CN101423422B - Method for coating silicon carbide on carbon material - Google Patents
Method for coating silicon carbide on carbon material Download PDFInfo
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- CN101423422B CN101423422B CN2008100797935A CN200810079793A CN101423422B CN 101423422 B CN101423422 B CN 101423422B CN 2008100797935 A CN2008100797935 A CN 2008100797935A CN 200810079793 A CN200810079793 A CN 200810079793A CN 101423422 B CN101423422 B CN 101423422B
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- charcoal material
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
Abstract
The invention discloses a method for coating silicon carbide on a carbon material, which comprises the following steps: silicon powder, acetone, an additive and an adhesive are mixed and ultrasonically dispersed for 3 to 5 minutes to obtain a steady suspension. The carbon material covering Si can be obtained by performing the electrophoretic deposition of the Si on the surface of the carbon material and taking the carbon material as an electrode. The carbon material is dried at a temperature of between 100 and 150 DEG C and is heated and sintered in an electrical resistance furnace. The heating temperature is between 1,000 and 1,500 DEG C, and the SiC coating of the carbon material can be prepared after the thermal insulation is performed for 20 to 60 minutes. The method has the advantages of relatively simple technical process, good repetitiveness, and quick deposition process, and the obtained coating has controllable thickness and is uniform.
Description
Technical field
The present invention relates to a kind of method of carrying out coat of silicon carbide at charcoal material surface.
Background technology
The raw material of wood-charcoal material has many advantages as high-temperature structural material, as thermostability, chemical stability, electroconductibility, anti-thermal shock etc., at 2000 ℃ high mechanical strength is arranged.Obtain widespread use in fields such as Aeronautics and Astronautics, metallurgy, nuclear energy.But performance is reduced with oxidizing gas reacting more than 400 ℃, make its application in high temperature oxidation stability atmosphere limited.Therefore, the raw material of wood-charcoal material being carried out the oxidation protection processing is the essential measure that improves its job stability and reliability.
It is a kind of main method that solves the protection of raw material of wood-charcoal material high temperature oxidation that the raw material of wood-charcoal material is carried out the coating processing.SiC has thermal expansivity as coated material and advantages such as matrix is approaching, low density, good mechanical character.And in high temperature air, SiC can oxidation generate the SiO that can effectively stop the atomic oxygen diffusion to be invaded
2Glass further improves antioxidant property.It is the main coated material that is used for the protection of raw material of wood-charcoal material at present.The main method of preparation SiC coating has at present: entrapping method, chemical Vapor deposition process, thermospray, wet chemistry method etc.But this several method complex process, poor controllability, cost height and coating usually have tiny crack, and resistance of oxidation is not high.Zhu etc. (carbon, 1999,37:1475-1484) prepared the SiC coating in graphite material surface-coated method, this coating has good antioxidant property, but the process complexity is unfavorable for promoting.Electrophoretic deposition prepares coating and has advantages such as quick, controlled, that cost is low, coating is even, and the research to this in recent years just progressively launches.Number of patent application 93100182.X is the coating method of a kind of electrophoretic deposition-reaction sintering covering type coating, has adopted agglomerating technology behind the first electrophoretic deposition to realize the preparation of MCrAlX coating.But, also increased preparation cost owing to adopt the embedding plating to cause the poor controllability of coating with the bonding force that improves settling and matrix.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, provide a kind of low cost, charcoal material surface that controllability is good to carry out the method for coat of silicon carbide.
The object of the present invention is achieved like this: by a certain percentage silica flour, acetone, additive, binding agent are mixed, ultra-sonic dispersion 3～5min makes stable suspension.At charcoal material surface electrophoretic deposition Si, as electrode, can obtain the raw material of wood-charcoal material of coated Si with the raw material of wood-charcoal material.Dry heat-agglomerating in resistance furnace afterwards in 100～150 ℃ environment.Heating temperature is 1000 ℃～1500 ℃, and insulation can prepare the SiC coating of raw material of wood-charcoal material in 20～60 minutes.
