CN111250009B - Method for preparing lithium ion battery material by using microfluidic technology - Google Patents
Method for preparing lithium ion battery material by using microfluidic technology Download PDFInfo
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Abstract
The invention relates to a method for preparing a lithium ion battery material by utilizing a microfluidic technology, wherein the lithium ion battery material is prepared by coupling a microfluidic chip with one or two production methods of a hydrothermal method, a gel method, a template method and a vapor deposition method. The invention utilizes the microfluidic technology to prepare the raw materials in the lithium battery industry so as to obtain the nano materials with uniform size, excellent quality and various shapes, thereby expanding the application field of the microfluidic technology.
Description
Technical Field
The invention relates to the technical field of microfluidics, in particular to a method for preparing a lithium ion battery material 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 shape of the material in the lithium battery industry needs to be changed to adapt to the production and assembly of batteries with different shapes, and the research on the application of the microfluidic technology in the lithium battery industry does not appear at present.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a method for preparing a lithium ion battery material 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: the lithium ion battery material is prepared by coupling a micro-fluidic chip with one or two production methods of a hydrothermal method, a gel method, a template method and a vapor deposition method.
Further: the method for preparing the solid carbon rod in the lithium ion battery material by coupling the first micro-fluidic chip only comprising one continuous fluid channel with a hydrothermal method comprises the following steps:
step 1a: dissolving glucose in deionized water to prepare a solution A with solute content of 5-25%;
step 2a: injecting the solution A from the input port of the first dispersion fluid channel of the first microfluidic chip, and injecting the silicone oil from the input port of the first continuous fluid channel of the first microfluidic chip; so that a single-layer liquid drop is formed in the first liquid drop forming channel of the first micro-fluidic chip, and a single-layer rod-shaped liquid drop is formed in the first liquid drop shape control channel of the first micro-fluidic chip;
step 3a: heating the formed single-layer rod-shaped liquid drop by using an ultraviolet radiation source at the first liquid drop shape control channel so as to form colloidal particles;
step 4a: and sintering the colloidal particles at the temperature of 1000-1500 ℃ to obtain the solid carbon rod in the lithium ion battery material.
Further: the output port of the first dispersion fluid channel and the output port of the first continuous fluid channel meet at the input port of the first droplet formation channel; the output port of the first droplet forming channel is connected with the input port of the first droplet morphology control channel; the first droplet topography control channel has an inner diameter smaller than an inner diameter of the first droplet forming channel.
Further: the first dispersive fluid channel, the first continuous fluid channel and the first liquid drop forming channel are in a T-shaped structure, a Y-shaped structure, a flow focusing structure or a confocal structure.
Further: in step 4a, the colloidal particles are washed with a detergent before being sintered.
Further: the method for preparing the hollow carbon rod in the lithium ion battery material by coupling the second micro-fluidic chip comprising two continuous fluid channels with a hydrothermal method comprises the following steps:
step 1b: dissolving glucose in deionized water to prepare a solution A with solute content of 5-25%;
and step 2b: injecting petroleum ether from an input port of a second dispersed fluid channel of the second micro-fluidic chip, injecting the solution A from an input port of a second continuous fluid channel of the second micro-fluidic chip, and injecting silicone oil from an input port of a third continuous fluid channel of the second micro-fluidic chip; so that a single-layer droplet is formed in a second droplet forming channel of the second microfluidic chip, a double-layer droplet is formed in a third droplet forming channel of the second microfluidic chip, and a double-layer rod-shaped droplet is formed in a second droplet shape control channel of the second microfluidic chip;
and step 3b: heating the formed double-layer rod-shaped liquid drop by using an ultraviolet radiation source at the second liquid drop shape control channel so as to form colloidal particles;
and 4b: heating the colloidal particles at a temperature of 80-120 ℃ to remove oil phase substances in the colloidal particles;
and step 5b: and sintering the colloidal particles at the temperature of 1000-1500 ℃ to obtain the hollow carbon rod in the lithium ion battery material.
