CN107573101B - Crucible and preparation method thereof - Google Patents
Crucible and preparation method thereof Download PDFInfo
- Publication number
- CN107573101B CN107573101B CN201710822379.8A CN201710822379A CN107573101B CN 107573101 B CN107573101 B CN 107573101B CN 201710822379 A CN201710822379 A CN 201710822379A CN 107573101 B CN107573101 B CN 107573101B
- Authority
- CN
- China
- Prior art keywords
- coating
- silicon nitride
- nitride powder
- mixed
- crucible
- 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.)
- Expired - Fee Related
Links
- 238000002360 preparation method Methods 0.000 title abstract description 15
- 239000011248 coating agent Substances 0.000 claims abstract description 123
- 238000000576 coating method Methods 0.000 claims abstract description 123
- 239000013078 crystal Substances 0.000 claims abstract description 55
- 239000011247 coating layer Substances 0.000 claims abstract description 26
- 239000012535 impurity Substances 0.000 claims abstract description 12
- 230000006911 nucleation Effects 0.000 claims abstract description 11
- 238000010899 nucleation Methods 0.000 claims abstract description 11
- 239000002184 metal Substances 0.000 claims abstract description 10
- 238000009792 diffusion process Methods 0.000 claims abstract description 6
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 93
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 93
- 239000000843 powder Substances 0.000 claims description 63
- 238000002156 mixing Methods 0.000 claims description 35
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 20
- 239000002002 slurry Substances 0.000 claims description 20
- 239000002245 particle Substances 0.000 claims description 19
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 14
- 239000011268 mixed slurry Substances 0.000 claims description 12
- 239000004570 mortar (masonry) Substances 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 7
- 239000010410 layer Substances 0.000 claims description 6
- 125000004430 oxygen atom Chemical group O* 0.000 claims description 6
- 239000010453 quartz Substances 0.000 claims description 4
- 239000006004 Quartz sand Substances 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 238000005245 sintering Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 229910021420 polycrystalline silicon Inorganic materials 0.000 abstract description 12
- 238000005266 casting Methods 0.000 description 6
- 210000004027 cell Anatomy 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- 230000007547 defect Effects 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000001125 extrusion Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000011241 protective layer Substances 0.000 description 2
- 239000004576 sand Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 210000001787 dendrite Anatomy 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
Images
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention provides a crucible and a preparation method thereof, wherein the crucible comprises: a crucible body including a bottom wall and a side wall; a first coating layer provided on the bottom wall and the side wall for preventing diffusion of metal impurities into crystal grains located in the crucible body; a second coating disposed over the first coating on the sidewall, the second coating for assisting in nucleation of grains located within the crucible body; and a third coating disposed on the bottom wall outside the first coating, the third coating being for assisting a crystal located within the crucible body to detach from the crucible body. The crucible can effectively reduce the diffusion of metal impurities in the crucible body to polycrystalline crystals in the crucible body, so that the prepared polycrystalline silicon has high purity.
Description
Technical Field
The invention relates to a crucible, in particular to a crucible for preparing polycrystalline silicon and a preparation method thereof.
Background
In recent years, with the increasing exhaustion of non-renewable energy sources, solar cells have been rapidly developed. Because the preparation process of the cast polycrystalline silicon is relatively simple and the cost is far lower than that of monocrystalline silicon, the polycrystalline silicon gradually replaces the leading position of czochralski silicon in the solar cell material market and becomes the most important photovoltaic material in the industry. However, various defects in the cast polycrystalline silicon, such as grain boundaries, dislocations, microdefects, and impurities of carbon and oxygen in the material, make the conversion efficiency of the polycrystalline silicon solar cell lower than that of the czochralski single crystal silicon solar cell, which is a bottleneck limiting the development of the polycrystalline silicon solar cell, compared to the czochralski single crystal silicon. The inherent quality of the polycrystalline silicon wafer has a direct influence on the final battery conversion efficiency, and the improvement of the inherent quality of the polycrystalline silicon wafer is an important means for improving the battery conversion efficiency. The intrinsic quality of a polycrystalline silicon wafer depends on the quality of the polycrystalline crystal before it is cut to shape. Therefore, it is a research direction of companies to improve the technology of polycrystalline silicon ingot casting and obtain high-quality polycrystalline crystals.
