CN102757260B - Repairing method of ceramic-based composite material coating with utilization temperature of being more than or equal to 1400 DEG C - Google Patents
Repairing method of ceramic-based composite material coating with utilization temperature of being more than or equal to 1400 DEG C Download PDFInfo
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Abstract
The invention relates to a repairing method of a ceramic based composite material coating with utilization temperature of being more than or equal to 1400 DEG C. The method is technically characterized in that silicon powder, carbide of difficulty-smelt metal, boride, oxide and low-smelting-point glass powder (oxide with a smelting point of 400-1400 DEG C) are taken as raw materials; organic silane and a solvent are added to prepare uniform slurry to be coated on the surface of a damaged coating of the ceramic-based composite material; and then the coated ceramic-based composite material is cured at low temperature to obtain the coating which is well combined with a base body and is dense. The method disclosed by the invention effectively solves the online repairing problem of damages on the ceramic-based composite material coating. Meanwhile, the preparation cycle is short, the process is simple and the repeatability is good. A prepared coating system is verified to effectively improve the oxidation resistance of the composite material with the use temperature within a range of being more than or equal to 1400 DEG C.
Description
Technical field
The present invention relates to a kind of ceramic matric composite high temperature coating (use temperature is more than or equal to 1400 ℃) method for repairing and mending, relate to a kind of ceramic matric composite high temperature coating (use temperature is more than or equal to 1400 ℃) at lines mending method, relate to a kind of ceramic matric composite high temperature coating (use temperature is more than or equal to 1400 ℃) low-temperature fabrication simultaneously.
Background technology
In recent years, along with the development of spationautics, space strength has become 21 century and has implemented the main dependence strength of national security and military strategy.In people's atmosphere process, because strong pneumatic heating, the nose cone of aircraft and the temperature of the leading edge of a wing can be up to 1650 ℃ again for aerospacecraft, and thermal protection system is one of 4 big gordian techniquies of aerospacecraft.Ceramic matric composite C/SiC has become empty day the most promising thermal protection struc ture integrated material of aircraft of the s-generation, comprises nose cone, guide vane, wing and the cover plate etc. of space shuttle and guided missile in the member of thermal structure material.
The subject matter that the C/SiC matrix material exists in application is exactly that at high temperature antioxidant property is relatively poor.Be on the one hand owing to the C/SiC matrix material because the density of material is lower; Be because the thermal expansivity (CTE) between SiC matrix and the fiber does not match on the other hand, make to have many fine cracks on the SiC matrix.These fine cracks can become the flow passage of oxygen corrosion carbon fiber in the use of C/SiC matrix material.Therefore, protection system that must development C/SiC matrix material is to stop oxygen by the diffusion to carbon fiber of crackle and ventilate.
The main method that present stage solves is the C/SiC material surface to be carried out oxidation resistant coating handle, and the main technique of coating has CVD method, sol-gel method etc.But the problem that exists is the C/SiC matrix material can cause top coat that certain destruction is arranged in processing and equipment process, the breaking-up of coating may cause carbon fiber to be exposed under the combustion gas environment, the oxidation of carbon fiber will cause the inefficacy of member, have a strong impact on the normal use of material.
Colombia's thermal protection system fatal crass's event of losing efficacy and causing for example, NASA is responsible for first engineer's Neil special saying difficult to understand of " Colombia " extra portion fuel container engineering, problem is that the process of laying foam materials with spray gun outside fuel container can stay the slit between each piece foam materials, and liquid hydrogen can infiltrate therebetween.After space shuttle took off, the hydrogen expanded by heating finally caused the bulk foam materials to come off.The foam materials that the external tank surface comes off hits the material of " strengthening carbon carbon " (namely the strengthening the carbon-to-carbon thermal baffle) by name of space shuttle left wing leading edge.When space shuttle returns, through atmospheric layer, produce violent friction and make temperature after pouring port wing, melt internal structure up to Celsius 1400 air of spending, cause wing and body to melt, caused the generation of tragedy.So any problem of potential safety hazard that might exist all is worth our thinking and research.
Can cause the damage of top coat for above-mentioned material in processing and preparation process is exactly a very good problem to study, and prepare again coating not only the cycle longer, and costly, in order to address this problem, research coating repairing technique becomes a focus.But use the online repairing technique of coating in zone but to rarely have report for high temperature coating (use temperature is more than or equal to 1400 ℃).
Summary of the invention
Technical problem to be solved by this invention provides a kind of ceramic matric composite use temperature more than or equal to the method for repairing and mending of 1400 ℃ coating, can be implemented in line and repairs.
