CN106970081A - 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
- Publication number
- CN106970081A CN106970081A CN201610024316.3A CN201610024316A CN106970081A CN 106970081 A CN106970081 A CN 106970081A CN 201610024316 A CN201610024316 A CN 201610024316A CN 106970081 A CN106970081 A CN 106970081A
- Authority
- CN
- China
- Prior art keywords
- silica crucible
- finished product
- inspection
- crucible finished
- crack defect
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 112
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 55
- 238000007689 inspection Methods 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 26
- 230000007547 defect Effects 0.000 title claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000000428 dust Substances 0.000 claims abstract description 16
- AEEAZFQPYUMBPY-UHFFFAOYSA-N [I].[W] Chemical compound [I].[W] AEEAZFQPYUMBPY-UHFFFAOYSA-N 0.000 claims abstract description 14
- 208000037656 Respiratory Sounds Diseases 0.000 claims abstract description 13
- 238000007639 printing Methods 0.000 claims abstract description 9
- 239000007921 spray Substances 0.000 claims description 19
- 238000001514 detection method Methods 0.000 claims description 16
- 238000001035 drying Methods 0.000 claims description 11
- 230000000007 visual effect Effects 0.000 claims description 5
- 238000009736 wetting Methods 0.000 claims description 5
- 239000000047 product Substances 0.000 description 37
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 10
- 238000004519 manufacturing process Methods 0.000 description 9
- 238000005266 casting Methods 0.000 description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 7
- 229910052710 silicon Inorganic materials 0.000 description 7
- 239000010703 silicon Substances 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 4
- 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
- 235000013399 edible fruits Nutrition 0.000 description 3
- 230000000694 effects Effects 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
- 238000007711 solidification Methods 0.000 description 3
- 230000008023 solidification Effects 0.000 description 3
- 239000000919 ceramic Substances 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
- 239000010453 quartz Substances 0.000 description 2
- 239000002210 silicon-based material Substances 0.000 description 2
- 239000004575 stone Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 230000009286 beneficial effect Effects 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
- 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
- 239000000178 monomer Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000011505 plaster Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000007634 remodeling 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
- 239000000243 solution 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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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- Investigating Materials By The Use Of Optical Means Adapted For Particular Applications (AREA)
- Analysing Materials By The Use Of Radiation (AREA)
Abstract
The invention discloses a kind of crack defect method of inspection of silica crucible finished product, dried silica crucible is carried out after the drifting dust processing of surface, with the watering can equipped with pure water, crucible Examination region is sprayed water, while printing opacity irradiation is carried out with 500W iodine-tungsten lamp finds crackle present in crucible to check.The present invention can accurately have found blind crack, simple and quick, efficiency high.
Description
Technical field
The present invention relates to a kind of silica crucible quality detecting method, more particularly to a kind of silica crucible finished product
The crack defect method of inspection.
Background technology
Silica crucible is the container for producing polycrystalline silicon ingot casting, is that polycrystalline is removed in polysilicon production process
The maximum running stores of the outer consumption of silicon raw material.Its production technology difficulty is big, material purity requires high, made
It is harsh with environment, disposable at a high temperature of 1550 DEG C continuously to work more than 50 hours, be polysilicon
Irreplaceable crucial consumable material in production process.In addition, in face of high-purity polycrystalline silicon raw material for not
The situation that should be asked, the melting that many countries have all carried out polycrystalline silicon raw material according to polycrystalline silicon ingot casting principle is carried
Pure work, silica crucible has also played the effect of no less important wherein.Therefore, it is with polysilicon light
Volt industry has the inseparable, relation of interdependence.As the production Technology of silica crucible,
It is general to have injection forming and two kinds of solidification forming of note.Slip-casting shaping process is the traditional forming technique of quartz,
I.e. the high-performance quartz ceramic mud modulated, injection forming obtains product, state granddad in plaster mold
Department typically uses the technique.Casting molding technique be added in quartz-ceramics mud a kind of organic monomer,
Directly solidification obtains product after being molded in non-punch die.Two kinds of technologies respectively have feature, injection forming production
Product density is slightly higher, wearability is good, is adapted to roll, the square solid product of manufacture simple shape, note
Solidification forming product gas porosity is slightly higher, thermal shock resistance more preferable, is adapted to the complex-shaped thin wall shape of manufacture empty
Core product.