Currently, various methods are commonly used in the industry to achieve uniform small grains during bottom initial nucleation. Although each large company in the industry has its own method for realizing uniform small grains, the idea is basically consistent, and mainly uses a quartz crucible with rough quartz sand particles at the bottom, and uses cold impact to increase nucleation amount at the primary stage of crystal growth, so as to obtain uniform small grains with a certain size.
However, the crucible and various crystal founders in the market at present focus on solving the nucleation problem of small polycrystal at the bottom, neglect that the side part of the crucible is relatively compact due to the smoothly sprayed silicon nitride powder, the side part can also nucleate in the ingot casting process, and because an excellent nucleation condition similar to the bottom is not created, the initial nucleation is random and free, is not an optimized crystal grain and crystal orientation, and has different crystal grain sizes and high local defect density, and the large dendrite generated at the side part can extrude the excellent columnar crystal at the bottom, or the growth direction of the original columnar crystal is changed, so that the columnar crystal grows obliquely, dislocation propagation is increased, or the excellent crystal at the bottom is phagocytosed, so that the excellent crystal at the bottom fails in competitive growth, and the effect of a high-efficiency layer at the bottom is weakened. And if the side silicon nitride coating is sprayed relatively loosely and unevenly during spraying, although conditions are created for nucleation of small crystal grains on the side, metal impurities in the crucible body far exceed those in silicon nitride and silicon materials, and the loose silicon nitride coating can be diffused continuously in an image crystal, so that the red area on the side of the silicon wafer is wider.
Disclosure of Invention
The invention aims to provide a crucible capable of preparing high-purity polycrystalline silicon and a preparation method of the crucible.
In order to solve the above problems, the present invention provides a crucible comprising:
a crucible body including a bottom wall and a side wall;
a first coating layer provided on the bottom wall and the side wall for preventing diffusion of metal impurities into crystal grains located in the crucible body;
a second coating disposed over the first coating on the sidewall, the second coating for assisting in nucleation of grains located within the crucible body; and
and the third coating is arranged outside the first coating on the bottom wall and is used for assisting the crystal in the crucible body to be separated from the crucible body.
Preferably, the first coating is a quartz sand layer;
the second coating is formed by silicon nitride slurry formed by mixing mixed silicon nitride powder, silica sol and water according to the mass ratio of 2:1:6, wherein the mixed silicon nitride powder is formed by mixing alpha-phase silicon nitride powder with the particle size of 1-3 mu m and beta-phase silicon nitride powder with the particle size of 13-15 mu m according to the mass ratio of 1:1-1: 1.5;
the third coating is formed by silicon nitride slurry formed by mixing mixed silicon nitride powder, silica sol and water according to the mass ratio of 2:1:6, wherein the mixed silicon nitride powder is formed by mixing alpha-phase silicon nitride powder with the particle size of 1.5-2 mu m and beta-phase silicon nitride powder with the particle size of 2.5-3 mu m according to the mass ratio of 1:1-1: 1.5.
Preferably, a fourth coating is further disposed between the first coating and the third coating, and the fourth coating is used for preventing oxygen atoms in the first coating from diffusing into crystals.
Preferably, the fourth coating is formed by mixing silica sol and silicon nitride particles with the diameter of 50 meshes to 70 meshes according to the mass ratio of 2: 1.
The invention also provides a preparation method of the crucible, which comprises the following steps:
step 1: preparing a crucible body;
step 2: coating quartz mortar on the bottom wall and the side wall of the crucible body to form a first coating;
and step 3: coating silicon nitride slurry on the first coating layer positioned on the side wall to form a second coating layer;
and 4, step 4: coating a silicon nitride slurry over the first coating on the bottom wall to form a third coating;
and 5: and drying the crucible body in the step 4.
Preferably, the preparation method of the silicon nitride slurry in the step 3 comprises the following steps:
mixing alpha-phase silicon nitride powder with the grain diameter of 1-3 mu m and beta-phase silicon nitride powder with the grain diameter of 13-15 mu m according to the mass ratio of 1:1-1:1.5 to form mixed silicon nitride powder;
mixing the mixed silicon nitride powder, silica sol and water according to the mass ratio of 2:1:6 to form mixed slurry;
and stirring the mixed slurry at the temperature of 25-30 ℃ for 0.5-1 h.
