CN102825036B - Cleaning method for furnace tube for diffusion - Google Patents
Cleaning method for furnace tube for diffusion Download PDFInfo
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- CN102825036B CN102825036B CN201210304062.2A CN201210304062A CN102825036B CN 102825036 B CN102825036 B CN 102825036B CN 201210304062 A CN201210304062 A CN 201210304062A CN 102825036 B CN102825036 B CN 102825036B
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- nitrogen
- boiler tube
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- cleaning method
- diffusion
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Abstract
The invention discloses a cleaning method for a furnace tube for diffusion. The method comprises the following steps of: (1) introducing nitrogen, source-carrying nitrogen and oxygen into the furnace tube for diffusion according to the volume ratio of 150: 1: 1-5: 1: 1, and continuing for above 30 minutes, wherein chloride ions are contained in the source-carrying nitrogen; and (2) stopping the introduction of the nitrogen, the source-carrying nitrogen and the oxygen, and completing cleaning. According to the technical scheme applying the cleaning method disclosed by the invention, Cl- is adopted for cleaning the furnace tube for diffusion, the chloride ions are very easy to be combined with metal ions, the metal ions can be taken out of the furnace tube after combination, then the metal ions of the furnace tube can be cleaned, the disassembly of the furnace tube is not required, and the furnace tube (quartz device) can be prevented from being damaged during the disassembly process.
Description
Technical field
The present invention relates to solar cell preparing technical field, in particular to a kind of cleaning method of furnace tube for diffusion.
Background technology
In manufacture of solar cells process, floating aerial metal ion can enter boiler tube with the silicon chip of turnover boiler tube.Metal ion accumulates in boiler tube, can cause have a strong impact on silicon chip, causes significant impact, so boiler tube needs to clean after using a period of time to the production efficiency of battery and battery quality.In prior art, common cleaning method has following two kinds:
One, produce chlorion by dichloroethylene under high temperature and oxygen reaction to clean boiler tube, but when adopting the method, boiler tube can not be passed in time if there is oxygen, there will be dichloroethylene high temperature cabonization phenomenon, produce black carbon particles and be attached to boiler tube inwall, pollute boiler tube.
Following two reaction equation: C are mainly contained under high temperature
2h
2cl
2+ 2O
2→ 2CO
2+ 2HCl
C
2H
2Cl
2→2HCl+2C
Adopt this kind of method to need to change dichloroethylene source bottle, misoperation easily causes dichloroethylene carbonization, pollutes boiler tube; In addition, because dichloroethylene is not phosphorous, there is no saturated boiler tube effect, also need to carry out saturated process in addition if clean new boiler tube.
Two, boiler tube is removed, be dipped in low concentration HF solution, utilize HF solution to be dissolved by metal ion, and then with a large amount of pure water, boiler tube is rinsed well.But this method wastes time and energy, but also very easily causes coil damage.Because boiler tube is quartz member, frangible in unloading process, dangerous, and high purity quartz boiler tube is very expensive; In addition, quartz components silica, also with HF reaction, causes certain damage to Quartz stove tube in cleaning process; Moreover the time of removing is longer, needs downtime also long.
Summary of the invention
The present invention aims to provide a kind of cleaning method of furnace tube for diffusion, to solve the technical problem of the cleaning step complexity of furnace tube for diffusion in prior art.
To achieve these goals, according to an aspect of the present invention, a kind of cleaning method of furnace tube for diffusion is provided.The method comprises the following steps: 1) in furnace tube for diffusion, pass into nitrogen at 150:1:1 ~ 5:1:1, take source nitrogen and oxygen by volume, continues more than 30 minutes, wherein, takes in the nitrogen of source containing chlorion; 2) stop passing into nitrogen, taking source nitrogen and oxygen, complete cleaning.
