CN102515555B - Quartz crucible surface processing method - Google Patents
Quartz crucible surface processing method Download PDFInfo
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- CN102515555B CN102515555B CN201110387727.6A CN201110387727A CN102515555B CN 102515555 B CN102515555 B CN 102515555B CN 201110387727 A CN201110387727 A CN 201110387727A CN 102515555 B CN102515555 B CN 102515555B
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Abstract
The invention discloses a quartz crucible surface processing method, which is characterized by comprising the steps of washing a quartz crucible by using tap water, soaking the quartz crucible by using mixing liquid, showering the quartz crucible by using deionized water, soaking the quartz crucible by using the deionized water, and showering quartz crucible by the deionized water and drying the quartz crucible. The mixing liquid used in a mixing liquid soaking step is mixed by salt with fluorine, muriatic acid and peralcohol, mass concentration of the salt with the fluorine, the muriatic acid and the peralcohol is respectively 0.1-99.99%, volume ratio of the three reagents is (1-99):(1-99):(1-99), soaking time is 50-100 minutes, and the temperature of the mixing liquid is 50-80 DEG C. The quartz crucible surface processing method has the advantages that the quartz crucible surface processing method is used for surface processing of the quartz crucible, content of metal impurities on the surface of the quartz crucible can finally reduce by 1-2 quantity levels, bubble concentration within the thickness of 0-150mum on the inner surface of the quartz crucible is reduced, and micro particles on the surface of the quartz crucible can be removed simultaneously.
Description
Technical field
The present invention relates to a kind of quartz crucible surface-treated method for growing single-crystal silicon that photovoltaic industry and semi-conductor industry are used.
Background technology
Day by day closing on of energy dilemma and becoming increasingly conspicuous of environmental problem, make to develop new forms of energy extremely urgent.Sun power reserves are almost unlimited, and ubiquity, can clean utilization, and be comparatively desirable renewable substitute energy.According to the prediction of European JRC, to solar energy power generating in 2030, in the supply of world's total electricity, reach more than 10%; Within 2040, this ratio will reach more than 20%; To 21 end of the centurys, solar electrical energy generation accounts for more than 60%.Therefore, solar energy power generating demonstrates important strategic position.
Silicon single crystal is as the parent material of manufacturing solar-energy photo-voltaic cell, conventionally by Czochralski(Cz) legal system is standby.Be about to melt in quartz crucible that polysilicon packs sidewall outside surface having heaters into, crystal seed contact with the silicon of fusing, through crystal puller extraction and the formation silicon single crystal ingot of growing.
Quartz crucible for pulling monocrystal silicon generally adopts arc process to make at present, in preparation process, understand due to the fusing of quartz sand generating portion gas, and some impurity at high temperature gasify, these gases can be present in inner surface of crucible with the beyond all recognition micron-sized bubble of naked eyes.Also have in preparation process quartz crucible surface to be inevitably subject to the pollution of harmful elements such as metal, basic metal and some microparticles.
In crystal pulling process; quartz crucible will stand to reach at argon gas the continuous high temperature of a few hours or tens of hours in the environment for protection gas; its inwall is also exposed in high temperature silicon melt simultaneously; above-mentionedly at the beyond all recognition micro-bubble of inner surface of crucible naked eyes, can grow up and merge with 5-10 volume doubly, gradually become visible and quantification.The combination of bubble often causes quartz crucible inner surface to break and the bubble interior metal oxide compound that discharges, thereby these escaping gas can cause the change of crystalline structure to form lattice imperfection; Breaking of bubble may cause collapsing of crucible, also quartz particles can be advanced in silicon melt, damages single crystal structure.The surface of quartz crucible exists above-mentioned pollutent on the other hand, in crystal pulling process, will in silicon crystal, spread, and having a strong impact on that crystal forming rate causes cannot crystal pulling.
Chinese patent 02154513.8(application number) provide a kind of crucible surface to have containing the surfaction quartz glass crucibles of the Clear coating of crystallization promotor and the method for modifying of crucible surface.On surface of quartz glass crucible, the mixed solution of the partial hydrolystate that coating contains metal-salt and alcoxyl silane low polymer, burn till, obtain surface and there is the crystallization promotor being formed by metal oxide or metal carbonate and be dispersed in quartz glass crucibles Clear coating, that pulling monocrystal is used in siliceous matrix.