Preferably, the preparation method of the silicon nitride slurry in the step 4 comprises the following steps:
mixing alpha-phase silicon nitride powder with the grain diameter of 1.5-2 mu m and beta-phase silicon nitride powder with the grain diameter of 2.5-3 mu m according to the mass ratio of 1:1-1:1.5 to form mixed silicon nitride powder;
mixing the mixed silicon nitride powder, silica sol and water according to the mass ratio of 2:1:6 to form mixed slurry;
and stirring the mixed slurry at the temperature of 25-30 ℃ for 0.5-1 h.
Preferably, a fourth coating layer is further applied between the first coating layer and the third coating layer, and the fourth coating layer is used for avoiding oxygen atoms in the first coating layer from diffusing into crystals.
Preferably, the preparation method of the fourth coating is as follows: mixing silica sol and silicon nitride particles with the diameter of 50 meshes to 70 meshes according to the mass ratio of 2:1, stirring for 0.5h to 1h at the temperature of 25 ℃ to 30 ℃ to form mixed mortar, coating the mixed mortar on the first coating positioned outside the bottom wall, and sintering for 1h to 2h at the temperature of 100 ℃ to 600 ℃ to form the fourth coating.
Preferably, the second coating layer and the third coating layer are coated by a crisscross method.
The crucible and the preparation method thereof have the beneficial effects that:
1. make the crucible body do benefit to the polycrystal ingot casting through setting up first coating, and can effectively reduce the metallic impurity in the crucible body to be located this internal polycrystalline crystal of crucible and spread.
2. The second coating is arranged, so that conditions are provided for nucleation of the lateral small grains during polycrystalline ingot casting, the defect density of the lateral small grains is low, the extrusion acting force on the bottom columnar crystal is small, and better vertical growth conditions are provided for the bottom columnar crystal.
3. The second coating and the third coating are both formed by mixing alpha-phase silicon nitride powder and beta-phase silicon nitride powder, and the alpha-phase silicon nitride powder is in a granular structure, and the beta-phase silicon nitride powder is in a needle-shaped structure, so that the combined silicon nitride powder has more advantages in a space structure, and the structure of the silicon nitride coating can be more compact. Meanwhile, the bonding strength of the third coating and the second coating can be greatly improved, a compact protective layer is formed, metal impurities in the crucible body can be prevented from diffusing into polycrystalline crystals, and the second coating and the third coating can be prevented from falling off to pollute the crystals in the polycrystalline crystal charging and ingot casting processes.
4. The fourth coating can avoid the reaction of the first coating and the third coating, increase the oxygen content in the prepared polycrystalline crystal and influence the quality of the polycrystalline crystal.
5. The second coating and the third coating are arranged in a coating mode by adopting a cross method, so that the structure layer formed on the inner surface of the crucible body is more uniform and compact, the metal impurities in the crucible body can be more effectively prevented from diffusing into the polycrystalline crystal to pollute the polycrystalline crystal, and meanwhile, the red area on the side part of the polycrystalline crystal can be effectively reduced.
Drawings
FIG. 1 is a schematic view of the structure of a crucible of the present invention.
FIG. 2 is a flow chart of a method of making the crucible of the present invention.
Reference numerals:
1-crucible body; 2-a first coating; 3-a second coating; 4-a third coating; 5-fourth coating.
Detailed Description
The present invention is described in detail below with reference to the attached drawings.
As shown in fig. 1, the present invention provides a crucible, comprising:
a crucible body 1;
the first coating 2 is arranged on the bottom wall and the side wall of the crucible body 1 and is used for preventing metal impurities in the crucible body 1 from diffusing into crystals in the crucible body 1 and influencing the quality of the crystals;
the second coating 3 is arranged outside the first coating 2 on the side wall, and the second coating 3 is used for assisting the nucleation of small crystal grains on the side wall of the crucible body 1, so that the defect density of the small crystal grains on the side part is low, the extrusion acting force on the columnar crystals at the bottom is small, and a better vertical growth condition is provided for the columnar crystals at the bottom; and
a third coating 4 provided outside the first coating 2 on the bottom wall, the third coating 4 serving to assist the crystal grains located inside the crucible body 1 to come off the crucible body 1, i.e., to be demolded.