Further, step 1) comprises: the temperature in boiler tube is risen to 900 ~ 960 DEG C, and oxygen, nitrogen, source of the taking nitrogen that carries POCl3 are passed into boiler tube and cleans boiler tube.
Further, the flow that passes into of oxygen is 0.1 ~ 1slm; The flow that passes into carrying source of the taking nitrogen of POCl3 is 0.1 ~ 1slm.
Further, taking a step forward of step 1) comprises: in diffusion furnace, arrange POCl3 source bottle, nitrogen is passed into the bottle formation of POCl3 source and takes source nitrogen.
Further, step 1) is, under the condition of being closed by the fire door of diffusion furnace, the temperature in boiler tube is risen to 900 ~ 960 DEG C.
Further, the temperature in boiler tube rises to 900 ~ 960 DEG C continuously.
Further, in the temperature-rise period of step 1), be nitrogen atmosphere in boiler tube.
Further, rate-determining steps 1) time at 30 ~ 180min.
Further, step 2) comprise further afterwards: the temperature in boiler tube is down to 750 ~ 850 DEG C.
Further, boiler tube was cleaned once in every 30 ~ 180 days.
Apply technical scheme of the present invention, adopt Cl
-furnace tube for diffusion is cleaned, chlorion very easily with metal ion combine, in conjunction with after metal ion band is gone out boiler tube, so just boiler tube metal ion is cleaned up, need not boiler tube be dismantled, avoid boiler tube (quartz member) and cause damage in unloading process.New replacing tube skin also can adhere to some metal ions, uses this technique not only can reach the effect of cleaning boiler tube, also produces phosphorus, have the effect of saturated boiler tube, kill two birds with one stone, save time in course of reaction.
Detailed description of the invention
It should be noted that, when not conflicting, the embodiment in the present invention and the feature in embodiment can combine mutually.The present invention is described in detail below in conjunction with embodiment.
According to the cleaning method of a kind of furnace tube for diffusion of the present invention, comprise the following steps: 1) in furnace tube for diffusion, pass into nitrogen at 150:1:1 ~ 5:1:1, take source nitrogen and oxygen by volume, continue more than 30 minutes, wherein, take in the nitrogen of source containing chlorion; 2) stop passing into nitrogen, taking source nitrogen and oxygen, complete cleaning.Apply technical scheme of the present invention, adopt Cl
-furnace tube for diffusion is cleaned, chlorion very easily with metal ion combine, in conjunction with after metal ion band is gone out boiler tube, so just boiler tube metal ion is cleaned up and need not dismantle boiler tube, avoid boiler tube (quartz member) and cause damage in unloading process.New replacing tube skin also can adhere to some metal ions, uses this technique not only can reach the effect of cleaning boiler tube, also produces phosphorus, have the effect of saturated boiler tube, kill two birds with one stone, save time in course of reaction.
Preferably, step 1) comprises: the temperature in boiler tube is risen to 900 ~ 960 DEG C, and oxygen, nitrogen, source of the taking nitrogen that carries POCl3 are passed into boiler tube and cleans boiler tube.Because POCl3 very easily decomposes generation Cl at 900 ~ 960 DEG C
-, POCl3, as a kind of conventional phosphorus source, adopts this method of operating and convenience thereof.Preferably, the flow that passes into of oxygen is 0.1 ~ 1slm; The flow that passes into carrying the nitrogen of POCl3 is 0.1 ~ 1slm, is convenient to Cl
-after fully reacting with metal ion, boiler tube can be discharged with the mist of nitrogen, oxygen.
According to a kind of typical embodiment of the present invention, if anemostat diffuse source used is not POCl3, taking a step forward to be included in diffusion furnace and arrange POCl3 source bottle in step 1), passes into POCl3 source bottle and is formed and take source nitrogen by nitrogen.If what diffuse source adopted is POCl3, namely this step can be omitted.