Preparation method of the present invention may further comprise the steps:
(1) charcoal material surface is cleaned, use distilled water ultrasonic cleaning, drying for standby then after the decontamination;
(2) configuration suspension: silica flour, binding agent polyvinyl butyral acetal (PVB) are put into acetone, add the additive n-Butyl Amine 99 afterwards, standby by supersound process 3～5min gained stable suspension, suspension remains on room temperature; The add-on of each component is that silica flour concentration is 10～60g/l acetone, and the add-on of additive is 0.5%～10% of an acetone volume, and the binding agent add-on is 0.5～10g/l acetone;
(3) electrophoretic deposition: the raw material of wood-charcoal material is put into suspension after as anodal closure, suspension is stirred, under the strength of electric field of 10～60V/cm, deposit, voltage constant in the deposition process, depositing time is 1～10min, make the cladding of raw material of wood-charcoal material, drying is 1～5 hour in 100-150 ℃ environment, obtains exsiccant raw material of wood-charcoal material cladding;
(4) with raw material of wood-charcoal material cladding, at first be heated to 300 ℃～500 ℃ insulations 10～60 minutes with 3～10 ℃/minute rate of heating, and then be heated to 1200 ℃～1600 ℃ with 3～6 ℃/minute rate of heating, be incubated 20～60 minutes, stop heating, after the cooling, obtain having the raw material of wood-charcoal material of coat of silicon carbide.
Aforesaid silicon particle size is less than 20 μ m.
Advantage of the present invention is as follows:
1. technological process is simple relatively, good reproducibility.2. deposition process is quick, and the gained coat-thickness is controlled and coating is even, and coat-thickness is at 20～200 μ m.3. have wide range of applications, be not subjected to the restriction of base shape, be fit to the mass preparation coating.4. adopt agglomerating method behind the first electrophoretic deposition to realize the Gradient distribution of SiC coating, promoted the Chemical bond of coating and body material, avoided the concentrated coating stripping that causes owing to thermal stresses.5. Zhi Bei oxidation resistant coating has thermal-shock resistance and good antioxidant property.
Embodiment
Embodiment 1
With particle diameter is the Si powder 2g of 40nm, and PVB1g mixes the back and adds 1ml n-Butyl Amine 99 acquisition mixed solution with 100ml acetone, and ultra-sonic dispersion 5min is uniformly dispersed suspension.The graphite material surface is cleaned, and the distilled water ultrasonic cleaning is used in decontamination afterwards, and dry back places suspension as anode, adopts the mode depositing silicon of electrophoretic deposition.Voltage constant in the deposition process, electrophoretic deposition parameter are strength of electric field 50V/cm, and depositing time 3min can be in the coating of graphite material surface coating 80 μ m.Be put in afterwards in 100 ℃ the loft drier dry 4 hours, and obtained the exsiccant cladding.This cladding is put in plumbago crucible, and crucible is put in the resistance furnace heats.Temperature rise rate is 3 ℃/minute to 400 ℃, is incubated 30 minutes, with 4 ℃/minute rate of heating stove is heated to 1200 ℃ then, is incubated 30 minutes.Stop heating, sample is taken out in the cooling back.In 1200 ℃ still air, carry out the antioxidant property test, not 1 hour weight loss 25% of the graphite oxidation of coating; After coating was handled, 10 hours weight loss of oxidation was 0.8%.
Embodiment 2
With particle diameter is the Si powder 3g of 100nm, and PVB5g mixes the back and adds 5ml n-Butyl Amine 99 acquisition mixed solution with 100ml acetone, and ultra-sonic dispersion 5min is uniformly dispersed mixed solution.Charcoal material surface is cleaned, and the distilled water ultrasonic cleaning is used in decontamination afterwards, and dry back places suspension as anode, adopts the mode depositing silicon of electrophoretic deposition.Voltage constant in the deposition process, electrophoretic deposition parameter are strength of electric field 35V/cm, and depositing time 5min can coat the coating of 90 μ m at charcoal material surface.Be put in afterwards in 150 ℃ the loft drier dry 3 hours, and obtained the exsiccant cladding.This cladding is put in plumbago crucible, and crucible is put in the resistance furnace heats.Temperature rise rate is 5 ℃/minute to 400 ℃, is incubated 20 minutes, with 5 ℃/minute rate of heating stove is heated to 1400 ℃ then, is incubated 40 minutes.Stop heating, sample is taken out in the cooling back.In 1200 ℃ still air, carry out the antioxidant property test, not 1 hour weight loss 33% of raw material of wood-charcoal material oxidation of coating; After coating was handled, 10 hours weight loss of oxidation was 1.1%.