Further, the first coating layer 2 in this embodiment is a silica sand layer (which may be formed by mixing high-purity silica sand with water), and the second coating layer 3 is formed of a silicon nitride slurry in which silicon nitride powder, silica sol (which may be formed by mixing nano-scale silica with an additive) and water are mixed in a mass ratio of 2:1: 6. Wherein the mixed silicon nitride powder is formed by mixing alpha-phase silicon nitride powder with the particle size of 1-3 mu m and beta-phase silicon nitride powder with the particle size of 13-15 mu m according to the mass ratio of 1:1-1: 1.5; the third coating 4 is formed by silicon nitride slurry obtained by mixing silicon nitride powder, silica sol and water according to the mass ratio of 2:1: 6. Wherein the mixed silicon nitride powder is formed by mixing alpha-phase silicon nitride powder with the grain diameter of 1.5-2 mu m and beta-phase silicon nitride powder with the grain diameter of 2.5-3 mu m according to the mass ratio of 1:1-1: 1.5. The second coating layer 3 and the third coating layer 4 are both formed by mixing alpha-phase silicon nitride powder and beta-phase silicon nitride powder, and the alpha-phase silicon nitride powder is in a granular structure, and the beta-phase silicon nitride powder is in a needle-like structure, so that the combined silicon nitride powder is more advantageous in space structure, and the structures of the second coating layer 3 and the third coating layer 4 can be more compact. Meanwhile, the bonding strength of the third coating 4 and the second coating 3 can be greatly improved, a compact protective layer is formed, the diffusion of metal impurities in the crucible body 1 into crystals can be prevented, and the second coating 3 and the third coating 4 can be prevented from falling off to pollute the crystals in the processes of charging and ingot casting of the crystals.
Further, in the present embodiment, a fourth coating 5 is further disposed between the first coating 2 and the third coating 4. The purpose of the fourth coating 5 is mainly to prevent oxygen atoms in the first coating 2 from diffusing into crystal grains in the crucible body 1, thereby affecting the crystal quality, and simultaneously assisting in attracting the crystal grains to nucleate. The fourth coating in this example is formed by mixing silica sol with silicon nitride particles having a diameter of 50 mesh to 70 mesh in a mass ratio of 2: 1.
As shown in fig. 2, the present invention also provides a method for preparing a crucible, comprising:
step 1: preparing a crucible body 1;
step 2: coating quartz mortar on the bottom wall and the side wall of the crucible body 1 to form a first coating 2;
and step 3: coating silicon nitride slurry outside the first coating 2 on the side wall to form a second coating 3;
and 4, step 4: coating the first coating 2 on the bottom wall with a silicon nitride slurry to form a third coating 4;
and 5: and drying the crucible body 1 in the step 4.
The preparation method of the silicon nitride slurry in the step 3 comprises the following steps:
step a: mixing alpha-phase silicon nitride powder with the grain diameter of 1-3 mu m and beta-phase silicon nitride powder with the grain diameter of 13-15 mu m according to the mass ratio of 1:1-1:1.5 to form mixed silicon nitride powder;
step b: mixing the mixed silicon nitride powder, silica sol and water according to the mass ratio of 2:1:6 to form mixed slurry;
step c: the mixed slurry is stirred for 0.5h to 1h at the temperature of 25 ℃ to 30 ℃.
The preparation method of the silicon nitride slurry in the step 4 comprises the following steps:
step a: mixing alpha-phase silicon nitride powder with the grain diameter of 1.5-2 mu m and beta-phase silicon nitride powder with the grain diameter of 2.5-3 mu m according to the mass ratio of 1:1-1:1.5 to form mixed silicon nitride powder;
step b: mixing the mixed silicon nitride powder, silica sol and water according to the mass ratio of 2:1:6 to form mixed slurry;
step c: the mixed slurry is stirred for 0.5h to 1h at the temperature of 25 ℃ to 30 ℃.
