CN106565280B - A kind of CfThe preparation method of/SiC ceramic matrix composite material surface optical coating - Google Patents
A kind of CfThe preparation method of/SiC ceramic matrix composite material surface optical coating Download PDFInfo
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- CN106565280B CN106565280B CN201510659158.4A CN201510659158A CN106565280B CN 106565280 B CN106565280 B CN 106565280B CN 201510659158 A CN201510659158 A CN 201510659158A CN 106565280 B CN106565280 B CN 106565280B
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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
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
- C04B41/87—Ceramics
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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 present invention relates to a kind of CfThe preparation method of/SiC ceramic matrix composite material surface optical coating, the optical coating is the optics dense coating that 1mm or more is reached using SiC/Si as main phase and thickness, and the preparation method comprises the following steps :(a) prepares the porous biscuit film that main phase is C and SiC by casting molding processes；(b) the resulting porous biscuit film of step (a) is placed in CfUnder vacuum conditions in 1450 DEG C~1650 DEG C reaction siliconisings behind/SiC ceramic matrix composite material surface, thus in the Cf/ SiC ceramic matrix composite material surface is formed using SiC/Si as the ceramic coating of main phase.Present invention firstly provides the method for preparing composite material surface optical coating using casting films reaction sintering technology, obtained SiC/Si optical coating can significantly improve CfThe consistency on/SiC ceramic matrix composite material surface.
Description
Technical field
The present invention relates to a kind of CfThe preparation method of/SiC ceramic matrix composite material surface optical coating belongs to preparation technology of coating neck
Domain.
Background technique
Carbon fibre reinforced silicon carbide based composites (Cf/ SiC) combine high temperature resistant, the corrosion resistant of SiC ceramic and carbon fiber
The advantages that erosion, high specific stiffness, highly thermally conductive, low-density.For ceramics, there are unique crack deflections, fiber for material internal
The energy dissipation mechanisms such as extraction, bridging expand to weak interface area when generating micro-crack in matrix under the action of plus load
When domain will not quick unstable propagation, show the non-catastrophic failure feature of metalloid.Therefore, Cf/ SiC ceramic matrix composite material is being navigated
Empty space industry is widely used as rocket tube and combustion chamber, super speed vehicle sharp leading edge etc., simultaneously because excellent
Different mechanics and thermal property, CfPotential application of/the SiC ceramic matrix composite material in space optics field also results in extensive concern.
Due to the limitation of preparation method, Cf/ SiC ceramic matrix composite material consistency is relatively low, can not be obtained by optical manufacturing
The optical surface of high quality.This becomes CfOne of the main problem that/SiC ceramic matrix composite material is faced in the application of space optics field.
Solution to this problem first is that Cf/ SiC ceramic matrix composite material surface is modified.Current process for modifying surface is broadly divided into two
Class: physical vapour deposition (PVD) silicon (PVD-Si) and chemical vapor deposition of silicon carbide (CVD-SiC).PVD-Si is difficult to obtain higher cause
Density is inadequate with substrate binding force；CVD-SiC is easy layering, peels off, uneven thickness, and residual stress is big.
Summary of the invention
In view of the above-mentioned problems, being prepared and C the object of the present invention is to provide a kind off/ SiC ceramic matrix composite material ground be well combined and
The method of microcosmic composition and the controllable SiC/Si densification optical coating of thickness.
Here, the present invention provides a kind of CfThe preparation method of/SiC ceramic matrix composite material surface optical coating, the optical coating
Be using SiC/Si it is main phase, thickness up to the optics dense coating of 1mm or more, the preparation method comprises the following steps:
(a) the porous biscuit film that main phase is C and SiC is prepared by casting molding processes；
(b) by the resulting porous biscuit film of step (a) and CfPorous biscuit film (is placed in C by/SiC ceramic matrix composite materialf/ SiC is multiple
Condensation material surface) under vacuum conditions in 1450 DEG C~1650 DEG C reaction siliconisings, thus in the Cf/ SiC ceramic matrix composite material surface
It is formed using SiC/Si as the ceramic coating of main phase.
Present invention firstly provides the method for preparing composite material surface optical coating using casting films reaction sintering technology,
Obtained SiC/Si optical coating, can significantly improve CfThe consistency on/SiC ceramic matrix composite material surface, realizes the table of high quality
Face optical manufacturing, this method also have simple moulding process, coating consistency height, microcosmic composition and thickness controllably and and substrate
The advantages that bond strength is high.
