CN106744985A - Silicon monoxide nano material and preparation method thereof - Google Patents
Silicon monoxide nano material and preparation method thereof Download PDFInfo
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- CN106744985A CN106744985A CN201611254324.3A CN201611254324A CN106744985A CN 106744985 A CN106744985 A CN 106744985A CN 201611254324 A CN201611254324 A CN 201611254324A CN 106744985 A CN106744985 A CN 106744985A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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Abstract
The invention discloses a kind of silicon monoxide nano material and preparation method thereof, material of the present invention includes following raw material：90 120 parts of Buddha's warrior attendant wire cutting silica flour, 20 30 parts of millimeter level polysilicon powder, 0 90 parts of silicon oxide compound.The inventive method；By raw material, wet method or dry method are mixed in proportion, and dry pack is put into crucible, and one layer of millimeter level polysilicon powder of uniform fold, delivers to vacuum drying oven on compound；Vavuum pump is opened, 400 700 DEG C, negative pressure heat preservation certain hour, control vacuum 500pa 1000pa are warming up to；Argon tanks are opened, above-mentioned negative pressure and vacuum is maintained, temperature is rapidly heated and maintains for 1,300 1400 DEG C, argon flow amount is controlled for 0.5L/min 10L/min, condensation collecting tank is opened, 100 200 DEG C are maintained the temperature at；Reaction is lowered the temperature after terminating, and closes vacuum, when vacuum drying oven is with the vacuum of collecting tank is condensed to normal pressure, closes argon tanks, obtains final product the silicon monoxide nano material, and particle diameter is 30 100nm.
Description
Technical field
The invention belongs to silica technical field, more particularly to a kind of silicon monoxide nano material and preparation method thereof.
Background technology
In photovoltaic industry chain, the silicon raw material for having 40% to 50% is cut into silica flour chip, its total amount reach tens thousand of tons/
Year.As technology is constantly reformed, silicon chip cutting main flow direction is Buddha's warrior attendant wire cutting, and the silica flour particle diameter of which cutting is smaller, category
In sub-micrometer range, with activity very high.Due to the surface oxidation in cutting and last handling process, while containing in powder
Other impurity such as diamond, metal object, toner, therefore in the recycling of silica flour, have no compared with high added value direction.
The cutting silica flour particle diameter of photovoltaic industry is small, active high, interior uclear purity is high, while in the market has substantial amounts of supply,
Price is low, and the recycling of the raw material can substantially reduce the production cost of lithium battery silicon-carbon negative electrode material.
Silicon monoxide nano material possesses theoretical specific capacity (1400Ahg higher-1More than), the characteristic with nanometer particle size
Reduce the violent Volume Changes in charge and discharge process.Therefore, silicon monoxide nano material is prepared using Buddha's warrior attendant wire cutting silica flour
With important economic worth and environmental value.
The content of the invention
The present invention provides silicon monoxide nano material and its preparation side to solve technical problem present in known technology
Method, greatly reduces the preparation cost of high-purity silicon monoxide, while solving the problem of environmental pollution that silica flour chip is caused.
In order to solve the above-mentioned technical problem, the technical solution adopted by the present invention is：
A kind of silicon monoxide nano material, including following weight portion raw material：90-120 parts of Buddha's warrior attendant wire cutting silica flour, millimeter
20-30 parts, silicon oxide compound 0-90 parts of level polysilicon powder.
The particle diameter of the Buddha's warrior attendant wire cutting silica flour is D50=0.5-0.8um；The particle diameter of the millimeter level polysilicon powder is
D50=2-5mm, the particle diameter of the silicon oxide compound is D50=20-50nm.
The silicon oxide compound is the one kind in gas-phase silica, silica flour, nonmetallic ion type Ludox or lithium metasilicate.
