CN107623113A - A kind of porous long circulating silicon-carbon cathode material preparation method - Google Patents
A kind of porous long circulating silicon-carbon cathode material preparation method Download PDFInfo
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Abstract
The invention discloses a kind of porous long circulating silicon-carbon cathode material preparation method, comprise the following steps：（1）Silicon monoxide is milled to nanoscale；（2）By nanometer silicon monoxide by liquid phase coating carbon source, then dry and powder is made；（3）By step（2）Obtained powder, which is placed in atmosphere furnace, carries out charing process, obtains precursor powder；（4）By step（3）Obtained presoma powder carries out secondary liquid phase coating with carbon source, conductive agent, is then dried to powder；（5）By step（4）Obtained powder is placed in atmosphere furnace carries out charing process again；（6）By step（5）Obtained powder, which is placed in hydrofluoric acid, to be soaked, and is then filtered and is cleaned with distilled water to neutrality, 90 150oPowder is dried under the conditions of C, obtains porous long circulating silicon-carbon cathode material.The present invention can effectively improve the effect of coulomb first and cycle performance of negative material, and technique is simple, bad border is friendly, is advantageous to large-scale production.
Description
Technical field
The present invention relates to field of lithium technology, especially provides a kind of porous macrocyclic silicon-carbon cathode material preparation side
Method.
Background technology
Development course of the lithium ion battery from nineteen ninety, lithium ion battery turn into current portable electronic equipment（Such as
Mobile phone, digital camera and portable notebook）The main selection of power supply, it is also more and more extensive to be applied to electric automobile, mix and move
In the multiple fields such as power electric automobile, extensive energy storage, space technology, national defense industry, therefore, the capacity and energy density of battery
Urgently increase substantially, for meeting the needs of in each field.At present, the lithium ion battery of commercialization is mainly modified natural stone
Ink and Delanium are as negative material, but its theoretical specific capacity 372mA/g is relatively low, thus people for Novel high-specific capacity flexible,
The negative material of long circulation life is placed high hopes.
Silicon based anode material theoretical capacity is up to 4200mA/g and relatively low discharge platform gets more and more people's extensive concerning.
Compare popular silicon monoxide negative material, although the reversible capacity of the material will be less than silicium cathode material, it fills in electrode
Bulk effect in discharge process will be significantly less than silicon materials, therefore attract the pass of lithium ion battery negative material researchers
Note, but silicon monoxide material still has a certain degree of bulk effect, so be also required to be improved the performance of material at place
Reason.Disproportionation processing to material is to improve a kind of important means of silicon monoxide material performance, passes through disproportionation, the transformation of SiO materials
For SiO2And Si, SiO2Performance is particularly stable, and Si then has higher capacity.SiO2During the dilation of material, by
In the stability of its structure, shell can be played a part of, so as to effectively slow down the dilatancy of material, so in discharge and recharge
During expansion-contraction, heavy damage will not occur for the skeleton of electrode material, so the efflorescence that can effectively slow down electrode is made
With reducing the loss of electrode capacity, improve the cyclical stability of electrode, simultaneously as adjoint generations of the Si in disproportionation, electric
The capacity of pole can also improve.However, although disproportionation can improve the performance of electrode to a certain extent, effect has
Limit, so researchers further alleviate the bulk effect of material further through the means that carbon coating is carried out to SiO negative materials.Mesh
Preceding the most frequently used means are uniformly to be mixed SiO materials with pitch, then pitch is carried out into high temperature pyrolysis, so as to produce pyrolysis
Carbon coats to SiO materials, but long-term stable circulation performance, first coulombic efficiency and volumetric properties still have much room for improvement.