Preferably, step (a) the following steps are included:
1) by as the silicon carbide powder of ceramic powder with carbon black, dispersing agent, binder, plastic agent by a certain percentage molten
It is uniformly dispersed in agent, slurry is obtained after ball milling；
It 2) is casting films by tape casting after resulting slurry degasification；
3) by resulting casting films drying, lamination, unsticking, porous biscuit film is obtained.
Preferably, by dispersing agent, ceramic powder, solvent mixing and ball milling 12~24 hours, bonding is then added in step 1)
Agent and plastic agent ball milling 12~24 hours again.
Preferably, the mass ratio of silicon carbide and carbon black is 1:(0.3~0.5 in step 1))；The solvent is ethyl alcohol and 2-
The mixed solvent of butanone, wherein the mass ratio of ethyl alcohol and 2- butanone is (30~40): (70~60)；The solvent and the ceramics
The volume ratio of powder is (60~80): (40~20).
Preferably, in step 1), the dispersing agent be herring oil, whale oil, olein, phosphate, castor oil or
Polyvinylpyrrolidone, additional amount are the 4%~6% of ceramic powder gross mass.
Preferably, the binder is polymethyl methacrylate or polyvinyl butyral, binder matter in step 1)
Amount is the 8%~12% of ceramic powder quality；Plastic agent is BBP(Butyl Benzyl Phthalate, and the quality of plastic agent is binder quality
0.5~2.0 times.
Preferably, controlling the height of scraper in step 2), in tape casting between 100 μm~500 μm.
Preferably, the casting films after lamination are in step 3) with a thickness of 1mm~4mm.Preferably, in step 3), when unsticking
Temperature is 600 DEG C~1200 DEG C, and heating rate is 1 DEG C/min~3 DEG C/min, and soaking time is 30~60 minutes.
Preferably, in step (b), the Cf/ SiC ceramic matrix composite material is surface-treated in advance, and the surface treatment includes
By the Cf/ SiC ceramic matrix composite material surface rubbing is polished and is cleaned, dries.
Preferably, the reaction time for reacting siliconising is 10~60 minutes in step (b).
Detailed description of the invention
The rheological behavior curve graph of the resulting slurry of Fig. 1 embodiment 1；
SEM figure after 2 casting films biscuit unsticking of Fig. 2 embodiment；
The XRD diagram of the coating after siliconising of Fig. 3 embodiment 4；
SEM figure of Fig. 4 embodiment 4 after siliconising after coating surface polishing；
Fig. 5 is that the section SEM of composite material base and coating after siliconising of embodiment 4 schemes.
Specific embodiment
Further illustrate the present invention below in conjunction with attached drawing and following specific embodiments, it should be appreciated that following embodiments and/
Or attached drawing is merely to illustrate the present invention, is not intended to limit the present invention.
It is difficult to obtain higher consistency for PVD-Si, it is inadequate with substrate binding force；CVD-SiC is easy layering, peels off,
Casting films are integrated to composite wood by liquid Si infiltration reaction sintering technology by uneven thickness, the big problem of residual stress, the present invention
Expect surface, is formed using SiC/Si as the ceramic coating of main phase.Specifically, in Cf/ SiC ceramic matrix composite material surface passes through casting technique
Prepare a layer thickness uniform, controllable, component it is uniform, it is flawless containing SiC, C be main phase casting films, through drying, lamination, de-
It is viscous, using liquid Si infiltration reaction sintering technology, convert casting films (porous biscuit film) to and Cf/ SiC ceramic matrix composite material ground knot
Good SiC/Si densification optical coating is closed, the surface with certain optical property is obtained finally by optical manufacturing.It is fresh at present
There is the pertinent literature of this respect to report.
As Cf/ SiC ceramic matrix composite material, preparation method is unlimited, such as can use precursor infiltration and pyrolysis (PIP) technique
Prepare Cf/ SiC ceramic matrix composite material substrate.Cf/ SiC ceramic matrix composite material can be surface-treated in advance.In one example, by Cf/
SiC ceramic matrix composite material substrate surface is polished, polished and, drying clean with alcohol washes.
