CN1793054A - Process for preparing heat guarding plate of Cf/SiC high temp, resistant and washing resistant by pioneer method - Google Patents
Process for preparing heat guarding plate of Cf/SiC high temp, resistant and washing resistant by pioneer method Download PDFInfo
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- CN1793054A CN1793054A CN 200510032364 CN200510032364A CN1793054A CN 1793054 A CN1793054 A CN 1793054A CN 200510032364 CN200510032364 CN 200510032364 CN 200510032364 A CN200510032364 A CN 200510032364A CN 1793054 A CN1793054 A CN 1793054A
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Abstract
The invention relates to precursor method to make C<SUB>f</SUB>/SiC high temperature resistance anti scour thermal protection board. The process includes the following steps: dipping carbon fiber fabric in vacuum into organic silicon precursor solution, putting to graphite mould to gain blank after crosslink, getting pre-mould after de-mouding; making precurcor solution and getting into the pore of the component to take cracking under high temperature; after density reaching 1.60g/cm<SUP>3</SUP>, adopting slurry dipping and cracking; using polusiloxane as precursor, divinyl benzene as curing agent to make solution, dipping the board into the solution, solidifying in oven to gain final production. The method has simple device, short manufacturing cycle, and suitable to take mass production.
Description
Technical field:
The present invention relates to the organosilicon polymer is precursor, adopts precursor infiltration and pyrolysis (PIP) prepared continuous carbon fibre fabric to strengthen silicon carbide (C
f/ SiC) the method for the high temperature resistant antiscour thermal protection sheet of matrix material.
Background technology:
Thermal protection is one of the critical problem in many fields such as aerospace, weaponry.The applied environment difference, the selection of thermo-lag method and thermally protective materials is also different.In many applied environments, to be thermal protection system also be accompanied by washing away of high velocity air (particle) standing pyritous to a Ke Ke class simultaneously the most.But this class applied environment is a lot, as sending out missile armament platform thermal protection system, hypersonic aircraft windward side (comprising wing plate, air rudder leading edge, nose cone etc.), space shuttle top layer thermal protection system, punching engine thermal protection wall etc. admittedly.
To send out missile armament platform thermal protection system admittedly is example, admittedly send out guided missile have simple in structure, reliability is high, cost is lower, maneuvering ability is good, launch preparation time is short, viability is stronger, advantage such as easy to use, is the developing direction of strategy and tactics guided missile.During the solid missile emission, the fuel gas temperature that SOLID PROPELLANT COMBUSTION is emitted is up to more than 3000 ℃, gas flow rate also reaches more than the 1000m/s, and solids content is higher in the combustion gas, and this performance such as high temperature resistant anti-particle erosion to weapon platform has proposed very high requirement.Existing weapon platform is difficult to adapt to such rigorous environment, therefore is necessary it is implemented thermal protection.At present generally adopt the method for coated with resins to protect, have obviously that anti-ablation property is poor, thermal conductivity is than problems such as height, the thermal protection effect is relatively poor.And Continuous Fiber Reinforced Ceramic Matrix Composites has the strong and high tenacity of low density, height ratio, excellent properties such as high temperature resistant, corrosion-resistant, can better satisfy the service requirements of high temperature resistant anti-particle erosion thermally protective materials.
At present, with C
f/ SiC is that the ceramic matric composite preparation technology of representative mainly contains chemical vapour deposition and two kinds of methods of organosilicon precursor infiltration and pyrolysis.And which kind of technology no matter, prepared C
fThe equal cost of/SiC matrix material is very high, and this has greatly limited its range of application.Use as thermally protective materials, large usage quantity has also proposed certain requirement to the cost of material.
Summary of the invention:
Technical problem solved by the invention is to utilize the organosilicon precursor to be raw material, is wild phase with the continuous carbon fibre fabric, and it is good to adopt the PIP prepared to go out mechanical property, surfacing, good weatherability, high temperature resistant scour resistance is good, and lower-cost precursor legal system is equipped with C
fThe method of/SiC is high temperature resistant antiscour thermal protection sheet.
