CN110148738A - A kind of preparation method of silicon-carbon composite powder material - Google Patents
A kind of preparation method of silicon-carbon composite powder material Download PDFInfo
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- CN110148738A CN110148738A CN201910511082.9A CN201910511082A CN110148738A CN 110148738 A CN110148738 A CN 110148738A CN 201910511082 A CN201910511082 A CN 201910511082A CN 110148738 A CN110148738 A CN 110148738A
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- H—ELECTRICITY
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- H01M10/00—Secondary cells; Manufacture thereof
- 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
- H01M4/386—Silicon or alloys based on silicon
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Abstract
The present invention provides a kind of preparation methods of silicon-carbon composite powder material, it is the following steps are included: silicon powder, graphite powder are added in ball mill after mixing, the grinding warehouse of ball mill is vacuumized and is passed through inert gas, recirculated cooling water is passed through into ball mill coolant jacket again, it sets milling parameters and carries out ball milling, ball milling terminates to obtain silicon-carbon composite powder material；Wherein, the mass ratio of the silicon powder and graphite powder is 1:1 ~ 1:9.Using technical solution of the present invention, preparation process is simple, and the period is short; at low cost, obtained silicon-carbon composite powder material is and environmental-friendly as lithium ion battery negative material specific discharge capacity with higher; no waste water and solvent generate, Yi Shixian scale industrial production.
Description
Technical field
The invention belongs to new energy and technical field of new material preparation more particularly to a kind of systems of silicon-carbon composite powder material
Preparation Method.
Background technique
Currently, commercialized lithium ion battery negative material is mainly graphite type material, studies have shown that graphite-like is negative
For the actual capacity of pole material very close to its theoretical capacity (372 MAhs/g), the space of promotion is extremely limited,
So exploitation high capacity, high performance ion cathode material lithium are extremely urgent.Silicon has as lithium ion battery negative material
Highest theoretical specific capacity (4200 MAhs/g), practical lithium storage content are 3579 MAhs/g, about graphite negative electrodes
10 times of material, it is considered to be most potential substitution graphite becomes next-generation lithium ion battery negative material.But silicon is as cathode
There are still defect, charge and discharge deintercalate lithium ions will cause very big volume expansion (about 300%) in the process for material.Silicon it is this
Volume change, which can generate mechanicals efforts, will cause the broken of particle, dusting, lead to the capacity sharp-decay of silicon materials, final table
It is now weaker cyclical stability.In view of the above-mentioned problems, there are two types of the solutions proposed, it, can one is particle size is reduced
To reduce the crackle of silicon particle, the granularity for reducing silicon particle is to reduce the necessary condition of stress, and generally known technology uses tens
The silicon powder of nanometer；Another kind is to prepare silicon composite granule, and studying at present more is silicon-carbon composite granule.It can effectively delay
Volume expansion of the silicon in charge and discharge process is solved, the method has been widely used for lithium ion battery negative material study on the modification and works as
In.
The preparation method of silicon-carbon composite granule mainly has wet process mechanical ball mill, chemical vapour deposition technique, spray drying at present
Method and high temperature pyrolytic cracking (HTP) etc..A kind of silicon-carbon composite cathode material of lithium ion battery of patent CN105895873A and preparation method thereof and
Inductively coupled plasma method is prepared nano silica fume with high energy wet ball grinding and mixed by introduction in, and mixed powder is combined
Organic carbon source dispersing agent, natural/artificial graphite with 1000 revs/min of high-speed stirreds, 60 minutes obtained suspensions, and be added go from
Sub- water is stirred 2 hours with 1500 revs/min, and silicon-carbon composite granule is made in heating anneal after being dried 3 hours with 700 degrees Celsius,
Specific capacity reaches 876 MAhs/g or more for the first time.A kind of carbon-coated nano silicon composite of patent CN106784732A and its system
It is introduced in Preparation Method and application and the silicon powder of surface oxidation is subjected to oxidized diffusion under 500~1300 degrees Celsius, then carry out carbon
Cladding, then removing oxide layer is removed with hydrofluoric acid solution immersion, the capacity of Si-C composite material obtained reaches 900 MAhs/g.It is vertical
The relevant disclosure of preparation method of current silicon-carbon composite granule is seen, although all having obtained Si-C composite material, there are one
Some insufficient, such as preparation process complexity, equipment requirement is higher, needs to be sintered technique in preparation process, wet ball grinding overlong time,
The problems such as energy consumption is high.
