CN106299290B - Amorphous manganese oxide/graphite composite nanomaterial, preparation method thereof and application thereof in lithium ion battery - Google Patents
Amorphous manganese oxide/graphite composite nanomaterial, preparation method thereof and application thereof in lithium ion battery Download PDFInfo
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Abstract
The invention discloses an amorphous manganese oxide/graphite composite nano material, a preparation method thereof and application thereof in a lithium ion battery, belonging to the technical field of lithium ion battery materials‑1After circulating for 250 circles under the current density of 977mA h g‑1And at a high current density (1000mA g)‑1) Under the condition of (1), after circulating for 200 circles, the reversible capacity can still be maintained at 300 mA h g‑1The above.
Description
Technical Field
The invention belongs to the technical field of lithium ion battery materials, and particularly relates to an amorphous manganese oxide/graphite composite nano material, a preparation method thereof and application thereof in a lithium ion battery.
Background
Currently, society, which is the subject of energy, information, and environment, is eagerly looking to develop new energy sources that are efficient, clean, and recyclable. Rechargeable lithium ion batteries have received great attention as one of green energy sources. The design and synthesis of the lithium battery cathode material with high reversible capacity, excellent rate performance, ultra-long cycle life and low price are one of the important development directions of the lithium ion battery. Transition metal oxides with high theoretical capacity, including CoO, Co3O4、Fe2O3、SnO2、Mn3O4、MoO2And the like, are promising new concept lithium battery negative electrode materials. Wherein the manganese oxide (MnO)x) Including MnO and Mn3O4、Mn2O3、MnO2Due to its low voltage plateau (0.2V-0.4V) and high theoretical capacity (e.g. MnO)2Theoretical capacity of 1223mAh g-1) And the environment-friendly property, etc., are increasingly concerned by people. The redox reaction of lithium and manganese oxide occurs in the charge-discharge process of the manganese oxide negative electrode material, and the reaction formula is as follows:
during the lithium removal/insertion process, the manganese oxide undergoes huge volume change, so that the capacity of the material is rapidly reduced; in addition, poor conductivity of manganese oxide makes rate performance poor. Therefore, inhibiting the volume expansion of the active material and increasing the conductivity are important means for improving the electrochemical performance of the material. The invention artificially designs and synthesizes the graphite-loaded amorphous manganese oxide nanoparticles to improve the electrochemical performance of the material.
Studies have shown that amorphous materials provide more lithium storage sites and shorter lithium ion diffusion paths. Juche Guo et al prepared amorphous MnO by spray drying methodx-C, and applying it to a lithium ion battery anode material. MnO of amorphous phase during lithium extraction and insertionxThe reaction rate is high, and is 200mA g-1After circulating for 135 circles under the current density, the reversible capacity of the lithium ion battery is still kept to be 650mAh g-1。
The invention successfully synthesizes amorphous MnO uniformly loaded on graphite flakes by a simple ball milling processxAnd (3) nanoparticles. When the amorphous manganese oxide/graphite composite nano material is used as a negative electrode material of a lithium ion battery, the amorphous manganese oxide/graphite composite nano material has excellent cycle stability of 200mA g-1After the current density of the material is circulated for 250 circles, the material can keep 977mAh g-1The reversible capacity of (a). The method has the advantages of simple process, cheap and easily-obtained raw materials, low cost, environmental friendliness, high efficiency and the like, and can be applied to large-scale industry.
Disclosure of Invention
In order to make up the defects of the prior art, the primary object of the invention is to provide an amorphous manganese oxide/graphite composite nano material.
The invention also aims to provide a method for preparing the amorphous manganese oxide/graphite composite nano material with low cost, high efficiency and large scale.
The invention further aims to provide the application of the amorphous phase manganese oxide/graphite composite nano material as a high-performance lithium ion battery cathode material.
The purpose of the invention is realized by the following technical scheme.
A preparation method of amorphous manganese oxide/graphite composite nano material is a ball milling method, and specifically comprises the following steps:
(1) weighing graphite and KMnO4Adding water and zirconium balls (milling media), and carrying out ball milling for 2-100 h;
(2) and then separating, ultrasonically treating, filtering, washing and drying the product to obtain the amorphous manganese oxide/graphite composite nano material.
Preferably, the graphite is one or more of natural graphite, expanded graphite and artificial graphite.
