CN105566919A - Carbon cloth and heat-vulcanized silicone rubber based ablation-resistant composite material and preparation method thereof - Google Patents
Carbon cloth and heat-vulcanized silicone rubber based ablation-resistant composite material and preparation method thereof Download PDFInfo
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Abstract
A carbon cloth and heat-vulcanized silicone rubber based ablation-resistant composite material is composed of heat-vulcanized silicone rubber, a reinforcing agent, fibers, an ablation-resistant filler, a vulcanizing agent, a silane coupling agent, hydroxyl silicone oil, polyborodiphenylsiloxane prepolymer and carbon fiber cloth. The preparation method includes: 1, preparing materials; 2, adding the materials into a double-roller blender mill to realize plasticating and mixing; 3, performing primary vulcanization treatment; 4, performing secondary vulcanization treatment; 5, impregnating the carbon fiber cloth; 6, taking out the carbon fiber cloth, and adhering the carbon fiber cloth to the surface of a heat-vulcanized silicone rubber based ablation-resistant material; 7, putting the heat-vulcanized silicone rubber based ablation-resistant material on a flat-plate vulcanizing machine, performing point pressurizing, taking out, and cooling to the room temperature to obtain a carbon cloth and heat-vulcanized silicone rubber based ablation-resistant composite material with one carbon fiber cloth layer attached to the surface; 8, repeating the step 5-7 to obtain the carbon cloth and heat-vulcanized silicone rubber based ablation-resistant composite material with 2-5 carbon fiber cloth layers attached to the surface.
Description
Technical field
The present invention relates to field of high polymer composite material preparation, particularly relate to a kind of heat insulation protective material of resistance to ablation that can be used on aerospace field and preparation method thereof.
Background technology
Aerospacecraft and guided missile all be unable to do without thrust-augmented rocket, and Ducted rocket is exactly a kind of important thrust device, and it can effectively utilize the oxygen in air as the primary oxidant of solid fuel ignition, for spacecraft flight provides lasting power.Solid rocket ramjet is made up of parts such as combustion chamber, jet pipe and lighter for ignitions, and every part all needs excellent resistance toheat.Ducted rocket Working environment is extremely severe, and during combustion chamber operational, propellant combustion produces nearly 4000 DEG C of high temperature, and pressure reaches mach one up to 1200 normal atmosphere, gas velocities.This just proposes high requirement to the thermal protection of Ducted rocket.Between combustion chamber and housing, have one deck thermofin, Main Function prevents housing from high temperature breaking, and therefore the material of resistance to ablating heat shield is the important component part of aerospacecraft.
Thermal insulation material is except requiring that having excellent ablation resistance also should have certain flexibility, therefore main based on the flexible ablation resistant material of rubber-like.But because paracril ozone resistance is poor, processing performance is complicated, and terpolymer EP rubber polarity is poor, and charring rate is low, and many disadvantages makes this bi-material start to meet the development of spationautics.Silicon rubber has great potentiality in resistance to ablation, carries out the research of silicone rubber based thermal insulation material significant.
By adding the method that stuffing means is most convenient, the most directly raising rubber ablation property, for improving silica-based thermal insulation material ablation resistance, scholars are studied the filler of resistance to ablation.Fibrous packing has critical role in silicon rubber ablation resistant material, is widely used in silicone rubber based resistance to ablative composite material always.Rubber matrix itself cannot meet ultrahigh-temperature ultra-high voltage short period of time working conditions, must by fillers such as the various fibers of resistance to ablation to provide resistance to ablation, the scour resistance of material.The use of new and effective resistance to ablation cloth makes rubber matrix degrade slowly, but obviously can reduce the mechanical property of material simultaneously, and the tensile yield of material is reduced.By to researchs such as fiber, nanometer inorganic filler, fire retardants, improve hot-vulcanized silicone rubber material ablation resistance and over-all properties.
