CN108400302A - A method of it purifying silicon from silicon carbide waste and prepares its compound as electrode material - Google Patents
A method of it purifying silicon from silicon carbide waste and prepares its compound as electrode material Download PDFInfo
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Abstract
The invention discloses a kind of from silicon carbide waste purification silicon and prepares method of its compound as electrode material.Using spray pyrolysis process, it is silicon by silicon carbide deacidizing in waste material, it is simultaneously that silicon is compound with graphene, silicon is that the spherical clusters pattern formed is assembled by silicon particle, there is " spitball " structure with the compound that reduced graphene is prepared after compound, it is embodied in the surface that fold is formed with graphene coated silicon.The silicon of preparation makees electrode material with graphene complex, its silicon is 200nm~1500nm with graphene complex size, pattern is chondritic, surface is graphene coated silicon, and have fold " spitball " structure as lithium ion battery negative material, 500~3000mAh/g of its specific discharge capacity after 20 circle cycles.Waste material and waste liquid will not be generated in the technical operating procedure again, it is environmentally friendly.The technique has many advantages, such as that equipment is simple, can amplify production, is pollution-free, zero-emission.
Description
Technical field
The invention belongs to field of inorganic nano material, and in particular to a kind of to purify silicon with spray pyrolysis and to prepare its compound
Object is used as the method for lithium ion battery electrode material.
Background technology
Contemporary mankind has been difficult to meet increasingly increasing of the society to the energy to the exploitation and supply of traditional energy oil, coal etc.
Long demand, energy crisis are the research hotspots of present society.In numerous new energy, solar energy is used as green, environmental protection, without dirt
Dye, inexhaustible clean energy resource make photovoltaic industry enter quick period of expansion.The quick hair of semiconductor silicon industry simultaneously
Exhibition also makes high-purity silicon material be quickly widely applied.However monocrystalline silicon and polysilicon required in two kinds of industries exists
Cutting processing is needed during use, about 50% HIGH-PURITY SILICON has entered mortar in the form of sawing material in the process,
As waste material.So that at present, photovoltaic and semiconductor industry cost are higher, are difficult to the universal use of large area.It is mainly wrapped in waste material
It includes：Silicon carbide, polyethylene glycol, silicon, metal impurities etc..At present both at home and abroad in waste material polyethylene glycol and silicon carbide formed compared with
Ripe technique, but to the recycling of silicon still in development phase, prior art processes are complicated, energy consumption is big, be easy to cause secondary dirt
Dye, and the purity that recycles silicon it is not high-leveled and difficult to meet photovoltaic, semiconductor applications are applied again.How simply and effectively to extract useless
Silicon in material and it is converted into useful commercial, realizes that recovery process maximizing the benefits is current area research blank.
Invention content
It is used as electrode material the purpose of the present invention is purifying silicon with simple technique and preparing its compound.The process equipment
Simply, the advantages that production, pollution-free, zero-emission can be amplified.
Purification silicon provided by the invention and the method for preparing its compound, the technique used is spray pyrolysis process.Not only
It can be silicon by silicon carbide deacidizing in waste material, while silicon is compound with graphene, improve the electric conductivity of silicon electrode, inhibit silicon electrode
Volume expansion in charge and discharge process.This method purification silicon be that the spherical clusters pattern formed is assembled by silicon particle, with also
The compound prepared after former graphene is compound has " spitball " structure, is embodied in graphene coated silicon, forms fold
Surface, and at spherical morphology.
Technical scheme is as follows：
A method of it purifying silicon from silicon carbide waste and prepares its compound；It is characterized in that using spray pyrolysis process,
It is silicon by silicon carbide deacidizing in waste material, while silicon is compound with graphene, silicon is that the spherical clusters shape formed is assembled by silicon particle
Looks have " spitball " structure with the compound that reduced graphene is prepared after compound, are embodied in graphene coated silicon, are formed
The surface of fold.