Preferably, the rotation speed during ball milling is 300-500 rpm.
Preferably, the mass fraction of graphite in the amorphous manganese oxide/graphite composite nano material is 5.2-58.6%.
More preferably, the mass fraction of graphite in the amorphous manganese oxide/graphite composite nanomaterial is 26.7% -43.2%.
More preferably, the mass fraction of graphite in the amorphous manganese oxide/graphite composite nanomaterial is 38.3%.
Preferably, the mass ratio of the zirconium balls to the raw materials is 3: 1-25: 1; the raw materials are graphite and KMnO4。
In the preparation method, the ball milling mainly has the following three functions; (1) so that KMnO4Carrying out oxidation-reduction reaction with graphite to generate manganese oxide; (2) the number of layers of graphite is effectively reduced; (3) so that the amorphous manganese oxide is uniformly dispersed on the exfoliated graphite sheet.
In the above preparation method, the main purpose of washing is to wash away potassium salt generated during the reaction.
The amorphous manganese oxide/graphite composite nano material prepared by the preparation method.
The amorphous manganese oxide/graphite composite nanomaterial is applied as a negative electrode material of a lithium ion battery.
Preferably, the above specific application process is: and mixing the amorphous manganese oxide/graphite composite nanomaterial, carbon black and PVDF to prepare slurry, and coating the slurry on copper foil to obtain the lithium ion battery cathode.
Further preferably, the application process is: weighing 0.2g of amorphous manganese oxide/graphite composite nano material, 0.025g of PVDF and 0.025g of carbon black, mixing and grinding the materials, transferring the materials into a small glass bottle, adding 1ml of NMP, magnetically stirring the materials for 4 hours, coating the materials on copper foil to prepare an electrode, and assembling the electrode into a CR2016 type button battery in a glove box by taking metal lithium as a counter electrode.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) the invention adopts a simple ball milling method to synthesize the amorphous manganese oxide/graphite composite nano material in one step and successfully apply the amorphous manganese oxide/graphite composite nano material to the lithium ion battery cathode material. The amorphous manganese oxide particles are dispersed on the surface of the stripped graphite, so that the volume change of the manganese oxide in the charging and discharging process is effectively relieved, the agglomeration of manganese oxide is inhibited, the conductivity is increased, and the electrochemical stability of the material is improved.
(2) The method adopts a simple ball milling method, utilizes mechanical force and strong oxidation effect of potassium permanganate, and successfully strips the natural graphite into fewer layers of graphite (10-15 layers).
(3) The raw material KMnO used in the invention4And graphite is cheap, and the method used by the invention is a ball milling method, so that the graphite can be synthesized in a large amount. Besides, the invention has the characteristics of simple process, no pollution and the like. Thus, the present invention has the potential for large-scale industrial production.
(4) The amorphous manganese oxide/graphite composite nano material is used for the negative pole of a lithium ion batteryVery often has good cycle performance: when the mass fraction of the graphite in the composite nano material is 11.9-43.2%, the current density is 200mAg-1After 50-250 circles of downward circulation, the reversible capacity is 510-977 mAh g-1. Therefore, the lithium ion negative electrode material prepared by the invention has good cycle performance and can bear more than 200 charge-discharge cycles.
(5) When the amorphous manganese oxide/graphite composite nano material is used for the negative electrode of a lithium ion battery, a sample with the graphite mass fraction of 26.7-38.3% has the current density of 1000mA g-1After circulating for 200-250 circles, the reversible capacity is 301-331 mAh g-1. Therefore, the lithium ion battery cathode material prepared by the invention is still suitable for use under a higher current density, and provides guarantee for the use of the lithium ion battery under a higher power.
Drawings
Fig. 1 and fig. 2 are TEM images of amorphous manganese oxide/graphite composite nanomaterial of example 3 of the present invention at different magnifications.
Fig. 3 is an SEM image of the amorphous manganese oxide/graphite composite nanomaterial obtained in example 4 of the present invention.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the present invention is not limited thereto.
Example 1
Weighing 0.75g of graphite, 14.25g of potassium permanganate and 75g of zirconium balls (grinding media) in sequence, adding the graphite, adding 50ml of water into a ball milling tank, adding a sealing ring, reacting for 48 hours at 400rpm, filtering the obtained sample by a screen, performing ultrasonic treatment on the zirconium balls for 2 hours, performing centrifugal washing for 4 times by using distilled water, and drying for 12 hours at 60 ℃ to obtain the amorphous manganese oxide/graphite composite nanomaterial.
