CN114655959A - High-purity micro-nano silicon powder purified by silicon cutting waste in photovoltaic industry and purification method and application thereof - Google Patents
High-purity micro-nano silicon powder purified by silicon cutting waste in photovoltaic industry and purification method and application thereof Download PDFInfo
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- CN114655959A CN114655959A CN202210466081.9A CN202210466081A CN114655959A CN 114655959 A CN114655959 A CN 114655959A CN 202210466081 A CN202210466081 A CN 202210466081A CN 114655959 A CN114655959 A CN 114655959A
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Abstract
The invention discloses high-purity micro-nano silicon powder purified by photovoltaic industry cut silicon waste, and a purification method and application thereof. The purification method is simple and efficient, reduces the manufacturing cost compared with the micro-nano silicon powder obtained by commercial silicon powder, and can achieve the economic benefit of recycling solid wastes. The purified micro-nano silicon powder has no other impurities, has higher purity, and has great application prospect in a plurality of fields such as silicon-based semiconductor materials, silicon-based cathode battery materials, silicon nitride ceramic materials, silicon carbide ceramic materials, nitrogen magnesium silicide heat conduction materials, magnesium silicide and manganese silicide thermoelectric materials and the like.
Description
Technical Field
The invention belongs to the technical field of solid waste recycling, and particularly relates to high-purity micro-nano silicon powder purified by silicon cutting waste in the photovoltaic industry, and a purification method and application thereof.
Background
The cutting of silicon wafers in the photovoltaic industry is mainly a diamond wire cutting technology, a large amount of silicon waste materials are generated every year in the process, and the stacking of the silicon waste materials not only causes serious resource waste and environmental pollution, but also causes safety accidents such as spontaneous combustion and the like, so that the high-added-value resource utilization of the photovoltaic waste silicon materials has important significance in the aspects of improving the resource utilization efficiency, improving the environmental quality, promoting the comprehensive green transformation of the economic and social development and the like.
In addition, in the cutting process, a small amount of water and organic matters are used as cutting liquid, oxygen atoms in the water react with silicon atoms, so that silicon oxide is formed and remained in the silicon waste, and the organic matters also remain in the silicon waste. Therefore, the impurities in the silicon cutting waste material in the photovoltaic industry account for more than 90 percent of silicon, and the rest components mainly comprise carbon, oxygen and some trace metal elements.
Silicon in the photovoltaic silicon waste material generally has submicron (400-. The particle size of the commercial silicon powder is micron-sized and is dozens to hundreds of microns, so the micro-nano silicon powder can obtain the target particle size only by secondary processing such as mechanical crushing, ball milling and the like, and the manufacturing cost of the raw material end of the micro-nano silicon powder is improved by times.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide high-purity micro-nano silicon powder purified by silicon cutting waste in the photovoltaic industry, a purification method and application thereof, so as to solve the problem that the silicon cutting waste contains carbon, oxygen and trace metal impurities, obtain the high-purity micro-nano silicon powder and realize resource utilization of the silicon cutting waste.
In order to achieve the purpose, the invention adopts the following technical scheme to realize the purpose:
the invention discloses a method for purifying high-purity micro-nano silicon powder by cutting silicon waste in photovoltaic industry, which comprises the following steps:
the method comprises the following steps: carrying out high-temperature calcination on photovoltaic cutting silicon waste serving as a raw material to obtain high-temperature calcined silicon powder;
step two: adding silicon powder into a hydrofluoric acid solution, stirring uniformly, and standing;
step three: carrying out vacuum filtration on the silicon powder in the hydrofluoric acid to obtain the silicon powder after acid washing;
step four: and drying the acid-washed silicon powder in an argon atmosphere to obtain the high-purity micro-nano silicon powder.
Preferably, in the step one, the high-temperature calcination is carried out for 1-10h at the temperature of 600-800 ℃ under the argon atmosphere.
Preferably, in the second step, the concentration of the hydrofluoric acid solution is 1-20%, and the standing time is 1-10 h.
Preferably, in the third step, the filter paper for vacuum filtration is a filter membrane with a pore size of 0.45 μm.
Preferably, in the fourth step, the drying temperature is 120-200 ℃ under the argon atmosphere, and the drying time is 1-10 h.
The invention also discloses high-purity micro-nano silicon powder obtained by the purification method, wherein the particle size of the high-purity micro-nano silicon powder is 450-800 nm.
Preferably, the purity of the high-purity micro-nano silicon powder is 99.55%.
