CN102891296A - Method for preparing cathode material of aluminum-silicon-based lithium ion battery - Google Patents
Method for preparing cathode material of aluminum-silicon-based lithium ion battery Download PDFInfo
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- CN102891296A CN102891296A CN201210358755XA CN201210358755A CN102891296A CN 102891296 A CN102891296 A CN 102891296A CN 201210358755X A CN201210358755X A CN 201210358755XA CN 201210358755 A CN201210358755 A CN 201210358755A CN 102891296 A CN102891296 A CN 102891296A
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention discloses a method for preparing a cathode material of an aluminum-silicon-based lithium ion battery. The method comprises the steps of: preparing alloy raw materials according the molar ratio in a molecular formula of Si50Al13Mg5Ni2Sn9Ga5; melting the alloy raw materials in vacuum or in an argon environment under 0.1MPa to prepare an ingot; melting the ingot by using radio-frequency induction, extruding an alloy composition to the upper surface of a rotary cooling wheel through a nozzle to form a strip-shaped alloy belt, and annealing; and adding materials including the alloy belt, polyimide coating powder and acetylene black as an electric conduction additive into a ball mill, grinding the materials, then sieving the ground materials through a 100-mesh sieve, mixing the ground materials, and dissolving the materials in N-methyl pyrrolidine to prepare uniform slurry to obtain the cathode material of the aluminum-silicon-based lithium ion battery. The cathode material of the aluminum-silicon-based lithium ion battery, prepared according to the invention, has both high energy density and good cyclic stability, and is high in capacity, good in cyclic stability and long in service life when applied to the lithium ion batteries.
Description
Technical field
The present invention relates to a kind of preparation method of lithium ion battery negative material, relate in particular to the preparation method of the silica-based lithium ion battery negative material of a kind of aluminium.
Background technology
Lithium ion battery is as a kind of novel secondary cell, has specific capacity height, voltage is high, fail safe is good characteristics, is widely used in the driving power of the portable electronics such as mobile phone, notebook computer, field camera, DVD, MP3.But along with the continuous upgrading of electronic product, the requirement of its power supply is also improved constantly, thereby the energy density of battery material is also had higher requirement.
At present commercial Li-ion batteries mainly adopts graphite as negative material, but because of its charged and discharged electric weight lower bound system the capacity of battery increase and the dwindling of volume.Some simple metal have the capacity more much higher than graphite, fail to be applied at lithium ion battery but its charge-discharge performance is too poor.Some intermetallic compounds that prepare that in all sorts of ways make moderate progress with respect to the simple metal charge-discharge performance take the sacrifice capacity as cost, but effect is limited.
Therefore in the urgent need to a kind of alloy material is provided, as lithium ion battery negative charging/discharging function materials'use, effectively improves the charge/discharge capacity of lithium ion battery negative and improve cycle performance.
Summary of the invention
The preparation method who the purpose of this invention is to provide the silica-based lithium ion battery negative material of a kind of aluminium uses the lithium ion battery of the silica-based lithium ion battery negative material of aluminium of the method preparation to have good, the characteristics such as energy density is high, long service life of cyclicity.
To achieve these goals, the preparation method of the silica-based lithium ion battery negative material of a kind of aluminium provided by the invention comprises the steps:
Step 1 is prepared alloy raw material
According to molecular formula Si
50Al
13Mg
5Ni
2Sn
9Ga
5In the mol ratio of each element prepare alloy raw material;
Step 2, the molten alloy raw material
The alloy raw material of above-mentioned preparation is had in the arc furnace of argon filling of copper burner hearth melting and make ingot bar under vacuum or 0.1MPa ar gas environment, wherein the temperature of melting is 1800-2000 ℃;
Step 3 is made the alloy band
After being placed into the ingot bar bar in the container, system is vacuumized 0.01-0.1MPa, and then be filled with argon gas to 0.1-1MPa, come the melting ingot bar with radio frequency induction, when temperature reaches 1500-1600 ℃, the argon pressure of 2-4MPa is applied to the alloy composite surface of melting, and with alloy composite by nozzle be expressed into rotary speed be 6000-8000 rev/min the rotation cooling wheel above, the ribbon width that forms is 1-2mm, thickness is the alloy band of 5-10 micron, in tube furnace, under argon atmospher, ribbon was annealed 2-4 hour under 250-300 ℃;
Step 4, the preparation ion cathode material lithium
Add the material of following mass parts in the ball mill:
Above-mentioned alloy band 50-60
Polyimide paint powder 5-7
Conductive agent acetylene black 8-10
Cross 100 mesh sieves after above-mentioned material ground, fully mix and be dissolved in and be mixed with uniform slurry in the 1-METHYLPYRROLIDONE, obtain the silica-based lithium ion battery negative material of aluminium.
Wherein, in the step 1, aluminium, silicon, magnesium, nickel, tin can adopt the simple substance element of purity 99.9wt%.
Wherein, in the step 1, it is the above rare earth Ga element of 99.5wt% that Ga can adopt purity.
