CN108910887A - A kind of monocrystalline silicon cuts the recovery and treatment method of slag and cutting waste liquor - Google Patents
A kind of monocrystalline silicon cuts the recovery and treatment method of slag and cutting waste liquor Download PDFInfo
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- CN108910887A CN108910887A CN201810827057.7A CN201810827057A CN108910887A CN 108910887 A CN108910887 A CN 108910887A CN 201810827057 A CN201810827057 A CN 201810827057A CN 108910887 A CN108910887 A CN 108910887A
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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
- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
- C01B32/914—Carbides of single elements
- C01B32/956—Silicon carbide
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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
- C01B33/02—Silicon
- C01B33/037—Purification
- C01B33/039—Purification by conversion of the silicon into a compound, optional purification of the compound, and reconversion into silicon
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G1/00—Mixtures of fertilisers belonging individually to different subclasses of C05
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J11/00—Recovery or working-up of waste materials
- C08J11/04—Recovery or working-up of waste materials of polymers
- C08J11/06—Recovery or working-up of waste materials of polymers without chemical reactions
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2371/00—Characterised by the use of polyethers obtained by reactions forming an ether link in the main chain; Derivatives of such polymers
- C08J2371/02—Polyalkylene oxides
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/62—Plastics recycling; Rubber recycling
Abstract
The invention discloses a kind of monocrystalline silicon cutting slag and the recovery and treatment methods of cutting waste liquor, include the following steps：(1), at place, monocrystalline silicon with stirring cuts in slag and cutting waste liquor and hydrochloric acid is added, and mixed liquor is obtained after being stirred to react；(2), mixed liquor heating evaporation is separated by solid-liquid separation, obtains the solid mixture and gas of silicon carbide, silicon and impurity, gas is steamed to the mixed liquor for obtaining water and polyethylene glycol after condensing, heating drains to obtain polyethylene glycol after dehydration；(3), the solid mixture of silicon carbide, silicon and impurity is obtained into the solid mixture of silicon carbide and silicon through concussion cleaning and Gravity Separation；(4), the solid mixture of silicon carbide and silicon is added in the mixed acid solution of nitric acid and HF composition, fluosilicic acid is steamed after reaction, condenses to obtain fluosilicic acid, then fluosilicic acid is processed into recycling silicon, remaining silicon carbide and acid solution after reaction, filtering pickling, washing and dry silicon carbide.The method of the present invention is environmentally friendly and has very big economic benefit.
Description
Technical field
The present invention relates to metallurgy and environment protection fields, and in particular to a kind of monocrystalline silicon cuts the recovery processing of slag and cutting waste liquor
Method.
Background technique
With the growing tension of the energy and the exacerbation of pollution, the attention for causing various countries to use clean energy resource.It all lifts in the whole world
It plays solar battery and builds agitation, China develops solar battery and have developed rapidly in recent years, and solar battery is widely applied
The production of the primary raw material monocrystalline silicon as solar battery is promoted also to grow rapidly.The monocrystalline silicon piece that solar battery uses is
Formed by silicon single crystal rod cutting processing, silicon single crystal rod must have been used in cutting process lubrication act on cut harmful liquid, because
This just generates a large amount of cutting waste liquor in cutting process.It includes poly- second two that the cutting liquid generallyd use at home at present, which is one,
Alcohol, silicon carbide, triethanolamine, saponification liquor, the mixture of kerosene etc., therefore the COD value of cutting waste liquor substantially exceeds discharge of wastewater
Standard forbids discharge by environmental requirement.And suitable liquid waste processing recovery method is not found at present, therefore domestic raw
A large amount of waste liquids can only be stacked by producing factory, and as production continues to develop, also pile up like a mountain for the cutting waste liquor accumulated year in year out,
Continue the roadblock of production through becoming enterprise.Therefore compel the processing for highly necessary finding a simple and effective monocrystalline silicon cutting waste liquor
Recovery method mainly recycles polyethylene glycol, silicon carbide and silicon from cutting waste liquor.Not only the processing recycling of waste liquid solves environmental protection
Problem, and have very big economic benefit.
CN201210246470.7 discloses a kind of silicon wafer cutting waste liquor processing method, this dispose waste liquid in without three ethyl alcohol
Amine, saponification liquor and kerosene, this method only needs to be separated by solid-liquid separation with equipment for separating liquid from solid, then is mutually tied using heavy-fluid separation with electrophoresis
The method of conjunction separates silicon powder therein and silicon-carbide particle, the process will not relate to the separating treatment to complicated mucus, and
And silicon carbide and silicon are obtained in subsequent recovery.But this method needs to be separated with heavy-fluid, heavy-fluid is expensive, and can produce to environment
Raw certain pollution；And this method has multiple high-temperature operation processes, and also needs for material to be heated to 2500 DEG C or more, no
Only energy consumption is high, and the high requirements on the equipment, equipment investment are big.
