CN102815700A - Method for preparing nanometer silicon carbide by recycling silicon cut wastes - Google Patents
Method for preparing nanometer silicon carbide by recycling silicon cut wastes Download PDFInfo
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- CN102815700A CN102815700A CN2012103459640A CN201210345964A CN102815700A CN 102815700 A CN102815700 A CN 102815700A CN 2012103459640 A CN2012103459640 A CN 2012103459640A CN 201210345964 A CN201210345964 A CN 201210345964A CN 102815700 A CN102815700 A CN 102815700A
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Abstract
The invention belongs to the field of nanometer silicon carbide preparation and in particular provides a method for preparing nanometer silicon carbide by recycling silicon cut wastes. The method specifically comprises the following steps of: firstly grinding recycled silicon wastes to the particles suitable for the melting stage, adopting cleaning agents such as water, hydrochloric acid and hydrogen peroxide mixed water solution, hydrofluoric acid water solution, ammonia water, ethanol water solution and the like to clean silicon powder, putting the dried silicon powder in a graphite crucible, and calcining the silicon powder in a vacuum electric furnace or a hydrogen protected electric furnace at 1600 DEG C for 3-5 hours, thus obtaining the nanometer silicon carbide. The method has the following beneficial effects: the problem of silicon cut waste treatment is solved; the preparation steps are simple, and the conditions are mild; and the diameter of the prepared nanometer silicon carbide is about 20-50nm, the length is about 4-5mu m, and the length-diameter ratio is far higher than 20.
Description
Technical field
The invention belongs to the nanometer silicon carbide preparation field, be specially a kind of recovery silicon waste cut materials and prepare method of nanometer carborundum.
Background technology
Silit is as a kind of inorganic materials of excellent performance; Have high temperature oxidation resistance, resistance to chemical corrosion, heat-shock resistance, wear resistance; And the physical strength under normal temperature and high temperature is also very high, is widely used in every field such as aviation, automobile, chemical industry, electronic industry, biological ceramics.。
Silicon carbide products mainly is divided into nano silicon carbide granulate and nanometer silicon carbide whiskers.It has purity height, particle diameter little, be evenly distributed; Specific surface area is big, high surface; Density is low, has fabulous mechanics, calorifics, electricity and chemical property, promptly has high firmness, high-wearing feature and the good big characteristics of self-lubricating, high thermoconductivity, low thermal coefficient of expansion and hot strength.
Nanometer silicon carbide is mainly used in following aspect: one, modified high-strength degree nylon alloy is used novel material: the good good dispersion degree of nanometer β-sic powder granule consistency in polymer composite; Good with matrix bond property; The high-strength nylon strength of alloy improves more than 10% than common PA6 after the modification; Wear resisting property improves more than 2.5 times, and customer responsiveness is fine.Be mainly used in a tracked armored vehicle polymer accessory, motor turning parts, textile manufacturing machine, the mining machinery liner plate, sintering such as train parts etc. at a lower temperature just can reach densification.Two, modification special engineering plastics polyetheretherketone (PEEK) wear resisting property: carry out the nanometer silicon carbide after the surface treatment with coupling agent, when addition is 10% left and right sides, can improve the wear resistance of PEEK greatly.(use abrasive manner that micron order silit fills PEEK with pears cut with abrasive wear be main, and the abrasive manner that uses nanometer silicon carbide to fill PEEK to shift wearing and tearing with slight adhesion be main.Three, nanometer silicon carbide is in the application of rubber tyre: add certain amount of nano silit and carry out modification and handle not changing the virgin rubber prescription, under the prerequisite that does not reduce its original performance and quality, its wear resistance can improve 15%-30%.In addition, 20 nanometer silicon carbides are applied in rubber products such as rubber roller, stamping machine photographic fixing film etc. are wear-resisting, heat radiation, heatproof.Four, metallic surface such as nano SiC composite nickel-plating: adopt second composite grain of nano_scale particle; Nickel is matrix metal; Form high-compactness in the metallic surface; The extraordinary galvanic deposit composite deposite of bonding force, its metallic surface have superhard (wear-resisting) and the resistant to elevated temperatures characteristics of anti-attrition (self-lubricating).Its composite deposite microhardness increases substantially, wear resistance improve 3-5 doubly, work-ing life improve 2-4 doubly, coating is strong with bonding force raising 30-40%, the covering power of matrix, coating is even, level and smooth, careful.Five, space material: the space shuttle fuselage covers and makes with the SiC matrix material, and it is made installation costs and reaches 10.8$/cm2, every watt of thick 50.8mm, 1.21kg/ sheet, 70,000 yuan/machine.Other application: high performance structure ceramic (like rocket nozzle, nuclear industry etc.), absorbing material, anti-wear lubricating grease, high-performance brake facing, high hardness wear-resisting powder coating, composite ceramics strengthen toughness reinforcing etc.
