CN108511693B - Method for manufacturing silicon cathode of lithium ion battery based on laser melt injection technology - Google Patents
Method for manufacturing silicon cathode of lithium ion battery based on laser melt injection technology Download PDFInfo
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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
- H01M4/1395—Processes of manufacture of electrodes based on metals, Si or alloys
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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
- H01M4/04—Processes of manufacture in general
- H01M4/0483—Processes of manufacture in general by methods including the handling of a melt
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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
- H01M4/134—Electrodes based on metals, Si or alloys
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- 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 discloses a method for manufacturing a silicon cathode of a lithium ion battery based on a laser melt injection technology. The lithium ion battery silicon electrode manufactured by the method can effectively realize metallurgical bonding of active material silicon and a nickel-based current collector, reduces the volume change and current collector falling of silicon particles in the lithium extraction and insertion process, and exerts the advantages of laser manufacturing to realize rapid large-area preparation of the silicon electrode at normal temperature, and is far superior to the harsh high-temperature environment, time consumption, possibility of generation of toxic gas and the like required by the traditional CVD and other methods. Meanwhile, the electrode prepared by the invention does not use a binder and a conductive agent.
Description
Technical Field
The invention relates to the technical field of laser manufacturing of lithium ion battery silicon electrodes, in particular to a method for manufacturing a lithium ion battery silicon cathode based on a laser melt injection technology.
Background
Lithium Ion Batteries (LIBs) have the advantages of high energy density, no memory effect, high capacity performance and the like, and since the advent, they rapidly replace traditional secondary Batteries such as nickel-cadmium, nickel-hydrogen, lead-acid and the like. The lithium ion battery consists of an anode, electrolyte, a high-molecular diaphragm and a cathode. At present, most of commercial lithium ion batteries use graphite cathodes, the theoretical capacity of which is only 372mA.h/g, and the ever-increasing demand cannot be met.
The silicon material has high theoretical specific capacity (4200mA · h/g) and is an ideal negative electrode material for replacing graphite. At present, a coating method is adopted, namely, a conductive agent, a binder and silicon particles are mixed and directly coated on the surface of a current collector to realize the structurization of a silicon negative electrode. By adopting a coating method, the binding force between the silicon particles and the current collector is weaker, and the pulverization and the crushing of the silicon particles and the falling of the current collector are caused due to the repeated expansion and contraction of the volume of the silicon particles in repeated charge and discharge cycles, so that the capacity is quickly attenuated. Meanwhile, the addition of the conductive agent and the binder reduces the loading capacity of silicon particles, and hinders the practical application of the silicon electrode.
The metallurgical bonding between the silicon particles and the current collector can effectively solve the problem that the silicon particles fall off in the process of charging and discharging for many times. At present, the metallurgical bonding of silicon particles and a current collector can be realized by adopting a chemical vapor deposition method, a high-temperature calcination method and an ion sputtering method. However, both the chemical vapor deposition method and the high-temperature calcination method require relatively long heating, heat preservation and cooling times, rapid large-area preparation cannot be realized, and the preparation conditions are harsh. The ion sputtering method is slow in speed and low in efficiency.
Regarding the selection of the current collector, the current collector used by the traditional lithium ion negative electrode material is basically a copper current collector, although the melting point (1083 ℃) of copper is lower than that (1414 ℃) of silicon, which is an ideal choice for laser melting, the thermal conductivity of copper (397 w/m · k at 20 ℃) is too high, and the laser reflectivity of copper to optical fiber is extremely large, so that a relatively proper laser melting bath tailing is not easy to generate. The thermal conductivity of the nickel-based material (90.7 w/m.k at 20 ℃) is suitable for laser melt injection to produce a suitable melt pool tail, but its melting point is 1455 ℃, so proper protection of the silicon particles by forming a silica (about 1600 ℃ to 1700 ℃) cladding on the silicon particles is required.