Summary of the invention
A kind of carbon cloth compound thermal sulphurated siliastic base ablation resistant material provided by the present invention, material composition comprises: hot-vulcanized silicone rubber, strengthening agent, fiber, the filler of resistance to ablation, vulcanizing agent, silane coupling agent, hydroxy silicon oil, poly-phenylbenzene Borosiloxane performed polymer and carbon cloth, concrete massfraction proportioning is: hot-vulcanized silicone rubber 100 mass parts, strengthening agent 5 ~ 50 mass parts, fiber 1 ~ 30 mass parts, the filler of resistance to ablation 1 ~ 20 mass parts, vulcanizing agent 1 ~ 3 mass parts, silane coupling agent 0.01 ~ 0.1 mass parts, hydroxy silicon oil 0.01 ~ 0.5 mass parts, poly-phenylbenzene Borosiloxane performed polymer 1 ~ 5 mass parts, carbon cloth 1 ~ 5 layer.Described hot-vulcanized silicone rubber adopt in methyl vinyl silicone rubber and methyl phenyl vinyl silicone rubber one or both.Described strengthening agent is gas-phase silica or precipitated silica.The described inorganic filler of resistance to ablation is one or more in zirconium boride 99.5004323A8ure, zirconium white, magnesium oxide and silicon carbide, and granularity is 200nm ~ 500 μm.Described fiber is one or more in carbon fiber, pbo fiber and aramid fiber.Described vulcanizing agent is one or both in 2,5-dimethyl-2,5-bishexane and dicumyl peroxide.
A preparation method for carbon cloth compound thermal sulphurated siliastic base ablation resistant material, is characterized in that comprising the following steps:
Step 1: prepare burden according to hot-vulcanized silicone rubber 100 mass parts, strengthening agent 5 ~ 50 mass parts, fiber 1 ~ 30 mass parts, the filler of resistance to ablation 1 ~ 20 mass parts, vulcanizing agent 1 ~ 3 mass parts, silane coupling agent 0.01 ~ 0.1 mass parts, hydroxy silicon oil 0.01 ~ 0.5 mass parts, poly-phenylbenzene Borosiloxane performed polymer 1 ~ 5 mass parts and carbon cloth 1 ~ 5 layer;
Step 2: add hot-vulcanized silicone rubber, strengthening agent, hydroxy silicon oil, fiber, the filler of resistance to ablation, vulcanizing agent and silane coupling agent successively in two roller mill, plasticate and mix, room temperature places 24 hours;
Step 3: the mixture processed through step 2 is placed in mould, carries out a sulfidizing 10-30min under be 5-10MPa and temperature being the condition of 170-190 DEG C with vulcanizing press at pressure;
Step 4: be placed in baking oven through step 3 process, carry out post cure process 1.8 ~ 2.0h under the condition of 190-210 DEG C, obtained hot-vulcanized silicone rubber base ablation resistant material;
Step 5: poly-phenylbenzene Borosiloxane performed polymer is heated to 220 ~ 260 DEG C to molten state, after melting, dip treating is carried out 1 ~ 8 minute to carbon cloth;
Step 6: take out the carbon cloth after dipping, adhered to the surface being compounded in hot-vulcanized silicone rubber base ablation resistant material, room temperature is placed 1 ~ 10 minute;
Step 7: the hot-vulcanized silicone rubber base ablation resistant material after processing through step 6 is placed on vulcanizing press, it is 180 ~ 220 DEG C in temperature, pressure is press 3 ~ 5 times under the condition of 0.1 ~ 1MPa, to take out and after being cooled to room temperature, obtained surface is with the carbon cloth compound thermal sulphurated siliastic base ablation resistant material of 1 layer of carbon cloth fiber;
Step 8: repeating step 5 ~ 7, can prepare the carbon cloth compound thermal sulphurated siliastic base ablation resistant material of surface with 2-5 layer carbon cloth.
Compared with prior art, the invention has the beneficial effects as follows:
A kind of carbon cloth compound thermal sulphurated siliastic base ablation resistant material provided by the present invention and preparation method thereof, improve ablation resistance and the intensity of hot-vulcanized silicone rubber based composites, increase the heat-proof quality of hot-vulcanized silicone rubber matrix material, reduce the line ablation velocity of hot-vulcanized silicone rubber matrix material.
Specific embodiments
Below in conjunction with embodiment, specific embodiment of the invention process is described further.
As follows to the performance test methods of obtained hot-vulcanized silicone rubber/boron bakelite resin base ablation resistant material:
Tensile property: according to GB/T528-2009, draw speed is 500mm/min;
Ablation property: according to national military standard GJB323A-1996, records hot-vulcanized silicone rubber/boron bakelite resin base ablation resistant material linear ablative rate, specific heat ratio when mass loss rate and underlayer temperature are 80 DEG C, ablation time 20s.Specimen size is diameter 30mm, and thickness is 10m, the long 81mm of graphite jig of dress ablation sample, wide 53mm, the dark 9mm of circular groove, diameter 30mm.
embodiment 1:
The carbon cloth compound thermal sulphurated siliastic base ablation resistant material composition of the present embodiment comprises: methyl vinyl silicone rubber 100 mass parts, gas-phase silica 30 mass parts, carbon fiber 10 mass parts, granularity are zirconium boride 99.5004323A8ure 5 mass parts of 200nm, hydroxy silicon oil 0.01 mass parts, silane coupling agent 0.01 mass parts, dicumyl peroxide 1 mass parts, poly-phenylbenzene Borosiloxane performed polymer 1 mass parts and carbon cloth 1 layer.
