CN111349316A - Preparation method of inorganic fullerene resin-based composite material for containing case - Google Patents
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- CN111349316A CN111349316A CN202010256877.2A CN202010256877A CN111349316A CN 111349316 A CN111349316 A CN 111349316A CN 202010256877 A CN202010256877 A CN 202010256877A CN 111349316 A CN111349316 A CN 111349316A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/06—Elements
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- C—CHEMISTRY; METALLURGY
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
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- C08K3/045—Fullerenes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K3/02—Elements
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0812—Aluminium
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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Abstract
The invention discloses a preparation method of an inorganic fullerene resin-based composite material for a containing casing, belonging to the technical field of biomass carbon fiber materials. The specific process comprises taking a certain amount of epoxy resin and inorganic fullerene nano-particles for ultrasonic treatment. Degassing the dispersed product under vacuum, and adding the degassed resin into a glue injection tank for later use. The carbon fiber unidirectional cord fabric was laid in a mold in the order of [60/0/-60]6s lay-up and resin injection was performed. The product after the resin injection was completed was cured. Naturally cooling the mould to below 60 ℃, and removing the mould and taking out. The inorganic fullerene resin-based composite material prepared by the invention has the characteristics of impact resistance, low density, specific strength, high specific modulus, strong designability, fatigue resistance, corrosion resistance and the like, and is expected to become a new generation of composite material for fan containing casings.
Description
Technical Field
The invention relates to the technical field of biomass carbon fiber materials, in particular to a preparation method of an inorganic fullerene resin-based composite material for a containing case.
Background
When the fan rotor blade of the civil turbofan engine works, the fan rotor blade rotates at a high speed in the engine, and under the action of external object impact or internal damage, if the fan blade fails, is broken and flies out, the fan blade needs to be effectively contained by a fan casing, otherwise, fan fragments are likely to puncture the engine body to endanger the flight safety.
Airlines at home and abroad put strict inclusion requirements on fan containing casings of civil turbofan engines, such as aeroengine airworthiness regulation (CCAR-33) and aeroturbine engine inclusion requirement (GJB3366-1998) in China, and engine structural integrity outline (MIL-STD-1783B) in the United states.
Airlines and scientific research institutions at home and abroad actively research and develop effective containment materials and structures, improve containment efficiency and reduce engine quality and oil consumption. The traditional civil turbofan engine fan containing casing mainly adopts titanium alloy, aluminum alloy or structural steel with enough thickness, and the metal materials have higher density, high oil consumption, weak designability and the like, so a more superior material needs to be designed.
Disclosure of Invention
The invention aims to provide a preparation method of an inorganic fullerene resin-based composite material for a containing casing, which solves the technical problems of traditional engine fans made of titanium alloy, aluminum alloy and the like. Compared with the traditional metal material, the resin-based composite material has the characteristics of low density, specific strength, high specific modulus, strong designability, fatigue resistance, corrosion resistance and the like.
The addition of the inorganic fullerene and the carbon fiber greatly improves the shock resistance and the wear resistance of the epoxy resin, and the high-temperature curing technology is adopted, so that the lower working temperature of the fan containing casing is completely met.
A preparation method of an inorganic fullerene resin-based composite material for containing a casing comprises the following steps:
step 1: taking epoxy resin: mixing inorganic fullerene in a beaker at a mass ratio of 15:1, and then putting the mixture into an ultrasonic instrument for ultrasonic dispersion for 15 min;
step 2: heating the dispersed product to 100 ℃ under vacuum, degassing for 10min, removing air in the epoxy resin, and adding the degassed resin into a glue injection tank for later use;
and step 3: laying carbon fibers in a mold, selecting a cushion frame with the thickness of 5mm, sealing and closing the mold, putting the mold and the glue injection tank in the step (2) into an oven, and performing resin injection when the temperature of the mold is heated to 80-90 ℃;
and 4, step 4: taking the product after the resin injection in the step (3), heating the product in an oven to 140-;
and 5: and after the mould is naturally cooled to below 60 ℃, removing the mould and taking out to obtain the inorganic fullerene/carbon fiber composite material laminated plate with the thickness of about 5 mm.
