CN108946744A - A kind of lithium ion battery preparation method for aoxidizing sub- silicium cathode material - Google Patents
A kind of lithium ion battery preparation method for aoxidizing sub- silicium cathode material Download PDFInfo
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- CN108946744A CN108946744A CN201810810729.3A CN201810810729A CN108946744A CN 108946744 A CN108946744 A CN 108946744A CN 201810810729 A CN201810810729 A CN 201810810729A CN 108946744 A CN108946744 A CN 108946744A
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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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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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Abstract
A kind of lithium ion battery aoxidizes the preparation method of sub- silicium cathode material, step: (1) raw material of sub- silicon using micron or submicron order silicon powder as preparation are aoxidized, first by micron or submicron order silicon powder high temperature sintering in air atmosphere, make Surface Creation silicon dioxide layer；(2) vacuum pump is opened, continue to increase temperature and controls vacuum degree in 500-1500pa, its reaction is generated and aoxidizes sub- silicon gas, finally obtain aoxidizing sub- silicon bulk in condensing collector；(3) it is crushed.Method advantage: the traditional handicraft that preparation aoxidizes sub- silicon is to be sufficiently mixed silicon powder and silicon dioxide powder, reaction, which generates, under elevated temperature in vacuo aoxidizes sub- silicon, this method is without the method for mixing silicon powder and silica, directly material is put into high temperature furnace and heats the regular hour, the oxidation Asia silicon product of subsequent vacuum high-temperature reaction, simplifies processing step.
Description
Technical field
The present invention relates to technical field of lithium ion, and in particular to a kind of lithium ion battery sub- silicium cathode material of oxidation
Preparation method.
Background technique
Silicon monoxide is a kind of inorganic compound, chemical formula SiO, be under normal temperature and pressure it is dark brown to loess color without fixed
Shape powder, 1880 DEG C of boiling point, 2.13 grams/cc of density, is insoluble in water, can be dissolved in diluted hydrofluoric acid and nitre by 1702 DEG C of fusing point
In the nitration mixture of acid and ocratation is released, the SiO 2 powder of white is generated when heating in air.Silicon monoxide is less steady
It is fixed, it can be oxidized to silica in air.It inverse can be disproportionated when silicon monoxide steam slowly condenses and form silicon and silica.
Generally it can be by being made under silica in a vacuum 1300 DEG C of high temperature with cooling rapidly after pure silicon effect.
SiO2 + Si → 2SiO。
All the time, because aoxidizing sub- silicon (SiO) good bulk effect, people are attempted as negative electrode of lithium ion battery
Material, it is considered that, SiO cathode Mechanism of electrochemical behaviors of anhydrous is as follows:
SiO+Li→Li2O+Si (1)
SiO+Li→Li4SiO4+Si (2)
Si+Li→Li4.4Si (3)
The Li of generation2O、Li4SiO4It is precipitated with back bone network, acts as a kind of good buffer matrix in situ, restrained effectively
The bulk effect of active metal silicon particle in charge and discharge process；The two also plays support and dispersed metal silicon accumulation regions simultaneously
The effect of grain, avoids agglomeration of small and dispersed metallic silicon accumulation regions particle during later period charge and discharge cycles, to following
Ring stability is advantageous.This also exactly aoxidizes sub- silicon (SiO) material and is had an optimistic view of by people always, most becomes next in realistic meaning fastly
For the most important reason of negative electrode material.
The traditional handicraft that preparation at present aoxidizes sub- silicon is to be sufficiently mixed silicon powder and silicon dioxide powder, under elevated temperature in vacuo
It carries out reaction and generates silica, the price of high-purity silicon powder and high-purity silicon dioxide powder is higher, so as to cause the system of high-purity silicon oxide
It is standby at high cost.Therefore the raw material for seeking low cost, develop new technique be the key that solve to aoxidize sub- silicon yield and its price because
Element.
