CN114914414A - Preparation method of silicon/titanium-niobium oxide composite anode material of lithium ion battery - Google Patents
Preparation method of silicon/titanium-niobium oxide composite anode material of lithium ion battery Download PDFInfo
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- CN114914414A CN114914414A CN202210456087.8A CN202210456087A CN114914414A CN 114914414 A CN114914414 A CN 114914414A CN 202210456087 A CN202210456087 A CN 202210456087A CN 114914414 A CN114914414 A CN 114914414A
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- H01M4/00—Electrodes
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- 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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- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
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- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/483—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides for non-aqueous cells
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
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Abstract
The invention belongs to the technical field of preparation of lithium ion battery electrode materials, and particularly relates to a preparation method of a silicon/titanium-niobium oxide composite anode material of a lithium ion battery, which comprises the following steps: 1) weighing raw materials of silicon powder, niobium pentachloride and isopropyl titanate according to the proportion, and adding alcohol for mixing; 2) evaporating at a proper temperature to obtain a dried precursor; 3) calcining the precursor in a tube furnace; cooling to room temperature and taking out to obtain the composite material; 4) and uniformly grinding the composite material, and then mixing the ground composite material, acetylene black and sodium alginate to obtain the slurry-shaped negative electrode material. According to the invention, the titanium niobium oxide and silicon are compounded to be used as the lithium ion battery cathode material, and the silicon and the matrix material are diffused to a certain degree through high-temperature heat treatment, so that the interface bonding force between the silicon and the titanium niobium oxide is improved, a firmer matrix structure is constructed, the volume effect of the silicon is buffered, and the cycle performance of the composite cathode material is improved.
Description
Technical Field
The invention belongs to the technical field of preparation of lithium ion battery electrode materials, and particularly relates to a preparation method of a silicon/titanium-niobium oxide composite anode material of a lithium ion battery.
Background
In recent years, high-speed development of novel mobile devices, artificial intelligence devices and the like puts higher demands on lithium ion battery technology, and the capacity and the cycle performance of the lithium ion battery are determined to a great extent by taking a negative electrode material as an important component of the lithium ion battery. Silicon is concerned about due to the advantages of high specific capacity, low cost of wood, environmental friendliness and the like, and becomes a novel negative electrode material one expected to replace graphite. The severe volume effect and poor conductivity of silicon materials limit their practical applications and continued development.
Among the numerous anode materials that are currently emerging, silicon-based anode materials are considered to be one of the most promising candidates for replacing commercial graphite anodes. The silicon-based material as the lithium ion battery cathode material has the advantages of the theoretical highest specific capacity (about 4200mA h/g) and the low working voltage (about 0.4Vvs + ) Abundant natural resources, etc. However, lithium intercalation/deintercalation with cycling leads to a drastic volume expansion (300%) of the electrode, resulting in severe pulverization, separation, and conductivity degradation of the electrode material, which leads to a rapid capacity decrease and a decrease in the cycle life of the silicon negative electrode. Besides the silicon is subjected to nano modification, the silicon can be compounded or alloyed with the silicon to relieve volume change and improve conductivity.
In view of the above, there is a need for a new method for preparing a negative electrode material of a lithium ion battery, so as to buffer the volume effect of silicon during the charging and discharging processes and improve the electrical contact of silicon particles.
Disclosure of Invention
The invention aims to overcome the problems in the prior art and provide a preparation method of a silicon/titanium-niobium oxide composite anode material of a lithium ion battery, which is characterized in that a stress buffer layer and an ion exchange layer are built around silicon particles by preparing the silicon/titanium-niobium oxide composite anode material with silicon as a reinforcement and titanium-niobium oxide as a base material so as to buffer the volume effect of silicon in the charging and discharging processes and improve the electrical contact of the silicon particles.
