CN104831351A - Crucible cover plate for polysilicon ingot furnace and cover plate surface coating method - Google Patents
Crucible cover plate for polysilicon ingot furnace and cover plate surface coating method Download PDFInfo
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- CN104831351A CN104831351A CN201510289666.8A CN201510289666A CN104831351A CN 104831351 A CN104831351 A CN 104831351A CN 201510289666 A CN201510289666 A CN 201510289666A CN 104831351 A CN104831351 A CN 104831351A
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Abstract
The invention relates to a crucible cover plate for a polysilicon ingot furnace and a cover plate surface coating method. The crucible cover plate for the polysilicon ingot furnace and the cover plate surface coating method have the advantages that a dense SiC coating high in bonding strength is prepared on the outer surface of the cover plate made of carbon-carbon composites by a technological method combining chemical vapor deposition with high-temperature treatment, so that carbon content of polysilicon ingots is reduced, service life of the cover plate is prolonged and the method is particularly applicable to development and application of the cover plate for the polysilicon ingot furnace.
Description
Technical field
The present invention relates to a kind of crucible used for polycrystalline silicon ingot casting cover plate.
Background technology
Polycrystalline silicon material accounts for over half in the demand of area of solar cell, and the good and bad quality being directly connected to solar-energy photo-voltaic cell of silicon chip, therefore produces high-quality silicon chip significant.Current polycrystalline silicon casting ingot process many employings directional solidification method, production process temperatures as high more than 1500 DEG C, crucible and the heat resistant structure part such as cover plate many employings graphite and carbon/carbon composite in ingot furnace.Under hot environment, the impurity such as the residual oxygen in ingot furnace, silicon oxide, easily CO (carbon monoxide converter) gas is generated as the carbon surface of crucible, cover plate reacts with heat resistant structure part, carbon monoxide and then react with silicon melt and discharge carbon, cause silicon melt Prevent Carbon Contamination, the carbon content in ingot casting increases, in follow-up slice process, add the quantity of carbon Hard Inclusion, affect polysilicon yield rate and quality.In addition, the free silica of ingot casting process release causes silicon corrosion phenomenon to plumbago crucible and carbon/carbon composite cover plate, destroys internal carbon fibers and carbon base body, makes plumbago crucible and charcoal/charcoal cover plate service life reduction.
Summary of the invention
In order to reduce the carbon content in silicon ingot, reducing the quantity of carbon Hard Inclusion, improving plumbago crucible and charcoal/charcoal cover plate life-span, the invention provides a kind of polycrystalline silicon ingot or purifying furnace crucible cover plate and lid surface coating process.
Polycrystalline silicon ingot or purifying furnace crucible cover plate provided by the present invention, crucible cover plate is carbon/carbon composite cover plate, and its special character is:
The outside surface of described carbon/carbon composite cover plate is provided with SiC coating.
Above-mentioned SiC coat-thickness is 10-100 μm.
Above-mentioned SiC coat-thickness is 50 μm.
The preparation method of polycrystalline silicon ingot or purifying furnace crucible cover plate surface provided by the present invention SiC coating, its special character is: comprise the following steps:
1] pyroprocessing
Cover plate is sent in vacuum sintering furnace the volatile matter carried out in pyroprocessing removal cover plate, temperature is 1500 ~ 1700 DEG C;
2] chemical vapour deposition
The cover plate crossed through pyroprocessing is sent into chemical vapor deposition stove, is reactant, is warming up to 1000 ~ 1100 DEG C with trichloromethyl silane, deposition 30 ~ 70h, preparation has the carbon/carbon composite cover plate of SiC coating.
1] also comprise before pyroprocessing: cleaning, to dry and the step of wiping.
In step 1] step 2 after pyroprocessing] also comprise cleaning between chemical vapour deposition, dry and the step of wiping.
Above-mentioned cleaning, to dry and the step of wiping is specially:
Lid surface is used flowing water clean surface floating dust, re-use ultrasonic apparatus cleaning, dry more than 2 hours at putting into 200 DEG C, baking oven, use alcohol wipe composite material surface.
Compared with prior art, advantage is in the present invention:
1, the SiC coating of lid surface of the present invention can effectively prevent the uncombined carbon of crucible cover plate volatilization in polycrystalline silicon ingot casting process to the pollution of silicon ingot, reduce the carbon content of polycrystalline silicon ingot casting, improve the yield rate of polycrystalline silicon ingot casting, be particularly useful for the development and application of polycrystalline silicon ingot casting stove cover plate.
2, the SiC coating of lid surface of the present invention is not easily reacted with free silica, reduces silicon corrosion phenomenon to the destruction of crucible cover plate, while raising ingot casting and Si wafer quality, can extend the work-ing life of cover plate.
