CN117790728A - Preparation method of carbon tube coated anode material - Google Patents
Preparation method of carbon tube coated anode material Download PDFInfo
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- CN117790728A CN117790728A CN202311785428.7A CN202311785428A CN117790728A CN 117790728 A CN117790728 A CN 117790728A CN 202311785428 A CN202311785428 A CN 202311785428A CN 117790728 A CN117790728 A CN 117790728A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 94
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 93
- 239000010405 anode material Substances 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims description 30
- 239000007789 gas Substances 0.000 claims description 30
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 28
- 239000010406 cathode material Substances 0.000 claims description 15
- 229910052786 argon Inorganic materials 0.000 claims description 14
- 239000007774 positive electrode material Substances 0.000 claims description 14
- MWPLVEDNUUSJAV-UHFFFAOYSA-N anthracene Chemical compound C1=CC=CC2=CC3=CC=CC=C3C=C21 MWPLVEDNUUSJAV-UHFFFAOYSA-N 0.000 claims description 12
- 239000011261 inert gas Substances 0.000 claims description 9
- BBEAQIROQSPTKN-UHFFFAOYSA-N pyrene Chemical compound C1=CC=C2C=CC3=CC=CC4=CC=C1C2=C43 BBEAQIROQSPTKN-UHFFFAOYSA-N 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 claims description 6
- 230000001590 oxidative effect Effects 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- 230000005284 excitation Effects 0.000 claims description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 4
- GVEPBJHOBDJJJI-UHFFFAOYSA-N fluoranthrene Natural products C1=CC(C2=CC=CC=C22)=C3C2=CC=CC3=C1 GVEPBJHOBDJJJI-UHFFFAOYSA-N 0.000 claims description 4
- NIHNNTQXNPWCJQ-UHFFFAOYSA-N fluorene Chemical compound C1=CC=C2CC3=CC=CC=C3C2=C1 NIHNNTQXNPWCJQ-UHFFFAOYSA-N 0.000 claims description 4
- YNPNZTXNASCQKK-UHFFFAOYSA-N phenanthrene Chemical compound C1=CC=C2C3=CC=CC=C3C=CC2=C1 YNPNZTXNASCQKK-UHFFFAOYSA-N 0.000 claims description 4
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 2
- CWRYPZZKDGJXCA-UHFFFAOYSA-N acenaphthene Chemical compound C1=CC(CC2)=C3C2=CC=CC3=C1 CWRYPZZKDGJXCA-UHFFFAOYSA-N 0.000 claims description 2
- 150000004945 aromatic hydrocarbons Chemical class 0.000 claims description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 2
- 239000001569 carbon dioxide Substances 0.000 claims description 2
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 2
- 239000001307 helium Substances 0.000 claims description 2
- 229910052734 helium Inorganic materials 0.000 claims description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 2
- 229910052743 krypton Inorganic materials 0.000 claims description 2
- DNNSSWSSYDEUBZ-UHFFFAOYSA-N krypton atom Chemical compound [Kr] DNNSSWSSYDEUBZ-UHFFFAOYSA-N 0.000 claims description 2
- 229910052754 neon Inorganic materials 0.000 claims description 2
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 238000000859 sublimation Methods 0.000 claims description 2
- 230000008022 sublimation Effects 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 4
- 239000004215 Carbon black (E152) Substances 0.000 claims 1
- 229930195733 hydrocarbon Natural products 0.000 claims 1
- 150000002430 hydrocarbons Chemical class 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 8
- 230000001351 cycling effect Effects 0.000 abstract description 2
- 238000007086 side reaction Methods 0.000 abstract description 2
- 238000000576 coating method Methods 0.000 description 19
- 230000000052 comparative effect Effects 0.000 description 19
- 239000011248 coating agent Substances 0.000 description 14
- 239000000843 powder Substances 0.000 description 12
- 239000002245 particle Substances 0.000 description 11
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 9
- 239000010410 layer Substances 0.000 description 9
- 238000012360 testing method Methods 0.000 description 8
- 229910052744 lithium Inorganic materials 0.000 description 7
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 6
- 230000014759 maintenance of location Effects 0.000 description 6
- 238000002156 mixing Methods 0.000 description 6
- 230000007547 defect Effects 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 239000011247 coating layer Substances 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 230000008021 deposition Effects 0.000 description 4
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 4
- 238000009423 ventilation Methods 0.000 description 4
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 229910052748 manganese Inorganic materials 0.000 description 3
- 239000011572 manganese Substances 0.000 description 3
- 238000001237 Raman spectrum Methods 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000002950 deficient Effects 0.000 description 2
- QHGJSLXSVXVKHZ-UHFFFAOYSA-N dilithium;dioxido(dioxo)manganese Chemical compound [Li+].[Li+].[O-][Mn]([O-])(=O)=O QHGJSLXSVXVKHZ-UHFFFAOYSA-N 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 238000007740 vapor deposition Methods 0.000 description 2
