CN111115634A - Method for preparing SiC fibers by using silicon wafer cutting waste - Google Patents

Method for preparing SiC fibers by using silicon wafer cutting waste Download PDF

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CN111115634A
CN111115634A CN202010054241.XA CN202010054241A CN111115634A CN 111115634 A CN111115634 A CN 111115634A CN 202010054241 A CN202010054241 A CN 202010054241A CN 111115634 A CN111115634 A CN 111115634A
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waste
silicon
sic
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alumina
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CN111115634B (en
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李翔
李振强
吉恒松
唐凯
张广清
张梅
夏燏杰
彭海涛
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Jiangsu University
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    • 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
    • C01B32/963—Preparation from compounds containing silicon
    • C01B32/97—Preparation from SiO or SiO2
    • C—CHEMISTRY; METALLURGY
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    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
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    • C01B32/914—Carbides of single elements
    • C01B32/956—Silicon carbide
    • C01B32/963—Preparation from compounds containing silicon
    • C01B32/984—Preparation from elemental silicon
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    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
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    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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Abstract

The invention provides a method for preparing SiC fibers by using silicon chip waste, which comprises the steps of firstly removing organic matters in the silicon chip waste through alcohol washing and water washing, then mixing with commercially available quartz powder, generating gas-phase SiO in a high-temperature reactor, and introducing CH4Reacting to generate SiC fibers; followed by high temperature, H2Roasting in the atmosphere to remove the surplus free carbon in the fiber; and cooling and collecting the high-quality SiC fibers with low carbon content. The raw materials used by the method are diamond wire cutting silicon chip waste materials in the photovoltaic industry, have wide sources and low price, and do not contain toxic and harmful substances; the preparation method of the high-quality SiC fiber is provided while the problem of recycling of the waste materials of the diamond wire-electrode cutting silicon wafer is solved, and the recycling of solid waste resources is developed towards the direction of green, high efficiency and high yield.