Disclosure of Invention
In view of the above, the invention provides a safe and efficient method for realizing metallurgical bonding between active particles of a lithium ion battery and a current collector, no harsh high-temperature equipment is used in the preparation process, the whole laser preparation process is carried out at room temperature, and the final electrode does not use a binder or a conductive agent, so that the light-weight, rapid and large-area manufacture of the electrode is realized. This is a clear advantage of laser fabrication over conventional fabrication.
In a first aspect of the present invention, there is provided a method for manufacturing a silicon negative electrode of a lithium ion battery based on a laser melt-injection technique, for forming a metallurgical bond between a powder material and a metal base material, wherein the melting point of the powder material is not lower than that of the metal base material, the method comprising the steps of:
step S1: pretreating the surface of the metal substrate;
step S2: providing a powder conveying device and an energy conveying device, and arranging the powder conveying device and the energy conveying device according to a preset position relation with the metal substrate;
step S3: the energy delivery device delivers energy to the metal substrate to form a melt pool on the surface of the metal substrate material while heating the powder material in the powder delivery device to a semi-molten state; the powder material in the semi-molten state collides with the tail of the molten pool in solidification to achieve metallurgical bonding;
step S4: multiple passes of overlapping are performed.
Further, the pretreatment in step S1 includes grinding, cleaning, and applying carbon powder on the surface of the metal substrate.
Further, the powder material in step S3 is pretreated to form an oxide coating to increase the melting point.
Further, the powder conveying device conveys the powder using a shielding gas.
Further, the energy delivery device comprises a laser generating device, a focusing device and a scanning driving device.
Further, the laser beam output by the energy conveying device and the powder feeding collision nozzle of the powder conveying device are arranged on two sides of the normal line, and the laser beam penetrates through the powder flow after being reflected.
Furthermore, the focusing device is a 300mm focusing mirror, the power of the laser output by the laser generating device is 3500W-5500W, the defocusing amount is 20 mm-40 mm or-40 mm-20 mm, and the scanning speed of the laser is 30 mm/s-70 mm/s; the amount of protective gas argon of the powder conveying device is 8L/min-25L/min; the included angle between the powder feeding collision nozzle and the normal direction is 0-45 degrees, and the included angle between the laser beam and the normal direction is 10-45 degrees.
Furthermore, the focusing device is a 300mm focusing mirror, the power of the laser output by the laser generating device is 900W-1800W, the defocusing amount is-10 mm-40 mm, and the scanning speed of the laser is 6 mm/s-15 mm/s; the amount of protective gas argon of the powder conveying device is 8L/min-25L/min; the included angle between the powder feeding collision nozzle and the normal direction is 0-45 degrees, and the included angle between the laser beam and the normal direction is 10-45 degrees.
Further, the powder is silicon particles, and the metal substrate is a nickel plate.
The invention provides a lithium ion battery electrode in another aspect, which comprises active particles, a conductive agent and a current collector, wherein the active particles and the current collector form metallurgical bonding, the active particles are powder materials, the current collector is a metal substrate, and the conductive agent is a deposited metal substrate material or graphite covered on the surface of the active particles.
In order to prevent the excessive melting of the reflected light to the silicon, the invention finishes the nickel plate treatment in step S1, and then uses a spin coater to coat a layer of thin carbon powder to enhance the absorption of the nickel to the fiber laser, thus greatly reducing the energy reflected to the silicon.
The focusing mirror with the long focal length is selected, because a wide welding line can be obtained in a thermal conduction mode, the focusing mirror with the long focal length has longer Rayleigh length, the change of the size of the light spot in a certain processing range is smaller than that of the focusing mirror with the short focal length, and the processing stability is facilitated.