0.2g of the amorphous manganese oxide/graphite composite nanomaterial prepared in the embodiment, 0.025g of PVDF and 0.025g of carbon black are weighed, mixed and ground, transferred into a small glass bottle, added with 1ml of NMP, magnetically stirred for 4 hours, coated on copper foil to prepare an electrode, and assembled into a CR2016 type button cell in a glove box by taking metal lithium as a counter electrode, and subjected to electrochemical performance test.
Example 2
Weighing 1.5g of graphite, 13.5g of potassium permanganate and 75g of zirconium balls (grinding media) in sequence, adding the graphite, adding 50ml of water into a ball milling tank, adding a sealing ring, reacting for 48 hours at 400rpm, filtering the obtained sample by a screen, performing ultrasonic treatment on the zirconium balls for 2 hours, performing centrifugal washing for 4 times by using distilled water, and drying for 12 hours at 60 ℃ to obtain the amorphous manganese oxide/graphite composite nanomaterial.
0.2g of the amorphous manganese oxide/graphite composite nanomaterial prepared in the embodiment, 0.025g of PVDF and 0.025g of carbon black are weighed, mixed and ground, transferred into a small glass bottle, added with 1ml of NMP, magnetically stirred for 4 hours, coated on copper foil to prepare an electrode, and assembled into a CR2016 type button cell in a glove box by taking metal lithium as a counter electrode, and subjected to electrochemical performance test.
Example 3
Weighing 4.5g of graphite, 10.5g of potassium permanganate and 75g of zirconium balls (grinding media) in sequence, adding the graphite, adding 50ml of water into a ball milling tank, adding a sealing ring, reacting for 48 hours at 400rpm, filtering the obtained sample by a screen, performing ultrasonic treatment on the zirconium balls for 2 hours, performing centrifugal washing for 4 times by using distilled water, and drying for 12 hours at 60 ℃ to obtain the amorphous manganese oxide/graphite composite nanomaterial.
The TEM images of the amorphous manganese oxide/graphite composite nanomaterial prepared in this example under different magnifications are shown in fig. 1 and fig. 2, and it can be seen from these images that the present invention successfully exfoliates natural graphite into graphite (10-15 layers) with a small number of layers by using mechanical force and strong oxidation effect of potassium permanganate with a simple ball milling method.
0.2g of the amorphous manganese oxide/graphite composite nanomaterial prepared in the embodiment, 0.025g of PVDF and 0.025g of carbon black are weighed, mixed and ground, transferred into a small glass bottle, added with 1ml of NMP, magnetically stirred for 4 hours, coated on copper foil to prepare an electrode, and assembled into a CR2016 type button cell in a glove box by taking metal lithium as a counter electrode, and subjected to electrochemical performance test.
Example 4
Weighing 3.75g of graphite, 11.25g of potassium permanganate and 75g of zirconium balls (grinding media) in sequence, adding the graphite, adding 50ml of water into a ball milling tank, adding a sealing ring, reacting for 48 hours at 400rpm, filtering the obtained sample by a screen, performing ultrasonic treatment on the zirconium balls for 2 hours, performing centrifugal washing for 4 times by using distilled water, and drying for 12 hours at 60 ℃ to obtain the amorphous manganese oxide/graphite composite nanomaterial.
The SEM image of the amorphous manganese oxide/graphite composite nanomaterial obtained in this example is shown in fig. 3.
0.2g of the amorphous manganese oxide/graphite composite nanomaterial prepared in the embodiment, 0.025g of PVDF and 0.025g of carbon black are weighed, mixed and ground, transferred into a small glass bottle, added with 1ml of NMP, magnetically stirred for 4 hours, coated on copper foil to prepare an electrode, and assembled into a CR2016 type button cell in a glove box by taking metal lithium as a counter electrode, and subjected to electrochemical performance test.
