CN103113123B - Preparation method of SiCf/SiC ceramic matrix composite turbine blades - Google Patents
Preparation method of SiCf/SiC ceramic matrix composite turbine blades Download PDFInfo
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- CN103113123B CN103113123B CN201310044298.1A CN201310044298A CN103113123B CN 103113123 B CN103113123 B CN 103113123B CN 201310044298 A CN201310044298 A CN 201310044298A CN 103113123 B CN103113123 B CN 103113123B
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Abstract
The invention discloses a preparation method of SiCf/SiC ceramic matrix composite turbine blades, which is characterized in that through analyzing the stress distribution of a blade in an application state, based on this point, a performance-controllable SiCf/SiC ceramic matrix composite turbine blade is manufactured through the designing and adopting of processes such as rapid forming, high-performance continuous yarn braiding, gel-casting, reactive sintering, and the like. According to the method, parts such as blades and the like are manufactured by using heterogeneous materials, the contradiction between the uniformity and nonuniform loaded structure of materials is solved, and the performances of materials can be set flexibly according to the bearing needs of manufactured parts; and prepared SiCf/SiC ceramic matrix composite turbine blades have the characteristics of near-net forming variable-cross-section complex structure, controllable material performance, flexible machining, short production cycle, low cost, and the like, and can be applied to the development and manufacturing of high-temperature-resistant complex structured parts for aerospace and the like.
Description
Technical field
The invention belongs to composite material parts manufacturing technology field, relate to a kind of SiC
fthe preparation method of/SiC ceramic matrix composite turbine blade.
Background technology
At present, the nickel base superalloy use temperature that aero engine turbine blades adopts is limited, and density is higher, has restricted the further lifting of motor performance.And continuous fibre weaves toughness reinforcing SiC ceramic matric composite blade and has high temperature resistant, high tenacity, high than features such as strong and low density, can greatly improve thrust-weight ratio and the high-temperature behavior of engine, be the ideal material that alternate-engine high-temperature component is manufactured.
Summary of the invention
The problem that the present invention solves is to provide a kind of SiC
fthe preparation method of/SiC ceramic matrix composite turbine blade, the method is the preparation method of a kind of structure and the toughness reinforcing SiC ceramic matric composite of performance controllable type continuous fibre three-dimensional structure.
The present invention is achieved through the following technical solutions:
A kind of SiC
fthe preparation method of/SiC ceramic matrix composite turbine blade, comprises the following steps:
1) state under working conditions according to turbine blade, obtains the performance requriements of its localized region material, respective material design criteria, and reverse obtains the Weave parameters of partial zones material;
2) by each Regional Integration, obtain design of part, the materials microstructure Integrated Model of ceramic matrix composite turbine blade, with light-curing quick moulding method, produce turbine blade shell mould and the guide support support with topological characteristic;
3) on prefabricated guide support support, weave SiC continuous fibre;
4) the guide support support that is woven with SiC continuous fibre being put into solid concentration is Polycarbosilane-xylene solution of 10～25%, carries out repeatedly vacuum impregnation-dry-crosslinking process;
5) adopt precursor to apply cracking process, at SiC continuous fibre surface preparation SiC interfacial layer;
6) the guide support support of fibrage is fixed in light-cured resin shell, cast ceramics slurry in type vacuum injecting and forming machine, obtains the ceramic blade green compact that there is SiC fiber reinforcement inside;
7) under protective atmosphere, ceramic blade green compact are warming up to 800 ℃ of organic crackings that make in base substrate, obtain blade biscuit;
8) blade biscuit is used after silicon embedding, be warming up to 1400～1600 ℃ and carry out reaction sintering, obtain SiC
f/ SiC ceramic matrix composite turbine blade.
Described turbine blade minus mould and the special guide support support of mould inside topology are:
The three-dimensional model that adopts CAD software building turbine blade minus mould and guide support support, is then converted into three-dimensional model STL formatted data; Adopt delamination software Magics to carry out layering processing to three-dimensional model, processing data is imported to photocureable rapid shaping manufacturing course SLARP; Adopt light-curing quick moulding method to produce minus mould and guide support support.