Patent CN 106299323A disclose a kind of hollow cladding silicon-carbon cathode material preparation method, the material preparation side
Method comprises the following steps（1）By the silicon monoxide for coating carbon source by spray drying granulation, under an inert atmosphere, it is heated at high temperature
To the silicon and silica generated by silicon monoxide disproportionated reaction；（2）Silica is fallen by hydrofluoric acid etch, obtains hollow bag
The silicon-carbon cathode material covered.Though the silicon-carbon cathode material alleviates efflorescence of the active material in charge and discharge process to a certain extent
Obscission, Volumetric expansion make moderate progress, but the effect of material cladding need to be improved, and material cycle performance is still
It is not good enough, and its first charge-discharge efficiency only has 85% or so, and commercialized degree is still difficult.
The content of the invention
The present invention proposes a kind of porous macrocyclic silicon-carbon cathode material preparation method to solve above technical problem,
Loose structure alleviate nano-silicon Volumetric expansion, and using in batches it is secondary cladding cause silicon monoxide or silicon cladding it is completeer
Entirely, conductive agent is added during cladding, the effect of coulomb first and cycle performance of negative material, the preparation method work can be effectively improved
Skill is simple, bad border is friendly, is advantageous to large-scale production.
The object of the present invention is achieved like this：A kind of porous macrocyclic silicon-carbon cathode material preparation method, includes
Following steps.
（1）Silicon monoxide and solvent are placed in planetary ball mill, wet method ball is carried out under rotating speed 100-400r/min
5-18h is ground, in 90-150 after ball millingo4-12h is dried under the conditions of C, obtains nanoscale silicon monoxide powder.
（2）By step（1）Nanometer silicon monoxide powder, solvent and the carbon source of processing, which are placed in homogenizer, carries out liquid phase
Cladding, stirs 3-6h, then in 90-150 under rotating speed 600-1200r/mino4-12h is dried under the conditions of C and powder is made.
（3）By step（2）Obtained powder, which is placed in atmosphere furnace, carries out charing process, with 5-10oC/min heating rate
Rise to 600-1100oC is simultaneously incubated 5-10h, obtains precursor powder.
（4）By step（3）Obtained presoma powder is placed in homogenizer with carbon source, conductive agent, solvent and carries out two
Secondary liquid phase coating, 3-6h is stirred under rotating speed 600-1200r/min, then in 90-150o4-12h is dried under the conditions of C and is made
Powder.
（5）By step（4）Obtained powder is placed in atmosphere furnace carries out charing process again, with 5-10oC/min heating
Speed rises to 600-1100oC is simultaneously incubated 5-10h.
（6）By step（5）Obtained powder, which is placed in hydrofluoric acid, carries out immersion 1-6h, then filters and is cleaned with distilled water
To neutrality, in 90-150oPowder is dried under the conditions of C, obtains porous long circulating silicon-carbon cathode material.
Further, step（1）、（2）With（4）Middle solvent is distilled water, absolute ethyl alcohol, ethanol, ethylene glycol, methylpyrrole
One or more in alkanone and tetrahydrofuran, preferably methyl pyrrolidone.
Further, step（2）With（4）Middle carbon source be sucrose, glucose, phenolic resin, polyvinyl alcohol, hard pitch or
One or more in modified pitch, preferably modified pitch.
Further, step（4）Middle conductive agent is Super p, acetylene black, 350G, carbon fiber (VGCF), CNT
（CNTs）, one or more in Ketjen black or graphene, preferably Super p.
Further, step（1）Middle silicon monoxide solid content is 20-70wt%, preferably 50-70%.
Further, step（2）The mass ratio of middle nanometer silicon monoxide powder, solvent and carbon source is 2-10：2-10:1, it is excellent
Select 5:5:1.
Further, step（3）With（5）Middle atmosphere is nitrogen, argon gas or 80-95 parts by volume argon gas and 5-20 parts by volume
The gaseous mixture of hydrogen, preferably argon gas.
Further, step（4）Middle presoma powder, carbon source, the mass ratio of conductive agent and solvent are 2-10:1:1-5:2-
10, preferably 5:1:1:5.