The preparation method of above-mentioned silicon monoxide nano material, comprises the following steps：
(1) by Buddha's warrior attendant wire cutting silica flour, millimeter level polysilicon powder is mixed using wet method or dry method in proportion with silicon oxide compound
Close uniform, the compound that wherein wet method is mixed must remove moisture removal through drying；
(2) above-mentioned dry pack is put into crucible, one layer of millimeter level polysilicon of uniform fold again on compound
Powder, delivers to vacuum drying oven；
(3) vavuum pump is opened, 400-700 DEG C is warming up to, negative pressure heat preservation certain hour controls vacuum for 500pa-
1000pa, the moisture and organic impurities remained in removal material；
(4) argon gas warmup heater is opened, argon tanks are opened, to argon gas is passed through in vacuum drying oven, above-mentioned negative pressure and true is maintained
Reciprocal of duty cycle, it is 1300-1400 DEG C to be rapidly heated and maintain temperature vacuum drying oven, temperature-rise period regulation argon gas tank valve, controls argon gas
Flow is 0.5L/min-10L/min, opens condensation collecting tank, opens condensation collecting tank exhaust outlet, keeps condensation collecting tank temperature
At 100-200 DEG C；
(5) lower the temperature after reaction terminates, close vacuum, when vacuum drying oven is with the vacuum of collecting tank is condensed to normal pressure, close argon
Gas tank, obtains final product the silicon monoxide nano material.
The mode of wet-mixing is in the step (1)：Raw material is mixed in high purity water, with 800-2000rpm/min's
Rotating speed high-speed stirred 0.5-1.5 hours, the slurry diaphragm filter press after mixing removes moisture removal, forms filter cake, and filter cake is by scraping
Piece film drier is dried, and forms uniform dry pack.
Keep material loose when compound is put into crucible in the step (2), the thickness of the millimeter level polysilicon powder of covering
It is 20mm.
Pressure is -900-20KPa in the step (3), and soaking time is 0.5-1.5 hours.
The method that is passed through of argon gas is in the step (4)：Crucible bottom is provided with porous ceramic filter, tunger tube connection
Porous ceramic filter bottom interface, argon gas is passed through from the porous ceramic filter of compound bottom, porous ceramic filter hole
Footpath size is 1-5um.
The Buddha's warrior attendant wire cutting silica flour first passes through treatment in advance, to remove organic impurities and metal impurities.
The mode of heating of the vacuum drying oven is resistance heating, sensing heating, electric arc heated, electron beam heating or heating using microwave
In one kind.
Principle of the invention is as follows：
Buddha's warrior attendant wire cutting silica flour is a kind of kernel high-purity material with excellent activity, and metallic silicon is with silica in high temperature
Under disproportionated reaction can occur, the distillation of product silicon monoxide exists in a gaseous form.
Si(S)+SiO2(S)======2SiO(g)
The present invention has the advantages and positive effects that：
(1) the Buddha's warrior attendant wire cutting silica flour using particle diameter in sub-micrometer range, with larger specific surface area, therefore has non-
Often activity high, effectively reduces the reaction time, substantially reduces energy consumption, while solve the environmental pollution that silica flour chip causes asking
Topic.
(2) raw silicon powder footpath is smaller, is easily pumped during vacuumizing, by porous ceramic filter and milli
The iris action of meter level polycrystalline silica flour is solved, and in raw material bottom is passed through high temperature argon, argon gas flow control, it is to avoid diamond wire
Silica flour is taken away by vavuum pump, and porous ceramic filter disperses beneficial to gas in raw material inner homogeneous, reduces material agglomeration, together
Shi Tianjia millimeters of level polysilicon powder is conducive to the silicon monoxide distilled after reaction to be escaped upwards from hole so as to form uniform pores
Go out, greatly improve the effusion rate of silicon monoxide.
(3) the flow control of high-purity argon gas and the temperature control of condensation collecting tank can effectively control silicon monoxide nanometer
The particle diameter and reduction disproportionated reaction of material.
