CN102312185A - Amorphous ceramic coated crucible and preparation method thereof - Google Patents
Amorphous ceramic coated crucible and preparation method thereof Download PDFInfo
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- CN102312185A CN102312185A CN201110185256A CN201110185256A CN102312185A CN 102312185 A CN102312185 A CN 102312185A CN 201110185256 A CN201110185256 A CN 201110185256A CN 201110185256 A CN201110185256 A CN 201110185256A CN 102312185 A CN102312185 A CN 102312185A
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Abstract
The invention relates to an amorphous ceramic coated crucible and a preparation method thereof. An inner wall of the amorphous ceramic coated crucible is coated with an amorphous ceramic film. The preparation method comprises the following steps of a, carrying out high-melting point ceramic powder spray granulation, wherein a particle size is controlled in a range of 15 to 60 micrometers and a particle micro-morphology is spherical or ellipsoidal, and b, carrying out amorphous coating thermal-spraying preparation. The amorphous ceramic coated crucible has the advantages that an amorphous compact film prepared form high-melting point powder by thermal spraying has porosity less than 5% and film thickness greater than 50 micrometers; an obvious diffraction peak cannot be observed under X-ray diffraction; and an electron probe shows that a nitrogen atom proportion is greater than 40%.
Description
Technical field
The present invention relates to a kind of amorphous phase ceramic coating crucible and preparation method.
Background technology
The sun power industry is diffused into the minority carrier life time of the serious restriction of the metallic element diffusion product of silicon material from crucible in crystal pulling and ingot casting process, and finally influences the performance of battery.Fine and close amorphous ceramic film has stronger ion diffusion barrier ability.Method for manufacturing thin film has following several kinds usually:
1. the chemical Vapor deposition process of amorphous silicon nitride: this method is a kind of sophisticated method for manufacturing thin film, and the film of this method preparation is evenly fine and close, but sedimentation velocity is limited, and thickness is that nano level is to several microns usually.
2. atomizing spraying sintering process: with crucible and coating sintering together, the softening temperature of crucible itself has limited the selection of machinable material, is not suitable for preparing the dense coating of materials with high melting point.
3. flame plating: flame plating relatively is fit to the coating prepn of materials with high melting point, and can introduce element such as oxygen carbon inevitably, therefore is not suitable for preparing the coating responsive to oxygen carbon.
4. thermal plasma spraying: the same coating prepn that relatively is fit to materials with high melting point with flame plating stops that at element the diffusion coating preparation field mainly concentrates on metal finishing at present.
Summary of the invention
Technical problem to be solved by this invention is: a kind of amorphous phase ceramic coating crucible and preparation method are provided, reduce being diffused into the metallic element the silicon material from crucible.
The present invention solves the scheme that its technical problem adopts: a kind of amorphous phase ceramic coating crucible, its inwall at crucible has the amorphous ceramic film.
A kind of preparation method of amorphous phase ceramic coating crucible, process is following:
A, HMP ceramic powder mist projection granulating, particle diameter is controlled at 15-60 μ m, and microscopic appearance is sphere or elliposoidal;
B, thermospray prepare amorphous coating.
The HMP ceramic powder is silicon nitride, SP 1, zirconium white or barium zirconate HMP ceramic powder in a process, powder median size 1 μ m, and purity is more than 99.99%.
Adopt plasma spraying and flame plating technology to carry out thermospray in the b process.
The b process need continue with nitrogen the crucible inwall to be cooled off when implementing.
The processing parameter of plasma spray coating process is: spraying current 550A, spray voltage 60V; Main gas Ar, pressure 0.55MPa, flow 40L/min; Spray distance 100mm, powder feeding gas N2, pressure 0.3MPa, flow 7L/min; Spray gun translational speed 100mm/s, spraying pass 6 times.