In order to achieve the technical purpose and achieve the technical effect, the invention is realized by the following technical scheme:
a preparation method of a silicon/titanium-niobium oxide composite anode material of a lithium ion battery comprises the following steps:
1) weighing raw materials of silicon powder, niobium pentachloride and isopropyl titanate according to the proportion, putting the raw materials into a beaker, and adding alcohol for mixing;
2) placing the beaker on a magnetic stirrer, adding magnetic seeds, evaporating at a proper temperature, and evaporating to obtain a dry precursor;
3) pouring the precursor into a crucible, putting the crucible into a tubular furnace filled with argon, and calcining at 835-900 ℃ for 4.5-5.5 h; cooling the calcined product to room temperature, and taking out to obtain the silicon/titanium-niobium oxide composite material;
4) fully and uniformly grinding the obtained composite material by using an agate mortar, and then mixing the ground composite material, acetylene black and sodium alginate according to the mass ratio of 6:2:2 to obtain the slurry-shaped negative electrode material.
Further, in the preparation method of the silicon/titanium-niobium oxide composite anode material for the lithium ion battery, in the step 1), the silicon powder is nano silicon powder, and the particle size of the nano silicon powder is 200-300 nm.
Further, in the preparation method of the silicon/titanium-niobium oxide composite anode material for the lithium ion battery, in the step 1), the mass ratio of the silicon powder to the niobium pentachloride to the isopropyl titanate is 2-4: 2: 1.
Further, in the preparation method of the silicon/titanium-niobium oxide composite anode material for the lithium ion battery, in the step 1), the proportion relationship between the alcohol and the isopropyl titanate is 200-400 ml/g.
Further, in the preparation method of the silicon/titanium-niobium oxide composite anode material of the lithium ion battery, in the step 2), the evaporation temperature is controlled to be 60-70 ℃.
Further, in the preparation method of the silicon/titanium-niobium oxide composite anode material for the lithium ion battery, in the step 3), the calcination is carried out at the temperature of 850 ℃ for 5 hours.
Further, according to the preparation method of the silicon/titanium-niobium oxide composite anode material of the lithium ion battery, in the step 3), the temperature rise rate of the tubular furnace is 3 ℃/min, and the temperature drop rate after calcination is-3 ℃/min.
Further, in the preparation method of the silicon/titanium-niobium oxide composite anode material for the lithium ion battery, in the step 4), sodium alginate is used as an aqueous binder, and is added into a sodium alginate solution with the mass fraction of 2.9-3.2%.
The invention has the beneficial effects that:
1. the preparation method provided by the invention has scientific and reasonable design, the titanium-niobium oxide is firstly used to be compounded with silicon, which is not found in all previous patents or literature reports, and the possibility of compounding the titanium-niobium oxide with the silicon is provided. The high-temperature solid phase method is applied to the current production process, so that the simplicity of the process is improved, and the possibility of large-scale production is realized.
2. The silicon/titanium-niobium oxide composite material prepared by the invention is different from a carbon material, the titanium-niobium oxide has a higher lithium extraction potential different from a silicon material, a voltage platform of the titanium-niobium oxide is between 1.5 and 2V, and a voltage platform of the silicon is below 0.6V, so that when the composite material is subjected to an electrochemical lithium extraction reaction under a voltage window of 0 to 1.5V, only silicon with higher capacity participates in an extraction and insertion process in the composite material, and a substrate material does not generate an extraction and insertion process, thereby being more beneficial to buffering the volume effect of the silicon in the charge and discharge process. In addition, compared with silicon/inert metal composite materials which do not undergo a de-intercalation process in the same way as the base materials, because silicon and oxygen have good affinity in the preparation process of the silicon/titanium-niobium oxide composite materials, silicon can be combined with oxygen atoms to undergo an oxidation-reduction reaction, and the transfer of the oxygen atoms between the silicon and the titanium-niobium oxide base materials is beneficial to obtaining the composite materials with stronger interface bonding force, so that the continuity of a lithium ion diffusion path is ensured.
Of course, it is not necessary for any one product that embodies the invention to achieve all of the above advantages simultaneously.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the description below are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a scanning electron micrograph and a spectrum characterization of a silicon/titanium-niobium oxide composite prepared in example 1 of the present invention;
FIG. 2 is a first-turn charge-discharge curve of a half-cell using the silicon/titanium-niobium oxide composite material and the nano silicon powder prepared in examples 1 to 3 of the present invention as the negative electrode material;
FIG. 3 is a graph showing the cycle life of a half-cell using the silicon/titanium-niobium oxide composite material and the nano-silicon powder prepared in examples 1 to 3 of the present invention as the negative electrode material;
FIG. 4 is a graph of half-cell rate performance of the silicon/titanium-niobium oxide composite material and the nano silicon powder prepared in examples 1 to 3 of the present invention as a negative electrode material;
FIG. 5 is a scanning electron micrograph of the silicon powder used in examples 1 to 3 of the present invention.