Further, step（6）Middle hydrofluoric acid concentration is 2-40wt%, preferably 30wt%.
The beneficial effects of the invention are as follows：The preparation method technique is simple, bad border is friendly, is advantageous to large-scale production.This hair
It is bright that the silica generated under silicon monoxide high temperature disproportionated reaction is fallen by hydrofluoric acid etch, leave hole, such porous knot
Structure alleviates nano-silicon Volumetric expansion, while can be more complete by silicon monoxide or silicon cladding using secondary cladding in batches,
Exposed silicon monoxide or silicon are reduced, avoids silicon monoxide or silicon and electrolyte contacts from occurring side reaction, during secondary cladding
It is in order to improve silicon carbon material electric conductivity, so as to effectively increase the effect of coulomb first of negative material and circulation to increase conductive agent
Performance.
Embodiment
The following example is further explanation of the present invention, and the present invention is not limited in any way.
Embodiment 1
A kind of porous macrocyclic silicon-carbon cathode material preparation method of this example, including have the following steps.
（1）Silicon monoxide and methyl pyrrolidone are placed in planetary ball mill, wherein silicon monoxide solid content is
60wt%, wet ball grinding 18h is carried out under rotating speed 400r/min, 130 after ball millingo10h is dried under the conditions of C, obtains nanoscale one
Silica powder.
（2）By step（1）Nanometer silicon monoxide powder, methyl pyrrolidone and the modified pitch of processing are according to mass ratio 5:
5:1 is placed in homogenizer and carries out liquid phase coating, 5h is stirred under rotating speed 1000r/min, then 130oDried under the conditions of C
Simultaneously powder is made in 8h.
（3）By step（2）Obtained powder, which is placed in argon gas atmosphere stove, carries out charing process, with 10oC/min heating speed
Rate rises to 1000oC is simultaneously incubated 8h, obtains precursor powder.
（4）By step（3）Obtained presoma powder is with modified pitch, Super p, methyl pyrrolidone according to mass ratio
5:1:1:5 are placed in homogenizer and carry out secondary liquid phase coating, 5h are stirred under rotating speed 1200r/min, then 130oC bars
8h is dried under part and powder is made.
（5）By step（4）Obtained powder is placed in argon gas atmosphere stove carries out charing process again, with 10oC/min liter
Warm speed rises to 1000oC is simultaneously incubated 10h.
（6）By step（5）Obtained powder, which is placed in 30wt% hydrofluoric acid, carries out immersion 3h, then filters and uses distilled water
Cleaning is to neutrality, 130oPowder is dried under the conditions of C, obtains porous long circulating silicon-carbon cathode material.
Embodiment 2
A kind of porous macrocyclic silicon-carbon cathode material preparation method of this example, including have the following steps.
（1）Silicon monoxide and absolute ethyl alcohol are placed in planetary ball mill, wherein silicon monoxide solid content is 30wt%,
Wet ball grinding 16h is carried out under rotating speed 300r/min, 100 after ball millingo9h is dried under the conditions of C, obtains nanoscale silicon monoxide
Powder.
（2）By step（1）Nanometer silicon monoxide powder, absolute ethyl alcohol and the sucrose of processing are according to mass ratio 3:8:1 is placed in
Liquid phase coating is carried out in homogenizer, 4h is stirred under rotating speed 900r/min, then 100o8h is dried under the conditions of C and is made
Powder.
（3）By step（2）Obtained powder, which is placed in nitrogen atmosphere stove, carries out charing process, with 10oC/min heating speed
Rate rises to 800oC is simultaneously incubated 4h, obtains precursor powder.
（4）By step（3）Obtained presoma powder is with sucrose, acetylene black, absolute ethyl alcohol according to mass ratio 8:1:3:7
It is placed in homogenizer and carries out secondary liquid phase coating, 4h is stirred under rotating speed 900r/min, then 100oDried under the conditions of C
Simultaneously powder is made in 9h.