In the step 3, the unidirectional cord fabric with carbon fibers is laid in the mould according to the layering sequence of [60/0/-60]6 s.
In the step 1, the inorganic fullerene is an aluminum-based nano composite fullerene material, and the synthesis process of the aluminum-based nano composite fullerene material is as follows: putting the inorganic fullerene nano-particles IF-WS2 into ethanol and dispersing by using an ultrasonic probe, mixing the inorganic fullerene nano-particles IF-WS2 and the ethanol mixture with vigorous stirring at 80-90 ℃ with Al powder until all ethanol is evaporated, drying in an oven at 110-130 ℃ for 11-13 hours to obtain a primary mixture sample, extruding the sample by a fused deposition modeling 3D printing technology, and controlling the temperature of a printing extrusion head to be 560-670 ℃ to complete synthesis.
The time for dispersing the ultrasonic probe is 0.8-1.2 hours, the ultrasonic frequency is 80-90 KHz, and in the fused deposition modeling 3D printing process, hot pressing is carried out for 30 minutes under the conditions that the hot pressing temperature is 560-650 ℃, the pressure is 75-85 KN, and the atmosphere is N2.
Heating the mixture of the inorganic fullerene nano-particles IF-WS2 and ethanol to 80 ℃, adding aluminum powder particles for mixing, rapidly stirring until the ethanol is completely volatilized to prepare a mixed solid sample of 20-30 wt% IF-WS2 and the aluminum powder, and then placing the mixed solid sample in an oven at 120 ℃ for drying for 12 hours.
The carbon fiber in the step 3 is bagasse-based carbon fiber, and the preparation process of the bagasse-based carbon fiber comprises the following steps: putting bagasse into a beaker filled with a sodium hypochlorite solution with the mass fraction of 5%, soaking for 12 hours, repeatedly filtering until the pH of the filtrate is close to neutral, putting the filtered bagasse into a drying box, and drying for 10 hours at 80 ℃;
the dried bagasse is contacted with an aqueous urea solution in a volume ratio of urea to deionized water of 1:1, soaked for 1h, the soaked bagasse is taken out, placed in a drying box, dried for 10h at 80 ℃, and repeatedly dried for 2-3 times to obtain sized bagasse;
putting the obtained sized bagasse into a vacuum tube furnace, sealing, introducing nitrogen, raising the temperature of the vacuum tube furnace to 400 ℃ at the speed of 5 ℃/min after exhausting air, and maintaining the temperature of the vacuum tube furnace for carbonization for 40min at 400 ℃;
then, the temperature of the vacuum tube furnace is increased to 1200 ℃ at the speed of 5 ℃/min, and the temperature is kept at 1200 ℃ for graphitization for 20min to obtain primary carbon fiber;
and (3) putting the primary carbon fiber into 45 wt% nitric acid water solution, soaking for 30min, taking out, putting into deionized water, rinsing for 2 times, putting the oxidized carbon fiber into a drying oven, and drying for 10h at 80 ℃ to obtain the bagasse-based carbon fiber.
By adopting the technical scheme, the invention has the following technical effects:
the inorganic fullerene and the ordered carbon fiber cloth are added to increase the epoxy resin, so that the inorganic fullerene resin-based composite material has the characteristics of high impact resistance, low density, high specific strength, high specific modulus, high designability, fatigue resistance, corrosion resistance and the like, is expected to become a new generation of composite material for fan containing casings, has the characteristics of light weight, excellent damping performance and shock wave absorption capacity, has good application prospect in light damping materials and high-performance protective materials, is low in preparation cost, can be industrially produced, and has high practical value.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail below with reference to preferred embodiments. It should be noted, however, that the numerous details set forth in the description are merely for the purpose of providing the reader with a thorough understanding of one or more aspects of the present invention, which may be practiced without these specific details.
