CN111517304B - Lithium ion battery cathode material and preparation method thereof - Google Patents
Lithium ion battery cathode material and preparation method thereof Download PDFInfo
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- CN111517304B CN111517304B CN202010479919.9A CN202010479919A CN111517304B CN 111517304 B CN111517304 B CN 111517304B CN 202010479919 A CN202010479919 A CN 202010479919A CN 111517304 B CN111517304 B CN 111517304B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
- C01B32/16—Preparation
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1393—Processes of manufacture of electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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- 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
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- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Abstract
The invention relates to the technical field of lithium batteries, and discloses a lithium ion battery cathode material and a preparation method thereof, wherein the lithium ion battery cathode material consists of a plurality of layers of carbon nano tubes, and the preparation method of the lithium ion battery cathode material uses the materials for preparation, and comprises the following steps: the method comprises the steps of starting a resistance heating furnace, adjusting a temperature controller to set a proper preheating temperature, carrying out heat preservation on the resistance heating furnace for the first time after preheating treatment, starting a raw material tank, observing ferrocene inside a quartz boat inside a quartz tube through an observation electron microscope, and checking the crystallization state of a multilayer carbon nano tube on the surface of the ferrocene. According to the lithium ion battery cathode material and the preparation method thereof, the purposes of improving the yield and quality of preparation are achieved through the arrangement of primary heat preservation and secondary heat preservation, the safety in the preparation process is improved through the arrangement of the laser emitter, and the purpose of rapid adjustment according to different problems is achieved through the arrangement of an observation electron microscope.
Description
Technical Field
The invention relates to the technical field of lithium batteries, in particular to a lithium ion battery cathode material and a preparation method thereof.
Background
The development of science and technology is driving the development of chemical power sources towards high capacity, low energy consumption, no pollution and the like. The development of chemical sources of electrical energy has mainly gone through several stages: lead-acid batteries, nickel-cadmium batteries, nickel-hydrogen batteries and lithium batteries. The lithium ion battery has the advantages of high energy density, long cycle life, small self-discharge rate, environmental protection and the like, and has attracted more and more attention, and the research on the lithium ion battery and the improvement on the performance of the lithium ion battery become a research hotspot in the field of chemical power sources. Negative electrode materials for lithium batteries are mainly classified into carbon materials and non-carbon materials, and non-carbon materials include metal oxides, intermetallic compounds, metal nitrides, and the like. Although the capacity of the non-carbon negative electrode material is higher than that of the carbon material, the non-carbon negative electrode material is inferior to the carbon material in terms of cycle stability. Because agglomeration, powdering, cracking and flaking of the electrode during the recycling process, although alleviated to some extent by various methods, are still not practically applicable.
The lithium ion battery cathode material generally uses carbon nano tubes, and has the advantages that the length of the carbon tubes is limited, the lithium ion extraction depth is small, the path is relatively short, the charge-discharge polarization degree of the electrodes under large current is small, in addition, the structure is stable, the conductivity is good, the chemical vapor deposition method is mostly adopted for preparing the carbon nano tubes, the operation is simple, the preparation effect is good, but the chemical vapor deposition method has the defects that the temperature of a heating furnace is high, the use is dangerous, the manufacturing quality of the poor heat preservation effect is reduced to some extent during the preparation, and the carbon nano tubes in the preparation are difficult to observe and detect.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides the lithium ion battery cathode material and the preparation method thereof, which have the advantages of convenience in observation, improved heat preservation effect, capability of carrying out auxiliary heating and the like, and solve the problems of danger caused by higher temperature of a heating furnace, reduced manufacturing quality and difficulty in observation.