Description

Method for preparing SiC fibers by using silicon wafer cutting waste
Technical Field
The invention relates to the technical field of semiconductor material preparation, in particular to a preparation method of a SiC fiber material, and especially relates to a method for preparing SiC fibers by using silicon wafer cutting waste.
Background
When a crystalline silicon solar cell is manufactured, a multi-wire cutting technology must be adopted to cut a polycrystalline silicon ingot or a single crystal silicon rod into silicon wafers. Because the diameter of the cutting line is very close to the thickness of the silicon wafer, at least more than 40% of the crystal silicon is cut into silicon powder to enter the cutting liquid, and the crystal silicon is basically in an idle or low-value utilization state. The waste materials generated by the diamond wire cutting technology which is the mainstream in the industry at present comprise Si, a small amount of C and metal impurities. In recent years, researchers at home and abroad have conducted researches on recycling high-purity silicon in waste materials, but the recycling process is complicated, and the purity of the recycled silicon powder cannot meet the requirements of producing photovoltaic-grade silicon ingots, for example, patent application publication No. CN102642835A, "a method for recycling silicon materials from waste materials generated by cutting crystalline silicon by diamond wires". The problems of low added value and the like exist in the preparation of SiC powder or refractory materials from crystalline silicon cutting waste materials, for example, patent application with publication number CN107651690B, "a method for preparing high-quality silicon carbide from diamond wire cutting waste materials", and journal article "preparation of Si from solar grade polycrystalline silicon cutting waste materials3N4-SiC composite refractory material, 2017,51(5):390-393. Therefore, a high value-added utilization way of the crystal silicon cutting waste is found, and the problem which needs to be solved urgently by the photovoltaic industry is solved.
The SiC fiber is a ceramic fiber having carbon and silicon as main components, and is morphologically divided into a whisker and a continuous fiber. The SiC fiber has good high-temperature performance, high strength, high modulus and chemical stability, the tensile strength can reach 2.5-3.5 GPa, the elastic modulus is 200GPa, the fiber has good chemical corrosion resistance, the linear expansion coefficient is small and is about 3.1 multiplied by 10-6K-1It has good radiation resistance and wave absorption, and has semiconductor properties. The composite material is mainly used for reinforcing metal and ceramic to prepare high-temperature-resistant metal or ceramic matrix composite materials. Because of its good performance, it has been used in advanced technological fields, such as aerospace, rocket engines, nuclear fusion furnaces, etcThe aspect is expanded to be applied. In addition, with the development of preparation technology, the application of SiC fibers is gradually expanded to the civil industries of high-grade sports equipment, automobile waste flue gas dust collection and the like.
The SiC fiber preparation method comprises a chemical vapor deposition method (for example, the patent application with the application number of CN201810086069.9, namely 'a silicon carbide nanowire aerogel and a preparation method thereof'), a precursor conversion method (tomming, mysterious chrysanthemum, lanine, and the like; research on preparation of silicon carbide fiber by blending solid/liquid polycarbosilane; functional materials, 2012,43(16): 2267-; ultra-fine powder extrusion spinning (Qihaipeng, Chengmei, Xiweijie, SiC/SiC CMC research and application, aeronautical manufacturing technology, 2015(4):94-97.) and Activated Carbon Fiber conversion (K.Okada, H.Kato, K.Nakajima, Preparation of silicon Carbide Fiber from Activated Carbon Fiber and gases silicon monomer. journal of the American Ceramic Society,1994, Vol.77(6), pp.1691-1693). The methods have the defects of complex preparation process, high cost, no contribution to industrial production and the like. In addition, to further increase the use temperature of silicon carbide fibers, the free carbon content in the fibers needs to be further reduced to 2% or less.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a method for preparing SiC fibers by using silicon wafer cutting waste materials. The prepared SiC fiber has low free carbon content, wide raw material source and low cost, and does not contain toxic and harmful substances. The invention provides a novel preparation method of high-quality SiC fibers while solving the problem of recycling of waste materials of diamond wire cutting silicon wafers, and develops solid waste resources towards the direction of greenness, high efficiency and high yield.
A method for preparing SiC fibers by using silicon chip waste is characterized by comprising the following steps:
(1) cleaning the silicon wafer cutting waste, removing organic matters in the silicon wafer cutting waste, filtering and drying to obtain clean waste silicon powder;
(2) preparing an SiO precursor: uniformly mixing waste silicon powder and quartz powder according to the mass ratio of 1:2 to obtain a SiO precursor;
(3) preparing SiC fibers: mixing SiOPlacing the precursor in an alumina crucible, loading the alumina crucible into an alumina reactor, and introducing Ar and H into the alumina reactor at normal pressure2、CH4Slowly inserting the alumina reactor into a high-temperature furnace preheated to 1550-1650 ℃ in advance, and reacting for 60-120 min in the high-temperature furnace; the silicon powder in the crucible reacts with the quartz powder to generate gaseous SiO, and the gaseous SiO is mixed with CH in the mixed gas4Reacting to generate SiC fibers;
(4) removing the surplus free carbon in the SiC fiber: the reaction gas is switched to pure H2Keeping the temperature in a high-temperature furnace at 1550-1650 ℃, and reserving free carbon and H in the SiC fiber2Reaction to form CH4Removing the surplus free carbon in the SiC fibers, reacting for 10-30 min, stopping introducing gas, and slowly lifting the alumina reactor out of the high-temperature furnace; and after the mixture is fully cooled, taking out the alumina crucible from the alumina reactor to obtain the SiC fiber with low carbon content.
Further, the mass percent of silicon contained in the silicon wafer cutting waste in the step (1) is more than or equal to 97 percent.
Further, the particle size of the fine quartz powder in the step (2) is 50-500 μm.
Further, Ar and H in the step (3)2、CH4CH in mixed gas4Content of (2 vol%), H2The content of (3) was 68 vol%, and the content of Ar was 30 vol%.
Further, the diameter of the low-carbon-content SiC fiber obtained in the step (4) is 0.3-0.6 μm, the length of the low-carbon-content SiC fiber is 50-200 μm, and the content of free carbon is less than 1.5%.