Further: the output of the second discrete fluidic channel and the output of the second continuous fluidic channel meet at the input of the second droplet-forming channel; the output of the third continuous fluidic channel and the output of the second droplet-forming channel meet at the input of the third droplet-forming channel; the output port of the third droplet-forming channel is connected with the input port of the second droplet morphology control channel; the inner diameter of the second droplet-forming passage and the inner diameter of the second droplet profile control passage are both smaller than the inner diameter of the third droplet-forming passage.
Further: the second dispersed fluid channel, the second continuous fluid channel and the second droplet forming channel are in a T-shaped structure, a Y-shaped structure, a flow focusing structure or a confocal structure; the second droplet-forming channel, the third continuous fluid channel, and the third droplet-forming channel are in a T-shaped structure, a Y-shaped structure, a flow-focusing structure, or a confocal structure.
Further: the second dispersion fluid channel, the second continuous fluid channel, the third continuous fluid channel, the second droplet-forming channel, the third droplet-forming channel, and the second droplet profile control channel each have an inner diameter in a range of 5 μm to 500 μm.
Further: the flow rate of the solution in the second dispersive fluid channel is 0.1-100 muL/h, the flow rates of the solutions in the second continuous fluid channel and the third continuous fluid channel are both 10-800 muL/h, and the flow rate of the solution in the third continuous fluid channel and the flow rate of the solution in the second continuous fluid channel are both greater than the flow rate of the solution in the second dispersive fluid channel.
The beneficial effects of the invention are: the raw materials in the lithium battery industry are prepared by utilizing the microfluidic technology so as to obtain the nano-materials with uniform size, excellent quality and various shapes, and the application field of the microfluidic technology is expanded.
Drawings
Fig. 1 is a perspective view of a first microfluidic chip of a flow focusing structure according to the present invention, which is used for preparing a solid carbon rod in a lithium ion battery material;
fig. 2 is a schematic diagram of a first microfluidic chip;
FIG. 3 is an SEM image of a solid carbon rod in a lithium ion battery material prepared by coupling a first microfluidic chip with a hydrothermal method;
FIG. 4 is a perspective view of a second microfluidic chip comprising two serially connected flow focusing structures according to the present invention for preparing a hollow carbon rod of a lithium ion battery material;
fig. 5 is a schematic diagram of a second microfluidic chip;
fig. 6 is a TEM image of a hollow carbon rod in a lithium ion battery material prepared by coupling a second microfluidic chip with a hydrothermal method.
In the figure: 1 is a first microfluidic chip, 11 is a first dispersive fluid channel, 12 is a first continuous fluid channel, 13 is a first droplet formation channel, 14 is a first droplet topography control channel, 2 is a second microfluidic chip, 21 is a second dispersive fluid channel, 22 is a second continuous fluid channel, 23 is a third continuous fluid channel, 24 is a second droplet formation channel, 25 is a third droplet formation channel, and 26 is a second droplet topography control 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.
The lithium ion battery material is prepared by coupling a micro-fluidic chip with one or two production methods 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.
Wherein: the method for preparing the lithium ion battery material by utilizing the microfluidic technology can be used for preparing the hollow nanosphere anode material of the lithium ion battery or the carbon-coated electrode material of the lithium ion battery.
As shown in fig. 1 to 3, in the first embodiment, a method for preparing a solid carbon rod in a lithium ion battery material by coupling a first microfluidic chip 1 including only one continuous fluid channel with a hydrothermal method includes the following steps:
step 1a: dissolving glucose in deionized water to prepare a solution A with the solute content of 10%; the solute content can be 5% -25%.