Continuous SiC fiber braiding is to use continuous SiC fiber bundle, and average fibre diameter 8～15 μ m, draw fibrous bundle with soft pin, on stent preform, weave.
SiC interfacial layer is prepared on the described surface at continuous fibre:
It is 15～40% PCS-xylene solution that Polycarbosilane and dimethylbenzene are mixed with to massfraction, adds the SiC micro mist that accounts for solution quality 20～45% in PCS-xylene solution, is mixed with SiC-PCS-xylene slurry;
The SiC fiber reinforcement weaving is immersed in SiC-PCS-xylene slurry, is placed in vacuum tank, after vacuumizing, add ultrasonication, add air pressure 5.0MPa～10.0MPa, pressurize 30min, to guarantee that steeping fluid fully enters fibrous bundle hole and is evenly coated on fiber surface;
After completing dipping, take out fiber reinforcement, in air, in 50～65 ℃ of dry 1～2h, then it is oxidation cross-linked in 120～150 ℃ of insulation 8～12h, to complete Polycarbosilane;
The fiber reinforcement that is coated with Polycarbosilane, under protective atmosphere, is warming up to 1000～1200 ℃ with the speed of 2～5 ℃/min and carries out cracking, and soaking time is 1～2h, makes inorganicization of Polycarbosilane that is coated in fiber surface generate SiC interfacial layer.
Being prepared as of the ceramic size of described step 6):
By liquid phenolic resin with pore-forming material according to 50:(65～100) mass ratio mixes, and obtains liquid phase component;
The SiC micro mist of 6～8.5 parts, the metal Ni micro mist of 0.05～0.2 part, the Graphite Powder 99 of 0.1～0.3 part and the nanometer carbon black of 0.1～1 part are fully mixed, obtain solid components;
Solid components and liquid phase component are fully mixed, obtain ceramic size after ball milling according to the volume ratio of 45～65:100;
Liquid phase component is mixed with the dispersion agent sodium polyacrylate of solid components quality 1～2%, together put into silicon carbide ball grinder with solid components again, add silicon carbide ball-milling medium, with 300～360r/min rotating speed ball milling, 30～120min, obtain the finely dispersed ceramic size of solid phase particles;
0.5～1h before ceramic size notes type, also adds 4～8% benzene sulfonyl chloride of resin quality in ceramic size in ceramic size and stirs, vacuum exhaust 10～30min.
Described liquid phase component comprises that the molten heat-reactive phenolic resin of alcohol, ethylene glycol volume parts are respectively 3.0～5.5 parts, 5～7 parts;
SiC micro mist in solid components, metal Ni micro mist, Graphite Powder 99, nanometer carbon black mass fraction are respectively: 8～8.5 parts, 0.15～0.2 part, 0.2～0.3 part, 0.8～1 part.
Being prepared as of the ceramic size of described step 6):
Liquid phase component is by acrylamide and N, N ＇-methylene-bisacrylamide is that 6～10:1 mixes according to mass ratio, add initiator again, catalyzer is made, wherein acrylamide and N, total mass content of N ＇-methylene-bisacrylamide is liquid phase component 12～20%;
Solid components is by the SiC micro mist of 6～8.5 parts, the Graphite Powder 99 of 0.2～0.5 part and the nanometer carbon black of 0.1～1 part are fully mixed;
Solid components and liquid phase component are fully mixed, obtain ceramic size after ball milling according to the volume ratio of 45～65:100;
Before ceramic size notes type, also the initiator of ceramic size and its quality 0.5～1%, 0.2～0.5% catalyzer are fully stirred.
Described is that liquid phase component is mixed with the dispersion agent sodium polyacrylate of solid components quality 1～2%, together put into silicon carbide ball grinder with solid components again, add silicon carbide ball-milling medium, with 300～360r/min rotating speed ball milling, 30～120min, obtain the finely dispersed ceramic size of solid phase particles;
Described SiC micro mist is the mixing of meal alpha-SiC micropowder and fine powder alpha-SiC micropowder, and wherein meal mean particle size is 40～65 μ m, and fine powder mean particle size is 2～5 μ m, meal: the mass ratio of fine powder is 2～3:1;
The mean particle size of metal Ni micro mist is 2～3 μ m, and the mean particle size of Graphite Powder 99 is 25～60, nanometer carbon black mean particle size <35nm.