Chinese patent 03108420.6(application number) disclose a kind of quartz glass crucibles of surface modification and for making the method for crucible modification, be included in the inner side all or in part of crucible and/or the metal oxide layer on outer surface, and it is cured.At least the internal surface of crucible is coated with the metal oxide of described magnesium, calcium, strontium or barium.The coating of crucible is not easy to wear and the high dislocation-free ratio of the silicon single crystal being drawn into crucible can be provided.
Chinese patent 201010271031.2(application number) provide a kind of preparation method of silicon nitride coating quartz crucible, comprise ceramic size preparation, applying coating, dry and firing process.Coating need be dried at the temperature of 80-100 ℃, then at the temperature nitrogen atmosphere of 1140 ℃-1300 ℃, fires and within 6-8 hour, makes silicon nitride coating quartz crucible.
In sum, the treatment process on quartz crucible surface is mainly modified as master with coating on inner surface at present, still needs a kind of purging method of crucible, to guarantee the cleanliness factor of the surfaces externally and internally of crucible, meets the preparation before the direct use of crucible or coating.
Summary of the invention
The object of the invention is: a kind of reduction quartz crucible metallic contaminants from surface content is provided, reduces inner surface of crucible bubble concentration, also can remove the treatment process of the microparticle on quartz crucible surface simultaneously.
For achieving the above object, the technical solution used in the present invention is:
A quartz crucible surface processing method, comprises the steps,
(1), rinse quartz crucible
Quartz crucible after sandblast cutting is rinsed with tap water, and after rinsing, back-off drenches surperficial water droplet on the top of the shelf;
(2), mixed liquid dipping quartz crucible
Quartz crucible after rinsing is placed in to special-purpose quartz crucible basket, then putting into together mixed solution soaks, described mixed solution is by being with villiaumite, hydrochloric acid and peralcohol mix, band villiaumite, the mass concentration of hydrochloric acid and peralcohol is respectively 0.1-99.99%, the volume ratio of three kinds of reagent is (1-99): (1-99): (1-99), mixed solution is placed in special-purpose tank, water circulating pump in tank, is equipped with, allow mixed solution circulate in tank, guarantee that mixing solutions fully reacts with quartz crucible surface in immersion process, soak time is 50-100min, the temperature of mixed solution: 50～80 ℃,
(3), quartz crucible after mixed liquid dipping is taken out, with resistance, be that after the deionized water of 15～21M Ω * cm rinses quartz crucible surface and crucible basket, putting into resistance is the deionization pond continuation immersion of 15～21M Ω * cm, soak time is 10-30min;
(4) on special-purpose cleaning machine for quartz crucible, with resistance, be, quartz crucible after deionized water soaks is taken out, the deionized water drip washing of 15～21M Ω * cm;
(5), the crucible after drip washing is put into the clean shed with heating unit, after 3-6 minute, quartz crucible is dried, so far, the process of surface treatment of quartz crucible finishes, and enters lower road packaging process.
Further, in step (2), the band villiaumite in described mixed solution is hydrogen fluoride amine, and the peralcohol in mixed solution is hydrogen peroxide, and the mass concentration of hydrogen fluoride amine, hydrochloric acid and hydrogen peroxide is respectively 12%～30%, 10%～30%, 1%～20%.
Advantage of the present invention is: quartz crucible surface processing method of the present invention, quartz crucible is carried out to surface treatment, the metallic contaminants from surface content of final quartz crucible can reduce 1-2 the order of magnitude, reduce the bubble concentration in inner surface of crucible 0-150 μ m thickness, also can remove the microparticle on quartz crucible surface simultaneously.
Accompanying drawing explanation
Below in conjunction with the drawings and specific embodiments, the present invention is described in further detail.
Fig. 1 is crucible surface processing flow chart of the present invention.
