CN103553002A - Method for preparation of high purity alpha phase silicon nitride powder from recovered silicon chip cut sawdust - Google Patents
Method for preparation of high purity alpha phase silicon nitride powder from recovered silicon chip cut sawdust Download PDFInfo
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Abstract
The invention provides a method for preparation of high purity alpha phase silicon nitride powder from recovered silicon chip cut sawdust. The method is characterized by: subjecting silicon chip sawdust powder to nitridation to obtain silicon nitride, then carrying out grinding, pickling, washing, drying and other processes, thus obtaining the high purity alpha phase silicon nitride powder. The obtained product has high purity, an alpha phase content of greater than 93%, an oxygen content of less than 1.5%, and high powder sintering activity. The method provided by the invention has the characteristics of no need for diluent and catalyst during production, simple process, low cost and easy mass production, and can be used for realizing high value-added utilization of silicon chip cut sawdust.
Description
Technical field
The present invention relates to the method for normal pressure Direct-Nitridation synthesizing silicon nitride powder, being particularly related to reclaim silicon chip sawdust powder is raw material, the method that once beta-silicon nitride powder is synthesized in nitrogenize in the condition of diluent free, catalyzer, belongs to ceramic preparing technical field.
Background technology
Silicon nitride ceramics has unique physical and mechanical properties, as low density, high strength, high rigidity, wear-resistant, corrosion-resistant, good thermostability, in fields such as Aeronautics and Astronautics, chemical industry, the energy, machinofacture, weapon industry, metal metallurgy smeltings, have a wide range of applications.But the quality of the expensive and beta-silicon nitride powder of silicon nitride ceramics has restricted the mass-producing application of silicon nitride.
The beta-silicon nitride powder technology of preparing of research and development respectively has relative merits in the world.The silicon imide pyrolysis method of UBE company, quality product is high, but complex process, preparation cost is expensive, and less enterprise adopts; Gas phase synthesis method is difficult to realize scale operation; In the prepared product of silicon-carbon oxide hot reducing method, contain higher Prevent Carbon Contamination; Current most enterprise still continues to use silicon powder nitride method, wherein generally needs to adopt secondary nitrogenize, adds thinner, adds the technology such as catalyzer, fluidization technology, the processing of silica flour mechanical activation.This class technology ubiquity preparation cycle is long, energy consumption is high, impurity in products content is high, equipment is complicated and high in cost of production shortcoming.
At solar cell substrate, produce a large amount of silicon chip sawdust in the preparation process of the thin sheet products such as substrate, electronic chip, accurate semi-conductor chip for unicircuit, comprise band sawdust, abrasive dust, diamond wire sawdust etc.With Silicon Wafer line, be cut into example, silicon wafer thickness is generally about 0.22mm, and line kerf width is 0.18～0.30mm, this means that 40～60% HIGH-PURITY SILICON material become sawdust and enter slip.Except the waste and old sawdust that silicon carbide abrasive sand slurry cooperation wire saw cutting silicon crystal circle produces, the waste and old sawdust main component that other cutting technique produces is silicon grain and a small amount of metallic impurity, in part sawdust, contains the cooling fluids such as polyoxyethylene glycol.Its silicon grain is only subject to the pollutions such as metallic impurity for surface, inside is still HIGH-PURITY SILICON material, and impurity does not enter silicon crystal lattice, therefore can obtain HIGH-PURITY SILICON powder by conventional pickling, washing process.But because the particle diameter of silicon powder is meticulous, too high oxygen level, cannot be directly used in pulling of crystals silicon rod, casting polycrystalline silicon ingot raw material.Therefore, how to make full use of the silicon sawdust of reclaim purifying and become urgent problem.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of the material powder for special cermacis preparation and photovoltaic crucible coating layer etc., the method of the high-purity α phase silicon nitride powder of a kind of low-cost preparation is particularly provided, has more particularly been to provide a kind of method of preparing high-purity α phase silicon nitride powder to reclaim filings obtained through silicon wafer cutting.Technique of the present invention is simple, and preparation cost is cheap.