Embodiment 3
With particle diameter is the Si powder 5g of 0.5 μ m, and PVB7g mixes the back and adds 10ml n-Butyl Amine 99 acquisition mixed solution with 100ml acetone, and ultra-sonic dispersion 5min is uniformly dispersed mixed solution.Charcoal material surface is cleaned, and the distilled water ultrasonic cleaning is used in decontamination afterwards, and dry back places suspension as anode, adopts the mode depositing silicon of electrophoretic deposition.Voltage constant in the deposition process, electrophoretic deposition parameter are strength of electric field 20V/cm, and depositing time 10min can coat the coating of 100 μ m at charcoal material surface.Be put in afterwards in 100 ℃ the loft drier dry 2 hours, and obtained the exsiccant cladding.This cladding is put in plumbago crucible, and crucible is put in the resistance furnace heats.Temperature rise rate is 10 ℃/minute to 400 ℃, is incubated 60 minutes, with 6 ℃/minute rate of heating stove is heated to 1450 ℃ then, is incubated 20 minutes.Stop heating, sample is taken out in the cooling back.In 1200 ℃ still air, carry out the antioxidant property test, not 1 hour weight loss 33% of raw material of wood-charcoal material oxidation of coating; After coating was handled, 10 hours weight loss of oxidation was 0.6%.
Embodiment 4
With particle diameter is the Si powder 3g of 5 μ m, and PVB2g mixes the back and adds 2ml n-Butyl Amine 99 acquisition mixed solution with 100ml acetone, and ultra-sonic dispersion 5min is uniformly dispersed mixed solution.Charcoal material surface is cleaned, and the distilled water ultrasonic cleaning is used in decontamination afterwards, and dry back places suspension as anode, adopts the mode depositing silicon of electrophoretic deposition.Voltage constant in the deposition process, electrophoretic deposition parameter are strength of electric field 50V/cm, and depositing time 3min can coat the coating of 120 μ m at charcoal material surface.Be put in afterwards in 120 ℃ the loft drier dry 1 hour, and obtained the exsiccant cladding.This cladding is put in plumbago crucible, and crucible is put in the resistance furnace heats.Temperature rise rate is 6 ℃/minute to 400 ℃, is incubated 50 minutes, with 5 ℃/minute rate of heating stove is heated to 1450 ℃ then, is incubated 30 minutes.Stop heating, sample is taken out in the cooling back.In 1200 ℃ still air, carry out the antioxidant property test, not 1 hour weight loss 33% of raw material of wood-charcoal material oxidation of coating; After coating was handled, 10 hours weight loss of oxidation was 0.3%.
Embodiment 5
With particle diameter is the Si powder 2g of 15 μ m, and PVB1g mixes the back and adds 3ml n-Butyl Amine 99 acquisition mixed solution with 100ml acetone, and ultra-sonic dispersion 4min is uniformly dispersed mixed solution.Charcoal material surface is cleaned, and the distilled water ultrasonic cleaning is used in decontamination afterwards, and dry back places suspension as anode, adopts the mode depositing silicon of electrophoretic deposition.Voltage constant in the deposition process, electrophoretic deposition parameter are strength of electric field 50V/cm, and depositing time 2min can coat the coating of 140 μ m at charcoal material surface.Be put in afterwards in 120 ℃ the loft drier dry 4 hours, and obtained the exsiccant cladding.This cladding is put in plumbago crucible, and crucible is put in the resistance furnace heats.Temperature rise rate is 4 ℃/minute to 450 ℃, is incubated 40 minutes, with 5 ℃/minute rate of heating stove is heated to 1500 ℃ then, is incubated 30 minutes.Stop heating, sample is taken out in the cooling back.In 1200 ℃ still air, carry out the antioxidant property test, not 1 hour weight loss 33% of raw material of wood-charcoal material oxidation of coating; After coating was handled, 10 hours weight loss of oxidation was 0.1%.
