CN112670453B - Silicon-based laminated anode material and preparation method and application thereof - Google Patents
Silicon-based laminated anode material and preparation method and application thereof Download PDFInfo
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- CN112670453B CN112670453B CN202011547244.3A CN202011547244A CN112670453B CN 112670453 B CN112670453 B CN 112670453B CN 202011547244 A CN202011547244 A CN 202011547244A CN 112670453 B CN112670453 B CN 112670453B
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Abstract
The invention discloses a silicon-based laminated negative electrode material and a preparation method and application thereof, and belongs to the technical field of negative electrode materials of lithium batteries. The preparation method comprises the following steps: depositing a graphite-like carbon layer on the substrate by adopting a magnetron sputtering technology; firstly, depositing nano Si or SiOx, and then depositing Li to obtain a silicon-based composite material; annealing to obtain nano silicon-based alloy particles, and performing graphite-like carbon deposition on the obtained nano silicon-based alloy particles to obtain a graphite-like carbon/silicon-based alloy particle layer; and repeating the cyclic deposition and annealing operation to obtain the silicon-based laminated negative electrode material. The invention adopts magnetron sputtering and annealing technology, effectively relieves the volume expansion of the silicon-based material in the process of lithium intercalation and deintercalation, realizes the refinement and pre-lithium of nano silicon particles, improves the first effect of the material obtained by the preparation method, and simplifies the preparation process of the negative pole piece. Therefore, the obtained silicon-based laminated negative electrode material is uniform in distribution and stable in structure, and can be used as a negative electrode plate of a lithium battery.
Description
Technical Field
The invention belongs to the technical field of lithium battery cathode materials, and relates to a silicon-based laminated cathode material, and a preparation method and application thereof.
Background
With the gradual increase of the requirements of new energy fields on the energy density of batteries, the improvement of the performance of the negative electrode material, which is the most effective means for improving the energy density of the batteries, is concerned by research institutions and various manufacturers. Compared with a graphite negative electrode, the silicon material has a capacity of 4200mAh/g, and the silicon monoxide also has a capacity of more than 2000mAh/g, and the source is wide, but the silicon material has large volume expansion in the lithium extraction process, and the volume expansion easily causes repeated growth of an SEI film generated by the negative electrode, so that the loss of active lithium is caused, and the capacity of the battery is reduced.
In order to solve this problem, silicon-based materials are usually subjected to nanocrystallization to inhibit expansion thereof, and the first effect of the nanomaterials is improved by pre-lithium through electrochemical, solid-phase doping and the like. Toxic and dangerous chemicals are generally used in the pre-lithiation process of the material, so that certain dangerousness exists and the environment is polluted. The problems of poor slurry stability and the like of the pre-lithium material in the later pulping and coating process exist.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a silicon-based laminated negative electrode material and a preparation method and application thereof, so that the problems of volume expansion in the process of lithium intercalation and deintercalation of the silicon-based negative electrode material and difficulty in considering both small particle size and dispersibility in the preparation of a nano silicon-based material are solved, and the first effect of the material is improved in a pre-lithium mode.
In order to achieve the purpose, the invention adopts the following technical scheme to realize the purpose:
the invention discloses a preparation method of a silicon-based laminated anode material, which comprises the following steps:
1) Depositing a graphite-like carbon layer on the substrate by adopting a magnetron sputtering technology;
2) Depositing nano Si or SiOx (wherein x is more than 0 and less than 2) on the graphite-like carbon layer obtained in the step 1), and then depositing Li to obtain a silicon-based composite material;
3) Annealing the silicon-based composite material obtained in the step 2) to obtain nano silicon-based alloy particles (Si/SiOx + Li particles), and performing graphite-like carbon deposition on the obtained nano silicon-based alloy particles to obtain graphite-like carbon/silicon-based alloy particle layers;
4) And repeating the step 2) to the step 3) to obtain the silicon-based laminated anode material.