Square silica crucible is used in during polycrystalline silicon ingot casting, under high temperature (1400 DEG C -1550 DEG C)
By the solar-grade high-purity polycrystalline silicon block material being loaded into crucible, one big whole ingot is fused into, then lead to
Cross post-production and silicon ingot evolution, section etc. are made to last solar battery sheet.Crucible is used as silicon material
Container, have very strict requirement in terms of quality.If crucible in ingot casting with the presence of crackle,
As the softening of crucible material at high temperature is acted on plus the pressure of silicon material, crackle can expand, so as to make
Leaked out into silicon liquid from crack, the silicon liquid of high temperature can produce corrosion to the graphite protective plate of crucible periphery
Penetrate, and may finally leak in ingot furnace, extremely hazardous infringement is caused to casting unit.Cause
This, crucible is using preceding having to pass through carefully strict quality restriction, it is ensured that do not have crackle to deposit in crucible
.
The content of the invention
, can be accurate it is an object of the invention to provide a kind of crack defect method of inspection of silica crucible finished product
Really find blind crack, simple and quick, efficiency high.
The technical solution adopted for the present invention to solve the technical problems is：
A kind of crack defect method of inspection of silica crucible finished product, comprises the following steps：
(1) by silica crucible finished product drying process；
(2) the silica crucible finished product after drying process is positioned on inspection desk, it is clean with air gun drifting dust；
(3) with equipped with pure water watering can to drifting dust processing after silica crucible finished product plan detection zone spray water with
Fully detection zone is intended in wetting, while the another side corresponding in silica crucible finished product water spray face is used
500W iodine-tungsten lamps carry out printing opacity irradiation, whether have 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 whole silica crucible finished product.
The corresponding another side in water spray face refers to being separated by with water spray face the face of silica crucible wall thickness, i.e.,
If water spray face is a certain region of lateral surface, corresponding another side is silica crucible medial surface
Corresponding region.Centered on silica crucible wall, water spray face is located at respectively with corresponding another side
The both sides of silica crucible wall.
The creation point of the present invention is with pure water as crack detection agent, coordinates 500W iodine-tungsten lamp printing opacities
Irradiation, to detect whether to have crackle.Pure water will not bring extra dirt into first as crack detection agent
Thing is contaminated, secondly, pure water does not have color, the silica crucible of white will not be polluted.Conventional crack detection
Major light is often used alone, the defect so existed is that often larger crackle is easily found,
And less crackle because major light transmit after color and surrounding without notable difference, naked eyes are difficult
To differentiate, these fine cracks are caused to be difficult to be found.And present invention pure water is as crack detection agent,
The irradiation collaboration of 500W iodine-tungsten lamps printing opacity is coordinated to play a role, after pure water first permeates to silica crucible, such as
There are fine cracks in fruit, water can be penetrated into crack, then be irradiated with red iodine-tungsten lamp printing opacity is shown, in folding
Penetrate under effect, obvious white occurs in fine cracks, and the region of surrounding normal still shows red,
So can fairly simple, the accurate presence for finding crackle.
Preferably, moisture content≤0.1% of step (1) drying process to silica crucible finished product.Control is square
The moisture content of silica crucible green compact is not higher than 0.1% very crucial, and such pure water can permeate rapidly, faster
It is more convenient for crack detection, 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 is：Resistivity is in more than 2M Ω .cm.Control
Pure water resistivity processed is in 2M Ω .cm the above object：The metal ion content in water is controlled, these
Metal ion can produce pollution to product, influence the crystal ingot quality after final ingot casting, therefore to control.
The beneficial effects of the invention are as follows：Blind crack, simple and quick, efficiency high can accurately be found.
Embodiment
Below by specific embodiment, technical scheme is described in further detail.
In the present invention, if not refering in particular to, raw material and equipment used etc. is commercially available or this
What field was commonly used.Method in following embodiments, is the routine side of this area unless otherwise instructed
Method.
Implement global schema：
A kind of crack defect method of inspection of silica crucible finished product, comprises the following steps：
(1) by moisture content≤0.1% of silica crucible finished product drying process to silica crucible finished product.
(2) the silica crucible finished product after drying process is positioned on inspection desk, gas clean with air gun drifting dust
The air pressure of rifle drifting dust is 0.3~0.6Mpa.
(3) with equipped with pure water watering can to drifting dust processing after silica crucible finished product plan detection zone spray water with
Fully detection zone is intended in wetting, and the quality standard of pure water is：Resistivity is in more than 2M Ω .cm.Simultaneously
Printing opacity irradiation is carried out with 500W iodine-tungsten lamps in the corresponding another side in silica crucible finished product water spray face,
Whether there is 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 whole silica crucible finished product.
Required to carry out subsequent job judgement according to quality specification according to assay.