The invention also discloses application of the high-purity micro-nano silicon powder in preparation of silicon-based semiconductor materials, silicon-based negative electrode battery materials, silicon nitride ceramic materials, silicon carbide ceramic materials, nitrogen magnesium silicide heat conduction materials, magnesium silicide thermoelectric materials or manganese silicide thermoelectric materials.
Compared with the prior art, the invention has the following beneficial effects:
the invention discloses a method for purifying high-purity micro-nano silicon powder from photovoltaic industry cut silicon waste, which takes the photovoltaic cut silicon waste as a raw material, can volatilize polymers in the silicon waste through high-temperature calcination, can remove trace metal impurities through acid washing and drying, and reduces the carbon content and the oxygen content in the photovoltaic cut silicon waste, thereby obtaining the high-purity micro-nano silicon powder with the purity of 99.55 percent. The purification method is simple and efficient, reduces the manufacturing cost compared with the micro-nano silicon powder obtained by commercial silicon powder, and can achieve the economic benefit of recycling solid wastes.
Furthermore, the concentration of the hydrofluoric acid solution is 1-20%, the standing time is 1-10h, and silicon dioxide in the photovoltaic cutting silicon waste can be removed.
Further, drying is performed under an argon atmosphere to remove residual hydrofluoric acid.
The invention also discloses the high-purity micro-nano silicon powder purified by the silicon waste cut in the photovoltaic industry, the purified micro-nano silicon powder has no other impurities, has higher purity, has great application prospect in numerous fields such as silicon-based semiconductor materials, silicon-based negative electrode battery materials, silicon nitride ceramic materials, silicon carbide ceramic materials, nitrogen magnesium silicide heat conduction materials, magnesium silicide and manganese silicide thermoelectric materials and the like, and can greatly improve the application value and the economic value of the silicon waste.
Drawings
FIG. 1 is an XRD pattern of a silicon waste before purification and a silicon powder after purification in example 1 of the present invention;
FIG. 2 is a graph showing a distribution of particle sizes of photovoltaic cut silicon waste in example 1 of the present invention.
Detailed Description
In order to make the technical solutions of the present invention better understood, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that the terms "first," "second," and the like in the description and claims of the present invention and in the drawings described above are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It is to be understood that the data so used is interchangeable under appropriate circumstances such that the embodiments of the invention described herein are capable of operation in sequences other than those illustrated or described herein. Furthermore, the terms "comprises," "comprising," and "having," and any variations thereof, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed, but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.
The invention discloses a method for purifying high-purity micro-nano silicon powder by cutting silicon waste in photovoltaic industry, which comprises the following steps:
the method comprises the following steps: and (3) placing the ceramic boat filled with 2-5g of photovoltaic cutting silicon waste into a tube furnace, introducing high-purity argon, and calcining for 1-10h at the temperature of 600-1000 ℃ to obtain high-temperature calcined silicon powder.
Step two: putting the silicon powder obtained in the step one after high-temperature calcination into a hydrofluoric acid solution with the concentration of 1-20%, uniformly stirring on a magnetic stirrer, and standing for 1-10 h;
step three: vacuum-filtering the solution obtained in the second step to separate the silicon powder from hydrofluoric acid, wherein a filter membrane with the aperture of 0.45 mu m is selected as the filter paper to obtain the silicon powder after acid washing;
step four: and (3) putting the ceramic boat containing the silicon powder after the acid washing into a tube furnace, introducing high-purity argon, and drying at the temperature of 120 plus materials and 200 ℃ for 1-10h to remove residual hydrofluoric acid, thereby finally obtaining the purified high-purity micro-nano silicon powder.
Example 1
A method for purifying high-purity micro-nano silicon powder by cutting silicon waste in photovoltaic industry comprises the following steps:
the method comprises the following steps: and (3) putting the ceramic boat containing 2g of photovoltaic cutting silicon waste into a tube furnace, introducing high-purity argon, and calcining for 1h at 1000 ℃ to obtain high-temperature calcined silicon powder.
Step two: putting the high-purity cut silicon waste calcined at high temperature obtained in the step one into 10% hydrofluoric acid solution, uniformly stirring the mixture on a magnetic stirrer, and standing the mixture for 10 hours;
step three: vacuum-filtering the solution obtained in the second step to separate the silicon powder from hydrofluoric acid, wherein a filter membrane with the aperture of 0.45 mu m is selected as the filter paper to obtain the silicon powder after acid washing;
step four: and (3) putting the ceramic boat containing the silicon powder after the acid cleaning into a tube furnace, introducing high-purity argon, and drying at 150 ℃ for 1h to remove residual hydrofluoric acid to finally obtain the purified high-purity micro-nano silicon powder, wherein the particle size of the high-purity micro-nano silicon powder is 450-plus-800 nm.