Its preparation method comprises the following steps:
Step 1: prepare burden according to methyl vinyl silicone rubber 100 mass parts, gas-phase silica 30 mass parts, carbon fiber 10 mass parts, zirconium boride 99.5004323A8ure 5 mass parts, hydroxy silicon oil 0.01 mass parts, silane coupling agent 0.01 mass parts, dicumyl peroxide 1 mass parts, poly-phenylbenzene Borosiloxane performed polymer 1 mass parts and carbon cloth 1 layer;
Step 2: add methyl vinyl silicone rubber, gas-phase silica, hydroxy silicon oil, carbon fiber, zirconium boride 99.5004323A8ure, dicumyl peroxide and silane coupling agent successively in two roller mill, be plasticate under the condition of 40 DEG C to mix in temperature, room temperature places 24 hours;
Step 3: the mixture processed through step 2 is placed in mould, carries out a sulfidizing 15min under be 7.0MPa and temperature being the condition of 170 DEG C with vulcanizing press at pressure;
Step 4: be placed in baking oven through step 3 process, carry out post cure process 2h under the condition of 200 DEG C, to prepare thickness be 10mm diameter is the cylinder hot-vulcanized silicone rubber base ablation resistant material of 30mm;
Step 5: poly-phenylbenzene Borosiloxane performed polymer is heated to 230 DEG C to molten state, after melting, dip treating is carried out 2 minutes to carbon cloth;
Step 6: take out the carbon cloth after dipping, adhered to the surface being compounded in hot-vulcanized silicone rubber base ablation resistant material, room temperature places 2 minutes;
Step 7: the hot-vulcanized silicone rubber base ablation resistant material after processing through step 6 is placed on vulcanizing press, it is 220 DEG C in temperature, pressure is press 3 times under the condition of 0.2MPa, to take out and after being cooled to room temperature, obtained surface is with the carbon cloth compound thermal sulphurated siliastic base ablation resistant material of 1 layer of carbon cloth fiber.
Record line ablation 0.0087mm/s, mass ablative rate 0.0303g/s, maximum stress value reaches 64.14Mpa.
embodiment 2:
The carbon cloth compound thermal sulphurated siliastic base ablation resistant material composition of the present embodiment comprises: methyl vinyl silicone rubber 70 mass parts, methyl phenyl vinyl silicone rubber 30 mass parts, precipitated silica 30 mass parts, pbo fiber 8 mass parts, granularity are magnesium oxide 10 mass parts, hydroxy silicon oil 0.01 mass parts, silane coupling agent 0.01 mass parts, 2 of 500 μm, 5-dimethyl-2,5-bishexane 1 mass parts, poly-phenylbenzene Borosiloxane performed polymer 1 mass parts and carbon cloth 1 layer.
Its preparation method comprises the following steps:
Step 1: according to methyl vinyl silicone rubber 70 mass parts, methyl phenyl vinyl silicone rubber 30 mass parts, precipitated silica 30 mass parts, pbo fiber 8 mass parts, magnesium oxide 10 mass parts, hydroxy silicon oil 0.01 mass parts and silane coupling agent 0.01 mass parts, 2,5-dimethyl-2,5-bishexane 1 mass parts, poly-phenylbenzene Borosiloxane performed polymer 1 mass parts and carbon cloth 1 ~ 5 layer are prepared burden;
Step 2: add methyl vinyl silicone rubber, methyl phenyl vinyl silicone rubber, precipitated silica, hydroxy silicon oil, pbo fiber, magnesium oxide, 2 in two roller mill successively, 5-dimethyl-2,5-bishexane and silane coupling agent, be plasticate under the condition of 40 DEG C to mix in temperature, room temperature places 24 hours;
Step 3: the mixture processed through step 2 is placed in mould, carries out a sulfidizing 15min under be 7.0MPa and temperature being the condition of 170 DEG C with vulcanizing press at pressure;
Step 4: be placed in baking oven through step 3 process, carry out post cure process 2h under the condition of 200 DEG C, to prepare thickness be 10mm diameter is the cylinder hot-vulcanized silicone rubber base ablation resistant material of 30mm;
Step 5: poly-phenylbenzene Borosiloxane performed polymer is heated to 220 DEG C to molten state, after melting, dip treating is carried out 3 minutes to carbon cloth;
Step 6: take out the carbon cloth after dipping, adhered to the surface being compounded in hot-vulcanized silicone rubber base ablation resistant material, room temperature places 3 minutes;
Step 7: the hot-vulcanized silicone rubber base ablation resistant material after processing through step 6 is placed on vulcanizing press, it is 210 DEG C in temperature, pressure is press 4 times under the condition of 0.1MPa, to take out and after being cooled to room temperature, obtained surface is with the carbon cloth compound thermal sulphurated siliastic base ablation resistant material of 1 layer of carbon cloth fiber.
