CN107651690B - A kind of method of diamond wire cutting waste material preparation high-quality silicon carbide - Google Patents
A kind of method of diamond wire cutting waste material preparation high-quality silicon carbide Download PDFInfo
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- CN107651690B CN107651690B CN201711057626.6A CN201711057626A CN107651690B CN 107651690 B CN107651690 B CN 107651690B CN 201711057626 A CN201711057626 A CN 201711057626A CN 107651690 B CN107651690 B CN 107651690B
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- silicon carbide
- waste material
- cutting waste
- diamond wire
- wire cutting
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- C01—INORGANIC CHEMISTRY
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- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention belongs to the technical fields of open pit mining, are related to a kind of method of diamond wire cutting waste material preparation high-quality silicon carbide.The problem of which solve the disposition of diamond wire cutting waste material, it is characterized in that by weight supplying carbonaceous reducing agent, catalyst and binder directly into cutting waste material, pressed pellet after uniform mixing, the pelletizing suppressed is dried, high temperature reaction stove is put into be reacted, silicon carbide ingot is prepared, finally broken, pickling, dry obtained high-quality silicon carbide powder by silicon carbide ingot.The present invention is not only high to the utilization rate of diamond wire cutting waste material, and production cost is low, and energy consumption is few, and the silicon carbide purity is high, the quality that produce are good.With very high commercial value.
Description
Technical field
The invention belongs to the technical fields of open pit mining, are related to a kind of crystalline silicon diamond wire cutting waste material preparation Gao Pin
The method of matter silicon carbide.
Background technique
With the high speed development of photovoltaic industry, the demand of crystalline silicon increases sharply.Prepare photovoltaic module solar battery
When, it needs that crystalline silicon ingot is cut into silicon wafer by multi-wire saw, multi-line cutting process includes mortar cutting technique and diamond wire
Cutting technique, wherein mortar cutting technique due to cutting efficiency it is relatively low, surface precision and surface roughness are not easily controlled
Etc. reasons be gradually eliminated.The cutting technique of mainstream is using Buddha's warrior attendant wire cutting at present.In its cutting process, about 40% or so
Crystalline silicon enters loss in cutting liquid in the form of a powder becomes slug.Its compared with traditional mortar cutting waste material slurry,
There is no polyethylene glycol and silicon carbide, composition is mainly high-purity silicon powder, some organic solvent cutting fluids and a small amount of metal impurities.Such as
Fruit can be recycled this part slug, can not only reduce environmental pollution, and improve resource utilization, and drop indirectly
The low production cost of crystal silicon chip, generates great economic benefit.
Currently, having about the waste recovery generated to diamond wire sliced crystal silicon and the related patents utilized: from diamond wire
The method (CN102642835A) of silicon material is recycled in the waste material that sliced crystal silicon generates；It is a kind of from the cutting waste material of crystalline silicon slurry in
Recycle the method (CN106865552A) of high-purity silicon powder；A kind of method of crystalline silicon diamond wire saw slug recycling and reusing
(CN105523557A)；A method of silicon-containing alloy is prepared with the diamond wire cutting waste material slurry of crystalline silicon
(CN106916978A).In above several inventions, smelting high-purity silicon and siliceous conjunction are broadly divided into the recycling of such waste material
Golden two classes, are also not directed to this kind of useless silicon material being used to prepare high-quality silicon carbide in the prior art at present.
Summary of the invention
The present invention provides a kind of method that diamond wire cutting waste material recycles, and prepares high-quality with diamond wire cutting waste material
Silicon carbide.The present invention not only solves pollution problem of the diamond wire cutting waste material to environment, avoids the wasting of resources, but become give up into
Treasured brings great economic benefit.
A kind of method of diamond wire cutting waste material preparation high-quality silicon carbide, includes the following steps:
(1) diamond wire cutting waste material, carbonaceous reducing agent are weighed by weight 1.9~2.3:1, then weighs and accounts for mixed material
The binder and account for the water that mixed material mass fraction is 8~15% that mass fraction is 1~10%；Mixing obtains mixed material；
(2) mixed material of acquisition is pressed on high-pressure ball press pelletizing, dried later；
(3) pelletizing after drying is put into high temperature reaction stove, carbon dust is covered above pelletizing, form carbon dust layer, the carbon
Bisque prevents raw material to be oxidized and improve the yield of silicon carbide with a thickness of 10~50mm for keeping the temperature；It is anti-that high temperature is carried out again
It answers, prepares silicon carbide ingot.
(4) the silicon carbide ingot of acquisition is obtained into high-quality silicon carbide powder after broken, pickling, drying.
Further, the carbon dust covered above pelletizing in step (3) is one in graphite, active carbon, petroleum coke or carbon black
Kind is a variety of.