This technique purifies silicon from silicon carbide waste and prepares its compound, and technique is to remove waste material by preliminary processing
Going metal impurities to obtain silicon and the mixture of silicon carbide becomes raw material, on the one hand directly mixes raw material with graphene oxide solution
Uniformly, the compound for silicon and graphene is heat-treated by the method for spray pyrolysis simultaneously in silicon carbide and graphene oxide, it should
Compound has many advantages, such as " spitball " structure, and being used as lithium ion battery negative material has high power capacity, long circulating.
On the other hand it is divided into the progress of two steps, the first step purifies silicon by the method for spray pyrolysis from raw material first, can be with
The uniform spherical clusters shape silicon of size is obtained, then the spray pyrolysis again after mixing by silicon and graphene oxide solution
It is compound to prepare silicon and graphene complex, equally there is " spitball structure " may be used as lithium ion battery negative material.
It is described as follows：
Method 1 is that waste material is removed metal impurities by preliminary processing to obtain the mixture of silicon and silicon carbide as original
Material, raw material, which is dissolved in deionized water, forms material solution, and material solution and graphene oxide solution are directly mixed to form raw material
With the mixed solution of graphene oxide, heat-treat simultaneously as silicon in silicon carbide and graphene oxide by the method for spray pyrolysis and
The compound of graphene, compound have " spitball " structure.
Preferred operations are：It takes wasted powder to be impregnated in the acid solution of 0.1~12M, removes the metal impurities in solution, wash
Suction filtration is washed, filter cake vacuum is dried to obtain silicon and silicon carbide blend raw material for 80 DEG C.Then it adds the raw material into certain solution
Form the mixed solution of a concentration of 5~30mg/mL.It is with graphene oxide content with graphene oxide solution by material solution
The ratio of 0.1~1.0wt% is mixed to get mixed solution.Mixed solution is added in atomizing generator, supersonic frequency 0.5
Droplet is added in the boiler tube of tube furnace by inert gas and is heat-treated by~2.4MHz, and flow velocity is 0.5~10L/min.
Heating temperature is 300~900 DEG C, and the product in exit is collected using polymeric membrane or electrostatic trap, is silicon and graphene
Compound.Finally its chemical property is tested as lithium ion battery negative material.
Method 2 is that silicon is purified from raw material by the method for spray pyrolysis first, obtains spherical clusters shape silicon, then will carry
Pure silicon powder is dissolved in the solution that deionized water forms silicon, finally is uniformly mixed to form silicon with graphene oxide solution by the solution of silicon
With the mixed solution of graphene oxide, then by mixed solution, spray pyrolysis is compound again prepares silicon and graphene complex, multiple
Closing object has " spitball " structure.
Preferred operations are：It takes wasted powder to be impregnated in the acid solution of 0.1~12M, removes the metal impurities in solution, wash
Suction filtration is washed, filter cake vacuum is dried to obtain silicon and silicon carbide blend raw material for 80 DEG C；Add raw materials into deionized water formed it is dense
Degree be 5~30mg/mL material solutions, then material solution is added in atomizing generator, supersonic frequency be 0.5~
Droplet is added in the boiler tube of tube furnace by argon gas and is heat-treated by 2.4MHz, and flow velocity is 0.5~10L/min.Heating temperature
Degree is 300~900 DEG C, and the product in exit is collected using polymeric membrane or electrostatic trap, for spherical silicon；By spherical silicon
Be dissolved in deionized water formation silicon solution, then with graphene oxide solution according to be 0.1 with graphene oxide content~
The ratio of 1.0wt% obtains the mixed solution of silicon and graphene oxide after mixing.Mixed solution is added to atomization hair again
In raw device, supersonic frequency is 0.5~2.4MHz, and droplet is added in the boiler tube of tube furnace by inert gas and carries out heat also
Original, flow velocity are 0.5~10L/min.Heating temperature is 300~900 DEG C, and outlet is collected using polymeric membrane or electrostatic trap
The product at place is silicon and graphene complex.
