CN102891297A - Silicon-carbon composite material for lithium ion battery and preparation method thereof - Google Patents
Silicon-carbon composite material for lithium ion battery and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a silicon-carbon composite material for a lithium ion battery and a preparation method for the silicon-carbon composite material, and belongs to the field of lithium ion batteries. The silicon-carbon composite material is characterized in that carboxymethylcellulose sodium is used as a bonding agent, a liquid phase coating technology is used for silicon-carbon compounding, and a spray drying technology is used for drying granulation to prepare the silicon-carbon composite material with uniform granularity and excellent performance for the lithium ion battery. The silicon-carbon composite material and the preparation method thereof have the advantages that 1, the composite material for the lithium ion battery is prepared through a silicon-carbon compounding technology, and the capacity of the composite material is higher than that of the conventional graphite cathode material, reaches over 500mAh/g, and can meet requirements on the growing of the market of lithium ion batteries; 2, carboxymethylcellulose is used as a bonding agent which can be effectively coated and bonded on the silicon-carbon material to prevent efflorescence caused by silicon during charging and discharging, so that the cycling performance of the silicon-carbon composite material is effectively improved; and 3, the liquid phase coating and spray drying granulation technologies are adopted, so that the silicon-carbon material can be uniformly coated and bonded, has uniform granules, and is small in specific area, and the cycling performance of the silicon-carbon composite material is further improved.
Description
Technical field
The present invention relates to a kind of negative electrode for lithium ion battery material and preparation method thereof, relate in particular to a kind of lithium ion battery Si-C composite material and preparation method thereof.
Background technology
The advantages such as lithium ion battery is high with its operating voltage, energy density is large, environmental pollution is little become the study hotspot of present new energy field.The negative material of current commercial Li-ion battery generally is material with carbon element, have low and stably operating potential and good cycle performance, but the specific capacity of material with carbon element is on the low side (for example, the graphite theoretical specific capacity is 372mAh/g), and this has limited its application as the high-energy-density power supply.Silicon is owing to having larger theoretical specific capacity (4200mAh/g) and lower embedding lithium current potential causes extensive concern.But silicon materials take off in high level/the embedding lithium under, exist serious bulk effect, easily cause the structural breakdown of material and coming off of active material, so that cyclical stability descends greatly.Therefore, when guaranteeing the silicon materials height ratio capacity, improving its cycle performance is the emphasis of research.At present, mainly improve the cycle performance of silicon materials by the following aspects: (1) reduces particle size; (2) preparation silicon thin film; (3) preparation silicon based composite material utilizes the cooperative effect buffering of each component of composite material or the change in volume of restriction silicon, reaches the optimization of material property, and high temperature solid-state method, high-energy ball milling method, vapour deposition process are the methods that the researcher commonly uses; (4) nano material of preparation special construction, by preparation special construction nano material, such as silicon nanowire material, core-shell type material, spherical silicon/graphite composite material, nido nano material etc., so that the pattern of material kept, thereby improve the cycle performance of electrode in cyclic process.
What in sum, be hopeful most to realize industrial applications is silicon/graphite/carbon composite material.From existing documents and materials, the composite materials of great majority reports circulated after tens weeks, and specific capacity is down to below 450 mAh/g, can not demonstrate fully the characteristics of silica-base material high power capacity.Patent of the present invention is by the standby silicon of liquid phase coating spray drying granulation legal system/graphite/carbon composite material, and the empirical tests excellent material performance can need by satisfying the market.
Summary of the invention
The object of the present invention is to provide a kind of silicon-carbon composite cathode material of lithium ion battery and preparation method thereof, it is characterized in that adopting sodium carboxymethylcellulose is binding agent, utilize Liquid Coating Technology to carry out silicon-carbon compound, by the spray drying technology drying-granulating, be prepared into the lithium ion battery Si-C composite material of epigranular, excellent performance simultaneously.
