CN106565280A - Method for preparing Cf/SiC composite material surface optical coating - Google Patents
Method for preparing Cf/SiC composite material surface optical coating Download PDFInfo
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- CN106565280A CN106565280A CN201510659158.4A CN201510659158A CN106565280A CN 106565280 A CN106565280 A CN 106565280A CN 201510659158 A CN201510659158 A CN 201510659158A CN 106565280 A CN106565280 A CN 106565280A
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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 invention relates to a method for preparing a Cf/SiC composite material surface optical coating. The optical coating is an optical compact coating with SiC/Si being used as the principal phase and the thickness reaching 1mm or above. The preparation method includes the following steps that (a) a porous bisque film with the principal phase being C and SiC is prepared through the tape casting technology; and (b) after the porous bisque film obtained in the step (a) is placed on the Cf/SiC composite material surface, reacting is performed at the temperature of 1450-1650 DEG C under the vacuum condition for siliconing, and thus a ceramic coating with the SiC/Si being used as the principal phase can be formed on the Cf/SiC composite material surface. By the adoption of the method, the method for preparing the composite material surface optical coating with the cast film reactive sintering technology is put forward for the first time, and the obtained SiC/Si optical coating can improve the compactness of the Cf/SiC composite material surface obviously.
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 technology
Carbon fibre reinforced silicon carbide based composites (Cf/ SiC) combine high temperature resistant, the corrosion resistant of SiC ceramic and carbon fiber
The advantages of erosion, high specific stiffness, highly thermally conductive, low-density.For comparing ceramics, there is unique crack deflection, fibre in material internal
The energy dissipation mechanisms such as dimension is extracted, bridging, when micro-crack is produced in matrix, expand to weak interface in the presence of plus load
During region will not quick unstable propagation, show the non-catastrophic failure feature of metalloid.Therefore, Cf/ SiC ceramic matrix composite material exists
Aerospace field 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 result in extensive concern.
Due to the restriction of preparation method, Cf/ SiC ceramic matrix composite material consistency is relatively low, it is impossible to obtain high-quality by optical manufacturing
The optical surface of amount.This becomes CfOne of main problem that/SiC ceramic matrix composite material faces in the application of space optics field.Solve
One of method of this problem is to Cf/ SiC ceramic matrix composite material surface is modified.Current process for modifying surface is broadly divided into two classes：
Physical vapour deposition (PVD) silicon (PVD-Si) and chemical vapor deposition of silicon carbide (CVD-SiC).PVD-Si is difficult to obtain higher
Consistency is inadequate with base material adhesion；CVD-SiC is easily layered, peels off, and uneven thickness, residual stress is big.
The content of the invention
For the problems referred to above, it is an object of the invention to provide one kind is prepared and Cf/ SiC ceramic matrix composite material ground is well combined and micro-
The method for seeing the composition SiC/Si densification optical coating controllable with thickness.
Here, the present invention provides a kind of CfThe preparation method of/SiC ceramic matrix composite material surface optical coating, the optical coating is
With SiC/Si as principal phase, thickness up to more than 1mm optics dense coating, the preparation method comprises the following steps：
A () prepares porous biscuit film of the principal phase for C and SiC by casting molding processes；
B () is by the porous biscuit film and C obtained by step (a)fPorous biscuit film (is placed in C by/SiC ceramic matrix composite materialf/ SiC composite woods
Material surface) under vacuum siliconising is reacted in 1450 DEG C～1650 DEG C, so as in the Cf/ SiC ceramic matrix composite material surface is formed
Ceramic coating with SiC/Si as principal phase.
Present invention firstly provides the method for preparing composite material surface optical coating using casting films reaction sintering technology, institute
The SiC/Si optical coatings for obtaining, can significantly improve CfThe consistency on/SiC ceramic matrix composite material surface, realizes high-quality surface
Optical manufacturing, the method also have that moulding process is simple, coating consistency is high, microcosmic composition is controllable with thickness and with substrate knot
The advantages of conjunction intensity is high.
It is preferred that step (a) is comprised the following steps：
1) will in a solvent divide by a certain percentage with carbon black, dispersant, binding agent, plastic agent as the silicon carbide powder of ceramic powder
Dissipate uniform, slurry is obtained after ball milling；
2) it is casting films by flow casting molding after the slurry degasification of gained；
3) by casting films drying, lamination, the unsticking of gained, porous biscuit film is obtained.