The invention designs an inorganic fullerene/carbon fiber resin matrix composite material, the addition of the inorganic fullerene and the carbon fiber greatly improves the shock resistance and the wear resistance of the epoxy resin, and the high-temperature curing technology is adopted, so that the lower working temperature of a fan containing casing is completely met.
Example 1:
(1) taking a certain amount of epoxy resin and inorganic fullerene nano-particles, and mixing the epoxy resin and the inorganic fullerene nano-particles according to the following ratio: mixing the inorganic fullerene with the mass ratio of 20:1 in a beaker, and then putting the mixture into an ultrasonic instrument for ultrasonic treatment for 15 min. The particle size of the inorganic fullerene nano-particles is 0.1-20 mu m.
(2) And (3) heating the dispersed product in the step (1) to 100 ℃ under vacuum, degassing for 10min, and removing air in the epoxy resin. And adding the degassed resin into a glue injection tank for later use.
(3) And (3) laying the carbon fiber unidirectional cord fabric into a mold according to the laying sequence of [60/0/-60]6s, selecting a cushion frame with the thickness of 5mm, sealing and closing the mold, putting the mold and the glue injection tank in the step (2) into an oven, and performing resin injection when the temperature of the mold is heated to 80-90 ℃.
(4) And (4) taking the product after the resin injection in the step (3), heating the product to 140-185 ℃ in an oven, and keeping the temperature for 2h, and then heating the product to 180-185 ℃ for 3h to finish the resin curing.
(5) And after the mould is naturally cooled to below 60 ℃, removing the mould and taking out to obtain the inorganic fullerene/carbon fiber composite material laminated plate with the thickness of about 5 mm.
Example 2:
(1) taking a certain amount of epoxy resin and inorganic fullerene nano-material, and mixing the epoxy resin: mixing the inorganic fullerene with the mass ratio of 15:1 in a beaker, and then putting the mixture into an ultrasonic instrument for ultrasonic treatment for 15 min.
The inorganic fullerene nano-material is an aluminum-based nano-composite fullerene material, and the synthesis process of the aluminum-based nano-composite fullerene material is as follows: putting the inorganic fullerene nano-particles IF-WS2 into ethanol and dispersing by using an ultrasonic probe, mixing the inorganic fullerene nano-particles IF-WS2 and the ethanol mixture with vigorous stirring at 80-90 ℃ with Al powder until all ethanol is evaporated, drying in an oven at 110-130 ℃ for 11-13 hours to obtain a primary mixture sample, extruding the sample by a fused deposition modeling 3D printing technology, and controlling the temperature of a printing extrusion head to be 560-670 ℃ to complete synthesis.
The time for dispersing the ultrasonic probe is 0.8-1.2 hours, the ultrasonic frequency is 80-90 KHz, and in the fused deposition modeling 3D printing process, hot pressing is carried out for 30 minutes under the conditions that the hot pressing temperature is 560-650 ℃, the pressure is 75-85 KN, and the atmosphere is N2.
(2) And (3) heating the dispersed product in the step (1) to 100 ℃ under vacuum, degassing for 10min, and removing air in the epoxy resin. And adding the degassed resin into a glue injection tank for later use.
(3) And (3) laying the carbon fiber unidirectional cord fabric into a mold according to the laying sequence of [60/0/-60]6s, selecting a cushion frame with the thickness of 5mm, sealing and closing the mold, putting the mold and the glue injection tank in the step (2) into an oven, and performing resin injection when the temperature of the mold is heated to 85 ℃.