Described blade biscuit is to take nitrogen under the atmosphere of protection gas, ceramic blade green compact are being carried out to resin carbonation: 30～180 ℃ of intervals, 1～3 ℃/min of temperature rise rate; 180～320 ℃ of intervals, 1～1.5 ℃/min of temperature rise rate; 320 ℃ of insulation 120～150min; 320～800 ℃ of intervals, 2～3 ℃/min of temperature rise rate, 800 ℃ of insulation 60～80min; With stove, being chilled to room temperature takes out.
Blade biscuit is imbedded after silica flour, with 8～10 ℃/min temperature rise rate, be heated to 1600 ℃, be incubated 30～120min.
Compared with prior art, the present invention has following useful technique effect:
The invention provides a kind of performance controllable type SiC
fthe manufacture method of/SiC ceramic matrix composite turbine blade, adopt continuous SiC fiber as toughness reinforcing body, by Introduction To Stereolithography, manufacture fibrage guide support and blade minus mould, and continuous SiC fiber is woven with type according to guide support, obtain structure, direction, the controlled toughness reinforcing skeleton in inside of density, and solved the contraction problem of resin in polymerization, pyrolytic process by preparation high solid loading slurry, improve blade forming precision and mechanical property.
Performance controllable type SiC provided by the invention
fthe manufacture method of/SiC ceramic matrix composite turbine blade is compared with traditional 2D, 3D fibrage technology, can meet the preparation requirement of different size complex construction heterogeneous material member, can realize the inner conformal Reinforcement structure design of different size parts with complex structures, and free forming External Shape and inner support.Blade as shown in Figure 2, can the support with equal stress distributing line parallel (or vertical) in blade interior design, according to the size of stress, adjust fiber bundle diameters, distribution density and the space structure of toughness reinforcing body (SiC fiber), thus the material structure performance of design blade.
Performance controllable type SiC provided by the invention
fthe manufacture method of/SiC ceramic matrix composite turbine blade, adopting Polycarbosilane is SiC source, applies cracking process prepare fiber surface interfacial layer based on precursor, improved resistant fiber silicon erosion ability and with the bonding strength of ceramic matrix.
Performance controllable type SiC provided by the invention
fthe manufacture method of/SiC ceramic matrix composite turbine blade, has solved traditional material design and has adopted the method for analog calculation to investigate the relation between material property and each design variable, and problem that cannot verification experimental verification design rationality.The present invention is based on the inner reinforcement of rapid shaping technique manufactured materials supports, can realize the meticulous manufacture (precision reaches 50～100 μ m) of complex space topological framework, therefore realize and calculate simulation and test the method combining and investigate the relation between material property and each parameter, can carry out flexible manufacturing, for the Design & preparation of structured material is expanded novel method.
Accompanying drawing explanation
Fig. 1 is process flow diagram of the present invention.
Fig. 2 is inner support, and wherein 1 for having the supporter (playing the effect of guiding fibrage) of topological framework; 2 is supporter listrium (playing the effect fixing with minus mould).
Fig. 3 is turbine blade minus mould, and wherein 10 is cast gate; 20 is shell.
Fig. 4 is inner support vertical view.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail, and the explanation of the invention is not limited.
The present invention can manufacture the fiber reinforced ceramic matric composite part of complex construction, can realize freely manufacturing of Arbitrary 3 D part in theory.
Lower mask body is specifically described with the preparation of turbine blade.