(4) preparation method of silicon monoxide nano material of the invention, using evaporative condenser technique, significantly improves reaction
Rate, preparing raw material is easy to get, low production cost, it is easy to large-scale industrial production；The silicon monoxide nano material purity of preparation
Height, particle diameter is 30-100nm.
Brief description of the drawings
Fig. 1 is silicon monoxide nano material SEM electron microscopes of the invention.
Specific embodiment
For the content of the invention of the invention, feature and effect can be further appreciated that, following examples are hereby enumerated, and coordinate accompanying drawing
Describe in detail as follows：
A kind of silicon monoxide nano material, including following weight portion raw material：90-120 parts of Buddha's warrior attendant wire cutting silica flour, millimeter
20-30 parts, silicon oxide compound 0-90 parts of level polysilicon powder.
The particle diameter of Buddha's warrior attendant wire cutting silica flour is D50=0.5-0.8um；The particle diameter of millimeter level polysilicon powder is D50=2-
5mm, the particle diameter of silicon oxide compound is D50=20-50nm.
Silicon oxide compound is the one kind in gas-phase silica, silica flour, nonmetallic ion type Ludox or lithium metasilicate.
The preparation method of above-mentioned silicon monoxide nano material, comprises the following steps：
(1) by Buddha's warrior attendant wire cutting silica flour, millimeter level polysilicon powder is mixed using wet method or dry method in proportion with silicon oxide compound
Close uniform, the compound that wherein wet method is mixed must remove moisture removal through drying.
(2) above-mentioned dry pack is put into crucible, one layer of millimeter level polysilicon of uniform fold again on compound
Powder, delivers to vacuum drying oven.
(3) vavuum pump is opened, 400-700 DEG C is warming up to, negative pressure heat preservation certain hour controls vacuum for 500pa-
1000pa, the moisture and organic impurities remained in removal material, it is to avoid the presence of impurity is impacted to product purity, is carried with this
High product quality.
(4) argon gas warmup heater is opened, argon tanks are opened, to argon gas is passed through in vacuum drying oven, above-mentioned negative pressure and true is maintained
Reciprocal of duty cycle, it is 1300-1400 DEG C to be rapidly heated and maintain temperature vacuum drying oven, temperature-rise period regulation argon gas tank valve, controls argon gas
Flow is 0.5L/min-10L/min, opens condensation collecting tank, opens condensation collecting tank exhaust outlet, keeps condensation collecting tank temperature
At 100-200 DEG C；Condensation collecting tank connects online monitor, according to every M3Monitored containing silicon monoxide granule number in gas anti-
Answer situation.
(5) lower the temperature after reaction terminates, close vacuum, when vacuum drying oven is with the vacuum of collecting tank is condensed to normal pressure, close argon
Gas tank, obtains final product silicon monoxide nano material.
The mode of wet-mixing is in step (1)：Raw material is mixed in high purity water, with the rotating speed of 800-2000rpm/min
High-speed stirred 0.5-1.5 hours, the slurry diaphragm filter press after mixing removed moisture removal, formed filter cake, and filter cake is thin by scraping blade
Film drier is dried, and forms uniform dry pack.
Holding material is loose when compound is put into crucible in step (2), and the thickness of the millimeter level polysilicon powder of covering is
20mm。
Pressure is -900-20KPa in step (3), and soaking time is 0.5-1.5 hours.
The method that is passed through of argon gas is in step (4)：Crucible bottom is provided with porous ceramic filter, and tunger tube connection is porous
Ceramic filter bottom interface, argon gas is passed through from the porous ceramic filter of compound bottom, and porous ceramic filter aperture is big
Small is 1-5um.Be conducive to argon gas to be equably passed through, so as to promote silicon monoxide to escape, prevent raw material from sintering frozen plug hole；
High-purity argon gas must be preheated to 1300-1400 DEG C, it is to avoid gaseous state silicon monoxide solidifies；Argon flow amount is covered according to vacuum and upper strata
The thickness regulation of millimeter level polysilicon powder；Porous ceramic filter is silicon carbide porous ceramic filter.