Summary of the invention
It is an object of that present invention to provide a kind of monocrystalline silicon cutting slag and the recovery and treatment methods of cutting waste liquor, solve existing list
The problem of crystal silicon cutting waste liquor processing.
The present invention is achieved through the following technical solutions：
A kind of monocrystalline silicon cuts the recovery and treatment method of slag and cutting waste liquor, includes the following steps：
(1), at place, monocrystalline silicon with stirring cuts in slag and cutting waste liquor and hydrochloric acid is added, and mixture is obtained after being stirred to react
Liquid；
(2), mixed liquor heating evaporation is separated by solid-liquid separation, obtain silicon carbide, silicon and impurity solid mixture and
Gas is steamed the mixed liquor that water and polyethylene glycol are obtained after condensing by gas, and heating drains to obtain polyethylene glycol after dehydration；
(3), the solid mixture of silicon carbide, silicon and impurity is obtained into silicon carbide and silicon through concussion cleaning and Gravity Separation
Solid mixture；
(4), the solid mixture of silicon carbide and silicon is added in the mixed acid solution of nitric acid and HF composition, it will after reaction
Fluosilicic acid steams, and condenses to obtain fluosilicic acid, then fluosilicic acid is processed recycling silicon, remaining silicon carbide and acid solution after reaction, filtering pickling,
It washes and dry silicon carbide.
Concentration of hydrochloric acid is 0.001~0.5mo1/L in step (1), and per kilogram monocrystalline silicon cuts slag and cutting waste liquor is added
200~700ml hydrochloric acid solution.
Reaction temperature is 40~60 DEG C in step (1), and mixing time is 15~35min.
Concussion cleaning in step (3) uses ultrasonic cleaning.
The water of the 10-20wt% of the solid mixture weight of silicon carbide, silicon and impurity, temperature are added during ultrasonic cleaning
Degree is 40~80 DEG C.
Concentration of nitric acid is 6wt%, and HF concentration is 25wt%.
The volume ratio of nitric acid and HF are 1:6~8.
The mixed acid of 1.5~2 kilograms of nitric acid and HF is added in the solid mixture of every 1 kilogram of silicon carbide and silicon in step (4)
Liquid.
Reaction temperature is first risen to 30~60 DEG C, after being stirred to react 10~30min in step (4), then will be in temperature
It is raised to 100~130 DEG C.
Dehydration is specific to be carried out with baffle-type dehydrator, gravity type dehydrator, cyclone type dehydrator, spraying dehydrator.
Monocrystalline silicon cutting slag and cutting waste liquor are that the very big mixing with solid powder/particle of a viscosity is sticky in the present invention
Material, is not easy flowing conveying, and process is difficult.The method of the present invention handles waste liquid with dilute hydrochloric acid, generates salt by neutralization
The alkaline matter triethanolamine and saponification liquor that contain in waste liquid are removed, while the viscosity of waste liquid is substantially reduced, by stirring
Mixing is conducive to process so that waste liquid becomes the uniform mixture for easily flowing conveying.Whipping process can be in high-speed stirring
It mixes in the agitating devices such as device and carries out.
The salt and other impurity that the neutralization contained in the solid mixture of silicon carbide and silicon generates are tight in the form of " shell "
The close outside for being wrapped in silicon carbide powder and silicon powder grain, is difficult to remove.By way of concussion cleaning, ultrasonic cleaning is such as used
Device cleaning treatment is cleaned by the concussion repeatedly of ultrasonic wave, and material molecule in mixture can be made to hit and rub with hydrone
Wipe, material particles refinement, " shell " pine splits and falls off, play cleaning action, then by gravity sieve for example, by using shaking table into
Row separation, due to the difference of specific gravity, separates both silicon carbide, silicon with " shell residue ", after the Slag recovering separated, it is possible to
Using as fertilizer.
Aqueous slkali washing aqueous slkali used includes sodium hydroxide, potassium hydroxide, sodium carbonate, wash temperature be room temperature or
40~60 DEG C.
Monocrystalline silicon cutting slag of the invention and cutting waste liquor can remove kerosene first to carry out subsequent processing.