The present invention also provides a kind of silica-based lithium ion battery negative material of aluminium of above-mentioned any means preparation.
The lithium ion battery aluminium silicon based anode material of the present invention's preparation when having high-energy-density, has good cyclical stability, and when being used for lithium ion battery, capacity is high, good cycling stability, long service life.
Embodiment
Embodiment one
Prepare alloy raw material
According to molecular formula Si
50Al
13Mg
5Ni
2Sn
9Ga
5In the mol ratio of each element prepare alloy raw material, aluminium, silicon, magnesium, nickel, tin can adopt the simple substance element of purity 99.9wt% to get, it is the above rare earth Ga element of 99.5wt% that Ga adopts purity.
The molten alloy raw material
The alloy raw material of above-mentioned preparation is had in the arc furnace of argon filling of copper burner hearth melting and make ingot bar under vacuum or 0.1MPa ar gas environment, wherein the temperature of melting is 1800 ℃.
Make the alloy band
After being placed into the ingot bar bar in the crucible, system is vacuumized 0.01MPa, and then be filled with argon gas to 0.1MPa, come the melting ingot bar with radio frequency induction.When temperature reaches 1500 ℃, the argon pressure of 2MPa is applied to the alloy composite surface of melting, and with alloy composite by nozzle be expressed into rotary speed be 6000 rev/mins the rotation cooling wheel above, the ribbon width that forms is 1mm, thickness is 5 microns alloy band, in tube furnace, under argon atmospher, ribbon was annealed 2 hours under 250 ℃.
The preparation ion cathode material lithium
Add the material of following mass parts in the ball mill:
Above-mentioned alloy band 50
Polyimide paint powder 5
Conductive agent acetylene black 8
Cross 100 mesh sieves after above-mentioned material ground, fully mix and be dissolved in the N methyl pyrrolidone (NMP) and be mixed with uniform slurry, obtain the silica-based lithium ion battery negative material of aluminium.
Embodiment two
Prepare alloy raw material
According to molecular formula Si
50Al
13Mg
5Ni
2Sn
9Ga
5In the mol ratio of each element prepare alloy raw material, aluminium, silicon, magnesium, nickel, tin can adopt the simple substance element of purity 99.9wt% to get, it is the above rare earth Ga element of 99.5wt% that Ga adopts purity.
The molten alloy raw material
The alloy raw material of above-mentioned preparation is had in the arc furnace of argon filling of copper burner hearth melting and make ingot bar under the 0.1MPa ar gas environment, wherein the temperature of melting is 2000 ℃.
Make the alloy band
After being placed into the ingot bar bar in the crucible, system is vacuumized 0.1MPa, and then be filled with argon gas to 0.1MPa-1MPa, come the melting ingot bar with radio frequency induction.When temperature reaches 1600 ℃, the argon pressure of 4MPa is applied to the alloy composite surface of melting, and with alloy composite by nozzle be expressed into rotary speed be 8000 rev/mins the rotation cooling wheel above, the ribbon width that forms is 2mm, thickness is 10 microns alloy band, in tube furnace, under argon atmospher, ribbon was annealed 4 hours under 300 ℃.
The preparation ion cathode material lithium
Add the material of following mass parts in the ball mill:
Above-mentioned alloy band 60
Polyimide paint powder 7
Conductive agent acetylene black 10
Cross 100 mesh sieves after above-mentioned material ground, fully mix and be dissolved in the N methyl pyrrolidone (NMP) and be mixed with uniform slurry, obtain the silica-based lithium ion battery negative material of aluminium.
Comparative example
Al-si-based alloy is that the iron of 67% aluminium, 30% silicon and 3% or the chromium of 3% cobalt or 3% nickel or 3% form by weight ratio, and the alloy raw material of above-mentioned preparation is prepared into ingot casting with common casting method after being smelted into uniform alloy being heated to 800 ℃-1000 ℃ under vacuum or the 0.1MPa ar gas environment with electric induction furnace; Ingot casting secondary fusion and be heated to 800 ℃-1000 ℃ in the fast melt-quenching stove of vacuum or 0.1MPa protective atmosphere condition; prepare strip or powder with melt-quenching method; the strip that melt-quenching method is prepared or powder ball milling in the aviation gasoline medium becomes size less than 50 microns powder; afterwards alloy powder is fully mixed with conductive agent acetylene black and polyvinylidene fluoride (PVDF) powder and be dissolved in the 1-METHYLPYRROLIDONE (NMP) and be mixed with uniform slurry, obtain the silica-based lithium ion battery negative material of aluminium.
With synthetic embodiment one, two and the sample of comparative example present embodiment gained lithium ion battery negative material is applied on the Copper Foil collector, be pressed into cathode pole piece after the vacuumize, put into battery case with the positive plate that contains lithium, organic barrier film, electrolyte etc., be assembled into lithium ion chargeable battery.Carry out battery performance test, battery testing charging and discharging currents density is 20mA/g, and voltage range is 2.0-4.8V, and selecting temperature is 25 ℃ of normal temperature tests.After tested this embodiment one with two material compare with the material of comparative example, first discharge specific capacity has promoted more than the 60-70%, cycle life has improved more than 1.5 times.
