CN110931720A - Low-cost preparation method of high-compaction-density negative electrode material for lithium ion battery - Google Patents
Low-cost preparation method of high-compaction-density negative electrode material for lithium ion battery Download PDFInfo
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Abstract
The invention discloses a low-cost preparation method of a high-compaction-density cathode material for a lithium ion battery, which comprises the following steps of: step 1, respectively weighing the following raw materials: 1 part of ferrosilicon ore, 1.5-2 parts of grinding balls, 0.1 part of ascorbic acid and 0.8-1.2 parts of ethanol; step 2, uniformly mixing the ferrosilicon ore, the grinding balls, ethanol and 10 wt% of ascorbic acid weighed in the step 1, adding the mixture into a ball milling tank, vacuumizing and ball milling to obtain ball-milled ferrosilicon powder; step 3, adding the ball-milled ferrosilicon powder prepared in the step 2 into a vinegar solution, stirring, centrifuging, cleaning and drying to obtain porous ferrosilicon powder corroded by acetic acid; and 4, sintering the porous ferrosilicon powder prepared in the step 3 in a tubular furnace, and performing CVD carbon deposition to obtain the ferrosilicon cathode material for the lithium ion battery. The lithium battery using the ferrosilicon material prepared by the invention as the cathode material has the advantages of high coulombic efficiency, high capacity, good cycling stability and the like on the aspect of electrical properties.
Description
Technical Field
The invention relates to a low-cost preparation method of a high-compaction-density cathode material for a lithium ion battery.
Background
Lithium ion batteries are widely used in a plurality of fields such as mobile electronic devices, electric vehicles, energy storage devices and the like as the current electric energy storage technical means with the highest energy density. With the vigorous development and increasing demand of the application market, higher requirements are also put forward on a plurality of technical indexes of the lithium ion battery, such as energy density, capacity density, power density and the like. The core part of the lithium ion battery is a positive electrode material and a negative electrode material, the service performance of the battery is directly determined, and the energy density, the cycle life, the cycle efficiency and the safety performance are all key indexes of the electrode materials. At present, the most common negative electrode materials of commercial lithium batteries are mainly carbon-based materials and silicon-carbon-based materials, which have the advantages of relatively stable cycle performance, relatively high cycle efficiency, safety, no pollution and the like, pure silicon has high theoretical specific capacity (4200mAh/g), but silicon materials are accompanied by huge volume change (300%) in the cycle process of lithium intercalation and deintercalation, so that the pulverization of silicon simple substances is caused, the breakage and pulverization of electrodes are caused, and the safety and cycle life of lithium ion batteries are greatly influenced.
In order to alleviate capacity fading caused by volume expansion of a silicon electrode during charge and discharge cycles, existing methods include (1) reducing the size of silicon, and preparing nanoscale silicon, such as nanoparticles and nanowires, to alleviate expansion and breakage of the silicon during electrochemical reactions; (2) silicon is coated, and other materials are coated on the surface of the silicon particles, so that the aims of preventing the silicon particles from agglomerating, improving the electric connection among the active particles and reducing the silicon expansion are fulfilled; (3) the preparation of silicon/carbon, silicon/metal (e.g., iron silicide, nickel silicide, and titanium carbide) composites also reduces the degree of volume expansion during charge/discharge cycles and optimizes the chemical composition of the unstable SEI layer on the silicon surface by preparing composites of inert materials that do not participate in the electrochemical reaction.
In addition, various methods of introducing pores into a bulk material or a agglomerated silicon particle structure to reduce collapse of the material structure due to repeated expansion and contraction during charge/discharge cycles have been proposed, which have been previously used to prepare various types of silicon-based active materials having a characteristic pore structure, which exhibit excellent cycle performance. However, most of the above methods are complicated in preparation process, high in cost, and remained in experimental stage.
The main problems of the prior art when silicon is used as a negative electrode material are as follows: the material has low compacted density (less than 1.5g/cm3), short cycle life, low first cycle efficiency and long charge and discharge time. The invention discloses a porous ferrosilicon negative electrode material for a lithium ion battery, which has unique alloy component design and microstructure, reasonable alloy granularity and pore structure distribution, can meet the coating requirement of the lithium ion battery, has higher specific capacity, and has the characteristics of high compaction density, long cycle life and high first cycle efficiency.