The processing parameter of flame plating technology is: oxygen flow 166.7L/min, combustion gas propane flow 20L/min, spray distance 120mm, powder feeding nitrogen pressure 0.6MPa, powder feeding nitrogen flow 10L/min, spray gun translational speed 100/min, spraying pass 4 times.
The invention has the beneficial effects as follows: adopt the non-crystalline state dense film of HMP powder through the thermospray preparation, its void content is less than 5%, and film thickness is greater than 50 μ m, and X-ray diffraction can not be observed obvious diffraction peak.Electronic probe shows that nitrogen element atomic ratio is greater than 40%.
Embodiment
Embodiment 1:
The spraying substrate is a solar energy polycrystal ingot casting side crucible, inwall size 840 * 840 * 420mm, staple quartzy (more than 99.5%); The spraying starting material are the high purity silicon nitride powder, median size 1 μ m, purity 99.99%.
The preparation process is following:
1. the suspension spray granulation that this powder and DI water is mixed with, the granularity of further sieving into 15-60 μ m again is so that powder feeding.
2. implement the thermal plasma spraying at above-mentioned crucible inwall, spray parameters is: spraying current 550A, spray voltage 60V; Main gas (Ar) pressure 0.55MPa, flow 40L/min; Spray distance 100mm, powder feeding gas (N
2) pressure 0.3MPa, flow 7L/min; Spray gun translational speed 100mm/s, spraying pass 6 times; Preparation coat-thickness 200 μ m.
3. continue in the spraying process crucible inwall to be cooled off with nitrogen.
Under these conditions, underlayer temperature is no more than 500 ℃ during spraying.
Embodiment 2:
The spraying substrate is a solar energy polycrystal ingot casting side crucible, inwall size 840 * 840 * 420mm, staple quartzy (more than 99.5%); The spraying starting material are high-purity SP 1 powder, median size 1 μ m, purity 99.99%.
Other processes are identical with embodiment 1
Embodiment 3:
The spraying substrate is a solar energy polycrystal ingot casting side crucible, inwall size 840 * 840 * 420mm, staple quartzy (more than 99.5%); The spraying starting material are the high purity silicon nitride powder, median size 1 μ m, purity 99.99%.
The preparation process is following:
1. the suspension spray granulation that this powder and DI water is mixed with, the granularity of further sieving into 15-60 μ m again is so that powder feeding
2. above-mentioned crucible is implemented flame plating, its concrete parameter is: oxygen flow 166.7L/min, combustion gas propane flow 20L/min; Spray distance 120mm, powder feeding nitrogen pressure 0.6MPa, powder feeding nitrogen flow 10L/min; Spray gun translational speed 100/min, spraying pass 4 times.
3. continue in the spraying process crucible inwall to be cooled off with nitrogen.Cool nitrogen pressure 0.8MPa, flow velocity 0.5L/min.
Under these conditions, underlayer temperature is no more than 500 ℃ during spraying.
Claims (7)
1. amorphous phase ceramic coating crucible, it is characterized in that: the inwall at crucible has the amorphous ceramic film.
2. the preparation method of the described amorphous phase ceramic coating of claim 1 crucible, it is characterized in that: process is following:
A, HMP ceramic powder mist projection granulating, particle diameter is controlled at 15-60 μ m, and microscopic appearance is sphere or elliposoidal;
B, thermospray prepare amorphous coating.
3. the preparation method of amorphous phase ceramic coating crucible according to claim 2; It is characterized in that: the HMP ceramic powder is silicon nitride, SP 1, zirconium white or barium zirconate HMP ceramic powder in the described a process; Powder median size 1 μ m, purity is more than 99.99%.
4. the preparation method of amorphous phase ceramic coating crucible according to claim 2 is characterized in that: adopt plasma spraying and flame plating technology to carry out thermospray in the described b process.
5. the preparation method of amorphous phase ceramic coating crucible according to claim 3 is characterized in that: described b process need continue with nitrogen the crucible inwall to be cooled off when implementing.