Summary of the invention
Against the above technical problems, the invention discloses a kind of preparation method of silicon-carbon composite powder material, simple process,
Period is short, Yi Shixian scale industrial production；No wastewater discharge in preparation process, it is at low cost.
In this regard, the technical solution adopted by the present invention are as follows:
A kind of preparation method of silicon-carbon composite powder material comprising following steps:
Silicon powder, graphite powder are added in ball mill after mixing, the grinding warehouse of ball mill is vacuumized and is passed through lazy
Property gas, then recirculated cooling water is passed through into ball mill coolant jacket, setting milling parameters carry out ball milling, and ball milling terminates to obtain
Silicon-carbon composite powder material；Wherein, the mass ratio of the silicon powder and graphite powder is 1:1~1:9.
Further, the mass ratio of the silicon powder and graphite powder is 1:9~6:4.
As a further improvement of the present invention, the median particle size D50 of the graphite powder is 5~20 microns；The silicon powder
Median particle size D50 is 200-500 nanometers.Further, the median particle size D50 of the graphite powder is 10 microns.
As a further improvement of the present invention, the mass ratio of abrasive media and silicon-carbon powder is (10- in the ball mill
20):1。
As a further improvement of the present invention, the abrasive media in the ball mill is zirconium oxide, bearing steel ball or carbon
At least one of SiClx.
As a further improvement of the present invention, the graphite powder is natural flake graphite, artificial graphite, carbonaceous mesophase spherules
At least one of.
As a further improvement of the present invention, the inert gas is one of nitrogen, argon gas, carbon dioxide.
As a further improvement of the present invention, the technological parameter of ball milling includes: first pre-grinding, and pre- time consuming is 3~15 minutes,
Agitator shaft speed is 400~600 revs/min when pre-grinding；Ball milling again, Ball-milling Time are 40~80 minutes, and agitator shaft speed is
800/900~1000/1100 rev/min；It finally cools down, cooling time is 5~15 minutes, and agitator shaft speed is 300~500
Rev/min, revolving speed uses 1 minute alternation.Wherein, it is 800 revs/min and 900 revs/min every that 800/900 rev/min, which is revolving speed,
1 minute alternation 1 time, 1000/1100 rev/min for 1000 revs/min with 1100 revs/min every 1 minute alternation 1 time.
As a further improvement of the present invention, the ball mill is Horizontal stirring ball mill, the level of the ball mill
A horizontal agitating shaft is equipped in warehouse, agitating shaft is equipped with 5 groups of stirring blades.The ball mill uses horizontal high-energy stirring
Ball mill, the equipment are mainly made of horizontally disposed grinding storehouse, control system and motor part, and grinding warehouse therein is one
A closed warehouse.
As a further improvement of the present invention, it is passed through recirculated cooling water into ball mill coolant jacket, makes to grind the interior of warehouse
Wall temperature is 15-25 DEG C.It is passed through recirculated cooling water in the condenser that grinding warehouse is externally provided with, the condensate temperature for grinding warehouse is
15-25℃。
Compared with prior art, the invention has the benefit that
Technical solution of the present invention uses dry type high-energy ball milling method, and Ball-milling Time is short, and 20-100 minutes, technological operation letter
It is single, the high temperature sintering and drying process of powder have been got rid of, energy consumption is lowered.Silicon-carbon is wherein prepared using 200-500 nanometers of silicon powder
The negative electrode material electrical property of composite granule preparation reaches generally known technology using 100 nanometers of nano silica fumes below, in this way may be used
The cost of lithium ion battery negative material is greatly reduced；Silicon-carbon ratio is 1:1~1:9, and the silicone content of powder is greater than 10%, one
As well-known technique silicone content 10% hereinafter, compared with prior art have advance.
