CN104926371A - Silicon steam corrosion resistant coating and preparation method thereof - Google Patents
Silicon steam corrosion resistant coating and preparation method thereof Download PDFInfo
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- CN104926371A CN104926371A CN201510311993.9A CN201510311993A CN104926371A CN 104926371 A CN104926371 A CN 104926371A CN 201510311993 A CN201510311993 A CN 201510311993A CN 104926371 A CN104926371 A CN 104926371A
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Abstract
The invention discloses a silicon steam corrosion resistant coating and a preparation method thereof. The coating is prepared from the following components in percentage by mass: 15-35% of hexagonal boron nitride, 1-10% of ethanol, 1-10% of glycerol and 50-80% of a diluent, wherein the total percentage of the components is 100%. The coating can be utilized for protecting a graphite crucible under the atmosphere of high-temperature silicon steam at 1700 DEG C or higher, so that the surface of the graphite crucible can be protected to a great extent, and the corrosion caused by the silicon steam is reduced; the coating can further be utilized for the surfaces of a heat preservation barrel, a heater and other main graphite toolings in addition to the crucible; moreover, the coating has the characteristics of being simple in technical process, low in cost, suitable for popularization and application, high in high-temperature property and harmless to a human body.
Description
Technical field
The present invention relates to anti-silicon vapor corrosion field, specifically a kind of preparation method of coating of anti-silicon vapor corrosion plumbago crucible.
Background technology
In China, the development of photovoltaic industry has driven the fast development of silicon industry as multiple in silicon single crystal, polysilicon etc.Current China production capacity has exceeded the over half of world's aggregated capacity.In these industries, generally relate to hot environment, so mostly adopt import isostatic pressing formed graphite or domestic three high graphite, need them to have the higher life-span, its major cause is that the price of photovoltaic industry constantly declines, and needs each industrial chain to reduce costs, and plumbago crucible is a very important frock, as main consumptive material, the life-span of improving plumbago crucible can be significantly reduced to this, so the life-span of how to improve plumbago crucible is an important issue.Successively carried out a large amount of research work for addressing this problem, CN102586754A provides a kind of method preparing boron nitride coating, and the method adopts chemical vapor deposition method, take nitrogen as shielding gas, with ammonia and gaseous state BCl
2for reaction gas, plumbago crucible deposits pyrolytic boron nitride coating layer, wherein, on matrix mould, the pyrolitic boron nitride precoated layer of 0.05 ~ 0.1mm is first deposited under temperature 1750 ~ 1850 DEG C of conditions, and isothermal holding is carried out to this precoated layer, then continue to be warmed up to 1800 ~ 2000 DEG C, prior art parameter reactive deposition pyrolytic boron nitride coating layer is pressed again on pyrolytic boron nitride coating layer, form boron nitride crucible goods, it is long, with high costs and affect comparatively large by equipment that the method prepares coating cycle, is unfavorable for application; CN103084325A discloses in a kind of method of crucible and coating thereof, disclosed coating formula comprises hexagonal boron nitride and pure water and tackiness agent, tackiness agent is silicon sol or polyvinyl alcohol, it is 1500 ~ 1600 DEG C that one of tackiness agent of this invention silicon sol bears high temperature, temperature is too high will lose cohesiveness, cause boron nitride coating to come off and lose protective effect, coating high-temp poor performance, and another kind of adhesive polyethylene alcohol sucks, takes in or is harmful to health after skin absorbs, there is hormesis to eyes and skin.
Summary of the invention
In order to overcome, the cost existed in prior art is high, high-temperature behavior is poor and to the disadvantageous deficiency of HUMAN HEALTH, the present invention proposes coating of a kind of anti-silicon vapor corrosion and preparation method thereof.
The present invention by 15 ~ 35% hexagonal boron nitride, the ethanol of 1 ~ 10%, the glycerol of 1 ~ 10% and 50 ~ 80% thinner, described per-cent is mass percent, and per-cent total amount is absolutely.
Described hexagonal boron nitride, purity content >=99%; Described purity of alcohol content >=99%; Described glycerol purity content >=99%; Described thinner is distilled water or deionized water.
The concrete steps of the coating of the described anti-silicon vapor corrosion of the preparation that the present invention proposes are:
Step 1, ratio weighs material;
Step 2, prepares solution: the thinner of weighing is put into beaker, in described beaker, add load weighted ethanol and glycerol.Be uniformly mixed after 30 ~ 35 DEG C are heated to described beaker; Obtain the solution mixed.
Step 3, prepares coating: being added by load weighted hexagonal boron nitride in the solution obtained and being stirred to solution becomes the pasty state that viscosity is 20 ~ 25s, obtains the coating prepared.