Waste material comes from the waste material silicon generated in photovoltaic industry process；Waste material silicon includes silicon carbide, silicon, polyethylene glycol
Or iron filings.
Soaking time is 5~300min in the acid of a concentration of 0.1~12M；Acid used in wherein is preferably hydrochloric acid, sulfuric acid
Or nitric acid.Purpose is away the metallic element in waste material.
It is preferred that solution solvent is water or ethyl alcohol.
It is preferred that being imported droplet in tube furnace by inert gas, inert gas includes argon gas, nitrogen or helium, and flow velocity is
0.5~10L/min.
Silicon prepared by this method is used as lithium ion battery negative material with graphene complex, and compound size is
200nm~1500nm, specific discharge capacity are 500~3000mAh/g.
Waste material and waste liquid will not be generated in the invention operating process again, it is environmentally friendly.The technique has equipment letter
It is single, production can be amplified, is pollution-free, zero-emission the advantages that；It is with a wide range of applications.
Description of the drawings
Fig. 1 is the XRD spectrum that embodiment 1 prepares silicon and graphene complex；
Fig. 2 is the scanned photograph of the silicon and graphene complex of different graphene contents prepared by embodiment 1, the production of preparation
Object shows as " spitball " structure；
Fig. 3 is the discharge cycles curve of 1 compound of embodiment；
Fig. 4 is the stereoscan photograph that embodiment 2 prepares purification silicon, and product shows as the cluster of particle composition.
Specific implementation mode
Embodiment 1：
Method 1：Take scrap silicon in 0.1M hydrochloric acid solutions, washing filters, and filter cake vacuum is dried to obtain silicon and carbon for 80 DEG C
SiClx mixture material will wash rear raw material 1g and the colloidal suspension that stirring forms solubility as 5mg/ml in 200ml deionized waters is added
Liquid.
Graphene oxide solution prepare reference literature (J.Y.Luo, H.D.Jang, T.Sun, L.Xiao, Z.He,
A.P.Katsoulidis,M.G.Kanatzidis,J.M.Gibson,J.X.Huang.Compression and
aggregation-resistant particles of crumpled soft sheets[J].ACS nano,2011,5
(11),8943-8949.)。
Ratio by material solution and graphene oxide solution with graphene oxide content for 0.1wt% is mixed to get silicon and gives up
The mixed solution of material and graphene oxide.Mixed solution is added in atomizing generator, supersonic frequency 0.5MHz is passed through argon
Droplet is added in the horizontal type boiler tube of tube furnace and heat-treats by gas, flow velocity 0.5L/min.Heating temperature is 300 DEG C, is adopted
The sample in exit is collected with polymeric membrane.Fig. 1 is to prepare sample XRD spectrum, is the diffraction maximum of elementary silicon, illustrates silicon carbide
Through being reduced to silicon, Fig. 2 is the SEM photograph for preparing compound, is " spitball " spherical morphology, size is relatively uniform, and size exists
200nm or so, finally tests its chemical property as lithium ion battery negative material, and Fig. 3 explanations are recycled by 60 circles
Specific discharge capacity is 1500mAh/g afterwards.
Embodiment 2：
Method 2：Take scrap silicon in 2M hydrochloric acid solutions, washing filters, and filter cake vacuum is dried to obtain silicon and carbonization for 80 DEG C
Silicon mixture material adds raw materials into deionized water solution and forms a concentration of 5mg/mL, and material solution is then added to atomization
In generator, droplet is added in the boiler tube of tube furnace by argon gas and is heat-treated by supersonic frequency 0.5MHz, and flow velocity is
2L/min.Heating temperature is 300 DEG C, and electrostatic trap collects the product in exit, for spherical silicon.By the provable preparations of Fig. 4
Silicon particle size in 1500nm or so.Graphene oxide solution prepares reference implementation example 1.
