CN106970081B - A kind of crack defect method of inspection of silica crucible finished product - Google Patents
A kind of crack defect method of inspection of silica crucible finished product Download PDFInfo
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- CN106970081B CN106970081B CN201610024316.3A CN201610024316A CN106970081B CN 106970081 B CN106970081 B CN 106970081B CN 201610024316 A CN201610024316 A CN 201610024316A CN 106970081 B CN106970081 B CN 106970081B
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- silica crucible
- finished product
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- crucible finished
- crucible
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 111
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 54
- 238000007689 inspection Methods 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims abstract description 25
- 230000007547 defect Effects 0.000 title claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000000428 dust Substances 0.000 claims abstract description 16
- 239000007921 spray Substances 0.000 claims abstract description 16
- 208000037656 Respiratory Sounds Diseases 0.000 claims abstract description 14
- AEEAZFQPYUMBPY-UHFFFAOYSA-N [I].[W] Chemical compound [I].[W] AEEAZFQPYUMBPY-UHFFFAOYSA-N 0.000 claims abstract description 14
- 230000005540 biological transmission Effects 0.000 claims abstract description 10
- 238000001514 detection method Methods 0.000 claims description 17
- 238000001035 drying Methods 0.000 claims description 5
- 230000000007 visual effect Effects 0.000 claims description 5
- 238000009736 wetting Methods 0.000 claims 1
- 239000000047 product Substances 0.000 description 37
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 11
- 238000005266 casting Methods 0.000 description 8
- 238000004519 manufacturing process Methods 0.000 description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 6
- 229910052710 silicon Inorganic materials 0.000 description 6
- 239000010703 silicon Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 3
- 229910052571 earthenware Inorganic materials 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000002347 injection Methods 0.000 description 3
- 239000007924 injection Substances 0.000 description 3
- 229920005591 polysilicon Polymers 0.000 description 3
- 239000010453 quartz Substances 0.000 description 3
- 238000007711 solidification Methods 0.000 description 3
- 230000008023 solidification Effects 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 239000012466 permeate Substances 0.000 description 2
- 239000002210 silicon-based material Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 231100001261 hazardous Toxicity 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000011505 plaster Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 238000007569 slipcasting Methods 0.000 description 1
- 239000012265 solid product Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/84—Systems specially adapted for particular applications
- G01N21/88—Investigating the presence of flaws or contamination
- G01N21/8803—Visual inspection
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2201/00—Features of devices classified in G01N21/00
- G01N2201/06—Illumination; Optics
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- General Health & Medical Sciences (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- Analysing Materials By The Use Of Radiation (AREA)
- Investigating Materials By The Use Of Optical Means Adapted For Particular Applications (AREA)
Abstract
The invention discloses a kind of crack defect methods of inspection of silica crucible finished product, after dried silica crucible is carried out the processing of surface drifting dust, with the watering can that pure water is housed, it sprays water to crucible Examination region, while carrying out light transmission irradiation with the iodine-tungsten lamp of 500W to check crackle present in discovery crucible.The present invention can accurately have found blind crack, simple and quick, high-efficient.
Description
Technical field
The present invention relates to a kind of silica crucible quality detecting method, in particular to a kind of crack defect of silica crucible finished product
The method of inspection.
Background technique
Silica crucible is the container for producing polycrystalline silicon ingot casting, is disappeared in addition to polycrystalline silicon raw material in polysilicon production process
The maximum consumables of consumption.Its production technology difficulty is big, material purity requires that high, use environment is harsh, be in 1550 DEG C of height
It is the key that irreplaceable consumable material in polysilicon production process disposable continuous work 50 hours or more in temperature.In addition, face
To the high-purity polycrystalline silicon raw material situation that supply falls short of demand, many countries have all carried out polycrystalline silicon raw material according to polycrystalline silicon ingot casting principle
Melting Purification, silica crucible is in the effect for wherein also having played no less important.Therefore, it and polysilicon photovoltaic industry have
There is inseparable, interdependence relationship.As the production technology of silica crucible, generally there are injection forming and note solidification forming
Two kinds.Slip-casting shaping process is the traditional forming technique of quartz, i.e., the high-performance quartz ceramic mud modulated in plaster mold
Middle injection forming obtains product, and offshore company generally uses the technique.Casting molding technique is added in quartz-ceramics mud
A kind of organic monomer, formed in non-punch die after directly solidification obtain product.Two kinds of technologies respectively have feature, injection forming product
Density is slightly higher, wearability is good, is suitble to roll, the square solid product of manufacture simple shape, and note solidification forming product gas porosity is omited
Height, thermal shock resistance are more preferable, are suitble to the complex-shaped thin wall shape hollow product of manufacture.