Preferably, the second coating layer 3 and the third coating layer 4 are applied in a criss-cross method. By adopting the coating mode to arrange the second coating 3 and the third coating 4, the structure layer formed on the inner surface of the crucible body 1 is more uniform and compact, the metal impurities in the crucible body 1 can be more effectively prevented from diffusing into the crystal to pollute the crystal, and meanwhile, the red area on the side part of the crystal can be effectively reduced.
Further, the preparation method of the embodiment further comprises the step of coating a fourth coating 5 between the first coating 2 and the third coating 4, wherein the fourth coating 5 is used for preventing oxygen atoms in the first coating 2 from diffusing into crystals located in the crucible body 1 to increase the oxygen content of the crystals, and thus the quality of the crystals is influenced. Specifically, the preparation method of the fourth coating in this embodiment is: the coating is formed by mixing silica sol and silicon nitride particles with the diameter of 50 meshes to 70 meshes according to the mass ratio of 2:1, stirring for 0.5h to 1h at the temperature of 25 ℃ to 30 ℃ to form mixed mortar, coating the mixed mortar on a first coating 2 positioned outside a bottom wall, and sintering for 1h to 2h at the temperature of 100 ℃ to 600 ℃.
The above embodiments are only exemplary embodiments of the present invention, and are not intended to limit the present invention, and the scope of the present invention is defined by the claims. Various modifications and equivalents may be made by those skilled in the art within the spirit and scope of the present invention, and such modifications and equivalents should also be considered as falling within the scope of the present invention.
Claims (9)
1. A crucible, comprising:
a crucible body including a bottom wall and a side wall;
a first coating layer provided on the bottom wall and the side wall for preventing diffusion of metal impurities in the crucible body into crystal grains in the crucible body;
a second coating disposed over the first coating on the sidewall, the second coating for assisting in nucleation of grains located within the crucible body; and
a third coating disposed over the first coating on the bottom wall, the third coating for assisting crystals located within the crucible body to detach from the crucible body;
the first coating is a quartz sand layer, the second coating and the third coating are both formed by silicon nitride slurry formed by mixing silicon nitride powder, silica sol and water, and the particle sizes of the mixed silicon nitride powder in the second coating and the third coating are different;
the second coating is formed by silicon nitride slurry formed by mixing mixed silicon nitride powder, silica sol and water according to the mass ratio of 2:1:6, wherein the mixed silicon nitride powder is formed by mixing alpha-phase silicon nitride powder with the particle size of 1-3 mu m and beta-phase silicon nitride powder with the particle size of 13-15 mu m according to the mass ratio of 1:1-1: 1.5;
the third coating is formed by silicon nitride slurry formed by mixing mixed silicon nitride powder, silica sol and water according to the mass ratio of 2:1:6, wherein the mixed silicon nitride powder is formed by mixing alpha-phase silicon nitride powder with the particle size of 1.5-2 mu m and beta-phase silicon nitride powder with the particle size of 2.5-3 mu m according to the mass ratio of 1:1-1: 1.5.
2. The crucible of claim 1, further comprising a fourth coating disposed between the first coating and the third coating, the fourth coating configured to prevent oxygen atoms in the first coating from diffusing into the crystal.
3. The crucible of claim 2, wherein the fourth coating is formed by mixing silica sol and silicon nitride particles with a diameter of 50-70 mesh according to a mass ratio of 2: 1.
4. A method of preparing a crucible for use in a crucible as claimed in any one of claims 1 to 3, the method comprising:
step 1: preparing a crucible body;
step 2: coating quartz mortar on the bottom wall and the side wall of the crucible body to form a first coating;
and step 3: coating silicon nitride slurry on the first coating layer positioned on the side wall to form a second coating layer;
and 4, step 4: coating a silicon nitride slurry over the first coating on the bottom wall to form a third coating;
and 5: drying the crucible body in the step 4;
the silicon nitride slurry is formed by mixing mixed silicon nitride powder, silica sol and water, and the particle sizes of the mixed silicon nitride powder in the second coating and the third coating are different.