(II) technical scheme
In order to realize the purposes of convenient observation, improved heat preservation effect and auxiliary heating, the invention provides the following technical scheme: the preparation method of the lithium ion battery cathode material comprises the following steps:
1) starting the resistance heating furnace, adjusting the temperature controller to be set to a proper preheating temperature to increase the temperature in the resistance heating furnace, preheating the interior of the resistance heating furnace, and performing primary heat preservation on the resistance heating furnace after preheating;
2) putting ferrocene into the middle part of a quartz boat, putting the quartz boat in the quartz tube, wrapping the outer wall of the quartz tube with a transparent heat transfer layer, and installing a heating belt at the end of the quartz tube;
3) inserting one end of a raw material tube at the inlet end of the quartz tube, fixedly connecting one end of a peristaltic pump with the outer wall of the quartz tube, and inserting an argon tube at the inlet end of the quartz tube to complete the preparation work before preparation;
4) starting a raw material tank, adding acetylene in the raw material tank into the quartz tube through a raw material tube, starting an argon tank, controlling the rate of argon flowing into the quartz tube through a flow controller on the surface of an argon tube, and preheating the acetylene and the argon through a heating belt;
5) moving one end of a quartz tube into the resistance heating furnace through a peristaltic pump to enable a quartz boat in the quartz tube to be just positioned at an emitting port of a laser emitter, additionally arranging a tail gas treatment device at the outlet end of the other end of the quartz tube, starting the laser emitter to heat the quartz tube, adjusting a temperature controller again to enable the temperature in the resistance heating furnace to rise, carrying out timing reaction, and timing for 15 minutes;
6) observing ferrocene inside a quartz boat inside the quartz tube through an observation electron microscope and checking the crystallization state of the multilayer carbon nano tube on the surface of the ferrocene;
7) and after the preparation is finished, carrying out secondary heat preservation on the quartz tube for 5 minutes, blowing air into the surface of the quartz tube and the inner wall of the resistance heating furnace through the air box after the heat preservation is finished, accelerating the cooling of the quartz tube and the resistance heating furnace, and taking out the multilayer carbon nano tubes in the quartz boat.
Preferably, the preheating temperature in the step 1 is between 500-700 ℃, and the first heat preservation time of the resistance heating furnace is 3 minutes.
Preferably, the flow rate of the peristaltic pump in the step 5 is 7.2ml/h, the distance between the laser emitter and the quartz tube is 2cm, and the maximum temperature of the resistance heating furnace is not more than 900 ℃.
Preferably, in the step 4, the flow rate of argon in the argon tube is less than 10ml/s, the flow rate of acetylene is 15ml/s, the length of the heating belt is 10cm, and the argon tube and the raw material tube are inserted into one end of the heating belt.
Preferably, the heating temperature of the heating zone in the step 4 is 170 ℃, and the heat transfer efficiency of the heating zone is 80%.
Preferably, the temperature of the second heat preservation in the step 7 is between 300 ℃ and 350 ℃, the cooling time is 10 minutes, and the temperature of the surface of the quartz tube when the quartz tube is taken out is less than 70 ℃.
(III) advantageous effects
Compared with the prior art, the invention provides a lithium ion battery cathode material and a preparation method thereof, and the lithium ion battery cathode material has the following beneficial effects:
1. according to the lithium ion battery cathode material and the preparation method thereof, the first heat preservation and the second heat preservation are adopted, carbon atoms in acetylene can be separated out better in the preparation process, the yield and the quality of preparation are improved, the laser emitter is adopted to perform auxiliary heating on the quartz tube in the preparation process, the heating temperature of the resistance heating furnace is reduced, the preparation temperature is greatly reduced, and the safety in the preparation process is improved.