The present invention adopts following technical scheme to solve the problems of the technologies described above:
(1) preparation of preform: with organosilicon precursor solution vacuum impregnation carbon fibre fabric, to flood good carbon fibre fabric then spreads in the graphite jig, the crosslinked base substrate that obtains after the mold pressing, obtain preform after the cracking demoulding, owing to easily produce distortion during the base substrate cracking, thus base substrate must cracking after just the demoulding to guarantee C
fThe planeness of/SiC thermal protection sheet;
(2) thermal protection sheet densification: organosilicon polymer is that solvent is made precursor solution with dimethylbenzene, the precursor mass concentration is controlled at 40～80%, precursor solution enters the member hole by vacuum or impregnating by pressure, cracking at high temperature then, and cracking temperature is controlled at 800～1600 ℃; This infiltration pyrolysis process need repeat 5～10 cycles;
(3) the mud infiltration pyrolysis is handled: thermal protection sheet density reaches 1.60g/cm
3Mud dipping-cracking is adopted in above back, mud is obtained by precursor, solvent, SiC micro mist ball milling, wherein, precursor can be Polycarbosilane or polysiloxane, solvent can be Vinylstyrene or dimethylbenzene, three's mass ratio is (30～50): (30～50): (20～30), steeping process are adopted vacuum impregnation or impregnating by pressure equally, and cracking temperature is controlled at 800～1600 ℃; Repeat this process 2～6 times;
(4) aftertreatment: with the polysiloxane is precursor, with the Vinylstyrene is that solidifying agent is configured to solution, both mass ratioes are controlled at (1.5～2.5): 1, with this solution for vacuum heat of immersion protective shield, and then in baking oven, solidify, solidification value is controlled at 100～300 ℃, is controlled at set time 2～12 hours.
The concrete preparation technology of described preform is: with Polycarbosilane, Vinylstyrene is configured to slurry by mass ratio at 2: 1, vacuum impregnation carbon fibre fabric (two dimension or three-dimensional carbon fibre fabric), the carbon fibre fabric that dipping is good is spread in the mould, be molded into base substrate under 3～5MPa pressure on the press, crosslinked back cracking, the demoulding obtains C
f/ SiC preform is cleared up maintenance so that use next time to mould after the demoulding is finished.
Described organosilicon polymer precursor is Polycarbosilane or polysiloxane, and solvent is a dimethylbenzene.
The cracking heat-up rate is controlled at 20～50 ℃/min.
Fortifying fibre is a carbon fibre fabric, and carbon fiber adopts polypropylene cyano group carbon fiber.
Present method both had been applicable to the preparation of tabular component, also went for the preparation of complex shaped components; Both be applicable to the preparation of thermally protective materials, also gone for the preparation of thermal structure material.
The present invention is with precursor infiltration and pyrolysis prepared C
f/ SiC matrix material thermal protection sheet, for density and the mechanical property that improves material, in conjunction with vacuum impregnation and heating and pressurizing impregnation technology, vacuum impregnation equipment is simple, is fit to dipping low viscosity precursor solution; And for the bigger precursor of viscosity, dipping apply during precursor solution certain pressure (4～20MPa), can make that precursor is as much as possible to be impregnated into material and to be converted into ceramic matrix.
In order to make precursor be converted into pottery, flood the thermal protection sheet cracking at high temperature of precursor, cracking temperature is controlled at 800～1600 ℃; In order to shorten preparation cycle, adopt cracking temperature rise rate (20～50 ℃/min) to shorten preparation cycle, reduce the time that fiber at high temperature experiences are improved the flexural strength and the fracture toughness property of material faster simultaneously.The present invention has following advantage:
(1) equipment requirements is simple: the equipment that whole process is mainly concerned with comprises vacuum and equipment such as high pressure steeping device, high-temperature cracking furnace and autoclave.Preparation process does not have corrosion to equipment, environmentally safe.
(2) preparation cycle is short: the technology of the present invention prepares C
fThe cycle of/SiC matrix material thermal protection sheet is no more than 20 days.
(3) product is fit to produce in batches, and batch property is good: the present invention adopts liquid impregnation technology, can fully realize the homogeneity of product performance.Simultaneously, dipping and cracking all can a plurality of samples of primary treatment, can realize batch process on the one hand, also can guarantee the quality of product batches on the other hand.