Record line ablation 0.0076mm/s, mass ablative rate 0.02608g/s, maximum stress value reaches 66.38Mpa.
embodiment 3:
The carbon cloth compound thermal sulphurated siliastic base ablation resistant material composition of the present embodiment comprises: methyl vinyl silicone rubber 60 mass parts, methyl phenyl vinyl silicone rubber 40 mass parts, gas-phase silica 40 mass parts, aramid fiber 10 mass parts, granularity are hafnia 10 mass parts of 400nm, hydroxy silicon oil 0.02 mass parts, silane coupling agent 0.01 mass parts, dicumyl peroxide 1 mass parts, poly-phenylbenzene Borosiloxane performed polymer 1 mass parts and carbon cloth 2 layers.
Its preparation method comprises the following steps:
Step 1: prepare burden according to methyl vinyl silicone rubber 60 mass parts, methyl phenyl vinyl silicone rubber 40 mass parts, gas-phase silica 40 mass parts, aramid fiber 10 mass parts, hafnia 10 mass parts, hydroxy silicon oil 0.02 mass parts, silane coupling agent 0.01 mass parts, dicumyl peroxide 1 mass parts, poly-phenylbenzene Borosiloxane performed polymer 1 mass parts and carbon cloth 2 layers;
Step 2: add methyl vinyl silicone rubber, methyl phenyl vinyl silicone rubber, gas-phase silica, aramid fiber, hafnia, hydroxy silicon oil, silane coupling agent, dicumyl peroxide successively in two roller mill, be plasticate under the condition of 40 DEG C to mix in temperature, room temperature places 24 hours;
Step 3: the mixture processed through step 2 is placed in mould, carries out a sulfidizing 15min under be 7.0MPa and temperature being the condition of 170 DEG C with vulcanizing press at pressure;
Step 4: be placed in baking oven through step 3 process, carry out post cure process 2h under the condition of 200 DEG C, to prepare thickness be 10mm diameter is the cylinder hot-vulcanized silicone rubber base ablation resistant material of 30mm;
Step 5: poly-phenylbenzene Borosiloxane performed polymer is heated to 220 DEG C to molten state, after melting, dip treating is carried out 3 minutes to carbon cloth;
Step 6: take out the carbon cloth after one deck dipping, adhered to the surface being compounded in hot-vulcanized silicone rubber base ablation resistant material, room temperature places 3 minutes;
Step 7: take out the carbon cloth after one deck dipping again, adhered to the surface being compounded in hot-vulcanized silicone rubber base ablation resistant material, room temperature places 3 minutes;
Step 8: the hot-vulcanized silicone rubber base ablation resistant material after processing through step 7 is placed on vulcanizing press, it is 210 DEG C in temperature, pressure is press 4 times under the condition of 0.1MPa, to take out and after being cooled to room temperature, obtained surface is with the carbon cloth compound thermal sulphurated siliastic base ablation resistant material of 2 layers of carbon cloth fiber.
Record line ablation 0.0073mm/smm/s, mass ablative rate 0.0258g/s, maximum stress value reaches 72.50Mpa.
embodiment 4:
The carbon cloth compound thermal sulphurated siliastic base ablation resistant material composition of the present embodiment comprises: methyl vinyl silicone rubber 50 mass parts, methyl phenyl vinyl silicone rubber 50 mass parts, gas-phase silica 30 mass parts, carbon fiber and each 5 mass parts of pbo fiber, granularity are silicon carbide 9 mass parts of 200nm, hydroxy silicon oil 0.01 mass parts, silane coupling agent 0.02 mass parts, dicumyl peroxide 1 mass parts, poly-phenylbenzene Borosiloxane performed polymer 1 mass parts and carbon cloth 3 layers.