In recent years, photovoltaic industry enters the fast-developing phase, and global monocrystalline silicon annual output is more than 100,000 tons.And it prepares too
When positive energy battery, it usually needs high purity silicon ingot is cut into unit silicon wafer.In cutting process, will have 44% according to theoretical calculation
Crystalline silicon cut and entered in cutting slurry for HIGH-PURITY SILICON (99.9999% purity) " sawdust ", and in the actual processing process
Then there is the up to crystalline silicon of 50%-55% to lose in the form of submicron order silicon powder, it means that annual photovoltaic industry there will be over 5
Ten thousand tons of scrap silicons generate.Aoxidize sub- silicon materials theoretical specific capacity with higher (> 2000mAh/g), lower storage lithium reaction electricity
Flattening bench, good bulk effect, it is clear that if can be that the sub- silicon of lithium ion battery oxidation is born by photovoltaic industry scrap silicon successful conversion
Pole material will bring huge economy and society to be worth.
Summary of the invention
For the deficiency of existing traditional handicraft, the purpose of the present invention is to provide a kind of cost is lower, technique is more simply made
The standby method for aoxidizing sub- silicon.The present invention aoxidizes the raw material of sub- silicon using micron or submicron order silicon powder as preparation, by micron
Or submicron order silicon powder carries out high-temperature process, its surface is made to form a certain amount of silicon dioxide layer, continues thereafter with and increases temperature simultaneously
It keeps it under vacuum state, generates its reaction and aoxidize sub- silicon gas, be finally condensed into the sub- silicon bulk of oxidation, it is broken to obtain
Aoxidize sub- silicon powder.
Technical solution is:
A kind of lithium ion battery aoxidizes the preparation method of sub- silicium cathode material, includes the following steps:
Micron or submicron order silicon powder are carried out high-temperature process, make a certain amount of silicon dioxide layer of its Surface Creation by step 1；2nd
Step continues thereafter with and increases temperature and keep it under vacuum state, generates its reaction and aoxidizes sub- silicon gas, is finally condensed into
Aoxidize sub- silicon bulk；Step 3, broken silica block obtain aoxidizing sub- silicon powder.
In step 1, the micron or submicron order silicon powder can pass through chemical vapour deposition technique, sol-gel method, magnetic
Control sputtering technology, vacuum coating technology, laser/electrical discharge machining and magnesiothermic reduction technology obtain, and average grain diameter control exists
Between 100nm~10 μm.
In one embodiment, in step 1, it is described by the atmosphere of micron or submicron order silicon powder high-temperature process be air
Or oxygen.
In one embodiment, in step 1, it is described by the temperature of micron or submicron order silicon powder high-temperature process 500
~700 DEG C.
In one embodiment, in step 1, it is described by the time of micron or submicron order silicon powder high-temperature process be 20~
500min。
It is in one embodiment, described to keep a certain amount of silicon dioxide layer of its Surface Creation fine and close in step 1,
With a thickness of 1.0~50nm.
It is in one embodiment, described to keep a certain amount of silicon dioxide layer of its Surface Creation fine and close in step 1,
The Control for Oxygen Content of the material is in 20-45%.
In one embodiment, in step 2, described continue thereafter with increases temperature and keeps it under vacuum state,
Its temperature range is at 1200~1600 DEG C, and heating time is 0.5~for 24 hours.
In one embodiment, in step 2, described continue thereafter with increases temperature and keeps it under vacuum state,
Vacuum degree is in 500~1500pa.
In one embodiment, the crushing obtains aoxidizing sub- silicon powder, and disintegrating apparatus is planetary ball mill, mechanical powder
Any one in broken machine, super-low temperature pulverizator, superheated steam pulverizer or airslide disintegrating mill, its particle size exists after crushing
2.0~15 μm.
In one embodiment, before step 1, micron or submicron order solar photovoltaic industry scrap silicon can be adopted
With sodium hydroxide etching processing.
In one embodiment, monocrystalline and/or polycrysalline silcon are contained in the obtained silica.
Before step 1, need to micron or submicron order silicon powder using sodium hydroxide etching processing.