Lithium ion battery of the present invention Si-C composite material and preparation method thereof, its feature may further comprise the steps:
The first step: the liquid phase ball milling coats: with purity be 99.99%, granularity is the silica flour of 1-100 μ m, adding simultaneously granularity is that 5-55 μ m, purity are the graphite more than 99.9%, two kinds of mass ratioes are 10/1≤Msi/Mc≤1/10, then add 3% ~ 10% soft pitch, softening point is 50-150 ℃, silica flour, graphite, pitch are added in the sodium carboxymethyl cellulose solution of 5%-30% percentage by weight, the solid content that water is adjusted slurry is 10% ~ 40%, then mechanical high-energy ball milling makes nano silicone carbon composite slurry to 10-100nm under the argon gas atmosphere protection;
Second step: spray drying granulation: the nano silicone carbon composite slurry for preparing is poured in the drying machine with centrifugal spray, and adjusting the drying machine with centrifugal spray temperature is 150 ℃, and adjust wind speed with the granularity D50 of drying-granulating at 15-20 μ m;
The 3rd step: carbonization: spray drying granulation gained Si-C composite material is sent into tunnel cave, under the nitrogen atmosphere protection, carry out carbonization treatment at 700-1200 ℃, obtain required Si-C composite material.
Described graphite comprises micro crystal graphite, the Delanium behind the high temperature graphitization, the MCMB after spherical natural flake graphite, the high temperature purification.
Advantage of the present invention is: 1, adopt the silicon-carbon complex technique to prepare lithium ion battery composite material, Capacity Ratio conventional graphite negative material is high, reaches more than the 500mAh/g, can satisfy growing lithium ion battery market demand; 2, adopt carboxymethyl cellulose as binding agent, can effectively coat the silicon bonded material with carbon element, prevent the powder phenomenon-tion that silicon causes in charge and discharge process, the cycle performance of Effective Raise Si-C composite material; 3, adopt liquid phase coating, spray drying granulation technology, can evenly coat the silicon bonded material with carbon element, uniform particles, specific area is little, further improves the cycle performance of Si-C composite material.
Embodiment
Embodiment 1
1,0.2kg sodium carboxymethylcellulose and 20L water are poured in the mixer, high-speed stirred 2 hours obtains the sodium carboxymethylcellulose glue.
2, glue is poured in the mechanical high energy ball mill; simultaneously with the spherical Delanium of 8kg granularity D50=11-13 μ m, purity 99.96%; the silica flour of 2kg granularity D50=4-5 μ m, purity 99.99%; 0.1kg being 80 ℃ soft pitch, pours in the mechanical high energy ball mill softening point; ball milling is about 3 hours under argon gas atmosphere protection, and the test material granularity gets final product below 100nm.
3, the slurry that ball milling is good is sent in the drying machine with centrifugal spray, 150 ℃ of lower centrifugal spray drying granulations, and granularity and the specific area of detection particle, granularity is at D50=15-19 μ m, and specific area gets final product below 4m2/g.
4, then material that spray drying granulation is good is processed processing time 5h in 1150 ℃ of lower charings of nitrogen protection.
5, the material that charing is good is cooled to room temperature, and the screening packing obtains that silicon-carbon composite cathode material of required lithium ion battery.
6, the making of button cell and detection
1), electrolyte: 1M-LiPF6 EC/DMC/EMC
2), binding agent: LA-133:3%
3), conductive agent: Super-P: 3%
4), to electrode: pour lithium slice
5), discharge and recharge system
(A) constant-current discharge (0.2mA, 0.001V)
(B) leave standstill (1min)
(C) constant current charge (0.2mA, 2.000V)
7, finished product cycle performance of battery test
1) electrolyte: 1M-LiPF6 EC/DMC/EMC
2) positive electrode: LiCoO2
3) discharge and recharge system
(A) constant current charge (1C, 4.2V)
(B) leave standstill (5min)
(C) constant current charge (1C, 3.0V)
4) circulation 200 detects its discharge capacitance
Testing result sees Table 1
Embodiment 2
1,0.2kg sodium carboxymethylcellulose and 20L water are poured in the mixer, high-speed stirred 2 hours obtains the sodium carboxymethylcellulose glue.