Its preparation method comprises the following steps:
Step 1: prepare burden according to methyl vinyl silicone rubber 50 mass parts, methyl phenyl vinyl silicone rubber 50 mass parts, gas-phase silica 30 mass parts, carbon fiber and each 5 mass parts of pbo fiber, silicon carbide 9 mass parts, hydroxy silicon oil 0.01 mass parts, silane coupling agent 0.02 mass parts, dicumyl peroxide 1 mass parts, poly-phenylbenzene Borosiloxane performed polymer 1 mass parts and carbon cloth 3 layers;
Step 2: add methyl vinyl silicone rubber, methyl phenyl vinyl silicone rubber, gas-phase silica, carbon fiber and pbo fiber, silicon carbide, hydroxy silicon oil, silane coupling agent and dicumyl peroxide successively in two roller mill, be plasticate under the condition of 40 DEG C to mix in temperature, room temperature places 24 hours;
Step 3: the mixture processed through step 2 is placed in mould, carries out a sulfidizing 15min under be 7.0MPa and temperature being the condition of 170 DEG C with vulcanizing press at pressure;
Step 4: be placed in baking oven through step 3 process, carry out post cure process 2h under the condition of 200 DEG C, to prepare thickness be 10mm diameter is the cylinder hot-vulcanized silicone rubber base ablation resistant material of 30mm;
Step 5: poly-phenylbenzene Borosiloxane performed polymer is heated to 225 DEG C to molten state, after melting, dip treating is carried out 2 minutes to carbon cloth;
Step 6: take out the carbon cloth after one deck dipping, adhered to the surface being compounded in hot-vulcanized silicone rubber base ablation resistant material, room temperature places 4 minutes;
Step 7: repetitive operation step 6 twice;
Step 8: the hot-vulcanized silicone rubber base ablation resistant material after processing through step 7 is placed on vulcanizing press, it is 220 DEG C in temperature, pressure is press 3 times under the condition of 0.2MPa, to take out and after being cooled to room temperature, the carbon cloth compound thermal sulphurated siliastic base ablation resistant material of the attached carbon cloth fiber that haves three layers in obtained surface.
Record line ablation 0.0035mm/smm/s, mass ablative rate 0.0208g/s, maximum stress value reaches 79.56Mpa.
embodiment 5:
The carbon cloth compound thermal sulphurated siliastic base ablation resistant material composition of the present embodiment comprises: methyl phenyl vinyl silicone rubber 100 mass parts, gas-phase silica 30 mass parts, carbon fiber and each 5 mass parts of aramid fiber, granularity are zirconium boride 99.5004323A8ure and each 5 mass parts of magnesium oxide, hydroxy silicon oil 0.01 mass parts, silane coupling agent 0.01 mass parts, the dicumyl peroxide and 2 of 200nm, each 1 mass parts of 5-dimethyl-2,5-bishexane, poly-phenylbenzene Borosiloxane performed polymer 1 mass parts and carbon cloth 1 layer.
Its preparation method comprises the following steps:
Step 1: according to methyl phenyl vinyl silicone rubber 100 mass parts, gas-phase silica 30 mass parts, carbon fiber and each 5 mass parts of aramid fiber, zirconium boride 99.5004323A8ure and each 5 mass parts of magnesium oxide, hydroxy silicon oil 0.01 mass parts, silane coupling agent 0.01 mass parts, dicumyl peroxide and 2, each 1 mass parts of 5-dimethyl-2,5-bishexane, poly-phenylbenzene Borosiloxane performed polymer 1 mass parts and carbon cloth 1 layer are prepared burden;
Step 2: add methyl phenyl vinyl silicone rubber, gas-phase silica, hydroxy silicon oil, carbon fiber and aramid fiber, zirconium boride 99.5004323A8ure and magnesium oxide, dicumyl peroxide, 2 in two roller mill successively, 5-dimethyl-2,5-bishexane and silane coupling agent, be plasticate under the condition of 40 DEG C to mix in temperature, room temperature places 24 hours;
Step 3: the mixture processed through step 2 is placed in mould, carries out a sulfidizing 15min under be 7.0MPa and temperature being the condition of 170 DEG C with vulcanizing press at pressure;
Step 4: be placed in baking oven through step 3 process, carry out post cure process 2h under the condition of 200 DEG C, to prepare thickness be 10mm diameter is the cylinder hot-vulcanized silicone rubber base ablation resistant material of 30mm;
Step 5: poly-phenylbenzene Borosiloxane performed polymer is heated to 230 DEG C to molten state, after melting, dip treating is carried out 2 minutes to carbon cloth;
Step 6: take out the carbon cloth after dipping, adhered to the surface being compounded in hot-vulcanized silicone rubber base ablation resistant material, room temperature places 2 minutes;
Step 7: the hot-vulcanized silicone rubber base ablation resistant material after processing through step 6 is placed on vulcanizing press, it is 220 DEG C in temperature, pressure is press 3 times under the condition of 0.2MPa, to take out and after being cooled to room temperature, obtained surface is with the carbon cloth compound thermal sulphurated siliastic base ablation resistant material of 1 layer of carbon cloth fiber.