Step 4, the pH value of adjustment solution: add NaOH in the coating obtained, to adjust the pH value of solution, make pH=8 ~ 11 of solution.
Step 5, preparation coating: evenly brushed by the coating of pH value=8 ~ 11 and to clean up and the plumbago crucible of drying is surperficial, and under being placed in normal temperature, make brushing at the coating natural air drying of this crucible surface, forms at this crucible surface the coating that anti-silicon vapor corrodes.
When preparing solution and when preparing coating, the rotating speed of agitator is 200 ~ 280r/min, and churning time is 4 ~ 6min.
The coating of the anti-silicon vapor corrosion plumbago crucible that the present invention proposes protects the coating of plumbago crucible more than 1700 DEG C under high temperature silicon vapor atmosphere, plumbago crucible surface is protected significantly, reduce the corrosion of silicon vapor, also can use on main graphite frock surface at the insulated tank, well heater, crucible etc. that manufacture order crystal silicon is used; When cost increases little, these graphite frock life-spans can be made to improve 50% ~ 100%, the work-ing life of significant prolongation graphite frock, and have the advantages that technological process is simple and cost is low, be suitable for applying, high-temperature behavior is good, to human body without harm.
The present invention selects hexagonal boron nitride, and hexagonal boron nitride has the title of white graphite, has the laminate structure of class graphite, has good oilness, thermal conductivity, electrical insulating property and chemical resistance.Stable chemical nature is unreactiveness to all molten metals, fusing point is 3000 DEG C under nitrogen pressure, under atmospheric pressure 2500 DEG C of distillations, but and argon gas in use fusing point to be 3000 DEG C, 2700 DEG C are still stable under an argon atmosphere, in vacuum environment 1800 DEG C can life-time service, can slowly decompose more than 1800 DEG C for a long time.High-temperature fusion siliconising completes below 1800 DEG C, so in whole process, boron nitride coating can well prevent silicon vapor from corroding crucible; Select ethanol, glycerol to be dispersion agent, contribute to boron nitride powder and be dispersed in uniformly in thinner; Binding agent is can be used as during low temperature, boron nitride is made tightly to be attached to plumbago crucible surface, ethanol, glycerol are as organic solvent, cracking can be there is during high temperature, coat of silicon carbide framework is generated with silicon vapor effect, play the bonding effect keeping boron nitride and plumbago crucible on the one hand, coat of silicon carbide self also can prevent silicon vapor to the corrosion of plumbago crucible on the other hand; Form boric acid because hydrolysis can occur hexagonal boron nitride in water, so the pH of adjustment solution, stop the formation of boric acid.After adopting coating of the present invention, in applied at elevated temperature process, the cracking state of plumbago crucible greatly takes a turn for the better, and cracking ratio is reduced to about 5% by original 90%, extends the work-ing life of plumbago crucible, there is no objectionable impurities in operating process, operator's health is not damaged.
Embodiment
Embodiment 1
The present embodiment is a kind of coating of anti-silicon vapor corrosion, formulated after adopting hexagonal boron nitride, ethanol, glycerol and thinner to stir, the mass percent of described each material is: hexagonal boron nitride is 15%, ethanol is 2%, glycerol be 3% and thinner be 80%, thinner is distilled water or deionized water.In the present embodiment, described thinner is distilled water.
The present embodiment also proposed a kind of method preparing described anti-silicon vapor corrosion resistant coating, and concrete steps are:
Step 1, ratio weigh material: comprise the hexagonal boron nitride of 15%, the ethanol of 2%, the glycerol of 3% and 80% thinner.In the present embodiment, described thinner is deionized water.
Step 2, prepares solution: the thinner of weighing is put into beaker, in described beaker, add load weighted ethanol and glycerol.After being heated to 30 ~ 35 DEG C to described beaker, DJ1C reinforcement electric mixer is adopted to be uniformly mixed; Agitator speed is 200 ~ 280r/min, churning time 4 ~ 6min; Obtain the solution mixed.In the present embodiment, beaker Heating temperature is 30 DEG C, and agitator speed is 200r/min, churning time 6min.
Step 3, prepares coating: be added to by load weighted hexagonal boron nitride in the solution obtained, and adopt DJ1C reinforcement electric mixer to stir, the rotating speed of described agitator is 200 ~ 280r/min, and continuously stirring 4 ~ 6min, until solution becomes pasty state.Adopt and flow out the viscosity that agar diffusion method detects solution, the viscosity being added with the solution of hexagonal boron nitride by being coated with the survey of 4-agar diffusion method is 20 ~ 25s, stops stirring; Obtain the coating prepared.In the present embodiment, the rotating speed of agitator is 200r/min, and continuously stirring 6min; The viscosity of solution is 20s.
