CN101913894A - Dual self-healing modification method for silicon carbide ceramic matrix composite material - Google Patents
Dual self-healing modification method for silicon carbide ceramic matrix composite material Download PDFInfo
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Abstract
The invention relates to a dual self-healing modification method for a silicon carbide ceramic matrix composite material, which is technologically characterized in that a fiber preform is used as a reinforcement, a pyrolytic carbon interface is prepared by chemical vapor infiltration, a silicon carbide matrix is prepared by the chemical vapor infiltration, and silicon carbide matrixes and amorphous boron carbide matrixes (alpha-B4C) are alternately prepared by the chemical vapor infiltration until the density of the composite material is greater than 2.0 g.cm<-3>; two silicon carbide coatings are formed by chemical vapor deposition, and borosilicate glass is used for sealing and filling by a method of brushing costing and sintering. The method has strong designability, simple process and good repeatability, can obviously improve the oxidation resistance of CMC-SiC and can meet the application requirement of sealing sheets/adjustment sheets, inner cones, floating wall tiles, flame tubes and other members of an aircraft engine with high thrust-weight ratio for long-life CMC-SiC.
Description
Technical field
The present invention relates to a kind of dual self-healing modification method of carbon/silicon carbide ceramic matrix composite, particularly relate to a kind of boron carbide-based body (α-B of multilayer amorphous of carbon/silicon carbide ceramic matrix composite
4C) in conjunction with the dual self-healing modification method of borosilicate glass packing.
Background technology
Fiber reinforced carbon/silicon carbide ceramic matrix composite (CMC-SiC) is novel fire resistant, low density, high performance thermal structure material, can effectively improve engine operating temperature, reduces the cold gas consumption, reduces element structure weight, reduces NO
xAnd CO
2Quantity discharged, all have huge application potential in fields such as high thrust-weight ratio aircraft engine, industry gas turbine and nuclear energy.The density of CMC-SiC is 2～2.5g/cm
3, be 1/4～1/6 of hot metal structured material, the highest life-time service temperature of potential is 1650 ℃, and is higher 150～350 ℃ than hot metal structured material.In addition, CMC-SiC has also overcome the big and poor reliability of structural ceramics fragility, anti-oxidant difference of carbon/carbon compound material and intensity are low, and shortcoming such as oxide ceramics based composites creep resistance difference, make it become the indispensable thermal structure materials of power system such as thrust-weight ratio 10 above aircraft engines and gas turbine, have the significantly potentiality of loss of weight, raising use temperature and over-all properties.
As described in Chinese patent (publication number CN101503305), hole and crackle that carbon/silicon carbide ceramic matrix composite exists have limited its work-ing life, must carry out self-healing modification to it, improve work-ing life.The manufacture method that United States Patent (USP) (US5246736) and Canadian Patent (CA2214465) have been invented multilayer Si-B-C matrix, this method adopts B
4C and Si-B-C carry out modification to the SiC matrix of carbon/silicon carbide ceramic matrix composite, and the material of manufacturing can be realized the self-healing of comparatively high temps, but complex process, the time is long, cost is high.In earlier stage, Northwestern Polytechnical University (Chinese invention patent, publication number CN101503305) has adopted amorphous norbide (α-B
4C) fiber reinforced carbon/silicon carbide ceramic matrix composite is carried out matrix modification, improved compound material antioxygenic property, but on the one hand, be subjected to the influence of self-healing phase (boric oxide glass) growing amount, the fully packing healing of the macropore of composite fiber interfascicular is subjected to the formation speed influence of self-healing phase on the other hand, causes material self-healing effect at high temperature to lag behind, be material self-healing immediately at high temperature, influenced the work-ing life of material.In order to solve macropore self-healing of above-mentioned materials interfascicular and self-healing effect hysteresis problem, the present invention is on the boron carbide-based structural reform of multilayer amorphous basis, introduce borosilicate glass matrix material interfascicular macropore is carried out packing, realize the matrix material dual self-healing modification.At present, also do not find the open report of this respect.