Embodiment
Embodiment 1
A kind of quartz crucible surface processing method, comprise the steps: the quartz crucible after sandblast cutting to rinse with tap water, after rinsing, back-off drenches surperficial water droplet on the top of the shelf, quartz crucible after rinsing is placed in to special-purpose quartz crucible basket, then putting into together mixed solution soaks, mixed solution is by hydrogen fluoride amine, hydrochloric acid and hydrogen peroxide mix, the mass concentration of hydrogen fluoride amine is 12%, the mass concentration of hydrochloric acid is 10%, the mass concentration of hydrogen peroxide is 1%, three's volume ratio is 1:3:6, the temperature of mixed solution is 50 ℃, ON cycle water pump, after soaking 95min, take out, the deionized water that with resistance is 15M Ω * cm will be put into 1# deionization pond after quartz crucible surface and the flushing of crucible basket, after 10 minutes, take out, with deionized water, rinsed one time again, put into 2# deionization pond, soak after 10 minutes and take out, on special-purpose cleaning machine for quartz crucible, use deionized water drip washing, last back-off is positioned in the clean shed that is equipped with infrared heating pipe on shelf, after 3 minutes, quartz crucible is continued to heated baking conversely, the surfaces externally and internally complete drying of crucible after 3 minutes, etc. to be packaged.
Embodiment 2.
A kind of quartz crucible surface processing method, comprise the steps: the quartz crucible after sandblast cutting to rinse with tap water, after rinsing, back-off drenches surperficial water droplet on the top of the shelf, quartz crucible after rinsing is placed in to special-purpose quartz crucible basket, then putting into together mixed solution soaks, mixed solution is by hydrogen fluoride amine, hydrochloric acid and hydrogen peroxide mix, the mass concentration of hydrogen fluoride amine is 20%, the mass concentration of hydrochloric acid is 15%, the mass concentration of hydrogen peroxide is 10%, three's volume ratio is 2:3:5, the temperature of mixed solution is 65 ℃, ON cycle water pump, after soaking 80min, take out, the deionized water that with resistance is 18M Ω * cm will be put into 1# deionization pond after quartz crucible surface and the flushing of crucible basket, after 15 minutes, take out, with deionized water, rinsed one time again, put into 2# deionization pond, soak after 15 minutes and take out, on special-purpose cleaning machine for quartz crucible, use deionized water drip washing, last back-off is positioned in the clean shed that is equipped with infrared heating pipe on shelf, after 2 minutes, quartz crucible is continued to heated baking conversely, the surfaces externally and internally complete drying of crucible after 3 minutes, etc. to be packaged.
Embodiment 3
A kind of quartz crucible surface processing method, comprise the steps: the quartz crucible after sandblast cutting to rinse with tap water, after rinsing, back-off drenches surperficial water droplet on the top of the shelf, quartz crucible after rinsing is placed in to special-purpose quartz crucible basket, then putting into together mixed solution soaks, mixed solution is by hydrogen fluoride amine, hydrochloric acid and hydrogen peroxide mix, the mass concentration of hydrogen fluoride amine is 25%, the mass concentration of hydrochloric acid is 25%, the mass concentration of hydrogen peroxide is 15%, three's volume ratio is 1:4:5, the temperature of mixed solution is 80 ℃, ON cycle water pump, after soaking 60min, take out, the deionized water that with resistance is 21M Ω * cm will be put into 1# deionization pond after quartz crucible surface and the flushing of crucible basket, after 18 minutes, take out, with deionized water, rinsed one time again, put into 2# deionization pond, soak after 15 minutes and take out, on special-purpose cleaning machine for quartz crucible, use deionized water drip washing, last back-off is positioned in the clean shed that is equipped with infrared heating pipe on shelf, after 3 minutes, quartz crucible is continued to heated baking conversely, the surfaces externally and internally complete drying of crucible after 3 minutes, etc. to be packaged.
Embodiment 4
A kind of quartz crucible surface processing method, comprise the steps: the quartz crucible after sandblast cutting to rinse with tap water, after rinsing, back-off drenches surperficial water droplet on the top of the shelf, quartz crucible after rinsing is placed in to special-purpose quartz crucible basket, then putting into together mixed solution soaks, mixed solution is by hydrogen fluoride amine, hydrochloric acid and hydrogen peroxide mix, the mass concentration of hydrogen fluoride amine is 30%, the mass concentration of hydrochloric acid is 30%, the mass concentration of hydrogen peroxide is 20%, three's volume ratio is 3:5:2, the temperature of mixed solution is 80 ℃, ON cycle water pump, after soaking 50min, take out, the deionized water that with resistance is 21M Ω * cm will be put into 1# deionization pond after quartz crucible surface and the flushing of crucible basket, after 18 minutes, take out, with deionized water, rinsed one time again, put into 2# deionization pond, soak after 15 minutes and take out, on special-purpose cleaning machine for quartz crucible, use deionized water drip washing, last back-off is positioned in the clean shed that is equipped with infrared heating pipe on shelf, after 3 minutes, quartz crucible is continued to heated baking conversely, the surfaces externally and internally complete drying of crucible after 2 minutes, etc. to be packaged.