FIG. 1 is an XRD pattern of the silicon waste before purification and the silicon powder after purification according to example 1 of the present invention, and it can be seen from the comparison of the XRD pattern with that of a standard card (PDF #78-2500) that SiO appears when the unrefined silicon waste is at about 10 degrees 2 θ2Peaks, and other impurity peaks do not appear in the purified micro-nano silicon powder, so that the purification process is proved to have an obvious effect on removing the oxygen content; FIG. 2 is a graph showing a particle size distribution of cut silicon scrap according to example 1 of the present invention, wherein the silicon scrap has a D10 value of 0.303. mu.m, a D50 value of 0.65. mu.m, and a D90 value of 1.491. mu.m.
Example 2
A method for purifying high-purity micro-nano silicon powder by cutting silicon waste in photovoltaic industry comprises the following steps:
the method comprises the following steps: and (3) putting the ceramic boat containing 2g of cut silicon waste into a tube furnace, introducing high-purity argon, and calcining for 3 hours at 800 ℃ to obtain high-temperature calcined silicon powder.
Step two: putting the silicon powder obtained in the step one after high-temperature calcination into 10% hydrofluoric acid solution, uniformly stirring the silicon powder on a magnetic stirrer, and standing for 10 hours;
step three: vacuum-filtering the solution obtained in the second step to separate the silicon powder from hydrofluoric acid, wherein a filter membrane with the aperture of 0.45 mu m is selected as the filter paper to obtain the silicon powder after acid washing;
step four: and (3) putting the ceramic boat containing the silicon powder after the acid cleaning into a tube furnace, introducing high-purity argon, and drying at 150 ℃ for 1h to remove residual hydrofluoric acid to finally obtain the purified high-purity micro-nano silicon powder, wherein the particle size of the high-purity micro-nano silicon powder is 450-plus-800 nm.
Example 3
A method for purifying high-purity micro-nano silicon powder by cutting silicon waste in photovoltaic industry comprises the following steps:
the method comprises the following steps: and (3) putting the ceramic boat containing 2g of cut silicon waste into a tube furnace, introducing high-purity argon, and calcining at 600 ℃ for 10 hours to obtain high-temperature calcined silicon powder.
Step two: putting the silicon powder obtained in the step one after high-temperature calcination into 10% hydrofluoric acid solution, uniformly stirring the silicon powder on a magnetic stirrer, and standing for 10 hours;
step three: vacuum-filtering the solution obtained in the second step to separate the silicon powder from hydrofluoric acid, wherein a filter membrane with the aperture of 0.45 mu m is selected as the filter paper to obtain the silicon powder after acid washing;
step four: and (3) putting the ceramic boat containing the silicon powder after the acid cleaning into a tube furnace, introducing high-purity argon, and drying at 150 ℃ for 1h to remove residual hydrofluoric acid to finally obtain the purified high-purity micro-nano silicon powder, wherein the particle size of the high-purity micro-nano silicon powder is 450-plus-800 nm.
Example 4
A method for purifying high-purity micro-nano silicon powder by cutting silicon waste in photovoltaic industry comprises the following steps:
the method comprises the following steps: and (3) putting the ceramic boat containing 5g of cut silicon waste into a tube furnace, introducing high-purity argon, and calcining at 600 ℃ for 10 hours to obtain high-temperature calcined silicon powder.
Step two: putting the silicon powder obtained in the step one after high-temperature calcination into a hydrofluoric acid solution with the concentration of 5%, uniformly stirring on a magnetic stirrer, and standing for 10 hours;
step three: vacuum-filtering the solution obtained in the second step to separate the silicon powder from hydrofluoric acid, wherein a filter membrane with the aperture of 0.45 mu m is selected as the filter paper to obtain the silicon powder after acid washing;
step four: and (3) putting the ceramic boat containing the silicon powder after the acid cleaning into a tube furnace, introducing high-purity argon, and drying at 120 ℃ for 10 hours to remove residual hydrofluoric acid to finally obtain the purified high-purity micro-nano silicon powder, wherein the particle size of the high-purity micro-nano silicon powder is 450-plus-800 nm.