At present, the method for synthesizing silicon carbide powder mainly contains Acheson method, direct chemical combination method, thermal decomposition method and gas-phase reaction method etc.Because synthesis step is complicated, energy consumption is big, and the nanometer silicon carbide market value is expensive, has reached 2000 yuan/kilogram.
Summary of the invention
The object of the invention is to provide a kind of recovery silicon waste cut materials to prepare method of nanometer carborundum; The polysilicon that this method prepares has utilization of waste material, green high-efficient, and technology is simple; Characteristics with low cost; The about 20-50nm of prepared nanometer silicon carbide diameter, about 4 ~ 5 μ m of length, length-to-diameter ratio is far above 20.
A kind of recovery silicon waste cut materials that the present invention proposes prepares method of nanometer carborundum, and concrete steps are following:
(1) the bulk si waste cut materials is added in the entry, utilize ultrasonic it to be dispersed as small-particle, clean, obtain black suspension after ultrasonic 25-35 minute with organic solvent is auxiliary; Said suspension-s obtains the silica flour of elementary cleaning through suction filtration or spinning;
(2) the mixing solutions ultrasonic cleaning that the elementary silica flour that step (1) is obtained is formed with hydrochloric acid, water and hydrogen peroxide 8-15 minute is filtered;
(3) in the silica flour that step (2) obtains, add deionized water, ultrasonic cleaning 8-15 minute, filter;
(4) in the silica flour that step (3) obtains, add hydrofluoric acid solution, ultrasonic cleaning 0.8-1.2 minute, filter;
(5) silica flour that obtains to step (4) adds excessive ammonia, ultrasonic cleaning 8-12 minute, filters;
(6) in the silica flour that step (5) obtains, add in the 10wt% aqueous ethanolic solution, ultrasonic 18-25 minute, filter;
(7) silica flour that step (6) is obtained is used washed with de-ionized water, filters oven dry;
(8) silica flour that step (7) is obtained is put into plumbago crucible, uses vacuum electric furnace or hydrogen shield electric furnace sintering 3 ~ 5 hours under 1550 ~ 1600 ℃ of conditions, and naturally cooling promptly obtains the nanometer silicon carbide of greyish-green.
Among the present invention, silicon waste cut materials described in the step (1) is through settled silicon mud in the cutting waste fluid that contains silica flour, the waste tank.
Among the present invention, organic solvent described in the step (1) adopts ethanol.
Among the present invention, the volume ratio of the said hydrochloric acid of step (2), water and hydrogen peroxide is 5:1:1 to 7:1:1.
Among the present invention, the said hydrofluoric acid solution proportioning of step (4) is according to HF:H
2The O volume ratio is 1:40 ~ 1:60.
Among the present invention, the said excessive ammonia of step (5) is that the pH value of scavenging solution is 8 ~ 10.
Among the present invention, oven dry described in the step (7) is meant and places 80 ~ 90 ℃ of vacuum drying ovens to dry silica flour.
Among the present invention, prepared nanometer silicon carbide diameter is 20-50nm, and length is 4 ~ 5 μ m, and length-to-diameter ratio is far above 20.
The present invention has following beneficial effect:
1, the invention solves silicon cutting waste disposal problem, preparation process is simple, mild condition.
2, the about 20-50nm of nanometer silicon carbide diameter of the present invention's preparation, about 4 ~ 5 μ m of length, length-to-diameter ratio is far above 20.
Description of drawings
The nanometer silicon carbide macro morphology that Fig. 1 makes for embodiment 1, tangent plane pattern and bottom pattern.Wherein: (a) being the side, (b) is tangent plane, (c) is the bottom.
Fig. 2 makes the SEM figure of nanometer silicon carbide for embodiment 1.Wherein: (a) for amplifying 50 times, (b) for amplifying 1000 times, (c) for amplifying 5000 times, (d) for amplifying 40000 times.
Fig. 3 is cleaning silica flour process schema.