A kind of ceramic matric composite use temperature is more than or equal to the method for repairing and mending of 1400 ℃ coating, and it is as follows to it is characterized in that repairing step:
Step 1: the mixed slurry of carbide, boride, oxide compound and the organosilane tackiness agent of employing Si powder, refractory metal is as internally coated coated material, then coated material is brushed in impaired coating place, under 40 ~ 120 ℃ of low temperature, make its curing, obtain undercoat; The mass ratio of the carbide of described You Ji Gui Wan ﹕ Si Fen ﹕ refractory metal is 1 ~ 3:4 ~ 7:1 ~ 3;
Step 2: the mixed slurry of carbide, boride, oxide compound and the silicone adhesive of employing refractory metal is as the coated material of high-temperaure coating, then high-temperaure coating is applied on the undercoat, under 80 ~ 120 ℃ of low temperature, make its curing, obtain high-temperaure coating; The mass ratio of the carbide of described You Ji Gui Wan ︰ refractory metal is 1 ~ 3:4 ~ 7;
Step 3: adopting softening temperature is that the mixed slurry of 400 ℃ ~ 1400 ℃ glass powder and organosilane tackiness agent is as external coating (EC) glass coating material, then the glass coating material is brushed on high-temperaure coating, under 40 ~ 120 ℃ of low temperature, make its curing, obtain glass coating, finish the repairing of coating; The mass ratio of described You Ji Gui Wan ︰ glass powder is 1 ~ 3:4 ~ 7.
Curing in described step 1, step 2 and the step 3 adopts infrared lamp, ultra violet lamp or baking oven to make its curing.
The carbide of described refractory metal substitutes with boride or oxide compound.
The carbide of described refractory metal is: the carbide of zirconium, aluminium, tungsten, molybdenum, tantalum, niobium, hafnium, chromium, vanadium and titanium.
Described oxide compound is that fusing point is 1000 ℃ ~ 1400 ℃ oxide compound, comprises the oxide compound of barium strontium aluminium silicon BSAS and carbonate, vitriol, barium, aluminium or five series of gallium.
Described glass powder is: bismuth glass powder, lead glass powder, vanadium glass powder, phosphate glass powder or borosilicate glass powder.
Described organosilane tackiness agent is: poly-nitrogen silane, polysiloxane, Polycarbosilane or poly-boron nitrogen silane.
Ceramic matric composite use temperature provided by the invention is more than or equal to the method for repairing and mending of 1400 ℃ coating, and based on rational coating structure design, each layer coating cooperatively interacts, and reaches the service requirements of relevant temperature.In coating system, the purpose that undercoat (mixolimnion of the carbide of silica flour and some refractory metals, boride, oxide compound) is added silica flour is in order to improve the bonding force of coating and matrix, adds carbide, the boride of refractory metal, the purpose of oxide compound is the internally coated high thermal resistance of raising; Inter coat (high-temperature-resistant layer) mainly is in order to improve the heat-resisting ability of coating system; External coating (EC) (glass coating) mainly is to form liquid phase under relevant temperature, and crackle and the hole to matrix carries out packing on the one hand, can carry out the self-healing of coating on the other hand, has also improved the reliability that coating system uses simultaneously.
Advantage is:
(1) this method preparation technology is simple, only needs simple brushing to prepare and finishes, and need not complicated heat treatment technology: (2) this method is low to the preparation equipment requirements, need not accurate equipment substantially; (3) this method preparation cycle is short: (4) this method cost is low: (5) this method provides a kind of ceramic matric composite high temperature coating (use temperature is more than or equal to 1400 ℃) online repairing technique.(6) this method can be carried out corresponding structural adjustment to adapt to the repairing demand according to different use temperature (use temperature is more than or equal to 1400 ℃) requirement.