Embodiment 1
Referring to Fig. 1, the preparation method of fiber reinforced SiC ceramic matrix composite turbine blade, comprises the following steps:
1. analyze part time job stress
First analyze the stress distribution of part under working conditions, according to the scope of stress, part is divided into different regions, the materials microstructure of different zones is different.Design meets the material cell structure of Introduction To Stereolithography feature, by analyzing the state of part under working conditions, obtains the performance requriements of its localized region material, respective material design criteria, the Weave parameters of reverse local material; By calculating each Regional Integration, finally obtain the model of stress equilibrium, this model can be considered the braiding model of reinforcement (SiC fiber), then by CAD modeling, obtains having the three-dimensional data of the fiber guide support of space topological structure.
2. the manufacture of inner support and negative shape mould
2.1 adopt 3 d modeling software to build blade interior supports, and as shown in Figure 2, Figure 4 shows, wherein 1 for having the supporter (playing the effect of guiding fibrage) of topological framework; 2 is supporter listrium (playing the effect fixing with minus mould).Then three-dimensional model being converted into STL formatted data preserves.
2.2 adopt delamination software Magics to carry out layering processing to three-dimensional model, and processing data is imported to photocureable rapid shaping machine RP manufacturing course.
2.3 blade interior that adopt Introduction To Stereolithography to produce blade support, and supporting mean diameter is 200～500 μ m.
By same step, produce the negative shape mould of blade, as shown in Figure 3, wherein 10 is cast gate; 20 is shell, and mould mean thickness is 0.6～1mm.
3. the preparation of ceramic size
3.1 liquid phase component preparations
Liquid phenolic resin and pore-forming material are held concurrently to thinner (ethylene glycol) according to 50:(65～100) mass ratio mixes.By changing pore-forming material addition, can realize controlledization of porous carbon support heterogeneous microstructure (porosity, pore size distribution, pore wall thickness) after resin matrix carbonization.
3.2 solid components preparations
Solid phase composition is that alpha-SiC micropowder (comprises meal and fine powder, 2～3:1), metal Ni micro mist (mean particle size 2～3 μ m), Graphite Powder 99 (mean particle size 25～60 μ m), nanometer carbon black (mean particle size <35nm) meal mean particle size 40～65 μ m, fine powder mean particle size 2～5 μ m, thickness powder quality umber ratio is:.Solid components SiC micro mist, metal Ni micro mist, Graphite Powder 99, nanometer carbon black parts by weight are respectively: 8.5 parts, 0.2 part, 0.3 part, 1 part.
By the above-mentioned liquid phase preparing and solid-phase material according to the ratio of volume ratio 45～65:100, put into silicon carbide ball grinder, adding quality is that the sodium polyacrylate of solid components 0.5～2% is made dispersion agent, after fully stirring, add silicon carbide ball-milling medium, with 360r/min rotating speed ball milling 45～120min, obtain the finely dispersed suspended nitride of solid phase particles.
4. prepare fiber interface layer
Polycarbosilane (PCS) and dimethylbenzene (xylene) are mixed with to 15～40%(massfraction, lower same) solution.The SiC micro mist (mean particle size 100nm) that adds solution quality 20～45% in 40%PCS-xylene solution, is mixed with SiC-PCS-xylene slurry.The SiC fiber reinforcement weaving is immersed in SiC-PCS-xylene slurry, is placed in vacuum tank, after vacuumizing, add ultrasonication, add air pressure 1.0MPa, pressurize 30min, to guarantee that steeping fluid fully enters fibrous bundle hole and is evenly coated on fiber surface.
After 1～5 circulation dipping, take out fiber reinforcement, dry 2h at 65～80 ℃, then make the Polycarbosilane interfacial layer of fiber surface completely crosslinked in 120～150 ℃ of insulation 12h.
There is the fiber reinforcement of Polycarbosilane to be placed in tube furnace surface-coated; logical Ar gas protection; speed with 2～5 ℃/min is warming up to 1200 ℃, and soaking time is 2h, and it is the SiC interfacial layer of 2～50 μ m that the Polycarbosilane cracking that makes to be coated in fiber surface generates thickness.
5. type vacuum injecting and forming
(vacuum tightness 6 * 10 in type vacuum injecting and forming machine
-2pa), slurry is stirred to 0.5h, then after after standing 1h, add solidifying agent benzene sulfonyl chloride (add-on be resol weight 4～8%), inject blade minus mould after then stirring 5min.