Embodiment
Following embodiment further specifies of the present invention, rather than limits scope of the present invention.
Embodiment 1:
The silicon waste cut materials that experiment is adopted is by providing between Shanghai silicon chip source mill monocrystalline cutting car, selects for use in the waste tank through settled silicon mud as raw material.
Get the settled silicon mud of 50g and add in the entry, utilize ultrasonic block smear metal to be dispersed as small-particle, clean with ethanol is auxiliary simultaneously, after ultrasonic 30 minutes, suction filtration obtains the silica flour of elementary cleaning.Use hydrochloric acid, water, (hydrochloric acid: water: hydrogen peroxide is 6:1:1) ultrasonic cleaning 10 minutes, after-filtration are dissolved in the mixing of hydrogen peroxide.The silica flour that obtains is added (HF:H in the hydrofluoric acid aqueous solution
2O is 1:50) ultrasonic 1 minute, after-filtration.The silica flour that obtains is with 10wt% aqueous ethanolic solution ultrasonic cleaning 20 minutes, filters the back with washed with de-ionized water 3 times, and the silica flour that suction filtration obtains places 80 ℃ of vacuum drying ovens to dry.The silica flour of oven dry is put into plumbago crucible, and calcining is 5 hours in 1600 ℃ vacuum electric furnace, and naturally cooling can obtain nanometer silicon carbide.Through test, the nanometer silicon carbide diameter that obtains is at 30-50nm, about 4 ~ 5 μ m of length.
Embodiment 2:
The silicon waste cut materials that experiment is adopted is by providing between Shanghai silicon chip source mill monocrystalline cutting car, selects for use in the waste tank through settled silicon mud as raw material.
Get the settled silicon mud of 20g and add in the entry, utilize ultrasonic block smear metal to be dispersed as small-particle, clean with ethanol is auxiliary simultaneously, after ultrasonic 30 minutes, suction filtration obtains the silica flour of elementary cleaning.Use hydrochloric acid, water, (hydrochloric acid: water: hydrogen peroxide is 5:1:1) ultrasonic cleaning 10 minutes, after-filtration are dissolved in the mixing of hydrogen peroxide.The silica flour that obtains is added (HF:H in the hydrofluoric acid aqueous solution
2O is 1:40) ultrasonic 1 minute, after-filtration.The silica flour that obtains is with 10wt% aqueous ethanolic solution ultrasonic cleaning 20 minutes, filters the back with washed with de-ionized water 3 times, and the silica flour that suction filtration obtains places 80 ℃ of vacuum drying ovens to dry.The silica flour of oven dry is put into plumbago crucible, and calcining is 4 hours in 1550 ℃ vacuum electric furnace, and naturally cooling can obtain nanometer silicon carbide.Through test, the nanometer silicon carbide diameter that obtains is at 20-40nm, about 4 ~ 5 μ m of length.
Through regulating the different proportionings of clean-out system, change calcining temperature and time, all can obtain the about 20-50nm of diameter, about 4 ~ 5 μ m of length, length-to-diameter ratio is far above 20 nanometer silicon carbide.
Claims (8)
1. a recovery silicon waste cut materials prepares method of nanometer carborundum, it is characterized in that concrete steps are following:
(1) the bulk si waste cut materials is added in the entry, utilize ultrasonic it to be dispersed as small-particle, clean, obtain black suspension after ultrasonic 25-35 minute with organic solvent is auxiliary; Said suspension-s obtains the silica flour of elementary cleaning through suction filtration or spinning;
(2) the mixing solutions ultrasonic cleaning that the elementary silica flour that step (1) is obtained is formed with hydrochloric acid, water and hydrogen peroxide 8-15 minute is filtered;
(3) in the silica flour that step (2) obtains, add deionized water, ultrasonic cleaning 8-15 minute, filter;
(4) in the silica flour that step (3) obtains, add hydrofluoric acid solution, ultrasonic cleaning 0.8-1.2 minute, filter;
(5) silica flour that obtains to step (4) adds excessive ammonia, ultrasonic cleaning 8-12 minute, filters;
(6) in the silica flour that step (5) obtains, add in the 10wt% aqueous ethanolic solution, ultrasonic 18-25 minute, filter;
(7) silica flour that step (6) is obtained is used washed with de-ionized water, filters oven dry;
(8) silica flour that step (7) is obtained is put into plumbago crucible, uses vacuum electric furnace or hydrogen shield electric furnace sintering 3 ~ 5 hours under 1550 ~ 1600 ℃ of conditions, and naturally cooling promptly obtains the nanometer silicon carbide of greyish-green.