Summary of the invention
The technical problem that solves
For fear of the deficiencies in the prior art part, the present invention proposes a kind of dual self-healing modification method of carbon/silicon carbide ceramic matrix composite, be the dual self-healing modification method of the boron carbide-based body of multilayer amorphous of a kind of CMC-SiC in conjunction with the borosilicate glass packing, this method of modifying can significantly improve the antioxidant property of CMC-SiC, satisfies high thrust-weight ratio aircraft engine jet pipe and position, the combustion chamber member demand to long lifetime CMC-SiC material.
Technical scheme
A kind of dual self-healing modification method of carbon/silicon carbide ceramic matrix composite is characterized in that step is as follows:
Step 1: fiber preform is put into chemical vapor infiltration poke infiltration pyrolytic carbon interfacial layer, the infiltration temperature: 750～1100 ℃, soaking time: 50～500h, furnace pressure: 0.5～500Pa, precursor is C
3H
6Or CH
4Interfacial layer thickness is 80～500nm;
Step 2: the precast body behind the above-mentioned infiltration interfacial layer is carried out pyroprocessing in argon gas atmosphere, treatment temp: 1300～2100 ℃, treatment time 0.5～10h;
Step 3: the precast body after the high-temperature heat treatment is put into chemical gas phase silicon carbide infiltration stove permeate silicon carbide substrate, the infiltration temperature: 800～1200 ℃, soaking time: 50～500h, furnace pressure: 2～50kPa, precursor is CH
3SiCl
3
Step 4: the precast body behind the above-mentioned infiltration silicon carbide substrate is put into the boron carbide-based body of chemical gas phase norbide infiltration stove infiltration amorphous, the infiltration temperature: 850～1100 ℃, soaking time: 10～200h, furnace pressure: 2～50kPa, precursor is BCl
3-CH
4
Step 5: the precast body after the above-mentioned infiltration is put into chemical gas phase silicon carbide infiltration stove permeate silicon carbide substrate, the infiltration temperature: 850～1100 ℃, soaking time: 20～100h, furnace pressure: 2～50kPa, precursor is CH
3SiCl
3
Step 6: repeating step 4～step 5 is to precast body composite density＞2.0g.cm
-3
Step 7: adopt borosilicate glass colloidal sol to brush matrix material, make that the total coating thickness that rests on composite material surface is 5～50 μ m; B in the described colloidal sol
2O
3Content is 15～35wt%;
Step 8: at vacuum atmosphere, carry out sintering under 1000～1200 ℃, sintering time is 2～10 hours.
Described fiber preform is that carbon fiber or ceramic fiber strengthen, and its structure formation is that 2 dimension fibers adopt shop layer, 2.5 dimension fibrages, 3 dimension fibrages or 3 dimension fiber needled felt structures, and precast body adopts the pyrographite mould shape before putting into stove.
The precursor of described step 3 is SiCl
4-CH
4
The precursor of described step 4 is BCl
3-C
3H
6Or BCl
3-CH
4-C
3H
6
The precursor of described step 5 is BCl
3-C
3H
6Or BCl
3-CH
4-C
3H
6
Beneficial effect
The dual self-healing modification method of a kind of carbon/silicon carbide ceramic matrix composite that the present invention proposes, major advantage is: the designability of (1) matrix is strong, can carry out nanoscale design and preparation to composition, thickness and the number of plies of matrix as required.(2) matrix material has the dual self-healing function.The boric oxide glass that the oxidation of amorphous norbide generates is packing healing matrix cracking effectively, and the borosilicate glass of introducing is macroscopic void and coatingsurface between packing healing fibrous bundle effectively, thereby realizes the dual self-healing function of material.(3) Zhi Bei matrix material resistance of oxidation is strong, can significantly improve the heating power oxidation life-span of C/SiC matrix material.(4) preparation temperature is low, and to fibrous zero damage, composite materials property is good.(5) substrates multilayer helps discharging stress, and reduces matrix cracking, and the interface between the substrates multilayer helps the prolongation in crack deflection and crack propagation path simultaneously, thereby material has better obdurability.(6) be easy to prepare large size, complex component.
Description of drawings
Fig. 1 is the SEM photo of hole between microstructure borosilicate packing fibrous bundle behind the C/SiC dual self-healing modification;
Fig. 2 is the photo of packing matrix cracking after the oxidation of microstructure substrates multilayer behind the C/SiC dual self-healing modification
Fig. 3: provided the C/SiC material through the substrates multilayer modification and dual modified after, in the contrast of combustion chamber environment result of appraisal diagram.