Further, the component of mixed material further includes additive in step (1), in additive NaCl, NaF or KCl
It is one or more；The mixed material mass fraction that accounts for of the additive is no more than 8%.
Further, above-mentioned carbonaceous reducing agent powder is one of graphite powder, petroleum coke, active carbon and carbon black or a variety of.
Further, the binder include one of cellulose, POLYPROPYLENE GLYCOL, polyacrylic acid, polyacrylamide or
It is a variety of.
Further, the pressing pressure of step (2) pressed pellet is 10~60Mpa, and the dwell time is 30~120s,
Pelletizing diameter is 20~80mm.
Further, the reaction temperature of step (3) pyroreaction is 1200-3000 DEG C.
Further, step (4) the pickling mode uses microwave pickling or ultrasonic wave added stirring and pickling, removes
Metal impurities in product, the condition of microwave pickling are as follows: heating rate be 1 DEG C/min~10 DEG C/min, pickling temperature be 30~
260 DEG C, pickling time is 0.25~3h；The condition of ultrasonic wave added stirring and pickling are as follows: supersonic frequency is 40~150kHz, stirring speed
Degree is 0~500rpm, and pickling temperature is 30~70 DEG C, and pickling time is 0.5~4h.
Further, the acid source of the pickling is one of hydrochloric acid, sulfuric acid, hydrofluoric acid or a variety of nitration mixture, sour total concentration
For 5~30wt%.
Purity >=95% of above-mentioned obtained high-quality silicon carbide, contents of free si are≤0.15%, and dissociate iron content
It is≤0.2%.
The medicine have the advantages that
(1) present invention is by being directly incorporated carbon source and catalyst, repressed pelletizing, pyrolytic semlting to diamond wire cutting waste material
High-quality silicon carbide powder can be obtained with pickling impurity removal.High-purity silicon powder in diamond wire cutting waste material is just effectively recycled benefit by this
With reducing environmental pollution, create economic benefit.
(2) high temperature is carried out using vaccum sensitive stove, normal pressure induction furnace, electric arc furnaces, resistance furnace and horizontal kryptol stone, it is simple easy
Row, it is easy to accomplish industrialized production.
(3) after being crushed the silicon carbide ingot after smelting, using microwave pickling and ultrasonic wave added stirring and pickling, make to be carbonized
Silicon particle pickling under dispersion condition can more guarantee the quality of obtained silicon carbide.
Detailed description of the invention
Fig. 1 is process flow chart of the invention.
Specific embodiment
Embodiment 1
Weigh diamond wire cutting waste material 63.33g, carbon black 13.23g, petroleum coke 20.10g sodium chloride 1.67g and POLYPROPYLENE GLYCOL
10g water is added in 1.67g, and (pressing pressure 60Mpa, dwell time 30s, pelletizing diameter are 50 to pressed pellet after evenly mixing
~60mm), it is put into electric arc furnaces, 30mm graphite powder is spread above pelletizing, is smelted under the conditions of 2000~2500 DEG C, after cooling down,
Take out silicon carbide ingot it is broken after, using 30wt% hydrochloric acid carry out the purifying of ultrasonic wave added stirring and pickling (wherein acid washing conditions are as follows:
Supersonic frequency is 100kHz, mixing speed 300rpm, pickling time 4h), the purity of carborundum powder obtained is after dry
97.5%, contents of free si 0.15%, the iron content that dissociates is 0.20%.
Embodiment 2
Diamond wire cutting waste material 65.36g, graphite powder 28.1g, sodium fluoride 2.62g and polyacrylamide 3.92g are weighed, is added
Enter 10g water, after evenly mixing pressed pellet (pressing pressure 20Mpa, dwell time 80s, pelletizing diameter are 40~50mm),
It is put into acheson furnace, 40mm graphite powder is spread above pelletizing, is smelted at 1600~1800 DEG C, after cooling down, takes out carbonization
After silicon ingot is broken, ultrasonic wave added stirring and pickling purifying (wherein acid washing conditions are as follows: supersonic frequency is are carried out using 20% sulfuric acid
50kHz, mixing speed 400rpm, pickling time 1.5h), the purity of carborundum powder obtained is 98.3% after dry, trip
It is 0.15% from silicone content, the iron content that dissociates is 0.22%.