Silicon after purification is dissolved in the aqueous solution that deionized water forms silicon, then with graphene oxide solution according to aoxidize stone
Black alkene content is that the ratio of 1wt% is mixed to get the mixed solution of uniform silicon and graphene oxide.Mixed solution is added again
Into atomizing generator, droplet is added in the boiler tube of tube furnace by argon gas and is heat-treated by supersonic frequency 2.4MHz,
Flow velocity is 10L/min.Heating temperature is 900 DEG C, and the sample in exit is collected using electrostatic trap, and resulting composite size is big
It is small in 1500nm or so.Its chemical property finally is tested as lithium ion battery negative material, into after crossing 60 circle cycles
Specific discharge capacity is in 500mAh/g.
Embodiment 3：
Method 1：Take scrap silicon in 3M hydrochloric acid solutions, washing filters, and filter cake vacuum is dried to obtain silicon and carbonization for 80 DEG C
Silicon mixture material will wash rear raw material and form soliquid according to stirring in a concentration of 30mg/ml addition deionized waters.Oxidation
Graphene solution prepares embodiment 1.
Material solution and graphene oxide solution are mixed to get with graphene oxide solution content for the ratio of 0.5wt%
The mixed solution of scrap silicon and graphene oxide.Mixed solution is added in atomizing generator, supersonic frequency 2.0MHz, is led to
Enter nitrogen and be added to droplet in the horizontal type boiler tube of tube furnace to heat-treat, flow velocity 5.0L/min.Heating temperature is 600
DEG C, using polymeric membrane collection exit at sample, sample size size is 750nm or so.Finally as lithium ion
Cell negative electrode material tests its chemical property, and specific discharge capacity is 760mAh/g after 20 circle cycles.
Embodiment 4：
Method 1：Take scrap silicon in 12M hydrochloric acid solutions, washing filters, and filter cake vacuum is dried to obtain silicon and carbonization for 80 DEG C
Silicon mixture material will wash rear raw material and form soliquid according to stirring in a concentration of 20mg/ml addition deionized waters.Oxidation
Graphene solution prepares embodiment 1.
It is molten that ratio by material solution and graphene oxide solution with graphene oxide content for 1wt% is mixed to get mixing
Liquid.Mixed solution is added in atomizing generator, supersonic frequency 2.4MHz is passed through nitrogen and droplet is added to tube furnace
It is heat-treated in horizontal type boiler tube, flow velocity 2L/min.Heating temperature is 500 DEG C, and the sample in exit is collected using polymeric membrane
Product, sample size size are 1000nm or so.Finally its chemical property is tested as lithium ion battery negative material, 20
Specific discharge capacity is 1300mAh/g after circle cycle.
Embodiment 5：
Method 2：Take scrap silicon in 12M hydrochloric acid solutions, washing filters, and filter cake vacuum is dried to obtain silicon and carbonization for 80 DEG C
Silicon mixture material adds raw materials into stirring in deionized water and forms the soliquid that solubility is 30mg/ml.Then by raw material
Solution is added in atomizing generator, supersonic frequency 0.7MHz, droplet is added to by argon gas in the boiler tube of tube furnace into
Row thermal reduction, flow velocity 1.2L/min.Heating temperature is 500 DEG C, and electrostatic trap collects the product in exit, is spherical
Silicon.Silicon particle size is in 550nm or so.Graphene oxide solution prepares reference implementation example 1.
Silicon after purification is dissolved in the aqueous solution that deionized water forms silicon, by silicon solution and graphene oxide solution according to oxygen
The ratio that graphite alkene content is 0.5wt%, which is added in solution, obtains mixed solution.Mixed solution is added to atomization again
In generator, droplet is added in the boiler tube of tube furnace by argon gas and is heat-treated by supersonic frequency 0.9MHz, and flow velocity is
1.2L/min.Heating temperature is 600 DEG C, and the sample in exit is collected using electrostatic trap, and resulting composite size exists
760nm or so.Its chemical property finally is tested as lithium ion battery negative material, the ratio that discharges is enclosed after cycle into crossing 50
Capacity is in 1645mAh/g.