It is preferred that step 1) in, dispersant, ceramic powder, solvent mixing and ball milling 12～24 hours are subsequently adding
Binding agent and plastic agent ball milling 12～24 hours again.
It is preferred that step 1) in, the mass ratio of carborundum and carbon black is 1：(0.3～0.5)；The solvent is ethanol
With the mixed solvent of 2- butanone, wherein ethanol and the mass ratio of 2- butanone are (30～40)：(70～60)；The solvent
It is (60～80) with the volume ratio of the ceramic powder：(40～20).
It is preferred that step 1) in, the dispersant is herring oil, whale oil, olein, phosphate, castor oil
Or polyvinylpyrrolidone, addition is the 4%～6% of ceramic powder gross mass.
It is preferred that step 1) in, the binding agent is polymethyl methacrylate or polyvinyl butyral resin, binding agent matter
Measure as the 8%～12% of ceramic powder quality；Plastic agent is BBP(Butyl Benzyl Phthalate, and the quality of plastic agent is binding agent quality
0.5～2.0 times.
It is preferred that step 2) in, the height of control scraper is between 100 μm～500 μm in flow casting molding.
It is preferred that step 3) in, the curtain coating film thickness after lamination is 1mm～4mm.It is preferred that step 3) in, take off
Temperature when viscous is 600 DEG C～1200 DEG C, and heating rate is 1 DEG C/min～3 DEG C/min, and temperature retention time is 30～60 minutes.
It is preferred that 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, polish and clean, dry.
It is preferred that in step (b), the reaction time for reacting siliconising is 10～60 minutes.
Description of the drawings
The rheological behavior curve map of the slurry of the gained of Fig. 1 embodiments 1；
SEM figures after the casting films biscuit unsticking of Fig. 2 embodiments 2；
The XRD of the coating after siliconising of Fig. 3 embodiments 4；
SEM figure of Fig. 4 embodiments 4 after siliconising after coating surface polishing；
Fig. 5 is that the composite material base after siliconising of embodiment 4 is schemed with the section SEM of coating.
Specific embodiment
Further illustrate the present invention below in conjunction with accompanying drawing and following specific embodiments, it should be appreciated that following embodiments and/or
Accompanying drawing is merely to illustrate the present invention, and the unrestricted present invention.
It is difficult to obtain higher consistency for PVD-Si, it is inadequate with base material adhesion；CVD-SiC is easily layered, shells
Fall, uneven thickness, the big problem of residual stress, the present invention is attached to casting films by liquid Si infiltration reaction sintering technology compound
Material surface, forms the ceramic coating with SiC/Si as principal phase.Specifically, in Cf/ SiC ceramic matrix composite material surface is by curtain coating
Technique prepare a layer thickness uniform, controllable, component it is uniform, it is flawless containing SiC, C for principal phase casting films, drying,
Lamination, unsticking, using liquid Si infiltration reaction sintering technology, casting films (porous biscuit film) are converted into and Cf/ SiC is combined
The SiC/Si densification optical coatings that material ground is well combined, finally by optical manufacturing the table with certain optical property is obtained
Face.Rarely has the pertinent literature report of this respect at present.
As Cf/ SiC ceramic matrix composite material, its preparation method is not limited, for example, can adopt precursor infiltration and pyrolysis (PIP) technique
Prepare Cf/ SiC ceramic matrix composite material base material.Cf/ SiC ceramic matrix composite material can be surface-treated in advance.In one example, will
Cf/ SiC ceramic matrix composite material substrate surface is polished, polished and be clean with alcohol washes, drying.
With casting molding processes in Cf/ SiC ceramic matrix composite material substrate surface prepares casting films of the principal phase for C, SiC.In a reality
In applying mode, casting molding processes comprise the steps：
1) will in a solvent divide by a certain percentage with carbon black, dispersant, binding agent, plastic agent as the silicon carbide powder of ceramic powder
Dissipate uniform, slurry is obtained after ball milling；
2) it is casting films by flow casting molding after the slurry degasification of gained；
3) by casting films drying, lamination, the unsticking of gained, carbon containing porous biscuit is obtained.