Beneficial effect
Have following advantage using this method: on the one hand, for the raw material used for photovoltaic industry scrap silicon, price advantage is bright
It is aobvious；On the other hand, the technique that traditional preparation aoxidizes sub- silicon is to be sufficiently mixed silicon powder and silicon dioxide powder, and pyroreaction generates
Silica, the present invention in method do not need using mixing silicon powder and silica method, material is directly put into high temperature furnace
Middle heating regular hour, the oxidation Asia silicon product of subsequent vacuum high-temperature reaction, to simplify processing step, and this method
Yield is also higher.
Detailed description of the invention
Fig. 1 is the X ray diffracting spectrum of the sub- silicon of oxidation of the embodiment of the present invention 1.
Fig. 2 is the scanning electron microscope (SEM) photograph of the sub- silicon of oxidation of the embodiment of the present invention 1.
Fig. 3 is the grain size distribution of the sub- silicon of oxidation of the embodiment of the present invention 1.
Fig. 4 is the first charge-discharge curve of the embodiment of the present invention 1.
Specific embodiment
To facilitate the understanding of the present invention, it is as follows to enumerate embodiment by the present invention.Those skilled in the art are it will be clearly understood that the reality
It applies example and is only to aid in the understanding present invention, should not be regarded as a specific limitation of the invention.
Embodiment 1
Lithium ion battery aoxidizes the preparation method of sub- silicium cathode material, includes the following steps:
Step 1, by 100g micron order silicon powder (average grain diameter control between 1~5 μm) in oxygen atmosphere, at 550 DEG C into
Row high-temperature process 300min makes its surface form the silicon dioxide layer with a thickness of 20nm thickness；
Step 2 continues thereafter with and is warming up to 1300 DEG C and keeps 5h, vacuum degree 500pa under vacuum conditions, makes to obtain in step 1
The be coated with silicon oxide silicon materials reaction of layer of surface generate and aoxidize sub- silicon gas, be finally condensed into the sub- silicon bulk of oxidation, lead to
It crosses that planetary ball mill is broken to obtain the sub- silicon powder 98.7g of 2.0~5.0 μm of oxidations, contains in the oxidation Asia silicon powder a certain amount of
Si nanocrystallite can be seen that by the X-ray diffractogram of Fig. 2 and respectively correspond crystalline substance positioned at 28.6,47.5,56.3 diffraction maximum
Body silicon (111), (220), (311) crystal plane, illustrate that a certain amount of nanocrystalline silicon is distributed in silica powder.Fig. 2 is
The scanning electron microscope (SEM) photograph of sub- silicon is aoxidized obtained by example 1, the average grain diameter of material is 5.48 μm.Fig. 4 is that Asia is aoxidized obtained by embodiment 1
The first charge-discharge curve of silicium cathode material, material discharging (embedding lithium) specific capacity are 2550.1mAh/g, and charge (de- lithium) specific capacity
For 1698.2mAh/g, first charge-discharge efficiency reaches 66.59%.
Embodiment 2
Step 1, by 100g submicron order silicon powder (average grain diameter controls between 100nm~500nm) in oxygen atmosphere,
High-temperature process 60min is carried out at 600 DEG C, forms its surface with a thickness of 5nm silicon dioxide layer；
Step 2 continues thereafter with and is warming up to 1300 DEG C and keeps 12h, vacuum degree 1500pa under vacuum conditions, makes to obtain in step 1
The silicon materials reaction arrived generates silica gas, is finally condensed into silica block, planetary ball mill crusher machine obtains 3.0~4.0 μ
M aoxidizes sub- silicon powder 96.4g.
Embodiment 3
Step 1, by 100g submicron order silicon powder (average grain diameter controls between 500nm~1 μm) in oxygen atmosphere, 700
High-temperature process 500min is carried out at DEG C, the silicon dioxide layer for making its surface form one with a thickness of 40nm；
Step 2 continues thereafter with and is warming up to 1450 DEG C and keeps 8h, vacuum degree 1000pa under vacuum conditions, makes to obtain in step 1
Silicon materials reaction generate silica gas, be finally condensed into silica block, planetary ball mill crusher machine obtains 10.0~15.0 μ
M aoxidizes sub- silicon powder 99.1g.