Example 5
A method for purifying high-purity micro-nano silicon powder by cutting silicon waste in photovoltaic industry comprises the following steps:
the method comprises the following steps: and (3) putting the ceramic boat containing 4g of cut silicon waste into a tube furnace, introducing high-purity argon, and calcining for 1h at 1000 ℃ to obtain high-temperature calcined silicon powder.
Step two: putting the silicon powder obtained in the step one after high-temperature calcination into a hydrofluoric acid solution with the concentration of 5%, uniformly stirring on a magnetic stirrer, and standing for 5 hours;
step three: vacuum-filtering the solution obtained in the second step to separate the silicon powder from hydrofluoric acid, wherein a filter membrane with the aperture of 0.45 mu m is selected as the filter paper to obtain the silicon powder after acid washing;
step four: and (3) putting the ceramic boat containing the silicon powder after the acid cleaning into a tube furnace, introducing high-purity argon, and drying at 200 ℃ for 1h to remove residual hydrofluoric acid to finally obtain the purified high-purity micro-nano silicon powder, wherein the particle size of the high-purity micro-nano silicon powder is 450-plus-800 nm.
The change of the carbon content of the photovoltaic cutting silicon waste material at different calcination temperatures is shown in table 1, and it can be known from table 1 that the higher the calcination temperature is, the smaller the carbon content in the photovoltaic cutting silicon waste material is, and finally the carbon content can be reduced to about 0.1% after calcination for 1 hour at 1000 ℃; the change of the oxygen content at different hydrofluoric acid concentrations is shown in table 2, and it can be seen from table 2 that the hydrofluoric acid concentration reaches the expected effect at 10%, the oxygen content is less, and the oxygen removing effect is obvious.
Table 1 variation of carbon content of photovoltaic cut silicon waste at different calcination temperatures
TABLE 2 variation of oxygen content of photovoltaic cut silicon waste at different hydrofluoric acid concentrations
The above-mentioned contents are only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited thereby, and any modification made on the basis of the technical idea of the present invention falls within the protection scope of the claims of the present invention.
Claims (8)
1. A method for purifying high-purity micro-nano silicon powder by cutting silicon waste in photovoltaic industry is characterized by comprising the following steps:
the method comprises the following steps: carrying out high-temperature calcination on photovoltaic cutting silicon waste serving as a raw material to obtain high-temperature calcined silicon powder;
step two: adding silicon powder into a hydrofluoric acid solution, stirring uniformly, and standing;
step three: carrying out vacuum filtration on the silicon powder in the hydrofluoric acid to obtain the silicon powder after acid washing;
step four: and drying the acid-washed silicon powder in an argon atmosphere to obtain the high-purity micro-nano silicon powder.
2. The method for purifying high-purity micro-nano silicon powder from silicon cutting waste in the photovoltaic industry as claimed in claim 1, wherein in the step one, the high-temperature calcination is carried out at 600-800 ℃ for 1-10h under argon atmosphere.
3. The method for purifying high-purity micro-nano silicon powder from silicon cutting waste in photovoltaic industry as claimed in claim 1, wherein in the second step, the concentration of the hydrofluoric acid solution is 1-20%, and the standing time is 1-10 h.
4. The method for purifying high-purity micro-nano silicon powder from silicon cutting waste in the photovoltaic industry as claimed in claim 1, wherein in the third step, the filter paper for vacuum filtration is a filter membrane with a pore size of 0.45 μm.
5. The method for purifying high-purity micro-nano silicon powder from silicon cutting waste in photovoltaic industry as claimed in claim 1, wherein in the fourth step, the drying temperature is 120-.
6. The high-purity micro-nano silicon powder obtained by the method of any one of claims 1 to 5, wherein the particle size of the high-purity micro-nano silicon powder is 450-800 nm.
7. The high-purity micro-nano silicon powder as claimed in claim 6, wherein the purity of the high-purity micro-nano silicon powder is 99.55%.
8. The application of the high-purity micro-nano silicon powder disclosed by claim 6 or 7 in preparation of silicon-based semiconductor materials, silicon-based negative electrode battery materials, silicon nitride ceramic materials, silicon carbide ceramic materials, nitrogen magnesium silicide heat conduction materials, magnesium silicide thermoelectric materials or manganese silicide thermoelectric materials.
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| CN115863555A (en) * | 2022-09-09 | 2023-03-28 | 滁州学院 | Preparation method of lithium ion battery negative electrode material |
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