- 241001391944 Commicarpus scandens Species 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 239000002033 PVDF binder Substances 0.000 description 1
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- HFCVPDYCRZVZDF-UHFFFAOYSA-N [Li+].[Co+2].[Ni+2].[O-][Mn]([O-])(=O)=O Chemical compound [Li+].[Co+2].[Ni+2].[O-][Mn]([O-])(=O)=O HFCVPDYCRZVZDF-UHFFFAOYSA-N 0.000 description 1
- RTTUXDWYMFNHKW-UHFFFAOYSA-N [Mn](=O)(=O)([O-])[O-].[Na+].[Co+2].[Ni+2] Chemical compound [Mn](=O)(=O)([O-])[O-].[Na+].[Co+2].[Ni+2] RTTUXDWYMFNHKW-UHFFFAOYSA-N 0.000 description 1
- 239000006230 acetylene black Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000011889 copper foil Substances 0.000 description 1
- 239000002180 crystalline carbon material Substances 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000009396 hybridization Methods 0.000 description 1
- 230000037427 ion transport Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- -1 nickel iron sodium manganate Chemical compound 0.000 description 1
- 238000006864 oxidative decomposition reaction Methods 0.000 description 1
- 238000009832 plasma treatment Methods 0.000 description 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 102220043159 rs587780996 Human genes 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000005019 vapor deposition process Methods 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Landscapes
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention relates to the technical field of battery material preparation, and discloses a preparation method of a carbon tube coated anode material, which comprises the following steps: the preparation method can effectively reduce the side reaction of the anode and cathode interfaces of the battery, thereby reducing interface impedance, and simultaneously, the surface carbon layer can improve electron conductivity and improve the multiplying power performance and the cycling stability of the battery.
Description
Technical Field
The invention relates to the technical field of battery material preparation, in particular to a preparation method of a carbon tube coated anode material.
Background
The conventional oxide cathode materials in lithium ion batteries, such as lithium cobaltate and lithium manganate, have the technical problems of capacity attenuation, short cycle life, low charging speed and the like, and the prior art generally adopts carbon-coated oxide cathode materials to improve the problems, however, the conventional carbon-coated process still has the following technical difficulties:
(1) Interface interactions: in the carbon-coated oxide cathode material, there is an interfacial interaction between the carbon coating and the oxide particles, which may result in an increase in interfacial resistance, a blocked ion transport, and thus an influence on the electrochemical performance and cycle life of the battery.
(2) Stability of the coating: the carbon coating layer may be separated out, broken, stripped and other phenomena in the charge-discharge cycle, so that the cathode material is exposed to the electrolyte, and the attenuation and cycle failure of the material are accelerated.
(3) Uniformity of the coating: the uniformity of the carbon coating has a significant impact on the performance and cycle life of the battery, and uneven coatings may lead to increased local resistance, uneven ion distribution, instability of the battery, and capacity fade.
(4) Conductivity of the carbon coating layer: the conductivity of the carbon coating itself has a direct effect on the performance and charging speed of the battery, and lower carbon coating conductivity may lead to increased resistance, slow charging speed, limiting the power output and fast charging capability of the battery.
Accordingly, there is a need in the art for improvements to carbon coating processes that address the technical difficulties of conventional carbon coating processes.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a preparation method of a carbon tube coated anode material.
The aim of the invention is realized by the following technical scheme:
the preparation method of the carbon tube coated positive electrode material comprises the following steps: and placing the anode material in a plasma reaction furnace, introducing inert gas, heating, introducing carbon source mixed gas, reacting under the condition of plasma excitation, and cooling to obtain the carbon tube coated anode material.
The positive electrode material is at least one of lithium cobaltate, nickel cobalt lithium manganate, nickel cobalt sodium manganate, nickel iron sodium manganate and lithium-rich lithium manganate.
Further, the inert gas is at least one of helium, neon, argon, krypton and nitrogen. Inert gas is introduced as protective gas to avoid oxidative decomposition of the anode material in the heating process.