Preferably, step 1) is, under the condition of being closed by the fire door of diffusion furnace, the temperature in boiler tube is risen to 900 ~ 960 DEG C.Because POCl3 is poisonous, fire door is closed and is guaranteed that POCl3 is not leaked in working environment.Better in the effect of 900 ~ 960 DEG C of cleanings, be unlikely to again to cause damage to quartz member and equipment.Preferably, the temperature in boiler tube rises to 900 ~ 960 DEG C continuously.Preferably, in the temperature-rise period of step 1), keep nitrogen atmosphere in boiler tube, namely keep that nitrogen is normal as normal operation circumstances to be passed into.Preferably, rate-determining steps 1) time at 30 ~ 180min.Preferably, step 2) comprise further afterwards: the temperature in boiler tube is down to 750 DEG C ~ 850 DEG C, prepares follow-up normal production, this easy to operate production management.
Preferably, boiler tube was cleaned once in every 30 ~ 180 days.In actual production process, adopt technical scheme of the present invention to clean once to boiler tube in every 30 ~ 180 days, the silicon chip caused can be reduced by 0.1% by defective productive rate by metal ion pollution boiler tube.
The present invention is illustrated below in conjunction with embodiment.
Embodiment 1
1) temperature in boiler tube is risen to 900 DEG C, oxygen, nitrogen, the nitrogen that carries POCl3 are passed into boiler tube and cleans boiler tube, keeps 30 minutes; Wherein, nitrogen, take source nitrogen, oxygen volume ratio at 150:1:1; The flow velocity that passes into of oxygen is 0.1slm;
2) stop passing into described gas, complete cleaning, the temperature in boiler tube is down to 750 DEG C.
Embodiment 2
1) temperature in boiler tube is risen to 960 DEG C, oxygen, nitrogen, the nitrogen that carries POCl3 are passed into boiler tube and cleans boiler tube, keeps 30 minutes; Wherein; Nitrogen, take source nitrogen, oxygen volume ratio at 5:1:1; The flow velocity that passes into of oxygen is 1slm;
2) stop passing into described gas, complete cleaning, the temperature in boiler tube is down to 850 DEG C.
Embodiment 3
1) temperature in boiler tube is risen to 940 DEG C, oxygen, nitrogen, the nitrogen that carries POCl3 are passed into boiler tube and cleans boiler tube, keeps 180 minutes; Wherein; Nitrogen, take source nitrogen, oxygen volume ratio at 100:1:1; The flow velocity that passes into of oxygen is 0.1slm;
2) stop passing into described gas, complete cleaning, the temperature in boiler tube is down to 800 DEG C.
Adopt the method in embodiment 1 ~ 3, within every 30 ~ 180 days, clean once to boiler tube, the silicon chip caused can be reduced by 0.1% by defective productive rate by metal ion pollution boiler tube.
To sum up, technical scheme of the present invention is adopted to possess following beneficial effect:
1) can realize on-line cleaning boiler tube without reforming equipment, simple and practical, the method cleans furnace process after may be used for long-time use, also can use as newly changing boiler tube saturation process;
2) the technical program produces phosphorus in reaction simultaneously, and cleaning, saturated boiler tube are carried out simultaneously, save time;
3) cleaning method of the present invention, close with diffusion technique of the prior art, therefore, on the basis of existing diffusion technique, impurity and remove Action of Metal Ions in cleaning boiler tube can be reached by only changing technological parameter;
4) need not boiler tube be dismantled, avoid dismounting boiler tube to cause quartz piece to damage;
5) pollution level that the present invention can be different according to boiler tube, nitrogen flow and the time of POCl3 are taken in adjustment, easy to operate.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, for a person skilled in the art, the present invention can have various modifications and variations.Within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (9)
1. a cleaning method for furnace tube for diffusion, is characterized in that, comprises the following steps:
1) in furnace tube for diffusion, pass into nitrogen at 150:1:1 ~ 5:1:1, take source nitrogen and oxygen by volume, continue more than 30 minutes, wherein, described in take in the nitrogen of source containing chlorion;
2) stop passing into described nitrogen, taking source nitrogen and oxygen, complete cleaning;
Described step 1) comprising:
Temperature in described boiler tube is risen to 900 ~ 960 DEG C, oxygen, nitrogen, source of the taking nitrogen that carries POCl3 are passed into described boiler tube and cleans described boiler tube.