Compared with prior art, the present invention having the following advantages and benefits：
Of the invention easy, equipment is simple, easy to control, at low cost, and the processing rate of recovery is high, is based on cutting waste liquor weight
The overall recovery of calculating is up to 28~50%, and wherein polyethylene glycol accounts for that 23~35%, silicon carbide accounts for 3-12%, silicon accounts for 1-2%.And
It recycles obtained product quality to be attained by or be near the mark the index of product, can directly be applied in manufacture of solar cells
Or it is applied in other industrial circles.The method of the present invention has very big economic benefit, has also made very big contribution for environmental protection, has been one
There is very much the processing recovery method of the monocrystalline silicon cutting waste liquor of development prospect.
Detailed description of the invention
Attached drawing described herein is used to provide to further understand the embodiment of the present invention, constitutes one of the application
Point, do not constitute the restriction to the embodiment of the present invention.In the accompanying drawings：
Fig. 1 is process flow chart of the invention.
Specific embodiment
To make the objectives, technical solutions, and advantages of the present invention clearer, below with reference to embodiment and attached drawing, to this
Invention is described in further detail, and exemplary embodiment of the invention and its explanation for explaining only the invention, are not made
For limitation of the invention.
In embodiment, step (1) can be used and be carried out in high speed agitator, and step (2) can be using anti-in enamel
It answers in kettle and carries out, these equipment should not be identified as the unique apparatus reacted restriction, as long as being able to carry out above-mentioned reaction,
Reaction unit in any case is ok.
Embodiment 1
As shown in Figure 1, certain solar energy high-tech limited liability company is removed the monocrystalline silicon cutting slag of kerosene and is cut useless
Liquid amounts to 1000kg and is put into high speed agitator, and the hydrochloric acid 500L that concentration is 0.1mo1/L, 40 DEG C of temperature, mixing time 20 is added
Minute, obtain mixture；The mixture being discharged from high speed agitator device enters enamel reaction still, and mixture is in enamel reaction still
The heating that temperature is 60 DEG C is carried out, water vapour and polyethylene glycol are steamed by steam, after mixed vapour is condensed by condenser,
Water and polyethylene glycol mixed liquor, mixeding liquid temperature is risen to 75 DEG C and is passed through in dehydrator be dehydrated 15 minutes, moisture is arranged
Polyethylene glycol is recycled to obtain after out, enamel reaction still bottom releases the solid mixture of silicon carbide and silicon；
The solid mixture of silicon carbide and silicon is added in ultrasonic cleaner, the 10% of solid mixture weight is added
Temperature is risen to 50 DEG C, cleans 15 minutes, obtain mixture after the cleaning of silicon carbide and silicon by water；By the clear of silicon carbide and silicon
It washes rear mixture and is put into shaking table, be separated off water and residue, obtain mixture after the slagging-off of silicon carbide and silicon；
Mixture after the slagging-off of silicon carbide and silicon is sent into polytetrafluoroethyllining lining reaction kettle, it is 6% that concentration, which is added,
HNO3The mix acid liquor that the HF for being 25% with concentration is formed, the volume ratio of the two are HNO3:HF=1:6.Every 1 kilogram of silicon carbide and
1.5 kilograms of mix acid liquors are added in mixture after the slagging-off of silicon, and temperature is risen to 40 DEG C, after being stirred to react 15 minutes, then will be warm
Degree rises to 110 DEG C, and silicate fluoride solution is steamed, and colorless and transparent silicate fluoride solution, silicate fluoride solution reprocessing are obtained after condensation
Silicon, residue silicon carbide and acid solution in polytetrafluoroethyllining lining reaction kettle, through filtering, aqueous slkali washing, washing can be recycled to obtain afterwards
It is 7-7.5 to pH, recycles to obtain silicon carbide after dry.
Based single crystal silicon cuts slag and cutting waste liquor 1000kg is calculated, and the polyethylene glycol rate of recovery is that 28%, silicon carbide recycles
Rate is 9%, the silicon rate of recovery is 1.3%.