Preferably, in step 1), the thickness of the obtained graphite-like carbon layer is 5-20 nm.
Preferably, in the step 2), the deposition thickness of the obtained nano Si or SiOx is 5-10 nm.
Preferably, in step 2), the deposition thickness of Li is 0-2 nm.
Preferably, in the step 2), the particle size of the nano silicon-based alloy particles is 5-10 nm.
Preferably, in the step 3), the thickness of the obtained graphite-like carbon/silicon-based alloy particle layer is 5-20 nm.
Preferably, in the step 4), the thickness of the obtained silicon-based anode laminated material is 500-1500 nm.
Preferably, in step 1), the substrate is a copper foil.
More preferably, the copper foil has a thickness of 4 to 8 μm.
Preferably, in the step 2), the deposition of the nano Si takes a silicon target as a target source, the silicon target is a P-type or N-type doped target, and direct current sputtering is adopted; siOx deposition is carried out by taking silicon monoxide as a target source and adopting intermediate frequency or radio frequency sputtering.
Preferably, in the step 2), the Li deposition is performed by using a direct current sputtering with a lithium target as a target source.
Preferably, in the step 3), the annealing treatment is pulse type rapid photo-thermal annealing, the annealing temperature is 400-500 ℃, the heating rate is 80-100 ℃/s, and the annealing time is 7-10 s.
The invention also discloses a silicon-based negative electrode laminated material prepared by the preparation method.
The invention also discloses an application of the silicon-based laminated negative electrode material as a negative electrode plate of a lithium battery.
Compared with the prior art, the invention has the following beneficial effects:
the invention discloses a preparation method of a silicon-based laminated cathode material, which adopts a roll-to-roll magnetron sputtering technology, introduces a Li source in the preparation process of a silicon-based material, realizes pre-lithium of the material, and improves the first effect and the cycle performance of the material; the lithium-silicon composite layer is treated by introducing rapid thermal annealing in the preparation process, so that the grain diameter of the nano silicon-based material (Si/SiOx) + Li is refined and well dispersed, and a graphite-like carbon/silicon-based alloy grain layer of the graphite-like carbon is coated and filled outside the formed lithium-silicon alloy grains by further sputtering graphite, so that the coating and filling of the nano Si/SiOx + Li grains are realized. Therefore, the preparation method solves the problems of volume expansion in the process of lithium intercalation and difficulty in considering both small particle size and dispersibility in the preparation of the nano silicon-based material, and effectively improves the first effect of the material. According to the preparation method, the silicon-based negative pole piece is prepared by adopting the magnetron sputtering technology, so that the preparation process is effectively simplified, and the pre-lithium is carried out in the preparation process of the pole piece, so that the volume expansion in the process of lithium release and insertion of the silicon-based material is effectively relieved, the first effect of the pole piece is improved, and the preparation process of the negative pole piece is simplified.
Furthermore, the preparation process of the pole piece adopts the sputtering of lithium and the rapid thermal annealing, thereby realizing the pre-lithium of the material and improving the first effect of the material.
The invention discloses a silicon-based laminated anode material prepared by the preparation method, which is characterized in that graphite-like carbon is coated and filled outside nano Si or SiOx and Li alloy particles, so that the nano silicon-based material is inhibited, and the conductivity of the material is improved. The pre-lithium of the pole piece is realized by a lithium sputtering mode, so that the first effect of the cathode material is improved. The obtained silicon-based laminated negative electrode material has small particle size, good dispersion and oxidation resistance, and the graphite is coated and filled outside the formed nano Si/SiOx + Li particles, so that on one hand, the conductivity is improved, the expansion of the silicon-based material is inhibited, on the other hand, the lithium is pre-supplemented by the laminated negative electrode material, the first effect of the negative electrode material is improved, and the quantity of active lithium is increased in a full battery.