6. resin solidification
The blade product that completes notes type is positioned over and in 60 ℃ of thermostat containers, is incubated Procuring in 8 hours, more slowly rise to 180 ℃ and be incubated 6 hours and make resol completely curing with the temperature rise rate of 2 ℃/h.
7. resin carbonation
7.1 carry out in atmosphere box-type furnace, and pass into nitrogen protection.
7.2 temperature rise rates: 30～180 ℃ of intervals, 3 ℃/min of temperature rise rate; 180～320 ℃ of intervals, 1 ℃/min of temperature rise rate; 320 ℃ of insulation 120min; 320～800 ℃ of intervals, 2 ℃/min of temperature rise rate; 800 ℃ of insulation 60min.
7.3 are chilled to room temperature pickup with stove.
8. infiltration reaction in－situ
Blade biscuit is imbedded in the high-purity silicon powder of 1～2 times of quality, put into vacuum high-temperature sintering stove, with 6～10 ℃/min temperature rise rate, be heated to 1600 ℃, insulation 30～120min, liquid-state silicon is infiltrated in porous carbon support by capillary force, generate β-SiC with resin carbon and nano-sized carbon reaction in－situ, with stove, be chilled to room temperature pickup.
Referring to Fig. 1, the preparation method of fiber reinforced SiC ceramic matrix composite turbine blade, comprises the following steps:
3. the preparation of ceramic size
3.1 prefabricated solution preparations
The monomer that gel casting forming is used, linking agent are respectively acrylamide and N, N ＇-methylene-bisacrylamide.It is initiator that initiator adopts ammonium persulphate, and Tetramethyl Ethylene Diamine is catalyzer.Adopt sodium polyacrylate as dispersion agent.
First by monomer acrylamide (AM, analytical pure) and linking agent N, N ＇-methylene-bisacrylamide (MBAM, analytical pure), make the pre-mixing liquor that gel casting forming is used, the mass ratio of monomer and linking agent is 6～10:1, and the content of monomer and linking agent is 12～20% of solution total mass.
3.2 solid components preparations
2～3:1), nanometer carbon black (mean particle size <35nm) solid phase composition is that (meal mean particle size 40～65 μ m, fine powder mean particle size 2～5 μ m, thickness powder quality umber ratio is alpha-SiC micropowder:.Solid components SiC micro mist, Graphite Powder 99, nanometer carbon black parts by weight are respectively: 8.5 parts, 0.5 part, 1 part.
The above-mentioned liquid phase preparing and solid-phase material are put into silicon carbide ball grinder according to the ratio of volume ratio 45～60:100, adding weight is that the sodium polyacrylate liquid of solid phase composition 1～3% is made dispersion agent, after fully stirring, add silicon carbide ball-milling medium, with 240～360r/min rotating speed ball milling, 1～6h, obtain the finely dispersed water base suspended nitride of solid phase particles.
4. prepare fiber interface layer
Polycarbosilane (PCS) and dimethylbenzene (xylene) are mixed with to 15～40%(massfraction, lower same) solution.The SiC micro mist (mean particle size 100nm) that adds solution quality 25～30% in 30%PCS-xylene solution, is mixed with SiC-PCS-xylene slurry.The SiC fiber reinforcement weaving is immersed in SiC-PCS-xylene slurry, is placed in vacuum tank, after vacuumizing, add ultrasonication, add air pressure 5.0MPa, pressurize 30min, to guarantee that steeping fluid fully enters fibrous bundle hole and is evenly coated on fiber surface.
After 1～5 circulation dipping, take out fiber reinforcement, dry 2h at 50～65 ℃, then make the Polycarbosilane interfacial layer of fiber surface completely crosslinked in 130～145 ℃ of insulation 12h;
There is the fiber reinforcement of Polycarbosilane to be placed in tube furnace surface-coated; logical Ar gas protection; speed with 3～4 ℃/min is warming up to 1150 ℃, and soaking time is 1.5h, and it is the SiC interfacial layer of 2～50 μ m that the Polycarbosilane cracking that makes to be coated in fiber surface generates thickness.
