CN106654230A - Method for preparing silicon-carbon negative electrode material employing suspended emulsion polymerization method - Google Patents
Method for preparing silicon-carbon negative electrode material employing suspended emulsion polymerization method Download PDFInfo
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Abstract
The invention provides a method for preparing a silicon-carbon negative electrode material employing a suspended emulsion polymerization method. The method comprises the following steps of weighing graphite, a silicon negative electrode, phenolic resin and a curing agent; (2) adding the silicon negative electrode in the step (1) to the graphite to prepare silicon/graphite mixed powder; (3) dissolving the phenolic resin in the step (1) into absolute ethyl alcohol; (4) adding the phenolic resin dissolved in the step (3) to the silicon/graphite powder prepared in the step (3) and stirring evenly to obtain a turbid liquid containing the silicon/graphite powder; (5) adding the turbid liquid prepared in the step (4) to silicone oil, carrying out ultrasonic oscillation, intensely stirring the silicone oil, heating the silicone oil and recycling volatile absolute ethyl alcohol; (6) further heating and stirring the silicone oil, and then filtering, washing and drying the silicon/graphite powder coated with the phenolic resin; and (7) carbonizing the silicon/graphite powder coated with the phenolic resin under inert gas protection. According to the method, the electrochemical properties can be effectively improved.
Description
Technical field
The invention belongs to energy storage material and electrochemical field, are related to a kind of preparation work of lithium battery silicon-carbon cathode material
Skill, more particularly to the method that Suspended Emulsion Polymerization method prepares silicon-carbon cathode material.
Background technology
Graphite material is widely used as the negative material of lithium ion battery.Master of the graphite as lithium ion battery negative material
The advantage is wanted to be：Discharge platform is more steady, and lithium storage content is high, and up to 372 mAh/g., it has the disadvantage graphite material to theoretical lithium storage content
Capacity is low and graphite is poor with the compatibility of electrolyte, the stripping of graphite linings is easily produced in process of intercalation, so as to cause
Its cycle performance is poor, limits it in the application in lithium ion battery.Nano silicon material is because of the lithium storage content of its superelevation, quilt
People pay close attention to, but volumetric expansion is severe in process of intercalation, and easy efflorescence causes capacity attenuation, uses so as to limit it.It is high
After degree graphitized carbon material and nano silicon material have complementary advantages, the compound silicon carbon material with core-shell structure is prepared, changed
The chemical property of nano-silicon and graphite material has been apt to it, has improve capacity, has expanded its use range.The shell material with carbon element of cladding
The presoma for being adopted mainly has：Phenolic resin, epoxy resin, polyacrylonitrile, ethylene, Colophonium etc..Presently used cladding side
Method is mainly liquid phase coating, is spray-dried shaping, during cladding, with the volatilization of solvent, is coated on nano-silicon/graphite granule
The resin on surface is uneven, and covered effect is deteriorated, and affects performance.
The content of the invention
In order to solve above technical problem, the present invention prepares silicon-carbon cathode material using Suspended Emulsion Polymerization method, should
Method obtains a kind of spherical silicon-carbon cathode material, and evenly, covered effect more preferably, can be effective for cladding compared with other cladding process
Raising its chemical property.
The Suspended Emulsion Polymerization method of the present invention prepares the preparation method of silicon-carbon cathode material and carries out according to the following steps：
Step one, weigh graphite, silicium cathode, phenolic resin, firming agent according to certain mass ratio；
Step 2, the silicium cathode in step one is added in graphite, silicon/graphite mixed-powder is obtained；
Step 3, the phenolic resin in step one is dissolved in dehydrated alcohol；
Step 4, the phenolic resin that step 3 has dissolved is added in silicon/graphite composite powder obtained in step 2 and is stirred,
Obtain the suspension containing silicon/graphite composite powder；
Step 5, the suspension that step 4 is obtained is added in silicone oil, sonic oscillation is simultaneously stirred vigorously silicone oil, then by silicone oil
Heating, then the dehydrated alcohol of volatilization is reclaimed；
Step 6, continuation heated and stirred silicone oil, the silicon that then phenolic resin is covered to complete/graphite composite powder is filtered, washing, is done
It is dry；
Step 7, phenolic resin is coated after the carbonization under inert gas shielding of silicon/graphite composite powder.