（5）By step（4）Obtained powder is placed in argon gas atmosphere stove carries out charing process again, with 10oC/min liter
Warm speed rises to 800oC is simultaneously incubated 4h.
（6）By step（5）Obtained powder, which is placed in 20wt% hydrofluoric acid, carries out immersion 5h, then filters and uses distilled water
Cleaning is to neutrality, 100oPowder is dried under the conditions of C, obtains porous long circulating silicon-carbon cathode material.
Embodiment 3
A kind of porous macrocyclic silicon-carbon cathode material preparation method of this example, including have the following steps.
（1）Silicon monoxide and distilled water are placed in planetary ball mill, wherein silicon monoxide solid content is 50wt%,
Wet ball grinding 18h is carried out under rotating speed 300r/min, 110 after ball millingo4h is dried under the conditions of C, obtains nanoscale silicon monoxide powder
Body.
（2）By step（1）Nanometer silicon monoxide powder, distilled water and the glucose of processing are according to mass ratio 8:10:1 is placed in
Liquid phase coating is carried out in homogenizer, 6h is stirred under rotating speed 800r/min, then 110o10h is dried under the conditions of C and is made
Cheng Fen.
（3）By step（2）Obtained powder, which is placed in nitrogen atmosphere stove, carries out charing process, with 10oC/min heating speed
Rate rises to 900oC is simultaneously incubated 5h, obtains precursor powder.
（4）By step（3）Obtained presoma powder is with glucose, carbon fiber (VGCF), distilled water according to mass ratio 4:
1:2:6 are placed in homogenizer and carry out secondary liquid phase coating, 6h are stirred under rotating speed 800r/min, then 110oC conditions
Simultaneously powder is made in lower dry 7h.
（5）By step（4）Obtained powder is placed in argon gas atmosphere stove carries out charing process again, with 10oC/min liter
Warm speed rises to 900oC/min is simultaneously incubated 5h.
（6）By step（5）Obtained powder, which is placed in 20wt% hydrofluoric acid, carries out immersion 4h, then filters and uses distilled water
Cleaning is to neutrality, 110oPowder is dried under the conditions of C, obtains porous long circulating silicon-carbon cathode material.
Comparative example 1
A kind of silicon-carbon cathode material preparation method of this example, including have the following steps.
（1）Silicon monoxide and methyl pyrrolidone are placed in planetary ball mill, wherein silicon monoxide solid content is
60wt%, wet ball grinding 18h is carried out under rotating speed 400r/min, 130 after ball millingo10h is dried under the conditions of C, obtains nanoscale one
Silica powder.
（2）By step（1）The nanometer silicon monoxide powder of processing and modified pitch, Super p, methyl pyrrolidone according to
Mass ratio 5:1:1:5 are placed in homogenizer and carry out liquid phase coating, 5h are stirred under rotating speed 1000r/min, then 130oC
Under the conditions of dry 8h and be made powder.
（3）By step（2）Obtained powder, which is placed in argon gas atmosphere stove, carries out charing process, with 10oC/min heating speed
Rate rises to 1000oC is simultaneously incubated 8h.
（4）By step（3）Obtained powder, which is placed in 30wt% hydrofluoric acid, carries out immersion 3h, then filters and uses distilled water
Cleaning is to neutrality, 130oPowder is dried under the conditions of C, obtains silicon-carbon cathode material.
Comparative example 2
A kind of silicon-carbon cathode material preparation method of this example, including have the following steps.
（1）Silicon monoxide and methyl pyrrolidone are placed in planetary ball mill, wherein silicon monoxide solid content is
60wt%, wet ball grinding 18h is carried out under rotating speed 400r/min, 130 after ball millingo10h is dried under the conditions of C, obtains nanoscale one
Silica powder.