The present invention is achieved like this, and a kind of method of preparing high-purity α phase silicon nitride powder to reclaim filings obtained through silicon wafer cutting, comprises the steps:
One, nitrogenize: adopt atmosphere protection stove to carry out nitrogenize to reclaiming the silicon chip sawdust powder of purifying, the protective atmosphere adopting during nitrogenize is one or more mixed gass in nitrogen, nitrogen and hydrogen mixture, ammonia, adopt argon gas as assist gas, top temperature is 1250 ℃～1380 ℃, in nitridation process, soaking time is determined according to the consumption of raw material, raw material consumption is more, and soaking time is longer;
Two, grinding: with milling equipment, as ball mill, vibration mill, stirring mill, micronizer mill etc. carry out grinding to nitrogenize product, until reach desired particle size requirement;
Three, pickling: the silicon nitride powder that uses mineral acid to go out grinding carries out pickling impurity removal;
Four, washing: remaining acid and other impurity after washing removal pickling;
Five, dry: to dry and obtain high-purity α phase silicon nitride powder.
On the basis of such scheme, the present invention can also do following improvement.
Described silicon chip sawdust powder is the sawdust waste material by the Silicon Wafer cutting of polysilicon and the industry use of monocrystaline silicon solar cell Pian, electronic semi-conductor is produced, comprise band sawdust, abrasive dust, diamond wire sawdust, and silane thermal decomposition process is produced the superfine silica powder producing in polysilicon process and is carried out conventional pickling, washing, stoving process and reclaim to purify and obtain.
The volume fraction of described argon gas can change between 0%～80%.And with the prolongation of nitridation time, argon gas volume fraction can reduce gradually.Be preferably 10%～60%.
In described nitrogen and hydrogen mixture, the volume fraction of hydrogen can change in 0%～50% scope, is preferably 5%～15%.
Described nitriding temperature can be chosen two sections or multistage and carry out, and first stage temperature is 600 ℃～900 ℃, can 5 ℃～10 ℃ intensifications of fast speed per minute; With 1 ℃～5 ℃ speed of per minute, heat up subsequently, top temperature is 1250 ℃～1380 ℃.
Technique effect of the present invention is: the present invention is based on contriver to high purity silicon nitride powder synthetic a large amount of system experimentations research and propose.Reclaim the silicon sawdust of purifying and after simple process, can directly prepare high purity silicon nitride powder at the nitrogenize initial stage, products obtained therefrom purity is high, α phase content > 93%, oxygen level < 1.5%, powder sintering activity is high, can be used as the material powder of special cermacis preparation and photovoltaic crucible coating layer etc.This preparation method not only can significantly reduce raw materials cost, and without any additive a nitrogenize, completes in preparation process, has reduced the preparation cost of product, has improved the purity of product simultaneously.
Accompanying drawing explanation
Fig. 1 is the silicon nitride product X RD collection of illustrative plates of preparation described in the embodiment of the present invention 1.
Embodiment
For the ease of understanding, below in conjunction with preferred embodiment, the present invention is further illustrated in detail.
Embodiment 1-embodiment 3 is raw materials used for reclaiming the silicon chip diamond wire sawdust of purifying.Derive from the waste and old sawdust that consolidated diamond wire saw cutting silicon wafer produces, its ICP-AES (plasmon coupling atomic spectrograph) analytical results that reclaims the front and back major metal foreign matter content of purifying is as shown in table 1.
Table 1 embodiment of the present invention 1-embodiment 3 silicon chip diamond wire sawdust used reclaims the major metal composition (ppmw) before and after purifying
Embodiment 4-embodiment 6 is raw materials used for reclaiming the silica brick band sawdust of purifying.Derive from the waste and old sawdust that consolidated diamond band saw cutting silica brick produces, its ICP-AES (plasmon coupling atomic spectrograph) analytical results that reclaims the front and back major metal foreign matter content of purifying is as shown in table 2.