The carbon fiber is bagasse-based carbon fiber, and the preparation process of the bagasse-based carbon fiber comprises the following steps: putting bagasse into a beaker filled with a sodium hypochlorite solution with the mass fraction of 5%, soaking for 12 hours, repeatedly filtering until the pH of the filtrate is close to neutral, putting the filtered bagasse into a drying box, and drying for 10 hours at 80 ℃;
the dried bagasse is contacted with an aqueous urea solution in a volume ratio of urea to deionized water of 1:1, soaked for 1h, the soaked bagasse is taken out, placed in a drying box, dried for 10h at 80 ℃, and repeatedly dried for 2-3 times to obtain sized bagasse;
putting the obtained sized bagasse into a vacuum tube furnace, sealing, introducing nitrogen, raising the temperature of the vacuum tube furnace to 400 ℃ at the speed of 5 ℃/min after exhausting air, and maintaining the temperature of the vacuum tube furnace for carbonization for 40min at 400 ℃;
then, the temperature of the vacuum tube furnace is increased to 1200 ℃ at the speed of 5 ℃/min, and the temperature is kept at 1200 ℃ for graphitization for 20min to obtain primary carbon fiber;
and (3) putting the primary carbon fiber into 45 wt% nitric acid water solution, soaking for 30min, taking out, putting into deionized water, rinsing for 2 times, putting the oxidized carbon fiber into a drying oven, and drying for 10h at 80 ℃ to obtain the bagasse-based carbon fiber. The bagasse-based carbon fiber is made into a unidirectional cord fabric structure through a die.
(4) And (4) taking the product after the resin injection in the step (3), heating the product to 140-185 ℃ in an oven, and keeping the temperature for 2h, and then heating the product to 180-185 ℃ for 3h to finish the resin curing.
(5) And after the mould is naturally cooled to below 60 ℃, removing the mould and taking out to obtain the inorganic fullerene/carbon fiber composite material laminated plate with the thickness of about 5 mm.
Example 3:
(1) taking a certain amount of epoxy resin and inorganic fullerene nano-particles, and mixing the epoxy resin and the inorganic fullerene nano-particles according to the following ratio: mixing the inorganic fullerene with the mass ratio of 15:1 in a beaker, and then putting the mixture into an ultrasonic instrument for ultrasonic treatment for 15 min.
(2) And (3) heating the dispersed product in the step (1) to 100 ℃ under vacuum, degassing for 10min, and removing air in the epoxy resin. And adding the degassed resin into a glue injection tank for later use.
(3) And (3) laying the carbon fiber unidirectional cord fabric into a mold according to the laying sequence of [60/0/-60]6s, selecting a cushion frame with the thickness of 5mm, sealing and closing the mold, putting the mold and the glue injection tank in the step (2) into an oven, and performing resin injection when the temperature of the mold is heated to 80-90 ℃.
(4) And (4) taking the product after the resin injection in the step (3), heating the product to 145 ℃ in an oven, preserving heat for 2h, and then preserving heat for 3h after heating to 185 ℃ to finish resin curing.
(5) And after the mould is naturally cooled to below 60 ℃, removing the mould and taking out to obtain the inorganic fullerene/carbon fiber composite material laminated plate with the thickness of about 5 mm.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that those skilled in the art can make various improvements and modifications without departing from the principle of the present invention, and these improvements and modifications should also be construed as the protection scope of the present invention.
Claims (6)
1. A preparation method of an inorganic fullerene resin-based composite material for containing a casing is characterized by comprising the following steps: the method comprises the following steps:
step 1: taking epoxy resin: mixing inorganic fullerene in a beaker at a mass ratio of 15:1, and then putting the mixture into an ultrasonic instrument for ultrasonic dispersion for 15 min;
step 2: heating the dispersed product to 100 ℃ under vacuum, degassing for 10min, removing air in the epoxy resin, and adding the degassed resin into a glue injection tank for later use;
and step 3: laying carbon fibers in a mold, selecting a cushion frame with the thickness of 5mm, sealing and closing the mold, putting the mold and the glue injection tank in the step (2) into an oven, and performing resin injection when the temperature of the mold is heated to 80-90 ℃;
and 4, step 4: taking the product after the resin injection in the step (3), heating the product in an oven to 140-;
and 5: and after the mould is naturally cooled to below 60 ℃, removing the mould and taking out to obtain the inorganic fullerene/carbon fiber composite material laminated plate with the thickness of about 5 mm.