Further, the temperature is raised to 250-400 ℃.
Further, the carbon source mixed gas is a mixed gas of a carbon source gas, a weak oxidizing gas and an inert gas.
Further, the volume ratio of the carbon source gas to the weak oxidizing gas to the inert gas is (1-4) to (0.5-2) to 20.
Further, the carbon source gas is obtained by sublimation treatment of a carbon source, and the carbon-hydrogen ratio of the carbon source is greater than 1.2.
Further, the carbon source is at least one aromatic hydrocarbon selected from anthracene, pyrene, naphthalene, acenaphthene, phenanthrene and fluorene.
Furthermore, the introducing speed of the carbon source mixed gas is 100-150 mL/min.
Further, the weak oxidizing gas is at least one of carbon monoxide and carbon dioxide.
Further, the reaction under the condition of plasma excitation specifically comprises the following steps: the reaction is carried out for 0.5 to 3 hours under the conditions of 20 to 50W of radio frequency power and 250 to 400 ℃.
Compared with the prior art, the invention has at least the following advantages:
according to the preparation method provided by the invention, the surface of the positive electrode material particles can be uniformly coated with the ordered crystalline carbon layer with defects by controlling the process conditions, the carbon layer is coated on the surface of the positive electrode material, so that the side reaction of the positive electrode and the negative electrode of the battery can be effectively reduced, the interface impedance is reduced, and meanwhile, the electron conductivity of the surface carbon layer can be improved, and the multiplying power performance and the cycling stability of the battery are improved; further, compared with the traditional carbon coating layer, the ordered crystalline carbon layer with defects has better stability, can better relieve the volume expansion of the anode material in charge and discharge cycles, is not easy to crack, and avoids the coating failure of the surface carbon layer.
Drawings
FIG. 1 is a projection electron microscope photograph of a crystalline carbon-coated positive electrode material prepared in example 1 of the present invention;
FIG. 2 is a Raman spectrum of the crystalline carbon-coated cathode material obtained in example 2 of the present invention;
fig. 3 is a battery rate cycle chart of the battery samples prepared in example 3 and comparative example 1 of the present invention.
Detailed Description
In order that the invention may be readily understood, a more complete description of the invention will be rendered by reference to the appended drawings. The drawings illustrate preferred embodiments of the invention. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Example 1: preparation method of carbon tube coated anode material
50g of single crystal NCM 613 Placing powder (powder particle size d50=5mu m) in a reaction chamber of a plasma reaction furnace, introducing argon, heating the reaction chamber to 350 ℃, and starting a radio frequency power supply of the reaction chamber;
gasifying and sublimating anthracene at 350 ℃ to be gaseous, and then mixing with argon and CO 2 Mixed to form a carbon source mixed gas (wherein anthracene is argon and CO) 2 The ratio of (2) is 1:100:0.5), and the carbon source mixed gas is introduced into the reaction chamber at the ventilation rate of 120mL/min, and the carbon tube coated anode material is obtained after the deposition reaction for 1h under the condition that the radio frequency power is 40W and the temperature is 350 ℃ and the temperature is reduced to the room temperature.
Example 2: preparation method of carbon tube coated anode material
50g of polycrystalline NCM 811 Placing powder (the particle size d50=9mu m) in a reaction chamber of a plasma reaction furnace, introducing argon, heating the reaction chamber to 250 ℃, and starting a radio frequency power supply of the reaction chamber;
and (3) gasifying and sublimating naphthalene into a gaseous state at the temperature of 250 ℃, mixing the gaseous state with argon and CO to form carbon source mixed gas (wherein the ratio of anthracene to argon to CO is 3:20:1), introducing the carbon source mixed gas into a reaction chamber at the ventilation rate of 150mL/min, carrying out deposition reaction for 1.5h at the temperature of 250 ℃ under the condition that the radio frequency power is 50W, and cooling to the room temperature to obtain the carbon tube coated anode material.
Example 3: preparation method of carbon tube coated anode material
Placing 50g of monocrystal lithium-rich manganese material (powder particle size D50=4.3 mu m) in a reaction chamber of a plasma reaction furnace, introducing argon, heating the reaction chamber to 400 ℃, and starting a radio frequency power supply of the reaction chamber;
gasifying and sublimating pyrene at 400 ℃ to be gaseous, and then mixing the gaseous pyrene with argon and CO 2 Mixing to form carbon source mixed gas (wherein the ratio of anthracene to argon to CO is 4:20:1), introducing the carbon source mixed gas into a reaction chamber at a ventilation rate of 150mL/min, carrying out deposition reaction for 2h under the condition that the radio frequency power is 50W and the temperature is 400 ℃, and cooling to the room temperature to obtain the carbon tube coated anode material.