Embodiment 6：
Method 2：Take scrap silicon in 8M hydrochloric acid solutions, washing filters, and filter cake vacuum is dried to obtain silicon and carbonization for 80 DEG C
Silicon mixture material adds raw materials into stirring in deionized water and forms the soliquid that solubility is 18mg/ml.Then by raw material
Solution is added in atomizing generator, supersonic frequency 2.4MHz, droplet is added to by helium in the boiler tube of tube furnace into
Row thermal reduction, flow velocity 2L/min.Heating temperature is 900 DEG C, and polymeric membrane collects the product in exit, for spherical silicon.Silicon
Granular size is in 900nm or so.Graphene oxide solution prepares reference implementation example 1.
Silicon after purification is dissolved in the aqueous solution that deionized water forms silicon, is by silicon solution and graphene oxide solution content
The ratio of 1.0wt% is added in solution and obtains mixed solution.Mixed solution is added in atomizing generator again, supersonic frequency
Rate is 2.4MHz, and droplet is added in the boiler tube of tube furnace by helium and is heat-treated, flow velocity 2L/min.Heating temperature
It is 900 DEG C, the sample in exit is collected using electrostatic trap, resulting composite size is in 1012nm or so.Finally will
It tests its chemical property as lithium ion battery negative material, and specific discharge capacity is in 1460mAh/g into after crossing 50 circle cycles.
What the present invention was disclosed and proposed a kind of from silicon carbide waste purify silicon and prepares its compound as electrode material
Method.Those skilled in the art can be by using for reference present disclosure, and the appropriate links such as condition route that change are realized, although the present invention
Method and technology of preparing are described by preferred embodiment, and related technical personnel can obviously not depart from the present invention
Hold, methods and techniques described herein route is modified or is reconfigured in spirit and scope, to realize final preparation
Technology.In particular, it should be pointed out that all similar replacements and change are apparent to those skilled in the art,
They are considered as being included in spirit of that invention, range and content.
Claims (10)
1. a kind of method for purifying silicon from silicon carbide waste and preparing its compound；It is characterized in that using spray pyrolysis process, it will
Silicon carbide deacidizing is silicon in waste material, while silicon is compound with graphene, and silicon is that the spherical clusters pattern formed is assembled by silicon particle,
There is " spitball " structure with the compound that reduced graphene is prepared after compound, be embodied in graphene coated silicon, form pleat
The surface of wrinkle.
2. the method as described in claim 1, it is characterized in that by waste material by preliminary processing remove metal impurities obtain silicon with
The mixture of silicon carbide becomes raw material, is directly uniformly mixed raw material with graphene oxide solution to form mixing for raw material and graphene
Solution is closed, the compound for silicon and graphene is heat-treated by the method for spray pyrolysis simultaneously in silicon carbide and graphene oxide,
Compound has " spitball " structure.
3. method as claimed in claim 2, it is characterized in that：It takes wasted powder to be impregnated in the acid solution of 0.1~12M, washs
It filters, filter cake vacuum is dried to obtain silicon and silicon carbide blend raw material for 80 DEG C；Then shape in deionized water is added the raw material into
At the material solution of a concentration of 5~30mg/mL；By material solution and graphene oxide solution with graphene oxide content for 0.1
The ratio of~1.0wt% is mixed to get the mixed solution of raw material and graphene oxide；Mixed solution is added to atomizing generator
In, supersonic frequency is 0.5~2.4MHz, and droplet is loaded into the boiler tube of tube furnace by inert gas and is heat-treated,
Flow velocity is 0.5~10L/min；Heating temperature is 300~900 DEG C, and exit is collected using polymeric membrane or electrostatic trap
Product, be silicon and graphene complex.
4. the method as described in claim 1 obtains it is characterized in that purifying silicon from raw material by the method for spray pyrolysis first
Silicon is dissolved in the colloidal solution for forming silicon in deionized water, is then uniformly mixed with graphene oxide solution by spherical clusters shape silicon
The mixed solution of silicon and graphene oxide is formed afterwards, and spray pyrolysis is compound again prepares silicon and graphene complex, compound tool
There is " spitball " structure.
