CN108529629A - A method of preparing silicon carbide using crystalline silicon cutting waste material - Google Patents
A method of preparing silicon carbide using crystalline silicon cutting waste material Download PDFInfo
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- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
- C01B32/914—Carbides of single elements
- C01B32/956—Silicon carbide
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- C01B32/984—Preparation from elemental silicon
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Abstract
The present invention relates to a kind of methods preparing silicon carbide using crystalline silicon cutting waste material, include the following steps：S1, crystalline silicon cutting waste material, carbon source, binder and water are mixed to get material to be molded.S2, material compression moulding to be molded is obtained into pelletizing.S3, precursor reagent is dried to obtain to pelletizing.S4, precursor reagent is placed in reacting furnace.S5, it is powered to reacting furnace, then makes to keep certain temperature in furnace body and keep the temperature to obtain silicon carbide ingot.S6, silicon carbide ingot is crushed and is handled, obtain beta silicon carbide powder.Crystalline silicon cutting waste material is combined with acheson furnace technique for the first time using the method that crystalline silicon cutting waste material prepares silicon carbide in the present invention, the problem of not only solving pollution problem and the wasting of resources of the existing middle crystalline silicon cutting waste material to environment, reaction temperature is relatively low when preparing simultaneously, greatly reduce energy consumption, cost-effective, and it is final it is obtained be single crystal form beta silicon carbide.
Description
Technical field
The invention belongs to the technical fields of open pit mining, and in particular to a kind of to prepare carbon using crystalline silicon cutting waste material
The method of SiClx.
Background technology
Since the 21th century, to solve the problems, such as that the energy such as oil, coal are increasingly in short supply, various countries open the mankind energetically one after another
Emerging energy, especially solar energy are sent out as green, environmental protection, free of contamination clean energy resource, so that photovoltaic industry is entered high speed and sends out
The duration of an exhibition.Meanwhile the fast development of semi-conductor industry is also widely applied high-purity crystal silicon materials, global demand amount is not
It is disconnected to increase.The monocrystalline silicon of semiconductor industry and polysilicon used for solar batteries, are required for by wire cutting at satisfactory
Silicon chip.
But have nearly 50% crystalline silicon that can enter in cutting slurry in the form of silica flour when sliced crystal silicon, slurry it is main
Group is divided into a small amount of impurity iron that silica flour, polyethylene glycol and cutting process introduce.Slurry is through rinsing dissolution, being separated by solid-liquid separation, molten at present
Liquid concentration, evaporative condenser can effectively recycle most of polyethylene glycol, but then become by the solid powder of key component of silica flour
Waste not only polluted environment, but also cause the great wasting of resources.
Crystalline silicon cutting waste material includes mainly a large amount of silica flour, a small amount of polyethylene glycol not being recovered and a small amount of impurity
Iron, for this discarded powder, many researchers attempt to handle it using various techniques, regenerated.Such as it much grinds
The person of studying carefully prepares silicon carbide using crystalline silicon cutting waste material, although can be recycled to the silica flour in crystalline silicon cutting waste material again sharp
With, but high temperature furnace is used in preparation process, reaction temperature is high, needs to consume mass energy, while needing to be passed through protection gas,
It is more demanding to consersion unit, increase production cost, while the crystal form of finally obtained product silicon carbide is not also single, leads
Cause silicon carbide products value not high.
Invention content
(1) technical problems to be solved
In order to solve the above problem of the prior art, present invention offer is a kind of to prepare silicon carbide using crystalline silicon cutting waste material
Method solve pollution problem and money of the existing middle crystalline silicon cutting waste material to environment using crystalline silicon cutting waste material as raw material
The problem of source wastes, while reaction temperature is relatively low when preparing, greatly reduces energy consumption, cost-effective, it is final it is obtained be single
The silicon carbide of crystal form.