Embodiment 3
Weigh diamond wire cutting waste material 61.52g, petroleum coke 15.15g, graphite powder 13.33g, sodium chloride and the total 5g of potassium chloride
With cellulose 5g, 10g water is added, (pressing pressure 35Mpa, dwell time 60s, pelletizing are straight for pressed pellet after evenly mixing
Diameter is 40~50mm), it is put into resistance furnace, 20mm graphite powder is spread above pelletizing, is smelted at 1400~1500 DEG C, wait cool down
Afterwards, after taking-up silicon carbide ingot is broken, ultrasonic wave added stirring and pickling is carried out using the nitration mixture of 10wt% hydrochloric acid and 5wt% sulfuric acid
Purifying (wherein acid washing conditions are as follows: heating rate is 1 DEG C/min~10 DEG C/min, and pickling temperature is 30~260 DEG C, pickling time
For 0.25~3h), the purity of carborundum powder obtained is 98.3% after dry, and contents of free si 0.14%, dissociate iron content
It is 0.20%.Embodiment 4
Diamond wire cutting waste material 60.97g, graphite powder 26.22g, sodium chloride 4.93g and polyacrylic acid 7.88g are weighed, is added
10g water, pressed pellet (pressing pressure 40Mpa, dwell time 40s, pelletizing diameter are 30~40mm), puts after evenly mixing
Enter normal pressure induction furnace, spread 15mm graphite powder above pelletizing, smelted at 1450~1550 DEG C, after cooling down, takes out carbonization
After silicon ingot is broken, microwave pickling purifying (wherein acid washing conditions are carried out using the nitration mixture of 15wt% hydrochloric acid and 5% hydrofluoric acid
Are as follows: heating rate is 4 DEG C/min, and pickling temperature is 180 DEG C, pickling time 1h), the purity of carborundum powder obtained after dry
It is 98.7%, contents of free si 0.15%, the iron content that dissociates is 0.18%.
Embodiment 5
Diamond wire cutting waste material 60.4g, petroleum coke 20g, active carbon 10.2g, polyacrylamide 9.4g are weighed, 10g is added
Water, pressed pellet (pressing pressure 10Mpa, dwell time 120s, pelletizing diameter are 70~80mm), is put into after evenly mixing
Electric arc furnaces spreads 10mm graphite powder above pelletizing, is smelted at 1800~2300 DEG C, after cooling down, takes out silicon carbide crystallization
After block is broken, microwave pickling purifying (wherein acid washing conditions are as follows: heating are carried out using the nitration mixture of 20wt% hydrochloric acid and 5% hydrofluoric acid
Rate is 10 DEG C/min, and pickling temperature is 40 DEG C, pickling time 3h), the purity of carborundum powder obtained is 96% after dry,
Contents of free si is 0.14%, and the iron content that dissociates is 0.19%.
Embodiment 6
Weigh diamond wire cutting waste material 63g, active carbon 30g, potassium chloride 1.5g, polyacrylamide 2g, POLYPROPYLENE GLYCOL 3.5g,
Be added 10g water, after evenly mixing pressed pellet (pressing pressure 30Mpa, dwell time 100s, pelletizing diameter be 30~
40mm), it is put into vaccum sensitive stove, vacuum degree 100pa spreads 20mm graphite powder above pelletizing, carries out at 1350~1450 DEG C
It smelts, after cooling down, after taking-up silicon carbide ingot is broken, microwave is carried out using the nitration mixture of 10wt% hydrochloric acid and 5% hydrofluoric acid
Pickling purifying (wherein acid washing conditions are as follows: heating rate is 2 DEG C/min, and pickling temperature is 240 DEG C, pickling time 0.25h), does
The purity of carborundum powder made from after dry is 96.8%, contents of free si 0.13%, and the iron content that dissociates is 0.17%.
Claims (10)
1. a kind of method of diamond wire cutting waste material preparation high-quality silicon carbide, which comprises the steps of:
(1) diamond wire cutting waste material, carbonaceous reducing agent are weighed by weight 1.9~2.3:1, then weighs and accounts for mixed material quality
The binder and account for the water that mixed material mass fraction is 8~15% that score is 1~10%；Mixing obtains mixed material；
(2) mixed material of acquisition is pressed on high-pressure ball press pelletizing, dried later；
(3) pelletizing after drying is put into high temperature reaction stove, carbon dust is covered above pelletizing, form carbon dust layer, the carbon dust layer
With a thickness of 10~50mm, then carry out pyroreaction, prepare silicon carbide ingot；
(4) the silicon carbide ingot of acquisition is obtained into high-quality silicon carbide powder after broken, pickling, drying.
2. a kind of method of diamond wire cutting waste material preparation high-quality silicon carbide according to claim 1, which is characterized in that
The carbon dust covered above pelletizing in step (3) is one of graphite, active carbon, petroleum coke or carbon black or a variety of.
3. a kind of method of diamond wire cutting waste material preparation high-quality silicon carbide according to claim 1 or 2, feature exist
In the component of mixed material further includes additive, one of additive NaCl, NaF or KCl or a variety of in step (1)；Institute
The mixed material mass fraction that accounts for for stating additive is no more than 8%.