Table 2 embodiment of the present invention 4-embodiment 6 silica brick band sawdust used reclaims the major metal composition (ppmw) before and after purifying
Embodiment 1
Get silicon chip diamond wire sawdust, reclaiming the rear silicon wafer wire saw bits powder of purifying is raw material, and its major metal foreign matter content analytical results is as shown in table 1.
Get 100 grams of this material powders, pine is loaded in atmosphere protection stove; The mode of taking segmentation insulation, holding temperature is chosen respectively 1000 ℃, 1300 ℃ and 1350 ℃, and soaking time is corresponding to be respectively 2 hours, 2 hours and 6 hours; The volume fraction of hydrogen is 5% of nitrogen and hydrogen total amount, and nitrogen hydrogen mixeding gas total flux is controlled at 200ml/min; Argon content original volume mark is gas gross 50%, with reaction process, is reduced to gradually zero.Be cooled to 700 ℃ of left and right and stop ventilation, cool to afterwards room temperature with the furnace and come out of the stove.
Synthetic product is soft block, and color homogeneous is removed after the portion of a small amount of limit, detects in product and only contains alpha silicon nitride and beta silicon nitride, as shown in Figure 1 with x-ray powder diffraction instrument.Wherein α phase content is 93.8%.It is 1.11% that oxygen-nitrogen analyzer records oxygen level in product, and nitrogen content is 38.2%.Product is after stirring abrasive dust mill, HCl pickling, washing, 50 ℃ and being dried, and its major metal foreign matter content is as shown in table 3.
The detection technique index of table 3 example 1 gained nitrogenize product of the present invention
Embodiment 2
Get silicon chip diamond wire sawdust, reclaiming the rear silicon wafer wire saw bits powder of purifying is raw material, and its major metal foreign matter content analytical results is as shown in table 1.
Get 160 grams of this material powders, pine is loaded in atmosphere protection stove; The mode of taking segmentation insulation, holding temperature is chosen respectively 800 ℃, 1200 ℃, 1300 ℃ and 1370 ℃, and soaking time is corresponding to be respectively 1 hour, 1 hour, 1 hour and 4 hours; The volume fraction of hydrogen is 15% of nitrogen and hydrogen total amount, and nitrogen hydrogen mixeding gas total flux is controlled at 150ml/min; Argon content original volume mark is gas gross 60%, with reaction process, is reduced to gradually zero.Be cooled to 700 ℃ of left and right and stop ventilation, cool to afterwards room temperature with the furnace and come out of the stove.
Synthetic product is soft block, and color homogeneous is removed after the portion of a small amount of limit, with x-ray powder diffraction instrument, detects in product and only contains alpha silicon nitride and beta silicon nitride, and wherein α phase content is 94.2%.It is 1.21% that oxygen-nitrogen analyzer records oxygen level in product, and nitrogen content is 38.4%.Product is through stirring abrasive dust mill, HNO
3after pickling, washing, 50 ℃ are dry, its major metal foreign matter content is as shown in table 4.
The detection technique index of table 4 example 2 gained nitrogenize products of the present invention
Embodiment 3
Get silicon chip diamond wire sawdust, reclaiming the rear silicon wafer wire saw bits powder of purifying is raw material, and its major metal foreign matter content analytical results is as shown in table 1.
Get 200 grams of this material powders, pine is loaded in atmosphere protection stove; The mode of taking segmentation insulation, holding temperature is chosen respectively 900 ℃, 1250 ℃ and 1350 ℃, and soaking time is corresponding to be respectively 2 hours, 2 hours and 8 hours; The volume fraction of hydrogen is 10% of nitrogen and hydrogen total amount, and nitrogen hydrogen mixeding gas total flux is controlled at 100ml/min; Argon content original volume mark is gas gross 20%, with reaction process, is reduced to gradually zero.Be cooled to 700 ℃ of left and right and stop ventilation, cool to afterwards room temperature with the furnace and come out of the stove.