The silicon-carbon composite powder material that technical solution of the present invention obtains is with higher as lithium ion battery negative material
Specific discharge capacity.In addition, this preparation method is environmental-friendly, wet ball grinding preparation process is substituted using dry ball milling technique, without useless
Water and solvent generate.
Detailed description of the invention
Fig. 1 is the SEM figure of silicon-carbon composite granule made from the embodiment of the present invention 1.
Fig. 2 is the TEM figure of silicon-carbon composite granule made from the embodiment of the present invention 1.
Specific embodiment
Preferably embodiment of the invention is described in further detail below.
Embodiment 1
A kind of preparation method of silicon-carbon composite powder material, comprising the following steps:
(1) artificial graphite that partial size is 200 nanometers in 30 grams silicon powder, 70 grams of medians are 10 microns is selected, mutually
It is added in high energy ball mill cabin after mixing.
(2) 2 kilograms of bearing steel ball is added into ball mill cabin, grinding cabin is passed through carbon dioxide gas after vacuumizing
Body, cooling water temperature are 15 DEG C.Set technological parameter are as follows: pre-grinding 5 minutes under conditions of revolving speed is 400 revs/min, when ball milling
Between be 40 minutes, agitator shaft speed is 1000/1100 rev/min, and cooling revolving speed is 300 revs/min, and cooling time is 10 points
Clock.Start to grind work until program operation finishes.
Discharge port lid is opened, silicon-carbon composite granule and abrasive media are taken out, with sieve separation abrasive media and composite granule,
The meso-position radius D of silicon-carbon composite granule50It is 4.5 microns, tap density 0.83g/cm3。
Silicon-carbon composite granule obtained is assembled into lithium ion battery negative material, detects its electrical property, silicon-carbon composite wood
The specific discharge capacity of material is 3145 MAhs/g, and coulombic efficiency is 93.9% for the first time.Fig. 1 and Fig. 2 is that embodiment 1 produces respectively
SEM, TEM of product scheme, and obtained diameter of particle is small, is uniformly dispersed.
Embodiment 2
A kind of preparation method of silicon-carbon composite powder material, comprising the following steps:
(1) natural flake graphite that silicon powder, 90 gram particle diameters that 10 gram particle diameters are 500 nanometers are 10 microns is selected, it is mutually mixed
It is added in high energy ball mill cabin after closing uniformly；
(2) 1.5 kilograms of zirconia balls are added into ball mill cabin, grinding cabin is passed through nitrogen, cooling water after vacuumizing
Temperature is 20 DEG C.Pre-grinding 8 minutes under conditions of revolving speed is 500 revs/min, Ball-milling Time is 60 minutes, and agitator shaft speed is
800/900 rev/min, cooling revolving speed is 400 revs/min, and the time is 5 minutes.Start to grind work until program operation finishes.
Silicon-carbon composite granule and abrasive media are taken out, with sieve separation abrasive media and composite granule, silicon-carbon composite granule
Partial size D50It is 4.10 microns, tap density 1.05g/cm3。
Silicon-carbon composite granule obtained is assembled into lithium ion battery negative material, detects its electrical property, silicon-carbon composite wood
The specific discharge capacity of material is 2932 MAhs/g, and coulombic efficiency is 88.5% for the first time.
Embodiment 3
(1) selecting 100 gram particle diameters is 300 nano silica fumes, 10 microns of 100g partial size of carbonaceous mesophase spherules, is mutually mixed
It is added in high energy ball mill warehouse after even.
(2) 2 kilograms of carbonization silicon ball is added into ball mill cabin, grinding cabin is passed through argon gas, cooling water after vacuumizing
Temperature is 25 DEG C.Pre-grinding 3 minutes under conditions of revolving speed is 600 revs/min, Ball-milling Time is 80 minutes, agitator shaft speed is
900/1000 rev/min, cooling revolving speed is 500 revs/min, and the time is 10 minutes.Start to grind work until program has been run
Finish.