Description of drawings
Fig. 1: embodiment 1 coating sample is at 1500 ℃, oxidation coatingsurface SEM figure after 60 minutes in the air;
Fig. 2: embodiment 1 coating sample is at 1500 ℃, oxidation coatingsurface SEM figure after 60 minutes in the air;
Fig. 3: embodiment 1 coating sample is at 1500 ℃, oxidation coating section SEM figure after 60 minutes in the air;
Fig. 4: embodiment 1 coating sample is at 1500 ℃, oxidation coating section EDS figure after 60 minutes in the air;
Fig. 5: embodiment 1 coating sample is at 1500 ℃, oxidation coating section EDS figure after 60 minutes in the air;
Embodiment
Now in conjunction with the embodiments, accompanying drawing is further described the present invention:
Embodiment 1:
Step 1: carried out ultrasonic cleaning 30 minutes for C/SiC composite material by adopting clear water to be repaired, place then in 100 ℃ of baking ovens and dried through 30 minutes, stand-by;
Step 2: add with silica flour 100% ethanol as solvent, add 20% poly-nitrogen silane as tackiness agent, add 20% aluminium hydroxide as solid filler, the about 30min of ball milling, the slurry that obtains mixing;
Step 3: the slurry that mixes is brushed in substrate surface, made its curing about 120 ℃ (scenes can adopt infrared lamp irradiation) through 5-6 hour, thereby obtain undercoat;
Step 4: add with aluminium hydrate powder 100% ethanol as solvent, add 20% poly-nitrogen silane as tackiness agent, the about 30min of ball milling, the slurry that obtains mixing;
Step 5: the slurry that mixes is brushed on the undercoat of step 2,3 preparations, through 5-6 hour it is solidified fully about 120 ℃ (the infrared lamp irradiation can be adopted in the scene), thereby obtain high-temperaure coating;
Step 6: add with borosilicate glass powder 100% ethanol as solvent, add 20% poly-nitrogen silane as tackiness agent, the about 30min of ball milling, the slurry that obtains mixing;
Step 7: the slurry that mixes is brushed on the high-temperaure coating of step 4,5 preparations, through 5-6 hour it is solidified fully about 120 ℃ (the infrared lamp irradiation can be adopted in the scene), can obtain glass coating;
To the coating sample that prepared and no coating sample with carry out oxidation experiment, the result is presented at 1500 ℃, and to be incubated 60 minutes coating sample weightlessness only about 4.31%, and the sample weightlessness that does not add coating is 53.7%.1 can see that coatingsurface is not very smooth from the graph, has some tiny cracks and hole, but by high power SEM figure (Fig. 2) as can be seen these holes be not through hole, also there is the coating of densification in hole inside.
We can draw as drawing a conclusion in conjunction with cross-section morphology figure (Fig. 3) and EDS figure (Fig. 4 and Fig. 5): coating is two-layer behind oxidation experiment, external coating (EC) is more fine and close than undercoat, undercoat and matrix bond are not very good, but phenomenons such as oxidation do not appear in matrix, and peeling off does not appear in coating yet; External coating (EC) is combined better with undercoat.Analyze in conjunction with EDS, we infer that external coating (EC) is the borosilicate glass coatings, and internal layer is the key coat of aluminum hydroxide layer and undercoat silicon layer.The thickness of inside and outside coating all is about 50 μ m.In conjunction with the microstructure of weightless value and coating sample, we are the provide protection of coating system as can be seen.
Embodiment 2:
Step 1: carried out ultrasonic cleaning 30 minutes for C/SiC composite material by adopting clear water to be repaired, place then in 100 ℃ of baking ovens and dried through 30 minutes, stand-by;
Step 2: add with silica flour 100% ethanol as solvent, add 20% Polycarbosilane as tackiness agent, add 20% zirconium diboride as solid filler, the about 30min of ball milling, the slurry that obtains mixing;
Step 3: the slurry that mixes is brushed in substrate surface, made its curing about 80 ℃ (scenes can adopt infrared lamp irradiation) through 10-12 hour, thereby obtain undercoat;
Step 4: add with zirconium diboride 100% ethanol as solvent, add 20% Polycarbosilane as tackiness agent, the about 30min of ball milling, the slurry that obtains mixing;
Step 5: the slurry that mixes is brushed on the undercoat of step 2,3 preparations, through 10-12 hour it is solidified fully about 80 ℃ (the infrared lamp irradiation can be adopted in the scene), thereby obtain high-temperaure coating;
Step 6: add with borosilicate glass powder 100% ethanol as solvent, add 20% Polycarbosilane as tackiness agent, the about 30min of ball milling, the slurry that obtains mixing;
Step 7: the slurry that mixes is brushed on the high-temperaure coating of step 4,5 preparations, through 10-12 hour it is solidified fully about 80 ℃ (the infrared lamp irradiation can be adopted in the scene), can obtain glass coating;
To the coating sample that prepared and no coating sample with carry out oxidation experiment, it is about 5.12% that the result is presented at 60 minutes coating samples of 1500 ℃ of oxidations weightlessness, and the sample weightlessness that does not add coating is 53.7%.