4. a kind of method of diamond wire cutting waste material preparation high-quality silicon carbide according to claim 1 or 2, feature exist
In above-mentioned carbonaceous reducing agent powder is one of graphite powder, petroleum coke, active carbon and carbon black or a variety of.
5. a kind of method of diamond wire cutting waste material preparation high-quality silicon carbide according to claim 3, which is characterized in that
Above-mentioned carbonaceous reducing agent powder is one of graphite powder, petroleum coke, active carbon and carbon black or a variety of.
6. a kind of method of diamond wire cutting waste material preparation high-quality silicon carbide, special described according to claim 1 or 2 or 5
Sign is that the binder includes one of cellulose, POLYPROPYLENE GLYCOL, polyacrylic acid, polyacrylamide or a variety of.
7. a kind of method of diamond wire cutting waste material preparation high-quality silicon carbide, special described according to claim 1 or 2 or 5
Sign is that the pressing pressure of step (2) pressed pellet is 10~60Mpa, and the dwell time is 30~120s, and pelletizing diameter is big
Small is 20~80mm.
8. a kind of method of diamond wire cutting waste material preparation high-quality silicon carbide, special described according to claim 1 or 2 or 5
Sign is that the reaction temperature of step (3) pyroreaction is 1200-3000 DEG C.
9. a kind of method of diamond wire cutting waste material preparation high-quality silicon carbide, special described according to claim 1 or 2 or 5
Sign is that step (4) the pickling mode uses microwave pickling or ultrasonic wave added stirring and pickling, removes the gold in product
Belong to impurity, the condition of microwave pickling are as follows: heating rate is 1 DEG C/min~10 DEG C/min, and pickling temperature is 30~260 DEG C, pickling
Time is 0.25~3h；The condition of ultrasonic wave added stirring and pickling are as follows: supersonic frequency be 40~150kHz, mixing speed be 0~
500rpm, pickling temperature are 30~70 DEG C, and pickling time is 0.5~4h.
10. a kind of method of diamond wire cutting waste material preparation high-quality silicon carbide, special described according to claim 1 or 2 or 5
Sign is, the acid source of the pickling is one of hydrochloric acid, sulfuric acid, hydrofluoric acid or a variety of mixing, sour total concentration is 5~
30wt%.
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108251893A (en) * | 2018-02-11 | 2018-07-06 | 中铭瓷(苏州)纳米粉体技术有限公司 | The method that silicon carbide and zirconium oxide composite crystal palpus are recycled from crystal silicon cutting waste material |
| CN109400166A (en) * | 2019-01-12 | 2019-03-01 | 东北大学 | The method of crystalline silicon diamond wire cutting waste material preparation Boron carbide silicon carbide composite ceramic |
| CN109734098A (en) * | 2019-03-20 | 2019-05-10 | 东北大学 | A method of nanometer silicon carbide is prepared with the diamond wire cutting waste material of crystalline silicon |
| 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 |
| CN111807369B (en) * | 2020-07-21 | 2022-11-01 | 昆明理工大学 | Pelletizing method for silicon wafer cutting waste for smelting and recycling regenerated silicon |
| CN111960420A (en) * | 2020-09-03 | 2020-11-20 | 上海第二工业大学 | Method for rapidly producing nano silicon carbide by microwave irradiation of electronic waste |
| CN112851356A (en) * | 2021-03-19 | 2021-05-28 | 哈尔滨科友半导体产业装备与技术研究院有限公司 | Method for preparing silicon carbide ceramic by using silicon carbide crystal diamond wire cutting waste liquid |
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| JP2010173916A (en) * | 2009-01-30 | 2010-08-12 | Mitsubishi Materials Corp | Method of manufacturing silicon carbide from silicon waste |
| CN103922404A (en) * | 2014-04-30 | 2014-07-16 | 攀枝花学院 | Method for preparing vanadium trioxide from vanadium pentoxide |
| CN106006645A (en) * | 2016-05-20 | 2016-10-12 | 朱胜利 | Method for smelting silicon carbide chunked crystal by using prefabrication waste micro-powdery particles |
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| JP2010173916A (en) * | 2009-01-30 | 2010-08-12 | Mitsubishi Materials Corp | Method of manufacturing silicon carbide from silicon waste |
| CN103922404A (en) * | 2014-04-30 | 2014-07-16 | 攀枝花学院 | Method for preparing vanadium trioxide from vanadium pentoxide |
| CN106006645A (en) * | 2016-05-20 | 2016-10-12 | 朱胜利 | Method for smelting silicon carbide chunked crystal by using prefabrication waste micro-powdery particles |
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