Detailed Description
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 derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The specific embodiment of the invention is as follows:
example 1
A preparation method of a silicon/titanium-niobium oxide composite anode material of a lithium ion battery specifically comprises the following steps:
1) 0.4g of sand grinding silicon powder, 0.4g of niobium pentachloride and 0.2g of isopropyl titanate solution are weighed and poured into a beaker, 40ml of alcohol is added for mixing;
2) placing the beaker on a magnetic stirrer, adding magnetic seeds, and evaporating at a proper rotating speed of 70 ℃ until a precursor of a sample is dried;
3) pouring the precursor of the sample into a crucible, putting the crucible into a tube furnace, and calcining for 5 hours at 850 ℃ at the heating rate of 3 ℃/min. After the calcination is finished, cooling at a cooling rate of-3 ℃/min, and taking out after the sample is cooled to room temperature to obtain the composite material;
4) and (2) fully and uniformly grinding the composite material by using an agate mortar for 20min, and then mixing the ground composite material, acetylene black and sodium alginate (the sodium alginate solution with the mass fraction of 3.0% is added) according to the mass ratio of 6:2:2 to obtain the cathode material slurry.
The application of the silicon/titanium-niobium oxide composite material for preparing the lithium ion battery as the cathode material specifically comprises the following steps:
s1, selecting a scraper with the scale of 200nm to evenly coat the mixed slurry on the current collector on the copper foil, putting the coated copper foil into an oven for drying, and drying for 8 hours at the temperature of 60 ℃;
s2, tabletting the copper foil dried in the step S1 by using a powder tablet machine, controlling the gauge pressure to be 10MPa, and processing the compacted tablets into electrode plates by using a tablet machine;
s3, drying the electrode slice in a vacuum oven at 60 ℃ for 12h, putting the electrode slice into a glove box filled with argon gas, assembling the battery, wherein the diaphragm is a polypropylene film, the electrolyte is the mixture of lithium hexafluorophosphate, ethylene carbonate and diethyl carbonate, the electrolyte is 10 wt% of vinyl fluoride carbonate, and the electrode slice is a negative electrode, and assembling the battery into a CR2025 button battery. Recording as STN 2: 2: 1.
example 2
On the basis of example 1, the mass of the nano silicon powder in the step 1) is adjusted to be 0.6g and the mass of the alcohol is adjusted to be 60ml, and the obtained product is marked as STN 3: 2: 1.
example 3
On the basis of example 1, the mass of the nano silicon powder in step 1) is adjusted to be 0.8g and the mass of the alcohol is adjusted to be 80ml, keeping other conditions unchanged, and the obtained product is marked with STN 4:2: 1.
fig. 1 is a scanning electron micrograph and an energy spectrum representation of the silicon/titanium-niobium oxide composite material, and it can be seen that a large amount of Ti, Nb, and O elements are attached to the surface of Si, thereby further verifying the successful compounding of silicon and titanium-niobium oxide.
Fig. 2 shows that the introduction of the titanium-niobium oxide does not have a great influence on the initial coulombic efficiency of silicon, and the coulombic efficiencies of the first turn of the silicon/titanium-niobium oxide composite materials prepared in examples 1 to 3 are all 75% to 90%.
Fig. 3 shows a cycle life diagram of a half-cell in which nano silicon powder and titanium-niobium oxide are compounded in different proportions, and it can be seen from the diagram that the cycle life performance of the compounded material is obviously improved compared with that of the nano silicon powder. Wherein STN 3: 2:1 the group of cathode materials has the best electrochemical performance, and after the cathode materials are cycled for 120 circles under the current density of 0.1C, the specific discharge capacity is kept at 582 mAh/g. The discharge specific capacity of the nano silicon powder less than 100mAh/g under the same condition is greatly exceeded.