5. The method according to claim 4, wherein the silicon nitride slurry in step 3 is prepared by:
mixing alpha-phase silicon nitride powder with the grain diameter of 1-3 mu m and beta-phase silicon nitride powder with the grain diameter of 13-15 mu m according to the mass ratio of 1:1-1:1.5 to form mixed silicon nitride powder;
mixing the mixed silicon nitride powder, silica sol and water according to the mass ratio of 2:1:6 to form mixed slurry;
and stirring the mixed slurry at the temperature of 25-30 ℃ for 0.5-1 h.
6. The method according to claim 5, wherein the silicon nitride slurry in step 4 is prepared by:
mixing alpha-phase silicon nitride powder with the grain diameter of 1.5-2 mu m and beta-phase silicon nitride powder with the grain diameter of 2.5-3 mu m according to the mass ratio of 1:1-1:1.5 to form mixed silicon nitride powder;
mixing the mixed silicon nitride powder, silica sol and water according to the mass ratio of 2:1:6 to form mixed slurry;
and stirring the mixed slurry at the temperature of 25-30 ℃ for 0.5-1 h.
7. The production method according to claim 4, characterized in that a fourth coating layer for avoiding diffusion of oxygen atoms in the first coating layer into crystals is further applied between the first coating layer and the third coating layer.
8. The method of claim 7, wherein the fourth coating is prepared by: mixing silica sol and silicon nitride particles with the diameter of 50 meshes to 70 meshes according to the mass ratio of 2:1, stirring for 0.5h to 1h at the temperature of 25 ℃ to 30 ℃ to form mixed mortar, coating the mixed mortar on the first coating positioned outside the bottom wall, and sintering for 1h to 2h at the temperature of 100 ℃ to 600 ℃ to form the fourth coating.
9. The method of claim 4, wherein the second coating and the third coating are applied by a criss-cross method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710822379.8A CN107573101B (en) | 2017-09-13 | 2017-09-13 | Crucible and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710822379.8A CN107573101B (en) | 2017-09-13 | 2017-09-13 | Crucible and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107573101A CN107573101A (en) | 2018-01-12 |
| CN107573101B true CN107573101B (en) | 2020-12-01 |
Family
ID=61033379
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710822379.8A Expired - Fee Related CN107573101B (en) | 2017-09-13 | 2017-09-13 | Crucible and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107573101B (en) |
Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108301049A (en) * | 2018-03-23 | 2018-07-20 | 镇江环太硅科技有限公司 | A kind of preparation method of hypoxemia ingot casting silicon nitride coating |
| CN108455874A (en) * | 2018-03-27 | 2018-08-28 | 晶科能源有限公司 | A kind of painting layer manufacturing method thereof of polycrystalline silicon ingot casting silica crucible |
| CN108754602B (en) * | 2018-06-12 | 2020-10-27 | 山东大海新能源发展有限公司 | Crucible for polycrystalline silicon semi-molten ingot casting and spraying process and application thereof |
| CN108560048B (en) * | 2018-06-12 | 2020-10-27 | 山东大海新能源发展有限公司 | Crucible for polycrystalline silicon full-melting ingot casting and preparation method and application thereof |
| CN108486651A (en) * | 2018-06-28 | 2018-09-04 | 英利能源（中国）有限公司 | The preparation method and polycrystal silicon ingot of polycrystal silicon ingot |
| CN109111102A (en) * | 2018-11-02 | 2019-01-01 | 宁夏富乐德石英材料有限公司 | A kind of semiconductor grade silica crucible and its manufacturing method |
| CN111349967B (en) * | 2018-12-20 | 2022-03-18 | 比亚迪股份有限公司 | Efficient crucible and preparation method thereof |
| CN112064112B (en) * | 2020-09-15 | 2021-12-31 | 晶科能源股份有限公司 | Crucible, preparation method thereof and device for preparing silicon crystal |
| CN114773091B (en) * | 2022-03-17 | 2023-05-26 | 象山创亿金属制品有限公司 | Electric furnace crucible preparation process and processing equipment thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102400214A (en) * | 2010-09-16 | 2012-04-04 | 扬州华尔光电子材料有限公司 | Quartz crucible with composite coating layers for preparing polycrystalline silicon ingot |
