CN116141706A - Prefabrication method for pore defects of composite material - Google Patents
Prefabrication method for pore defects of composite material Download PDFInfo
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- CN116141706A CN116141706A CN202310419092.6A CN202310419092A CN116141706A CN 116141706 A CN116141706 A CN 116141706A CN 202310419092 A CN202310419092 A CN 202310419092A CN 116141706 A CN116141706 A CN 116141706A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
- B29C70/04—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising reinforcements only, e.g. self-reinforcing plastics
- B29C70/28—Shaping operations therefor
- B29C70/40—Shaping or impregnating by compression not applied
- B29C70/42—Shaping or impregnating by compression not applied for producing articles of definite length, i.e. discrete articles
- B29C70/44—Shaping or impregnating by compression not applied for producing articles of definite length, i.e. discrete articles using isostatic pressure, e.g. pressure difference-moulding, vacuum bag-moulding, autoclave-moulding or expanding rubber-moulding
- B29C70/443—Shaping or impregnating by compression not applied for producing articles of definite length, i.e. discrete articles using isostatic pressure, e.g. pressure difference-moulding, vacuum bag-moulding, autoclave-moulding or expanding rubber-moulding and impregnating by vacuum or injection
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
- B29C70/04—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising reinforcements only, e.g. self-reinforcing plastics
- B29C70/28—Shaping operations therefor
- B29C70/54—Component parts, details or accessories; Auxiliary operations, e.g. feeding or storage of prepregs or SMC after impregnation or during ageing
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02T—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO TRANSPORTATION
- Y02T50/00—Aeronautics or air transport
- Y02T50/40—Weight reduction
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Abstract
A method for prefabricating a composite void defect, comprising the steps of: 1. selecting pore defect prefabrication filling particles according to the molding process of the carbon fiber reinforced resin matrix composite component and the size requirement of prefabrication pore defects; 2. screening the microparticles; 3. converting particles with corresponding volumes into corresponding masses according to a density formula according to the porosity required by the defects of the prefabricated holes, and weighing the screened particles with corresponding masses; 4. uniformly placing the pore defect prefabrication filling particles at positions where the pore defects are required to be prefabricated, and pasting the pore defect prefabrication filling particles and the composite material layering into a whole; 5. vibrating and precompacting the carbon fiber reinforced resin matrix composite material member after being paved; 6. and transferring the carbon fiber reinforced resin matrix composite material component subjected to the vibration precompaction treatment into an autoclave, connecting a vacuum pump, and performing hot pressing, solidification and molding. The invention solves the problem that the defect of the prefabricated specific pore of the composite material is difficult.
Description
Technical Field
The invention belongs to the technical field of composite material forming, and particularly relates to a prefabrication method of a composite material pore defect.
Background
The composite material storage tank is widely applied in multiple industries due to the characteristics of light weight and high strength. The raw material adopted by the composite material storage tank is carbon fiber reinforced resin matrix composite material. However, in the production process, the inside of the carbon fiber reinforced resin matrix composite member inevitably generates pore defects, and the pore defects have obvious influence on the mechanical property, leakage property and the like of the member, so that the research on the performance of the composite member aiming at the pore defects is necessary. However, since the formation of voids has extremely high randomness, it is difficult to study a member intended to form voids having a specific porosity or a specific average diameter.
The prior method generally adopts a specific molding process to obtain the pore defects with statistical rules, but still has higher randomness, and can obtain the closer pore defect characteristics by taking samples for multiple times. Therefore, it is necessary to design a prefabrication method for pore defects of composite materials, which can accurately prefabricate the pore defects with the characteristics required for research.
Disclosure of Invention
The invention aims to provide a prefabrication method for pore defects of a composite material, which aims to solve the problem that in the process of producing a carbon fiber reinforced resin matrix composite material component, the research is difficult for the component which is required to generate pores with specific porosity or specific average diameter because the generation of the pores has extremely high randomness.