2, glue is poured in the mechanical high energy ball mill; simultaneously with the spherical Delanium of 6kg granularity D50=11-13 μ m, purity 99.95%; the silica flour of 4kg granularity D50=4-5 μ m, purity 99.99%; 0.1kg being 80 ℃ soft pitch, pours in the mechanical high energy ball mill softening point; ball milling is about 3 hours under argon gas atmosphere protection, and the test material granularity gets final product below 100nm.
3, the slurry that ball milling is good is sent in the drying machine with centrifugal spray, 150 ℃ of lower centrifugal spray drying granulations, and granularity and the specific area of detection particle, granularity is at D50=15-19 μ m, and specific area gets final product below 4m2/g.
4, then material that spray drying granulation is good is processed processing time 5h in 1150 ℃ of lower charings of nitrogen protection.
5, the material that charing is good is cooled to room temperature, and the screening packing obtains that silicon-carbon composite cathode material of required lithium ion battery.
6, the making of button cell and detection
1), electrolyte: 1M-LiPF6 EC/DMC/EMC
2), binding agent: LA-133:3%
3), conductive agent: Super-P: 3%
4), to electrode: pour lithium slice
5), discharge and recharge system
(A) constant-current discharge (0.2mA, 0.001V)
(B) leave standstill (1min)
(C) constant current charge (0.2mA, 2.000V)
Testing result sees Table 1
Embodiment 3
1,0.2kg sodium carboxymethylcellulose and 20L water are poured in the mixer, high-speed stirred 2 hours obtains the sodium carboxymethylcellulose glue.
2, glue is poured in the mechanical high energy ball mill; simultaneously with the micro crystal graphite of 8kg granularity D50=11-13 μ m, purity 99.95%; the silica flour of 2kg granularity D50=4-5 μ m, purity 99.99%; 0.1kg being 80 ℃ soft pitch, pours in the mechanical high energy ball mill softening point; ball milling is about 3 hours under argon gas atmosphere protection, and the test material granularity gets final product below 100nm.
3, the slurry that ball milling is good is sent in the drying machine with centrifugal spray, 150 ℃ of lower centrifugal spray drying granulations, and granularity and the specific area of detection particle, granularity is at D50=15-19 μ m, and specific area gets final product below 4m2/g.
4, then material that spray drying granulation is good is processed processing time 5h in 1150 ℃ of lower charings of nitrogen protection.
5, the material that charing is good is cooled to room temperature, and the screening packing obtains that silicon-carbon composite cathode material of required lithium ion battery.
6, the making of button cell and detection
1), electrolyte: 1M-LiPF6 EC/DMC/EMC
2), binding agent: LA-133:3%
3), conductive agent: Super-P: 3%
4), to electrode: pour lithium slice
5), discharge and recharge system
(A) constant-current discharge (0.2mA, 0.001V)
(B) leave standstill (1min)
(C) constant current charge (0.2mA, 2.000V)
Testing result sees Table 1
Embodiment 4
1,0.2kg sodium carboxymethylcellulose and 20L water are poured in the mixer, high-speed stirred 2 hours obtains the sodium carboxymethylcellulose glue.
2, glue is poured in the mechanical high energy ball mill; simultaneously with the Delanium of 8kg granularity D50=15-17 μ m, purity 99.98%; the silica flour of 2kg granularity D50=4-5 μ m, purity 99.99%; 0.1kg being 80 ℃ soft pitch, pours in the mechanical high energy ball mill softening point; ball milling is about 3 hours under argon gas atmosphere protection, and the test material granularity gets final product below 100nm.
3, the slurry that ball milling is good is sent in the drying machine with centrifugal spray, 150 ℃ of lower centrifugal spray drying granulations, and granularity and the specific area of detection particle, granularity is at D50=15-19 μ m, and specific area gets final product below 4m2/g.