Comparative example 1
And directly preparing a battery sample from the monocrystal lithium-rich manganese material without carbon coating treatment.
Comparative example 2
Placing 50g of monocrystal lithium-rich manganese material (powder particle size d50=4.3 mu m) in a reaction chamber of a reaction furnace, introducing argon, and heating the reaction chamber to 600 ℃;
and mixing methane and argon to form a carbon source mixed gas (wherein the ratio of methane to argon is 5:100), introducing the carbon source mixed gas into a reaction chamber at the ventilation rate of 120mL/min, carrying out deposition reaction for 1h at 600 ℃, and cooling to room temperature to obtain the carbon-coated anode material.
Comparative example 3
Comparative example 3 differs from example 1 in that the carbon source used was benzene.
Comparative example 4
Comparative example 4 differs from example 1 in that the plasma excitation treatment was not performed during vapor deposition.
The carbon-coated cathode materials prepared in examples and comparative examples were subjected to a powder conductivity test, a powder particle diameter test, and respectively mixed with acetylene black and polyvinylidene fluoride (binder) in a mass ratio of 80:10:10, mixing to prepare slurry, and uniformly coating the slurry on a copper foil current collector to obtain the positive electrode plate. A coin cell was assembled in an argon-protected glove box using a lithium metal (sodium) sheet as the negative electrode, and then subjected to cell performance testing, with specific results shown in table 1.
Table 1 test results of different examples and comparative examples
| Testing battery | Conductivity of powder (S/cm) | First circle coulombic efficiency (%) | Capacity retention (%) |
| Example 1 | 0.117 | 90.5 | 91.2 (cycle 100 weeks) |
| Example 2 | 0.121 | 91.9 | 90.4 (cycle 100 weeks) |
| Example 3 | 0.127 | 91.5 | 87.3 (cycle 325 weeks) |
| Comparative example 1 | 0.019 | 80.3 | 61.5 (cycle 100 weeks) |
| Comparative example 2 | 0.088 | 89.7 | 69.2 (cycle 325 weeks) |
| Comparative example 3 | 0.087 | 86.7 | 85.4 (cycle 100 weeks) |
| Comparative example 4 | 0.072 | 71.3 | 76.5 (cycle 100 weeks) |
Referring to Table 1 and FIG. 3, the test results of examples 1 to 3 and comparative example 1 show that the conductivity of the prepared powder can be maintained above 0.1S/cm after the carbon coating process of the invention, the initial coulomb efficiency and the capacity retention rate of 100 circles can reach above 90%, the cycle capacity retention rate of 325 circles is above 85%, the conductivity of the cathode material of comparative example 1 without carbon coating is about 0.02S/cm, the capacity retention rate after 100 circles is only 61.5, which indicates that the preparation method of the carbon tube coated cathode material provided by the invention can remarkably improve the conductivity and cycle performance of the cathode material; meanwhile, the particle size distribution (D50) of the positive electrode particles before and after coating in examples 1 to 3 was found to be uniform, (D90-D10)/D50 of 1.2, indicating that the carbon coating of the present invention had little effect on the particle size of the positive electrode particle powder.
FIG. 1 is a crystalline carbon-coated NCM prepared in example 1 613 The projection electron microscope photomicrograph of the material can show that the carbon coating structure with the ordered structure of the type of carbon tube exists, and the crystal lattice of the crystalline carbon material is discontinuous, which is related to the residual alkali corrosion action on the surface of the positive electrode material; FIG. 2 is a crystalline carbon-coated NCM obtained in example 2 811 Raman spectrum of the material. D peak (about 1330 cm) -1 Where) represents defects of carbon atom crystals (characteristic peaks of defective carbon), G peak (about 1580 cm) -1 Where) represents the in-plane stretching vibration (characteristic peak of crystalline carbon) of sp2 hybridization of carbon atoms, the intensity ratio of D peak to G peak of raman is generally used to react the order of the carbon material. From the view I d /I g The number of (2) is about 0.989, indicating that the ordered component of the synthesized carbon structure is comparable to the disordered component content; it can be seen from fig. 1 and fig. 2 that the corrosion of residual alkali on the surface of the positive electrode material can be controlled by the process control of the invention, so that the surface of the positive electrode material is ordered crystalline carbon with defects.