2. The method of claim 1, wherein the inorganic fullerene resin-based composite material for a containment casing comprises: in the step 3, the unidirectional cord fabric with carbon fibers is laid in the mould according to the layering sequence of [60/0/-60]6 s.
3. The method of claim 1, wherein the inorganic fullerene resin-based composite material for a containment casing comprises: in the step 1, the inorganic fullerene is an aluminum-based nano composite fullerene material, and the synthesis process of the aluminum-based nano composite fullerene material is as follows: putting the inorganic fullerene nano-particles IF-WS2 into ethanol and dispersing by using an ultrasonic probe, mixing the inorganic fullerene nano-particles IF-WS2 and the ethanol mixture with vigorous stirring at 80-90 ℃ with Al powder until all ethanol is evaporated, drying in an oven at 110-130 ℃ for 11-13 hours to obtain a primary mixture sample, extruding the sample by a fused deposition modeling 3D printing technology, and controlling the temperature of a printing extrusion head to be 560-670 ℃ to complete synthesis.
4. The method according to claim 3, wherein the inorganic fullerene resin-based composite material for a containment casing comprises: the time for dispersing the ultrasonic probe is 0.8-1.2 hours, the ultrasonic frequency is 80-90 KHz, and in the fused deposition modeling 3D printing process, hot pressing is carried out for 30 minutes under the conditions that the hot pressing temperature is 560-650 ℃, the pressure is 75-85 KN, and the atmosphere is N2.
5. The method according to claim 4, wherein the inorganic fullerene resin-based composite material for a containment casing comprises: heating the mixture of the inorganic fullerene nano-particles IF-WS2 and ethanol to 80 ℃, adding aluminum powder particles for mixing, rapidly stirring until the ethanol is completely volatilized to prepare a mixed solid sample of 20-30 wt% IF-WS2 and the aluminum powder, and then placing the mixed solid sample in an oven at 120 ℃ for drying for 12 hours.
6. The method of claim 1, wherein the inorganic fullerene resin-based composite material for a containment casing comprises: the carbon fiber in the step 3 is bagasse-based carbon fiber, and the preparation process of the bagasse-based carbon fiber comprises the following steps: putting bagasse into a beaker filled with a sodium hypochlorite solution with the mass fraction of 5%, soaking for 12 hours, repeatedly filtering until the pH of the filtrate is close to neutral, putting the filtered bagasse into a drying box, and drying for 10 hours at 80 ℃;
the dried bagasse is contacted with an aqueous urea solution in a volume ratio of urea to deionized water of 1:1, soaked for 1h, the soaked bagasse is taken out, placed in a drying box, dried for 10h at 80 ℃, and repeatedly dried for 2-3 times to obtain sized bagasse;
putting the obtained sized bagasse into a vacuum tube furnace, sealing, introducing nitrogen, raising the temperature of the vacuum tube furnace to 400 ℃ at the speed of 5 ℃/min after exhausting air, and maintaining the temperature of the vacuum tube furnace for carbonization for 40min at 400 ℃;
then, the temperature of the vacuum tube furnace is increased to 1200 ℃ at the speed of 5 ℃/min, and the temperature is kept at 1200 ℃ for graphitization for 20min to obtain primary carbon fiber;
and (3) putting the primary carbon fiber into 45 wt% nitric acid water solution, soaking for 30min, taking out, putting into deionized water, rinsing for 2 times, putting the oxidized carbon fiber into a drying oven, and drying for 10h at 80 ℃ to obtain the bagasse-based carbon fiber.
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