(2) technical solution
In order to achieve the above object, the main technical schemes that the present invention uses include：
The present invention provides a kind of method preparing silicon carbide using crystalline silicon cutting waste material, includes the following steps：S1, will be brilliant
Body silicon cutting waste material, carbon source, binder and water are mixed, and material to be molded is obtained, wherein crystalline silicon cutting waste material and carbon source
Mass ratio be 1.8~2.5:1；S2, will material compression moulding be molded, obtain pelletizing；S3, pelletizing is dried, is obtained
Precursor reagent；S4, precursor reagent is placed in reacting furnace, and so that the furnace core of reacting furnace is buried and is distributed in precursor reagent
Center, wherein reacting furnace include with opening furnace body, in furnace body be equipped with furnace core, and furnace core two termination electricity；S5, general
Reacting furnace is powered, and the temperature of furnace core is made to reach 1000~1500 DEG C, then by controlling the electric current of furnace core, makes the temperature in furnace body
1500~1900 DEG C are maintained at, and is kept the temperature, silicon carbide ingot is obtained after heat preservation；S6, silicon carbide ingot is broken
It is broken, after the carbon component for then removing broken silicon carbide ingot surface, obtain beta -silicon carbide powder.
According to the present invention, in step sl, the mass percent that binder accounts for material to be molded is 3~8%, and water, which accounts for, waits for mould
It is 5~10% to press the mass percent of material.
According to the present invention, binder includes the group of one or more of cellulose, polyacrylic acid or POLYPROPYLENE GLYCOL
It closes；Carbon source includes the combination of one or more of graphite powder, carbon black, activated carbon or petroleum coke.
According to the present invention, in step s 2, the pressing pressure of compression moulding is 10~55MPa, the dwell time is 2~
3min, a diameter of 5~30mm of pelletizing.
According to the present invention, in step s3, dry temperature is 130~150 DEG C, and the dry time is 5~20h.
According to the present invention, in step s 4, reacting furnace is acheson furnace, and furnace core is graphite rod.
According to the present invention, in step s 5, the time of heat preservation is 10~200h.
According to the present invention, in step s 6, broken silicon carbide ingot is placed in high temperature furnace, and will be in high temperature furnace
Temperature be warming up to 700~900 DEG C, and 1~3h is kept the temperature, to remove the carbon component on broken silicon carbide ingot surface.
(3) advantageous effect
The beneficial effects of the invention are as follows：
Crystalline silicon cutting waste material is combined with reacting furnace energization reaction process to prepare beta silicon carbide by the present invention for the first time, and
Furnace body is open furnace body, and when reaction does not need to be passed through protection gas.Since the main component of crystalline silicon cutting waste material is silica flour,
Si is exothermic reaction, heat production and reaction self-heat generation two parts of the heat source essentially from reacting furnace with reacting for C.So such
The initial temperature of method reaction only needs to reach 1000 DEG C, and by material inner heat, the heat that reaction itself is released is enough to make instead
It should the constantly sprawling from inside to outside centered on furnace core.
The center of furnace body is furnace core, and material is buried in the surrounding of furnace core, using synthesis by internal resistance electric melting, make the reaction of material from inside to outside into
Row, heat hardly scatter and disappear, substantially increase the thermal efficiency, reduce energy consumption.Therefore, entire reaction is that synthesis by internal resistance electric melting self- propagating is anti-
It answers, greatly reduces energy consumption, while using crystalline silicon cutting waste material as raw material, realize the recycling of waste, solve crystalline silicon
The problem of cutting waste material is to the pollution problem and the wasting of resources of environment.In addition, in the present invention also by control furnace core electric current with
The temperature of control furnace body is maintained in the range of 1500~1900 DEG C, it is possible thereby to which the crystal form for controlling finally obtained product is single
One β-SiC, and better crystallinity degree, purity are high, precision height, epigranular can reach the national standard of abrasive material silicon B-carbide.
Description of the drawings
Fig. 1 is the X ray diffracting spectrum of beta -silicon carbide powder obtained in following examples 1；
Fig. 2 is the SEM figures of beta -silicon carbide powder obtained in following examples 1；
Fig. 3 is the particle size distribution figure of beta -silicon carbide powder obtained in following examples 1.
Specific implementation mode
In order to preferably explain the present invention, in order to understand, below in conjunction with the accompanying drawings, by specific implementation mode, to this hair
It is bright to be described in detail.