Embodiment
Now in conjunction with the embodiments, accompanying drawing is further described the present invention:
Embodiment 1
(1) adopting the trade mark is the enhancing body of the carbon fiber of T700 as matrix material, adopts three-dimensional four-way weaving method to be woven into the 3D fiber preform, and the precast body specification is 250.0mm * 125.0mm, and thickness is 2.0mm;
(2) adopt high strength, high-modulus graphite jig that precast body is finalized the design, the thickness of fiber preform is 4.0mm;
(3) the prefabricated carbon fiber body is put into chemical gas phase pyrolytic carbon infiltration stove, infiltration RESEARCH OF PYROCARBON interfacial layer, the infiltration temperature: 750 ℃, soaking time: 200h, furnace pressure: 150Pa, precursor is C
3H
6Its thickness is 150nm;
(4) precast body that will prepare behind the interfacial layer carries out pyroprocessing, treatment temp: 1750 ℃, handle atmosphere: Ar gas, 2.0 hours treatment times;
(5) precast body after the high-temperature heat treatment is put into chemical gas phase silicon carbide infiltration stove and permeated silicon carbide substrate, the infiltration temperature: 950 ℃, soaking time: 300h, furnace pressure: 5kPa, precursor is SiCl
4-CH
4
(6) precast body behind the above-mentioned infiltration silicon carbide is put into the boron carbide-based body (α-B of chemical gas phase silicon carbide infiltration stove infiltration amorphous
4C), the infiltration temperature: 920 ℃, soaking time: 100h, furnace pressure: 3kPa, precursor is BCl
3-C
3H
6
(7) continue to put into chemical gas phase silicon carbide infiltration stove infiltration silicon carbide substrate, the infiltration temperature: 950 ℃, soaking time: 80h, furnace pressure: 5kPa, precursor is SiCl
4-CH
4
(8) repeating step (6) and (7) to composite density is 2.1g.cm
-3
(9) adopt borosilicate glass colloidal sol to brush matrix material, B
2O
3Content is 20wt%, and brushing number of times is 2 times, and borosilicate glass partly is impregnated into composite inner, and the borosilicate glass that rests on composite material surface partly is impregnated into composite inner, and the total coating thickness that rests on composite material surface is 20 μ m;
(10) at vacuum atmosphere, 1000 ℃ of following sinter fuse coatings, sintering time are 8 hours.
Embodiment 2
(1) adopting the trade mark is the enhancing body of the carbon fiber of T300 as matrix material, is 2.5 dimension fiber preforms with fibrage, and the precast body length and width are 250mm * 125mm, and thickness is 4.5mm;
(2) directly use graphite jig fixed-type 2.5 dimension carbon fiber knit precast bodies;
(3) the prefabricated carbon fiber body is put into chemical gas phase silicon carbide infiltration stove infiltration RESEARCH OF PYROCARBON interfacial layer, the infiltration temperature: 1000 ℃, soaking time: 80h, furnace pressure: 100Pa, precursor is CH
4Its thickness is 250nm;
(4) precast body after the carburizing is carried out pyroprocessing, treatment temp: 2050 ℃, handle atmosphere: Ar gas, 1.0 hours treatment times;
(5) precast body after the high-temperature heat treatment is put into chemical gas phase silicon carbide infiltration stove and permeated silicon carbide substrate, the infiltration temperature: 1100 ℃, soaking time: 500h, furnace pressure: 10kPa, precursor is CH
3SiCl
3
(6) precast body behind the above-mentioned infiltration silicon carbide is put into the boron carbide-based body (α-B of chemical gas phase norbide infiltration stove infiltration amorphous
4C), the infiltration temperature: 1050 ℃, soaking time: 90h, furnace pressure: 2kPa, precursor is BCl
3-CH
4
(7) precast body behind the above-mentioned infiltration norbide is put into chemical gas phase silicon carbide infiltration stove and permeated silicon carbide substrate, the infiltration temperature: 1100 ℃, soaking time: 100h, furnace pressure: 10kPa, precursor is CH
3SiCl
3
(8) repeating step (6) and (7) to composite density is 2.0g.cm
-3
(9) adopt borosilicate glass colloidal sol to brush matrix material, B
2O
3Content is 30wt%, and borosilicate glass partly is impregnated into composite inner, and the total coating thickness that rests on composite material surface is 45 μ m;
(10) at vacuum atmosphere, 1200 ℃ of following sinter fuse coatings, sintering time are 2 hours.