The present invention is using Suspended Emulsion Polymerization method in silicon/graphite hybrid particles coated with uniform resin and then carbonization
Obtain the compound silicon-carbon cathode of core-shell structure.Suspended Emulsion Polymerization method has suspended with emulsion polymerization Partial Feature concurrently
Plant polymerization.Preparing silicon-carbon cathode using the technique has following remarkable advantage：Ethanol and resin can not be dissolved in silicone oil, resin
Ethanol can be dissolved in, ethanol has good wettability to silicon/graphite hybrid particles, in silicone oil solvent by ethanol to silicon/graphite
The good wettability of hybrid particles, resin can be coated in hybrid particles uniform surface in the case of agitating heating, with other
The method for preparing silicon-carbon cathode compares all nano-silicons/synthetic graphite particles surface and has uniformly been coated resin, does not exist
Uncoated granule；The cladding thickness of all coated particles is substantially uniform, and resin is fully cured, and there is no post bake and sticks.
Preferably, graphite, silicium cathode, phenolic resin, the mass ratio of firming agent are weighed in step one is：52.75-94.7:
2-30:3-15:0.24-2.25。
Preferably, the graphite adopts Delanium, and silicium cathode is using nano-silicon or silicon monoxide.
Preferably, the Delanium is from the Delanium micropowder that d50 is 0.5-6 microns；Phenolic resin is using common
Phenolic resin；The quality of firming agent adopts the 8-15% of phenolic resin quality；
Preferably, the quality of the dehydrated alcohol in step 3 is 2-4 times of graphite quality；
Preferably, mixing speed is that 80-150 turns/min in step 4, and mixing time is 30-90min；
Preferably, 5-10 times of the suspension vol that the volume of silicone oil is obtained for step 4 in step 5；It is outstanding that step 4 is obtained
In the stirring reaction of supernatant liquid and silicone oil, mixing speed 300-350 turns/min, mixing time 60-90min；It is outstanding that step 4 is obtained
In the reacting by heating of supernatant liquid and silicone oil, reaction temperature is 100-110 DEG C, and temperature retention time is 60-180 min.
Preferably, silicone oil heating-up temperature 130-180 DEG C in step 6, temperature retention time is 60-180 min；Baking temperature 80-
120 DEG C, drying time is 60-180 min.
Preferably, the atmosphere of carbonization reaction is nitrogen in step 7, and carbonization temperature is interval 150-1050 DEG C, carbonization total duration
24 hours, the body fltting speed 1m/h of carbonization case.
Because the Suspended Emulsion Polymerization method of the present invention is by controlling when raw material material, mixing speed and heating
Between, the clad structure being actually needed is obtained in that, reach the purpose for preparing core-shell structure silicon-carbon cathode material.Covered effect
It is good, main equipment is not required to, process is simple, it is easy to accomplish industrialization.
Description of the drawings
Fig. 1 be according to specific embodiment prepare siliceous 2% silicon-carbon cathode material half-cell test performance curve.
Fig. 2 be according to specific embodiment prepare siliceous 4% silicon-carbon cathode material half-cell test performance curve.
Fig. 3 is the SEM figures of the silicon-carbon cathode material that the present invention is obtained.
Fig. 4 is the silicon-carbon cathode material half-cell cycle life curve.
Specific embodiment
Below in conjunction with the accompanying drawings, the preferably embodiment of the present invention is described in further detail：
Embodiment 1
Step one, weigh Delanium 94.7g, nano-silicon 2g, phenolic resin 3g, firming agent 0.3g that d50 is 1 micron；
Step 2, the nano-silicon in step one is added in Delanium micropowder, nano-silicon/Delanium mixed powder is obtained
End；
Step 3, the phenolic resin in step one is dissolved in 189.4g dehydrated alcohol forms solution；
Step 4, phenolic resin ethanol solution are added in Delanium obtained in step 2/nano-silicon powder body and stir,
Mixing speed is 80 turns/min, and mixing time is 30min, obtains the suspension containing Delanium/nano-silicon powder body；
Step 5, the suspension that step 4 is obtained is added in the silicone oil that volume is 5 times of suspension volume, sonic oscillation is simultaneously acute
Then silicone oil is heated to 100 DEG C by strong stirring silicone oil, 300 turns/min of mixing speed, mixing time 60min, and temperature retention time is 60
Min, the dehydrated alcohol of volatilization is reclaimed by being arranged on the condenser condensation above agitating device；
Step 6, continuation heated and stirred silicone oil, 130 DEG C of silicone oil heating-up temperature, temperature retention time is 60 min, then by phenolic resin
The Delanium being covered to complete/nano-silicon powder body is filtered, washing, is dried, and baking temperature is 80 DEG C, and drying time is 60 min；
Step 7, phenolic resin is coated after Delanium/nano-silicon powder body carbonization under nitrogen protection, carbonization temperature is interval
150-1050 DEG C, carbonization total duration 24 hours, the body fltting speed 1m/h of carbonization case.
