CN111115634B - Method for preparing SiC fibers by using silicon wafer cutting waste - Google Patents
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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 CH 4 Reacting to generate SiC fibers; followed by high temperature, H 2 Roasting 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 invention 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 solving the problem of recycling of the diamond wire-cutting silicon wafer waste, and the recycling of solid waste resources is developed towards the direction of green, high efficiency and high yield.
Description
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 develop the research of high-purity silicon in the recycled wasteHowever, the recovery process is complicated, and the purity of the silicon powder obtained by recovery cannot meet the requirements for producing photovoltaic-grade silicon ingots, for example, patent application No. CN102642835A, "method for recovering silicon material from waste generated by cutting crystalline silicon by diamond wire". The problems of low added value and the like in the preparation of SiC powder or refractory materials from crystalline silicon cutting waste materials are solved, for example, in the patent application with publication No. CN107651690B, "a method for preparing high-quality silicon carbide from diamond wire cutting waste materials", and journal article, "preparation of Si from solar grade polysilicon cutting waste materials 3 N 4 -SiC composite material refractory material 2017,51 (5): 390-393. Therefore, a high value-added utilization way of the crystalline silicon cutting waste is found, and the problem to be solved by the photovoltaic industry is urgently needed.
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 and small linear expansion coefficient which is about 3.1 multiplied by 10- 6 K- 1 It has good radiation resistance and wave absorption, and has semiconductor properties. The method is mainly used for reinforcing metal and ceramic to prepare high-temperature-resistant metal or ceramic matrix composite. Because of its good performance, it has been used in advanced technology fields, such as aerospace, rocket engines, nuclear fusion furnaces, etc. 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 preparation method of the SiC fiber comprises a chemical vapor deposition method (for example, a patent application with the application number of CN201810086069.9, namely 'a silicon carbide nanowire aerogel and a preparation method thereof'), a precursor conversion method (tommy, mysterious chrysanthemum, lanlin, and the like; research on preparation of the silicon carbide fiber by blending solid/liquid polycarbosilane; functional materials, 2012,43 (16): 2267-2272.); 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 transformation (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 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;
(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 pressure 2 、CH 4 Mixing the gas, slowly inserting the alumina reactor into a high-temperature furnace preheated to 1550-1650 ℃, 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 gas 4 Reacting to obtain SiC fibers;
(4) Removing the surplus free carbon in the SiC fibers: switching the reaction gas to pure H 2 Keeping the temperature in a high temperature furnace at 1550-1650 ℃, and obtaining the surplus free carbon and H in the SiC fiber 2 Reaction to form CH 4 Removing the residual free carbon in the SiC fiber, stopping introducing gas after reacting for 10-30 min, and slowly lifting out the alumina reactorA high temperature furnace; and after the mixture is fully cooled, taking the alumina crucible out of 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.
Furthermore, 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 、CH 4 CH in mixed gas 4 Content of (2 vol%), H 2 The content of (3) was 68vol%, and the content of Ar was 30vol%.
Furthermore, the diameter of the low-carbon SiC fiber obtained in the step (4) is 0.3-0.6 μm, the length is 50-200 μm, and the free carbon content is less than 1.5%.
Further, the silicon wafer cutting waste material is rinsed by 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 the introduced CH 4 And reacting to generate SiC fibers. Followed by H at elevated temperature 2 And (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 fiber prepared by the invention has the diameter of 0.3-0.6 mu m, the length of 50-200 mu m and the content of free carbon less than 1.5 percent, has low carbon content, improves the high temperature resistance of the fiber and has excellent performance.
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 of 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 image of the SiC fiber prepared in example 1.
Description of the 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 illustrative 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 CH 4 Reacting to generate SiC fibers; the chemical reaction formula involved in the process is as follows:
Si(s)+SiO2(s)＝2SiO(g)
SiO(g)+2CH 4 (g)＝SiC(s)+CO(g)+4H 2 (g)
CH 4 (g)＝C(s)+2H 2 (g)
then at high temperature, H 2 Roasting 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)+2H 2 (g)＝CH 4 (g)
and finally, cooling and collecting the high-quality SiC fibers with low carbon content.