Wherein, silicon carbide powder and the mass ratio of carbon black can be 1：(0.3～0.5).The solvent for being adopted can for ethanol with
The mixed solvent of 2- butanone, wherein ethanol can be (30～40) with the mass ratio of 2- butanone：(70～60), for example,
34:66。
Dispersant includes but is not limited to herring oil, whale oil, olein, phosphate, castor oil or polyvinyl pyrrole
Alkanone, its addition can be the 4%-6% of ceramic powder gross mass.
Binding agent includes but is not limited to polymethyl methacrylate or polyvinyl butyral resin, and binding agent quality can be ceramic powder
The 8%-12% of weight.
Plastic agent includes but is not limited to BBP(Butyl Benzyl Phthalate, and the quality of plastic agent can be the 0.5-2.0 of binding agent quality
Times.
Step 1) in, it is highly preferred that first dispersant, ceramic powder, solvent mixing and ball milling 12-24h are subsequently adding viscous
Knot agent and plastic agent ball milling 12-24h again.Dispersant, ceramic powder, binding agent and modeling are gradually added by way of substep is added
Property agent etc. can increase the solid content of slurry, be conducive to preparing the casting films of high solids content.
Step 2) in, the height of scraper can be 100～500 μm in flow casting molding.By the height for adjusting scraper, can be with
Adjust the thickness of casting films.In the present invention, the thickness of monolayer cast film can be 50～300 μm.
Step 3) in, drying can be spontaneously dried at room temperature, and drying time can be 3-5h.Curtain coating thickness after lamination
Degree can be 1mm～4mm.Unsticking can be carried out in 600 DEG C -1200 DEG C.Heating rate during unsticking can be 1 DEG C -3 DEG C/min, protect
The warm time can be 30-60min.
The density of the carbon containing porous biscuit of gained can be 1.52g/cm3, apparent porosity can be 45%～65%, pore size
For 0.02～0.20 μm.
Then composite material base and carbon containing porous curtain coating membranogen base are placed in the graphite crucible for scribbling boron nitride, in vacuum
Under the conditions of liquid phase reactor siliconising.The silicon for being adopted can be HIGH-PURITY SILICON that purity is more than 99.0%.Reaction temperature can for 1450 DEG C-
1650 DEG C, the reaction time can be 10-60min.Vacuum can be 1～10pa.Jing liquid phase reactor siliconisings, carbon containing porous casting films
Biscuit is converted into the ceramic coating with SiC/Si as principal phase of densification, and combines closely with composite material base.
After above-mentioned optical coating is obtained, optical manufacturing can also be carried out and obtain the surface with certain optical property.
The invention has the beneficial effects as follows：
(1) process is simple；
(2) coating microcosmic composition is controllable with thickness, i.e. can control coating microcosmic by regulating and controlling technological parameter during flow casting molding
Composition and thickness, for example, control coating microcosmic composition by regulating and controlling slurry solid content, and by regulating and controlling blade thickness coating is regulated and controled
Thickness；
(3) coating is strong with composite substrate adhesion.
Embodiment of illustrating further below is to describe the present invention in detail.It will similarly be understood that following examples are served only for this
Bright to be further described, it is impossible to be interpreted as limiting the scope of the invention, those skilled in the art is of the invention
Some nonessential modifications and adaptations that the above is made belong to protection scope of the present invention.The specific temperature of following examples,
Time etc. is also only an example in OK range, i.e., those skilled in the art suitable model can be done by the explanation of this paper
Interior selection is enclosed, and does not really want to be defined in the concrete numerical value of hereafter example.
Embodiment 1：21.8g carbon blacks, 43.6g carborundum, 3.0g polyvinylpyrrolidones are dissolved in into ethanol, 2- butanone matter
Amount is than being 34:66 mixed solvent, ball milling 12 hours；Then 5.2g polyvinyl butyral resins and 2.6g O-phthalics are added
Sour butyl benzyl ball milling 24 hours, the viscosity and shear stress for measuring slurry obtains the stream of slurry with the change curve of shear rate
Become performance as shown in figure 1, slurry is presented the characteristic of typical shear shinning, suitable flow casting molding；The slurry for obtaining is cast into
Type, drying at room temperature 4 hours.Casting films are folded 4 layers, and thickness is 1.0mm.Then casting films biscuit is put in vacuum drying oven and is taken off
It is viscous, 1200 DEG C are warming up to the speed of 1 DEG C/min, 30 minutes are incubated, lower the temperature with stove afterwards.