Embodiment 4
Difference with embodiment 1 is: using sodium hydroxide solution etching processing in advance to scrap silicon.
Step 1 first exists 150g microns or submicron order scrap silicon (average grain diameter controls between 500nm~5 μm)
5min is etched in 40 DEG C of sodium hydroxide solutions of 20wt%, obtains the scrap silicon particle that the surface 115g forms etching micropore；Then again
It takes the surface 100g to form the scrap silicon particle of etching micropore, in oxygen atmosphere, high-temperature process 300min is carried out at 550 DEG C, is made
The silicon dioxide layer that its surface is formed with a thickness of 20nm thickness；
Step 2 continues thereafter with and is warming up to 1300 DEG C and keeps 5h, vacuum degree 500pa under vacuum conditions, makes to obtain in step 1
The be coated with silicon oxide silicon materials reaction of layer of surface generate and aoxidize sub- silicon gas, be finally condensed into the sub- silicon bulk of oxidation, lead to
Cross that planetary ball mill is broken to obtain 2.0~5.0 μm of oxidations Asia silicon powder 113.6g.From the aforegoing it can be seen that by micron or Asia
After the surface of micron silicon waste material carries out NaOH etching, it can be formed on its surface etching micropore, silica can be improved
Layer is conducive to the conversion reaction process of subsequent silica in the infiltration degree on its surface.
Claims (10)
1. the preparation method that a kind of lithium ion battery aoxidizes sub- silicium cathode material, which comprises step 1, by micron or Asia
Micron order silicon powder carries out high-temperature process, makes a certain amount of silicon dioxide layer of its Surface Creation；Step 2 continues thereafter with raising temperature
And keep it under vacuum state, it generates its reaction and aoxidizes sub- silicon gas, be finally condensed into the sub- silicon bulk of oxidation；Step 3,
The broken Asia silicon bulk that aoxidizes obtains aoxidizing sub- silicon powder.
2. the preparation method that lithium ion battery as described in claim 1 aoxidizes sub- silicium cathode material, which is characterized in that step 1
In, the micron or submicron order silicon powder can be by chemical vapour deposition techniques, sol-gel method, magnetron sputtering technique, true
Empty coating technique, laser/electrical discharge machining and magnesiothermic reduction technology obtain, average grain diameter control 100nm~10 μm it
Between.
3. the preparation method that lithium ion battery as described in claim 1 aoxidizes sub- silicium cathode material, which is characterized in that step 1
In, it is described by the atmosphere of micron or submicron order silicon powder high-temperature process be air or oxygen.
4. the preparation method that lithium ion battery as described in claim 1 aoxidizes sub- silicium cathode material, which is characterized in that step 1
In, it is described by the temperature of micron or submicron order silicon powder high-temperature process at 500~700 DEG C.
5. the preparation method that lithium ion battery as described in claim 1 aoxidizes sub- silicium cathode material, which is characterized in that step 1
In, it is described by the time of micron or submicron order silicon powder high-temperature process be 20~500min.
6. the preparation method that lithium ion battery as described in claim 1 aoxidizes sub- silicium cathode material, which is characterized in that step 1
In, it is described to keep a certain amount of silicon dioxide layer of its Surface Creation fine and close, with a thickness of 1.0~50nm.
7. the preparation method that lithium ion battery as described in claim 1 aoxidizes sub- silicium cathode material, which is characterized in that step 1
In, described to keep a certain amount of silicon dioxide layer of its Surface Creation fine and close, the Control for Oxygen Content of the material is in 20-45%.
8. the preparation method that lithium ion battery as described in claim 1 aoxidizes sub- silicium cathode material, which is characterized in that step 2
In, described continue thereafter with increases temperature and keeps it under vacuum state, and temperature range is at 1200~1600 DEG C, heating
Between for 0.5~for 24 hours.