Buddha's warrior attendant wire cutting silica flour first passes through treatment in advance, to remove organic impurities and metal impurities.
The removal of organic impurities is volatilized using organic solvent washing or high temperature sintering in Buddha's warrior attendant wire cutting silica flour, used organic
Solvent is ethanol or acetone.
The removal of metal impurities uses acid treatment in Buddha's warrior attendant wire cutting silica flour, makes its metal impurities less than 100ppm, used
Acid is the one kind in hydrochloric acid, oxalic acid or acetic acid.
The mode of heating of vacuum drying oven be resistance heating, sensing heating, electric arc heated, electron beam heating or heating using microwave in
It is a kind of.
Embodiment 1
120 parts of Buddha's warrior attendant wire cutting silica flour is taken, 30 parts of millimeter level polysilicon powder, dry mixed is uniform, and dry pack is put
Enter bottom to set in the crucible of porous ceramic filter, keep material loose, uniform fold a layer thickness again on compound
It is the millimeter level polysilicon powder of 20mm, delivers to vacuum drying oven；Vavuum pump is opened, 400-700 DEG C is warming up to, pressure is -900-20KPa
Under the conditions of, soaking time is 0.5-1.5 hour, control vacuum for 500pa-1000pa, in removal material the moisture of residual with
Organic impurities；Argon gas warmup heater is opened, argon tanks are opened, to being passed through argon gas in vacuum drying oven, argon gas is from compound bottom
Porous ceramic filter is passed through, and maintains above-mentioned pressure and vacuum, and it is 1300-1400 to be rapidly heated and maintain temperature vacuum drying oven
DEG C, temperature-rise period regulation argon gas tank valve controls argon flow amount for 10L/min, opens condensation collecting tank, opens condensation collecting tank
Exhaust outlet, keeps condensation collecting tank temperature at 100-200 DEG C；Condensation collecting tank connects online monitor, according to every M3In gas
Response situation is monitored containing silicon monoxide granule number；Reaction is lowered the temperature after terminating, and closes vacuum, vacuum drying oven and condensation collecting tank
When vacuum is to normal pressure, argon tanks are closed, obtain final product silicon monoxide nano material, particle diameter is 30nm.
Embodiment 2
90 parts of Buddha's warrior attendant wire cutting silica flour is taken, 20 parts of millimeter level polysilicon powder, 50 parts of silicon oxide compound is mixed in high purity water
In, with rotating speed high-speed stirred 0.5-1.5 hours of 800-2000rpm/min, the slurry diaphragm filter press after mixing goes water removal
Point, filter cake is formed, filter cake is dried by scraping blade film drier, forms uniform dry pack；Dry pack is put into
Bottom is set in the crucible of porous ceramic filter, and holding material is loose, and uniform fold a layer thickness is again on compound
The millimeter level polysilicon powder of 20mm, delivers to vacuum drying oven；Vavuum pump is opened, 400-700 DEG C is warming up to, pressure is -900-20KPa bars
Under part, soaking time is 0.5-1.5 hours, controls vacuum for 500pa-1000pa, removes the moisture of residual in material and has
Machine impurity；Argon gas warmup heater is opened, argon tanks are opened, to argon gas is passed through in vacuum drying oven, argon gas is more from compound bottom
Hole ceramic filter is passed through, and maintains above-mentioned pressure and vacuum, and it is 1300-1400 to be rapidly heated and maintain temperature vacuum drying oven
DEG C, temperature-rise period regulation argon gas tank valve controls argon flow amount for 5L/min, opens condensation collecting tank, opens condensation collecting tank
Exhaust outlet, keeps condensation collecting tank temperature at 100-200 DEG C；Condensation collecting tank connects online monitor, according to every M3In gas
Response situation is monitored containing silicon monoxide granule number；Reaction is lowered the temperature after terminating, and closes vacuum, vacuum drying oven and condensation collecting tank
When vacuum is to normal pressure, argon tanks are closed, obtain final product silicon monoxide nano material, particle diameter is 80nm.