Embodiment 3
(1) adopting the trade mark is the enhancing body of silicon carbide (SiC) fiber of Nicalon as matrix material, is 2 dimension lamination precast bodies with 2 dimension Nicalon cloth shop layers, and the precast body length and width are 380mm * 380mm, and thickness is 5.0mm;
(2) directly use graphite jig fixed-type 2 dimension lamination precast bodies;
(3) the silicon carbide fiber precast body is put into chemical gas phase silicon carbide infiltration stove infiltration RESEARCH OF PYROCARBON interfacial layer, the infiltration temperature: 900 ℃, soaking time: 200h, furnace pressure: 10Pa, precursor is CH
4Its thickness is 300nm;
(4) precast body after the carburizing is carried out pyroprocessing, treatment temp: 1300 ℃, handle atmosphere: Ar gas, 2.0 hours treatment times;
(5) precast body after the high-temperature heat treatment is put into chemical gas phase silicon carbide infiltration stove and permeated silicon carbide substrate, the infiltration temperature: 1000 ℃, soaking time: 300h, furnace pressure: 20kPa, precursor is CH
3SiCl
3
(6) precast body behind the above-mentioned infiltration silicon carbide is put into the boron carbide-based body (α-B of chemical gas phase norbide infiltration stove infiltration amorphous
4C), the infiltration temperature: 950 ℃, soaking time: 100h, furnace pressure: 5kPa, precursor is BCl
3-CH
4
(7) precast body behind the above-mentioned infiltration norbide is put into chemical gas phase silicon carbide infiltration stove and permeated silicon carbide substrate, the infiltration temperature: 1000 ℃, soaking time: 90h, furnace pressure: 15kPa, precursor is CH
3SiCl
3
(8) repeating step (6) and (7) to composite density is 2.3g.cm
-3
(9) adopt borosilicate glass colloidal sol to brush matrix material, B
2O
3Content is 15wt%, and borosilicate glass partly is impregnated into composite inner, and the total coating thickness that rests on composite material surface is 20 μ m;
(10) at vacuum atmosphere, 1100 ℃ of following sinter fuse coatings, sintering time are 1.5 hours.
Embodiment 4
(1) adopting the trade mark is the enhancing body of silicon carbide (SiC) fiber of Hi-Nicalon as matrix material, is 2.5 dimension fiber preforms with fibrage, and the precast body length and width are 250mm * 80mm, and thickness is 3.0mm;
(2) directly use graphite jig fixed-type 2.5 dimension carbon fiber knit precast bodies;
(3) the silicon carbide fiber precast body is put into chemical gas phase silicon carbide infiltration stove infiltration RESEARCH OF PYROCARBON interfacial layer, the infiltration temperature: 800 ℃, soaking time: 300h, furnace pressure: 5Pa, precursor is CH
4Its thickness is 300nm;
(4) precast body after the carburizing is carried out pyroprocessing, treatment temp: 1400 ℃, handle atmosphere: Ar gas, 1.5 hours treatment times;
(5) precast body after the high-temperature heat treatment is put into chemical gas phase silicon carbide infiltration stove and permeated silicon carbide substrate, the infiltration temperature: 1100 ℃, soaking time: 500h, furnace pressure: 10kPa, precursor is CH
3SiCl
3
(6) precast body behind the above-mentioned infiltration silicon carbide is put into the boron carbide-based body (α-B of chemical gas phase norbide infiltration stove infiltration amorphous
4C), the infiltration temperature: 1050 ℃, soaking time: 90h, furnace pressure: 2kPa, precursor is BCl
3-CH
4
(7) precast body behind the above-mentioned infiltration norbide is put into chemical gas phase silicon carbide infiltration stove and permeated silicon carbide substrate, the infiltration temperature: 1100 ℃, soaking time: 100h, furnace pressure: 10kPa, precursor is CH
3SiCl
3
(8) repeating step (6) and (7) to composite density is 2.4g.cm
-3
(9) adopt borosilicate glass colloidal sol to brush matrix material, B
2O
3Content is 30wt%, and borosilicate glass partly is impregnated into composite inner, and the total coating thickness that rests on composite material surface is 45 μ m;
(10) at vacuum atmosphere, 1200 ℃ of following sinter fuse coatings, sintering time are 2 hours.