Step 2a: injecting the solution A from the input port of the first dispersed fluid channel 11 of the first micro-fluidic chip 1 at a flow rate of 20 muL/h and injecting the silicone oil from the input port of the first continuous fluid channel 12 of the first micro-fluidic chip 1 at a flow rate of 100 muL/h by using a syringe pump respectively; so that a single-layer droplet is formed in the first droplet forming channel 13 of the first microfluidic chip 1, and a single-layer rod-shaped droplet is formed in the first droplet morphology control channel 14 of the first microfluidic chip 1;
wherein the output of the first dispersive fluid channel 11 and the output of the first continuous fluid channel 12 meet at the input of the first droplet formation channel 13; the output port of the first droplet formation channel 13 is connected with the input port of the first droplet morphology control channel 14; the inner diameter of the first droplet topography control channel 14 is smaller than the inner diameter of the first droplet forming channel 13.
The flow rate of the solution in the first dispersion fluid channel 11 can be between 0.1 muL/h and 100 muL/h, and the flow rate of the solution in the first continuous fluid channel 12 can be between 10 muL/h and 800 muL/h, but the flow rate of the solution in the first continuous fluid channel 12 is required to be larger than that of the solution in the first dispersion fluid channel 11.
Wherein the inner diameters of the first dispersion fluid channel 11, the first continuous fluid channel 12, the first droplet formation channel 13 and the first droplet morphology control channel 14 are all 5-500 μm; the inner diameter of the first dispersion fluid channel 11, the inner diameter of the first continuous fluid channel 12 and the inner diameter of the first droplet forming channel 13 are preferably equal. In the present embodiment, the first dispersion fluid channel 11, the first continuous fluid channel 12, and the first droplet forming channel 13 each have an inner diameter of 70 μm, and the first droplet profile controlling channel 14 has an inner diameter of 40 μm.
The first dispersion fluid channel 11, the first continuous fluid channel 12 and the first 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 3a: heating the formed single-layer rod-shaped liquid drop by using an ultraviolet radiation source at the first liquid drop morphology control channel 14 so as to form colloidal particles in a short time and collect the colloidal particles;
step 4a: and sintering the colloidal particles at 1500 ℃ to obtain the solid carbon rod in the lithium ion battery material. 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, alcohol, etc.
Wherein, the first microfluidic chip 1 is made of transparent material so as to facilitate observation.
As shown in FIG. 3, the solid carbon rods in the lithium ion battery material prepared by the invention have uniform size and good dispersibility.
As shown in fig. 4 to 6, in the second embodiment, a method for preparing a hollow carbon rod in a lithium ion battery material by coupling a second microfluidic chip 2 including two continuous fluid channels with a hydrothermal method includes the following steps:
step 1b: dissolving glucose in deionized water to prepare a solution A with the solute content of 10%; the solute content can be 5% -25%.
And step 2b: respectively injecting petroleum ether from the input ports of the second dispersed fluid channels 21 of the second micro-fluidic chip 2 at a flow rate of 10 muL/h, injecting the solution A from the input ports of the second continuous fluid channels 22 of the second micro-fluidic chip 2 at a flow rate of 80 muL/h, and injecting silicone oil from the input ports of the third continuous fluid channels 23 of the second micro-fluidic chip 2 at a flow rate of 300 muL/h by using a syringe pump; so that a single-layer droplet is formed in the second droplet-forming channel 24 of the second microfluidic chip 2, a double-layer droplet is formed in the third droplet-forming channel 25 of the second microfluidic chip 2, and a double-layer rod-shaped droplet is formed in the second droplet shape control channel 26 of the second microfluidic chip 2;
wherein the output of the second discrete fluid passage 21 and the output of the second continuous fluid passage 22 meet at the input of the second droplet-forming passage 24; the output of the third continuous fluidic channel 23 and the output of the second drop forming channel 24 meet at the input of a third drop forming channel 25; the output port of the third droplet-forming passage 25 is connected to the input port of the second droplet profile-controlling passage 26; the inner diameter of the second droplet-forming passage 24 and the inner diameter of the second droplet profile control passage 26 are both smaller than the inner diameter of the third droplet-forming passage 25.