Embodiment 1
The present embodiment provides a kind of methods preparing silicon carbide using polycrystalline silicon wastes, specifically comprise the following steps：
S1, crystalline silicon cutting waste material, graphite powder, cellulose and water are mixed, obtains material to be molded.
Wherein, the mass ratio of crystalline silicon cutting waste material and graphite powder is 2.2:1, cellulose accounts for the quality hundred of material to be molded
Score is 5%, and the mass percent that water accounts for material to be molded is 8%.Graphite powder is in the present embodiment mainly as carbon source, subsequently
It is reacted with the silica flour in crystalline silicon cutting waste material as reactant.Cellulose in the present embodiment mainly as binder,
What it is due to binder use is organic matter, can be volatilized in subsequent high temperature, therefore can't introduce impurity in the final product.
Only it is mixing physically it should be noted that not chemically reacted in entire mixed process.
S2, material to be molded is pressed using high-pressure ball press under the pressing pressure of 40Mpa, and pressurize
2.5min obtains the pelletizing of a diameter of 10~20mm.
Wherein, material to be molded needs to carry out compression process, rather than powder is placed in reacting furnace and is directly reacted, mainly
Be because：The micron-sized powder is very fluffy, and tap density is very low, and the air being mingled between powder makes silica in temperature Gao Shiyi
Change.And suppressing can make material combine closely, the air reduced between raw material is aoxidized with reducing, while increasing connecing between raw material
Contacting surface product promotes subsequent reaction rate.But the material store and transportational process in surface oxidation be it is inevitable, because
This, the reaction of the main body of the present embodiment is the reaction of silicon and carbon, can also be accompanied by reacting for a small amount of silica and carbon, which has
Carbon monoxide generates, and can be burnt by expecting that the gap between block is diffused into surface of material, the accumulation in stove is avoided to bring safety hidden
Suffer from.
S3, it pelletizing is placed in drying box is dried, drying temperature is 140 DEG C, and drying time 10h obtains forerunner
Precursor reactant object.
In this drying process, the main water and organic matter removed in pelletizing.Wherein, organic matter here refers to crystalline silicon
Polyethylene glycol in cutting waste material, crystalline silicon cutting waste material used in the present embodiment refers to carrying out recycling most of polyethylene glycol
Waste material afterwards includes mainly a large amount of silica flour, a small amount of polyethylene glycol not being recovered and a small amount of impurity iron.Therefore, crystalline silicon
A small amount of polyethylene glycol contained in cutting waste material can also volatilize when being dried, and impurity iron therein is due to measuring very
Lack, shared quality be less than 0.2%, therefore, the purity of the silicon carbide subsequently prepared can't be influenced too much.
S4, precursor reagent is placed in reacting furnace, and so that the furnace core of reacting furnace is buried and is distributed in precursor reagent
Centre.Wherein, reacting furnace includes the furnace body with opening, furnace core, and two termination electricity of furnace core is equipped in furnace body, in the present embodiment
Middle reacting furnace is acheson furnace, and furnace core is graphite rod, cost-effective.
S5, reacting furnace is powered, the temperature of furnace core is made to reach 1400 DEG C, then by controlling the electric current of furnace core, make furnace body
Interior temperature is maintained at 1800 DEG C, and keeps the temperature 80h, and silicon carbide ingot is obtained after heat preservation.
Specifically, main during this electrified regulation to react in the silica flour and graphite powder in crystalline silicon cutting waste material
The anti-raw reaction of carbon generate silicon carbide, react for exothermic reaction, the heat of release makes the temperature of charge of surrounding increase, and then makes instead
It should constantly be spread to periphery.That is, above-mentioned reaction occurs at first for the material around furnace core, the heat released with reaction makes surrounding
After material heats up, again above-mentioned reaction is occurring for the material of periphery, and reaction is constantly outside with the continuous raising of periphery temperature of charge
Sprawling carries out.And react when spreading to most peripheral material, remaining material ratio is relatively thin, the high temperature being not enough to inside maintaining, therefore,
Reaction just stops when spreading to periphery temperature deficiency continuing to spread, the unreacted material of most peripheral it is can be recycled for next time after
Continuous reaction uses.