Disclosure of Invention
The invention aims to provide a ferrosilicon cathode material for a lithium ion battery and a preparation method thereof, which aim to solve the problems of short cycle life, low first cycle efficiency, low compaction density and the like of a silicon-based cathode material in the background technology; and the preparation method is simple to operate, has extremely low production cost and is easy to realize industrialization.
In order to solve the technical problems, the invention provides the following technical scheme: a high-compaction-density negative electrode material for a lithium ion battery adopts ferrosilicon as a raw material, wherein the ferrosilicon comprises the following elements in percentage by mass:
80% of silicon element and 20% of iron element, wherein the sum of the mass percentages of the components is 100%;
the preparation method of the high-compaction-density cathode material for the lithium ion battery specifically comprises the following steps:
step 1, respectively weighing the following raw materials:
1 part of ferrosilicon ore, 1.5-2 parts of grinding balls, 0.1 part of ascorbic acid and 0.8-1.2 parts of ethanol;
step 2, uniformly mixing the ferrosilicon ore, the grinding balls, ethanol and 10 wt% of ascorbic acid weighed in the step 1, then adding the mixture into a ball milling tank, vacuumizing and ball milling to obtain ball-milled ferrosilicon powder;
step 3, adding the ball-milled ferrosilicon powder prepared in the step 2 into a vinegar solution, stirring, centrifuging, cleaning and drying to obtain porous ferrosilicon powder corroded by acetic acid;
and 4, sintering the porous ferrosilicon powder prepared in the step 3 in a tubular furnace, and performing CVD carbon deposition to obtain the ferrosilicon cathode material for the lithium ion battery.
Furthermore, the crystal granularity of the ferrosilicon negative electrode material is not more than 500nm, and the secondary particle granularity is not more than 5 mu m.
Further, the ball milling time in the step 2 is 2h-4 h.
Further, the granularity of the ball-milled ferrosilicon powder obtained in the step 2 is not more than 5 μm.
Further, the acid solution in step 3 is acetic acid with a concentration of 1M.
Further, the vinegar solution is in excess compared to the ferrosilicon powder in step 3.
Further, in the step 3, the drying process is that the drying temperature is 80-120 ℃, the drying time is 3-8 h, and the drying atmosphere is vacuum.
Further, the sintering process in the step 4 is that the temperature is firstly raised to 650-750 ℃, acetylene is introduced for 10-30 min, and then sintering is carried out for 2-3 h.
Compared with the prior art, the invention has the following beneficial effects:
1) the ferrosilicon anode material for the lithium ion battery is a controllable porous silicon/ferrosilicon alloy composite material, has unique alloy component design and microstructure, and reasonable alloy granularity and pore structure distribution, wherein silicon is used for providing high capacity, the ferrosilicon is embedded in the ferrosilicon, and the volume expansion of the material in the charging and discharging process is relieved by combining the porous structure and carbon coating, so that the ferrosilicon anode material not only has higher specific capacity (more than 500mAh/g in stability), but also has the characteristics of long cycle life and high first cycle efficiency of high compaction density (1.75g/cm 3).
2) The preparation method of the ferrosilicon cathode material for the lithium ion battery is simple to operate, low in cost and easy to realize industrialization.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention. In the drawings:
FIG. 1 is a SEM of a ball-milled ferrosilicon powder as provided in example 1 of the present invention;
FIG. 2 is a test result of XRD of the ball-milled Si-Fe powder and the porous Si-Fe powder provided in example 2 of the present invention;
fig. 3 is a TEM result of a ferrosilicon anode material for a battery provided in example 2 of the present invention;
fig. 4 is a charge-discharge characteristic curve diagram of a lithium battery prepared from the ferrosilicon negative electrode material for the lithium ion battery provided in embodiment 5 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.
Referring to fig. 1 to 4, the present invention provides a low-cost preparation method of a high-compaction-density negative electrode material for a lithium ion battery, wherein the high-compaction-density negative electrode material uses ferrosilicon ore as a raw material, and the ferrosilicon ore comprises the following elements by mass:
80% of silicon element and 20% of iron element, wherein the sum of the mass percentages of the components is 100%;
wherein the crystal granularity of the ferrosilicon anode material is not more than 500nm, and the secondary particle granularity is not more than 5 mu m.
