CN102357493B - Method for cleaning drum of polycrystalline silicon reduction furnace - Google Patents
Method for cleaning drum of polycrystalline silicon reduction furnace Download PDFInfo
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- CN102357493B CN102357493B CN 201110213570 CN201110213570A CN102357493B CN 102357493 B CN102357493 B CN 102357493B CN 201110213570 CN201110213570 CN 201110213570 CN 201110213570 A CN201110213570 A CN 201110213570A CN 102357493 B CN102357493 B CN 102357493B
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- wiping
- reduction furnace
- cylinder inwall
- woven fabric
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Abstract
The invention discloses a method for cleaning a drum of a polycrystalline silicon reduction furnace. The method comprises the following steps of: (1) detaching a sight glass of the polycrystalline silicon reduction furnace; (2) flushing the inner wall of the drum of the reduction furnace by using deionized water; (3) wiping the inner wall of the drum by using a polyester non-woven fabric dipped with 5 to 10 mass percent ammonium hydrogen fluoride solution, and stagnating the solution on the inner wall for 10 to 15 minutes; (4) flushing the inner wall of the drum of the reduction furnace by using the deionized water; (5) wiping the inner wall of the drum by using the polyester non-woven fabric dipped with 2 to 4 mass percent ammonium hydrogen fluoride solution, and stagnating the solution on the inner wall for 10 to 15 minutes; (6) flushing the inner wall of the drum by using the deionized water; and drying the inner wall by using nitrogen; and (7) wiping the inner wall of the drum by using absolute ethanol, and wiping the inner wall again by using the dried polyester non-woven fabric after the ethanol is completely volatilized. The method has the advantages of simplicity, feasibility, high cleaning efficiency and the like.
Description
Technical field
The present invention relates to a kind of reduction furnace cylinder cleaning method, especially a kind of method for cleaning drum of polycrystalline silicon reduction furnace.
Background technology
" silicone oil " is a kind of silicon halide of macromolecule, and siliceous 25% is the material of oily, and this grease low temperature place in reduction process produces (being lower than 300 ℃), often is deposited on the cold wall places such as furnace wall, chassis, peep hole quartz plate.Silicone oil has strong water imbibition, thereby when tearing stove open, the moisture content in the strong absorbing air of silicone oil dissociate simultaneously hydrogen chloride and etching apparatus.So the stove cylinder must regularly clean.General cleaning method washes with giant, dries up with nitrogen again, and then the absolute ethyl alcohol wiping is used in polishing at last again.Facts have proved, owing to will polish to the furnace wall in the cleaning process, cause a large amount of heavy metals to be separated out, cause the purity of the polysilicon of processing first after the cleaning on the low side, have a strong impact on the production of polysilicon.
Summary of the invention
The technical problem to be solved in the present invention provide have simple possible, a kind of method for cleaning drum of polycrystalline silicon reduction furnace of cleaning efficiency advantages of higher.
Reduction furnace cylinder cleaning method of the present invention comprises the steps:
(1) takes the visor of polycrystalline silicon reducing furnace apart;
(2) adopt giant with deionized water the reduction furnace cylinder inwall to be washed;
(3) dipping mass fraction with terylene non-woven fabric is that the ammonium hydrogen fluoride solution of 5%-10% carries out wiping to stove cylinder inwall, allows its solution stagnate 10-15min at inwall;
(4) adopt giant with deionized water the reduction furnace cylinder inwall to be washed;
(5) again dipping mass fraction with terylene non-woven fabric is that the ammonium hydrogen fluoride solution of 2%-4% carries out wiping to stove cylinder inwall, allows its solution stagnate 10-15min at stove cylinder inwall;
(6) adopt giant to wash with deionized water stove cylinder inwall, and dry up with nitrogen;
(7) with absolute ethyl alcohol wiping stove cylinder inwall, by the time after the ethanol volatilization fully, with the again wiping one time of dry terylene non-woven fabric.
For the first time wiping stove cylinder inwall adopts the high concentration ammonium hydrogen fluoride solution, is in order to remove the impurity such as the silicone oil that is deposited on the furnace wall, dust.For the second time fluoridize the hydrogen ammonium salt solution with low concentration and clean, also cry smart scouring, guaranteed stove cylinder inwall fineness, understand some heat energy after can making in the production process heat radiation of silicon core to the furnace wall to reflect, play energy-conservation purpose.
Key is to wipe examination ammonium hydrogen fluoride solution and operating sequence and to the assurance of time in the operating process, the time oversize can etching apparatus, the time too weak point can cause cleaning dirty.
The beneficial effect that adopts technique scheme to produce is:
1. the present invention carries out the scouring first time with the high concentration ammonium hydrogen fluoride solution, removes and is deposited on the impurity such as silicone oil, dust on the furnace wall.Fluoridize the secondary that the hydrogen ammonium salt solution carries out with low concentration and clean, guarantee that stove cylinder inwall fineness is good, understand some heat energy after can making in the production process heat radiation of silicon core to the furnace wall to reflect, play energy-conservation purpose.
2. after with ammonium hydrogen fluoride solution the furnace wall being cleaned among the present invention, can avoid the stainless steel protection film to suffer to destroy and separate out iron ion without grinder buffing, guaranteed the purity of polysilicon product in the production process.
3. with terylene non-woven fabric the furnace wall is cleaned, can reduce the existence that causes furnace wall inwall measuring fiber because of wiping.
4. adopt washed with de-ionized water stove cylinder, remove residual ammonium acid fluoride, avoid ammonium acid fluoride that reduction furnace cylinder inwall is produced corrosion.