With casting molding processes in Cf/ SiC ceramic matrix composite material substrate surface prepares the casting films that main phase is C, SiC.At one
In embodiment, casting molding processes include the following steps:
1) by as the silicon carbide powder of ceramic powder with carbon black, dispersing agent, binder, plastic agent by a certain percentage molten
It is uniformly dispersed in agent, slurry is obtained after ball milling；
It 2) is casting films by tape casting after resulting slurry degasification；
3) by resulting casting films drying, lamination, unsticking, carbon containing porous biscuit is obtained.
Wherein, the mass ratio of silicon carbide powder and carbon black can be 1:(0.3~0.5).Used solvent can for ethyl alcohol with
The mixed solvent of 2- butanone, wherein the mass ratio of ethyl alcohol and 2- butanone can be (30~40): (70~60), for example, 34:66.
Dispersing agent includes but is not limited to herring oil, whale oil, olein, phosphate, castor oil or polyvinyl pyrrole
Alkanone, additional amount can be the 4%-6% of ceramic powder gross mass.
Binder includes but is not limited to polymethyl methacrylate or polyvinyl butyral, and binder quality can be ceramics
The 8%-12% of powder quality.
Plastic agent includes but is not limited to BBP(Butyl Benzyl Phthalate, and the quality of plastic agent can be the 0.5- of binder quality
2.0 again.
In step 1), it is highly preferred that bonding is then added first by dispersing agent, ceramic powder, solvent mixing and ball milling 12-24h
Agent and plastic agent ball milling 12-24h again.Dispersing agent, ceramic powder, binder and plasticity are gradually added in such a way that substep is added
Agent etc. can increase the solid content of slurry, be conducive to the casting films for preparing high solids content.
In step 2), the height of scraper can be 100~500 μm in tape casting.By adjusting the height of scraper, can adjust
Save the thickness of casting films.In the present invention, the thickness of monolayer cast film can be 50~300 μm.
In step 3), dry can be spontaneously dries at room temperature, and drying time can be 3-5h.Curtain coating film thickness after lamination
Degree can be 1mm~4mm.Unsticking can be in 600 DEG C of -1200 DEG C of progress.Heating rate when unsticking can be 1 DEG C -3 DEG C/min, heat preservation
Time can be 30-60min.
The density of resulting carbon containing porous biscuit can be 1.52g/cm3, apparent porosity can be 45%~65%, and aperture is big
Small is 0.02~0.20 μm.
Then composite material base and carbon containing porous curtain coating membranogen base are placed in the graphite crucible for being coated with boron nitride, true
Liquid phase reactor siliconising under empty condition.Used silicon can be the HIGH-PURITY SILICON that purity is 99.0% or more.Reaction temperature can be 1450
DEG C -1650 DEG C, the reaction time can be 10-60min.Vacuum degree can be 1~10pa.Through liquid phase reactor siliconising, carbon containing porous curtain coating
Membranogen base is converted into fine and close using SiC/Si as the ceramic coating of main phase, and combines closely with composite material base.
After above-mentioned optical coating is made, optical manufacturing can also be carried out and obtain the surface with certain optical property.
The beneficial effects of the present invention are:
(1) simple process；
(2) the microcosmic composition of coating is controllable with thickness, that is, technological parameter when can be by regulation tape casting applies to control
The microcosmic composition of layer and thickness, such as the microcosmic composition of coating is controlled by regulation slurry solid content, by regulation blade thickness come
Regulate and control coating layer thickness；
(3) coating and composite substrate binding force are strong.
Embodiment of illustrating further below is with the present invention will be described in detail.It will similarly be understood that following embodiment is served only for this
Invention is further described, and should not be understood as limiting the scope of the invention, those skilled in the art is according to this hair
Some nonessential modifications and adaptations that bright above content is made all belong to the scope of protection of the present invention.Following examples are specific
Temperature, time etc. are also only an examples in OK range, i.e., those skilled in the art can close by the explanation of this paper
Selection in suitable range, and do not really want to be defined in hereafter exemplary specific value.
