CN111261849A - Method for preparing solid spherical material for negative electrode of lithium ion battery by using microfluidic technology - Google Patents
Method for preparing solid spherical material for negative electrode of lithium ion battery by using microfluidic technology Download PDFInfo
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- CN111261849A CN111261849A CN201811464397.4A CN201811464397A CN111261849A CN 111261849 A CN111261849 A CN 111261849A CN 201811464397 A CN201811464397 A CN 201811464397A CN 111261849 A CN111261849 A CN 111261849A
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0093—Microreactors, e.g. miniaturised or microfabricated reactors
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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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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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
Abstract
The invention relates to a method for preparing a solid spherical material for a cathode of a lithium ion battery by utilizing a microfluidic technology, which comprises the following steps: step 1: dissolving glucose in deionized water to prepare a solution A; step 2: injecting the solution A from an input port of a dispersed fluid channel of the microfluidic chip, and injecting silicone oil from an input port of a continuous fluid channel of the microfluidic chip; so that the droplet forming channel of the microfluidic chip forms spherical droplets; and step 3: heating the formed spherical liquid drops by using an ultraviolet radiation source at the liquid drop forming channel so as to form colloidal particles; and 4, step 4: and sintering the colloidal particles at the temperature of 1000-1500 ℃ to obtain the solid spherical material of the lithium ion battery cathode. The invention utilizes the microfluidic technology to prepare the raw materials in the lithium ion battery industry, so that the prepared solid spherical material of the lithium ion battery cathode has uniform size and good dispersibility.
Description
Technical Field
The invention relates to the technical field of microfluidics, in particular to a method for preparing a solid spherical material for a cathode of a lithium ion battery by utilizing the microfluidics technology.
Background
Microfluidic chip (microfluidcchip) refers to a technology for integrating basic operation units of a conventional laboratory into a chip of several square centimeters (or even smaller), and forming a network by microchannels, thereby controlling fluid to penetrate through the whole system to replace various functions of the conventional laboratory. The microfluidic technology has the following obvious advantages: the system is closed, the reagent consumption is low, the reaction condition is stable, and the control is easy; the liquid drop generation operation is simple, external acting force is not required to be introduced, and particles with target sizes can be synthesized in one step; the liquid drops have good monodispersity and uniform size.
The preparation process of the material in the lithium ion battery industry has strong requirements on the uniformity and regularity of the negative electrode material, and no research related to the application of the microfluidic technology in the lithium battery industry exists at present.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for preparing a solid spherical material of a lithium ion battery cathode by utilizing a microfluidic technology so as to overcome the defects in the prior art.
The technical scheme for solving the technical problems is as follows: a method for preparing a solid spherical material for a negative electrode of a lithium ion battery by utilizing a microfluidic technology comprises the following steps:
step 1: dissolving glucose in deionized water to prepare a solution A with solute content of 5-25%;
step 2: injecting the solution A from an input port of a dispersed fluid channel of the microfluidic chip, and injecting silicone oil from an input port of a continuous fluid channel of the microfluidic chip; so that the droplet forming channel of the microfluidic chip forms spherical droplets;
and step 3: heating the formed spherical liquid drops by using an ultraviolet radiation source at the liquid drop forming channel so as to form colloidal particles;
and 4, step 4: and sintering the colloidal particles at the temperature of 1000-1500 ℃ to obtain the solid spherical material of the lithium ion battery cathode.
Further: the output of the dispersive fluidic channel and the output of the continuous fluidic channel meet at the input of the droplet-forming channel.
Further: the dispersive fluid channel, the continuous fluid channel and the droplet forming channel are in a T-shaped structure, a Y-shaped structure, a flow focusing structure or a confocal structure.
Further: the internal diameters of the dispersive fluidic channel, the continuous fluidic channel, and the droplet-forming channel each range from 10 μm to 200 μm.
Further: the internal diameters of the dispersion fluid channel, the continuous fluid channel, and the droplet-forming channel are equal.
Further: the internal diameters of the dispersion flow channel, the continuous flow channel and the droplet-forming channel were all 70 μm.
Further: the flow rate of the solution in the dispersion flow channel is 0.1-100 muL/h, the flow rate of the solution in the continuous flow channel is 10-500 muL/h, and the flow rate of the solution in the continuous flow channel is greater than the flow rate of the solution in the dispersion flow channel.
Further: the flow rate of the solution in the dispersion flow channel was 20. mu.L/h, and the flow rate of the solution in the continuous flow channel was 100. mu.L/h.
Further: in step 4, before the colloidal particles are sintered, the colloidal particles need to be washed by a detergent.
Further: the detergent is water or hydroxyl-containing polymer solution.
The invention has the beneficial effects that: the raw materials in the lithium ion battery industry are prepared by utilizing the microfluidic technology, so that the prepared solid spherical material for the negative electrode of the lithium ion battery has uniform size and good dispersibility.
