CN102891297B - 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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- Y02E60/10—Energy storage using batteries
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 cathode material of lithium ion battery and preparation method thereof, particularly relate to a kind of Silicon-carbon composite material for lithium ion battery 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 current new energy field.The negative material of Current commercial lithium ion battery is generally material with carbon element, there is low and stably operating potential and good cycle performance, but the specific capacity of material with carbon element is on the low side (such as, graphite theoretical specific capacity is 372mAh/g), which has limited its application as high-energy-density power supply.Silicon is owing to having larger theoretical specific capacity (4200mAh/g) and lower intercalation potential and causing extensive concern.But silicon materials high level de-/embedding lithium under, there is serious bulk effect, easily cause coming off of the structural breakdown of material and active material, cyclical stability is declined greatly.Therefore, while guarantee silicon materials height ratio capacity, the emphasis that its cycle performance is research is improved.At present, the cycle performance of silicon materials is improved mainly through the following aspects: (1) reduces particle size; (2) silicon thin film is prepared; (3) prepare silicon based composite material, utilize the cooperative effect buffering of each component of composite material or the change in volume of restriction silicon, reach the optimization of material property, high temperature solid-state method, high-energy ball milling method, vapour deposition process are the methods that researcher commonly uses; (4) nano material of special construction is prepared, by preparing special construction nano material, as silicon nanowire material, core-shell type material, spherical silicon/graphite composite material, nido nano material etc., the pattern of material is kept in cyclic process, thus improves the cycle performance of electrode.
In sum, what be hopeful most to realize industrial applications is silicon/graphite/carbon composite material.From existing documents and materials, after the composite material that great majority are reported circulates tens weeks, specific capacity is down to 450 below mAh/g, can not fully demonstrate the feature of silica-base material high power capacity.Patent of the present invention is by liquid phase coating spray drying granulation legal system for silicon/graphite/carbon composite material, and empirical tests excellent material performance, can meet market demand.
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 to be binding agent, Liquid Coating Technology is utilized to carry out silicon-carbon compound, simultaneously by spray drying technology drying-granulating, be prepared into the Silicon-carbon composite material for lithium ion battery of epigranular, excellent performance.
Silicon-carbon composite material for lithium ion battery of the present invention and preparation method thereof, its feature comprises the following steps:
The first step: liquid phase ball milling is coated: be 99.99% by purity, granularity is the silica flour of 1-100 μm, add that granularity is 5-55 μm, purity is the graphite of more than 99.9% simultaneously, two kinds of mass ratioes are 10/1≤Msi/Mc≤1/10, then the soft pitch of 3% ~ 10% is added, softening point is 50-150 DEG C, silica flour, graphite, pitch are added in the sodium carboxymethyl cellulose solution of 5%-30% percentage by weight, the solid content adjusting slurry with water is 10% ~ 40%, then under argon gas atmosphere protection, mechanical high-energy ball milling, to 10-100nm, obtains nano silicone carbon composite slurry;
Second step: spray drying granulation: the nano silicone carbon composite slurry prepared is poured in drying machine with centrifugal spray, adjustment drying machine with centrifugal spray temperature is 150 DEG C, and adjusts wind speed by the granularity D50 of drying-granulating at 15-20 μm;
3rd step: carbonization: spray drying granulation gained Si-C composite material is sent into tunnel cave, under nitrogen atmosphere protection, carries out carbonization treatment at 700-1200 DEG C, obtains required Si-C composite material.
Described graphite comprises micro crystal graphite, the Delanium after high temperature graphitization, MCMB after spherical natural flake graphite, high temperature purification.
Advantage of the present invention is: 1, adopt silicon-carbon complex technique to prepare lithium ion battery composite material, Capacity Ratio conventional graphite negative material is high, reaches more than 500mAh/g, can meet growing lithium ion battery market demand; 2, adopt carboxymethyl cellulose as binding agent, can effective coated silicon bonded material with carbon element, prevent the powder phenomenon-tion that silicon causes in charge and discharge process, effectively improve the cycle performance of Si-C composite material; 3, adopt liquid phase coating, spray drying granulation technology, the even coated silicon bonded material with carbon element of energy, uniform particles, specific area is little, improves the cycle performance of Si-C composite material further.