Rectangular silica crucible is used in during polycrystalline silicon ingot casting, will be loaded into earthenware under high temperature (1400 DEG C -1550 DEG C)
Solar-grade high-purity polycrystalline silicon block material in crucible is fused into one big whole ingot, then passes through post-production for silicon ingot evolution, slice
Etc. last solar battery sheet is made.Container of the crucible as silicon material, there is very strict requirement in terms of quality.If
Crucible is in ingot casting with the presence of crackle, and as the softening of crucible material at high temperature is acted on plus the pressure of silicon material, crackle can expand
Greatly, so that silicon liquid be caused to leak out from crack, the silicon liquid of high temperature can generate corrosion to the graphite protective plate of crucible periphery and penetrate,
And may finally leak in ingot furnace, extremely hazardous damage is caused to casting unit.Therefore, crucible is must be through before
Cross carefully stringent quality restriction, it is ensured that there is no crackle presence in crucible.
Summary of the invention
The purpose of the present invention is to provide a kind of crack defect methods of inspection of silica crucible finished product, can accurately find subtle
Crackle, it is simple and quick, it is high-efficient.
The technical solution adopted by the present invention to solve the technical problems is:
A kind of crack defect method of inspection of silica crucible finished product, includes the following steps:
(1) silica crucible finished product is dried；
(2) the silica crucible finished product after drying process is placed on inspection desk, it is clean with air gun drifting dust；
(3) it is sprayed water with quasi- detection zone of the watering can equipped with pure water to drifting dust treated silica crucible finished product sufficiently to moisten
Wet quasi- detection zone, while light transmission photograph is carried out with 500W iodine-tungsten lamp in the corresponding another side in silica crucible finished product water spray face
It penetrates, whether has crackle with visual method inspection water spray face.
(4) mobile watering can and iodine-tungsten lamp are by all inspections one time of the surfaces externally and internally of entire silica crucible finished product.
The corresponding another side in water spray face refers to the face for being separated by silica crucible wall thickness with water spray face, i.e., if water spray face
It is a certain region of lateral surface, then corresponding another side is the corresponding region of silica crucible medial surface.With silica crucible wall
Centered on, water spray face is located at the two sides of silica crucible wall with corresponding another side.
Creation point of the invention is to use pure water as crack detection agent, cooperation 500W iodine-tungsten lamp light transmission irradiation, with detection
With the presence or absence of crackle.Pure water will not bring additional pollutant into as crack detection agent first, secondly, pure water does not have color, no
The silica crucible of white can be polluted.Major light is often used alone in conventional crack detection, has a defect that in this way, often compared with
Big crackle is easy to be found, and lesser crackle because color and surrounding after major light transmission without notable difference,
Naked eyes are difficult to differentiate, these fine cracks is caused to be difficult to be found.And the present invention uses pure water to cooperate 500W as crack detection agent
Iodine-tungsten lamp light transmission irradiation collaboration plays a role, and after pure water first permeates silica crucible, if there is fine cracks, water can be penetrated into and be split
In seam, then with red iodine-tungsten lamp light transmission irradiation is shown, under refraction action, fine cracks will appear apparent white, and around
Normal region is still displayed in red, in this way can fairly simple, the accurate presence for finding crackle.
Preferably, step (1) is dried to moisture content≤0.1% of silica crucible finished product.Control rectangular quartzy earthenware
The moisture content of crucible green compact is very crucial not higher than 0.1%, and such pure water can permeate rapidly, crack detection of being faster more convenient for, and improves
Detection efficiency.
Preferably, the air pressure of step (2) air gun drifting dust is 0.3~0.6Mpa.
Preferably, the quality standard of step (3) described pure water are as follows: resistivity is more than 2M Ω .cm.Control pure water resistance
Rate is in 2M Ω .cm the above object: the metal ion content in control water, these metal ions can generate pollution to product,
Crystal ingot quality after influencing final ingot casting, therefore to control.
The beneficial effects of the present invention are: can accurately find blind crack, and it is simple and quick, it is high-efficient.
Specific embodiment
Below by specific embodiment, technical scheme of the present invention will be further explained in detail.
In the present invention, if not refering in particular to, used raw material and equipment etc. are commercially available or commonly used in the art.
Method in following embodiments is unless otherwise instructed the conventional method of this field.
Implement global schema:
A kind of crack defect method of inspection of silica crucible finished product, includes the following steps:
(1) silica crucible finished product is dried to moisture content≤0.1% of silica crucible finished product.
(2) the silica crucible finished product after drying process is placed on inspection desk, it is clean with air gun drifting dust, air gun drifting dust
Air pressure is 0.3~0.6Mpa.
(3) it is sprayed water with quasi- detection zone of the watering can equipped with pure water to drifting dust treated silica crucible finished product sufficiently to moisten
Wet quasi- detection zone, the quality standard of pure water are as follows: resistivity is more than 2M Ω .cm.Simultaneously in silica crucible finished product water spray face phase
Corresponding another side carries out light transmission irradiation with 500W iodine-tungsten lamp, whether has crackle with visual method inspection water spray face.
(4) mobile watering can and iodine-tungsten lamp are by all inspections one time of the surfaces externally and internally of entire silica crucible finished product.
It is required to carry out subsequent job judgement according to quality specification according to inspection result.
Case 1 is embodied
A kind of crack defect method of inspection of silica crucible finished product, includes the following steps:
(1) silica crucible finished product is dried to moisture content≤0.1% of silica crucible finished product.