Comparative example 2 is a conventional carbon coating process, a carbon layer with continuous crystal lattice can be formed on the surface of the positive electrode material, but test results show that the battery sample of comparative example 2 has a capacity retention rate of only 69.2% after 325 cycles, and the battery sample of example 3 has a capacity retention rate of 87.3% after 325 cycles, which indicates that the defective ordered crystalline carbon layer has better stability than the conventional carbon coating layer, can better relieve the volume expansion of the positive electrode material in charge and discharge cycles, is not easy to break, and avoids the coating failure of the surface carbon layer.
In comparative example 3, benzene is used as a carbon source, the carbon-hydrogen ratio is 1, and from the test result, it can be seen that the electric conductivity of the powder coated by using benzene as the carbon source and the electric performance of the battery sample are reduced compared with the embodiment, which shows that the carbon source with high carbon-hydrogen ratio can obviously improve the electrochemical performance of the anode material coated by the carbon tube.
The difference between comparative example 4 and example 1 is that the radio frequency power supply is not turned on in the vapor deposition process, i.e. the carbon source gas is not subjected to plasma treatment, and the final prepared sample is tested, so that the powder conductivity and the first circle coulomb effect of the battery sample are both obviously reduced, and the introduction of plasma energy at a lower reaction temperature and a shorter reaction time can improve the vapor deposition efficiency and effect, and simultaneously has an enhancement effect on the adhesion and compactness of the carbon layer.
The above examples illustrate only a few embodiments of the invention, which are described in detail and are not to be construed as limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention. Accordingly, the scope of protection of the present invention is to be determined by the appended claims.
Claims (10)
1. The preparation method of the carbon tube coated positive electrode material is characterized by comprising the following steps of: and placing the anode material in a plasma reaction furnace, introducing inert gas, heating, introducing carbon source mixed gas, reacting under the condition of plasma excitation, and cooling to obtain the carbon tube coated anode material.
2. The method for producing a carbon tube-coated positive electrode material according to claim 1, wherein the inert gas is at least one of helium, neon, argon, krypton, and nitrogen.
3. The method for preparing a carbon tube coated cathode material according to claim 1, wherein the temperature is raised to 250-400 ℃.
4. The method for producing a carbon-tube-coated positive electrode material according to claim 1, wherein the carbon source mixed gas is a mixed gas of a carbon source gas, a weak oxidizing gas and an inert gas.
5. The method for preparing a carbon tube coated cathode material according to claim 4, wherein the volume ratio of the carbon source gas, the weak oxidizing gas and the inert gas is (1-4): (0.5-2): 20.
6. The method for producing a carbon-tube-coated cathode material according to claim 4, wherein the carbon source gas is obtained by sublimation treatment of a carbon source having a hydrocarbon ratio of more than 1.2.
7. The method for preparing a carbon tube coated cathode material according to claim 6, wherein the carbon source is at least one aromatic hydrocarbon selected from anthracene, pyrene, naphthalene, acenaphthene, phenanthrene and fluorene.
8. The method for preparing the carbon tube coated cathode material according to claim 1, wherein the introducing speed of the carbon source mixed gas is 100-150 mL/min.
9. The method for producing a carbon-tube-coated positive electrode material according to claim 5, wherein the weakly oxidizing gas is at least one of carbon monoxide and carbon dioxide.
10. The method for preparing a carbon tube coated cathode material according to claim 1, wherein the reaction under the condition of plasma excitation specifically comprises: the reaction is carried out for 0.5 to 3 hours under the conditions of 20 to 50W of radio frequency power and 250 to 400 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311785428.7A CN117790728A (en) | 2023-12-25 | 2023-12-25 | Preparation method of carbon tube coated anode material |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311785428.7A CN117790728A (en) | 2023-12-25 | 2023-12-25 | Preparation method of carbon tube coated anode material |
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| Publication Number | Publication Date |
|---|---|
| CN117790728A true CN117790728A (en) | 2024-03-29 |
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| CN202311785428.7A Pending CN117790728A (en) | 2023-12-25 | 2023-12-25 | Preparation method of carbon tube coated anode material |
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- 2023-12-25 CN CN202311785428.7A patent/CN117790728A/en active Pending
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