Example 1
(1) And (3) taking 25g of diamond wire-electrode cutting silicon wafer waste, rinsing the waste for 10 minutes by using ethanol, and rinsing the 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 commercial quartz powder with the particle size of 50-500 mu m, 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. An air inlet pipe 6 is inserted into an opening at the upper end of the alumina inner pipe, and Ar and H are introduced into the alumina reactor under normal pressure 2 、CH 4 Mixed gas of (1), wherein Ar is 30vol%, and H 2 68vol％、CH 4 2vol%, 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 90min.
(4) After 90min, the reaction gas was switched to pure H 2 The temperature of the high temperature furnace is maintained at 1600 ℃ and maintained for 20min. The gas feed was then 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 beta-SiC. According to SEM images and TEM images shown in FIGS. 3 and 4, the prepared SiC fibers have a length of 50 to 200 μm and a diameter of 0.3 to 0.6. Mu.m. The free carbon content of the SiC fiber was 1.37% on average as measured by an infrared carbon sulfur analyzer (temperature set at 940 ℃). The invention reduces the content of free carbon in the SiC fiber to below 1.5 percent and improves the high temperature resistance.
Example 2
The procedure is as in example 1, except thatSetting the temperature in high temperature furnace at 1550 deg.C in Ar, H 2 、CH 4 Maintaining in mixed gas atmosphere for 120min in pure H 2 The atmosphere was maintained for 30min. The prepared SiC fiber has the length of 15-80 μm, the diameter of 0.3-0.5 μm and the average content of free carbon of 1.23 percent.
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 H 2 、CH 4 Keeping in mixed gas atmosphere for 60min, and keeping in pure H 2 The atmosphere was maintained for 10min. The prepared SiC fiber has the length of 20-100 mu m, the diameter of 0.3-0.5 mu m and the average content of free carbon of 1.41 percent.
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 (5)
1. A method for preparing SiC fibers by using silicon chip waste is characterized by comprising the following steps:
(1) Cleaning 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;
(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 pressure 2 、CH 4 Mixing the gas, slowly inserting the alumina reactor into a high-temperature furnace preheated to 1550-1650 ℃, 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 gas 4 Reacting to generate SiC fibers;
(4) Removing the surplus free carbon in the SiC fiber: switching the reaction gas to pure H 2 Keeping the temperature in a high temperature furnace at 1550-1650 ℃, and obtaining the surplus free carbon and H in the SiC fiber 2 Reaction ofGenerating CH 4 Removing the surplus free carbon in the SiC fiber, stopping introducing gas after reacting for 10-30 min, and slowly lifting the alumina reactor out of the high-temperature furnace; and after fully cooling, taking out the alumina crucible from the alumina reactor to obtain the low-carbon SiC fiber, wherein the diameter of the low-carbon SiC fiber is 0.3-0.6 mu m, the length of the low-carbon SiC fiber is 50-200 mu m, and the content of free carbon is less than 1.5%.
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 、CH 4 CH in the mixed gas 4 Content of (2 vol%), H 2 The content of (3) was 68vol%, and the content of Ar was 30vol%.
5. The method of claim 1, wherein: and (2) rinsing the silicon wafer cutting waste by using ethanol and deionized water in the step (1).
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| CN101812730A (en) * | 2010-04-23 | 2010-08-25 | 中南大学 | Preparation method of ultralong monocrystal beta-SiC nanowire metal-free catalyst |
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| 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)
| Title |
|---|
| Carbothermal Reduction of Quartz in Different Gas Atmospheres;XIANG LI等;《METALLURGICAL AND MATERIALS TRANSACTIONS B》;20150630;1343-1352 * |
| Synthesis of SiC whiskers by VLS and VS process;Xiang Li等;《Ceramics International》;20151228;2. Experimental，3.2. Carbothermal reduction in H2 atmosphere，3.3. Carbothermal reduction in CH4-H2-Ar gasmixture * |
| 氢气气氛下SiC纤维的热稳定性;王华等;《材料工程》;20091220;1实验方法 * |
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