6. the preparation method of amorphous phase ceramic coating crucible according to claim 3 is characterized in that: the processing parameter of described plasma spray coating process is: spraying current 550A, spray voltage 60V; Main gas Ar, pressure 0.55MPa, flow 40L/min; Spray distance 100mm, powder feeding gas N2, pressure 0.3MPa, flow 7L/min; Spray gun translational speed 100mm/s, spraying pass 6 times.
7. the preparation method of amorphous phase ceramic coating crucible according to claim 3; It is characterized in that: the processing parameter of described flame plating technology is: oxygen flow 166.7L/min, combustion gas propane flow 20L/min, spray distance 120mm; Powder feeding nitrogen pressure 0.6MPa; Powder feeding nitrogen flow 10L/min, spray gun translational speed 100/min, spraying pass 4 times.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201110185256A CN102312185A (en) | 2011-07-04 | 2011-07-04 | Amorphous ceramic coated crucible and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201110185256A CN102312185A (en) | 2011-07-04 | 2011-07-04 | Amorphous ceramic coated crucible and preparation method thereof |
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| CN102312185A true CN102312185A (en) | 2012-01-11 |
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| CN201110185256A Pending CN102312185A (en) | 2011-07-04 | 2011-07-04 | Amorphous ceramic coated crucible and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102618707A (en) * | 2012-04-12 | 2012-08-01 | 郭亚辉 | Tool for metal thermal deformation process and production method |
| WO2013115726A1 (en) * | 2012-02-01 | 2013-08-08 | Memc Singapore Pte, Ltd. | Crucibles for holding molten material and methods for producing them and for their use |
| CN103979979A (en) * | 2014-05-05 | 2014-08-13 | 华东师范大学 | Method for preparing barium zirconate crucible by slip casting |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5916969A (en) * | 1982-07-19 | 1984-01-28 | Sumitomo Electric Ind Ltd | Boron nitride coated parts |
| US20030183161A1 (en) * | 2002-03-29 | 2003-10-02 | Japan Super Quartz Corporation | Surface modified quartz glass crucible and its modification process |
| CN101590525A (en) * | 2009-07-02 | 2009-12-02 | 哈尔滨工业大学 | Amorphous-nanocrystalline ceramic composite powder and preparation method thereof |
| CN101660115A (en) * | 2009-09-18 | 2010-03-03 | 武汉理工大学 | Preparation method of nanometer zirconia heat barrier coating |
| CN102041467A (en) * | 2010-12-07 | 2011-05-04 | 华中科技大学 | Hydrophobic amorphous alloy coating and preparation method thereof |
-
2011
- 2011-07-04 CN CN201110185256A patent/CN102312185A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5916969A (en) * | 1982-07-19 | 1984-01-28 | Sumitomo Electric Ind Ltd | Boron nitride coated parts |
| US20030183161A1 (en) * | 2002-03-29 | 2003-10-02 | Japan Super Quartz Corporation | Surface modified quartz glass crucible and its modification process |
| CN101590525A (en) * | 2009-07-02 | 2009-12-02 | 哈尔滨工业大学 | Amorphous-nanocrystalline ceramic composite powder and preparation method thereof |
| CN101660115A (en) * | 2009-09-18 | 2010-03-03 | 武汉理工大学 | Preparation method of nanometer zirconia heat barrier coating |
| CN102041467A (en) * | 2010-12-07 | 2011-05-04 | 华中科技大学 | Hydrophobic amorphous alloy coating and preparation method thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2013115726A1 (en) * | 2012-02-01 | 2013-08-08 | Memc Singapore Pte, Ltd. | Crucibles for holding molten material and methods for producing them and for their use |
| CN102618707A (en) * | 2012-04-12 | 2012-08-01 | 郭亚辉 | Tool for metal thermal deformation process and production method |
| CN103979979A (en) * | 2014-05-05 | 2014-08-13 | 华东师范大学 | Method for preparing barium zirconate crucible by slip casting |
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Application publication date: 20120111 |