(4) excellent product performance: the C of the present invention's preparation
f/ SiC thermal protection sheet has many excellent properties, comprising:
A) thermal protection sheet has mechanical property preferably: flexural strength is greater than 600MPa, and fracture toughness property is greater than 27MPam
1/2
B) thermal protection sheet has high temperature thermal shock resistance energy preferably: experience crooked strength retention ratio 〉=80% after 10 1300 ℃ ← → 20 ℃ thermal shocks.
C) thermal protection sheet has excellent high-temperature oxidation resistance: after antioxidation treatment, 1500 ℃ of following oxidations are 10 minutes in air, and strength retention ratio is all greater than 98%.
D) thermal protection sheet has anti-preferably ablation property: adopt oxy-acetylene flame test (with reference to GJB-96 323A standard), the mass ablative rate of material is 1.57 * 10
-3G/s.
E) the thermal protection sheet material has thermal characteristics preferably: by test and calculating, the thermal conductivity of material is 1.59W/mK under the normal temperature.The thermal conductivity of material is lower, is suitable as thermally protective materials and uses.
F) thermal protection sheet has excellent weather resistance: material is placed 180 days strength of materials retention rates near 100% in air.
G) thermal protection sheet has high temperature resistant preferably erosion resistibility: thermal protection sheet has excellent high temperature resistant anti-airflow scouring ability, washes away environment examination back C at high temperature gas flow
f/ SiC thermal protection sheet structure is kept perfectly, and smooth surface does not have obvious ablation vestige; Thermal protection sheet has high temperature resistant preferably anti-particle erosion ability, at high temperature particle erosion environment examination back C
f/ SiC thermal protection sheet structure all is kept perfectly.
Embodiment:
Embodiment 1:
Preparation:
(1) preparation C
f/ SiC preform: Polycarbosilane, Vinylstyrene are configured to solution by mass ratio at 2: 1, cut out good two-dimentional carbon fibre fabric with the solution for vacuum dipping, behind the dipping 60min carbon fibre fabric being taken out the shop goes in the graphite jig, mold pressing 10min under 5MPa, 120 ℃ of crosslinking curing 1000 ℃ of cracking in high-temperature cracking furnace again after 4 hours in baking oven, the demoulding obtains C
f/ SiC preform is cleared up so that use next time mould after the demoulding is finished.Preform density is 1.04g/cm
3
(2) Polycarbosilane, dimethylbenzene are configured to solution by mass ratio at 50: 50, with this solution for vacuum dipping C
f/ SiC thermal protection sheet, Pintsch process then, cracking temperature is controlled at 1000 ℃.7 infiltration pyrolysis processes make density reach 1.71g/cm repeatedly
3
(3) Polycarbosilane, dimethylbenzene, SiC micro mist are configured to slurry by mass ratio at 30: 50: 20, continue vacuum and high-pressure impregnation C with mud
f/ SiC thermal protection sheet, 1000 ℃ of cracking then.4 infiltration pyrolysis processes make density near 1.96g/cm repeatedly
3
(4) polysiloxane and Vinylstyrene are mixed with solution by mass ratio at 2: 1.Then by vacuum impregnation, 120 ℃ of crosslinking curings 4 hours in baking oven at last.The unnecessary cured product of removing the surface obtains 2D C
f/ SiC thermal protection sheet.
Ground run examination 1:
(1) operating mode: adopt the 75mm solid propellant rocket, solid aluminium content 15wt% in the propelling agent, time 3s.Thermal protection sheet is vertical with the combustion gas direction, apart from engine export 25mm.In the actual examination, the fuel gas temperature of contact thermal protection sheet is about 1500K, and gas flow rate is about 1000m/s.
(2) result of appraisal: the thermal protection sheet structure is kept perfectly, but because thermal protection sheet and engine export are nearer, contain more solids in the combustion gas, be subjected to more serious particle erosion during the thermal protection sheet examination, maximum ablation scour depth reached 0.72mm after the thermal protection sheet examination was finished.