Silicon-carbon composite granule and abrasive media are taken out, with sieve separation abrasive media and composite granule, silicon-carbon composite granule grain
Diameter D50It is 3.6 microns, tap density 0.80g/cm3。
Silicon-carbon composite granule obtained is assembled into lithium ion battery negative material, detects its electrical property, silicon-carbon composite wood
The specific discharge capacity of material is 3078 MAhs/g, and coulombic efficiency is 90.8% for the first time.
Comparative example 1
It is essentially identical with the preparation process of embodiment 1, it is unique the difference is that granularity is 500 in silicon powder when preparing composite granule
Nanometer.
Comparative example 2
It is essentially identical with the preparation process of embodiment 1, it is unique the difference is that granularity is 800 in silicon powder when preparing composite granule
Nanometer.
Comparative example 3
It is essentially identical with the preparation process of embodiment 1, it is unique the difference is that granularity is in silicon powder when preparing composite granule
1000 nanometers.
Comparative example 4
It is essentially identical with the preparation process of embodiment 1, it is unique the difference is that silicon powder content is 10% when preparing composite granule.
Comparative example 5
It is essentially identical with the preparation process of embodiment 1, it is unique the difference is that silicon powder content is 50% when preparing composite granule.
Comparative example 6
It is essentially identical with the preparation process of embodiment 1, it is unique the difference is that silicon powder content is 70% when preparing composite granule.
Comparative example 7
It is essentially identical with the preparation process of embodiment 1, it is unique the difference is that Ball-milling Time 100 divides when preparing composite granule
Clock.
Comparative example 8
It is essentially identical with the preparation process of embodiment 1, it is unique the difference is that Ball-milling Time 120 divides when preparing composite granule
Clock.
Comparative example 9
It is essentially identical with the preparation process of embodiment 1, it is unique the difference is that agitating shaft turns when ball milling when preparing composite granule
Speed is 1100/1200 rev/min.
Comparative example 10
It is essentially identical with the preparation process of embodiment 1, it is unique the difference is that agitating shaft turns when ball milling when preparing composite granule
Speed is 1200/1300 rev/min.
Granularity, tap density and specific discharge capacity in the product progress of embodiment 1-3 and comparative example 1-10 preparation are carried out
Detection, as a result as shown in table 1 below.
Table 1
As seen from the above table, embodiment 1-3 and comparative example 2,3,9,10 prepare silicon-carbon composite granule and ion cathode material lithium
Specific discharge capacity and circulation conservation rate data, the D of embodiment 1-350, tap density, initial discharge specific capacity and coulomb for the first time
Efficiency is all remarkably higher than comparative example 2,3,9,10；It is simultaneously optimum embodiment by the visible embodiment 1 of data of embodiment 1-3.
When by the data of embodiment 1 and comparative example 1-3 as it can be seen that preparing that granularity is greater than 500 nanometers in the silicon powder of composite granule,
The tap density of the silicon-carbon cathode material of lithium ion battery, specific discharge capacity are significantly reduced with coulombic efficiency data for the first time, explanation
Silicon medium silt degree D50Control has unexpected technical effect, silicon-carbon composite granule preparation of the invention at 200-500 nanometers
Negative electrode material have excellent electrical property.
By the data of embodiment 1 and comparative example 4-6 as it can be seen that preparing the silicon powder content of composite granule at 10,50,70%,
Although the initial discharge specific capacity of silicon-carbon cathode material is higher when silicone content 70%, coulombic efficiency sharply declines for the first time, existing
The general silicon-carbon cathode material silicone content of well-known technique can only be added to 10% and hereinafter, this technology silicone content is compound in 30% silicon-carbon
The negative electrode material of powder preparation has excellent electrical property.