Record line ablation 0.0084mm/s, mass ablative rate 0.0298g/s, maximum stress value reaches 62.82Mpa.
embodiment 6:
The carbon cloth compound thermal sulphurated siliastic base ablation resistant material composition of the present embodiment comprises: methyl vinyl silicone rubber 100 mass parts, gas-phase silica 40 mass parts, pbo fiber and each 5 mass parts of aramid fiber, granularity are zirconium boride 99.5004323A8ure and each 5 mass parts of hafnia, hydroxy silicon oil 0.01 mass parts, silane coupling agent 0.01 mass parts, dicumyl peroxide 1 mass parts, poly-phenylbenzene Borosiloxane performed polymer 1 mass parts and the carbon cloth 1 layer of 200nm.
Its preparation method comprises the following steps:
Step 1: prepare burden according to methyl vinyl silicone rubber 100 mass parts, gas-phase silica 40 mass parts, pbo fiber and each 5 mass parts of aramid fiber, zirconium boride 99.5004323A8ure and each 5 mass parts of hafnia, hydroxy silicon oil 0.01 mass parts, silane coupling agent 0.01 mass parts, dicumyl peroxide 1 mass parts, poly-phenylbenzene Borosiloxane performed polymer 1 mass parts and carbon cloth 1 layer;
Step 2: add methyl vinyl silicone rubber, gas-phase silica, hydroxy silicon oil, pbo fiber and aramid fiber, zirconium boride 99.5004323A8ure and hafnia, dicumyl peroxide and silane coupling agent in two roller mill successively, be plasticate under the condition of 40 DEG C to mix in temperature, room temperature places 24 hours;
Step 3: the mixture processed through step 2 is placed in mould, carries out a sulfidizing 15min under be 7.0MPa and temperature being the condition of 170 DEG C with vulcanizing press at pressure;
Step 4: be placed in baking oven through step 3 process, carry out post cure process 2h under the condition of 200 DEG C, to prepare thickness be 10mm diameter is the cylinder hot-vulcanized silicone rubber base ablation resistant material of 30mm;
Step 5: poly-phenylbenzene Borosiloxane performed polymer is heated to 230 DEG C to molten state, after melting, dip treating is carried out 2 minutes to carbon cloth;
Step 6: take out the carbon cloth after dipping, adhered to the surface being compounded in hot-vulcanized silicone rubber base ablation resistant material, room temperature places 2 minutes;
Step 7: the hot-vulcanized silicone rubber base ablation resistant material after processing through step 6 is placed on vulcanizing press, it is 220 DEG C in temperature, pressure is press 3 times under the condition of 0.2MPa, to take out and after being cooled to room temperature, obtained surface is with the carbon cloth compound thermal sulphurated siliastic base ablation resistant material of 1 layer of carbon cloth fiber.
Record line ablation 0.0079mm/s, mass ablative rate 0.0310g/s, maximum stress value reaches 65.01Mpa.
embodiment 7:
The carbon cloth compound thermal sulphurated siliastic base ablation resistant material composition of the present embodiment comprises: methyl vinyl silicone rubber 100 mass parts, gas-phase silica 40 mass parts, pbo fiber, aramid fiber and each 5 mass parts of carbon fiber, granularity are zirconium boride 99.5004323A8ure and each 5 mass parts of silicon carbide, hydroxy silicon oil 0.01 mass parts, silane coupling agent 0.01 mass parts, dicumyl peroxide 1 mass parts, poly-phenylbenzene Borosiloxane performed polymer 1 mass parts and the carbon cloth 1 layer of 200nm.