Embodiment 1:21.8g carbon black, 43.6g silicon carbide, 3.0g polyvinylpyrrolidone are dissolved in ethyl alcohol, 2- butanone quality
Than the mixed solvent for 34:66, ball milling 12 hours；Then 5.2g polyvinyl butyral and 2.6g phthalic acid fourth are added
Benzyl ester ball milling 24 hours, the viscosity and shear stress for measuring slurry with the change curve of shear rate obtained the rheological characteristic of slurry
It can be suitble to tape casting as shown in Figure 1, the characteristic of typical shear shinning is presented in slurry；The slurry tape casting that will be obtained, room
Temperature is 4 hours dry.Casting films are folded 4 layers, with a thickness of 1.0mm.Then casting films biscuit is put into unsticking in vacuum drying oven, with 1 DEG C/
The speed of min is warming up to 1200 DEG C, keeps the temperature 30 minutes, cools down later with furnace.
Embodiment 2:15.3g carbon black, 51.0g silicon carbide, 3.0g polyvinylpyrrolidone are dissolved in ethyl alcohol, 2- butanone quality
Than the mixed solvent for 34:66, ball milling 12 hours；Then 5.2g polyvinyl butyral and 2.6g phthalic acid fourth are added
Benzyl ester ball milling 24 hours.The slurry tape casting that will be obtained, drying at room temperature 4 hours.Casting films are folded 8 layers, with a thickness of 2.0mm.
Then casting films biscuit is put into unsticking in vacuum drying oven, is warming up to 900 DEG C with the speed of 2 DEG C/min, keeps the temperature 30 minutes, later
Cool down with furnace.The microstructure of casting films is as shown in Figure 2, it can be seen that and the casting films are after unsticking, without lamination,
Carbon, silicon carbide are uniformly distributed.
Embodiment 3:15.3g carbon black, 51.0g silicon carbide, 3.0g polyvinylpyrrolidone are dissolved in ethyl alcohol, 2- butanone quality
Than the mixed solvent for 34:66, ball milling 12 hours；Then 5.2g polyvinyl butyral and 2.6g phthalic acid fourth are added
Benzyl ester ball milling 24 hours.The slurry tape casting that will be obtained, drying at room temperature 4 hours.Casting films are folded 16 layers, with a thickness of 4.0mm.
Then casting films biscuit is put into unsticking in vacuum drying oven, is warming up to 900 DEG C with the speed of 2 DEG C/min, keeps the temperature 30 minutes, later
Cool down with furnace.
Embodiment 4:To through obtained in the composite material base for polishing, polishing and cleaning up and embodiment 1 and takes off
The casting films glued are placed in the graphite crucible for being coated with boron nitride, and siliconising is reacted at vacuum condition (vacuum degree 1pa), reaction
Temperature is 1550 DEG C, and the reaction time is 20 minutes.The XRD curve of coating is as shown in Figure 3, it can be seen that coating mainly by α-SiC,
Tri- phase composition of β-SiC and Si, the powder that wherein α-SiC is added mainly from ceramic slurry, β-SiC are anti-mainly from Si's and C
It answers.SEM figure after coating surface polishing is as shown in figure 4, white phase is free silica phase, and grey form and aspect are silicon carbide, and pitch black form and aspect are
Unreacted stomata.The section SEM of composite material base and coating figure is as shown in Figure 5, it can be seen that coating and composite material base
Material is combined closely.
Embodiment 5:To through obtained in the composite material base for polishing, polishing and cleaning up and embodiment 2 and takes off
The casting films glued are placed in the graphite crucible for being coated with boron nitride, and siliconising is reacted at vacuum condition (vacuum degree 1pa), reaction
Temperature is 1450 DEG C, and the reaction time is 60 minutes.
Embodiment 6:To through obtained in the composite material base for polishing, polishing and cleaning up and embodiment 3 and takes off
The casting films glued are placed in the graphite crucible for being coated with boron nitride, react siliconising under vacuum conditions, and reaction temperature is 1650 DEG C,
Reaction time is 10 minutes.Coating surveys its roughness by polishing, polishing.Coating shows preferable suface processing quality,
Surface roughness is up to 5nm RMS.
Embodiment 7:To through obtained in the composite material base for polishing, polishing and cleaning up and embodiment 2 and takes off
The casting films glued are placed in the graphite crucible for being coated with boron nitride, react siliconising under vacuum conditions, and reaction temperature is 1550 DEG C,
Reaction time is 30 minutes.Coating surveys its roughness by polishing, polishing.Coating shows preferable suface processing quality,
Surface roughness is up to 2.2nm RMS.