（2）By step（1）Nanometer silicon monoxide powder, methyl pyrrolidone and the modified pitch of processing are according to mass ratio 5:
5:1 is placed in homogenizer and carries out liquid phase coating, 5h is stirred under rotating speed 1000r/min, then 130oDried under the conditions of C
Simultaneously powder is made in 8h.
（3）By step（2）Obtained powder, which is placed in argon gas atmosphere stove, carries out charing process, with 10oC/min heating speed
Rate rises to 1000oC is simultaneously incubated 8h, obtains precursor powder.
（4）By step（3）Obtained presoma powder is with modified pitch, methyl pyrrolidone according to mass ratio 5:1:5 put
Secondary liquid phase coating is carried out in homogenizer, 5h is stirred under rotating speed 1200r/min, then 130oDried under the conditions of C
Simultaneously powder is made in 8h.
（5）By step（4）Obtained powder is placed in argon gas atmosphere stove carries out charing process again, with 10oC/min liter
Warm speed rises to 1000oC is simultaneously incubated 10h.
（6）By step（5）Obtained powder, which is placed in 30wt% hydrofluoric acid, carries out immersion 3h, then filters and uses distilled water
Cleaning is to neutrality, 130oPowder is dried under the conditions of C, obtains silicon-carbon cathode material.
For the performance of the lithium ion battery negative material of the detection present invention, tested with half-cell method of testing, by embodiment
The silicon-carbon cathode material that 1-3 and comparative example 1-2 are prepared is made into slurry as negative active core-shell material, and wet end furnish is:
Active material：Super p：CMC：SBR=90：4：2：4（Mass ratio）, then slurry is coated on copper foil and is dried in vacuo 12h systems
Into negative plate, electrolyte is commercialization purchase, and PE is barrier film, and lithium piece is to electrode, and half-cell is assembled into glove box.
LAND battery test systems carry out constant current charge-discharge experiment, and charging/discharging voltage is limited in 0-2V, the discharge and recharge computerizedd control
Cabinet carries out the collection and control of data.
Following table is negative material performance comparision in embodiment 1-3 and comparison example example 1-2.
| Embodiment/comparative example | 0.1C specific capacities first（mAh/g） | 0.1C efficiency first（%） | 500 circulation volume conservation rates of 0.1C（%） |
| Embodiment 1 | 923.7 | 91.2% | 87.5 |
| Embodiment 2 | 836.4 | 90.3% | 82.4 |
| Embodiment 3 | 975.9 | 89.6% | 83.6 |
| Comparative example 1 | 938.2 | 89.1% | 63.5 |
| Comparative example 2 | 918.3 | 83.4% | 82.6 |
As can be seen from the table, as the porous long circulating silicon-carbon cathode material prepared by embodiment 1-3, it is very good to possess
Volumetric properties, first charge-discharge efficiency and cycle performance.Embodiment 1 is the porous long circulating silicon-carbon cathode material of optimum performance
Material, compared with comparison example 1 is using the effect once coated, it is evident that 500 circulation volume conservation rates are higher by a lot, this explanation
Secondary covered effect is more preferable, reduces exposed silicon monoxide or silicon, avoids itself and electrolyte contacts that side reaction occurs,
Electrolyte is consumed, therefore long-term cycle performance is more preferable.Do not add conductive agent during secondary cladding in comparison example 2, its efficiency ratio first
Embodiment 1 is low, and this illustrates that addition conductive agent can improve the efficiency first of silicon-carbon cathode material during cladding.
The present invention by above-described embodiment come illustrate the present invention details, but the present invention not office this.Affiliated technology
The technical staff in field is it will be clearly understood that any improvement in the present invention, to the equivalence replacement and auxiliary of each raw material of product of the present invention
The increase of composition, selection of concrete mode etc., within the scope of all falling within protection scope of the present invention and disclosing.