Embodiment 2：15.3g carbon blacks, 51.0g carborundum, 3.0g polyvinylpyrrolidones are dissolved in into ethanol, 2- butanone matter
Amount is than being 34:66 mixed solvent, ball milling 12 hours；Then 5.2g polyvinyl butyral resins and 2.6g neighbour's benzene two are added
Formic acid butyl benzyl ball milling 24 hours.By the slurry flow casting molding for obtaining, drying at room temperature 4 hours.Casting films are folded 8 layers, it is thick
Spend for 2.0mm.Then casting films biscuit is put into into unsticking in vacuum drying oven, is warming up to 900 DEG C with the speed of 2 DEG C/min, insulation
30 minutes, lower the temperature with stove afterwards.The microstructure of casting films is as shown in Figure 2, it can be seen that the casting films after unsticking,
Without lamination, carbon, carborundum are uniformly distributed.
Embodiment 3：15.3g carbon blacks, 51.0g carborundum, 3.0g polyvinylpyrrolidones are dissolved in into ethanol, 2- butanone matter
Amount is than being 34:66 mixed solvent, ball milling 12 hours；Then 5.2g polyvinyl butyral resins and 2.6g neighbour's benzene two are added
Formic acid butyl benzyl ball milling 24 hours.By the slurry flow casting molding for obtaining, drying at room temperature 4 hours.Casting films are folded 16 layers, it is thick
Spend for 4.0mm.Then casting films biscuit is put into into unsticking in vacuum drying oven, is warming up to 900 DEG C with the speed of 2 DEG C/min, insulation
30 minutes, lower the temperature with stove afterwards.
Embodiment 4：By the unsticking of gained in the composite material base and embodiment 1 through polishing, polishing and cleaning up
Good casting films are placed in the graphite crucible for scribbling boron nitride, and under vacuum condition (vacuum is 1pa) siliconising is reacted, and are reacted
Temperature is 1550 DEG C, and the reaction time is 20 minutes.The XRD curves of coating are as shown in Figure 3, it can be seen that coating mainly by
α-SiC, β-SiC and the phase compositions of Si tri-, the powder that wherein α-SiC add essentially from ceramic size, β-SiC mainly come
From the reaction of Si and C..As shown in figure 4, white phase is free silica phase, grey form and aspect are for SEM figures after coating surface polishing
Carborundum, pitch black form and aspect are unreacted pore.The section SEM figures of composite material base and coating are as shown in figure 5, can be with
Find out that coating is combined closely with composite material base.
Embodiment 5：By the unsticking of gained in the composite material base and embodiment 2 through polishing, polishing and cleaning up
Good casting films are placed in the graphite crucible for scribbling boron nitride, and under vacuum condition (vacuum is 1pa) siliconising is reacted, and are reacted
Temperature is 1450 DEG C, and the reaction time is 60 minutes.
Embodiment 6：By the unsticking of gained in the composite material base and embodiment 3 through polishing, polishing and cleaning up
Good casting films are placed in the graphite crucible for scribbling boron nitride, and siliconising is reacted under vacuum, and reaction temperature is 1650 DEG C,
Reaction time is 10 minutes.Coating surveys its roughness through polishing, polishing.Coating shows preferably Surface Machining matter
Amount, its surface roughness is up to 5nm RMS.
Embodiment 7：By the unsticking of gained in the composite material base and embodiment 2 through polishing, polishing and cleaning up
Good casting films are placed in the graphite crucible for scribbling boron nitride, and siliconising is reacted under vacuum, and reaction temperature is 1550 DEG C,
Reaction time is 30 minutes.Coating surveys its roughness through polishing, polishing.Coating shows preferably Surface Machining matter
Amount, its 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, it is characterised in that the optical coating is with SiC/Si as principal phase and thickness reaches the optics dense coating of more than 1mm, and the preparation method is comprised the following steps：
（a）Porous biscuit film of the principal phase for C and SiC is prepared by casting molding processes；
（b）By step（a）The porous biscuit film of gained is placed in CfUnder vacuum in 1450 DEG C～1650 DEG C reaction siliconisings behind/SiC ceramic matrix composite material surface, so as in the Cf/ SiC ceramic matrix composite material surface forms the ceramic coating with SiC/Si as principal phase.