Synthetic product is soft block, and color homogeneous is removed after the portion of a small amount of limit, with x-ray powder diffraction instrument, detects in product and only contains alpha silicon nitride and beta silicon nitride, and wherein α phase content is 93.9%.It is 1.06% that oxygen-nitrogen analyzer records oxygen level in product, and nitrogen content is 38.4%.Product is through stirring abrasive dust mill, HNO
3after pickling, washing, 50 ℃ are dry, its major metal foreign matter content is as shown in table 5.
The detection technique index of table 5 example 3 gained nitrogenize products of the present invention
Embodiment 4
Get silica brick band sawdust, reclaiming the rear sawdust powder of purifying is raw material, and its major metal foreign matter content analytical results is as shown in table 2.
Get 150 grams of this material powders, pine is loaded in atmosphere protection stove; The mode of taking segmentation insulation, holding temperature is chosen respectively 1000 ℃, 1300 ℃ and 1360 ℃, and soaking time is corresponding to be respectively 1 hour, 2 hours and 7 hours; The volume fraction of hydrogen is 5% of nitrogen and hydrogen total amount, and nitrogen hydrogen mixeding gas total flux is controlled at 200ml/min; Argon content original volume mark is gas gross 30%, with reaction process, is reduced to gradually zero.Be cooled to 700 ℃ of left and right and stop ventilation, cool to afterwards room temperature with the furnace and come out of the stove.
Synthetic product is soft block, and color homogeneous is removed after the portion of a small amount of limit, with x-ray powder diffraction instrument, detects in product and only contains alpha silicon nitride and beta silicon nitride, and wherein α phase content is 95.1%.It is 1.23% that oxygen-nitrogen analyzer records oxygen level in product, and nitrogen content is 38.1%.Product is after stirring abrasive dust mill, HF pickling, washing, 50 ℃ and being dried, and its major metal foreign matter content is as shown in table 6.
The detection technique index of table 6 example 4 gained nitrogenize products of the present invention
Embodiment 5
Get silica brick band sawdust, reclaiming the rear sawdust powder of purifying is raw material, and its major metal foreign matter content analytical results is as shown in table 2.
Get 180 grams of this material powders, pine is loaded in atmosphere protection stove; The mode of taking segmentation insulation, holding temperature is chosen respectively 1000 ℃, 1270 ℃ and 1370 ℃, and soaking time is corresponding to be respectively 1 hour, 3 hours and 6 hours; The volume fraction of hydrogen is 15% of nitrogen and hydrogen total amount, and nitrogen hydrogen mixeding gas total flux is controlled at 150ml/min; Argon content original volume mark is gas gross 10%, with reaction process, is reduced to gradually zero.Be cooled to 700 ℃ of left and right and stop ventilation, cool to afterwards room temperature with the furnace and come out of the stove.
Synthetic product is soft block, and color homogeneous is removed after the portion of a small amount of limit, with x-ray powder diffraction instrument, detects in product and only contains alpha silicon nitride and beta silicon nitride, and wherein α phase content is 93.2%.It is 0.94% that oxygen-nitrogen analyzer records oxygen level in product, and nitrogen content is 38.5%.Product through stir abrasive dust mill, HF and HCl mixing pickling, washing, 50 ℃ be dried after, its major metal foreign matter content is as shown in table 7.
The detection technique index of table 7 example 5 gained nitrogenize products of the present invention
Embodiment 6
Get silica brick band sawdust, reclaiming the rear sawdust powder of purifying is raw material, and its major metal foreign matter content analytical results is as shown in table 2.
Get 300 grams of this material powders, pine is loaded in atmosphere protection stove; The mode of taking segmentation insulation, holding temperature is chosen respectively 900 ℃, 1250 ℃, 1300 ℃ and 1350 ℃, and soaking time is corresponding to be respectively 2 hours, 4 hours, 4 hours and 6 hours; The volume fraction of hydrogen is 5% of nitrogen and hydrogen total amount, and nitrogen hydrogen mixeding gas total flux is controlled at 200ml/min; Argon content original volume mark is gas gross 40%, with reaction process, is reduced to gradually zero.Be cooled to 700 ℃ of left and right and stop ventilation, cool to afterwards room temperature with the furnace and come out of the stove.