5. type vacuum injecting and forming
(vacuum tightness 8 * 10 in type vacuum injecting and forming machine
-2), deaeration after standing 1h, rear interpolation initiator (30% ammonium persulfate aqueous solution) and catalyzer Tetramethyl Ethylene Diamine (the 25% Tetramethyl Ethylene Diamine aqueous solution), 0.5wt%～1wt% that initiator add-on is prefabricated solution, catalyzer add-on is 0.2wt%～0.5wt%., rapid stirring is the rear blade minus mould that injects evenly.
6. lyophilize
After monomer and the complete crosslinking curing of linking agent, part is put into refrigeration case in-30 ℃～-60 ℃ freezing 1～2h, make the complete freezing and crystallizing of moisture in green compact, then put into negative pressure of vacuum cabin, continue to vacuumize that (vacuum keep is 10 * 10
-3pa～5 * 10
-2pa) 12h～24h, distils crystal water completely, realizes drying purpose.
7. atmosphere degreasing
7.1 carry out in atmosphere box-type furnace, and pass into nitrogen protection.
7.2 temperature rise rates: 30～140 ℃ of intervals, 5 ℃/min of temperature rise rate; 140～320 ℃ of intervals, 2 ℃/min of temperature rise rate; 320～600 ℃ of intervals, 2 ℃/min of temperature rise rate; 600～800 ℃ of intervals, 5 ℃/min of temperature rise rate; 800 ℃ of insulation 60min.
7.3 are chilled to room temperature pickup with stove.
8. infiltration reaction in－situ
Blade biscuit is imbedded in the high-purity silicon powder of 1～2 times of quality, put into vacuum high-temperature sintering stove, with 6～10 ℃/min temperature rise rate, be heated to 1600 ℃, be incubated 30～120min, complete silico-carbo reaction infiltration, with stove, be chilled to room temperature pickup.
Claims (2)
1. a SiC
fthe preparation method of/SiC ceramic matrix composite turbine blade, is characterized in that, comprises the following steps:
1) state under working conditions according to turbine blade, obtains the performance requriements of its localized region material, respective material design criteria, and reverse obtains the Weave parameters of partial zones material;
2) by each Regional Integration, obtain design of part, the materials microstructure Integrated Model of ceramic matrix composite turbine blade, with light-curing quick moulding method, produce turbine blade shell mould and the guide support support with topological characteristic;
3) on prefabricated guide support support, weave SiC continuous fibre;
4) the guide support support that is woven with SiC continuous fibre being put into solid concentration is Polycarbosilane-xylene solution of 10～25%, carries out repeatedly vacuum impregnation-dry-crosslinking process;
5) adopt precursor to apply cracking process, at SiC continuous fibre surface preparation SiC interfacial layer;
6) the guide support support of fibrage is fixed in light-cured resin shell, cast ceramics slurry in type vacuum injecting and forming machine, obtains the ceramic blade green compact that there is SiC fiber reinforcement inside;
Being prepared as of described ceramic size:
By liquid phenolic resin with pore-forming material according to 50:(65～100) mass ratio mixes, and obtains liquid phase component;
The SiC micro mist of 6～8.5 parts, the metal Ni micro mist of 0.05～0.2 part, the Graphite Powder 99 of 0.1～0.3 part and the nanometer carbon black of 0.1～1 part are fully mixed, obtain solid components;
Solid components and liquid phase component are fully mixed, obtain ceramic size after ball milling according to the volume ratio of 45～65:100;
Liquid phase component is mixed with the dispersion agent sodium polyacrylate of solid components quality 1～2%, together put into silicon carbide ball grinder with solid components again, add silicon carbide ball-milling medium, with 300～360r/min rotating speed ball milling, 30～120min, obtain the finely dispersed ceramic size of solid phase particles;
0.5～1h before ceramic size notes type, also adds 4～8% benzene sulfonyl chloride of resin quality in ceramic size in ceramic size and stirs, vacuum exhaust 10～30min;
7) by ceramic blade green compact at 50～60 ℃ of Procuring 5～8h, then with the temperature rise rate of 1～2 ℃/h, rise to 180～200 ℃ and be incubated 3～6 hours and make it completely curing;
Then under protective atmosphere, ceramic blade green compact are warming up to 800 ℃ of organic crackings that make in base substrate, obtain blade biscuit;
8) blade biscuit is used after silicon embedding, be warming up to 1400～1600 ℃ and carry out reaction sintering, sintering 30～120min, makes liquid-state silicon infiltrate in blade biscuit by capillary force, generates β-SiC with resin carbon and nano-sized carbon reaction in－situ, obtains SiC after furnace cooling
f/ SiC ceramic matrix composite turbine blade.