2. a kind of recovery silicon waste cut materials according to claim 1 prepares method of nanometer carborundum, it is characterized in that: silicon waste cut materials described in the step (1) is through settled silicon mud in the cutting waste fluid that contains silica flour, the waste tank.
3. a kind of recovery silicon waste cut materials according to claim 1 prepares method of nanometer carborundum, it is characterized in that: organic solvent described in the step (1) adopts ethanol.
4. a kind of recovery silicon waste cut materials according to claim 1 prepares method of nanometer carborundum, it is characterized in that: the volume ratio of the said hydrochloric acid of step (2), water and hydrogen peroxide is 5:1:1 to 7:1:1.
5. a kind of recovery silicon waste cut materials according to claim 1 prepares method of nanometer carborundum, it is characterized in that: the said hydrofluoric acid solution proportioning of step (4) is according to HF:H
2The O volume ratio is 1:40 ~ 1:60.
6. a kind of recovery silicon waste cut materials according to claim 1 prepares method of nanometer carborundum, it is characterized in that: the said excessive ammonia of step (5) is that the pH value of scavenging solution is 8 ~ 10.
7. a kind of recovery silicon waste cut materials according to claim 1 prepares method of nanometer carborundum, it is characterized in that: oven dry described in the step (7) is meant and places 80 ~ 90 ℃ of vacuum drying ovens to dry silica flour.
8. a kind of recovery silicon waste cut materials according to claim 1 prepares method of nanometer carborundum, and it is characterized in that: prepared nanometer silicon carbide diameter is 20-50nm, and length is 4 ~ 5 μ m, and length-to-diameter ratio is far above 20.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103359736A (en) * | 2013-07-17 | 2013-10-23 | 海南大学 | Method for purifying and preparing silicon carbide powder from crystalline silicon cutting waste mortar |
| CN103586229A (en) * | 2013-11-08 | 2014-02-19 | 无锡英普林纳米科技有限公司 | Method for improving nanometer stamper bonding resistance |
| CN105293498A (en) * | 2015-10-30 | 2016-02-03 | 北京科技大学 | Method for preparing silicon carbide powder from polycrystalline silicon cutting wastes |
| CN105818287A (en) * | 2016-05-31 | 2016-08-03 | 上海纳晶科技有限公司 | Method for preparing high-purity submicron hydrated silica and silica microparticles in batch |
| CN110791356A (en) * | 2019-11-14 | 2020-02-14 | 王思记 | Method for preparing solid lubricating material by using cutting slurry after silicon wafer cutting |
| US20210253435A1 (en) * | 2018-06-14 | 2021-08-19 | Rosi | Treatment process for recycling silicon ingot cutting waste |
| CN113908633A (en) * | 2021-10-25 | 2022-01-11 | 安徽欣创节能环保科技股份有限公司 | Low-resistance high-efficiency bag type dust collector based on high-strength filter bag |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103359736A (en) * | 2013-07-17 | 2013-10-23 | 海南大学 | Method for purifying and preparing silicon carbide powder from crystalline silicon cutting waste mortar |
| CN103586229A (en) * | 2013-11-08 | 2014-02-19 | 无锡英普林纳米科技有限公司 | Method for improving nanometer stamper bonding resistance |
| CN105293498A (en) * | 2015-10-30 | 2016-02-03 | 北京科技大学 | Method for preparing silicon carbide powder from polycrystalline silicon cutting wastes |
| CN105818287A (en) * | 2016-05-31 | 2016-08-03 | 上海纳晶科技有限公司 | Method for preparing high-purity submicron hydrated silica and silica microparticles in batch |
| US20210253435A1 (en) * | 2018-06-14 | 2021-08-19 | Rosi | Treatment process for recycling silicon ingot cutting waste |
| CN110791356A (en) * | 2019-11-14 | 2020-02-14 | 王思记 | Method for preparing solid lubricating material by using cutting slurry after silicon wafer cutting |
| CN113908633A (en) * | 2021-10-25 | 2022-01-11 | 安徽欣创节能环保科技股份有限公司 | Low-resistance high-efficiency bag type dust collector based on high-strength filter bag |
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Application publication date: 20121212 |