The preparation method of the high-compaction-density cathode material for the lithium ion battery specifically comprises the following steps:
step 1, respectively weighing the following raw materials:
1 part of ferrosilicon ore, 1.5-2 parts of grinding balls, 0.1 part of ascorbic acid and 0.8-1.2 parts of ethanol;
step 2, uniformly mixing the ferrosilicon ore, the grinding balls, the ethanol and the ascorbic acid weighed in the step 1, adding the mixture into a ball milling tank, vacuumizing and carrying out ball milling to obtain ball-milled ferrosilicon powder, wherein the ball milling time is 2-4 h, and the particle size of the obtained ball-milled ferrosilicon powder is not more than 5 microns;
step 3, adding the ball-milled silicon iron powder prepared in the step 2 into excessive acetic acid, stirring, centrifuging, cleaning and vacuum drying, wherein the drying temperature is 80-120 ℃, and the drying time is 3-8 h, so as to obtain porous silicon iron powder;
and 4, placing the porous ferrosilicon powder prepared in the step 3 into a tube furnace for sintering, and performing CVD carbon deposition, wherein the sintering process is as follows: firstly heating to 650-750 ℃, introducing acetylene for 10-30 min, and sintering for 2-3 h to obtain the ferrosilicon cathode material for the lithium ion battery.
Example 1:
step 1, respectively weighing the following raw materials:
1 part of ferrosilicon ore, 1.5 parts of grinding balls, 1.2 parts of ethanol and 0.1 part of ascorbic acid;
step 2, uniformly mixing the ferrosilicon ore, the grinding balls, the ethanol and the ascorbic acid weighed in the step 1, adding the mixture into a ball milling tank, vacuumizing and carrying out ball milling to obtain ball-milled ferrosilicon powder, wherein the ball milling time is 2.5 hours, and the particle size of the obtained ball-milled ferrosilicon powder is not more than 5 microns;
step 3, adding the ball-milled ferrosilicon powder prepared in the step 2 into excessive acetic acid, stirring, centrifuging, cleaning, and placing in a vacuum drying oven for vacuumizing at 80 ℃ and drying for 8 hours to obtain porous ferrosilicon powder;
and 4, sintering the porous ferrosilicon powder prepared in the step 3 in a tubular furnace, heating to 680 ℃, introducing acetylene for 15min, and continuing sintering for 3h to obtain the ferrosilicon cathode material for the lithium ion battery.
And (4) SEM characterization:
the lithium ion battery obtained in the embodiment 1 of the invention is characterized by a silicon iron negative electrode material SEM, as shown in figure 1, it can be seen that the material particles are not more than 5um and are accompanied with holes.
Example 2:
step 1, respectively weighing the following raw materials:
1 part of ferrosilicon ore, 2 parts of grinding balls and 0.8 part of ethanol;
step 2, uniformly mixing the ferrosilicon ore weighed in the step 1, grinding balls and ethanol, adding the mixture into a ball milling tank, vacuumizing and carrying out ball milling to obtain ball-milled ferrosilicon powder, wherein the ball milling time is 2 hours, and the particle size of the obtained ball-milled ferrosilicon powder is not more than 5 microns;
step 3, adding the ball-milled ferrosilicon powder prepared in the step 2 into excessive acetic acid, stirring, centrifuging, cleaning, and placing in a vacuum drying oven for vacuumizing at 120 ℃ and drying for 3 hours to obtain porous ferrosilicon powder;
and 4, sintering the porous ferrosilicon powder prepared in the step 3 in a tubular furnace, heating to 750 ℃, introducing acetylene for 10min, and continuing sintering for 2h to obtain the ferrosilicon cathode material for the lithium ion battery.
XRD characterization:
XRD representation is carried out on the ball-milled silicon iron powder and the porous silicon iron powder obtained in the embodiment 2 of the invention, as shown in figure 2, the ball-milled silicon iron powder is a composite phase of a silicon simple substance and FeSi2 alloy, no other impurities exist, the peak intensity of the FeSi2 alloy can be seen to be reduced after acid corrosion, and the situation that the FeSi2 alloy is partially corroded to form a porous structure is shown.
TEM representation:
the lithium ion battery obtained in the embodiment 2 of the invention is characterized by using a ferrosilicon negative electrode material in a TEM mode, as shown in FIG. 3, the silicon simple substance in the ferrosilicon negative electrode material and the crystal lattice of FeSi2 can be seen, the silicon simple substance and FeSi2 are well combined together, and the composite material can be seen to have a layer of amorphous carbon coating structure after CVD.