In the aspect of laser parameter matching, a defocusing mode is used for realizing a nickel plate thermal conduction welding mode, the drawing of a molten pool trailing is realized at a higher speed, if the welding is carried out near a focus, a wider welding line cannot be obtained, and if the deep melting mode is realized, because silicon powder is too light, the injection of the silicon powder is not favorable, and the strong steam recoil pressure can prevent the silicon powder from being combined with nickel.
In the invention, silicon particles are placed in an open air atmosphere for 1-3 weeks in the treatment of the silicon particles, so that the silicon particles can form an oxidation coating, the surface melting point of the particles is increased, and the melting point of the silicon particles is far away from the melting point of nickel. If the silicon particles are not oxidized, although the temperature before the silicon particles are injected into a molten pool to be trailing is far lower than the melting point of nickel, the trailing of the molten pool is equivalent to the combination of an emergency cold source and high-temperature liquid nickel, the damage to silicon is large, and nickel-silicon intermetallic compounds which are not beneficial to a lithium battery are generated in the process. The silicon oxide can be used as an electrode of a lithium ion battery, but the capacity performance of the silicon oxide is inferior to that of the silicon, and the purity of the silicon can be protected after an oxidation coating is formed, so that the reaction with nickel is inhibited to a certain extent.
According to the invention, the carbon powder is coated on the metal substrate, so that the burning loss of the reflected laser to silicon is reduced, and the carbon powder serves as a carbon source to form graphite which is a cathode of a lithium ion battery for commercial utilization. When the silicon particles are trailing in a molten pool where nickel is impacted, nickel liquid is adhered to the particles, and graphite is formed by carbon powder under the catalysis of the nickel and attached to the silicon particles. Both enhancing the conductivity of the silicon particles and acting as an electrode. In the case of relatively high power and high speed, this graphite cannot be stored due to overburning of the laser.
Compared with the CVD, high-temperature sintering in a furnace, ion sputtering and other methods in the prior art, the method improves the processing efficiency and shortens the time, and the method is not carried out in a high-temperature environment, the whole process is carried out in a mild room-temperature environment, the prepared sample amount is greatly improved, and the prepared electrode does not need a binder or a conductive agent.
Drawings
The above and other objects, features and advantages of the present invention will become more apparent from the following description of the embodiments of the present invention with reference to the accompanying drawings, in which:
FIG. 1 is a schematic diagram of the invention for manufacturing a silicon cathode of a lithium ion battery based on a laser melt injection technology;
FIG. 2 is a schematic view of the observation of the trailing of the molten pool by high-speed camera shooting without adding silicon powder and only opening the shielding gas in the earlier stage of the embodiment of the invention;
FIG. 3 is a schematic view of an SEM of a sample obtained according to an embodiment of the invention;
FIG. 4 is a schematic view of SEM observation of a sample obtained in the second embodiment of the present invention.
Detailed Description
The present invention will be described below based on examples, but the present invention is not limited to only these examples. In the following detailed description of the present invention, certain specific details are set forth. It will be apparent to one skilled in the art that the present invention may be practiced without these specific details. Well-known methods, procedures, components and circuits have not been described in detail so as not to obscure the present invention.
Further, those of ordinary skill in the art will appreciate that the drawings provided herein are for illustrative purposes and are not necessarily drawn to scale.
Unless the context clearly requires otherwise, throughout the description and the claims, the words "comprise", "comprising", and the like are to be construed in an inclusive sense as opposed to an exclusive or exhaustive sense; that is, what is meant is "including, but not limited to".
In the description of the present invention, it is to be understood that the terms "first," "second," and the like are used for descriptive purposes only and are not to be construed as indicating or implying relative importance. In addition, in the description of the present invention, "a plurality" means two or more unless otherwise specified.