2. SiC as claimed in claim 1
fthe preparation method of/SiC ceramic matrix composite turbine blade, is characterized in that, described turbine blade minus mould and the special guide support support of mould inside topology are:
The three-dimensional model that adopts CAD software building turbine blade minus mould and guide support support, is then converted into three-dimensional model STL formatted data; Adopt delamination software Magics to carry out layering processing to three-dimensional model, processing data is imported to photocureable rapid shaping manufacturing course SLARP; Adopt light-curing quick moulding method to produce minus mould and guide support support.
3
.siC as claimed in claim 1
fthe preparation method of/SiC ceramic matrix composite turbine blade, is characterized in that, continuous SiC fiber braiding is to use continuous SiC fiber bundle, and average fibre diameter 8～15 μ m, draw fibrous bundle with soft pin, on stent preform, weave.
4
.siC as claimed in claim 1
fthe preparation method of/SiC ceramic matrix composite turbine blade, is characterized in that, the described surface at continuous fibre is prepared SiC interfacial layer and is:
It is 15～40% PCS-xylene solution that Polycarbosilane and dimethylbenzene are mixed with to massfraction, adds the SiC micro mist that accounts for solution quality 20～45% in PCS-xylene solution, is mixed with SiC-PCS-xylene slurry;
The SiC fiber reinforcement weaving is immersed in SiC-PCS-xylene slurry, is placed in vacuum tank, after vacuumizing, add ultrasonication, add air pressure 1.0 MPa～10.0 MPa, pressurize 30 min, to guarantee that steeping fluid fully enters fibrous bundle hole and is evenly coated on fiber surface;
After completing dipping, take out fiber reinforcement, in air, in 50～80 ℃ of dry 1～2h, then it is oxidation cross-linked in 120～150 ℃ of insulation 8～12h, to complete Polycarbosilane;
The fiber reinforcement that is coated with Polycarbosilane, under protective atmosphere, is warming up to 1000～1200 ℃ with the speed of 2～5 ℃/min and carries out cracking, and soaking time is 1～2 h, makes inorganicization of Polycarbosilane that is coated in fiber surface generate SiC interfacial layer.
5
.siC as claimed in claim 1
fthe preparation method of/SiC ceramic matrix composite turbine blade, is characterized in that, described liquid phase component comprises that the molten heat-reactive phenolic resin of alcohol, ethylene glycol volume parts are respectively 3.0～5.5 parts, 5～7 parts;
SiC micro mist in solid components, metal Ni micro mist, Graphite Powder 99, nanometer carbon black mass fraction are respectively: 8～8.5 parts, 0.15～0.2 part, 0.2～0.3 part, 0.8～1 part.
6
.siC as claimed in claim 1
fthe preparation method of/SiC ceramic matrix composite turbine blade, is characterized in that, the preparation of the ceramic size of described step 6) replaces with:
Liquid phase component is by acrylamide and N, N ＇-methylene-bisacrylamide is that 6～10:1 mixes according to mass ratio, add initiator again, catalyzer is made, wherein acrylamide and N, total mass content of N ＇-methylene-bisacrylamide is liquid phase component 12～20%;
Solid components is by the SiC micro mist of 6～8.5 parts, the Graphite Powder 99 of 0.2～0.5 part and the nanometer carbon black of 0.1～1 part are fully mixed;
Solid components and liquid phase component are fully mixed, obtain ceramic size after ball milling according to the volume ratio of 45～65:100;
Before ceramic size notes type, also the initiator of ceramic size and its quality 0.5～1%, 0.2～0.5% catalyzer are fully stirred.
