram of the hollow tubular structure FeOOH @ rGO negative electrode material prepared in this example is shown in fig. 1, and it can be seen from fig. 1 that a crystal peak of FeOOH is well matched with a standard spectrum, and no impurity peak exists.
The TEM spectrogram of the hollow tubular structure FeOOH @ rGO negative electrode material prepared in this example is shown in fig. 2, and it can be seen from fig. 2 that FeOOH @ rGO maintains the structure of the nickel foam, and the hollow pore size is about 10 um.
The 0.2A/g cycle performance test curve of the hollow tubular FeOOH @ rGO negative electrode material prepared in the embodiment is shown in FIG. 3, and it can be seen that the FeOOH @ rGO is cycled for 100 circles and the capacity reaches 912mAh g–1The capacity of (c).
The multiplying power performance test curve of the hollow tubular structure FeOOH @ rGO negative electrode material prepared in the embodiment is shown in fig. 4, after a 5C high-current test, the hollow tubular structure FeOOH @ rGO negative electrode material is recovered to 0.2C circulation, the capacity is not attenuated, and a stable rising trend still appears, which indicates that the hollow tubular structure FeOOH @ rGO has better circulation stability and multiplying power performance.
The hollow structure of the product prepared by the embodiment effectively relieves the volume expansion, and provides a space for the volume change of FeOOH in the process of lithium intercalation and deintercalation; the micron holes also increase the diffusion of electrolyte to electrode materials, and meanwhile, the three-dimensionally communicated carbon skeleton provides a conductive network, so that the reaction rate is increased; the FeOOH @ rGO obtained by the method shortens the lithium ion transmission path and improves the rate capability.
Claims (10)
1. A preparation method of a hollow tubular structure FeOOH @ rGO lithium ion battery anode material is characterized by comprising the following steps:
firstly, performing ultrasonic treatment on foamed nickel by using acetone, hydrochloric acid, absolute ethyl alcohol and deionized water in sequence, and drying in a vacuum oven to obtain dried foamed nickel;
secondly, dissolving graphene oxide in deionized water, stirring, and performing ultrasonic treatment to obtain a graphene oxide aqueous solution;
thirdly, soaking the dried foam nickel obtained in the first step into the graphene oxide aqueous solution obtained in the second step, taking out the foam nickel, drying the foam nickel, and repeating the soaking and drying processes for three times to obtain dried foam nickel-graphene oxide;
fourthly, placing the dried foam nickel-graphene oxide in a tubular furnace, and calcining in an inert atmosphere to obtain a product A;
fifthly, dipping the product A obtained in the fourth step into a ferric salt solution, washing with water, filtering and drying to obtain the hollow tubular structure FeOOH @ rGO lithium ion battery cathode material;
wherein the concentration of the graphene oxide aqueous solution in the second step is 2 mg/ml-10 mg/ml;
in the third step, the mass-to-volume ratio of the foam nickel to the graphene oxide aqueous solution is (200-800) mg (20-80) ml;
the calcining temperature is 400-900 ℃, the time is 2-5 h, and the heating rate is 10 ℃/min;
in the fifth step, the ferric salt is ferric trichloride or ferric nitrate;
and in the fifth step, the mass-to-volume ratio of the product A to the ferric salt solution is (10-100) mg:40 mL.
2. The preparation method of the hollow tubular structure FeOOH @ rGO lithium ion battery anode material according to claim 1, characterized in that the hydrochloric acid concentration in the step one is 1 mol/L-5 mol/L; the ultrasonic treatment time is 5min to 30 min; the drying temperature is 40-80 ℃, and the drying time is 1-5 h.
3. The preparation method of the hollow tubular structure FeOOH @ rGO lithium ion battery anode material according to claim 1, wherein the stirring speed in the second step is 500-2000 rpm, and the time is 60-180 min.
4. The preparation method of the hollow tubular structure FeOOH @ rGO lithium ion battery anode material according to claim 1, wherein the ultrasonic treatment in the second step has a frequency of 20KHz to 50KHz and a time of 30min to 60 min.
5. The preparation method of the hollow tubular structure FeOOH @ rGO lithium ion battery anode material according to claim 1, characterized in that the dipping time in the third step is 0.5-6 h each time.
6. The preparation method of the hollow tubular structure FeOOH @ rGO lithium ion battery anode material according to claim 1, characterized in that the first two times of drying in the third step are vacuum-dried for 1h at 60 ℃; the third drying adopts freeze drying, the freeze drying temperature is-30 ℃ to-80 ℃, and the freezing time is 20h to 60 h.
7. The preparation method of the hollow tubular structure FeOOH @ rGO lithium ion battery anode material according to claim 1, characterized in that the inert atmosphere in the step four is argon or nitrogen.
8. The preparation method of the hollow tubular structure FeOOH @ rGO lithium ion battery anode material according to claim 1, wherein the concentration of the iron salt solution in the fifth step is 5-20 mg/ml.
9. The preparation method of the hollow tubular structure FeOOH @ rGO lithium ion battery anode material according to claim 1, characterized in that the dipping time in the fifth step is 24-48 h; and the water washing is performed for 1-3 times by using deionized water.
10. The preparation method of the hollow tubular structure FeOOH @ rGO lithium ion battery anode material according to claim 1, characterized in that in the fifth step, the drying temperature is 50-80 ℃ and the drying time is 2-4 h.
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| CN112290002A (en) * | 2020-11-04 | 2021-01-29 | 齐鲁工业大学 | Titanium dioxide hydroxyl ferric oxide cathode material of lithium ion battery and preparation method and application thereof |
| CN112897591A (en) * | 2021-01-21 | 2021-06-04 | 哈尔滨理工大学 | alpha-FeOOH @3DGF quadrangular prism material and synthesis method and application thereof |
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