Claims (11)
1. a kind of CfThe preparation method of/SiC ceramic matrix composite material surface optical coating, which is characterized in that the optical coating is with SiC/
Si is the optics dense coating that main phase and thickness reach 1mm or more, and the preparation method comprises the following steps:
(a) the porous biscuit film that main phase is C and SiC is prepared by casting molding processes；
(b) the resulting porous biscuit film of step (a) is placed in CfBehind/SiC ceramic matrix composite material surface under vacuum conditions in 1450 DEG C~
1650 DEG C of reaction siliconisings, thus in the Cf/ SiC ceramic matrix composite material surface is formed using SiC/Si as the ceramic coating of main phase, described
Ceramic coating and Cf/ SiC ceramic matrix composite material is combined closely.
2. preparation method according to claim 1, which is characterized in that step (a) the following steps are included:
1) by as the silicon carbide powder of ceramic powder and carbon black, dispersing agent, binder, plastic agent by a certain percentage in a solvent
It is uniformly dispersed, slurry is obtained after ball milling；
It 2) is casting films by tape casting after resulting slurry degasification；
3) by resulting casting films drying, lamination, unsticking, porous biscuit film is obtained.
3. preparation method according to claim 2, which is characterized in that in step 1), by dispersing agent, ceramic powder, solvent
Mixing and ball milling 12~24 hours, binder and plastic agent ball milling 12~24 hours again are then added.
4. preparation method according to claim 2, which is characterized in that in step 3), the casting films after lamination are with a thickness of 1mm
~4mm.
5. preparation method according to claim 2, which is characterized in that in step 1), the mass ratio of silicon carbide and carbon black is
1:(0.3~0.5)；The solvent is the mixed solvent of ethyl alcohol and 2- butanone, wherein the mass ratio of ethyl alcohol and 2- butanone for (30~
40): (70~60)；The volume ratio of the solvent and the ceramic powder is (60~80): (40~20).
6. preparation method according to claim 2, which is characterized in that in step 1), the dispersing agent is herring oil, whale
Oil, olein, phosphate, castor oil or polyvinylpyrrolidone, additional amount are the 4%~6% of ceramic powder gross mass.
7. preparation method according to claim 2, which is characterized in that in step 1), the binder is polymethyl
Sour methyl esters or polyvinyl butyral, binder quality are the 8%~12% of ceramic powder quality；Plastic agent is phthalic acid fourth
Benzyl ester, the quality of plastic agent are 0.5~2.0 times of binder quality.
8. preparation method according to claim 2, which is characterized in that in step 2, the height of scraper is controlled in tape casting
Degree is between 100 μm~500 μm.
9. preparation method according to claim 2, which is characterized in that in step 3), temperature when unsticking is 600 DEG C~
1200 DEG C, heating rate is 1 DEG C/min~3 DEG C/min, and soaking time is 30~60 minutes.
10. preparation method according to any one of claim 1 to 9, which is characterized in that in step (b), the Cf/SiC
Composite material is surface-treated in advance, and the surface treatment includes by the Cf/ SiC ceramic matrix composite material surface rubbing, polishing are simultaneously
It cleans, drying.
11. preparation method according to any one of claim 1 to 9, which is characterized in that in step (b), react siliconising
Reaction time is 10~60 minutes.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1258657A (en) * | 1999-12-22 | 2000-07-05 | 中国科学院上海硅酸盐研究所 | Water-base curtain coating process for preparing ceramic film |
| CN102180674A (en) * | 2011-01-31 | 2011-09-14 | 中国科学院上海硅酸盐研究所 | Preparation method of reaction-sintered SiC ceramic |
| CN104356696A (en) * | 2014-10-21 | 2015-02-18 | 西北工业大学 | Rare earth silicate coating and method for preparing coating on surface of C/SiC composite material |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE50015159D1 (en) * | 2000-03-31 | 2008-06-26 | Ecm Ingenieur Unternehmen Fuer | A method of making a carbon fiber reinforced ceramic component having a solid ceramic and nonporous coating |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1258657A (en) * | 1999-12-22 | 2000-07-05 | 中国科学院上海硅酸盐研究所 | Water-base curtain coating process for preparing ceramic film |
| CN102180674A (en) * | 2011-01-31 | 2011-09-14 | 中国科学院上海硅酸盐研究所 | Preparation method of reaction-sintered SiC ceramic |
| CN104356696A (en) * | 2014-10-21 | 2015-02-18 | 西北工业大学 | Rare earth silicate coating and method for preparing coating on surface of C/SiC composite material |
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