| CN203485502U (en) * | 2013-07-30 | 2014-03-19 | 东海晶澳太阳能科技有限公司 | Quartz crucible coating for producing efficient polycrystalline silicon ingot |
| CN105133007A (en) * | 2015-09-12 | 2015-12-09 | 无锡舜阳新能源科技股份有限公司 | High-purity coating type polycrystalline silicon crucible |
| CN106277823A (en) * | 2016-08-26 | 2017-01-04 | 河北高富氮化硅材料有限公司 | A kind of grain size distribution improves the method for silicon nitride coating compactness |
| WO2017036822A1 (en) * | 2015-09-02 | 2017-03-09 | Alzchem Ag | Crucible for producing silicon ingots, method for its production and silicon ingot |
-
2017
- 2017-09-13 CN CN201710822379.8A patent/CN107573101B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102400214A (en) * | 2010-09-16 | 2012-04-04 | 扬州华尔光电子材料有限公司 | Quartz crucible with composite coating layers for preparing polycrystalline silicon ingot |
| CN203485502U (en) * | 2013-07-30 | 2014-03-19 | 东海晶澳太阳能科技有限公司 | Quartz crucible coating for producing efficient polycrystalline silicon ingot |
| WO2017036822A1 (en) * | 2015-09-02 | 2017-03-09 | Alzchem Ag | Crucible for producing silicon ingots, method for its production and silicon ingot |
| CN105133007A (en) * | 2015-09-12 | 2015-12-09 | 无锡舜阳新能源科技股份有限公司 | High-purity coating type polycrystalline silicon crucible |
| CN106277823A (en) * | 2016-08-26 | 2017-01-04 | 河北高富氮化硅材料有限公司 | A kind of grain size distribution improves the method for silicon nitride coating compactness |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107573101A (en) | 2018-01-12 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107573101B (en) | Crucible and preparation method thereof | |
| CN104018219B (en) | A kind of preparation method of narrow black surround high-efficiency polycrystalline silicon chip | |
| US10138572B2 (en) | Crystalline silicon ingot and method of fabricating the same | |
| TWI534307B (en) | Method of manufacturing crystalline silicon ingot | |
| CN104032368B (en) | A kind of preparation method of efficient polycrystal silicon ingot | |
| JP2014129228A (en) | Seed used for casting crystal silicon ingot | |
| TWI620838B (en) | Crystalline silicon ingot including nucleation promotion particles and method of fabricating the same | |
| KR101779267B1 (en) | Polycrystalline silicon ingot, method for producing the same, and crucible | |
| TWI493082B (en) | Method of fabricating crystalline silicon ingot | |
| CN107955970B (en) | Growth method of high-quality aluminum nitride single crystal | |
| JP5930637B2 (en) | Silicon nitride powder for mold release agent and method for producing the same | |
| CN103014852A (en) | Casting method of efficient polycrystalline silicon ingot | |
| CN103436959B (en) | The preparation method of polycrystalline silicon ingot casting | |
| JP2011524849A (en) | Germanium-enriched silicon material for solar cell manufacturing | |
| CN102041550A (en) | Method for prolonging service life of single crystal furnace thermal field crucible, and Czochralski crystal growing furnace | |
| CN206204475U (en) | A kind of crucible used for polycrystalline silicon ingot casting | |
| CN202898597U (en) | Crucible for silicon ingot | |
| CN114540951B (en) | Method for preparing polycrystalline silicon ingot by recycling silicon mud | |
| CN106986554B (en) | Manufacturing method of quartz crucible with ultra-pure coating | |
| TW201715097A (en) | Crucible for manufacturing silicon ingots, method of manufacturing same and silicon ingot | |
| CN107974710A (en) | The growing method of high-performance polycrystal silicon based on quartzy seed crystal | |
| CN203474952U (en) | Quartz crucible for ingot casting | |
| CN217499496U (en) | Quartz crucible of polycrystalline silicon ingot furnace | |
| CN103014834A (en) | Method for improving casting quality of polycrystalline silicon ingot | |
| CN102826737A (en) | Quartz ceramic crucible for producing high-efficiency polycrystals and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20201201 |