Example 3:
step 1, respectively weighing the following raw materials:
1 part of ferrosilicon ore, 1.8 parts of grinding balls and 1 part of ethanol;
step 2, uniformly mixing the ferrosilicon ore weighed in the step 1, grinding balls and ethanol, adding the mixture into a ball milling tank, vacuumizing and carrying out ball milling to obtain ball-milled ferrosilicon powder, wherein the ball milling time is 4 hours, and the particle size of the obtained ball-milled ferrosilicon powder is not more than 5 microns;
step 3, adding the ball-milled ferrosilicon powder prepared in the step 2 into excessive acetic acid, stirring, centrifuging, cleaning, and placing in a vacuum drying oven for vacuumizing at 100 ℃ and drying for 5 hours to obtain porous ferrosilicon powder;
and 4, sintering the porous ferrosilicon powder prepared in the step 3 in a tubular furnace, heating to 700 ℃, introducing acetylene for 30min, and continuing sintering for 2.5h to obtain the ferrosilicon cathode material for the lithium ion battery.
Example 4:
step 1, respectively weighing the following raw materials:
1 part of ferrosilicon ore, 1.8 parts of grinding balls and 1.2 parts of ethanol;
step 2, uniformly mixing the ferrosilicon ore weighed in the step 1, grinding balls and ethanol, adding the mixture into a ball milling tank, vacuumizing and carrying out ball milling to obtain ball-milled ferrosilicon powder, wherein the ball milling time is 3.5 hours, and the particle size of the obtained ball-milled ferrosilicon powder is not more than 5 microns;
step 3, adding the ball-milled ferrosilicon powder prepared in the step 2 into excessive hydrochloric acid, stirring, centrifuging, cleaning, and placing in a vacuum drying oven for vacuumizing at 80 ℃ and drying for 5 hours to obtain porous ferrosilicon powder;
and 4, sintering the porous ferrosilicon powder prepared in the step 3 in a tubular furnace, heating to 700 ℃, introducing acetylene for 20min, and continuing sintering for 2h to obtain the ferrosilicon cathode material for the lithium ion battery.
Example 5:
step 1, respectively weighing the following raw materials:
1 part of ferrosilicon ore, 2 parts of grinding balls and 1.2 parts of ethanol;
step 2, uniformly mixing the ferrosilicon ore weighed in the step 1, grinding balls and ethanol, adding the mixture into a ball milling tank, vacuumizing and carrying out ball milling to obtain ball-milled ferrosilicon powder, wherein the ball milling time is 3 hours, and the particle size of the obtained ball-milled ferrosilicon powder is not more than 5 microns;
step 3, adding the ball-milled ferrosilicon powder prepared in the step 2 into excessive hydrochloric acid, stirring, centrifuging, cleaning, and placing in a vacuum drying oven for vacuumizing at 90 ℃ and drying for 5 hours to obtain porous ferrosilicon powder;
and 4, sintering the porous ferrosilicon powder prepared in the step 3 in a tubular furnace, heating to 750 ℃, introducing acetylene for 20min, and continuing sintering for 3h to obtain the ferrosilicon cathode material for the lithium ion battery.
And (3) testing the charge and discharge performance:
the ferrosilicon negative electrode material for the lithium ion battery obtained in the embodiment 5 of the invention is made into a battery pole piece.
The manufacturing process of the battery pole piece comprises the following steps: mixing and grinding the prepared ferrosilicon negative electrode material, super-p and CMC according to the mass ratio of 8:1:1, using water as a solvent, stirring for 4h, coating on a copper foil, drying in vacuum for 12h, slicing into a wafer with the diameter of 12mm, and testing the surface density of a pole piece to be about 85g/m 2.
And (3) battery cycle test: in a glove box filled with high-purity argon, water and oxygen with the concentration less than 0.1ppm, a metal lithium sheet is taken as a counter electrode to assemble a 2032 button cell, after the cell is placed for 12 hours, the charging limiting voltage of the cell is 2.0V, and the discharging termination voltage is 0.01V under a constant current mode. The test results are shown in fig. 4, and it can be seen that: the charging and discharging performance test is carried out when the charging current and the discharging current are 0.2C, the first cycle coulombic efficiency reaches 85 percent, and the average charging and discharging specific capacity is about 780 mAh/g. At the 27 th circle, the charge and discharge multiplying power is set to be 0.5C, the average specific charge and discharge capacity is about 570mAh/g, and the coulombic efficiency is 99.0 percent. The capacity retention rate after 100 times of charge-discharge cycles is 83.5%.