Unless expressly stated or limited otherwise, the terms "mounted," "connected," "secured," and the like are intended to be inclusive and mean that, for example, they may be fixedly connected or detachably connected or integrally formed; can be mechanically or electrically connected; they may be directly connected or indirectly connected through intervening media, or they may be connected internally or in any other suitable relationship, unless expressly stated otherwise. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
The first embodiment is as follows: the method for preparing the silicon electrode of the lithium ion battery by the high-power optical fiber laser melt injection method is carried out according to the following steps:
the method comprises the following steps: polishing a metal substrate nickel plate to be rough by using abrasive paper, cleaning the surface of the nickel plate by using acetone, and fixing the nickel plate on a workbench by using a clamp;
step two: installing a laser processing head focusing lens, a powder feeding touch nozzle and other devices, and setting welding process parameters:
a 300mm focusing mirror is used, the power of laser is set to be 3500W-5500W, the defocusing amount is 20 mm-40 mm or-40 mm-20 mm, the scanning speed of the laser is 30 mm/s-70 mm/s, the argon amount of powder feeding protective gas is 8L/min-25L/min, silicon powder is brought in by the protective gas, the included angle between a powder feeding collision nozzle and the normal direction is 0-45 degrees, the included angle between a laser beam and the normal direction is 10-45 degrees, and the laser beam and the powder feeding nozzle are separated at two sides of the normal, as shown in figure 1;
step three: feeding silicon particles of mixed shielding gas to a tailing position of a molten pool by using a powder feeding head, carrying out laser process parameters in the step two, wherein part of front-blown shielding gas can protect the molten pool formed by a nickel plate under irradiation of a front laser beam, reflecting the laser beam to pass through a powder flow to heat the silicon particles to a semi-molten state, and leading the silicon particles in the semi-molten state dragged by the shielding gas to form complete inelastic collision with the tailing of the molten pool of the nickel plate in solidification so as to achieve metallurgical bonding;
step four: carrying out multi-pass lapping;
step five: the final laser-infused samples were assembled into half-cells using wire-cut into 8mm diameter disks for electrochemical performance testing.
The second embodiment is as follows: the present embodiment differs from the first embodiment in that: in the first step, a spin coater is additionally used to coat carbon powder after the nickel plate is processed, and the rest is the same as that in the first embodiment.
The third concrete implementation mode: the present embodiment differs from the second embodiment in that: and step three, placing the silicon powder in the air for 1-3 weeks for pretreatment to form an oxide coating. The other embodiments are the same as the second embodiment.
The fourth concrete implementation mode: the present embodiment differs from the first embodiment in that: the technological parameters of the second step are as follows:
a300 mm focusing lens is used, the power of laser is set to be 900W-1800W, the defocusing amount is-10 mm-40 mm, the scanning speed of the laser is 6 mm/s-15 mm/s, the argon amount of powder feeding protective gas is 8L/min-25L/min, silicon powder is brought in through the protective gas, the included angle alpha between a powder feeding collision nozzle and the normal direction is 0-45 degrees, the included angle beta between a laser beam and the normal direction is 10-45 degrees, and the laser beam and the powder feeding nozzle are separated at two sides of the normal, as shown in figure 1. The other embodiments are the same as the first embodiment.
The fifth concrete implementation mode: the present embodiment differs from the fourth embodiment in that: and in the step one, carbon powder is additionally coated by using a spin coater after the nickel plate is treated. The other embodiments are the same as the fourth embodiment.
The sixth specific implementation mode: the present embodiment differs from the fifth embodiment in that: and step three, placing the silicon powder in the air for 1-3 weeks for pretreatment to form an oxide coating. The other embodiments are the same as the fifth embodiment.
In order to prevent the excessive melting of the reflected light to the silicon, the nickel plate is processed in the first step, and a spin coater is used for coating a layer of thin carbon powder to enhance the absorption of the nickel to the fiber laser, so that the energy reflected to the silicon is greatly reduced.
The focusing lens with the long focal length is selected, so that a wide welding seam is hoped to be obtained in a thermal conduction mode, the focusing lens with the long focal length has a longer Rayleigh length, the change of the size of the light spot in a certain processing range is smaller than that of the focusing lens with the short focal length, and the processing stability is facilitated.