Embodiment 3
90 parts of Buddha's warrior attendant wire cutting silica flour is taken, 20 parts of millimeter level polysilicon powder, 90 parts of silica chemical combination is mixed in high purity water,
With rotating speed high-speed stirred 0.5-1.5 hours of 800-2000rpm/min, the slurry diaphragm filter press after mixing removes moisture removal,
Filter cake is formed, filter cake is dried by scraping blade film drier, form uniform dry pack；Dry pack is put into bottom
Set in the crucible of porous ceramic filter, keep material loose, uniform fold a layer thickness is 20mm again on compound
Millimeter level polysilicon powder, deliver to vacuum drying oven；Vavuum pump is opened, 400-700 DEG C is warming up to, pressure is -900-20KPa conditions
Under, soaking time is 0.5-1.5 hour, control vacuum for 500pa-1000pa, removes the moisture of residual in material and organic
Impurity；Argon gas warmup heater is opened, argon tanks are opened, to argon gas is passed through in vacuum drying oven, argon gas is porous from compound bottom
Ceramic filter is passed through, and maintains above-mentioned pressure and vacuum, and vacuum drying oven is rapidly heated and temperature is maintained for 1300-1400 DEG C,
Temperature-rise period adjusts argon gas tank valve, controls argon flow amount for 0.5L/min, opens condensation collecting tank, opens condensation collecting tank row
Gas port, keeps condensation collecting tank temperature at 100-200 DEG C；Condensation collecting tank connects online monitor, according to every M3Contain in gas
There is silicon monoxide granule number to monitor response situation；Reaction is lowered the temperature after terminating, and closes vacuum, and vacuum drying oven is true with condensation collecting tank
When reciprocal of duty cycle is to normal pressure, argon tanks are closed, obtain final product silicon monoxide nano material, particle diameter is 100nm.
Although being described to the preferred embodiments of the present invention above in conjunction with accompanying drawing, the invention is not limited in upper
The specific embodiment stated, above-mentioned specific embodiment is only schematical, be not it is restricted, this area it is common
Technical staff in the case of present inventive concept and scope of the claimed protection is not departed from, may be used also under enlightenment of the invention
To make many forms, these are belonged within protection scope of the present invention.
Claims (10)
1. a kind of silicon monoxide nano material, it is characterised in that the raw material including following weight portion：Buddha's warrior attendant wire cutting silica flour 90-
120 parts, 20-30 parts, silicon oxide compound 0-90 parts of millimeter level polysilicon powder.
2. silicon monoxide nano material according to claim 1, it is characterised in that the particle diameter of the Buddha's warrior attendant wire cutting silica flour
It is D50=0.5-0.8um；The particle diameter of the millimeter level polysilicon powder is D50=2-5mm, and the particle diameter of the silicon oxide compound is
D50=20-50nm.
3. silicon monoxide nano material according to claim 1, it is characterised in that the silicon oxide compound is gas phase hard charcoal
One kind in black, silica flour, nonmetallic ion type Ludox or lithium metasilicate.
4. a kind of preparation method of silicon monoxide nano material, it is characterised in that comprise the following steps：
(1) by Buddha's warrior attendant wire cutting silica flour, millimeter level polysilicon powder is equal using wet method or dry mixed in proportion with silicon oxide compound
Even, the compound that wherein wet method is mixed must remove moisture removal through drying；
(2) above-mentioned dry pack is put into crucible, one layer of millimeter level polysilicon powder of uniform fold again on compound send
To vacuum drying oven；
(3) vavuum pump is opened, 400-700 DEG C is warming up to, negative pressure heat preservation certain hour controls vacuum for 500pa-1000pa,
The moisture and organic impurities remained in removal material；
(4) argon gas warmup heater is opened, argon tanks are opened, to argon gas is passed through in vacuum drying oven, above-mentioned negative pressure and vacuum is maintained,
Vacuum drying oven is rapidly heated and temperature is maintained for 1300-1400 DEG C, temperature-rise period regulation argon gas tank valve controls the argon flow amount to be
0.5L/min-10L/min, opens condensation collecting tank, opens condensation collecting tank exhaust outlet, keeps condensation collecting tank temperature in 100-
200℃；
(5) lower the temperature after reaction terminates, close vacuum, when vacuum drying oven is with the vacuum of collecting tank is condensed to normal pressure, close argon tanks,
Obtain final product the silicon monoxide nano material.