FIG. 4 is a graph of multiplying power performance of nano silicon powder and titanium-niobium oxide compounded in different proportions. Compared with a nano silicon electrode, the composite material added with the titanium-niobium oxide has more excellent rate performance. Wherein STN 3: 2: the 1 sample recovered more rapidly than the others, showing the best rate performance.
FIG. 5 is a scanning electron micrograph of the silicon powder used in examples 1 to 3.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims (8)
1. A preparation method of a silicon/titanium-niobium oxide composite anode material of a lithium ion battery is characterized by comprising the following steps:
1) weighing raw materials of silicon powder, niobium pentachloride and isopropyl titanate according to the proportion, putting the raw materials into a beaker, and adding alcohol for mixing;
2) placing the beaker on a magnetic stirrer, adding magnetic seeds, evaporating at a proper temperature, and evaporating to obtain a dry precursor;
3) pouring the precursor into a crucible, putting the crucible into a tubular furnace filled with argon, and calcining at 835-900 ℃ for 4.5-5.5 h; cooling the calcined product to room temperature, and taking out to obtain the silicon/titanium-niobium oxide composite material;
4) fully and uniformly grinding the obtained composite material by using an agate mortar, and then mixing the ground composite material, acetylene black and sodium alginate according to the mass ratio of 6:2:2 to obtain the slurry-shaped negative electrode material.
2. The method for preparing the silicon/titanium-niobium oxide composite anode material of the lithium ion battery as claimed in claim 1, wherein the method comprises the following steps: in the step 1), the silicon powder is nano silicon powder, and the particle size of the nano silicon powder is 200-300 nm.
3. The method for preparing the silicon/titanium-niobium oxide composite anode material of the lithium ion battery as claimed in claim 1, wherein the method comprises the following steps: in the step 1), the mass ratio of the silicon powder to the niobium pentachloride to the isopropyl titanate is 2-4: 2: 1.
4. The method for preparing the silicon/titanium-niobium oxide composite anode material of the lithium ion battery as claimed in claim 1, wherein the method comprises the following steps: in the step 1), the proportion relationship of the alcohol and the isopropyl titanate is 200-400 ml/g.
5. The method for preparing the silicon/titanium-niobium oxide composite anode material of the lithium ion battery as claimed in claim 1, wherein the method comprises the following steps: in the step 2), the evaporation temperature is controlled to be 60-70 ℃.
6. The method for preparing the silicon/titanium-niobium oxide composite anode material of the lithium ion battery as claimed in claim 1, wherein the method comprises the following steps: in step 3), calcination was carried out at a temperature of 850 ℃ for 5 h.
7. The method for preparing the silicon/titanium-niobium oxide composite anode material of the lithium ion battery as claimed in claim 1, wherein the method comprises the following steps: in the step 3), the temperature rising rate of the tubular furnace is 3 ℃/min, and the temperature reduction rate after the calcination is-3 ℃/min.
8. The method for preparing the silicon/titanium-niobium oxide composite anode material of the lithium ion battery as claimed in claim 1, wherein the method comprises the following steps: in the step 4), sodium alginate is used as an aqueous binder, and the sodium alginate solution with the mass fraction of 2.9-3.2% is added.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116722129A (en) * | 2023-08-09 | 2023-09-08 | 泰鼎新能源(浙江)有限公司 | High-performance silicon-oxygen anode material and preparation method and application thereof |
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| CN111463419A (en) * | 2020-04-28 | 2020-07-28 | 苏州宇豪纳米材料有限公司 | Silicon-based @ titanium niobium oxide core-shell structure anode material and preparation method thereof |
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| CN103022448A (en) * | 2012-12-19 | 2013-04-03 | 天津巴莫科技股份有限公司 | Method for preparing lithium battery silicon carbon anode material |
| CN111463419A (en) * | 2020-04-28 | 2020-07-28 | 苏州宇豪纳米材料有限公司 | Silicon-based @ titanium niobium oxide core-shell structure anode material and preparation method thereof |
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| CN116722129A (en) * | 2023-08-09 | 2023-09-08 | 泰鼎新能源(浙江)有限公司 | High-performance silicon-oxygen anode material and preparation method and application thereof |
| CN116722129B (en) * | 2023-08-09 | 2023-11-03 | 泰鼎新能源(浙江)有限公司 | High-performance silicon-oxygen anode material and preparation method and application thereof |
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