5. method as claimed in claim 4, it is characterized in that：It takes wasted powder to be impregnated in the acid solution of 0.1~12M, washs
It filters, filter cake vacuum is dried to obtain silicon and silicon carbide blend raw material for 80 DEG C；It adds raw materials into and forms concentration in deionized water
For 5~30mg/mL material solutions；Then material solution being added in atomizing generator, supersonic frequency is 0.5~2.4MHz,
Droplet is added in the boiler tube of tube furnace by inert gas and is heat-treated, flow velocity is 0.5~10L/min；Heating temperature
It is 300~900 DEG C, the product in exit is collected using polymeric membrane or electrostatic trap, for spherical silicon；Silicon is dissolved in
In ionized water formed silicon colloidal solution, then with graphene oxide solution according to graphene oxide content be 0.1~
The ratio of 1.0wt% forms the mixed solution of silicon and graphene oxide after mixing；Mixed solution is added to atomization hair again
In raw device, supersonic frequency is 0.5~2.4MHz, and droplet is added in the boiler tube of tube furnace by inert gas and carries out heat also
Original, flow velocity are 0.5~10L/min；Heating temperature is 300~900 DEG C；Outlet is collected using polymeric membrane or electrostatic trap
The product at place is silicon and graphene complex.
6. the method as described in claim 1, it is characterized in that waste material comes from the waste material silicon generated in photovoltaic industry process；
Waste material silicon includes silicon carbide, silicon, polyethylene glycol or iron filings.
7. the method as described in claim 3 or 5, it is characterized in that in the acid of a concentration of 0.1~12M soaking time be 5~
300min；Acid used in wherein is hydrochloric acid, sulfuric acid or nitric acid.
8. the method as described in claim 3 or 5, it is characterized in that solution solvent is water or ethyl alcohol.
9. the method as described in claim 3 or 5, it is characterized in that being imported droplet in tube furnace by inert gas, indifferent gas
Body includes argon gas, nitrogen or helium, and flow velocity is 0.5~10L/min.
10. silicon prepared by method described in claim 1 makees electrode material, silicon and graphene complex with graphene complex
Size is 200nm~1500nm, and pattern is chondritic, and surface is graphene coated silicon, and has fold " spitball " structure
As lithium ion battery negative material, 500~3000mAh/g of its specific discharge capacity after 20 circle cycles.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105336922A (en) * | 2014-08-08 | 2016-02-17 | 苏州格瑞动力电源科技有限公司 | Preparation method and application for lithium ion battery negative electrode material based on photovoltaic silicon waste material |
| CN105752988A (en) * | 2016-03-02 | 2016-07-13 | 安徽正丰再生资源有限公司 | Recycling method of high-purity silicon carbide and silicon |
| CN105990568A (en) * | 2014-12-12 | 2016-10-05 | 韩国地质资源研究院 | Method for recovering of silicon particles, and manufacturing of cathode material for secondary battery |
| WO2017027831A1 (en) * | 2015-08-13 | 2017-02-16 | The Regents Of The University Of California | Lithium sulfide electrode and method |
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2018
- 2018-02-23 CN CN201810155059.6A patent/CN108400302A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105336922A (en) * | 2014-08-08 | 2016-02-17 | 苏州格瑞动力电源科技有限公司 | Preparation method and application for lithium ion battery negative electrode material based on photovoltaic silicon waste material |
| CN105990568A (en) * | 2014-12-12 | 2016-10-05 | 韩国地质资源研究院 | Method for recovering of silicon particles, and manufacturing of cathode material for secondary battery |
| WO2017027831A1 (en) * | 2015-08-13 | 2017-02-16 | The Regents Of The University Of California | Lithium sulfide electrode and method |
| CN105752988A (en) * | 2016-03-02 | 2016-07-13 | 安徽正丰再生资源有限公司 | Recycling method of high-purity silicon carbide and silicon |
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Application publication date: 20180814 |