2. According to the lithium ion battery cathode material and the preparation method thereof, the carbon nano tube precipitated on the ferrocene surface in the quartz boat is observed through the observation electron microscope in the preparation process through the arrangement of the observation electron microscope, the effect of implementation observation is achieved, the purpose of monitoring the prepared carbon nano tube in real time and performing quick adjustment according to different problems is achieved.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Opening a resistance heating furnace, adjusting a temperature controller to a proper preheating temperature to raise the temperature inside the resistance heating furnace, preheating the inside of the resistance heating furnace, performing heat preservation on the resistance heating furnace for the first time after preheating, placing ferrocene in the middle of a quartz boat, placing the quartz boat in the quartz tube, wrapping the outer wall of the quartz tube with a transparent heat transfer layer, installing a heating belt at the end of the quartz tube, inserting one end of a raw material tube in the inlet end of the quartz tube, fixedly connecting one end of a peristaltic pump with the outer wall of the quartz tube, inserting an argon tube in the inlet end of the quartz tube, completing the preparation work before preparation, opening the raw material tank, adding acetylene in the raw material tank into the quartz tube through the raw material tube, opening the argon tank, controlling the flow rate of argon flowing into the quartz tube through the flow controller on the surface of the argon tube, and preheating the acetylene and the argon through the heating belt, one end of the quartz tube is moved to the interior of the resistance heating furnace through the peristaltic pump, so that the quartz boat in the quartz tube is just positioned at the transmitting port of the laser transmitter, a tail gas treatment device is additionally arranged at the outlet end of the other end of the quartz tube, the laser emitter is started to heat the quartz tube, the temperature controller is adjusted again to increase the temperature in the resistance heating furnace, the timing reaction is carried out, the timing time is 15 minutes, observe and inspect the brilliant state of formation of multilayer carbon nanotube on ferrocene surface through observing electron microscope to the inside ferrocene of quartz boat of quartz tube inside, keep warm the quartz tube for the second time after the preparation, the heat preservation time is 5 minutes, blow in the air through bellows to the surface of quartz tube and resistance heating furnace's inner wall after the heat preservation is accomplished for the cooling of quartz tube and resistance heating furnace takes out the inside multilayer carbon nanotube of quartz boat.
The first embodiment is as follows:
a preparation method of a lithium ion battery negative electrode material comprises the following steps:
and starting the resistance heating furnace, adjusting the temperature controller to be set to a proper preheating temperature, raising the temperature in the resistance heating furnace, preheating the interior of the resistance heating furnace, and performing primary heat preservation on the resistance heating furnace after preheating.
The ferrocene is placed in the middle of the quartz boat, the quartz boat is placed in the quartz tube, the outer wall of the quartz tube is wrapped with the transparent heat transfer layer, and the end of the quartz tube is provided with the heating belt.
One end of the raw material tube is inserted into the inlet end of the quartz tube, one end of the peristaltic pump is fixedly connected with the outer wall of the quartz tube, and the argon tube is inserted into the inlet end of the quartz tube, so that the preparation work before preparation is completed.
The raw material tank is opened, acetylene inside the raw material tank is added into the quartz tube through the raw material tube, the argon tank is opened, the flow controller on the surface of the argon tube controls the rate of argon flowing into the quartz tube, and acetylene and argon are subjected to preheating treatment through the heating belt.
Move the inside of resistance heating furnace through the one end of peristaltic pump with the quartz capsule, make the quartz boat of quartz capsule inside just be in laser emitter's transmission mouth department, install tail gas processing apparatus additional at the other end exit end of quartz capsule, open laser emitter and heat the quartz capsule, adjust temperature controller once more, make the inside temperature rise of resistance heating furnace, carry out the timing reaction, timing time 15 minutes.
Observing the ferrocene in the quartz boat inside the quartz tube through an observation electron microscope and checking the crystallization state of the multilayer carbon nano tube on the surface of the ferrocene.
And after the preparation is finished, carrying out secondary heat preservation on the quartz tube for 5 minutes, blowing air into the surface of the quartz tube and the inner wall of the resistance heating furnace through the air box after the heat preservation is finished, accelerating the cooling of the quartz tube and the resistance heating furnace, and taking out the multilayer carbon nano tubes in the quartz boat.
Compared with the prior art, the first embodiment has better heat preservation effect, and the prepared carbon nano tube has more uniform structure.
Example two:
a preparation method of a lithium ion battery negative electrode material comprises the following steps:
and starting the resistance heating furnace, adjusting the temperature controller to be set to a proper preheating temperature, raising the temperature in the resistance heating furnace, preheating the interior of the resistance heating furnace, and performing primary heat preservation on the resistance heating furnace after preheating.
The ferrocene is placed in the middle of the quartz boat, the quartz boat is placed in the quartz tube, the outer wall of the quartz tube is wrapped with the transparent heat transfer layer, and the end of the quartz tube is provided with the heating belt.
One end of the raw material tube is inserted into the inlet end of the quartz tube, one end of the peristaltic pump is fixedly connected with the outer wall of the quartz tube, and the argon tube is inserted into the inlet end of the quartz tube, so that the preparation work before preparation is completed.