In the aspect of laser parameter matching, a defocusing mode is used for realizing a nickel plate thermal conduction welding mode, the drawing of a molten pool trailing is realized at a higher speed, if the welding is carried out near a focus, a wider welding line cannot be obtained, and if the deep melting mode is realized, because silicon powder is too light, the injection of the silicon powder is not favorable, and the strong steam recoil pressure can prevent the silicon powder from being combined with nickel.
In the invention, silicon particles are placed in an open air atmosphere for 1-3 weeks in the treatment of the silicon particles, so that the silicon particles can form an oxidation coating, the surface melting point of the particles is increased, and the melting point of the silicon particles is far away from the melting point of nickel. If the silicon particles are not oxidized, although the temperature before the silicon particles are injected into a molten pool to be trailing is far lower than the melting point of nickel, the trailing of the molten pool is equivalent to the combination of an emergency cold source and high-temperature liquid nickel, the damage to silicon is large, and nickel-silicon intermetallic compounds which are not beneficial to a lithium battery are generated in the process. The silicon oxide can be used as an electrode of a lithium ion battery, but the capacity performance of the silicon oxide is inferior to that of the silicon, and the purity of the silicon can be protected after an oxidation coating is formed, so that the reaction with nickel is inhibited to a certain extent.
The first embodiment is as follows:
the process for preparing the lithium ion silicon electrode by laser melt injection comprises the following steps:
grinding a 50mm multiplied by 5mm nickel plate by using 400-mesh sand paper, cleaning the nickel plate by using acetone, uniformly coating 30s of carbon powder suspension added with alcohol by using a spin coater at 150r/min, airing and carrying out laser melt injection.
Laser parameters:
a300 mm focusing lens is used, the power of laser is set to be 4500W, the defocusing amount is-30 mm, the scanning speed of the laser is 50mm/s, the argon amount of powder feeding protective gas is 12L/min, silicon powder is brought in through the protective gas, the included angle alpha between a powder feeding collision nozzle and the normal direction is 15 degrees, the included angle beta between a laser beam and the normal direction is 30 degrees, and the laser beam and the powder feeding nozzle are separated at two sides of the normal. The tailing of the molten pool observed by high-speed camera shooting without adding silicon powder is shown in figure 2, and the SEM picture of the sample obtained by adding silicon powder is shown in figure 3.
Example two:
the method for preparing the silicon electrode with the carbon coating in the large area is fast, and needs to be carried out at low power and low speed.
The carbon-coated silicon electrode differs from the previous solution most in laser parameters, using the same focusing mirror, at a relatively low power and low speed.
The process for preparing the carbon-coated lithium ion silicon electrode by laser melt injection comprises the following steps:
grinding a 50mm multiplied by 5mm nickel plate by using 400-mesh sand paper, cleaning the nickel plate by using acetone, uniformly coating 30s of carbon powder suspension added with alcohol by using a spin coater at 150r/min, airing and carrying out laser melt injection.
Laser parameters:
a300 mm focusing lens is used, the power of laser is set to be 950W, the defocusing amount is-40 mm, the scanning speed of the laser is 10mm/s, the argon amount of powder feeding protective gas is 18L/min, silicon powder is brought in through the protective gas Ar, the included angle alpha between a powder feeding collision nozzle and the normal direction is 5 degrees, the included angle beta between a laser beam and the normal direction is 40 degrees, the laser beam and the powder feeding nozzle are separated at two sides of the normal, and the obtained SEM picture of a sample is shown in figure 4.
In both of the above examples, the silicon particles are considered to be fed onto the molten pool tail because the silicon particles fed onto the molten pool are vaporized due to the intense laser beam irradiation. The silicon particles sent to the tail of the molten pool are far less damaged by high temperature.