Embodiment 2
Step one, weigh spherical graphite 92.76g, nano-silicon 4g, phenolic resin 3g, firming agent 0.24g；
Step 2, the nano-silicon in step one is added in spherical graphite micropowder, nano-silicon/spherical graphite mixed powder is obtained
End；
Step 3, the phenolic resin in step one is dissolved in 371.04g dehydrated alcohol forms solution；
Step 4, phenolic resin ethanol solution are added in spherical graphite obtained in step 2/nano-silicon powder body and stir,
Mixing speed is 150 turns/min, and mixing time is 90min, obtains the suspension containing spherical graphite/nano-silicon powder body；
Step 5, the suspension that step 4 is obtained is added to volume be 10 times of suspension volume silicone oil in, sonic oscillation is simultaneously
Silicone oil is stirred vigorously, then silicone oil is heated to 110 DEG C by 350 turns/min of mixing speed, mixing time 90min, and temperature retention time is
180 min, the dehydrated alcohol of volatilization is reclaimed by being arranged on the condenser condensation above agitating device；
Step 6, continuation heated and stirred silicone oil, 180 DEG C of silicone oil heating-up temperature, temperature retention time is 180 min, then by phenolic aldehyde tree
The spherical graphite that fat is covered to complete/nano-silicon powder body is filtered, washing, is dried, and baking temperature is 120 DEG C, and drying time is 180
min；
Step 7, phenolic resin is coated after spherical graphite/nano-silicon powder body carbonization under nitrogen protection, carbonization temperature is interval
150-1050 DEG C, carbonization total duration 24 hours, the body fltting speed 1m/h of carbonization case.
Embodiment 3
Step one, weigh Delanium 74.1g, silicon monoxide 16g, phenolic resin 9g, firming agent 0.9g that d50 is 6 microns；
Step 2, the silicon monoxide in step one is added in Delanium micropowder, silicon monoxide/Delanium mixing is obtained
Powder；
Step 3, the phenolic resin in step one is dissolved in 222.3g dehydrated alcohol forms solution；
Step 4, phenolic resin ethanol solution are added in Delanium obtained in step 2/silicon monoxide powder body and stir
Even, mixing speed is 110 turns/min, and mixing time is 60min, obtains the suspension containing Delanium/silicon monoxide powder body；
Step 5, the suspension that step 4 is obtained is added to volume be 7.5 times of suspension volume silicone oil in, sonic oscillation is simultaneously
Silicone oil is stirred vigorously, then silicone oil is heated to 105 DEG C by 325 turns/min of mixing speed, mixing time 75min, and temperature retention time is
120min, the dehydrated alcohol of volatilization is reclaimed by being arranged on the condenser condensation above agitating device；
Step 6, continuation heated and stirred silicone oil, 155 DEG C of silicone oil heating-up temperature, temperature retention time is 120 min, then by phenolic aldehyde tree
The Delanium that fat is covered to complete/silicon monoxide powder body is filtered, washing, is dried, and baking temperature is 100 DEG C, and drying time is 120
min；
Step 7, phenolic resin is coated after Delanium/silicon monoxide powder body carbonization under nitrogen protection, carbonization temperature area
Between 150-1050 DEG C, carbonization total duration 24 hours, the body fltting speed 1m/h of carbonization case.
Embodiment 4
Step one, weigh Delanium 63.8g, nano-silicon 23g, phenolic resin 12g, firming agent 1.2g that d50 is 3 microns；
Step 2, the nano-silicon in step one is added in Delanium micropowder, nano-silicon/Delanium mixed powder is obtained
End；
Step 3, the phenolic resin in step one is dissolved in 159.5g dehydrated alcohol forms solution；
Step 4, phenolic resin ethanol solution are added in Delanium obtained in step 2/nano-silicon powder body and stir,
Mixing speed is 100 turns/min, and mixing time is 45min, obtains the suspension containing Delanium/nano-silicon powder body；
Step 5, the suspension that step 4 is obtained is added in the silicone oil that volume is 6 times of suspension volume, sonic oscillation is simultaneously acute
Then silicone oil is heated to 103 DEG C by strong stirring silicone oil, 315 turns/min of mixing speed, mixing time 70min, and temperature retention time is
100 min, the dehydrated alcohol of volatilization is reclaimed by being arranged on the condenser condensation above agitating device；
Step 6, continuation heated and stirred silicone oil, 140 DEG C of silicone oil heating-up temperature, temperature retention time is 90min, then by phenolic resin
The Delanium being covered to complete/nano-silicon powder body is filtered, washing, is dried, and baking temperature is 90 DEG C, and drying time is 90 min；
Step 7, phenolic resin is coated after Delanium/nano-silicon powder body carbonization under nitrogen protection, carbonization temperature is interval
150-1050 DEG C, carbonization total duration 24 hours, the body fltting speed 1m/h of carbonization case.