Example 5
Weighing 3g of graphite, 12g of potassium permanganate and 75g of zirconium balls (grinding media) in sequence, adding the graphite, the potassium permanganate and the zirconium balls into a ball milling tank, adding 50ml of water into the ball milling tank, adding a sealing ring, reacting for 48 hours at 400rpm, filtering the obtained sample by a screen, ultrasonically treating for 2 hours, centrifugally washing for 4 times by using distilled water, and drying for 12 hours at 60 ℃ to obtain the amorphous manganese oxide/graphite composite nanomaterial.
0.2g of the amorphous manganese oxide/graphite composite nanomaterial prepared in the embodiment, 0.025g of PVDF and 0.025g of carbon black are weighed, mixed and ground, transferred into a small glass bottle, added with 1ml of NMP, magnetically stirred for 4 hours, coated on copper foil to prepare an electrode, and assembled into a CR2016 type button cell in a glove box by taking metal lithium as a counter electrode, and subjected to electrochemical performance test.
Example 6
Weighing 5.25g of graphite, 9.75g of potassium permanganate and 75g of zirconium balls (grinding media) in sequence, adding the graphite, adding 50ml of water into a ball milling tank, adding a sealing ring, reacting for 48 hours at 400rpm, filtering the obtained sample by a screen, performing ultrasonic treatment on the zirconium balls for 2 hours, performing centrifugal washing for 4 times by using distilled water, and drying for 12 hours at 60 ℃ to obtain the amorphous manganese oxide/graphite composite nanomaterial.
0.2g of the amorphous manganese oxide/graphite composite nanomaterial prepared in the embodiment, 0.025g of PVDF and 0.025g of carbon black are weighed, mixed and ground, transferred into a small glass bottle, added with 1ml of NMP, magnetically stirred for 4 hours, coated on copper foil to prepare an electrode, and assembled into a CR2016 type button cell in a glove box by taking metal lithium as a counter electrode, and subjected to electrochemical performance test.
Example 7
Weighing 7.5g of graphite, 7.5g of potassium permanganate and 75g of zirconium balls (grinding media) in sequence, adding the graphite, adding 50ml of water into a ball milling tank, adding a sealing ring, reacting for 48 hours at 400rpm, filtering the obtained sample by a screen, performing ultrasonic treatment on the zirconium balls for 2 hours, performing centrifugal washing for 4 times by using distilled water, and drying for 12 hours at 60 ℃ to obtain the amorphous manganese oxide/graphite composite nanomaterial.
0.2g of the amorphous manganese oxide/graphite composite nanomaterial prepared in the embodiment, 0.025g of PVDF and 0.025g of carbon black are weighed, mixed and ground, transferred into a small glass bottle, added with 1ml of NMP, magnetically stirred for 4 hours, coated on copper foil to prepare an electrode, and assembled into a CR2016 type button cell in a glove box by taking metal lithium as a counter electrode, and subjected to electrochemical performance test.
Example 8
Weighing 3g of graphite, 12g of potassium permanganate and 45g of zirconium balls (grinding media) in sequence, adding the graphite, adding 50ml of water into a ball milling tank, adding a sealing ring, reacting for 2 hours at 500rpm, filtering the obtained sample by a screen to obtain the zirconium balls, carrying out ultrasonic treatment for 2 hours, carrying out centrifugal washing for 4 times by using distilled water, and drying for 12 hours at 60 ℃ to obtain the amorphous manganese oxide/graphite composite nanomaterial.
0.2g of the amorphous manganese oxide/graphite composite nanomaterial prepared in the embodiment, 0.025g of PVDF and 0.025g of carbon black are weighed, mixed and ground, transferred into a small glass bottle, added with 1ml of NMP, magnetically stirred for 4 hours, coated on copper foil to prepare an electrode, and assembled into a CR2016 type button cell in a glove box by taking metal lithium as a counter electrode, and subjected to electrochemical performance test.
Example 9
Weighing 3g of graphite, 12g of potassium permanganate and 375g of zirconium balls (grinding media) in sequence, adding the graphite, the potassium permanganate and the zirconium balls into a ball milling tank, adding 50ml of water into the ball milling tank, adding a sealing ring, reacting for 100 hours at 300rpm, filtering the obtained sample by a screen, ultrasonically treating for 2 hours, centrifugally washing for 4 times by using distilled water, and drying for 12 hours at 60 ℃ to obtain the amorphous manganese oxide/graphite composite nanomaterial.