Step 4, the pH value of adjustment solution: add NaOH in the coating obtained, to adjust the pH value of solution, make pH=8 ~ 11.In the present embodiment, pH value=8 of solution.
Step 5, preparation coating: plumbago crucible is cleaned up post-drying, and bake out temperature is 40 ~ 140 DEG C; The coating of pH value=8 is evenly brushed on plumbago crucible surface.Under being had by external coating the crucible of coating to be placed in normal temperature, make brushing at the coating natural air drying of this crucible surface, form the coating of anti-silicon vapor corrosion at this crucible surface.In the present embodiment, the bake out temperature of plumbago crucible is 40 DEG C;
Adopt the plumbago crucible of the present embodiment coating can prevent silicon vapor from corroding, in applied at elevated temperature process, the cracking state of plumbago crucible greatly takes a turn for the better, cracking ratio is reduced to 5% by original 90%, extend the work-ing life of plumbago crucible, there is no objectionable impurities in operating process, operator's health is not damaged.
Embodiment 2
The present embodiment is a kind of coating of anti-silicon vapor corrosion, formulated after adopting hexagonal boron nitride, ethanol, glycerol and thinner to stir, the mass percent of described each material is: hexagonal boron nitride is 20%, ethanol is 5%, glycerol be 5% and thinner be 70%, thinner is distilled water or deionized water.In the present embodiment, described thinner is deionized water.
The present embodiment also proposed a kind of method preparing described anti-silicon vapor corrosion resistant coating, and concrete steps are:
Step 1, ratio weigh material: comprise the hexagonal boron nitride of 20%, the ethanol of 5%, the glycerol of 5% and 70% thinner.
Step 2, prepares solution: the thinner of weighing is put into beaker, in described beaker, add load weighted ethanol and glycerol.After being heated to 30 ~ 35 DEG C to described beaker, DJ1C reinforcement electric mixer is adopted to be uniformly mixed; Agitator speed is 200 ~ 280r/min, churning time 4 ~ 6min; Obtain the solution mixed.In the present embodiment, beaker Heating temperature is 32 DEG C, and agitator speed is 220r/min, churning time 6min.
Step 3, prepares coating: be added to by load weighted hexagonal boron nitride in the solution obtained, and adopt DJ1C reinforcement electric mixer to stir, the rotating speed of described agitator is 200 ~ 280r/min, and continuously stirring 4 ~ 6min, until solution becomes pasty state.Adopt and flow out the viscosity that agar diffusion method detects solution, the viscosity being added with the solution of hexagonal boron nitride by being coated with the survey of 4-agar diffusion method is 20 ~ 25s, stops stirring; Obtain the coating prepared.In the present embodiment, the rotating speed of agitator is 220r/min, and continuously stirring 6min; The viscosity of solution is 21s.
Step 4, the pH value of adjustment solution: add NaOH in the coating obtained, to adjust the pH value of solution, make pH=8 ~ 11.In the present embodiment, pH value=9 of solution.
Step 5, preparation coating: plumbago crucible is cleaned up post-drying, and bake out temperature is 40 ~ 140 DEG C; The coating of pH value=9 is evenly brushed on plumbago crucible surface.Under being had by external coating the crucible of coating to be placed in normal temperature, make brushing at the coating natural air drying of this crucible surface, form the coating of anti-silicon vapor corrosion at this crucible surface.In the present embodiment, the bake out temperature of plumbago crucible is 80 DEG C;
Adopt the plumbago crucible of the present embodiment coating can prevent silicon vapor from corroding, in applied at elevated temperature process, the cracking state of plumbago crucible greatly takes a turn for the better, cracking ratio is reduced to 5% by original 90%, extend the work-ing life of plumbago crucible, there is no objectionable impurities in operating process, operator's health is not damaged.
Embodiment 3
The present embodiment is a kind of coating of anti-silicon vapor corrosion, formulated after adopting hexagonal boron nitride, ethanol, glycerol and thinner to stir, the mass percent of described each material is: hexagonal boron nitride is 30%, ethanol is 2%, glycerol be 3% and thinner be 65%, thinner is distilled water or deionized water.In the present embodiment, described thinner is for removing distilled water.
The present embodiment also proposed a kind of method preparing described anti-silicon vapor corrosion resistant coating, and concrete steps are:
Step 1, ratio weigh material: comprise the hexagonal boron nitride of 30%, the ethanol of 2%, the glycerol of 3% and 65% thinner.