Embodiment 2
Certain monocrystalline silicon piece manufacturing enterprise is removed into the monocrystalline silicon cutting slag of kerosene and cutting waste liquor amounts to 600kg and is put into high speed
In blender, the hydrochloric acid 180L that concentration is 0.1mo1/L is added, temperature 45 C, mixing time 25 minutes obtain mixture；From height
The mixture of fast blender device discharge enters enamel reaction still, and mixture carries out temperature and be 65 DEG C adding in enamel reaction still
Heat, water vapour and polyethylene glycol are steamed by steam, after mixed vapour is condensed by condenser, obtain the mixed of water and polyethylene glycol
Liquid is closed, mixeding liquid temperature is risen to 70 DEG C and is passed through in dehydrator be dehydrated 20 minutes, is to recycle to obtain poly- second two after moisture discharge
Alcohol, enamel reaction still bottom release the solid mixture of silicon carbide and silicon；
The solid mixture of silicon carbide and silicon is added in ultrasonic cleaner, the 10% of solid mixture weight is added
Temperature is risen to 55 DEG C, cleans 20 minutes, obtain mixture after the cleaning of silicon carbide and silicon by water；By the clear of silicon carbide and silicon
It washes rear mixture and is put into shaking table, be separated off water and residue, obtain mixture after the slagging-off of silicon carbide and silicon；
Mixture after the slagging-off of silicon carbide and silicon is sent into polytetrafluoroethyllining lining reaction kettle, it is 6% that concentration, which is added,
HNO3The mix acid liquor that the HF for being 25% with concentration is formed, the volume ratio of the two are HNO3:HF=1:6.Every 1 kilogram of silicon carbide and
1.7 kilograms of mix acid liquors are added in mixture after the slagging-off of silicon, and temperature is risen to 45 DEG C, is stirred to react after twenty minutes, then will be warm
Degree rises to 120 DEG C, and silicate fluoride solution is steamed, and colorless and transparent silicate fluoride solution, silicate fluoride solution reprocessing are obtained after condensation
Silicon, residue silicon carbide and acid solution in polytetrafluoroethyllining lining reaction kettle, through filtering, aqueous slkali washing, washing can be recycled to obtain afterwards
It is 7-7.5 to pH, recycles to obtain silicon carbide after dry.
Based single crystal silicon cuts slag and cutting waste liquor 600kg is calculated, and the polyethylene glycol rate of recovery is 30%, the silicon carbide rate of recovery
It is 1.4% for 10%, the silicon rate of recovery.
Embodiment 3
Certain monocrystalline silicon piece manufacturing enterprise is removed into the monocrystalline silicon cutting slag of kerosene and cutting waste liquor amounts to 800kg and is put into high speed
In blender, the sulfuric acid 2000L that concentration is 0.1mo1/L is added, temperature 60 C, mixing time 20 minutes obtain mixture；From
The mixture of high speed agitator device discharge enters enamel reaction still, and mixture carries out temperature and be 70 DEG C adding in enamel reaction still
Heat, water vapour and polyethylene glycol are steamed by steam, after mixed vapour is condensed by condenser, obtain the mixed of water and polyethylene glycol
Liquid is closed, mixeding liquid temperature is risen to 65 DEG C and is passed through in dehydrator be dehydrated 20 minutes, is to recycle to obtain poly- second two after moisture discharge
Alcohol, enamel reaction still bottom release the solid mixture of silicon carbide and silicon；
The solid mixture of silicon carbide and silicon is added in ultrasonic cleaner, the 15% of solid mixture weight is added
Temperature is risen to 55 DEG C, cleans 20 minutes, obtain mixture after the cleaning of silicon carbide and silicon by water；By the clear of silicon carbide and silicon
It washes rear mixture and is put into shaking table, be separated off water and residue, obtain mixture after the slagging-off of silicon carbide and silicon；
Mixture after the slagging-off of silicon carbide and silicon is sent into polytetrafluoroethyllining lining reaction kettle, it is 6% that concentration, which is added,
HNO3The mix acid liquor that the HF for being 25% with concentration is formed, the volume ratio of the two are HNO3:HF=1:6.Every 1 kilogram of silicon carbide and
2.1 kilograms of mix acid liquors are added in mixture after the slagging-off of silicon, and temperature is risen to 50 DEG C, is stirred to react after twenty minutes, then will be warm
Degree rises to 130 DEG C, and silicate fluoride solution is steamed, and colorless and transparent silicate fluoride solution, silicate fluoride solution reprocessing are obtained after condensation
Silicon, residue silicon carbide and acid solution in polytetrafluoroethyllining lining reaction kettle, through filtering, aqueous slkali washing, washing can be recycled to obtain afterwards
It is 7-7.5 to pH, recycles to obtain silicon carbide after dry.
Based single crystal silicon cuts slag and cutting waste liquor 800kg is calculated, and the polyethylene glycol rate of recovery is 32%, the silicon carbide rate of recovery
It is 1.7% for 12%, the silicon rate of recovery.
Above-described specific embodiment has carried out further the purpose of the present invention, technical scheme and beneficial effects
It is described in detail, it should be understood that being not intended to limit the present invention the foregoing is merely a specific embodiment of the invention
Protection scope, all within the spirits and principles of the present invention, any modification, equivalent substitution, improvement and etc. done should all include
Within protection scope of the present invention.