Ground run examination 2:
(1) operating mode: adopt liquid oxygen/kerosene double elements engine, thermal protection sheet is identical with air flow line.The fuel gas temperature of contact thermal protection sheet is about 1300K, and gas flow rate is about 800m/s.
(2) result of appraisal: the thermal protection sheet structure is kept perfectly, and the surface does not have obviously ablation and washes away vestige.
Ground run examination 3:
(1) operating mode: adopt liquid oxygen/kerosene double elements engine, thermal protection sheet is identical with air flow line.The fuel gas temperature of contact thermal protection sheet is about 2200K, and gas flow rate is about 1200m/s.
(2) result of appraisal: the thermal protection sheet structure is destroyed, and layering occurs.
Embodiment 2:
Preparation:
(1) preparation C
f/ SiC preform: Polycarbosilane, Vinylstyrene are configured to solution by mass ratio at 2: 1, flood three-dimensional carbon fiber preform with solution for vacuum, behind the dipping 60min carbon fibre fabric being taken out the shop goes in the graphite jig, mold pressing 10min under 5MPa, 120 ℃ of crosslinking curing 1000 ℃ of cracking in high-temperature cracking furnace again after 4 hours in baking oven, the demoulding obtains C
f/ SiC preform is cleared up so that use next time mould after the demoulding is finished.Preform density is 1.14g/cm
3
(2) Polycarbosilane, dimethylbenzene are configured to solution by mass ratio at 60: 40, with this solution impregnating by pressure C
f/ SiC thermal protection sheet, impregnation pressure is controlled at 4MPa, and then 1000 ℃ of Pintsch processs.7 impregnating by pressure cracking process make density reach 1.78g/cm repeatedly
3
(3) Polycarbosilane, dimethylbenzene, SiC micro mist are configured to slurry by mass ratio at 30: 50: 20, continue high-pressure impregnation C with mud
f/ SiC thermal protection sheet, impregnation pressure is controlled at 4MPa, and then 1000 ℃ of Pintsch processs.4 infiltration pyrolysis processes make density near 2.01g/cm repeatedly
3
(4) polysiloxane and Vinylstyrene are mixed with solution by mass ratio at 2: 1.Then by vacuum impregnation, 120 ℃ of crosslinking curings 4 hours in baking oven at last.The unnecessary cured product of removing the surface obtains 3D C
f/ SiC thermal protection sheet.
Ground run examination 1:
(1) operating mode: adopt the 75mm solid propellant rocket, solid aluminium content 15wt% in the propelling agent, time 3s.Thermal protection sheet is apart from engine export 25mm.In the actual examination, the fuel gas temperature of contact thermal protection sheet is about 1500K, and gas flow rate is about 1000m/s.
(2) result of appraisal: the thermal protection sheet structure is kept perfectly, and shows good high temperature resistant anti-particle erosion ability, and maximum ablation scour depth was 0.14mm after the thermal protection sheet examination was finished.
Ground run examination 2:
(1) operating mode: adopt liquid oxygen/kerosene double elements engine, thermal protection sheet is identical with air flow line.The fuel gas temperature of contact thermal protection sheet is about 2200K, and gas flow rate is about 1200m/s.
(2) result of appraisal: the thermal protection sheet material structure is kept perfectly, and shows excellent high temperature resistant anti-airflow scouring ability, and the rear surface is finished in the thermal protection sheet examination is not had obvious ablation vestige.