In both examples, the silicon particles of the active material and the nickel substrate are bonded atomically to a metallurgical grade. For the former embodiment, the deposited nickel vapor, which was silicon surface coated, acts as a conductive agent, and for the other embodiment, graphite acts as a conductive agent.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (4)
1. A method for manufacturing a silicon negative electrode of a lithium ion battery based on a laser melt-injection technique, for forming a metallurgical bond between a powder material and a metal base material, the melting point of the powder material being not lower than the melting point of the metal base material, the method comprising the steps of:
step S1: pretreating the surface of the metal substrate;
step S2: providing a powder conveying device and an energy conveying device, and arranging the powder conveying device and the energy conveying device according to a preset position relation with the metal substrate; the laser beam output by the energy conveying device and the powder conveying nozzle of the powder conveying device are separated on two sides of a normal line, and the laser beam penetrates through the powder flow after being reflected;
step S3: the energy delivery device delivers energy to the metal substrate to form a melt pool on the surface of the metal substrate material while heating the powder material in the powder delivery device to a semi-molten state; the powder material in the semi-molten state collides with the tail of the molten pool in solidification to achieve metallurgical bonding;
step S4: carrying out multi-pass lapping;
the powder is silicon particles, and the metal substrate is a nickel plate; the energy transmission device comprises a laser generating device, a focusing device and a scanning driving device;
in the step S3, the powder conveying device sends silicon particles of mixed shielding gas to a trailing position of the molten pool, a part of the forward-blown shielding gas protects the molten pool formed by the nickel plate under the irradiation of the forward laser beam, the reflected laser beam passes through the powder flow to heat the silicon particles to a semi-molten state, and the silicon particles in the semi-molten state dragged by the shielding gas and the trailing position of the molten pool of the nickel plate being solidified form complete inelastic collision to achieve metallurgical bonding;
the focusing device is a 300mm focusing mirror, the power of the laser output by the laser generating device is 3500W-5500W, the defocusing amount is 20 mm-40 mm or-40 mm-20 mm, and the scanning speed of the laser is 30 mm/s-70 mm/s; the Ar gas amount of the protective gas of the powder conveying device is 8L/min-25L/min; the included angle between the powder feeding nozzle and the normal direction is 0-45 degrees, and the included angle between the laser beam and the normal direction is 10-45 degrees; or
The focusing device is a 300mm focusing lens, the power of the laser output by the laser generating device is 900W-1800W, the defocusing amount is-10 mm-40 mm, and the scanning speed of the laser is 6 mm/s-15 mm/s; the Ar gas amount of the protective gas of the powder conveying device is 8L/min-25L/min; the included angle between the powder feeding nozzle and the normal direction is 0-45 degrees, and the included angle between the laser beam and the normal direction is 10-45 degrees.
2. The method as claimed in claim 1, wherein the pretreatment in step S1 includes grinding, cleaning, and applying carbon powder on the surface of the metal substrate.
3. The method according to claim 1 or 2, wherein the powder material in step S3 is pre-treated to form an oxide coating to increase the melting point.
4. A lithium ion battery electrode comprising active particles, a conductive agent, and a current collector, wherein the lithium ion battery electrode is a silicon negative electrode manufactured according to the method of any one of claims 1-3.
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| CN105967740A (en) * | 2016-05-02 | 2016-09-28 | 北京工业大学 | Method for preparing micro-nano structured block silicon material through compounding laser cladding and chemical dealloying |
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| CN103313937A (en) * | 2010-09-03 | 2013-09-18 | 奈克松有限公司 | Porous electroactive material |
| CN105967740A (en) * | 2016-05-02 | 2016-09-28 | 北京工业大学 | Method for preparing micro-nano structured block silicon material through compounding laser cladding and chemical dealloying |
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| 赵海波，黄婷，肖荣诗.锂离子电池硅电极激光熔注工艺研究.《第17届全国特种加工学术会议论文集（摘要）》.2017,第166页. * |
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