Embodiment 3:
Step 1: carried out ultrasonic cleaning 30 minutes for C/SiC composite material by adopting clear water to be repaired, place then in 100 ℃ of baking ovens and dried through 30 minutes, stand-by;
Step 2: add with silica flour 100% ethanol as solvent, add 20% poly-nitrogen silane as tackiness agent, add 20% norbide as solid filler, the about 30min of ball milling, the slurry that obtains mixing;
Step 3: the slurry that mixes is brushed in substrate surface, made its curing about 120 ℃ (scenes can adopt infrared lamp irradiation) through 5-6 hour, thereby obtain undercoat;
Step 4: add with aluminium hydrate powder 100% ethanol as solvent, add 20% poly-nitrogen silane as tackiness agent, the about 30min of ball milling, the slurry that obtains mixing;
Step 5: the slurry that mixes is brushed on the undercoat of step 2,3 preparations, through 5-6 hour it is solidified fully about 120 ℃ (the infrared lamp irradiation can be adopted in the scene), thereby obtain high-temperaure coating;
Step 6: add with barium strontium aluminium silica flour (BSAS) 100% ethanol as solvent, add 20% poly-nitrogen silane as tackiness agent, the about 30min of ball milling, the slurry that obtains mixing;
Step 7: the slurry that mixes is brushed on the high-temperaure coating of step 4,5 preparations, through 5-6 hour it is solidified fully about 120 ℃ (the infrared lamp irradiation can be adopted in the scene), can obtain glass coating;
To the coating sample that prepared and no coating sample with carry out oxidation experiment, it is about 4.91% that the result is presented at 60 minutes coating samples of 1500 ℃ of oxidations weightlessness, and the sample weightlessness that does not add coating is 53.7%.
Claims (6)
1. a ceramic matric composite use temperature is more than or equal to the method for repairing and mending of 1400 ℃ coating, and it is as follows to it is characterized in that repairing step:
Step 1: the oxide compound of the carbide of employing Si powder and refractory metal or the boride of refractory metal or refractory metal and the mixed slurry of organosilane tackiness agent are as internally coated coated material, then coated material is brushed in impaired coating place, under 40～120 ℃ of low temperature, make its curing, obtain undercoat; The mass ratio of the oxide compound of the carbide of described You Ji Gui Wan ﹕ Si Fen ﹕ refractory metal or the boride of refractory metal or refractory metal is 1～3:4～7:1～3;
Step 2: the oxide compound of the carbide of employing refractory metal or the boride of refractory metal or refractory metal and the mixed slurry of silicone adhesive are as the coated material of high-temperaure coating, then high-temperaure coating is applied on the undercoat, under 80～120 ℃ of low temperature, make its curing, obtain high-temperaure coating; The mass ratio of the oxide compound of the carbide of described You Ji Gui Wan ︰ refractory metal or the boride of refractory metal or refractory metal is 1～3:4～7;
Step 3: adopting softening temperature is that the mixed slurry of 400 ℃～1400 ℃ glass powder and organosilane tackiness agent is as external coating (EC) glass coating material, then the glass coating material is brushed on high-temperaure coating, under 40～120 ℃ of low temperature, make its curing, obtain glass coating, finish the repairing of coating; The mass ratio of described You Ji Gui Wan ︰ glass powder is 1～3:4～7.
2. according to the method for repairing and mending of the described ceramic matric composite use temperature of claim 1 more than or equal to 1400 ℃ coating, it is characterized in that: the curing in described step 1, step 2 and the step 3 adopts infrared lamp, ultra violet lamp or baking oven to make its curing.
According to claim 1 or 2 described ceramic matric composite use temperatures more than or equal to the method for repairing and mending of 1400 ℃ coating, it is characterized in that: the carbide of described refractory metal substitutes with boride or oxide compound.
3. according to claim 1 or the 2 described a kind of ceramic matric composite use temperatures method for repairing and mending more than or equal to 1400 ℃ coating, it is characterized in that: the carbide of described refractory metal is: the carbide of zirconium, aluminium, tungsten, molybdenum, tantalum, niobium, hafnium, chromium, vanadium and titanium.
4. according to claim 1 or the 2 described ceramic matric composite use temperatures method for repairing and mending more than or equal to 1400 ℃ coating, it is characterized in that: described oxide compound is that fusing point is 1000 ℃～1400 ℃ oxide compound, comprises the oxide compound of barium strontium aluminium silicon BSAS and carbonate, vitriol, barium, aluminium or five series of gallium.
5. according to claim 1 or the 2 described ceramic matric composite use temperatures method for repairing and mending more than or equal to 1400 ℃ coating, it is characterized in that: described glass powder is: bismuth glass powder, lead glass powder, vanadium glass powder, phosphate glass powder or borosilicate glass powder.
According to claim 1 or 2 described ceramic matric composite use temperatures more than or equal to the method for repairing and mending of 1400 ℃ coating, it is characterized in that: described organosilane tackiness agent is: poly-nitrogen silane, polysiloxane, Polycarbosilane or poly-boron nitrogen silane.
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