Also needing to the electric current of control furnace core in entire reaction process simultaneously makes the temperature in entire furnace body be maintained at 1800 DEG C,
Specifically, the electric current of furnace core can be increased when the temperature in furnace body is less than 1800 DEG C, and when temperature is more than 1800 DEG C, can subtract
The electric current of small furnace core, so that the temperature in entire stove is maintained at stationary temperature.Due to when between 1400~1900 DEG C, reacting
β-SiC are generated, therefore, finally obtained silicon carbide ingot is β-SiC, the silicon carbide essence of this kind of crystal form after above-mentioned reaction
Higher, intensity higher are spent, there is higher value.
S6, after obtaining in step S5 by silicon carbide ingot natural cooling, silicon carbide ingot is crushed, so
After the carbon component for removing broken silicon carbide ingot surface afterwards, carborundum powder is obtained.
Specifically, broken silicon carbide ingot is placed in high temperature furnace, and the temperature in high temperature furnace is warming up to 700
DEG C, and 2h is kept the temperature, the carbon component to remove broken silicon carbide ingot surface (refers to excessive graphite in the present embodiment
Powder).When due to carrying out dispensing in step sl, graphite powder used is excessive, so in step s 5, the carbon in graphite powder
It can also remaining a part of unreacted graphite powder after being reacted with the silica flour in crystalline silicon cutting waste material.Therefore, in step S6
In into being about to after broken silicon carbide ingot is placed in high temperature furnace, be substantially carried out to be carbon react with oxygen, it is specific anti-
Answer formula as follows：
C+O2=CO2
Remaining carbon component is converted into carbon dioxide gas in material, therefore, by that can remove carbonization after step S6
After the residual carbon component on silicon ingot surface, to obtain the higher carborundum powder of purity, ingredient is β-SiC.
Further, referring to Fig.1, it is the X ray diffracting spectrum of beta -silicon carbide powder obtained.From figure 1 it appears that material
Material is the diffraction maximum of β-SiC, and carborundum powder obtained is simple β-SiC, and the sharp peak that diffraction maximum is high intensity, is shown
Carborundum powder has good crystallinity, i.e., only single-phase, lattice is more stable in obtained carborundum powder.
Further, be that the SEM of beta -silicon carbide powder obtained schemes with reference to Fig. 2, the figure be accelerating potential (EHT)=
15.00kV, secondary electron detectable signal SignalA=SE2, operating distance (WD)=8.1mm, amplification factor (Mag)=200x
Under conditions of obtain.From figure 2 it can be seen that the object of carborundum powder obtained is mutually single.
Further, it is the particle size distribution figure of beta -silicon carbide powder obtained with reference to Fig. 3, from figure 3, it can be seen that being made
Carborundum powder epigranular.
Further, the existing middle method for preparing silicon carbide can be mainly divided into following two：The first, utilize crystalline silicon
Cutting waste material prepares silicon carbide, carries out high temperature burning after usually being mixed crystalline silicon cutting waste material with carbon dust in high temperature furnace
Knot, while needing to be passed through and gas is protected to be prepared with completely oxygen barrier.Although the silicon in polycrystalline silicon cut waste can be recycled
Powder, but the generally bad control of the completely oxygen-impermeable atmosphere of such method, it is more demanding to consersion unit, simultaneous reactions temperature also compared with
Height, considerably increases production cost, and reaction-sintered temperature is generally between 1500~3000 DEG C, the crystalline substance of obtained silicon carbide
Type is not single.
Second, the method that silicon carbide is commonly prepared in industry is to use traditional Acheson's method, with quartz sand
(since silica flour is expensive, will not generally use silica flour as raw material in existing industry) and coke add simultaneously for primary raw material
Enter salt and sawdust is placed in electric furnace, makes the powder of quartz sand and coke that carbon heat directly occur at high temperature using high power electric heating
Reduction reaction generates silicon carbide products.But the initial temperature of such method reaction needs to reach 2000 DEG C, therefore in production
It needs persistently to provide a large amount of heat by acheson furnace, undoubtedly consumes energy higher, considerably increase cost.