The invention also discloses application of the silicon-based laminated negative electrode material as a negative electrode plate of a lithium battery, and the silicon-based laminated negative electrode material prepared by the magnetron sputtering technology can be directly used for the negative electrode of the lithium battery, can obtain uniformly distributed negative electrode plates, does not need wet coating, does not need to add a conductive agent, a binder and the like. The lithium battery negative pole piece prepared by the process has high first effect and low expansion performance.
Drawings
FIG. 1 is a schematic structural diagram of a silicon-based laminated anode material according to the present invention; wherein, A is a negative current collector, B is a graphite-like carbon layer, and C is nano Si/SiOx + Li particles coated by the graphite-like carbon.
Detailed Description
In order to make the technical solutions of the present invention better understood, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in 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 obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, shall fall within the protection scope of the present invention.
It should be noted that the terms "first," "second," and the like in the description and claims of the present invention and in the drawings described above are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It is to be understood that the data so used is interchangeable under appropriate circumstances such that the embodiments of the invention described herein are capable of operation in sequences other than those illustrated or described herein. Furthermore, the terms "comprises," "comprising," and "having," and any variations thereof, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed, but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.
The invention is described in further detail below with reference to the accompanying drawings:
referring to fig. 1, the silicon-based laminated negative electrode material disclosed by the invention is formed by alternately stacking graphite-like carbon layers and graphite-like carbon-coated silicon-based alloy particles, the thickness of the silicon-based laminated negative electrode material is 500-1500 nm, the thickness of the graphite-like layer is 5-20 nm, and the particle size of the graphite-like carbon-coated nano silicon-based alloy particles (Si/SiOx + Li particles, wherein x is more than 0 and less than 2) is 5-20 nm. The structural schematic diagram of the silicon-based laminated negative electrode material is shown in fig. 1, wherein a is a negative electrode current collector, B is a graphite-like carbon layer, and C is a graphite-like carbon/silicon-based alloy particle layer formed by graphite-like carbon-coated nano Si/SiOx + Li particles.
The invention also discloses a preparation method of the silicon-based laminated anode material, which comprises the following steps:
(1) Depositing graphite-like carbon on the copper foil by adopting a magnetron sputtering technology, wherein the thickness of a graphite-like layer is 5-20 nm;
(2) Sputtering and depositing Si or SiOx (x is more than 0 and less than 2) on the graphite-like carbon layer in the step (1), wherein the thickness of the Si or SiOx (x is more than 0 and less than 2) layer is 5-10 nm;
(3) Sputtering Li on the basis of the step (2), wherein the thickness of the Li layer is 0-2 nm;
(4) Performing pulse type rapid photo-thermal annealing treatment on the nano composite layer in the step (3) to obtain nano silicon-based alloy particles;
(5) And (5) sputtering and depositing graphite-like carbon on the basis of the nano silicon-based alloy particles obtained in the step (4) to obtain a graphite-like carbon/silicon-based alloy particle layer, wherein the thickness of the graphite-like carbon/silicon-based alloy particle layer is 5-20 nm.
The preparation method also comprises the step of repeating the steps (2) to (5) until the thickness of the whole film layer reaches 500-1500 nm.
The substrate material in the step (1) is copper foil, and the thickness of the copper foil is 4-8 mu m.
And (3) in the Si sputtering in the step (2), a silicon target is used as a target source, the silicon target is a P-type or N-type doped target, and direct current sputtering is adopted.
In the SiOx (x is more than 0 and less than 2) in the step (2), the silicon monoxide is used as a target source, and intermediate frequency or radio frequency sputtering is adopted.
And (4) in the step (3), li takes a lithium target as a target source and adopts direct current sputtering.
The rapid annealing treatment in the step (4) is pulse type rapid photo-thermal annealing, the annealing temperature is 400-500 ℃, the heating rate is 80-100 ℃/s, and the time is 7-10 s.