Drawings
FIG. 1 is a perspective view of a microfluidic chip selected for preparing a solid spherical material for a negative electrode of a lithium ion battery according to the present invention;
FIG. 2 is a schematic diagram of a microfluidic chip;
FIG. 3 is an SEM image of a solid spherical material of a negative electrode of a lithium ion battery prepared by the invention;
FIG. 4 is an XRD pattern of the solid spherical material for the negative electrode of the lithium ion battery prepared by the invention.
In the figure: 1 is a microfluidic chip, 11 is a dispersed fluid channel, 12 is a continuous fluid channel, and 13 is a droplet forming channel.
Detailed Description
The principles and features of this invention are described below in conjunction with the following drawings, which are set forth by way of illustration only and are not intended to limit the scope of the invention.
A method for preparing a solid spherical material for a lithium ion battery cathode by utilizing a microfluidic technology is prepared by coupling a microfluidic chip with one or two of a hydrothermal method, a gel method, a template method and a vapor deposition method.
In the hydrothermal method, the carbon source can be petroleum asphalt, coal asphalt, sucrose, glucose, starch, cellulose, sodium citrate, phenolic resin, epoxy resin and other organic carbon sources.
In the gel method, the gel can be organic matters such as resorcinol and formaldehyde which can be subjected to dehydration or alcohol loss condensation polymerization so as to synthesize carbon sources such as phenolic resin and epoxy resin.
In the template method, the template agent can be a low-boiling-point water-insoluble organic matter or a gas-phase organic matter.
In the vapor deposition method, the continuous phase is an organic gas.
The method for preparing the solid spherical material for the cathode of the lithium ion battery by coupling the microfluidic chip 1 with a hydrothermal method comprises the following steps:
step 1: dissolving glucose in deionized water to prepare a solution A with the solute content of 10%; the solute content can be 5% -25%.
Step 2 a: injecting the solution A from the input port of the dispersion fluid channel 11 of the micro-fluidic chip 1 at the flow rate of 20 muL/h and injecting the silicone oil from the input port of the continuous fluid channel 12 of the micro-fluidic chip 1 at the flow rate of 100 muL/h by using a syringe pump respectively; so that spherical liquid drops are formed in the liquid drop forming channel 13 of the microfluidic chip 1;
wherein the output of the dispersive fluid channel 11 and the output of the continuous fluid channel 12 meet at the input of the droplet-forming channel 13.
Wherein, the flow rate of the solution in the dispersion fluid channel 11 can be between 0.1 muL/h and 100 muL/h, and the flow rate of the solution in the continuous fluid channel 12 can be between 10 muL/h and 500 muL/h, but the flow rate of the solution in the continuous fluid channel 12 is ensured to be larger than that of the solution in the dispersion fluid channel 11.
Wherein the dispersion flow channel 11, the continuous flow channel 12 and the droplet-forming channel 13 each have an inner diameter in the range of 10 μm to 200 μm; the inner diameter of the dispersion flow channel 11, the inner diameter of the continuous flow channel 12, and the inner diameter of the droplet-forming channel 13 are preferably equal. In the present embodiment, the dispersion flow channel 11, the continuous flow channel 12, and the droplet-forming channel 13 each have an inner diameter of 70 μm.
The dispersive fluid channel 11, the continuous fluid channel 12 and the droplet forming channel 13 are in a T-shaped structure, a Y-shaped structure, a flow focusing structure or a confocal structure. In this embodiment, a flow focusing structure is selected.
Step 3 a: heating the formed spherical liquid drops by using an ultraviolet radiation source at the first liquid drop shape control channel 14 so as to form colloidal particles in a short time and collecting the colloidal particles;
step 4 a: and sintering the colloidal particles at 1500 ℃ to obtain the solid spherical material of the lithium ion battery cathode. The temperature during sintering can be between 1000 ℃ and 1500 ℃.
Wherein, before sintering the colloidal particles, the colloidal particles need to be washed by a detergent. The detergent can be water or hydroxyl-containing polymer (alcohol) solution.
The microfluidic chip 1 is made of a transparent material, such as a transparent glass material, so as to facilitate observation.
As shown in fig. 3, the raw materials in the lithium ion battery industry are prepared by using the microfluidic technology, so that the prepared solid spherical material for the negative electrode of the lithium ion battery has uniform size and good dispersibility.
The present invention is not limited to the above preferred embodiments, and any modifications, equivalent replacements, improvements, etc. within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A method for preparing a solid spherical material for a cathode of a lithium ion battery by utilizing a microfluidic technology is characterized by comprising the following steps of: the method comprises the following steps:
step 1: dissolving glucose in deionized water to prepare a solution A with solute content of 5-25%;
step 2: injecting the solution A from an input port of a dispersion fluid channel (11) of the microfluidic chip (1), and injecting silicone oil from an input port of a continuous fluid channel (12) of the microfluidic chip (1); so as to form spherical liquid drops in the liquid drop forming channel (13) of the microfluidic chip (1);
and step 3: at the droplet forming channel (13), heating the formed spherical droplets with an ultraviolet radiation source to form colloidal particles;
and 4, step 4: and sintering the colloidal particles at the temperature of 1000-1500 ℃ to obtain the solid spherical material of the lithium ion battery cathode.