And passes through a large amount of experimental study and find：For above-mentioned second of preparation method, the raw material used is quartz
Sand and coke, i.e. reaction are SiO2With reacting for C, due to the reaction be the endothermic reaction, so heat is led entirely from electric heating
It needs that a large amount of heat is persistently provided and causes the raising largely consumed energy with cost when causing using above-mentioned second of preparation method.
And reacting for Si and C is exothermic reaction, can constantly discharge heat, but existing middle silica flour price is prohibitively expensive can not direct profit
With therefore, being reacted with carbon using crystalline silicon cutting waste material as raw material, the cost of raw material can not only be substantially reduced, simultaneously
Since silicon can greatly save energy consumption with reacting for carbon for exothermic reaction.
Crystalline silicon cutting waste material is combined by the present embodiment with reacting furnace energization reaction process for the first time as a result, specifically will
Crystalline silicon cutting waste material is combined to prepare silicon carbide with acheson furnace technique for the first time, and furnace body is open furnace body, when reaction
It does not need to be passed through protection gas.Since the main component of crystalline silicon cutting waste material is silica flour, Si is exothermic reaction with reacting for C,
Heat production and reaction self-heat generation two parts of the heat source essentially from reacting furnace.So the initial temperature of such method reaction only needs
Reach 1000 DEG C, by material inner heat, heat that reaction itself is released be enough to make reaction centered on furnace core from inside to outside
Constantly sprawling.
The center of furnace body is furnace core, and material is buried in the surrounding of furnace core, using synthesis by internal resistance electric melting, make the reaction of material from inside to outside into
Row, heat hardly scatter and disappear, substantially increase the thermal efficiency, reduce energy consumption.Therefore, entire reaction is that synthesis by internal resistance electric melting self- propagating is anti-
It answers, greatly reduces energy consumption, while using crystalline silicon cutting waste material as raw material, realize the recycling of waste, solve crystalline silicon
The problem of cutting waste material is to the pollution problem and the wasting of resources of environment.In addition, the electric current in the present embodiment also by controlling furnace core
Temperature to control furnace body is maintained in the range of 1500~1900 DEG C, it is possible thereby to which the crystal form for controlling finally obtained product is
Single β-SiC, and better crystallinity degree, purity are high, epigranular, can reach the national standard of abrasive material silicon B-carbide.
Embodiment 2
The present embodiment provides a kind of methods preparing silicon carbide using polycrystalline silicon wastes, specifically comprise the following steps：
S1, crystalline silicon cutting waste material, carbon black, polyacrylic acid and water are mixed, obtains material to be molded.Wherein, brilliant
The mass ratio of body silicon cutting waste material and carbon black is 1.8:1, the mass percent that polyacrylic acid accounts for material to be molded is 3%, and water accounts for
The mass percent of material to be molded is 5%.
S2, material to be molded is pressed using high-pressure ball press under the pressing pressure of 10Mpa, and pressurize
3min obtains the pelletizing of a diameter of 5~10mm.
S3, it pelletizing is placed in drying box is dried, drying temperature is 130 DEG C, and drying time 20h obtains forerunner
Precursor reactant object.
S4, precursor reagent is placed in reacting furnace, and so that the furnace core of reacting furnace is buried and is distributed in precursor reagent
Centre.Wherein, reacting furnace is acheson furnace in the present embodiment, and furnace core is graphite rod.
S5, reacting furnace is powered, the temperature of furnace core is made to reach 1200 DEG C, then by controlling the electric current of furnace core, make furnace body
Interior temperature is maintained at 1500 DEG C, and keeps the temperature 120h, and silicon carbide ingot is obtained after heat preservation, and obtained silicon carbide crystallization
Block is β-SiC.
S6, after obtaining in step S5 by silicon carbide ingot natural cooling, silicon carbide ingot is crushed, so
Broken silicon carbide ingot is placed in high temperature furnace afterwards, and the temperature in high temperature furnace is warming up to 800 DEG C, and keeps the temperature 3h,
To remove the carbon component (referring to excessive carbon black in the present embodiment) on broken silicon carbide ingot surface, silicon carbide is obtained
The ingredient of powder, final carborundum powder obtained is β-SiC.