Embodiment 5
Step one, weigh Delanium 52.75g, nano-silicon 30g, phenolic resin 15g, firming agent 2.25g that d50 is 2 microns；
Step 2, the nano-silicon in step one is added in Delanium micropowder, nano-silicon/Delanium mixed powder is obtained
End；
Step 3, the phenolic resin in step one is dissolved in 158.25g dehydrated alcohol forms solution；
Step 4, phenolic resin ethanol solution are added in Delanium obtained in step 2/nano-silicon powder body and stir,
Mixing speed is 130 turns/min, and mixing time is 75min, obtains the suspension containing Delanium/nano-silicon powder body；
Step 5, the suspension that step 4 is obtained is added to volume be 8.5 times of suspension volume silicone oil in, sonic oscillation is simultaneously
Silicone oil is stirred vigorously, then silicone oil is heated to 108 DEG C by 340 turns/min of mixing speed, mixing time 80min, and temperature retention time is
150 min, the dehydrated alcohol of volatilization is reclaimed by being arranged on the condenser condensation above agitating device；
Step 6, continuation heated and stirred silicone oil, 160 DEG C of silicone oil heating-up temperature, temperature retention time is 150 min, then by phenolic aldehyde tree
The Delanium that fat is covered to complete/nano-silicon powder body is filtered, washing, is dried, and baking temperature is 110 DEG C, and drying time is 150
min；
Step 7, phenolic resin is coated after Delanium/nano-silicon powder body carbonization under nitrogen protection, carbonization temperature is interval
150-1050 DEG C, carbonization total duration 24 hours, the body fltting speed 1m/h of carbonization case.
As shown in figure 3, being successfully prepared core-shell structure silicon-carbon cathode material using emulsion polymerisation process, SEM pictures show
Show, the silicon-carbon cathode material even particle size distribution prepared by suspension emulsion polymerization, pattern rule subglobular, phenolic resin
Carbon coating is uniform.
As shown in figure 4, siliceous 5% silicon-carbon cathode material, after 50 circulations, capacity is almost undamped, absolutely proves gained
Nano silica fume is uniformly dispersed in silicon-carbon cathode material, and clad and micron graphous graphite powder serve good repression of swelling and carry
The effect of high material lifetime.
The charge-discharge performance of silicon-carbon cathode material prepared by present embodiment is excellent.Based on spherical graphite, in phenolic aldehyde tree
Fat content is 3%, and the silicon-carbon cathode first time discharge capacity prepared according to preparation technology in the case of nanometer silicone content 3% can reach
440mAh/g, first charge-discharge efficiency can reach 94%, effectively improve negative material capacity.
Above content is to combine specific preferred implementation further description made for the present invention, it is impossible to assert
The present invention be embodied as be confined to these explanations.For general technical staff of the technical field of the invention,
On the premise of without departing from present inventive concept, some simple deduction or replace can also be made, should all be considered as belonging to the present invention's
Protection domain.
Claims (9)
1. a kind of method that Suspended Emulsion Polymerization method prepares silicon-carbon cathode material, it is characterised in that include：
Step one, weigh graphite, silicium cathode, phenolic resin, firming agent according to certain mass ratio；
Step 2, the silicium cathode in step one is added in graphite, silicon/graphite mixed-powder is obtained；
Step 3, the phenolic resin in step one is dissolved in dehydrated alcohol；
Step 4, the phenolic resin that step 3 has dissolved is added in silicon/graphite composite powder obtained in step 2 and is stirred,
Obtain the suspension containing silicon/graphite composite powder；
Step 5, the suspension that step 4 is obtained is added in silicone oil, sonic oscillation is simultaneously stirred vigorously silicone oil, then by silicone oil
Heating, then the dehydrated alcohol of volatilization is reclaimed；
Step 6, continuation heated and stirred silicone oil, the silicon that then phenolic resin is covered to complete/graphite composite powder is filtered, washing, is done
It is dry；
Step 7, phenolic resin is coated after the carbonization under inert gas shielding of silicon/graphite composite powder.