0.2g of the amorphous manganese oxide/graphite composite nanomaterial prepared in the embodiment, 0.025g of PVDF and 0.025g of carbon black are weighed, mixed and ground, transferred into a small glass bottle, added with 1ml of NMP, magnetically stirred for 4 hours, coated on copper foil to prepare an electrode, and assembled into a CR2016 type button cell in a glove box by taking metal lithium as a counter electrode, and subjected to electrochemical performance test.
And (3) performance testing:
the materials prepared in the above examples were analyzed for composition, morphology, particle size, and graphite content using X-ray diffraction (XRD), Raman spectroscopy (Raman Spectra), fourier transform infrared spectroscopy (FT-IR), Scanning Electron Microscope (SEM), Transmission Electron Microscope (TEM), and thermogravimetric analysis (TGA) as characterization means.
After the battery prepared in the embodiment is placed for 12h, the battery tester (Shenzhen Xinwei) and BTS7.5.5 software are adopted, the test temperature is room temperature, and the current density is 50mA g-1～1000mA g-1In the case of (2), the battery was subjected to constant current charge and discharge (discharge cutoff voltage of 0.01V, charge voltage of 3V), and the cycle performance and rate performance of the battery were tested. The electrical properties of the samples are detailed in table 1. It was subjected to Cyclic Voltammetry (CV) and alternating current impedance testing using an electrochemical workstation (CHI600E, shanghai chenhua).
TABLE 1
Note: the "content of graphite" in the table refers to the mass fraction of graphite in the product, obtained by a thermal analyzer.
The invention prepares the amorphous manganese oxide/graphite composite nano material by using a ball milling method, researches the synthesis conditions of the material by changing the proportion of raw materials and the ball-to-material ratio, and researches the electrochemical properties of the corresponding material, including the cycle performance, the rate performance and the like. By comparing 9 examples, the samples with the graphite mass fraction of 26.7-43.2% have good circulation performance when the ball-to-feed ratio is 5:1, and the graphite mass fraction can be 200mA g-1Current density hold after 50 cycles500mA h g-1The above reversible capacity; and the capacity is continuously increased along with the increase of the cycle number, particularly after the sample with the graphite mass fraction of 38.3% is circulated for 250 circles, the reversible capacity reaches 977mA h g-1. Meanwhile, the sample with a graphite mass fraction of 43.2% was used even at a relatively large current density (1000mA g)-1) After circulating for 200 circles, the electric heating kettle can maintain 331mA h g-1The reversible capacity of (a).
The present invention is not limited to the above-described embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (8)
1. The preparation method of the amorphous manganese oxide/graphite composite nano material is characterized by comprising the following steps of:
(1) weighing graphite and KMnO4Adding water and zirconium balls, and carrying out ball milling for 2 ~ 100h, wherein the zirconium balls are milling media;
(2) then separating, ultrasonically treating, filtering, washing and drying the product to obtain the amorphous manganese oxide/graphite composite nano material, wherein the graphite in the amorphous manganese oxide/graphite composite nano material is graphite with a small number of layers, and the number of the layers of the graphite is 10 ~ 15 layers;
the rotating speed during ball milling is 300 ~ 500 rpm;
the mass ratio of the zirconium balls to the raw materials is 3:1 ~ 25:1, and the raw materials are graphite and KMnO4。
2. The method according to claim 1, wherein the graphite is one or more of natural graphite and artificial graphite.
3. The preparation method of claim 1, wherein the mass fraction of graphite in the amorphous manganese oxide/graphite composite nanomaterial is 5.2% ~ 58.6.6%.
4. The preparation method of claim 1, wherein the mass fraction of graphite in the amorphous manganese oxide/graphite composite nanomaterial is 26.7% ~ 43.2.2%.
5. The preparation method according to claim 1, wherein the mass fraction of graphite in the amorphous manganese oxide/graphite composite nanomaterial is 38.3%.
6. An amorphous manganese oxide/graphite composite nanomaterial prepared by the preparation method of any one of claims 1 to 5.
7. The use of the amorphous manganese oxide/graphite composite nanomaterial of claim 6 as a negative electrode material of a lithium ion battery.
8. The application of claim 7, wherein the specific application process is as follows: and mixing the amorphous manganese oxide/graphite composite nanomaterial, carbon black and PVDF to prepare slurry, and coating the slurry on copper foil to obtain the lithium ion battery cathode.
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