3, the method that the present invention adopts pyroprocessing and chemical vapour deposition to combine prepares SiC coating, many heats use back shroud coating not come off, insensitive to silicon corrosion phenomenon in ingot casting process, and process cycle is short, delivery cycle is short, single heat cost is lower than the not cated carbon/carbon composite cover plate of tool.The present invention is applied to production of polysilicon, effectively can improve productivity effect.
Figure of description
Fig. 1 has the charcoal/charcoal cover plate schematic diagram of SiC coating, 1-carbon/carbon composite cover plate, 2-SiC coating.
Embodiment
Polycrystalline silicon ingot or purifying furnace crucible cover plate provided by the invention and lid surface coating process, by arranging SiC coating 2 to reduce the carbon content of polycrystalline silicon ingot casting, to extend the work-ing life of cover plate at the outside surface of carbon/carbon composite cover plate 1.
The preparation method of polycrystalline silicon ingot or purifying furnace crucible cover plate of the present invention surface SiC coating, adopts the processing method that chemical vapour deposition combines with pyroprocessing, and prepare densification, SiC coating that bonding force is good at crucible surface, a preferred implementation process is as follows:
1) cleaning, drying: carbon/carbon composite lid surface is used flowing water clean surface floating dust, re-uses ultrasonic apparatus cleaning 2 ~ 3 times, each 30 minutes.Dry more than 2 hours at putting into 200 DEG C, baking oven, use alcohol wipe lid surface.
Because carbon/carbon composite is mesoporous material, therefore the present invention has carried out cleaning, oven dry, wiping to cover plate before pyroprocessing, and object is mainly in order to remove the floating dust of cover plate supplied materials surface attachment.
2) pyroprocessing: sent in vacuum sintering furnace by carbon/carbon composite cover plate and carry out pyroprocessing, temperature is 1500 ~ 1700 DEG C, and soaking time is 1 hour.
Presedimentary pyroprocessing, object carries out purifying to carbon/carbon composite cover plate, in order to avoid under the condition of high temperature of follow-up chemical vapor deposition processes, the volatile matter in cover plate has an impact to the generation of coating and homogeneity.The temperature 1500-1700 DEG C of pyroprocessing, higher than the use temperature (1400-1500 DEG C) of cover plate, arranges this parameter and can reach technique object, can save production cost again.Pyroprocessing 1 hour, can reach the object of purifying.
3) cleaning, drying
Carbon/carbon composite cover plate after pyroprocessing is used flowing water clean surface floating dust, re-use ultrasonic apparatus cleaning 2 ~ 3 times, each 30 minutes.Dry more than 2 hours at putting into 200 DEG C, baking oven, use alcohol wipe lid surface.
Floating dust and impurity attachment can reduce the bonding force of SiC coating, therefore the present invention has carried out the step of cleaning, drying wiping after pyroprocessing before chemical vapour deposition, main purpose is the floating dust in order to remove the attachment of the lid surface after pyroprocessing, increases the smooth finish of lid surface; Cleaning process requires to use ultrasonic apparatus, and object is more thorough in order to clean, and makes lid surface brighter and cleaner, increases the bonding force of SiC coating and lid surface.
4) chemical vapour deposition (CVI) technique
Carbon/carbon composite cover plate is sent into chemical vapor deposition stove, is warming up to 1000 ~ 1100 DEG C, deposition 30 ~ 70h, preparation has the carbon/carbon composite cover plate of SiC coating, has the schematic diagram of the carbon/carbon composite cover plate of SiC coating as Fig. 1.
In this step, the selection of depositing time mainly sets according to the requirement of finished product coat-thickness, and depositing time is more of a specified duration, and the finished product coat-thickness obtained is higher.
The carbon/carbon composite cover plate of SiC coating that prepared by the present invention have, the uncombined carbon volatilized in ingot casting process obviously reduces, thus significantly reduces in silicon chip because of stria quantity that carbon Hard Inclusion produces.Effect after certain producer tries out: under same test conditions, with the ratio of Hard Inclusion stria sheet in some amount silicon chip for criterion, use the contrast of the crucible and cover plate with SiC coating not use the pact of coating to decline 61%, single heat benefit increase about 400 yuan, detailed data is in table 1.
Table 1 SiC coating cover plate with contrast without Hard Inclusion stria sheet accounting under coating cover plate same experimental conditions
Claims (7)
1. a polycrystalline silicon ingot or purifying furnace crucible cover plate, crucible cover plate is carbon/carbon composite cover plate, it is characterized in that: the outside surface of described carbon/carbon composite cover plate is provided with SiC coating.