2. the method for claim 1, it is characterised in that graphite, silicium cathode, phenolic resin, solidification are weighed in step one
The mass ratio of agent is：52.75-94.7: 2-30:3-15:0.24-2.25.
3. the method for claim 1, it is characterised in that the graphite adopts Delanium, silicium cathode to adopt nano-silicon
Or silicon monoxide.
4. method as claimed in claim 3, it is characterised in that the Delanium from d50 for 0.5-6 microns artificial stone
Black micropowder；Phenolic resin adopts phenolic resin；The quality of firming agent adopts the 8-15% of phenolic resin quality.
5. the method for claim 1, it is characterised in that the quality of the dehydrated alcohol in step 3 for graphite quality 2-
4 times.
6. the method for claim 1, it is characterised in that mixing speed is that 80-150 turns/min in step 4, during stirring
Between be 30-90min.
7. the method for claim 1, it is characterised in that the suspension that the volume of silicone oil is obtained for step 4 in step 5
5-10 times of volume；In suspension and the stirring reaction of silicone oil that step 4 is obtained, mixing speed 300-350 turns/min, stirring
Time 60-90min；In suspension and the reacting by heating of silicone oil that step 4 is obtained, reaction temperature is 100-110 DEG C, during insulation
Between be 60-180 min.
8. the method for claim 1, it is characterised in that silicone oil heating-up temperature 130-180 DEG C in step 6, temperature retention time
For 60-180 min；80-120 DEG C of baking temperature, drying time is 60-180 min.
9. the method for claim 1, it is characterised in that the atmosphere of carbonization reaction is nitrogen in step 7, carbonization temperature
Interval 150-1050 DEG C, carbonization total duration 24 hours, the body fltting speed 1m/h of carbonization case.
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| CN112164793A (en) * | 2020-09-09 | 2021-01-01 | 中国科学院山西煤炭化学研究所 | Core-shell silicon-carbon material and preparation method thereof |
| CN112186181A (en) * | 2020-09-09 | 2021-01-05 | 中国科学院山西煤炭化学研究所 | Silicon-carbon composite material and preparation method thereof, lithium battery cathode and lithium battery |
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| CN100386906C (en) * | 2006-05-26 | 2008-05-07 | 清华大学 | Active-carbon-microball coated metal composition negative polar material and preparing method |
| CN100386905C (en) * | 2006-05-26 | 2008-05-07 | 清华大学 | Metal particle-cladded active carbon microsphere cathode composite materials and method for preparing same |
| CN101202341B (en) * | 2007-12-13 | 2011-08-31 | 复旦大学 | Carbon cladding alloy nanometer particle material for lithium ion battery and method for making same |
| CN101859886A (en) * | 2010-05-27 | 2010-10-13 | 深圳市德兴富电池材料有限公司 | Lithium ion battery anode material and preparation method thereof |
| CN102637872A (en) * | 2012-01-07 | 2012-08-15 | 天津市贝特瑞新能源材料有限责任公司 | High-capacity silicon-carbon composited anode material, preparation method and application thereof |
| CN104577084A (en) * | 2015-01-20 | 2015-04-29 | 深圳市贝特瑞新能源材料股份有限公司 | Nano silicon composite negative electrode material for lithium ion battery, preparation method and lithium ion battery |
| CN106025211A (en) * | 2016-06-06 | 2016-10-12 | 田东 | Preparation method of high-capacity silicon-based negative electrode material of lithium-ion battery |
-
2017
- 2017-01-21 CN CN201710044714.6A patent/CN106654230A/en not_active Withdrawn
- 2017-10-21 CN CN201710988598.3A patent/CN107863507B/en active Active
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112164794A (en) * | 2020-09-09 | 2021-01-01 | 中国科学院山西煤炭化学研究所 | Lithium battery and preparation method thereof |
| CN112164793A (en) * | 2020-09-09 | 2021-01-01 | 中国科学院山西煤炭化学研究所 | Core-shell silicon-carbon material and preparation method thereof |
| CN112186181A (en) * | 2020-09-09 | 2021-01-05 | 中国科学院山西煤炭化学研究所 | Silicon-carbon composite material and preparation method thereof, lithium battery cathode and lithium battery |
| CN114220956A (en) * | 2021-12-06 | 2022-03-22 | 厦门理工学院 | Si @ MnO @ C composite material, preparation method thereof, negative electrode material and battery |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107863507A (en) | 2018-03-30 |
| CN107863507B (en) | 2019-11-12 |
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