Although with reference to preferred embodiment, invention has been described, one skilled in the art should appreciate that without departing from the scope of the invention, can make various changes and can replace on an equal basis its key element according to practical situation.The invention is not restricted to as the published specific embodiments of implementing best way of the present invention, but all embodiments in the scope that comprises claims.
Claims (1)
1. a quartz crucible surface processing method, is characterized in that: comprises the steps,
(1), rinse quartz crucible
Quartz crucible after sandblast cutting is rinsed with tap water, and after rinsing, back-off drenches surperficial water droplet on the top of the shelf;
(2), mixed liquid dipping quartz crucible
Quartz crucible after rinsing is placed in to special-purpose quartz crucible basket, then putting into together mixed solution soaks, described mixed solution is by being with villiaumite, hydrochloric acid and peralcohol mix, band villiaumite in described mixed solution is hydrogen fluoride amine, peralcohol in mixed solution is hydrogen peroxide, hydrogen fluoride amine, the mass concentration of hydrochloric acid and hydrogen peroxide is respectively 12%～30%, 10%～30%, 1%～20%, the volume ratio of three kinds of reagent is 1:3:6, 2:3:5, 1:4:5 or 3:5:2, mixed solution is placed in special-purpose tank, water circulating pump in tank, is equipped with, allow mixed solution circulate in tank, guarantee that mixing solutions fully reacts with quartz crucible surface in immersion process, soak time is 50-100min, the temperature of mixed solution: 50～80 ℃,
(3), quartz crucible after mixed liquid dipping is taken out, with resistance, be that after the deionized water of 15～21M Ω * cm rinses quartz crucible surface and crucible basket, putting into resistance is the deionization pond continuation immersion of 15～21M Ω * cm, soak time is 10-30min;
(4) on special-purpose cleaning machine for quartz crucible, with resistance, be, quartz crucible after deionized water soaks is taken out, the deionized water drip washing of 15～21M Ω * cm;
(5), the crucible after drip washing is put into the clean shed with heating unit, after 3-6 minute, quartz crucible is dried, so far, the process of surface treatment of quartz crucible finishes, and enters lower road packaging process.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201110387727.6A CN102515555B (en) | 2011-11-30 | 2011-11-30 | Quartz crucible surface processing method |
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| CN201110387727.6A CN102515555B (en) | 2011-11-30 | 2011-11-30 | Quartz crucible surface processing method |
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| CN102515555A CN102515555A (en) | 2012-06-27 |
| CN102515555B true CN102515555B (en) | 2014-04-02 |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103011611B (en) * | 2012-12-24 | 2017-03-15 | 上海申和热磁电子有限公司 | A kind of surface treatment method of quasiconductor quartz |
| CN105177708A (en) * | 2015-07-27 | 2015-12-23 | 奥特斯维能源（太仓）有限公司 | Purification method for crucible used for polycrystalline cast ingot |
| CN111390770A (en) * | 2020-04-08 | 2020-07-10 | 四川富乐德科技发展有限公司 | Cleaning method for O L ED evaporation equipment tantalum crucible surface material residues |
| CN111482423A (en) * | 2020-04-08 | 2020-08-04 | 四川富乐德科技发展有限公司 | Cleaning regeneration method of titanium crucible |
| CN115108841A (en) * | 2021-03-23 | 2022-09-27 | 新沂市中鑫光电科技有限公司 | Heat treatment method for high-strength quartz crucible |
| CN114349358B (en) * | 2021-12-24 | 2023-03-24 | 连云港福典石英科技有限公司 | Surface treatment process and processing equipment for quartz crucible |
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| JP2009289960A (en) * | 2008-05-29 | 2009-12-10 | Tokyo Electron Ltd | Method and system for cleaning quartz member |
| KR20100007461A (en) * | 2008-07-14 | 2010-01-22 | 삼성전자주식회사 | Cleaning solution for quartz part and method of cleaning using the same |
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