Synthetic product is soft block, and color homogeneous is removed after the portion of a small amount of limit, with x-ray powder diffraction instrument, detects in product and only contains alpha silicon nitride, beta silicon nitride and silicon carbide.Wherein silicon nitride α/(alpha+beta) phase content is 95.5%.It is 1.23% that oxygen-nitrogen analyzer records oxygen level in product.
Synthetic product is soft block, and color homogeneous is removed after the portion of a small amount of limit, with x-ray powder diffraction instrument, detects in product and only contains alpha silicon nitride and beta silicon nitride, and wherein α phase content is 95.5%.It is 1.23% that oxygen-nitrogen analyzer records oxygen level in product, and nitrogen content is 38.6%.Product is through stirring abrasive dust mill, H
2sO
4after pickling, washing, 50 ℃ are dry, its major metal foreign matter content is as shown in table 8.
The detection technique index of table 8 example 6 gained nitrogenize products of the present invention
Above-described embodiment is explained in detail embodiments of the present invention; but can not be interpreted as limiting the scope of the invention; in the ken that one skilled in the relevant art possesses, can also under the prerequisite that does not depart from aim of the present invention, make various variations.
Claims (6)
1. a method of preparing high-purity α phase silicon nitride powder to reclaim filings obtained through silicon wafer cutting, it is characterized in that, in protective atmosphere, silicon chip sawdust powder is carried out to high-temperature ammonolysis, in employing nitrogen, nitrogen and hydrogen mixture, ammonia, one or more mixed gass are as protective atmosphere, the assist gas of argon gas during as nitrogenize, the highest nitriding temperature is 1250 ℃ ~ 1380 ℃, and in nitridation process, soaking time is determined according to the consumption of raw material; Then use milling equipment to carry out grinding to nitrogenize product, adopt afterwards mineral acid to the pickling of grinding gained silicon nitride powder, washing afterwards, final drying obtains high-purity α phase silicon nitride powder.
2. a kind of method of preparing high-purity α phase silicon nitride powder to reclaim filings obtained through silicon wafer cutting according to claim 1, it is characterized in that described silicon chip sawdust powder is the sawdust waste material by the Silicon Wafer cutting of polysilicon and the industry use of monocrystaline silicon solar cell Pian, electronic semi-conductor is produced, comprise band sawdust, abrasive dust, diamond wire sawdust, and silane thermal decomposition process is produced the superfine silica powder producing in polysilicon process and is carried out conventional pickling, washing, stoving process and reclaim to purify and obtain.
3. a kind of method of preparing high-purity α phase silicon nitride powder to reclaim filings obtained through silicon wafer cutting according to claim 1, is characterized in that the volume fraction of described argon gas is 0% ~ 80%, is preferably 10% ~ 60%.
4. a kind of method of preparing high-purity α phase silicon nitride powder to reclaim filings obtained through silicon wafer cutting according to claim 3, is characterized in that the volume fraction of hydrogen in described nitrogen and hydrogen mixture is 0% ~ 50%, is preferably 5% ~ 15%.
5. a kind of method of preparing high-purity α phase silicon nitride powder to reclaim filings obtained through silicon wafer cutting according to claim 1, is characterized in that described mineral acid is HCl, HF, HNO
3, H
2sO
4in one or more mixing.