Further, the silicon wafer cutting waste is rinsed by using ethanol and deionized water in the step (1).
Firstly, removing organic matters in silicon wafer waste through alcohol washing and water washing, and mixing the organic matters with quartz powder; reacting the mixed powder in a high-temperature reactor to generate gas-phase SiO; with introduction of CH4And reacting to generate the SiC fiber. Followed by H at elevated temperature2And (3) roasting in the atmosphere, effectively removing the surplus free carbon in the fiber, and cooling to collect the high-quality SiC fiber with low carbon content. The SiC fibers prepared by the method have the diameter of 0.3-0.6 mu m and the length of 50-E200 mu m, the content of free carbon is less than 1.5 percent, the obtained SiC fiber has low carbon content, the high temperature resistance of the fiber is improved, and the performance is excellent.
The method utilizes the diamond wire cutting silicon chip waste in the photovoltaic industry to prepare the SiC fiber, has wide raw material source and low price, and does not contain toxic and harmful substances. The preparation method of the high-quality SiC fiber is provided while the problem of recycling of the diamond wire-cut silicon wafer waste is solved, the problem caused by recycling of the diamond wire-cut silicon wafer waste in the prior art is solved, and the preparation method can be widely popularized in the fields of silicon powder waste recycling and the like; the solid waste resources are developed towards the direction of green, high efficiency and high yield.
Drawings
FIG. 1 is a schematic view showing the structure of an alumina reactor used in the production method of the present invention.
Fig. 2 is an XRD diffractogram of the SiC fiber prepared in example 1.
Fig. 3 is an SEM picture of the SiC fiber prepared in example 1.
Fig. 4 is a TEM picture of the SiC fiber prepared in example 1.
Description of reference numerals:
1-crucible, 2-alumina inner tube, 3-support rod, 4-SiO precursor, 5-aluminum alloy flange, 6-air inlet tube, 7-air outlet and 8-alumina outer tube.
Detailed Description
The following detailed description of the embodiments of the present invention will be made with reference to the accompanying drawings, so as to make the technical solutions claimed in the present invention more clear and complete. The specific embodiments are examples of some, but not all embodiments of the invention, and the scope of the invention is not limited in this respect.
According to the method for preparing the SiC fibers by using the silicon wafer cutting waste, organic matters in the silicon wafer waste are removed through alcohol washing and water washing, and then the silicon wafer waste is mixed with commercially available quartz powder with the particle size of 50-500 mu m to serve as an SiO precursor. The SiO precursor generates gas phase SiO in a high-temperature reactor and is mixed with the introduced CH4Reacting to generate SiC fibers; chemical reaction formula involved in the processComprises the following steps:
Si(s)+SiO2(s)＝2SiO(g)
SiO(g)+2CH4(g)＝SiC(s)+CO(g)+4H2(g)
CH4(g)＝C(s)+2H2(g)
followed by high temperature, H2Roasting in the atmosphere to remove the surplus free carbon in the fiber; the chemical reaction formula involved in the process is as follows:
C(s)+2H2(g)＝CH4(g)
and finally, cooling and collecting the high-quality SiC fibers with low carbon content.
Example 1
(1) And taking 25g of diamond wire-electrode cutting silicon wafer waste, rinsing the silicon wafer waste for 10 minutes by using ethanol, and rinsing the silicon wafer waste for 2 times by using deionized water after suction filtration. And (3) carrying out suction filtration and drying to obtain clean waste silicon powder, wherein the element composition is shown in table 1.
TABLE 1 elemental composition of Diamond wire-cut silicon wafer scrap
Element(s) Si C O Ca Ni K Na Mg Al Fe
Content (wt%) 97.30 1.14 1.35 0.0703 0.0524 0.0085 0.0318 0.0306 0.0087 0.0054
(2) Weighing 3 g of the waste silicon powder cleaned in the step (1), weighing 6 g of commercially available quartz powder with the particle size of 50-500 microns, and uniformly mixing to obtain the SiO precursor.
(3) Pouring the SiO precursor 4 obtained in the step (2) into an alumina crucible 1, placing the crucible 1 in an alumina inner tube and on a support rod 3 at the bottom of the alumina inner tube 2 with openings at two ends, then inserting the alumina inner tube 3 into an alumina outer tube 8 with an opening at one end, and sealing the alumina outer tube 8 by using an aluminum alloy flange 5, wherein an air outlet 7 communicated with the inside of the alumina outer tube 8 is arranged on the aluminum alloy flange 5 as shown in fig. 1. The upper end opening of the alumina inner tube is inserted into an air inlet tube 6, and Ar and H are introduced into the alumina reactor under normal pressure2、CH4Wherein Ar is 30 vol% and H is268vol％、CH 42 vol%, and the gas flow rate was set to 2L/min. The alumina reactor was slowly inserted into a high temperature furnace preheated to 1600 ℃ and the reaction was held for 90 min.
(4) After 90min, the reaction gas was switched to pure H2The temperature of the high temperature furnace is maintained at 1600 ℃ for 20 min. Then, theThe gas feed was stopped and the alumina reactor was slowly lifted out of the high temperature furnace. After sufficient cooling, the alumina crucible was taken out from the alumina reactor to obtain SiC fibers in the crucible.
The XRD pattern of the obtained SiC fiber is shown in figure 2, which shows that the crystal form of the prepared SiC fiber is β -SiC, according to the SEM and TEM patterns shown in figures 3 and 4, the length of the prepared SiC fiber is 50-200 mu m, the diameter of the prepared SiC fiber is 0.3-0.6 mu m, the content of free carbon in the SiC fiber is averagely 1.37% when an infrared carbon-sulfur analyzer (the temperature is set to 940 ℃), the content of the free carbon in the SiC fiber is reduced to below 1.5%, and the high temperature resistance is improved.
Example 2
The procedure is as in example 1, except that the temperature of the high temperature furnace is set to 1550 ℃ under Ar, H2、CH4Maintaining in mixed gas atmosphere for 120min in pure H2The atmosphere was maintained for 30 min. The length of the prepared SiC fiber is 15-80 mu m, the diameter is 0.3-0.5 mu m, and the average content of free carbon is 1.23%.
Example 3
The procedure is as in example 1, except that the temperature in the high temperature furnace is set to 1650 ℃ under Ar or H2、CH4Keeping in mixed gas atmosphere for 60min, and keeping in pure H2The atmosphere was maintained for 10 min. The length of the prepared SiC fiber is 20-100 mu m, the diameter is 0.3-0.5 mu m, and the average content of free carbon is 1.41%.
The present invention is not limited to the above-described embodiments, and any obvious improvements, substitutions or modifications can be made by those skilled in the art without departing from the spirit of the present invention.