Embodiment 3
The present embodiment provides a kind of methods preparing silicon carbide using polycrystalline silicon wastes, specifically comprise the following steps：
S1, crystalline silicon cutting waste material, activated carbon, polypropylene alcohol and water are mixed, obtains material to be molded.Wherein,
The mass ratio of crystalline silicon cutting waste material and activated carbon is 2.4:1, the mass percent that POLYPROPYLENE GLYCOL accounts for material to be molded is 8%,
The mass percent that water accounts for material to be molded is 10%.
S2, material to be molded is pressed using high-pressure ball press under the pressing pressure of 55Mpa, and pressurize
2min obtains the pelletizing of a diameter of 20~30mm.
S3, it pelletizing is placed in drying box is dried, drying temperature is 150 DEG C, and drying time 5h obtains presoma
Reactant.
S4, precursor reagent is placed in reacting furnace, and so that the furnace core of reacting furnace is buried and is distributed in precursor reagent
Centre.Wherein, reacting furnace is acheson furnace in the present embodiment, and furnace core is graphite rod.
S5, reacting furnace is powered, the temperature of furnace core is made to reach 1500 DEG C, then by controlling the electric current of furnace core, make furnace body
Interior temperature is maintained at 1900 DEG C, and keeps the temperature 50h, and silicon carbide ingot is obtained after heat preservation, and obtained silicon carbide crystallization
Block is β-SiC.
S6, after obtaining in step S5 by silicon carbide ingot natural cooling, silicon carbide ingot is crushed, so
Broken silicon carbide ingot is placed in high temperature furnace afterwards, and the temperature in high temperature furnace is warming up to 900 DEG C, and keeps the temperature 1h,
To remove the carbon component (referring to excessive activated carbon in the present embodiment) on broken silicon carbide ingot surface, silicon carbide is obtained
The ingredient of powder, final carborundum powder obtained is β-SiC.
Certainly, the present invention is also not limited to this, in step sl, binder preferably comprise cellulose, polyacrylic acid or
The combination of one or more of person's POLYPROPYLENE GLYCOL, carbon source preferably comprise in graphite powder, carbon black, activated carbon or petroleum coke
One or more kinds of combinations.Crystalline silicon cutting waste material and the mass ratio of carbon source are preferably 1.8~2.5:1, under this range,
Ensure that carbon source is excessive, thus enables that the silica flour in crystalline silicon cutting waste material fully reacts, and then can fully recycle profit
With the silica flour in crystalline silicon cutting waste material, increase operation rate.The mass percent that binder accounts for material to be molded is preferably 3~
8%, the mass percent that water accounts for material to be molded is preferably 5~10%, under this proportional region, both can guarantee that material can glue
Knot together, and will not cause water that waste that is excessive and causing water resource is added.
In step s 2, the pressing pressure of compression moulding is preferably 10~55MPa, and the dwell time is preferably 2~3min, ball
The diameter of group is preferably 5~30mm, under this particle size range, can increase the specific surface area of pelletizing, so that reaction is more abundant.
In step s3, dry temperature is preferably 130~150 DEG C, and the dry time is preferably 5~20h.In step s 5, furnace core
Preferably up to 1000~1500 DEG C of temperature, the temperature in furnace body is preferably kept in 1500~1900 DEG C, so that final
The crystal form of the product arrived is single β-SiC, and the time of heat preservation is preferably 10~200h.In step s 6, the temperature in high temperature furnace
Degree is preferably warming up to 700~900 DEG C, and soaking time is preferably 1~3h so that the oxygen in unreacted carbon source and air into
Row reaction generates carbon dioxide.
More than, only it is presently preferred embodiments of the present invention, is not the limitation for doing other forms to invention, it is any to be familiar with
Professional and technical personnel is changed or is modified as the equivalence enforcement of equivalent variations possibly also with the technology contents of the disclosure above
Example.But it is every without departing from technical solution of the present invention content, according to the technical essence of the invention to appointing made by above example
What simple modification, equivalent variations and remodeling, still falls within the protection domain of technical solution of the present invention.