4, then material that spray drying granulation is good is processed processing time 5h in 1150 ℃ of lower charings of nitrogen protection.
5, the material that charing is good is cooled to room temperature, and the screening packing obtains that silicon-carbon composite cathode material of required lithium ion battery.
6, the making of button cell and detection
1), electrolyte: 1M-LiPF6 EC/DMC/EMC
2), binding agent: LA-133:3%
3), conductive agent: Super-P: 3%
4), to electrode: pour lithium slice
5), discharge and recharge system
(A) constant-current discharge (0.2mA, 0.001V)
(B) leave standstill (1min)
(C) constant current charge (0.2mA, 2.000V)
Testing result sees Table 1
Embodiment 4
1,0.2kg sodium carboxymethylcellulose and 20L water are poured in the mixer, high-speed stirred 2 hours obtains the sodium carboxymethylcellulose glue.
2, glue is poured in the mechanical high energy ball mill; simultaneously with the MCMB of 8kg granularity D50=15-17 μ m, purity 99.98%; the silica flour of 2kg granularity D50=4-5 μ m, purity 99.99%; 0.1kg being 80 ℃ soft pitch, pours in the mechanical high energy ball mill softening point; ball milling is about 3 hours under argon gas atmosphere protection, and the test material granularity gets final product below 100nm.
3, the slurry that ball milling is good is sent in the drying machine with centrifugal spray, 150 ℃ of lower centrifugal spray drying granulations, and granularity and the specific area of detection particle, granularity is at D50=15-19 μ m, and specific area gets final product below 4m2/g.
4, then material that spray drying granulation is good is processed processing time 5h in 1150 ℃ of lower charings of nitrogen protection.
5, the material that charing is good is cooled to room temperature, and the screening packing obtains that silicon-carbon composite cathode material of required lithium ion battery.
6, the making of button cell and detection
1), electrolyte: 1M-LiPF6 EC/DMC/EMC
2), binding agent: LA-133:3%
3), conductive agent: Super-P: 3%
4), to electrode: pour lithium slice
5), discharge and recharge system
(A) constant-current discharge (0.2mA, 0.001V)
(B) leave standstill (1min)
(C) constant current charge (0.2mA, 2.000V)
Testing result sees Table 1
Table 1
Claims (2)
1. a lithium ion battery is with the preparation method of Si-C composite material, it is characterized in that adopting sodium carboxymethylcellulose is binding agent, utilize Liquid Coating Technology to carry out silicon-carbon compound, by the spray drying technology drying-granulating, be prepared into the lithium ion battery Si-C composite material of epigranular, excellent performance simultaneously; Its method step is as follows:
1) the liquid phase ball milling coats: be 99.99% with purity, granularity is the silica flour of 1-100 μ m, adding simultaneously granularity is 5-55 μ m, purity is the graphite more than 99.9%, two kinds of mass ratioes are 10/1≤Msi/Mc≤1/10, then add 3%～10% soft pitch, the soft pitch softening point is 50-150 ℃, with silica flour, graphite, pitch adds in the sodium carboxymethyl cellulose solution of 5%～30% percentage by weight, the solid content that water is adjusted slurry is 10%-40%, then mechanical high-energy ball milling makes nano silicone carbon composite slurry to 10-100nm under the argon gas atmosphere protection;
2) spray drying granulation: the nano silicone carbon composite slurry for preparing is poured in the drying machine with centrifugal spray, and adjusting the drying machine with centrifugal spray temperature is 150 ℃, and adjust wind speed with the granularity D50 of drying-granulating at 15-20 μ m;
3) carbonization: spray drying granulation gained Si-C composite material is sent into tunnel cave, under the nitrogen atmosphere protection, carry out carbonization treatment at 700-1200 ℃, obtain required Si-C composite material.
2. described a kind of lithium ion battery is characterized in that micro crystal graphite, the Delanium behind the high temperature graphitization, MCMB after described graphite comprises spherical natural flake graphite, high temperature purification with the preparation method of Si-C composite material according to claim 1.
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