Embodiment
Embodiment 1
1, pour in mixer by 0.2kg sodium carboxymethylcellulose and 20L water, high-speed stirred 2 hours, obtains sodium carboxymethylcellulose glue.
2, glue is poured in mechanical high energy ball mill; simultaneously by 8kg granularity D50=11-13 μm, the spherical artificial graphite of purity 99.96%; 2kg granularity D50=4-5 μm, the silica flour of purity 99.99%; 0.1kg softening point is that the soft pitch of 80 DEG C is poured in mechanical high energy ball mill; ball milling 3 hours under argon gas atmosphere protection, and test material granularity is at below 100nm.
3, sent in drying machine with centrifugal spray by slurry good for ball milling, centrifugal spray drying granulation at 150 DEG C, and the granularity and the specific area that detect particle, granularity is at D50=15-19 μm, and specific area is at below 4m2/g.
4, then material good for spray drying granulation is carbonized process at nitrogen protection 1150 DEG C, processing time 5h.
5, the material carbonized is cooled to room temperature, screening packaging, 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) (1min) is left standstill
(C) constant current charge (0.2mA, 2.000V)
7, resultant battery cycle performance 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) (5min) is left standstill
(C) constant current charge (1C, 3.0V)
4) circulate 200 its discharge capacitances of detection
Testing result is in table 1
Embodiment 2
1, pour in mixer by 0.2kg sodium carboxymethylcellulose and 20L water, high-speed stirred 2 hours, obtains sodium carboxymethylcellulose glue.
2, glue is poured in mechanical high energy ball mill; simultaneously by 6kg granularity D50=11-13 μm, the spherical artificial graphite of purity 99.95%; 4kg granularity D50=4-5 μm, the silica flour of purity 99.99%; 0.1kg softening point is that the soft pitch of 80 DEG C is poured in mechanical high energy ball mill; ball milling 3 hours under argon gas atmosphere protection, and test material granularity is at below 100nm.
3, sent in drying machine with centrifugal spray by slurry good for ball milling, centrifugal spray drying granulation at 150 DEG C, and the granularity and the specific area that detect particle, granularity is at D50=15-19 μm, and specific area is at below 4m2/g.
4, then material good for spray drying granulation is carbonized process at nitrogen protection 1150 DEG C, processing time 5h.
5, the material carbonized is cooled to room temperature, screening packaging, 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) (1min) is left standstill
(C) constant current charge (0.2mA, 2.000V)
Testing result is in table 1
Embodiment 3
1, pour in mixer by 0.2kg sodium carboxymethylcellulose and 20L water, high-speed stirred 2 hours, obtains sodium carboxymethylcellulose glue.
2, glue is poured in mechanical high energy ball mill; simultaneously by 8kg granularity D50=11-13 μm, the micro crystal graphite of purity 99.95%; 2kg granularity D50=4-5 μm, the silica flour of purity 99.99%; 0.1kg softening point is that the soft pitch of 80 DEG C is poured in mechanical high energy ball mill; ball milling 3 hours under argon gas atmosphere protection, and test material granularity is at below 100nm.
3, sent in drying machine with centrifugal spray by slurry good for ball milling, centrifugal spray drying granulation at 150 DEG C, and the granularity and the specific area that detect particle, granularity is at D50=15-19 μm, and specific area is at below 4m2/g.
4, then material good for spray drying granulation is carbonized process at nitrogen protection 1150 DEG C, processing time 5h.
5, the material carbonized is cooled to room temperature, screening packaging, 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) (1min) is left standstill
(C) constant current charge (0.2mA, 2.000V)
Testing result is in table 1
Embodiment 4
1, pour in mixer by 0.2kg sodium carboxymethylcellulose and 20L water, high-speed stirred 2 hours, obtains sodium carboxymethylcellulose glue.