Claims (9)
1. a kind of porous macrocyclic silicon-carbon cathode material preparation method, it is characterised in that including having the following steps：
（1）Silicon monoxide and solvent are placed in planetary ball mill, wet ball grinding 5- is carried out under rotating speed 100-400r/min
18h, in 90-150 after ball millingo4-12h is dried under the conditions of C, obtains nanoscale silicon monoxide powder；
（2）By step（1）Obtained nanometer silicon monoxide powder, solvent and carbon source is placed in progress liquid phase bag in homogenizer
Cover, 3-6h is stirred under rotating speed 600-1200r/min, then in 90-150o4-12h is dried under the conditions of C and powder is made；
（3）By step（2）Obtained powder, which is placed in atmosphere furnace, carries out charing process, with 5-10oC/min heating rate rises to
600-1100oC is simultaneously incubated 5-10h, obtains precursor powder；
（4）By step（3）Obtained presoma powder is placed in homogenizer with carbon source, conductive agent, solvent and carries out two not good liquors
Mutually coat, 3-6h is stirred under rotating speed 600-1200r/min, then in 90-150o4-12h is dried under the conditions of C and powder is made；
（5）By step（4）Obtained powder is placed in atmosphere furnace carries out charing process again, with 5-10oC/min heating rate
Rise to 600-1100oC is simultaneously incubated 5-10h；
（6）By step（5）Obtained powder, which is placed in hydrofluoric acid, to be soaked, and is then filtered and is cleaned with distilled water to neutrality,
In 90-150oPowder is dried under the conditions of C, obtains porous long circulating silicon-carbon cathode material.
2. a kind of porous macrocyclic silicon-carbon cathode material preparation method according to claims 1, it is characterised in that described
Step（1）、（2）With（4）Middle solvent is in distilled water, absolute ethyl alcohol, ethanol, ethylene glycol, methyl pyrrolidone and tetrahydrofuran
One or more.
3. a kind of porous macrocyclic silicon-carbon cathode material preparation method according to claims 1, it is characterised in that described
Step（2）With（4）Middle carbon source is one kind in sucrose, glucose, phenolic resin, polyvinyl alcohol, hard pitch or modified pitch
It is or a variety of.
A kind of 4. porous macrocyclic silicon-carbon cathode material preparation method according to claims 1, it is characterised in that：It is described
Step（4）Middle conductive agent is Super p, acetylene black, 350G, carbon fiber (VGCF), CNT（CNTs）, Ketjen black or graphite
One or more in alkene, preferably Super p.
5. a kind of porous macrocyclic silicon-carbon cathode material preparation method according to claims 1, it is characterised in that described
Step（1）Middle silicon monoxide solid content is 20-70wt%, preferably 50-70%.
6. a kind of porous macrocyclic silicon-carbon cathode material preparation method according to claims 1, it is characterised in that described
Step（2）The mass ratio of middle nanometer silicon monoxide powder, solvent and carbon source is 2-10：2-10:1, preferably 5:5:1.
7. a kind of porous macrocyclic silicon-carbon cathode material preparation method according to claims 1, it is characterised in that described
Step（3）With（5）Middle atmosphere is the gaseous mixture of nitrogen, argon gas or 80-95 parts by volume argon gas and 5-20 parts by volume hydrogen.
8. a kind of porous macrocyclic silicon-carbon cathode material preparation method according to claims 1, it is characterised in that described
Step（4）Middle presoma powder, carbon source, the mass ratio of conductive agent and solvent are 2-10:1:1-5:2-10, preferably 5:1:1:5.
9. a kind of porous macrocyclic silicon-carbon cathode material preparation method according to claims 1, it is characterised in that described
Step（6）Middle hydrofluoric acid concentration is 2-40wt%.
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| CN114864890A (en) * | 2022-04-19 | 2022-08-05 | 赣州市瑞富特科技有限公司 | Surface porous micro hollow sphere silicon carbon negative electrode material and preparation method thereof |
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