The flow rate of the solution in the second dispersion fluid channel 21 can be between 0.1 muL/h and 100 muL/h, the flow rate of the solution in the second continuous fluid channel 22 and the third continuous fluid channel 23 can be between 10 muL/h and 800 muL/h, and the flow rate of the solution in the third continuous fluid channel 23 and the flow rate of the solution in the second continuous fluid channel 22 are both larger than the flow rate of the solution in the second dispersion fluid channel 21.
Wherein the second dispersion fluid passage 21, the second continuous fluid passage 22, the third continuous fluid passage 23, the second droplet-forming passage 24, the third droplet-forming passage 25, and the second droplet profile-controlling passage 26 each have an inner diameter in the range of 5 μm to 500 μm; the inner diameter of the second dispersed fluid passage 21, the inner diameter of the second continuous fluid passage 22, and the inner diameter of the second droplet-forming passage 24 are preferably equal; the inner diameter of the third continuous fluid channel 23 and the inner diameter of the third droplet-forming channel 25 are preferably equal. In the present embodiment, the second dispersion fluid passage 21, the second continuous fluid passage 22, and the second droplet-forming passage 24 each have an inner diameter of 60 μm, the third continuous fluid passage 23 and the third droplet-forming passage 25 each have an inner diameter of 100 μm, and the second droplet-form control passage 26 has an inner diameter of 40 μm.
Wherein the second dispersed fluid channel 21, the second continuous fluid channel 22 and the second droplet-forming channel 24 are in a T-shaped structure, a Y-shaped structure, a flow focusing structure or a confocal structure; the second droplet-forming channel 24, the third continuous fluid channel 23 and the third droplet-forming channel 25 are in a T-shaped configuration, a Y-shaped configuration, a flow-focusing configuration or a confocal configuration. In this embodiment, two flow focusing structures connected in series are selected.
And step 3b: at the second droplet morphology control channel 26, the formed double-layer rod-shaped droplets are heated by an ultraviolet radiation source so as to form colloidal particles in a short time and collect the colloidal particles;
and 4b: heating the colloidal particles at a temperature of 100 ℃ to remove oil phase substances inside the colloidal particles; the temperature during heating can be between 80 ℃ and 120 ℃.
And step 5b: and sintering the colloidal particles at the temperature of 1500 ℃ to obtain the hollow carbon rod in the lithium ion battery material. The temperature during sintering can be between 1000 ℃ and 1500 ℃.
Wherein, the micro-fluidic chip is made of transparent materials so as to be convenient for observation.
As shown in FIG. 6, the hollow carbon rods in the lithium ion battery material prepared by the invention have 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 (6)
1. A method for preparing a lithium ion battery material by utilizing a microfluidic technology is characterized by comprising the following steps: the lithium ion battery material is prepared by coupling a micro-fluidic chip and a hydrothermal method, wherein the method for preparing the solid carbon rod in the lithium ion battery material by coupling the first micro-fluidic chip (1) only comprising one continuous fluid channel and the hydrothermal method comprises the following steps:
step 1a: dissolving glucose in deionized water to prepare a solution A with solute content of 5-25%;
step 2a: injecting a solution A from an input port of a first dispersed fluid channel (11) of a first microfluidic chip (1), and injecting silicone oil from an input port of a first continuous fluid channel (12) of the first microfluidic chip (1); so that a single-layer liquid drop is formed in the first liquid drop forming channel (13) of the first micro-fluidic chip (1), and a single-layer rod-shaped liquid drop is formed in the first liquid drop appearance control channel (14) of the first micro-fluidic chip (1);
step 3a: heating the formed single-layer rod-shaped liquid drop by using an ultraviolet radiation source at the first liquid drop morphology control channel (14) so as to form colloidal particles;
step 4a: sintering the colloidal particles at the temperature of 1000-1500 ℃ to obtain the solid carbon rod in the lithium ion battery material,
the method for preparing the hollow carbon rod in the lithium ion battery material by coupling the second micro-fluidic chip (2) comprising two continuous fluid channels with a hydrothermal method comprises the following steps:
step 1b: dissolving glucose in deionized water to prepare a solution A with solute content of 5-25%;
and step 2b: injecting petroleum ether from an input port of a second dispersed fluid channel (21) of the second microfluidic chip (2), injecting a solution A from an input port of a second continuous fluid channel (22) of the second microfluidic chip (2), and injecting silicone oil from an input port of a third continuous fluid channel (23) of the second microfluidic chip (2); so that a single-layer droplet is formed in the second droplet-forming channel (24) of the second microfluidic chip (2), a double-layer droplet is formed in the third droplet-forming channel (25) of the second microfluidic chip (2), and a double-layer rod-shaped droplet is formed in the second droplet profile control channel (26) of the second microfluidic chip (2);
and step 3b: heating the formed double-layer rod-shaped liquid drops at the second liquid drop shape control channel (26) by using an ultraviolet radiation source so as to form colloidal particles;
and 4b: heating the colloidal particles at a temperature of 80-120 ℃ to remove oil phase substances in the colloidal particles;
and step 5b: sintering the colloidal particles at the temperature of 1000-1500 ℃ to obtain the hollow carbon rod in the lithium ion battery material, wherein the output port of the first dispersion fluid channel (11) and the output port of the first continuous fluid channel (12) are intersected at the input port of the first liquid drop forming channel (13); the output port of the first droplet forming channel (13) is connected with the input port of the first droplet morphology control channel (14); the inner diameter of the first droplet topography control channel (14) is smaller than the inner diameter of the first droplet formation channel (13),
the output of the second discrete fluid passage (21) and the output of the second continuous fluid passage (22) meet at the input of the second droplet-forming passage (24); the output of the third continuous fluidic channel (23) and the output of the second droplet-forming channel (24) meet at the input of the third droplet-forming channel (25); the output port of the third droplet-forming passage (25) is connected to the input port of the second droplet profile control passage (26); the inner diameter of the second droplet-forming passage (24) and the inner diameter of the second droplet profile control passage (26) are both smaller than the inner diameter of the third droplet-forming passage (25).
2. The method of claim 1, wherein the method comprises the steps of: the first dispersion fluid channel (11), the first continuous fluid channel (12) and the first droplet formation channel (13) are in a T-shaped structure, a Y-shaped structure, a flow focusing structure or a confocal structure.
3. The method of claim 1, wherein the method comprises the steps of: in the step 4a, before sintering the colloidal particles, the colloidal particles are washed by using a detergent.
4. The method of claim 1, wherein the method comprises the steps of: the output of the second discrete fluid passage (21) and the output of the second continuous fluid passage (22) meet at the input of the second droplet-forming passage (24); the output of the third continuous fluidic channel (23) and the output of the second droplet-forming channel (24) meet at the input of the third droplet-forming channel (25); the output port of the third droplet-forming channel (25) is connected to the input port of the second droplet profile-controlling channel (26); the inner diameter of the second droplet-forming passage (24) and the inner diameter of the second droplet profile control passage (26) are both smaller than the inner diameter of the third droplet-forming passage (25).
5. The method of claim 1, wherein the method comprises the steps of: the second dispersion fluid channel (21), the second continuous fluid channel (22), the third continuous fluid channel (23), the second droplet-forming channel (24), the third droplet-forming channel (25), and the second droplet profile control channel (26) each have an inner diameter in the range of 5 μm to 500 μm.
6. The method of claim 1, wherein the method comprises the steps of: the flow rate of the solution in the second dispersion fluid channel (21) is 0.1-100 muL/h, the flow rates of the solutions in the second continuous fluid channel (22) and the third continuous fluid channel (23) are both 10-800 muL/h, and the flow rate of the solution in the third continuous fluid channel (23) and the flow rate of the solution in the second continuous fluid channel (22) are both greater than the flow rate of the solution in the second dispersion fluid channel (21).
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