Case 1 is embodied
A kind of crack defect method of inspection of silica crucible finished product, comprises the following steps：
(1) by moisture content≤0.1% of silica crucible finished product drying process to silica crucible finished product.
(2) the silica crucible finished product after drying process is positioned on inspection desk, gas clean with air gun drifting dust
The air pressure of rifle drifting dust is 0.3Mpa.
(3) with equipped with pure water watering can to drifting dust processing after silica crucible finished product plan detection zone spray water with
Fully detection zone is intended in wetting, and the quality standard of pure water is：Resistivity is in 3.5M Ω .cm.Simultaneously in stone
The corresponding another side of English crucible finished product water spray face (silica crucible medial surface) is (on the outside of silica crucible
Face) printing opacity irradiation is carried out with 500W iodine-tungsten lamps, whether there is crackle with visual method inspection water spray face.
Mobile watering can and iodine-tungsten lamp tie all inspections one time of the surfaces externally and internally of whole crucible according to examining
Fruit requires to carry out subsequent job judgement according to quality specification.
Case 2 is embodied
A kind of crack defect method of inspection of silica crucible finished product, comprises the following steps：
(1) by moisture content≤0.1% of silica crucible finished product drying process to silica crucible finished product.
(2) the silica crucible finished product after drying process is positioned on inspection desk, gas clean with air gun drifting dust
The air pressure of rifle drifting dust is 0.6Mpa.
(3) with equipped with pure water watering can to drifting dust processing after silica crucible finished product plan detection zone spray water with
Fully detection zone is intended in wetting, and the quality standard of pure water is：Resistivity is in 4M Ω .cm.Simultaneously in stone
The corresponding another side of English crucible finished product water spray face (silica crucible lateral surface) is (on the inside of silica crucible
Face) printing opacity irradiation is carried out with 500W iodine-tungsten lamps, whether there is crackle with visual method inspection water spray face.
Mobile watering can and iodine-tungsten lamp tie all inspections one time of the surfaces externally and internally of whole crucible according to examining
Fruit requires to carry out subsequent job judgement according to quality specification.
Effect judges：
According to the present invention method to silica crucible product inspection after, carry out polycrystalline silicon ingot casting production, investigate leakage
Silicon rate, leakage silicon rate standard is less than 0.2% for leakage silicon rate.
Result of the test：
From upper table result data, after method of the invention is to silica crucible product inspection, can effectively it examine
The blind crack tested out in crucible, it is ensured that crucible has high-quality.
Embodiment described above is a kind of preferably scheme of the present invention, and not the present invention is appointed
What formal limitation, it is also other on the premise of without departing from the technical scheme described in claim
Variant and remodeling.
Claims (4)
1. a kind of crack defect method of inspection of silica crucible finished product, it is characterised in that comprise the following steps：
(1) by silica crucible finished product drying process；
(2) the silica crucible finished product after drying process is positioned on inspection desk, it is clean with air gun drifting dust；
(3) with equipped with pure water watering can to drifting dust processing after silica crucible finished product plan detection zone spray water with
Fully detection zone is intended in wetting, while the another side corresponding in silica crucible finished product water spray face is used
500W iodine-tungsten lamps carry out printing opacity irradiation, whether have 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 whole silica crucible finished product.
2. the crack defect method of inspection according to claim 1, it is characterised in that：Step (1) is done
It is dry to handle to moisture content≤0.1% of silica crucible finished product.
3. the crack defect method of inspection according to claim 1 or 2, it is characterised in that：Step (2)
The air pressure of air gun drifting dust is 0.3~0.6Mpa.
4. the crack defect method of inspection according to claim 1 or 2, it is characterised in that：Step (3)
The quality standard of the pure water is：Resistivity is in more than 2M Ω .cm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| 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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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610024316.3A CN106970081B (en) | 2016-01-14 | 2016-01-14 | A kind of crack defect method of inspection of silica crucible finished product |
Publications (2)
| Publication Number | Publication Date |
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| CN106970081A true CN106970081A (en) | 2017-07-21 |
| CN106970081B CN106970081B (en) | 2019-09-03 |
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| CN201610024316.3A Active 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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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111308866A (en) * | 2020-04-01 | 2020-06-19 | 烟台核晶陶瓷新材料有限公司 | Developing solution for crucible detection and preparation method and use method thereof |
| 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 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| CN111308866A (en) * | 2020-04-01 | 2020-06-19 | 烟台核晶陶瓷新材料有限公司 | Developing solution for crucible detection and preparation method and use 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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| CN106970081B (en) | 2019-09-03 |
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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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