Embodiment 6
With particle diameter is the Si powder 3g of 15 μ m, and PVB1.5g mixes the back and adds 1ml n-Butyl Amine 99 acquisition mixed solution with 100ml acetone, and ultra-sonic dispersion 5min is uniformly dispersed mixed solution.Charcoal material surface is cleaned, and the distilled water ultrasonic cleaning is used in decontamination afterwards, and dry back places suspension as anode, adopts the mode depositing silicon of electrophoretic deposition.Voltage constant in the deposition process, electrophoretic deposition parameter are strength of electric field 40V/cm, and depositing time 4min can coat the coating of 160 μ m at charcoal material surface.Be put in afterwards in 120 ℃ the loft drier dry 2 hours, and obtained the exsiccant cladding.This cladding is put in plumbago crucible, and crucible is put in the resistance furnace heats.Temperature rise rate is 5 ℃/minute to 450 ℃, is incubated 30 minutes, with 3 ℃/minute rate of heating stove is heated to 1500 ℃ then, is incubated 60 minutes.Stop heating, sample is taken out in the cooling back.Sample is carried out the heat shock resistance experiment, and concrete steps are that stove is warming up to 1000 ℃, put into sample 10 minutes, take out in the water that drops into room temperature rapidly, repeat above operation 10 times, and coating is complete, does not see coating crack.The sample weight rate of loss is 0.5%, and coating has good thermal-shock resistance.
Claims (2)
1. one kind is carried out the method for coat of silicon carbide at charcoal material surface, it is characterized in that comprising the steps:
(1) charcoal material surface is cleaned, use distilled water ultrasonic cleaning, drying for standby then after the decontamination;
(2) configuration suspension: silica flour, binding agent polyvinyl butyral acetal are put into acetone, add the additive n-Butyl Amine 99 afterwards, standby by supersound process 3～5min gained stable suspension, suspension remains on room temperature; The add-on of each component is that silica flour concentration is 10～60g/l acetone, and the add-on of additive is 0.5%～10% of an acetone volume, and the binding agent add-on is 0.5～10g/l acetone;
(3) electrophoretic deposition: the raw material of wood-charcoal material is put into suspension after as anodal closure, suspension is stirred, under the strength of electric field of 10～60V/cm, deposit, voltage constant in the deposition process, depositing time is 1～10min, make the cladding of raw material of wood-charcoal material, drying is 1～5 hour in 100-150 ℃ environment, obtains exsiccant raw material of wood-charcoal material cladding;
(4) with raw material of wood-charcoal material cladding, at first be heated to 300 ℃～500 ℃ insulations 10～60 minutes with 3～10 ℃/minute rate of heating, and then be heated to 1200 ℃～1600 ℃ with 3～6 ℃/minute rate of heating, be incubated 20～60 minutes, stop heating, after the cooling, obtain having the raw material of wood-charcoal material of coat of silicon carbide.
2. as claimed in claim 1ly a kind ofly carry out the method for coat of silicon carbide, it is characterized in that described silicon particle size is less than 20 μ m at charcoal material surface.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2008100797935A CN101423422B (en) | 2008-11-12 | 2008-11-12 | Method for coating silicon carbide on carbon material |
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| CN2008100797935A CN101423422B (en) | 2008-11-12 | 2008-11-12 | Method for coating silicon carbide on carbon material |
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| CN101423422B true CN101423422B (en) | 2011-04-06 |
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| CN102850085A (en) * | 2012-09-21 | 2013-01-02 | 青岛天地碳素有限公司 | Method for preparation of graphite surface silicon carbide coating |
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