Step 2, prepares solution: the thinner of weighing is put into beaker, in described beaker, add load weighted ethanol and glycerol.After being heated to 30 ~ 35 DEG C to described beaker, DJ1C reinforcement electric mixer is adopted to be uniformly mixed; Agitator speed is 200 ~ 280r/min, churning time 4 ~ 6min; Obtain the solution mixed.In the present embodiment, beaker Heating temperature is 32 DEG C, and agitator speed is 240r/min, churning time 5min.
Step 3, prepares coating: be added to by load weighted hexagonal boron nitride in the solution obtained, and adopt DJ1C reinforcement electric mixer to stir, the rotating speed of described agitator is 200 ~ 280r/min, and continuously stirring 4 ~ 6min, until solution becomes pasty state.Adopt and flow out the viscosity that agar diffusion method detects solution, the viscosity being added with the solution of hexagonal boron nitride by being coated with the survey of 4-agar diffusion method is 20 ~ 25s, stops stirring; Obtain the coating prepared.In the present embodiment, the rotating speed of agitator is 240r/min, and continuously stirring 5min; The viscosity of solution is 23s.
Step 4, the pH value of adjustment solution: add NaOH in the coating obtained, to adjust the pH value of solution, make pH=8 ~ 11.In the present embodiment, pH value=10 of solution.
Step 5, preparation coating: plumbago crucible is cleaned up post-drying, and bake out temperature is 40 ~ 140 DEG C; The coating of pH value=10 is evenly brushed on plumbago crucible surface.Under being had by external coating the crucible of coating to be placed in normal temperature, make brushing at the coating natural air drying of this crucible surface, form the coating of anti-silicon vapor corrosion at this crucible surface.In the present embodiment, the bake out temperature of plumbago crucible is 110 DEG C;
Adopt the plumbago crucible of the present embodiment coating can prevent silicon vapor from corroding, in applied at elevated temperature process, the cracking state of plumbago crucible greatly takes a turn for the better, cracking ratio is reduced to 5% by original 90%, extend the work-ing life of plumbago crucible, there is no objectionable impurities in operating process, operator's health is not damaged.
Embodiment 4
The present embodiment is a kind of coating of anti-silicon vapor corrosion, formulated after adopting hexagonal boron nitride, ethanol, glycerol and thinner to stir, the mass percent of described each material is: hexagonal boron nitride is 35%, ethanol is 2%, glycerol be 3% and thinner be 60%, thinner is distilled water or deionized water.In the present embodiment, described thinner is deionized water.
The present embodiment also proposed a kind of method preparing described anti-silicon vapor corrosion resistant coating, and concrete steps are:
Step 1, ratio weigh material: comprise the hexagonal boron nitride of 35%, the ethanol of 2%, the glycerol of 3% and 60% thinner.In the present embodiment, described thinner is for removing distilled water.
Step 2, prepares solution: the thinner of weighing is put into beaker, in described beaker, add load weighted ethanol and glycerol.After being heated to 30 ~ 35 DEG C to described beaker, DJ1C reinforcement electric mixer is adopted to be uniformly mixed; Agitator speed is 200 ~ 280r/min, churning time 4 ~ 6min; Obtain the solution mixed.In the present embodiment, beaker Heating temperature is 35 DEG C, and agitator speed is 280r/min, churning time 4min.
Step 3, prepares coating: be added to by load weighted hexagonal boron nitride in the solution obtained, and adopt DJ1C reinforcement electric mixer to stir, the rotating speed of described agitator is 200 ~ 280r/min, and continuously stirring 4 ~ 6min, until solution becomes pasty state.Adopt and flow out the viscosity that agar diffusion method detects solution, the viscosity being added with the solution of hexagonal boron nitride by being coated with the survey of 4-agar diffusion method is 20 ~ 25s, stops stirring; Obtain the coating prepared.In the present embodiment, the rotating speed of agitator is 280r/min, and continuously stirring 4min; The viscosity of solution is 25s.
Step 4, the pH value of adjustment solution: add NaOH in the coating obtained, to adjust the pH value of solution, make pH=8 ~ 11.In the present embodiment, pH value=11 of solution.
Step 5, preparation coating: plumbago crucible is cleaned up post-drying, and bake out temperature is 40 ~ 140 DEG C; The coating of pH value=11 is evenly brushed on plumbago crucible surface.Under being had by external coating the crucible of coating to be placed in normal temperature, make brushing at the coating natural air drying of this crucible surface, form the coating of anti-silicon vapor corrosion at this crucible surface.In the present embodiment, the bake out temperature of plumbago crucible is 140 DEG C;
Adopt the plumbago crucible of the present embodiment coating can prevent silicon vapor from corroding, in applied at elevated temperature process, the cracking state of plumbago crucible greatly takes a turn for the better, cracking ratio is reduced to 5% by original 90%, extend the work-ing life of plumbago crucible, there is no objectionable impurities in operating process, operator's health is not damaged.