9. the preparation method that lithium ion battery as described in claim 1 aoxidizes sub- silicium cathode material, which is characterized in that step 2
In, described continue thereafter with increases temperature and keeps it under vacuum state, and vacuum degree is in 500~1500pa.
10. the preparation method that lithium ion battery as described in claim 1 aoxidizes sub- silicium cathode material, it is characterised in that the powder
Broken to obtain aoxidizing sub- silicon powder, disintegrating apparatus is planetary ball mill, mechanical crusher, super-low temperature pulverizator, superheated steam crushing
Any one in machine or airslide disintegrating mill, its particle size is at 2.0~15 μm after crushing；Contain in the obtained silica
Monocrystalline and/or polycrysalline silcon；Before step 1, need to micron or submicron order silicon powder using sodium hydroxide etching processing.
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Cited By (12)
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| CN109650858A (en) * | 2018-12-18 | 2019-04-19 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of silicon oxygen negative electrode material and products thereof and application |
| CN110357111A (en) * | 2019-07-11 | 2019-10-22 | 苏州大学 | Oxidation Asia silicium cathode material based on silicon ash, preparation method and lithium ion battery |
| CN110854377A (en) * | 2019-12-05 | 2020-02-28 | 中南大学 | Porous silica composite material and preparation and application thereof |
| CN110993907A (en) * | 2019-11-25 | 2020-04-10 | 宁波广新纳米材料有限公司 | Preparation method of nanocrystalline silicon-silicon monoxide-carbon composite powder |
| CN111082006A (en) * | 2019-12-06 | 2020-04-28 | 深圳市比克动力电池有限公司 | Silicon monoxide composite negative electrode material, preparation method thereof and lithium ion battery |
| CN111900366A (en) * | 2020-07-02 | 2020-11-06 | 有研资源环境技术研究院(北京)有限公司 | SiO containing lithiumxMethod for preparing powder |
| CN111969196A (en) * | 2020-08-05 | 2020-11-20 | 有研资源环境技术研究院(北京)有限公司 | Nano flaky silicon oxide and composite negative electrode material thereof |
| CN112701270A (en) * | 2020-12-28 | 2021-04-23 | 宁德新能源科技有限公司 | Negative electrode material, pole piece containing negative electrode material and electrochemical device |
| CN113571678A (en) * | 2021-06-24 | 2021-10-29 | 惠州锂威新能源科技有限公司 | Preparation method of negative electrode material, product and application |
| CN113735572A (en) * | 2021-08-24 | 2021-12-03 | 王立卓 | Preparation method of magnesium-containing silicon monoxide |
| CN113998702A (en) * | 2021-10-13 | 2022-02-01 | 昆明理工大学 | Method for preparing Si/C negative electrode material by using micro silicon powder as raw material |
| CN116332193A (en) * | 2023-05-18 | 2023-06-27 | 深圳软硅材料科技有限公司 | Method for sintering silicon-oxygen negative electrode material |
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| CN110357111A (en) * | 2019-07-11 | 2019-10-22 | 苏州大学 | Oxidation Asia silicium cathode material based on silicon ash, preparation method and lithium ion battery |
| CN110993907B (en) * | 2019-11-25 | 2021-05-07 | 宁波广新纳米材料有限公司 | Preparation method of nanocrystalline silicon-silicon monoxide-carbon composite powder |
| CN110993907A (en) * | 2019-11-25 | 2020-04-10 | 宁波广新纳米材料有限公司 | Preparation method of nanocrystalline silicon-silicon monoxide-carbon composite powder |
| CN110854377A (en) * | 2019-12-05 | 2020-02-28 | 中南大学 | Porous silica composite material and preparation and application thereof |
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| CN113571678A (en) * | 2021-06-24 | 2021-10-29 | 惠州锂威新能源科技有限公司 | Preparation method of negative electrode material, product and application |
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| CN113998702A (en) * | 2021-10-13 | 2022-02-01 | 昆明理工大学 | Method for preparing Si/C negative electrode material by using micro silicon powder as raw material |
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Application publication date: 20181207 |