2, glue is poured in mechanical high energy ball mill; simultaneously by 8kg granularity D50=15-17 μm, the Delanium of purity 99.98%; 2kg granularity D50=4-5 μm, the silica flour of purity 99.99%; 0.1kg softening point is that the soft pitch of 80 DEG C is poured in mechanical high energy ball mill; ball milling 3 hours under argon gas atmosphere protection, and test material granularity is at below 100nm.
3, sent in drying machine with centrifugal spray by slurry good for ball milling, centrifugal spray drying granulation at 150 DEG C, and the granularity and the specific area that detect particle, granularity is at D50=15-19 μm, and specific area is at below 4m2/g.
4, then material good for spray drying granulation is carbonized process at nitrogen protection 1150 DEG C, processing time 5h.
5, the material carbonized is cooled to room temperature, screening packaging, 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) (1min) is left standstill
(C) constant current charge (0.2mA, 2.000V)
Testing result is in table 1
Embodiment 4
1, pour in mixer by 0.2kg sodium carboxymethylcellulose and 20L water, high-speed stirred 2 hours, obtains sodium carboxymethylcellulose glue.
2, glue is poured in mechanical high energy ball mill; simultaneously by 8kg granularity D50=15-17 μm, the MCMB of purity 99.98%; 2kg granularity D50=4-5 μm, the silica flour of purity 99.99%; 0.1kg softening point is that the soft pitch of 80 DEG C is poured in mechanical high energy ball mill; ball milling 3 hours under argon gas atmosphere protection, and test material granularity is at below 100nm.
3, sent in drying machine with centrifugal spray by slurry good for ball milling, centrifugal spray drying granulation at 150 DEG C, and the granularity and the specific area that detect particle, granularity is at D50=15-19 μm, and specific area is at below 4m2/g.
4, then material good for spray drying granulation is carbonized process at nitrogen protection 1150 DEG C, processing time 5h.
5, the material carbonized is cooled to room temperature, screening packaging, 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) (1min) is left standstill
(C) constant current charge (0.2mA, 2.000V)
Testing result is in table 1
Table 1
Claims (2)
1. the preparation method of a Silicon-carbon composite material for lithium ion battery, it is characterized in that adopting sodium carboxymethylcellulose to be binding agent, Liquid Coating Technology is utilized to carry out silicon-carbon compound, simultaneously by spray drying technology drying-granulating, be prepared into the Silicon-carbon composite material for lithium ion battery of epigranular, excellent performance; Its method step is as follows:
1) liquid phase ball milling is coated: be 99.99% by purity, granularity is the silica flour of 1-100 μm, add granularity is 5-55 μm simultaneously, purity is the graphite of more than 99.9%, two kinds of mass ratioes are 1/10≤Msi/Mc≤10/1, then the soft pitch of 3% ~ 10% is added, soft pitch softening point is 50-150 DEG C, by silica flour, graphite, pitch adds in the sodium carboxymethyl cellulose solution of 5% ~ 30% percentage by weight, the solid content adjusting slurry with water is 10%-40%, then argon gas atmosphere protection under mechanical high-energy ball milling to 10-100nm, obtained nano silicone carbon composite slurry,
2) spray drying granulation: pour in drying machine with centrifugal spray by the nano silicone carbon composite slurry prepared, adjustment drying machine with centrifugal spray temperature is 150 DEG C, and adjusts wind speed by the granularity D of drying-granulating
50at 15-20 μm;
3) carbonization: spray drying granulation gained Si-C composite material is sent into tunnel cave, under nitrogen atmosphere protection, carries out carbonization treatment at 700-1200 DEG C, obtains required Si-C composite material.
2. the preparation method of a kind of Silicon-carbon composite material for lithium ion battery according to claim 1, it is characterized in that described graphite comprise spherical natural flake graphite, high temperature purification after micro crystal graphite, the Delanium after high temperature graphitization, MCMB.
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