2. cleaning method according to claim 1, is characterized in that, the flow that passes into of described oxygen is 0.1 ~ 1slm; The described flow that passes into carrying source of the taking nitrogen of POCl3 is 0.1 ~ 1slm.
3. cleaning method according to claim 1, is characterized in that, described step 1) take a step forward and comprise:
POCl3 source bottle is set in diffusion furnace, nitrogen is passed into described in the bottle formation of described POCl3 source and take source nitrogen.
4. cleaning method according to claim 3, is characterized in that, described step 1) be, under the condition of being closed by the fire door of described diffusion furnace, the temperature in described boiler tube is risen to 900 ~ 960 DEG C.
5. cleaning method according to claim 4, is characterized in that, the temperature in described boiler tube rises to 900 ~ 960 DEG C continuously.
6. cleaning method according to claim 1, is characterized in that, in described step 1) temperature-rise period in, be nitrogen atmosphere in described boiler tube.
7. cleaning method according to claim 1, is characterized in that, controls described step 1) time at 30 ~ 180min.
8. cleaning method according to claim 1, is characterized in that, described step 2) comprise further afterwards:
Temperature in described boiler tube is down to 750 ~ 850 DEG C.
9. cleaning method according to claim 1, is characterized in that, within every 30 ~ 180 days, cleans once described boiler tube.
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CN102825036B true CN102825036B (en) | 2014-12-24 |
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Families Citing this family (10)
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CN103928367A (en) * | 2014-03-20 | 2014-07-16 | 上海华力微电子有限公司 | Furnace tube device and method for reducing Cu pollution in furnace tube process |
CN103894381A (en) * | 2014-03-20 | 2014-07-02 | 上海华力微电子有限公司 | Furnace pipe cleaning method |
CN104259153B (en) * | 2014-07-24 | 2017-12-22 | 上海华力微电子有限公司 | furnace tube cleaning process |
CN104741335A (en) * | 2015-04-02 | 2015-07-01 | 中建材浚鑫科技股份有限公司 | Method for cleaning quartz boat for diffusion |
CN105537207B (en) * | 2015-12-11 | 2018-09-25 | 上海交通大学 | A kind of cleaning method of high temperature quartz ampoule |
CN108728901B (en) * | 2018-06-15 | 2021-01-22 | 常州亿晶光电科技有限公司 | Maintenance method of diffusion furnace tube |
CN110813936B (en) * | 2019-11-01 | 2021-05-04 | 江苏亚电科技有限公司 | Quartz furnace tube immersion cleaning method |
CN112893337A (en) * | 2021-01-21 | 2021-06-04 | 联物科技实业无锡有限公司 | High-temperature ethylene dichloride oxide cleaning process for wafer processing |
CN113600565B (en) * | 2021-06-30 | 2022-10-25 | 英利能源(中国)有限公司 | Cleaning method of N-type solar cell boron diffusion furnace tube |
CN115522264B (en) * | 2022-10-30 | 2024-06-14 | 平煤隆基新能源科技有限公司 | Cleaning method for phosphorus diffusion furnace tube of crystalline silicon solar cell |
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JP5604803B2 (en) * | 2008-03-28 | 2014-10-15 | 三菱マテリアル株式会社 | Polymer deactivation method in polycrystalline silicon production equipment |
CN102569501B (en) * | 2011-12-15 | 2014-06-18 | 苏州阿特斯阳光电力科技有限公司 | Phosphorous diffusion method for polycrystalline silicon solar battery |
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