Finally, the lithium battery using the ferrosilicon material prepared by the technical scheme of the invention as the cathode material has the advantages of high coulombic efficiency, high capacity, good cycling stability and the like in the aspect of electrical properties.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. 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 (8)
1. A low-cost preparation method of a high-compaction-density cathode material for a lithium ion battery is characterized by comprising the following steps of: the method adopts the ferrosilicon ore as a raw material, wherein the ferrosilicon ore comprises the following elements in percentage by mass:
80% of silicon element and 20% of iron element, wherein the sum of the mass percentages of the components is 100%;
the preparation method of the high-compaction-density cathode material for the lithium ion battery specifically comprises the following steps:
step 1, respectively weighing the following raw materials:
1 part of ferrosilicon ore, 1.5-2 parts of grinding balls, 0.1 part of ascorbic acid and 0.8-1.2 parts of ethanol;
step 2, uniformly mixing the ferrosilicon ore, the grinding balls, ethanol and 10 wt% of ascorbic acid weighed in the step 1, then adding the mixture into a ball milling tank, vacuumizing and ball milling to obtain ball-milled ferrosilicon powder;
step 3, adding the ball-milled ferrosilicon powder prepared in the step 2 into a vinegar solution, stirring, centrifuging, cleaning and drying to obtain porous ferrosilicon powder corroded by acetic acid;
and 4, sintering the porous ferrosilicon powder prepared in the step 3 in a tubular furnace, and performing CVD carbon deposition to obtain the ferrosilicon cathode material for the lithium ion battery.
2. The low-cost preparation method of the high-compaction-density negative electrode material for the lithium ion battery according to claim 1, characterized by comprising the following steps: the crystal granularity of the ferrosilicon negative electrode material is not more than 500nm, and the secondary particle granularity is not more than 5 mu m.
3. The low-cost preparation method of the high-compaction-density negative electrode material for the lithium ion battery according to claim 1, characterized by comprising the following steps: the ball milling time in the step 2 is 2-4 h.
4. The low-cost preparation method of the high-compaction-density negative electrode material for the lithium ion battery according to claim 1, characterized by comprising the following steps: and (3) the granularity of the ball-milled ferrosilicon powder obtained in the step (2) is not more than 5 mu m.
5. The low-cost preparation method of the high-compaction-density negative electrode material for the lithium ion battery according to claim 1, characterized by comprising the following steps: the acid solution in step 3 is acetic acid with the concentration of 1M.
6. The low-cost preparation method of the high-compaction-density negative electrode material for the lithium ion battery according to claim 1, characterized by comprising the following steps: the vinegar solution in step 3 is in excess compared to ferrosilicon powder.
7. The low-cost preparation method of the high-compaction-density negative electrode material for the lithium ion battery according to claim 1, characterized by comprising the following steps: the drying process in the step 3 is that the drying temperature is 80-120 ℃, the drying time is 3-8 h, and the drying atmosphere is vacuum.
8. The low-cost preparation method of the high-compaction-density negative electrode material for the lithium ion battery according to claim 1, characterized by comprising the following steps: the sintering process in the step 4 is that the temperature is firstly raised to 650-750 ℃, acetylene is introduced for 10-30 min, and then sintering is carried out for 2-3 h.
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| CN105609740A (en) * | 2016-03-01 | 2016-05-25 | 中国科学院化学研究所 | Silicon alloy composite microspheres and preparation method and application thereof |
| CN108987724A (en) * | 2018-08-16 | 2018-12-11 | 浙江衡远新能源科技有限公司 | A kind of hollow Si/C composite negative pole material of lithium ion battery and preparation method thereof |
| CN109461921A (en) * | 2018-11-09 | 2019-03-12 | 广东省稀有金属研究所 | A kind of preparation method based on modified lithium ion battery silicon-base alloy composite negative pole material |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105609740A (en) * | 2016-03-01 | 2016-05-25 | 中国科学院化学研究所 | Silicon alloy composite microspheres and preparation method and application thereof |
| CN108987724A (en) * | 2018-08-16 | 2018-12-11 | 浙江衡远新能源科技有限公司 | A kind of hollow Si/C composite negative pole material of lithium ion battery and preparation method thereof |
| CN109461921A (en) * | 2018-11-09 | 2019-03-12 | 广东省稀有金属研究所 | A kind of preparation method based on modified lithium ion battery silicon-base alloy composite negative pole material |
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