7
.siC as claimed in claim 6
fthe preparation method of/SiC ceramic matrix composite turbine blade, it is characterized in that, liquid phase component is mixed with the dispersion agent sodium polyacrylate of solid components quality 1～2%, together put into silicon carbide ball grinder with solid components again, add silicon carbide ball-milling medium, with 300～360r/min rotating speed ball milling, 30～120min, obtain the finely dispersed ceramic size of solid phase particles;
Described SiC micro mist is the mixing of meal alpha-SiC micropowder and fine powder alpha-SiC micropowder, and wherein meal mean particle size is 40～65 μ m, and fine powder mean particle size is 2～5 μ m, meal: the mass ratio of fine powder is 2～3:1;
The mean particle size of Graphite Powder 99 is 25～60 μ m, nanometer carbon black mean particle size <35nm.
8
.siC as claimed in claim 1
fthe preparation method of/SiC ceramic matrix composite turbine blade, it is characterized in that, liquid phase component is mixed with the dispersion agent sodium polyacrylate of solid components quality 1～2%, together put into silicon carbide ball grinder with solid components again, add silicon carbide ball-milling medium, with 300～360r/min rotating speed ball milling, 30～120min, obtain the finely dispersed ceramic size of solid phase particles;
Described SiC micro mist is the mixing of meal alpha-SiC micropowder and fine powder alpha-SiC micropowder, and wherein meal mean particle size is 40～65 μ m, and fine powder mean particle size is 2～5 μ m, meal: the mass ratio of fine powder is 2～3:1;
The mean particle size of metal Ni micro mist is 2～3 μ m, and the mean particle size of Graphite Powder 99 is 25～60 μ m, nanometer carbon black mean particle size <35nm.
9
.siC as claimed in claim 1
fthe preparation method of/SiC ceramic matrix composite turbine blade, is characterized in that, described blade biscuit is to take nitrogen under the atmosphere of protection gas, ceramic blade green compact are being carried out to resin carbonation: 30～180 ℃ of intervals, 1～3 ℃/min of temperature rise rate; 180～320 ℃ of intervals, 1～1.5 ℃/min of temperature rise rate; 320 ℃ of insulation 120～150min; 320～800 ℃ of intervals, 2～3 ℃/min of temperature rise rate, 800 ℃ of insulation 60～80min; With stove, being chilled to room temperature takes out.
10
.siC as claimed in claim 1
fthe preparation method of/SiC ceramic matrix composite turbine blade, is characterized in that, blade biscuit is imbedded after silica flour, with 8～10 ℃/min temperature rise rate, is heated to 1600 ℃, is incubated 30～120min.
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| CN103553616B (en) * | 2013-10-23 | 2016-03-23 | 中国科学院上海硅酸盐研究所 | Growth in situ SiC nanowire strengthens C/SiC matrix material and preparation method thereof |
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| CN104496508B (en) * | 2014-12-01 | 2016-08-17 | 西安交通大学 | Manufacture method based on the SiC ceramic base turbine blade that photocuring 3D prints |
| CN104529458B (en) * | 2014-12-01 | 2016-08-17 | 西安交通大学 | The manufacture method of high-performance SiC ceramic based composites blade of aviation engine |
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| CN110143824B (en) * | 2019-05-29 | 2020-07-10 | 中南大学 | Non-residual stress homogeneous high-temperature-resistant SiCfPreparation method of/SiC turbine integral blade disc |
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| CN113698220A (en) * | 2021-09-26 | 2021-11-26 | 中国科学院长春光学精密机械与物理研究所 | Preparation method of fiber-reinforced silicon carbide composite material and fiber-reinforced silicon carbide composite material |
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