The raw material tank is opened, acetylene inside the raw material tank is added into the quartz tube through the raw material tube, the argon tank is opened, the flow controller on the surface of the argon tube controls the rate of argon flowing into the quartz tube, and acetylene and argon are subjected to preheating treatment through the heating belt.
Move the inside of resistance heating furnace through the one end of peristaltic pump with the quartz capsule, make the quartz boat of quartz capsule inside just be in laser emitter's transmission mouth department, install tail gas processing apparatus additional at the other end exit end of quartz capsule, open laser emitter and heat the quartz capsule, adjust temperature controller once more, make the inside temperature rise of resistance heating furnace, carry out the timing reaction, timing time 15 minutes.
Observing the ferrocene in the quartz boat inside the quartz tube through an observation electron microscope and checking the crystallization state of the multilayer carbon nano tube on the surface of the ferrocene.
And after the preparation is finished, carrying out secondary heat preservation on the quartz tube for 5 minutes, blowing air into the surface of the quartz tube and the inner wall of the resistance heating furnace through the air box after the heat preservation is finished, accelerating the cooling of the quartz tube and the resistance heating furnace, and taking out the multilayer carbon nano tubes in the quartz boat.
In comparison with the first embodiment, the distance between each layer of the carbon nanotubes is changed from 0.3nm to 0.32nm.
Example three:
a preparation method of a lithium ion battery negative electrode material comprises the following steps:
and starting the resistance heating furnace, adjusting the temperature controller to be set to a proper preheating temperature, raising the temperature in the resistance heating furnace, preheating the interior of the resistance heating furnace, and performing primary heat preservation on the resistance heating furnace after preheating.
The ferrocene is placed in the middle of the quartz boat, the quartz boat is placed in the quartz tube, the outer wall of the quartz tube is wrapped with the transparent heat transfer layer, and the end of the quartz tube is provided with the heating belt.
One end of the raw material tube is inserted into the inlet end of the quartz tube, one end of the peristaltic pump is fixedly connected with the outer wall of the quartz tube, and the argon tube is inserted into the inlet end of the quartz tube, so that the preparation work before preparation is completed.
The raw material tank is opened, acetylene inside the raw material tank is added into the quartz tube through the raw material tube, the argon tank is opened, the flow controller on the surface of the argon tube controls the rate of argon flowing into the quartz tube, and acetylene and argon are subjected to preheating treatment through the heating belt.
Move the inside of resistance heating furnace through the one end of peristaltic pump with the quartz capsule, make the quartz boat of quartz capsule inside just be in laser emitter's transmission mouth department, install tail gas processing apparatus additional at the other end exit end of quartz capsule, open laser emitter and heat the quartz capsule, adjust temperature controller once more, make the inside temperature rise of resistance heating furnace, carry out the timing reaction, timing time 15 minutes.
Observing the ferrocene in the quartz boat inside the quartz tube through an observation electron microscope and checking the crystallization state of the multilayer carbon nano tube on the surface of the ferrocene.
And after the preparation is finished, carrying out secondary heat preservation on the quartz tube for 5 minutes, blowing air into the surface of the quartz tube and the inner wall of the resistance heating furnace through the air box after the heat preservation is finished, accelerating the cooling of the quartz tube and the resistance heating furnace, and taking out the multilayer carbon nano tubes in the quartz boat.
In comparison with example one, the distance between each layer of carbon nanotubes was changed from 0.3nm to 0.35 nm.