Claims (4)
1. a coating for anti-silicon vapor corrosion, it is characterized in that, the hexagonal boron nitride by 15 ~ 35%, the ethanol of 1 ~ 10%, the glycerol of 1 ~ 10% and the thinner of 50 ~ 80%, described per-cent is mass percent, and per-cent total amount is absolutely.
2. the coating of anti-silicon vapor corrosion as claimed in claim 1, is characterized in that, described hexagonal boron nitride, purity content >=99%; Described purity of alcohol content >=99%; Described glycerol purity content >=99%; Described thinner is distilled water or deionized water.
3. prepare a method for the coating of anti-silicon vapor corrosion described in claim 1, it is characterized in that, concrete steps are:
Step 1, ratio weighs material;
Step 2, prepares solution: the thinner of weighing is put into beaker, in described beaker, add load weighted ethanol and glycerol; Be uniformly mixed after 30 ~ 35 DEG C are heated to described beaker; Obtain the solution mixed;
Step 3, prepares coating: being added by load weighted hexagonal boron nitride in the solution obtained and being stirred to solution becomes the pasty state that viscosity is 20 ~ 25s, obtains the coating prepared;
Step 4, the pH value of adjustment solution: add NaOH in the coating obtained, to adjust the pH value of solution, make pH=8 ~ 11 of solution;
Step 5, preparation coating: evenly brushed by the coating of pH value=8 ~ 11 and to clean up and the plumbago crucible of drying is surperficial, and under being placed in normal temperature, make brushing at the coating natural air drying of this crucible surface, forms at this crucible surface the coating that anti-silicon vapor corrodes.
4. prepare a method for the coating of anti-silicon vapor corrosion described in claim 3, it is characterized in that, when preparing solution and when preparing coating, the rotating speed of agitator is 200 ~ 280r/min, and churning time is 4 ~ 6min.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107244943A (en) * | 2017-07-10 | 2017-10-13 | 巩义市泛锐熠辉复合材料有限公司 | A kind of reaction melt method of impregnation prepares the preparation method of C/C SiC ceramic matrix composite material graphite crucible face coats |
| CN110643209A (en) * | 2019-10-25 | 2020-01-03 | 长江师范学院 | Coating, smelting container, and manufacturing method and application of smelting container |
| CN112479743A (en) * | 2020-12-15 | 2021-03-12 | 山田研磨材料有限公司 | Graphite heating body protection process for vacuum sintering furnace |
| CN112694347A (en) * | 2020-12-28 | 2021-04-23 | 湖南世鑫新材料有限公司 | Carbon-carbon composite material crucible with silicon carbide coating and preparation method |
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| CN102167626A (en) * | 2010-12-30 | 2011-08-31 | 光为绿色新能源有限公司 | Preparation method of ceramic crucible coating layer for ingoting polysilicon |
| CN104292890A (en) * | 2013-07-17 | 2015-01-21 | 西门子公司 | Preparation method and application of ultra-hydrophobic coating |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102167626A (en) * | 2010-12-30 | 2011-08-31 | 光为绿色新能源有限公司 | Preparation method of ceramic crucible coating layer for ingoting polysilicon |
| CN104292890A (en) * | 2013-07-17 | 2015-01-21 | 西门子公司 | Preparation method and application of ultra-hydrophobic coating |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107244943A (en) * | 2017-07-10 | 2017-10-13 | 巩义市泛锐熠辉复合材料有限公司 | A kind of reaction melt method of impregnation prepares the preparation method of C/C SiC ceramic matrix composite material graphite crucible face coats |
| CN110643209A (en) * | 2019-10-25 | 2020-01-03 | 长江师范学院 | Coating, smelting container, and manufacturing method and application of smelting container |
| CN112479743A (en) * | 2020-12-15 | 2021-03-12 | 山田研磨材料有限公司 | Graphite heating body protection process for vacuum sintering furnace |
| CN112694347A (en) * | 2020-12-28 | 2021-04-23 | 湖南世鑫新材料有限公司 | Carbon-carbon composite material crucible with silicon carbide coating and preparation method |
| CN112694347B (en) * | 2020-12-28 | 2022-06-07 | 湖南世鑫新材料有限公司 | Carbon-carbon composite material crucible with silicon carbide coating and preparation method |
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Application publication date: 20150923 |