Embodiment 3:
Preparation:
(1) preparation C
f/ SiC preform: Polycarbosilane, Vinylstyrene are configured to solution by mass ratio at 2: 1, cut out good two-dimentional carbon fibre fabric with the solution for vacuum dipping, behind the dipping 60min carbon fibre fabric being taken out the shop goes in the graphite jig, mold pressing 10min under 4MPa, 120 ℃ of crosslinking curing 1300 ℃ of cracking in high-temperature cracking furnace again after 4 hours in baking oven, the demoulding obtains C
f/ SiC preform is cleared up so that use next time mould after the demoulding is finished.Preform density is 0.98g/cm
3
(2) Polycarbosilane, dimethylbenzene are configured to solution by mass ratio at 50: 50, with this solution for vacuum dipping C
f/ SiC thermal protection sheet, 1300 ℃ of Pintsch processs then.6 infiltration pyrolysis processes make density reach 1.65g/cm repeatedly
3
(3) Polycarbosilane, dimethylbenzene, SiC micro mist are configured to slurry by mass ratio at 25: 50: 25, continue vacuum and high-pressure impregnation C with mud
f/ SiC thermal protection sheet, Pintsch process then.5 infiltration pyrolysis processes make density near 2.02g/cm repeatedly
3
(4) polysiloxane and Vinylstyrene are mixed with solution by mass ratio at 2: 1.Then by vacuum impregnation, 150 ℃ of crosslinking curings 3 hours in baking oven at last.The unnecessary cured product of removing the surface obtains 2D C
f/ SiC thermal protection sheet.
Simulation test run examination:
Operating mode: adopt the 200mm solid propellant rocket, solid aluminium content 20wt% in the propelling agent, time 2s.Thermal protection sheet is apart from engine export 70mm.In the actual examination, the fuel gas temperature of contact thermal protection sheet is about 2000K, and gas flow rate is about 1100m/s.
The result of appraisal: the thermal protection sheet structure is kept perfectly, and shows anti-preferably ablation property, and the maximum ablation scour depth in examination back is 0.6mm.
Embodiment 4 (4
#The preparation of thermal protection sheet and examination):
(1) preparation C
f/ SiC preform: Polycarbosilane, Vinylstyrene are configured to solution by mass ratio at 2: 1, cut out good two-dimentional carbon fibre fabric with the solution for vacuum dipping, behind the dipping 60min carbon fibre fabric being taken out the shop goes in the graphite jig, mold pressing 10min under 3MPa, 120 ℃ of crosslinking curing 1600 ℃ of cracking in high-temperature cracking furnace again after 4 hours in baking oven, the demoulding obtains C
f/ SiC preform is cleared up so that use next time mould after the demoulding is finished.Preform density is 0.94g/cm
3
(2) Polycarbosilane, dimethylbenzene are configured to solution by mass ratio at 50: 50, with this solution for vacuum dipping C
f/ SiC thermal protection sheet, 1000 ℃ of Pintsch processs then.5 infiltration pyrolysis processes make density reach 1.60g/cm repeatedly
3
(3) Polycarbosilane, dimethylbenzene, SiC micro mist are configured to slurry by mass ratio at 25: 45: 30, continue vacuum and high-pressure impregnation C with mud
f/ SiC thermal protection sheet, 1000 ℃ of Pintsch processs then.6 infiltration pyrolysis processes make density near 2.06g/cm repeatedly
3
(4) polysiloxane and Vinylstyrene are mixed with solution by mass ratio at 2.5: 1.Then by vacuum impregnation, 200 ℃ of crosslinking curings 4 hours in baking oven at last.The unnecessary cured product of removing the surface obtains 2D C
f/ SiC thermal protection sheet.
Simulation test run examination:
Operating mode: adopt the 200mm solid propellant rocket, solid aluminium content 20wt% in the propelling agent, time 2s.Thermal protection sheet is apart from engine export 85mm.In the actual examination, the fuel gas temperature of contact thermal protection sheet is about 2000K, and gas flow rate is about 1100m/s.
The result of appraisal: the thermal protection sheet structure is kept perfectly, and shows good anti-ablation property, and the maximum ablation scour depth in examination back is 0.5mm.
Application:
Present method is applied to precursor method C
fThe preparation of/SiC is high temperature resistant antiscour thermal protection sheet has carried out taking all factors into consideration and process optimization the C that obtains to mechanical property, antioxidant property, anti-ablation property, weather resistance and the scour resistance of material
f/ SiC matrix material thermal protection sheet has low density, height ratio strong and high tenacity, anti-oxidant, anti-ablation and antiscour, excellent many excellent properties such as corrosion-resistant and weathering resistance, and the thermally protective materials and the thermal structure material that especially are suitable as fields such as space flight and aviation, weaponry use.Preparation technology is very flexible, and equipment requirements is simple, also can prepare the comparatively member of complicated shape simultaneously.