The present invention will now be described in further detail with reference to specific examples, which are intended to be illustrative, but not limiting, of the invention.
Example 1
(1) Depositing a graphite-like carbon layer on the flexible copper foil by adopting a magnetron sputtering technology, wherein the thickness is 10nm;
(2) Sputtering and depositing a nano Si layer on the graphite-like carbon layer in the step (1), wherein the thickness of the nano Si layer is 5nm;
(3) Sputtering Li on the basis of the step (2), wherein the thickness of the Li layer is 1nm;
(4) Performing pulse type rapid photo-thermal annealing treatment on the composite layer in the step (3), wherein the temperature is 500 ℃, the heating rate is 100 ℃/s, and the time is 10s; obtaining 6nm nano silicon-based alloy particles;
(5) And (5) sputtering and depositing graphite-like carbon on the basis of the step (4) to obtain a graphite-like carbon/silicon-based alloy particle layer, wherein the thickness of the graphite-like carbon/silicon-based alloy particle layer is 20nm.
(6) And (5) repeating the steps (2) to (5) to obtain the silicon-based laminated negative electrode material with the thickness of 500nm.
Example 2
(1) Depositing a graphite-like carbon layer on the flexible copper foil by adopting a magnetron sputtering technology, wherein the thickness is 5nm;
(2) Sputtering and depositing a nano Si layer on the graphite layer in the step (1), wherein the thickness of the nano Si layer is 8nm;
(3) Sputtering Li on the basis of the step (2), wherein the thickness of the Li layer is 1nm;
(4) Performing pulse type rapid photo-thermal annealing treatment on the composite layer in the step (3), wherein the temperature is 400 ℃, the heating rate is 80 ℃/s, and the time is 7s; obtaining 9nm nanometer silicon-based alloy particles;
(5) And (4) sputtering and depositing graphite-like carbon on the basis of the step (4) to obtain a graphite-like carbon/silicon-based alloy particle layer, wherein the thickness of the graphite-like carbon/silicon-based alloy particle layer is 19nm.
(6) And (5) repeating the steps (2) to (5) to obtain the silicon-based laminated negative electrode material with the thickness of 800 nm.
Example 3
(1) Depositing a graphite-like carbon layer on the flexible copper foil by adopting a magnetron sputtering technology, wherein the thickness of the graphite-like carbon layer is 8nm;
(2) Sputtering and depositing a nano SiOx layer with the thickness of 8nm on the graphite layer in the step (1);
(3) Sputtering Li on the basis of the step (2), wherein the thickness of the Li layer is 1nm;
(4) Performing pulse type rapid photo-thermal annealing treatment on the composite layer in the step (3), wherein the temperature is 400 ℃, the heating rate is 80 ℃/s, and the time is 7s; obtaining 9nm nano silicon-based alloy particles;
(5) And (4) sputtering and depositing graphite-like carbon on the basis of the step (4) to obtain a graphite-like carbon/silicon-based alloy particle layer, wherein the thickness of the graphite-like carbon/silicon-based alloy particle layer is 14nm.
(6) And (5) repeating the steps (2) to (5) to obtain the silicon-based laminated negative electrode material with the thickness of 1500nm.
Example 4
(1) Depositing a graphite-like carbon layer on the flexible copper foil by adopting a magnetron sputtering technology, wherein the thickness of the graphite-like carbon layer is 15nm;
(2) Sputtering and depositing a nano SiOx layer with the thickness of 10nm on the graphite layer in the step (1);
(3) Sputtering Li on the basis of the step (2), wherein the thickness of the Li layer is 2nm;
(4) Performing pulse type rapid photo-thermal annealing treatment on the composite layer in the step (3), wherein the temperature is 430 ℃, the heating rate is 95 ℃/s, and the time is 8s; obtaining 12nm nano silicon-based alloy particles;
(5) And (5) sputtering and depositing graphite-like carbon on the basis of the step (4) to obtain a graphite-like carbon/silicon-based alloy particle layer, wherein the thickness of the graphite-like carbon/silicon-based alloy particle layer is 10nm.