The invention has the beneficial effects that: according to the lithium ion battery cathode material and the preparation method thereof, through the arrangement of primary heat preservation and secondary heat preservation, carbon atoms in acetylene can be better separated out in the preparation process, the improvement of the yield and the quality of preparation is achieved, the arrangement of the laser emitter is adopted, the quartz tube is subjected to auxiliary heating through the laser emitter in the preparation process, the heating temperature of the resistance heating furnace is reduced, the preparation temperature is greatly reduced, the safety in the preparation process is improved, the carbon nano tube precipitated on the ferrocene surface in the quartz boat is observed through the observation electron microscope in the preparation process through the arrangement of the observation electron microscope, the observation effect is achieved, the real-time monitoring on the prepared carbon nano tube is achieved, and the purpose of rapid adjustment can be carried out according to different problems.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (8)
1. The preparation method of the lithium ion battery negative electrode material is characterized by comprising the following steps:
1) starting the resistance heating furnace, adjusting the temperature controller to be set to a proper preheating temperature to increase the temperature in the resistance heating furnace, preheating the interior of the resistance heating furnace, and performing primary heat preservation on the resistance heating furnace after preheating;
2) putting ferrocene into the middle part of a quartz boat, putting the quartz boat in the quartz tube, wrapping the outer wall of the quartz tube with a transparent heat transfer layer, and installing a heating belt at the end of the quartz tube;
3) inserting one end of a raw material tube at the inlet end of the quartz tube, fixedly connecting one end of a peristaltic pump with the outer wall of the quartz tube, and inserting an argon tube at the inlet end of the quartz tube to complete the preparation work before preparation;
4) starting a raw material tank, adding acetylene in the raw material tank into the quartz tube through a raw material tube, starting an argon tank, controlling the rate of argon flowing into the quartz tube through a flow controller on the surface of an argon tube, and preheating the acetylene and the argon through a heating belt;
5) moving one end of a quartz tube into the resistance heating furnace through a peristaltic pump to enable a quartz boat in the quartz tube to be just positioned at an emitting port of a laser emitter, additionally arranging a tail gas treatment device at the outlet end of the other end of the quartz tube, starting the laser emitter to heat the quartz tube, adjusting a temperature controller again to enable the temperature in the resistance heating furnace to rise, carrying out timing reaction, and timing for 15 minutes;
6) observing ferrocene inside a quartz boat inside the quartz tube through an observation electron microscope and checking the crystallization state of the multilayer carbon nano tube on the surface of the ferrocene;
7) and after the preparation is finished, carrying out secondary heat preservation on the quartz tube for 5 minutes, blowing air into the surface of the quartz tube and the inner wall of the resistance heating furnace through the air box after the heat preservation is finished, accelerating the cooling of the quartz tube and the resistance heating furnace, and taking out the multilayer carbon nano tubes in the quartz boat.
2. The method for preparing the lithium ion battery anode material as claimed in claim 1, wherein the preheating temperature in the step 1 is between 500-700 ℃, and the first heat preservation time of the resistance heating furnace is 3 minutes.
3. The method for preparing the lithium ion battery cathode material according to claim 1, wherein the flow rate of the peristaltic pump in the step 5 is 7.2ml/h, the distance between the laser emitter and the quartz tube is 2cm, and the maximum temperature of the resistance heating furnace is not more than 900 ℃.
4. The method for preparing the lithium ion battery anode material according to claim 1, wherein in the step 4, the flow rate of argon in the argon pipe is less than 10ml/s, the flow rate of acetylene is 15ml/s, the length of the heating belt is 10cm, and the argon pipe and the raw material pipe are inserted into one end of the heating belt.
5. The method for preparing the negative electrode material of the lithium ion battery according to claim 1, wherein the heating temperature of the heating zone in the step 4 is 170 ℃, and the heat transfer efficiency of the heating zone is 80%.
6. The method as claimed in claim 1, wherein the temperature of the second heat preservation in step 7 is between 300-350 ℃, the cooling time is 10 minutes, and the temperature of the surface of the quartz tube is less than 70 ℃ when the quartz tube is taken out.
7. A lithium ion battery negative electrode material is characterized in that: the lithium ion battery cathode material is prepared by the method for preparing the lithium ion battery cathode material according to any one of claims 1 to 6.
8. The negative electrode material of a lithium ion battery according to claim 7, wherein: the cathode material is composed of multi-layer carbon nanotubes, and the distance between each layer of the multi-layer carbon nanotubes is 0.34 nm.
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| US7651773B2 (en) * | 2005-03-25 | 2010-01-26 | Institut National De La Recherche Scientifique | Macroscopic assembly of nanometric filamentary structures and method of preparation thereof |
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