The specific embodiment
Embodiment 1
(1) takes the visor of polycrystalline silicon reducing furnace apart;
(2) adopt giant with deionized water the reduction furnace cylinder inwall to be washed;
(3) dipping mass fraction with terylene non-woven fabric is that 5% ammonium hydrogen fluoride solution carries out wiping to inwall, allows its solution stagnate 15min at inwall;
(4) adopt giant with deionized water stove cylinder inwall to be washed;
(5) again dipping mass fraction with terylene non-woven fabric is that 2% ammonium hydrogen fluoride solution carries out wiping to inwall, allows its solution stagnate 15min at inwall;
(6) adopt giant with deionized water stove cylinder inwall to be washed, and dry up with nitrogen;
(7) with absolute ethyl alcohol wiping stove cylinder inwall, by the time after the ethanol volatilization fully, with the again wiping one time of dry terylene non-woven fabric.
Embodiment 2
(1) takes the visor of polycrystalline silicon reducing furnace apart;
(2) adopt giant with deionized water the reduction furnace cylinder inwall to be washed;
(3) dipping mass fraction with terylene non-woven fabric is that 10% ammonium hydrogen fluoride solution carries out wiping to inwall, allows its solution stagnate 10min at inwall;
(4) adopt giant with deionized water stove cylinder inwall to be washed;
(5) again dipping mass fraction with terylene non-woven fabric is that 4% ammonium hydrogen fluoride solution carries out wiping to inwall, allows its solution stagnate 10min at inwall;
(6) adopt giant with deionized water stove cylinder inwall to be washed, and dry up with nitrogen;
(7) with absolute ethyl alcohol wiping stove cylinder inwall, by the time after the ethanol volatilization fully, with the again wiping one time of dry terylene non-woven fabric.
Embodiment 3
(1) takes the visor of polycrystalline silicon reducing furnace apart;
(2) adopt giant with deionized water the reduction furnace cylinder inwall to be washed;
(3) dipping mass fraction with terylene non-woven fabric is that 8% ammonium hydrogen fluoride solution carries out wiping to inwall, allows its solution stagnate 12min at inwall;
(4) adopt giant with deionized water stove cylinder inwall to be washed;
(5) again dipping mass fraction with terylene non-woven fabric is that 3% ammonium hydrogen fluoride solution carries out wiping to stove cylinder inwall, allows its solution stagnate 13min at inwall;
(6) adopt giant to wash with deionized water stove cylinder inwall, and dry up with nitrogen;
(7) with absolute ethyl alcohol wiping stove cylinder inwall, by the time after the ethanol volatilization fully, with the again wiping one time of dry terylene non-woven fabric.
Claims (1)
1. a method for cleaning drum of polycrystalline silicon reduction furnace is characterized in that it comprises the steps:
(1) takes the visor of polycrystalline silicon reducing furnace apart;
(2) adopt giant with deionized water the reduction furnace cylinder inwall to be washed;
(3) dipping mass fraction with terylene non-woven fabric is that the ammonium hydrogen fluoride solution of 5%-10% carries out wiping to stove cylinder inwall, allows its solution stagnate 10-15min at inwall;
(4) adopt giant with deionized water the reduction furnace cylinder inwall to be washed;
(5) again dipping mass fraction with terylene non-woven fabric is that the ammonium hydrogen fluoride solution of 2%-4% carries out wiping to stove cylinder inwall, allows its solution stagnate 10-15min at stove cylinder inwall;
(6) adopt giant to wash with deionized water stove cylinder inwall, and dry up with nitrogen;
(7) with absolute ethyl alcohol wiping stove cylinder inwall, by the time after the ethanol volatilization fully, with the again wiping one time of dry terylene non-woven fabric.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110213570 CN102357493B (en) | 2011-07-28 | 2011-07-28 | Method for cleaning drum of polycrystalline silicon reduction furnace |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110213570 CN102357493B (en) | 2011-07-28 | 2011-07-28 | Method for cleaning drum of polycrystalline silicon reduction furnace |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102357493A CN102357493A (en) | 2012-02-22 |
| CN102357493B true CN102357493B (en) | 2013-04-24 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201110213570 Expired - Fee Related CN102357493B (en) | 2011-07-28 | 2011-07-28 | Method for cleaning drum of polycrystalline silicon reduction furnace |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103042009B (en) * | 2012-12-31 | 2015-08-05 | 江西赛维Ldk光伏硅科技有限公司 | A kind of polycrystalline silicon material produces the cleaning method of reduction furnace electrode protective cover |
| CN114164486A (en) * | 2021-12-17 | 2022-03-11 | 新疆大全新能源股份有限公司 | Method for controlling product quality in production process of czochralski or zone-melting single crystal material |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US3522093A (en) * | 1967-02-27 | 1970-07-28 | Chem Cleaning & Equipment Serv | Processes of cleaning and passivating reactor equipment |
| JP2004143530A (en) * | 2002-10-24 | 2004-05-20 | Ekusebun:Kk | Metal surface cleaning agent |
| US20060160239A1 (en) * | 2005-01-14 | 2006-07-20 | Sung-Jae Lee | Method of measuring a level of contamination in a chemical solution and systems thereof |
| EP2082814B1 (en) * | 2008-01-25 | 2011-04-27 | Mitsubishi Materials Corporation | Reactor cleaning apparatus |
| KR20110077604A (en) * | 2009-12-30 | 2011-07-07 | 주식회사 하이닉스반도체 | Apparatus for cleaning wafer and wafer cleaning method using the same |
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| CN102357493A (en) | 2012-02-22 |
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