More than specific embodiments of the invention are described in detail, but it is just as example, the present invention is not restricted to specific embodiment described above.To those skilled in the art, any equivalent modifications that the present invention is carried out and substituting also all among category of the present invention.Therefore, not breaking away from impartial conversion and the modification of doing under the spirit and scope of the present invention, all should contain within the scope of the invention.
Claims (4)
1. the preparation method of the silica-based lithium ion battery negative material of aluminium is characterized in that, comprises the steps:
Step 1 is prepared alloy raw material
According to molecular formula Si
50Al
13Mg
5Ni
2Sn
9Ga
5In the mol ratio of each element prepare alloy raw material;
Step 2, the molten alloy raw material
The alloy raw material of above-mentioned preparation is had in the arc furnace of argon filling of copper burner hearth melting and make ingot bar under vacuum or 0.1MPa ar gas environment, wherein the temperature of melting is 1800-2000 ℃;
Step 3 is made the alloy band
After being placed into the ingot bar bar in the crucible, system is vacuumized 0.01-0.1MPa, and then be filled with argon gas to 0.1-1MPa, come the melting ingot bar with radio frequency induction, when temperature reaches 1500-1600 ℃, the argon pressure of 2-4MPa is applied to the alloy composite surface of melting, and with alloy composite by nozzle be expressed into rotary speed be 6000-8000 rev/min the rotation cooling wheel above, the ribbon width that forms is 1-2mm, thickness is the alloy band of 5-10 micron, in tube furnace, under argon atmospher, ribbon was annealed 2-4 hour under 250-300 ℃;
Step 4, the preparation ion cathode material lithium
Add the material of following mass parts in the ball mill:
Above-mentioned alloy band 50-60
Polyimide paint powder 5-7
Conductive agent acetylene black 8-10
Cross 100 mesh sieves after above-mentioned material ground, fully mix and be dissolved in and be mixed with uniform slurry in the 1-METHYLPYRROLIDONE, obtain the silica-based lithium ion battery negative material of aluminium.
2. method according to claim 1 is characterized in that, in the step 1, aluminium, silicon, magnesium, nickel, tin adopt the simple substance element of purity 99.9wt%.
3. method according to claim 1 is characterized in that, it is the above rare earth Ga element of 99.5wt% that Ga adopts purity.
4. the silica-based lithium ion battery negative material of aluminium of the method for claim 1 preparation.
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| CN201210358755XA CN102891296A (en) | 2012-09-25 | 2012-09-25 | Method for preparing cathode material of aluminum-silicon-based lithium ion battery |
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| CN201210358755XA CN102891296A (en) | 2012-09-25 | 2012-09-25 | Method for preparing cathode material of aluminum-silicon-based lithium ion battery |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105406074A (en) * | 2015-12-09 | 2016-03-16 | 江苏科技大学 | Secondary ion battery with graphene composite electrode as positive electrode and preparation method |
| CN106532025A (en) * | 2016-12-16 | 2017-03-22 | 天津理工大学 | Preparation method and application of porous negative electrode material for lithium-ion battery |
| WO2017190587A1 (en) * | 2016-05-02 | 2017-11-09 | 北京工业大学 | Method for preparing lithium ion battery silicon anode through combination of diffusion welding and dealloying with laser surface remelting technique |
| CN109811227A (en) * | 2019-02-02 | 2019-05-28 | 拓米(成都)应用技术研究院有限公司 | It is used to prepare the silicon stannum alloy block and its preparation method and application of lithium cell cathode material |
| CN110085851A (en) * | 2019-05-20 | 2019-08-02 | 拓米(成都)应用技术研究院有限公司 | A kind of lithium battery is containing silicon stannum alloy cathode material and preparation method thereof |
-
2012
- 2012-09-25 CN CN201210358755XA patent/CN102891296A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105406074A (en) * | 2015-12-09 | 2016-03-16 | 江苏科技大学 | Secondary ion battery with graphene composite electrode as positive electrode and preparation method |
| WO2017190587A1 (en) * | 2016-05-02 | 2017-11-09 | 北京工业大学 | Method for preparing lithium ion battery silicon anode through combination of diffusion welding and dealloying with laser surface remelting technique |
| CN106532025A (en) * | 2016-12-16 | 2017-03-22 | 天津理工大学 | Preparation method and application of porous negative electrode material for lithium-ion battery |
| CN106532025B (en) * | 2016-12-16 | 2019-05-17 | 天津理工大学 | A kind of preparation method and application of the porous negative electrode material of lithium ion battery |
| CN109811227A (en) * | 2019-02-02 | 2019-05-28 | 拓米(成都)应用技术研究院有限公司 | It is used to prepare the silicon stannum alloy block and its preparation method and application of lithium cell cathode material |
| CN110085851A (en) * | 2019-05-20 | 2019-08-02 | 拓米(成都)应用技术研究院有限公司 | A kind of lithium battery is containing silicon stannum alloy cathode material and preparation method thereof |
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Application publication date: 20130123 |