Claims (6)

1. A method for preparing SiC fibers by using silicon chip waste is characterized by comprising the following steps:
(1) cleaning the silicon wafer cutting waste, removing organic matters in the silicon wafer cutting waste, filtering and drying to obtain clean waste silicon powder;
(2) preparing an SiO precursor: uniformly mixing waste silicon powder and quartz powder according to the mass ratio of 1:2 to obtain a SiO precursor;
(3) preparing SiC fibers: placing the SiO precursor into an alumina crucible, loading the alumina crucible into an alumina reactor, and introducing Ar and H into the alumina reactor at normal pressure2、CH4Slowly inserting the alumina reactor into a high-temperature furnace preheated to 1550-1650 ℃ in advance, and reacting for 60-120 min in the high-temperature furnace; the silicon powder in the crucible reacts with the quartz powder to generate gaseous SiO, and the gaseous SiO is mixed with CH in the mixed gas4Reacting to generate SiC fibers;
(4) removing the surplus free carbon in the SiC fiber: the reaction gas is switched to pure H2Keeping the temperature in a high-temperature furnace at 1550-1650 ℃, and reserving free carbon and H in the SiC fiber2Reaction to form CH4Removing the surplus free carbon in the SiC fibers, reacting for 10-30 min, stopping introducing gas, and slowly lifting the alumina reactor out of the high-temperature furnace; and after the mixture is fully cooled, taking out the alumina crucible from the alumina reactor to obtain the SiC fiber with low carbon content.
2. The method of claim 1, wherein: the mass percentage of silicon contained in the silicon wafer cutting waste in the step (1) is that Si is more than or equal to 97%.
3. The method of claim 1, wherein: the particle size of the fine quartz powder in the step (2) is 50-500 μm.
4. The method of claim 1, wherein: ar and H in the step (3)2、CH4CH in mixed gas4Content of (2 vol%), H2The content of (3) was 68 vol%, and the content of Ar was 30 vol%.
5. The method of claim 1, wherein: the diameter of the low-carbon-content SiC fiber obtained in the step (4) is 0.3-0.6 mu m, the length of the low-carbon-content SiC fiber is 50-200 mu m, and the free carbon content is less than 1.5%.
6. The method of claim 1, wherein: and (2) rinsing the silicon wafer cutting waste material by using ethanol and deionized water in the step (1).
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Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101812730A (en) * 2010-04-23 2010-08-25 中南大学 Preparation method of ultralong monocrystal beta-SiC nanowire metal-free catalyst

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101812730A (en) * 2010-04-23 2010-08-25 中南大学 Preparation method of ultralong monocrystal beta-SiC nanowire metal-free catalyst

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
XIANG LI等: "Carbothermal Reduction of Quartz in Different Gas Atmospheres", 《METALLURGICAL AND MATERIALS TRANSACTIONS B》 *
XIANG LI等: "Synthesis of SiC whiskers by VLS and VS process", 《CERAMICS INTERNATIONAL》 *
王华等: "氢气气氛下SiC纤维的热稳定性", 《材料工程》 *

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