2. The method for preparing the solid spherical material for the negative electrode of the lithium ion battery by using the microfluidic technology as claimed in claim 1, wherein the method comprises the following steps: the outlet of the dispersion flow channel (11) and the outlet of the continuous flow channel (12) meet at the inlet of the droplet formation channel (13).
3. The method for preparing the solid spherical material for the negative electrode of the lithium ion battery by using the microfluidic technology as claimed in claim 1, wherein the method comprises the following steps: the dispersive fluid channel (11), the continuous fluid channel (12) and the droplet forming channel (13) are in a T-shaped structure, a Y-shaped structure, a flow focusing structure or a confocal structure.
4. The method for preparing the solid spherical material for the negative electrode of the lithium ion battery by using the microfluidic technology as claimed in claim 1, wherein the method comprises the following steps: the internal diameters of the dispersion fluid channel (11), the continuous fluid channel (12) and the droplet-forming channel (13) each range from 10 μm to 200 μm.
5. The method for preparing the solid spherical material for the negative electrode of the lithium ion battery by using the microfluidic technology as claimed in claim 4, wherein the method comprises the following steps: the dispersion fluid channel (11), the continuous fluid channel (12) and the droplet forming channel (13) have equal inner diameters.
6. The method for preparing the solid spherical material for the negative electrode of the lithium ion battery by using the microfluidic technology as claimed in claim 5, wherein the method comprises the following steps: the dispersion flow channel (11), the continuous flow channel (12) and the droplet forming channel (13) all have an internal diameter of 70 μm.
7. The method for preparing the solid spherical material for the negative electrode of the lithium ion battery by using the microfluidic technology as claimed in claim 1, wherein the method comprises the following steps: the flow rate of the solution in the dispersion fluid channel (11) is 0.1-100 mu L/h, the flow rate of the solution in the continuous fluid channel (12) is 10-500 mu L/h, and the flow rate of the solution in the continuous fluid channel (12) is greater than the flow rate of the solution in the dispersion fluid channel (11).
8. The method for preparing the solid spherical material for the negative electrode of the lithium ion battery by using the microfluidic technology as claimed in claim 7, wherein the method comprises the following steps: the flow rate of the solution in the dispersion fluid channel (11) is 20 mu L/h, and the flow rate of the solution in the continuous fluid channel (12) is 100 mu L/h.
9. The method for preparing the solid spherical material for the negative electrode of the lithium ion battery by using the microfluidic technology as claimed in claim 1, wherein the method comprises the following steps: in the step 4, before the colloidal particles are sintered, the colloidal particles need to be washed by using a detergent.
10. The method for preparing the solid spherical material for the negative electrode of the lithium ion battery by using the microfluidic technology as claimed in claim 9, wherein the method comprises the following steps: the detergent is water or hydroxyl-containing polymer solution.
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Citations (7)
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| CN102522545A (en) * | 2011-12-16 | 2012-06-27 | 北京工业大学 | Preparation method for lithium ion battery electrode material |
| KR20120080267A (en) * | 2011-01-07 | 2012-07-17 | 공주대학교 산학협력단 | Preparation of biodegradable microparticles with structural complexity on the surface and inside by using a microfluidic device |
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| CN106732213A (en) * | 2016-12-27 | 2017-05-31 | 中国科学院合肥物质科学研究院 | A kind of golden nanometer particle/hydrogel composite material and its preparation method and application |
| CN107497378A (en) * | 2017-10-09 | 2017-12-22 | 南京慧联生物科技有限公司 | The method that one-step method prepares the polyvinyl alcohol/silicon dioxide complex microsphere of core shell structure |
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2018
- 2018-12-03 CN CN201811464397.4A patent/CN111261849B/en active Active
Patent Citations (7)
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| KR20120080267A (en) * | 2011-01-07 | 2012-07-17 | 공주대학교 산학협력단 | Preparation of biodegradable microparticles with structural complexity on the surface and inside by using a microfluidic device |
| CN102522545A (en) * | 2011-12-16 | 2012-06-27 | 北京工业大学 | Preparation method for lithium ion battery electrode material |
| CN102881872A (en) * | 2012-09-11 | 2013-01-16 | 天津大学 | Method for synthesizing silicon oxide/carbon nanotube membranous lithium ion battery anode material by one step by utilizing chemical vapor deposition method |
| CN104779384A (en) * | 2015-03-19 | 2015-07-15 | 广西大学 | Preparation method of lithium ion battery negative electrode materials |
| CN104829850A (en) * | 2015-04-14 | 2015-08-12 | 华中科技大学 | Spherical calcium alginate gel micro-particle preparation method |
| CN106732213A (en) * | 2016-12-27 | 2017-05-31 | 中国科学院合肥物质科学研究院 | A kind of golden nanometer particle/hydrogel composite material and its preparation method and application |
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