Claims (7)
1, a kind of precursor legal system is equipped with C
fThe method of/SiC is high temperature resistant antiscour thermal protection sheet is characterized in that:
(1) preparation of preform: with organosilicon precursor solution vacuum impregnation carbon fibre fabric, will flood good carbon fibre fabric then and spread in the graphite jig, the crosslinked base substrate that obtains after the mold pressing obtains preform after the cracking demoulding;
(2) thermal protection sheet densification: organosilicon polymer is that solvent is made precursor solution with dimethylbenzene, the precursor mass concentration is controlled at 40～80%, precursor solution is by vacuum or be forced into 4～20MPa dipping and enter the member hole, cracking at high temperature then, cracking temperature are controlled at 800～1600 ℃; This infiltration pyrolysis process need repeat 5～10 cycles;
(3) the mud infiltration pyrolysis is handled: thermal protection sheet density reaches 1.60g/cm
3Mud dipping-cracking is adopted in above back, mud is obtained by precursor, solvent, SiC micro mist ball milling, wherein, precursor can be Polycarbosilane or polysiloxane, solvent can be Vinylstyrene or dimethylbenzene, three's mass ratio is 30～50: 30～50: 20～30, and steeping process adopts vacuum impregnation equally or is forced into 4～20MPa dipping, and cracking temperature is controlled at 800～1600 ℃; Repeat this process 2～6 times;
(4) aftertreatment: with the polysiloxane is precursor, with the Vinylstyrene is that solidifying agent is configured to solution, both are controlled at 1.5～2.5 by mass ratio: 1, with this solution for vacuum heat of immersion protective shield, and then in baking oven, solidify, solidification value is controlled at 100～300 ℃, is controlled at set time 2～12 hours.
2, precursor legal system according to claim 1 is equipped with C
fThe method of/SiC is high temperature resistant antiscour thermal protection sheet, it is characterized in that: the concrete preparation technology of described preform is: with Polycarbosilane, Vinylstyrene is configured to solution by mass ratio at 2: 1, vacuum impregnation two dimension or three-dimensional carbon fibre fabric, the carbon fibre fabric that dipping is good is spread in the mould, is molded into base substrate under 3～5MPa pressure on the press, crosslinked back cracking, cracking temperature is controlled at 800～1600 ℃, and the demoulding obtains C
f/ SiC preform is cleared up maintenance so that use next time to mould after the demoulding is finished.
3, precursor legal system according to claim 1 and 2 is equipped with C
fThe method of/SiC is high temperature resistant antiscour thermal protection sheet, it is characterized in that: described organosilicon polymer precursor is Polycarbosilane or polysiloxane.
4, precursor legal system according to claim 1 and 2 is equipped with C
fThe method of/SiC is high temperature resistant antiscour thermal protection sheet, it is characterized in that: the cracking heat-up rate is controlled at 20～50 ℃/min.
5, precursor legal system according to claim 1 and 2 is equipped with C
fThe method of/SiC is high temperature resistant antiscour thermal protection sheet, it is characterized in that: fortifying fibre is a carbon fibre fabric, carbon fiber adopts polypropylene cyano group carbon fiber.
6, precursor legal system according to claim 1 and 2 is equipped with C
fThe method of/SiC is high temperature resistant antiscour thermal protection sheet, it is characterized in that: preform is tabular component or complex shaped components.
7, a kind of precursor legal system as claimed in claim 2 is equipped with C
fThe method of/SiC is high temperature resistant antiscour thermal protection sheet, it is characterized in that: described method is applicable to the preparation of thermal structure material.
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|---|---|---|---|
| CNB2005100323649A CN100503518C (en) | 2005-11-11 | 2005-11-11 | Process for preparing heat guarding plate of Cf/SiC high temp, resistant and washing resistant by pioneer method |
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|---|---|---|---|
| CNB2005100323649A CN100503518C (en) | 2005-11-11 | 2005-11-11 | Process for preparing heat guarding plate of Cf/SiC high temp, resistant and washing resistant by pioneer method |
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| CN1793054A true CN1793054A (en) | 2006-06-28 |
| CN100503518C CN100503518C (en) | 2009-06-24 |
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