2. preparation method according to claim 1, it is characterised in that step（a）Comprise the following steps：
1）To in a solvent be uniformly dispersed by a certain percentage with carbon black, dispersant, binding agent, plastic agent as the silicon carbide powder of ceramic powder, slurry is obtained after ball milling；
2）It is casting films by flow casting molding after the slurry degasification of gained；
3）By casting films drying, lamination, the unsticking of gained, porous biscuit film is obtained.
3. preparation method according to claim 2, it is characterised in that step 1）In, by dispersant, ceramic powder, solvent mixing and ball milling 12～24 hours, it is subsequently adding binding agent and plastic agent ball milling 12～24 hours again.
4. the preparation method according to Claims 2 or 3, it is characterised in that step 3）In, the curtain coating film thickness after lamination is 1mm～4mm.
5. the preparation method according to any one of claim 2 to 4, it is characterised in that step 1）In, the mass ratio of carborundum and carbon black is 1：（0.3～0.5）；The solvent is the mixed solvent of ethanol and 2- butanone, and wherein ethanol is with the mass ratio of 2- butanone（30～40）：（70～60）；The solvent is with the volume ratio of the ceramic powder（60～80）：（40～20）.
6. the preparation method according to any one of claim 2 to 5, it is characterised in that step 1）In, the dispersant is herring oil, whale oil, olein, phosphate, castor oil or polyvinylpyrrolidone, and addition is the 4%～6% of ceramic powder gross mass.
7. the preparation method according to any one of claim 2 to 6, it is characterised in that step 1）In, the binding agent is polymethyl methacrylate or polyvinyl butyral resin, and binding agent quality is the 8%～12% of ceramic powder quality；Plastic agent is BBP(Butyl Benzyl Phthalate, and the quality of plastic agent is 0.5～2.0 times of binding agent quality.
8. the preparation method according to any one of claim 2 to 7, it is characterised in that step 2）In, the height of control scraper is between 100 μm～500 μm in flow casting molding.
9. the preparation method according to any one of claim 2 to 8, it is characterised in that step 3）In, temperature during unsticking is 600 DEG C～1200 DEG C, and heating rate is 1 DEG C/min～3 DEG C/min, and temperature retention time is 30～60 minutes.
10. preparation method according to any one of claim 1 to 9, it is characterised in that step（b）In, the Cf/ SiC ceramic matrix composite material is surface-treated in advance, and the surface treatment is included the Cf/ SiC ceramic matrix composite material surface rubbing, polish and clean, dry.
11. preparation methods according to any one of claim 1 to 10, it is characterised in that step（b）In, the reaction time for reacting siliconising is 10～60 minutes.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107790683A (en) * | 2017-11-02 | 2018-03-13 | 哈尔滨工业大学 | Doctor-blade casting process, stacked-foil method and pressure infiltration method combine the method for preparing stratiform aluminum matrix composite |
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| 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 |
| EP1138654A1 (en) * | 2000-03-31 | 2001-10-04 | ECM Ingenieur-Unternehmen für Energie-und Umwelttechnik GmbH | Making of a ceramic coating for optical uses and method of applying it to surfaces of carbon fibre reinforced silicon carbide |
| 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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2015
- 2015-10-13 CN CN201510659158.4A patent/CN106565280B/en active Active
Patent Citations (4)
| 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 |
| EP1138654A1 (en) * | 2000-03-31 | 2001-10-04 | ECM Ingenieur-Unternehmen für Energie-und Umwelttechnik GmbH | Making of a ceramic coating for optical uses and method of applying it to surfaces of carbon fibre reinforced silicon carbide |
| 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 |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107790683A (en) * | 2017-11-02 | 2018-03-13 | 哈尔滨工业大学 | Doctor-blade casting process, stacked-foil method and pressure infiltration method combine the method for preparing stratiform aluminum matrix composite |
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