2. polycrystalline silicon ingot or purifying furnace crucible cover plate according to claim 1, is characterized in that:
Described SiC coat-thickness is 10-100 μm.
3. polycrystalline silicon ingot or purifying furnace crucible cover plate according to claim 2, is characterized in that:
Described SiC coat-thickness is 50 μm.
4. a polycrystalline silicon ingot or purifying furnace preparation method for crucible cover plate surface SiC coating, is characterized in that: comprise the following steps:
1] pyroprocessing
Carbon/carbon composite cover plate is sent in vacuum sintering furnace the volatile matter carried out in pyroprocessing removal cover plate, treatment temp is 1500 ~ 1700 DEG C;
2] chemical vapour deposition
The cover plate crossed through pyroprocessing is sent into chemical vapor deposition stove, is reactant, is warming up to 1000 ~ 1100 DEG C with trichloromethyl silane, deposition 30 ~ 70h, preparation has the carbon/carbon composite cover plate of SiC coating.
5. the preparation method of polycrystalline silicon ingot or purifying furnace crucible cover plate surface according to claim 4 SiC coating, is characterized in that:
1] also comprise before pyroprocessing: cleaning, to dry and the step of wiping.
6. the preparation method of polycrystalline silicon ingot or purifying furnace crucible cover plate surface according to claim 4 SiC coating, is characterized in that:
In step 1] step 2 after pyroprocessing] also comprise between chemical vapour deposition and lid surface is cleaned, dry and the step of wiping.
7. the preparation method of crucible cover plate surface SiC coating of the polycrystalline silicon ingot or purifying furnace described in claim 5 or 6, is characterized in that:
Described cleaning, to dry and the step of wiping is specially:
Lid surface is used flowing water clean surface floating dust, re-uses ultrasonic apparatus cleaning,
Dry more than 2 hours at putting into 200 DEG C, baking oven,
Use alcohol wipe lid surface.
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| CN201510289666.8A CN104831351A (en) | 2015-05-29 | 2015-05-29 | Crucible cover plate for polysilicon ingot furnace and cover plate surface coating method |
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Cited By (5)
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| CN105442042A (en) * | 2016-02-02 | 2016-03-30 | 江西赛维Ldk太阳能高科技有限公司 | Ingot furnace for reducing carbon content of polycrystalline silicon ingot and preparation method of ingot furnace |
| CN105506735A (en) * | 2015-12-10 | 2016-04-20 | 江西赛维Ldk太阳能高科技有限公司 | Carbon material structural part for polycrystalline silicon ingots and preparation method of carbon material structural part |
| CN106048717A (en) * | 2016-07-20 | 2016-10-26 | 湖南红太阳光电科技有限公司 | Crucible cover plate for polycrystalline silicon ingot casting |
| CN109161961A (en) * | 2018-11-27 | 2019-01-08 | 晶科能源有限公司 | A kind of polycrystalline cast ingot crucible cover plate and preparation method thereof |
| CN111377754A (en) * | 2018-12-29 | 2020-07-07 | 洛阳阿特斯光伏科技有限公司 | Composite carbon cover plate for ingot furnace, and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105506735A (en) * | 2015-12-10 | 2016-04-20 | 江西赛维Ldk太阳能高科技有限公司 | Carbon material structural part for polycrystalline silicon ingots and preparation method of carbon material structural part |
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| CN105442042B (en) * | 2016-02-02 | 2018-01-12 | 江西赛维Ldk太阳能高科技有限公司 | It is a kind of to be used to reduce ingot furnace of polycrystal silicon ingot carbon content and preparation method thereof |
| CN106048717A (en) * | 2016-07-20 | 2016-10-26 | 湖南红太阳光电科技有限公司 | Crucible cover plate for polycrystalline silicon ingot casting |
| CN106048717B (en) * | 2016-07-20 | 2019-07-26 | 湖南红太阳光电科技有限公司 | A kind of crucible used for polycrystalline silicon ingot casting cover board |
| CN109161961A (en) * | 2018-11-27 | 2019-01-08 | 晶科能源有限公司 | A kind of polycrystalline cast ingot crucible cover plate and preparation method thereof |
| CN111377754A (en) * | 2018-12-29 | 2020-07-07 | 洛阳阿特斯光伏科技有限公司 | Composite carbon cover plate for ingot furnace, and preparation method and application thereof |
| CN111377754B (en) * | 2018-12-29 | 2022-05-03 | 洛阳阿特斯光伏科技有限公司 | Composite carbon cover plate for ingot furnace, and preparation method and application thereof |
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Application publication date: 20150812 |