Its preparation method comprises the following steps:
Step 1: prepare burden according to methyl vinyl silicone rubber 100 mass parts, gas-phase silica 40 mass parts, pbo fiber, aramid fiber and each 5 mass parts of carbon fiber, zirconium boride 99.5004323A8ure and each 5 mass parts of silicon carbide, hydroxy silicon oil 0.01 mass parts, silane coupling agent 0.01 mass parts, dicumyl peroxide 1 mass parts, poly-phenylbenzene Borosiloxane performed polymer 1 mass parts and carbon cloth 1 layer;
Step 2: add methyl vinyl silicone rubber, gas-phase silica, hydroxy silicon oil, pbo fiber, aramid fiber and carbon fiber, zirconium boride 99.5004323A8ure and silicon carbide, dicumyl peroxide and silane coupling agent in two roller mill successively, be plasticate under the condition of 40 DEG C to mix in temperature, room temperature places 24 hours;
Step 3: the mixture processed through step 2 is placed in mould, carries out a sulfidizing 15min under be 7.0MPa and temperature being the condition of 170 DEG C with vulcanizing press at pressure;
Step 4: be placed in baking oven through step 3 process, carry out post cure process 2h under the condition of 200 DEG C, to prepare thickness be 10mm diameter is the cylinder hot-vulcanized silicone rubber base ablation resistant material of 30mm;
Step 5: poly-phenylbenzene Borosiloxane performed polymer is heated to 230 DEG C to molten state, after melting, dip treating is carried out 2 minutes to carbon cloth;
Step 6: take out the carbon cloth after dipping, adhered to the surface being compounded in hot-vulcanized silicone rubber base ablation resistant material, room temperature places 2 minutes;
Step 7: the hot-vulcanized silicone rubber base ablation resistant material after processing through step 6 is placed on vulcanizing press, it is 220 DEG C in temperature, pressure is press 3 times under the condition of 0.2MPa, to take out and after being cooled to room temperature, obtained surface is with the carbon cloth compound thermal sulphurated siliastic base ablation resistant material of 1 layer of carbon cloth fiber.
Record line ablation 0.0078mm/s, mass ablative rate 0.0302g/s, maximum stress value reaches 64.12Mpa.
embodiment 8:
The carbon cloth compound thermal sulphurated siliastic base ablation resistant material composition of the present embodiment comprises: methyl vinyl silicone rubber 100 mass parts, gas-phase silica 40 mass parts, pbo fiber, aramid fiber and each 5 mass parts of carbon fiber, granularity are the zirconium boride 99.5004323A8ure of 200nm, magnesium oxide and each 5 mass parts of silicon carbide, hydroxy silicon oil 0.01 mass parts, silane coupling agent 0.01 mass parts, dicumyl peroxide 1 mass parts, poly-phenylbenzene Borosiloxane performed polymer 1 mass parts and carbon cloth 1 layer.
Its preparation method comprises the following steps:
Step 1: prepare burden according to methyl vinyl silicone rubber 100 mass parts, gas-phase silica 40 mass parts, pbo fiber, aramid fiber and each 5 mass parts of carbon fiber, zirconium boride 99.5004323A8ure, magnesium oxide and each 5 mass parts of silicon carbide, hydroxy silicon oil 0.01 mass parts, silane coupling agent 0.01 mass parts, dicumyl peroxide 1 mass parts, poly-phenylbenzene Borosiloxane performed polymer 1 mass parts and carbon cloth 1 layer;
Step 2: add methyl vinyl silicone rubber, gas-phase silica, hydroxy silicon oil, pbo fiber, aramid fiber and carbon fiber, zirconium boride 99.5004323A8ure, magnesium oxide and silicon carbide, dicumyl peroxide and silane coupling agent in two roller mill successively, be plasticate under the condition of 40 DEG C to mix in temperature, room temperature places 24 hours;
Step 3: the mixture processed through step 2 is placed in mould, carries out a sulfidizing 15min under be 7.0MPa and temperature being the condition of 170 DEG C with vulcanizing press at pressure;
Step 4: be placed in baking oven through step 3 process, carry out post cure process 2h under the condition of 200 DEG C, to prepare thickness be 10mm diameter is the cylinder hot-vulcanized silicone rubber base ablation resistant material of 30mm;
Step 5: poly-phenylbenzene Borosiloxane performed polymer is heated to 230 DEG C to molten state, after melting, dip treating is carried out 2 minutes to carbon cloth;
Step 6: take out the carbon cloth after dipping, adhered to the surface being compounded in hot-vulcanized silicone rubber base ablation resistant material, room temperature places 2 minutes;
Step 7: the hot-vulcanized silicone rubber base ablation resistant material after processing through step 6 is placed on vulcanizing press, it is 220 DEG C in temperature, pressure is press 3 times under the condition of 0.2MPa, to take out and after being cooled to room temperature, obtained surface is with the carbon cloth compound thermal sulphurated siliastic base ablation resistant material of 1 layer of carbon cloth fiber.
Record line ablation 0.0072mm/s, mass ablative rate 0.0300g/s, maximum stress value reaches 63.88Mpa.