Claims (10)
1. the recovery and treatment method of a kind of monocrystalline silicon cutting slag and cutting waste liquor, which is characterized in that include the following steps：
(1), at place, monocrystalline silicon with stirring cuts and acid is added in slag and cutting waste liquor, and mixed liquor is obtained after being stirred to react；
(2), mixed liquor heating evaporation is separated by solid-liquid separation, obtains the solid mixture and gas of silicon carbide, silicon and impurity,
Gas is steamed to the mixed liquor that water and polyethylene glycol are obtained after condensing, heating drains to obtain polyethylene glycol after dehydration；
(3), the solid mixture of silicon carbide, silicon and impurity is obtained into the solid of silicon carbide and silicon through concussion cleaning and Gravity Separation
Mixture；
(4), the solid mixture of silicon carbide and silicon is added in the mixed acid solution of nitric acid and HF composition, by fluorine silicon after reaction
Acid steams, and condenses to obtain fluosilicic acid, then fluosilicic acid is processed recycling silicon, remaining silicon carbide and acid solution after reaction, filtering pickling, washing
And dry silicon carbide.
2. recovery and treatment method according to claim 1, which is characterized in that in step (1) concentration of hydrochloric acid be 0.001~
0.5mo1/L, per kilogram monocrystalline silicon cuts slag and 200~700ml hydrochloric acid solution is added in cutting waste liquor.
3. recovery and treatment method according to claim 1, which is characterized in that reaction temperature is 40~60 DEG C in step (1),
Mixing time is 15~35min.
4. recovery and treatment method according to claim 1, which is characterized in that the concussion cleaning in step (3) is using ultrasound
Wave cleaning.
5. recovery and treatment method according to claim 4, which is characterized in that the weight of water is added during ultrasonic cleaning
For the 10-20wt% of the solid mixture weight of silicon carbide, silicon and impurity, temperature is 40~80 DEG C.
6. recovery and treatment method according to claim 1, which is characterized in that concentration of nitric acid 6wt%, HF concentration is
25wt%.
7. recovery and treatment method according to claim 1, which is characterized in that the volume ratio of nitric acid and HF are 1:6~8.
8. recovery and treatment method according to claim 1, which is characterized in that every 1 kilogram of silicon carbide and silicon in step (4)
The mix acid liquor of 1.5~2 kilograms of nitric acid and HF is added in solid mixture.
9. recovery and treatment method according to claim 1, which is characterized in that first rising reaction temperature in step (4)
To 30~60 DEG C, after being stirred to react 10~30min, then temperature risen to 100~130 DEG C.
10. recovery and treatment method according to claim 1, which is characterized in that baffle-type dehydrator, gravity are specifically used in dehydration
Formula dehydrator, cyclone type dehydrator, spraying dehydrator carry out.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114621756A (en) * | 2022-03-28 | 2022-06-14 | 南昌大学 | Method for preparing Mn4+ activated fluoride red fluorescent powder by using recycled silicon sawdust powder |
| CN117585679A (en) * | 2024-01-19 | 2024-02-23 | 昆明理工大学 | Method for preparing high-purity semi-insulating SiC powder by high-temperature solution method |
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| CN101474511A (en) * | 2008-12-17 | 2009-07-08 | 西安交通大学 | Process for recovering polyethylene glycol and silicon carbide in waste mortar from silicon wafer wire cutting |
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| CN101113029A (en) * | 2006-07-26 | 2008-01-30 | 金柏林 | Treatment recovery method for monocrystalline silicon cutting waste liquor |
| CN101327622A (en) * | 2007-06-21 | 2008-12-24 | 正申科技（北京）有限责任公司 | Mortar recovery technique for cutting single-crystal and polycrystalline silicon wire |
| CN101239246A (en) * | 2008-02-20 | 2008-08-13 | 江南大学 | Method for recovering cutting solution from by-product of silicon chip cutting processing |
| CN101474511A (en) * | 2008-12-17 | 2009-07-08 | 西安交通大学 | Process for recovering polyethylene glycol and silicon carbide in waste mortar from silicon wafer wire cutting |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114621756A (en) * | 2022-03-28 | 2022-06-14 | 南昌大学 | Method for preparing Mn4+ activated fluoride red fluorescent powder by using recycled silicon sawdust powder |
| CN117585679A (en) * | 2024-01-19 | 2024-02-23 | 昆明理工大学 | Method for preparing high-purity semi-insulating SiC powder by high-temperature solution method |
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Application publication date: 20181130 |