By embodiment 1 and the data of comparative example 7-8 as it can be seen that preparing Ball-milling Time in the ball-milling technology of composite granule is greater than 80
Minute, the tap density of silicon-carbon composite granule, the initial discharge specific capacity of silicon-carbon composite cathode material of lithium ion battery with for the first time
Coulombic efficiency significantly reduces, and illustrates there is unexpected technical effect when Ball-milling Time is 40-80 minutes.
Turned by embodiment 1 and the data of comparative example 9-10 as it can be seen that preparing ball grinding stirring axis in the ball-milling technology of composite granule
Speed is more than 1000/1100 rev/min, and initial discharge specific capacity and the coulombic efficiency for the first time of composite material significantly reduce, therefore
Agitator shaft speed, which is maintained at 800/900~1000/1100 rev/min, in milling parameters unexpected technical effect.
The above content is a further detailed description of the present invention in conjunction with specific preferred embodiments, and it cannot be said that
Specific implementation of the invention is only limited to these instructions.For those of ordinary skill in the art to which the present invention belongs, exist
Under the premise of not departing from present inventive concept, a number of simple deductions or replacements can also be made, all shall be regarded as belonging to of the invention
Protection scope.
Claims (10)
1. a kind of preparation method of silicon-carbon composite powder material, it is characterised in that: itself the following steps are included:
Silicon powder, graphite powder are added in ball mill after mixing, the grinding warehouse of ball mill is vacuumized and are passed through indifferent gas
Body, then recirculated cooling water is passed through into ball mill coolant jacket, setting milling parameters carry out ball milling, and ball milling terminates to obtain silicon-carbon
Composite powder material.
2. the preparation method of silicon-carbon composite powder material according to claim 1, it is characterised in that: the silicon powder and graphite
The mass ratio of powder is 1:1 ~ 1:9.
3. the preparation method of silicon-carbon composite powder material according to claim 1, it is characterised in that: in the graphite powder
Position granularity D50 is 5 ~ 20 microns；The median particle size D of the silicon powder50It is 200-500 nanometers.
4. the preparation method of silicon-carbon composite powder material according to claim 1, it is characterised in that: ground in the ball mill
The mass ratio of grinding media and silicon-carbon powder is (10-20): 1.
5. the preparation method of silicon-carbon composite powder material according to claim 4, it is characterised in that: in the ball mill
Abrasive media is at least one of zirconium oxide, bearing steel ball or silicon carbide.
6. the preparation method of silicon-carbon composite powder material according to claim 1, it is characterised in that: to ball mill coolant jacket
In be passed through recirculated cooling water, make to grind 15-25 DEG C of inner wall temperature of warehouse.
7. the preparation method of silicon-carbon composite powder material according to claim 1, it is characterised in that: the graphite powder is day
At least one of right crystalline flake graphite, artificial graphite, carbonaceous mesophase spherules.
8. the preparation method of silicon-carbon composite powder material according to claim 1, it is characterised in that: the inert gas is
One of nitrogen, argon gas, carbon dioxide.
9. the preparation method of silicon-carbon composite powder material described in any one according to claim 1 ~ 8, it is characterised in that: ball milling
Technological parameter include: first pre-grinding, pre- time consuming is 3 ~ 15 minutes, and agitator shaft speed is 400 ~ 600 revs/min when pre-grinding；Again
Ball milling, Ball-milling Time are 40 ~ 80 minutes, and agitator shaft speed is 800/900 ~ 1000/1100 rev/min；Finally cool down, it is cooling
Time is 5 ~ 15 minutes, and agitator shaft speed is 300 ~ 500 revs/min, and revolving speed uses 1 minute alternation.
10. the preparation method of silicon-carbon composite powder material according to claim 9, it is characterised in that: the ball mill is
Horizontal stirring ball mill, the horizontal warehouse of the ball mill is interior to be equipped with a horizontal agitating shaft, and agitating shaft is equipped with 5 groups and stirs
Mix blade.
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| CN111900348A (en) * | 2020-07-14 | 2020-11-06 | 中国科学院山西煤炭化学研究所 | Method for preparing silicon-carbon composite material based on ball milling method and application thereof |
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