Claims (7)
1. a carbon cloth compound thermal sulphurated siliastic base ablation resistant material, it is characterized in that material composition comprises: hot-vulcanized silicone rubber, strengthening agent, fiber, the filler of resistance to ablation, vulcanizing agent, silane coupling agent, hydroxy silicon oil, poly-phenylbenzene Borosiloxane performed polymer and carbon cloth, concrete massfraction proportioning is:
Hot-vulcanized silicone rubber: 100 mass parts;
Strengthening agent: 5 ~ 50 mass parts;
Fiber: 1 ~ 30 mass parts;
The filler of resistance to ablation: 1 ~ 20 mass parts;
Vulcanizing agent: 1 ~ 3 mass parts;
Silane coupling agent: 0.01 ~ 0.1 mass parts;
Hydroxy silicon oil: 0.01 ~ 0.5 mass parts;
Poly-phenylbenzene Borosiloxane performed polymer: 1 ~ 5 mass parts;
Carbon cloth: 1 ~ 5 layer.
2. a kind of carbon cloth compound thermal sulphurated siliastic base ablation resistant material according to claim 1, it is characterized in that described hot-vulcanized silicone rubber adopts in methyl vinyl silicone rubber and methyl phenyl vinyl silicone rubber one or both.
3. a kind of carbon cloth compound thermal sulphurated siliastic base ablation resistant material according to claim 1, is characterized in that described strengthening agent is gas-phase silica or precipitated silica.
4. a kind of carbon cloth compound thermal sulphurated siliastic base ablation resistant material according to claim 1, it is characterized in that the described inorganic filler of resistance to ablation is one or more in zirconium boride 99.5004323A8ure, zirconium white, magnesium oxide and silicon carbide, granularity is 200nm ~ 500 μm.
5. a kind of carbon cloth compound thermal sulphurated siliastic base ablation resistant material according to claim 1, is characterized in that described fiber is one or more in carbon fiber, pbo fiber and aramid fiber.
6. a kind of carbon cloth compound thermal sulphurated siliastic base ablation resistant material according to claim 1, is characterized in that described vulcanizing agent is one or both in 2,5-dimethyl-2,5-bishexane and dicumyl peroxide.
7. a preparation method for a kind of carbon cloth compound thermal sulphurated siliastic base ablation resistant material according to claim 1, is characterized in that comprising the following steps:
Step 1: prepare burden according to hot-vulcanized silicone rubber 100 mass parts, strengthening agent 5 ~ 50 mass parts, fiber 1 ~ 30 mass parts, the filler of resistance to ablation 1 ~ 20 mass parts, vulcanizing agent 1 ~ 3 mass parts, silane coupling agent 0.01 ~ 0.1 mass parts, hydroxy silicon oil 0.01 ~ 0.5 mass parts, poly-phenylbenzene Borosiloxane performed polymer 1 ~ 5 mass parts and carbon cloth 1 ~ 5 layer;
Step 2: add hot-vulcanized silicone rubber, strengthening agent, hydroxy silicon oil, fiber, the filler of resistance to ablation, vulcanizing agent and silane coupling agent successively in two roller mill, plasticate and mix, room temperature places 24 hours;
Step 3: the mixture processed through step 2 is placed in mould, carries out a sulfidizing 10-30min under be 5-10MPa and temperature being the condition of 170-190 DEG C with vulcanizing press at pressure;
Step 4: be placed in baking oven through step 3 process, carry out post cure process 1.8 ~ 2.0h under the condition of 190-210 DEG C, obtained hot-vulcanized silicone rubber base ablation resistant material;
Step 5: poly-phenylbenzene Borosiloxane performed polymer is heated to 220 ~ 260 DEG C to molten state, after melting, dip treating is carried out 1 ~ 8 minute to carbon cloth;
Step 6: take out the carbon cloth after dipping, adhered to the surface being compounded in hot-vulcanized silicone rubber base ablation resistant material, room temperature is placed 1 ~ 10 minute;
Step 7: the hot-vulcanized silicone rubber base ablation resistant material after processing through step 6 is placed on vulcanizing press, it is 180 ~ 220 DEG C in temperature, pressure is press 3 ~ 5 times under the condition of 0.1 ~ 1MPa, to take out and after being cooled to room temperature, obtained surface is with the carbon cloth compound thermal sulphurated siliastic base ablation resistant material of 1 layer of carbon cloth fiber;
Step 8: repeating step 5 ~ 7, can prepare the carbon cloth compound thermal sulphurated siliastic base ablation resistant material of surface with 2-5 layer carbon cloth.
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