(2) the silica crucible finished product after drying process is placed on inspection desk, it is clean with air gun drifting dust, air gun drifting dust
Air pressure is 0.3Mpa.
(3) it is sprayed water with quasi- detection zone of the watering can equipped with pure water to drifting dust treated silica crucible finished product sufficiently to moisten
Wet quasi- detection zone, the quality standard of pure water are as follows: resistivity is in 3.5M Ω .cm.Simultaneously in silica crucible finished product water spray face (quartz
Crucible medial surface) corresponding another side (silica crucible lateral surface) with 500W iodine-tungsten lamp carries out light transmission irradiation, use visual method
Check whether water spray face has crackle.
Mobile watering can and iodine-tungsten lamp are by all inspections one time of the surfaces externally and internally of entire crucible, according to inspection result according to quality
Specification requirement carries out subsequent job judgement.
Case 2 is embodied
A kind of crack defect method of inspection of silica crucible finished product, includes the following steps:
(1) silica crucible finished product is dried to moisture content≤0.1% of silica crucible finished product.
(2) the silica crucible finished product after drying process is placed on inspection desk, it is clean with air gun drifting dust, air gun drifting dust
Air pressure is 0.6Mpa.
(3) it is sprayed water with quasi- detection zone of the watering can equipped with pure water to drifting dust treated silica crucible finished product sufficiently to moisten
Wet quasi- detection zone, the quality standard of pure water are as follows: resistivity is in 4M Ω .cm.Simultaneously in silica crucible finished product water spray face (quartzy earthenware
Crucible lateral surface) corresponding another side (silica crucible medial surface) with 500W iodine-tungsten lamp carries out light transmission irradiation, it is examined with visual method
Look into whether water spray face has crackle.
Mobile watering can and iodine-tungsten lamp are by all inspections one time of the surfaces externally and internally of entire crucible, according to inspection result according to quality
Specification requirement carries out subsequent job judgement.
Effect judgement:
After the method according to the invention is to silica crucible product inspection, polycrystalline silicon ingot casting production is carried out, investigates leakage silicon rate, leakage
Silicon rate standard is that leakage silicon rate is lower than 0.2%.
Test result:
From upper table result data, after method of the invention is to silica crucible product inspection, crucible can be effectively verified
In blind crack, it is ensured that crucible have high-quality.
Above-mentioned embodiment is only a preferred solution of the present invention, not the present invention is made in any form
Limitation, there are also other variations and modifications on the premise of not exceeding the technical scheme recorded in the claims.
Claims (3)
1. a kind of crack defect method of inspection of silica crucible finished product, which comprises the steps of:
(1) silica crucible finished product is dried to moisture content≤0.1% of silica crucible finished product；
(2) the silica crucible finished product after drying process is placed on inspection desk, it is clean with air gun drifting dust；
(3) quasi- with abundant wetting to the quasi- detection zone water spray of drifting dust treated silica crucible finished product with the watering can equipped with pure water
Detection zone, while light transmission irradiation is carried out with 500W iodine-tungsten lamp at the back side in silica crucible finished product water spray face, it is checked with visual method
Whether water spray face has crackle；
(4) mobile watering can and iodine-tungsten lamp are by all inspections one time of the surfaces externally and internally of entire silica crucible finished product.
2. the crack defect method of inspection according to claim 1, it is characterised in that: the air pressure of step (2) air gun drifting dust is
0.3~0.6Mpa.
3. the crack defect method of inspection according to claim 1, it is characterised in that: the quality mark of step (3) described pure water
It is quasi- are as follows: resistivity is more than 2M Ω cm.
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| CN201610024316.3A CN106970081B (en) | 2016-01-14 | 2016-01-14 | A kind of crack defect method of inspection of silica crucible finished product |
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| CN201610024316.3A CN106970081B (en) | 2016-01-14 | 2016-01-14 | A kind of crack defect method of inspection of silica crucible finished product |
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| CN106970081A CN106970081A (en) | 2017-07-21 |
| CN106970081B true CN106970081B (en) | 2019-09-03 |
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| CN111323431A (en) * | 2020-03-10 | 2020-06-23 | 欧贝黎新能源科技股份有限公司 | Silicon wafer microcrack detection device based on solar cell and application method thereof |
| CN111308866B (en) * | 2020-04-01 | 2023-08-22 | 烟台核晶陶瓷新材料有限公司 | Developing solution for crucible detection and preparation method and application method thereof |
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| CN204241385U (en) * | 2014-11-17 | 2015-04-01 | 天津英利新能源有限公司 | A kind of polycrystalline cast ingot crucible checking system |
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Effective date of registration: 20190805 Address after: 310000 No. 6515, Jiangdong Third Road, Dajiangdong Industrial Agglomeration Area, Hangzhou City, Zhejiang Province Applicant after: Hangzhou Da he Jiangdong new Mstar Technology Ltd Address before: 311222 No. 668 Qingliu North Road, Jiangdong Industrial Park, Binjiang District, Hangzhou City, Zhejiang Province Applicant before: Hangzhou Jingxin Technology Co., Ltd. |
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