5. the preparation method of silicon monoxide nano material according to claim 4, it is characterised in that in the step (1)
The mode of wet-mixing is：Raw material is mixed in high purity water, small with the rotating speed high-speed stirred 0.5-1.5 of 800-2000rpm/min
When, the slurry diaphragm filter press after mixing removes moisture removal, forms filter cake, and filter cake is dried by scraping blade film drier, is formed
Uniform dry pack.
6. the preparation method of silicon monoxide nano material according to claim 4, it is characterised in that in the step (2)
Compound keeps material loose when being put into crucible, and the thickness of the millimeter level polysilicon powder of covering is 20mm.
7. the preparation method of silicon monoxide nano material according to claim 4, it is characterised in that in the step (3)
Pressure is -900-20KPa, and soaking time is 0.5-1.5 hours.
8. the preparation method of silicon monoxide nano material according to claim 4, it is characterised in that in the step (4)
The method that is passed through of argon gas is：Crucible bottom is provided with porous ceramic filter, and tunger tube connection porous ceramic filter bottom connects
Mouthful, argon gas is passed through from the porous ceramic filter of compound bottom, and porous ceramic filter pore size is 1-5um.
9. the preparation method of silicon monoxide nano material according to claim 4, it is characterised in that the Buddha's warrior attendant wire cutting
Silica flour first passes through treatment in advance, to remove organic impurities and metal impurities.
10. the preparation method of silicon monoxide nano material according to claim 4, it is characterised in that the vacuum drying oven
Mode of heating is the one kind in resistance heating, sensing heating, electric arc heated, electron beam heating or heating using microwave.
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Cited By (6)
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| CN109205631A (en) * | 2018-11-12 | 2019-01-15 | 杭州致德新材料有限公司 | Silicon monoxide nano material continuous production device and production technology |
| CN109879290A (en) * | 2019-03-11 | 2019-06-14 | 杭州致德新材料有限公司 | The method for preparing silicon monoxide using silicon containing biomass serialization |
| CN110282634A (en) * | 2019-08-12 | 2019-09-27 | 东北大学 | A method of micron silica is prepared with crystalline silicon diamond wire cutting waste material |
| CN110357115A (en) * | 2019-08-12 | 2019-10-22 | 东北大学 | A method of nano silica is prepared with crystalline silicon diamond wire cutting waste material |
| CN112495336A (en) * | 2020-12-08 | 2021-03-16 | 中南大学 | Vertical reaction furnace for preparing silicon monoxide, preparation device and preparation process |
| 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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| CN110282634A (en) * | 2019-08-12 | 2019-09-27 | 东北大学 | A method of micron silica is prepared with crystalline silicon diamond wire cutting waste material |
| CN110357115A (en) * | 2019-08-12 | 2019-10-22 | 东北大学 | A method of nano silica is prepared with crystalline silicon diamond wire cutting waste material |
| CN110282634B (en) * | 2019-08-12 | 2022-11-04 | 东北大学 | Method for preparing micron-sized silicon dioxide by using crystalline silicon diamond wire cutting waste |
| CN110357115B (en) * | 2019-08-12 | 2022-12-27 | 东北大学 | Method for preparing nano silicon dioxide by using crystalline silicon diamond wire cutting waste material |
| CN112495336A (en) * | 2020-12-08 | 2021-03-16 | 中南大学 | Vertical reaction furnace for preparing silicon monoxide, preparation device and preparation process |
| 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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