(6) And (5) repeating the steps (2) to (5) to obtain the silicon-based laminated negative electrode material with the thickness of 1200 nm.
Example 5
(1) Depositing a graphite-like carbon layer on the flexible copper foil by adopting a magnetron sputtering technology, wherein the thickness of the graphite-like carbon layer is 20nm;
(2) Sputtering and depositing a nano SiOx layer with the thickness of 5nm on the graphite layer in the step (1);
(3) Li is not sputtered;
(4) Performing pulse type rapid photo-thermal annealing treatment on the composite layer in the step (3), wherein the temperature is 470 ℃, the heating rate is 82 ℃/s, and the time is 9s; obtaining 5nm nano silicon-based alloy particles;
(5) And (5) sputtering and depositing graphite-like carbon on the basis of the step (4) to obtain a graphite-like carbon/silicon-based alloy particle layer, wherein the thickness of the graphite-like carbon/silicon-based alloy particle layer is 5nm.
(6) And (6) repeating the steps (2) to (5) to obtain the silicon-based laminated anode material with the thickness of 650 nm.
The silicon-based laminated anode materials obtained in the above examples 1 to 5 were tested by using a standard button cell, and the discharge rate was 0.1C to a voltage of 5mV. The expansion rate of the pole piece is tested by a battery disassembly method. The results are shown in table 1 below.
Table 1 table of performance test results of the silicon-based laminated anode materials obtained in examples 1 to 3
The above-mentioned contents are only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited thereby, and any modification made on the basis of the technical idea of the present invention falls within the protection scope of the claims of the present invention.
Claims (8)
1. The preparation method of the silicon-based laminated anode material is characterized by comprising the following steps of:
1) Depositing a graphite-like carbon layer on the substrate by adopting a magnetron sputtering technology;
2) Depositing a nano silicon-based material on the graphite-like carbon layer obtained in the step 1), and then depositing Li to obtain a silicon-based composite material;
3) Annealing the silicon-based composite material obtained in the step 2) to obtain nano silicon-based alloy particles, and performing graphite-like carbon deposition on the obtained nano silicon-based alloy particles to obtain a graphite-like carbon/silicon-based alloy particle layer;
4) Repeating the step 2) to the step 3) to obtain a silicon-based laminated negative electrode material;
in the step 3), the annealing treatment is pulse type rapid photo-thermal annealing, the annealing temperature is 400-500 ℃, the heating rate is 80-100 ℃/s, and the annealing time is 7-10s;
in the step 4), the thickness of the obtained silicon-based laminated negative electrode material is 500-1500 nm.
2. The method for preparing a silicon-based laminated anode material as claimed in claim 1, wherein in the step 1), the thickness of the obtained graphite-like carbon layer is 5 to 20nm.
3. The method for preparing a silicon-based laminated negative electrode material as claimed in claim 1, wherein in the step 2), the nano silicon-based material is nano Si or nano SiOx, x is more than 0 and less than 2, and the deposition thickness of the nano silicon-based material is 5 to 10nm.
4. The method for preparing the silicon-based laminated negative electrode material as claimed in claim 1, wherein in the step 2), the deposition thickness of Li is 1 to 2nm.
5. The method for preparing a silicon-based laminated anode material as claimed in claim 1, wherein in the step 3), the thickness of the obtained graphite-like carbon/silicon-based alloy particle layer is 5 to 20nm.
6. The method for preparing a silicon-based laminated anode material according to claim 1, wherein in the step 1), the substrate is a copper foil.
7. A silicon-based laminated negative electrode material prepared by the preparation method of any one of claims 1 to 6.
8. The use of the silicon-based laminated negative electrode material of claim 7 as a negative electrode sheet for a lithium battery.
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