Claims (5)
1. the dual self-healing modification method of a carbon/silicon carbide ceramic matrix composite is characterized in that step is as follows:
Step 1: fiber preform is put into chemical vapor infiltration poke infiltration pyrolytic carbon interfacial layer, the infiltration temperature: 750～1100 ℃, soaking time: 50～500h, furnace pressure: 0.5～500Pa, precursor is C
3H
6Or CH
4Interfacial layer thickness is 80～500nm;
Step 2: the precast body behind the above-mentioned infiltration interfacial layer is carried out pyroprocessing in argon gas atmosphere, treatment temp: 1300～2100 ℃, treatment time 0.5～10h;
Step 3: the precast body after the high-temperature heat treatment is put into chemical gas phase silicon carbide infiltration stove permeate silicon carbide substrate, the infiltration temperature: 800～1200 ℃, soaking time: 50～500h, furnace pressure: 2～50kPa, precursor is CH
3SiCl
3
Step 4: the precast body behind the above-mentioned infiltration silicon carbide substrate is put into the boron carbide-based body of chemical gas phase norbide infiltration stove infiltration amorphous, the infiltration temperature: 850～1100 ℃, soaking time: 10～200h, furnace pressure: 2～50kPa, precursor is BCl
3-CH
4
Step 5: the precast body after the above-mentioned infiltration is put into chemical gas phase silicon carbide infiltration stove permeate silicon carbide substrate, the infiltration temperature: 850～1100 ℃, soaking time: 20～100h, furnace pressure: 2～50kPa, precursor is CH
3SiCl
3
Step 6: repeating step 4～step 5 is to precast body composite density＞2.0g.cm
-3
Step 7: adopt borosilicate glass colloidal sol to brush matrix material, make that the total coating thickness that rests on composite material surface is 5～50 μ m; B in the described colloidal sol
2O
3Content is 15～35wt%;
Step 8: at vacuum atmosphere, carry out sintering under 1000～1200 ℃, sintering time is 2～10 hours.
2. carbon/silicon carbide ceramic matrix composite dual self-healing modification method according to claim 1, it is characterized in that: described fiber preform is that carbon fiber or ceramic fiber strengthen, its structure formation is that 2 dimension fibers adopt shop layer, 2.5 dimension fibrages, 3 dimension fibrages or 3 dimension fiber needled felt structures, and precast body adopts the pyrographite mould shape before putting into stove.
3. carbon/silicon carbide ceramic matrix composite dual self-healing modification method according to claim 1 is characterized in that: the precursor of described step 3 is SiCl
4-CH
4
4. carbon/silicon carbide ceramic matrix composite dual self-healing modification method according to claim 1 is characterized in that: the precursor of described step 4 is BCl
3-C
3H
6Or BCl
3-CH
4-C
3H
6
5. carbon/silicon carbide ceramic matrix composite dual self-healing modification method according to claim 1 is characterized in that: the precursor of described step 5 is BCl
3-C
3H
6Or BCl
3-CH
4-C
3H
6
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| CN102344294A (en) * | 2011-06-30 | 2012-02-08 | 山东理工大学 | Method for preparing carbon-silicon carbide composite material by using chemical gas-phase permeation method |
| CN102910927A (en) * | 2012-11-16 | 2013-02-06 | 中国航空工业集团公司北京航空制造工程研究所 | Method for preparing self-healing silicon carbide ceramic-based composite material |
| CN103253938A (en) * | 2013-05-15 | 2013-08-21 | 西北工业大学 | Chemical vapor deposition method of Si-B-C-N amorphous ceramic |
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Application publication date: 20101215 |