6. a kind of method of preparing high-purity α phase silicon nitride powder to reclaim filings obtained through silicon wafer cutting according to claim 1, is characterized in that nitriding temperature minute two ends or multistage carry out, and being preferably first stage temperature is 600 ℃ ~ 900 ℃, with 5 ℃ ~ 10 ℃ intensifications of per minute; With 1 ℃ ~ 5 ℃ speed of per minute, heat up subsequently, top temperature is 1250 ℃ ~ 1380 ℃.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107365156A (en) * | 2017-07-19 | 2017-11-21 | 北京科技大学 | A kind of method that silicon nitride is prepared using diamond wire saw polycrystalline silicon wastes |
| CN107758634A (en) * | 2016-08-16 | 2018-03-06 | 上海纳晶科技有限公司 | A kind of method based on the clay standby high-purity α phase silicon nitride powders of silicon caused by crystal silicon solar batteries |
| CN108947539A (en) * | 2018-09-11 | 2018-12-07 | 中国科学院上海硅酸盐研究所 | A kind of silicon nitride ceramic material and preparation method thereof for mobile phone backboard |
| CN109179347A (en) * | 2018-09-28 | 2019-01-11 | 镇江环太硅科技有限公司 | A kind of method of silicon nitride powder recycling and reusing |
| CN109265172A (en) * | 2018-08-30 | 2019-01-25 | 济宁泉达实业有限责任公司 | A kind of high-performance Si3N4In conjunction with SiC ceramic honey comb and preparation method thereof |
| CN110357051A (en) * | 2019-07-09 | 2019-10-22 | 南昌大学 | A kind of preparation method of monocrystalline α phase silicon nitride nano whisker |
| CN110357050A (en) * | 2019-07-03 | 2019-10-22 | 南昌大学 | The shaft-like beta phase silicon nitride raw powder's production technology such as a kind of |
| CN112408992A (en) * | 2020-12-11 | 2021-02-26 | 安阳亨利高科实业有限公司 | Production method of high alpha-phase silicon nitride powder |
| CN114790107A (en) * | 2022-04-29 | 2022-07-26 | 江苏大学 | Preparation of SiO by utilizing polycrystalline silicon cutting waste at low temperature 2 -Si 3 N 4 Method for compounding ceramic |
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| CN107758634A (en) * | 2016-08-16 | 2018-03-06 | 上海纳晶科技有限公司 | A kind of method based on the clay standby high-purity α phase silicon nitride powders of silicon caused by crystal silicon solar batteries |
| CN107365156A (en) * | 2017-07-19 | 2017-11-21 | 北京科技大学 | A kind of method that silicon nitride is prepared using diamond wire saw polycrystalline silicon wastes |
| CN109265172A (en) * | 2018-08-30 | 2019-01-25 | 济宁泉达实业有限责任公司 | A kind of high-performance Si3N4In conjunction with SiC ceramic honey comb and preparation method thereof |
| CN108947539A (en) * | 2018-09-11 | 2018-12-07 | 中国科学院上海硅酸盐研究所 | A kind of silicon nitride ceramic material and preparation method thereof for mobile phone backboard |
| CN108947539B (en) * | 2018-09-11 | 2021-05-25 | 中国科学院上海硅酸盐研究所 | Silicon nitride ceramic material for mobile phone back plate and preparation method thereof |
| CN109179347A (en) * | 2018-09-28 | 2019-01-11 | 镇江环太硅科技有限公司 | A kind of method of silicon nitride powder recycling and reusing |
| CN110357050A (en) * | 2019-07-03 | 2019-10-22 | 南昌大学 | The shaft-like beta phase silicon nitride raw powder's production technology such as a kind of |
| CN110357051A (en) * | 2019-07-09 | 2019-10-22 | 南昌大学 | A kind of preparation method of monocrystalline α phase silicon nitride nano whisker |
| CN110357051B (en) * | 2019-07-09 | 2023-03-14 | 南昌大学 | Preparation method of single crystal alpha-phase silicon nitride nanowhiskers |
| CN112408992A (en) * | 2020-12-11 | 2021-02-26 | 安阳亨利高科实业有限公司 | Production method of high alpha-phase silicon nitride powder |
| CN112408992B (en) * | 2020-12-11 | 2022-08-02 | 安阳亨利高科实业有限公司 | Production method of high alpha-phase silicon nitride powder |
| CN114790107A (en) * | 2022-04-29 | 2022-07-26 | 江苏大学 | Preparation of SiO by utilizing polycrystalline silicon cutting waste at low temperature 2 -Si 3 N 4 Method for compounding ceramic |
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Application publication date: 20140205 |