Claims (8)
1. a kind of method preparing silicon carbide using crystalline silicon cutting waste material, which is characterized in that include the following steps：
S1, crystalline silicon cutting waste material, carbon source, binder and water are mixed, obtains material to be molded, wherein the crystal
The mass ratio of silicon cutting waste material and the carbon source is 1.8~2.5:1；
S2, by the material compression moulding to be molded, obtain pelletizing；
S3, the pelletizing is dried, obtains precursor reagent；
S4, the precursor reagent is placed in reacting furnace, and so that the furnace core of the reacting furnace is buried to be distributed in the presoma anti-
Answer the center of object, wherein the reacting furnace includes the furnace body with opening, the furnace core is equipped in the furnace body, and described
Two termination electricity of furnace core；
S5, the reacting furnace is powered, the temperature of the furnace core is made to reach 1000~1500 DEG C, then by controlling the furnace core
Electric current, so that the temperature in the furnace body is maintained at 1500~1900 DEG C, and keep the temperature, obtained after heat preservation silicon carbide crystallization
Block；
S6, the silicon carbide ingot is crushed, then removes the carbon group on the broken silicon carbide ingot surface
After point, beta -silicon carbide powder is obtained.
2. the method for preparing silicon carbide using crystalline silicon cutting waste material as described in claim 1, which is characterized in that
In step sl, the mass percent that the binder accounts for the material to be molded is 3~8%, and the water accounts for described wait for
The mass percent for being molded material is 5~10%.
3. the method for preparing silicon carbide using crystalline silicon cutting waste material as claimed in claim 2, which is characterized in that
The binder includes the combination of one or more of cellulose, polyacrylic acid or POLYPROPYLENE GLYCOL；
The carbon source includes the combination of one or more of graphite powder, carbon black, activated carbon or petroleum coke.
4. the method for preparing silicon carbide using crystalline silicon cutting waste material as described in claim 1, which is characterized in that
In step s 2, the pressing pressure of compression moulding is 10~55MPa, and the dwell time is 2~3min, the diameter of the pelletizing
For 5~30mm.
5. the method for preparing silicon carbide using crystalline silicon cutting waste material as described in claim 1, which is characterized in that
In step s3, the temperature of the drying is 130~150 DEG C, and the time of the drying is 5~20h.
6. the method for preparing silicon carbide using crystalline silicon cutting waste material as described in claim 1, which is characterized in that
In step s 4, the reacting furnace is acheson furnace, and the furnace core is graphite rod.
7. the method for preparing silicon carbide using crystalline silicon cutting waste material as described in claim 1, which is characterized in that
In step s 5, the time of the heat preservation is 10~200h.
8. the method as described in any one of claim 1 to 7 for preparing silicon carbide using crystalline silicon cutting waste material, feature exist
In,
In step s 6, the broken silicon carbide ingot is placed in high temperature furnace, and the temperature in high temperature furnace is heated up
To 700~900 DEG C, and 1~3h is kept the temperature, to remove the carbon component on the broken silicon carbide ingot surface.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109748281A (en) * | 2019-03-20 | 2019-05-14 | 东北大学 | A method of high-quality silicon carbide is prepared using discarded silicon powder |
| CN109987606A (en) * | 2019-05-13 | 2019-07-09 | 穆建东 | It is a kind of to utilize silicon powder and high purity graphite powder synthesizing β-SiC technique for producing miropowder |
| CN111704471A (en) * | 2020-06-18 | 2020-09-25 | 北京精冶源新材料股份有限公司 | Method for in-situ preparation of refractory castable for blast furnace bottom and hearth by using industrial waste |
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| CN109748281A (en) * | 2019-03-20 | 2019-05-14 | 东北大学 | A method of high-quality silicon carbide is prepared using discarded silicon powder |
| CN109987606A (en) * | 2019-05-13 | 2019-07-09 | 穆建东 | It is a kind of to utilize silicon powder and high purity graphite powder synthesizing β-SiC technique for producing miropowder |
| CN111704471A (en) * | 2020-06-18 | 2020-09-25 | 北京精冶源新材料股份有限公司 | Method for in-situ preparation of refractory castable for blast furnace bottom and hearth by using industrial waste |
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