In order to achieve the above object, the present invention provides a method for prefabricating a composite material void defect, comprising the steps of:
step 1, selecting pore defect prefabricated filling particles according to a molding process of a carbon fiber reinforced resin matrix composite member and the size requirement of prefabricated pore defects, wherein the pore defect prefabricated filling particles meet the size requirement of the prefabricated pore defects, the glass transition temperature of the pore defect prefabricated filling particles is higher than the highest temperature in the molding process of the member, and the pore defect prefabricated filling particles are not adhered with resin used in the carbon fiber reinforced resin matrix composite member;
step 2, screening the pore defect prefabricated filling particles;
step 3, converting the pore defect prefabricated filling particles with corresponding volumes into corresponding masses according to a density formula according to the porosity required by the prefabricated pore defects, and weighing the pore defect prefabricated filling particles with the screened corresponding masses;
step 4, uniformly placing the pore defect prefabrication filling particles at positions where the pore defects need to be prefabricated, and pasting the pore defect prefabrication filling particles and the composite material layering into a whole;
step 5, vibrating and pre-compacting the carbon fiber reinforced resin matrix composite member after the paving;
and 6, transferring the carbon fiber reinforced resin matrix composite material component subjected to the vibration precompaction treatment into an autoclave, connecting a vacuum pump, and performing hot pressing, curing and forming.
In a specific embodiment, in the step 1, the particle size of the pore defect pre-filling particles is 2-700 μm; the pore defect prefabricated filling particles comprise polytetrafluoroethylene particles or/and silicon dioxide particles.
In a specific embodiment, in the step 2, before screening the pore defect pre-filling particles, the pore defect pre-filling particles are subjected to ultrasonic vibration treatment; in the step 4, before the pore defect prefabricated filling particles are uniformly placed at the positions where the pore defects are required to be prefabricated, ultrasonic vibration treatment is carried out on the pore defect prefabricated filling particles.
In a specific embodiment, when the pore defect prefabricated filling particles are subjected to ultrasonic vibration treatment, a proper amount of pore defect prefabricated filling particles are uniformly paved on an ultrasonic vibration platform, sealing is carried out above the ultrasonic vibration platform by using a sealant and a isolating film, and then ultrasonic vibration treatment is carried out; the ultrasonic vibration treatment time is more than 1min.
In a specific embodiment, during the screening in the step 2, screening the pore defect prefabricated filling particles by using a standard screen with screening size larger than the required size, and removing the oversized particles; the weighing process in the step 3 adopts a milligram-grade electronic scale as a tool.
In one embodiment, after oversized particles are removed, the resulting void defect pre-filled particles are screened with a standard screen having a screening size less than the desired size, and undersized particles are removed.
In a specific embodiment, in the step 4, the pore defect pre-filling particles are uniformly placed at the positions where the pore defects need to be pre-formed, and are placed in a manner of dipping the pore defect pre-filling particles by electrostatic adsorption of the glass rod.
In a specific embodiment, before electrostatic adsorption dipping of the glass rod, carrying out frictional electrification treatment on the glass rod on silk; when the glass rod is placed to adsorb and dip the pore defect prefabricated filling particles, the composite material is heated to improve the desorption effect.
In a specific embodiment, in the step 5, the step of vibration precompaction is as follows:
step 5.1, paving the composite material component on a die, sealing by using a vacuum bag, vacuumizing until the pressure in the bag is less than or equal to-0.09 mpa, and closing a vacuum pump to perform pressure maintaining operation to check the air tightness;
step 5.2, measuring an exothermic peak of the resin system in the used composite material by using a DSC differential scanning calorimeter, wherein the temperature corresponding to the measured exothermic peak is the temperature of the resin system for crosslinking and curing reaction, and is marked as K;
and 5.3, placing the vacuum sealed die on a random vibration table, fixedly connecting the die with the random vibration table by using a pressing bar, connecting a vacuum pump, setting the temperature and vibration acceleration in a cavity of the random vibration table, setting the temperature in the cavity of the random vibration table to be less than K, starting the vacuum pump, running a heating program and a vibration program of the vibration table, continuing to run for a period of time after the temperature reaches the set temperature, closing the heating program and the vibration program, taking out after the die and the components are cooled, and completing vibration precompaction treatment.
In a specific embodiment, in the step 5.3, the vibration acceleration is set to 8-12 g; continuously running for 5-12 min after the temperature of the random vibration table reaches the set temperature;
temperature setting range in cavity of random vibration table: the minimum temperature is the temperature corresponding to the point with the slope larger than-1 in the viscosity-temperature curve of the resin system, the maximum temperature is K-30 ℃, and the viscosity corresponding to the set temperature is smaller than 200 Pa sec.
Compared with the prior art, the invention has the following beneficial effects:
the pore defect is a small cavity formed by internal gas in the forming process of the carbon fiber reinforced resin matrix composite material. The polytetrafluoroethylene particles and the silicon dioxide particles adopted by the invention have good lubricity and non-adhesion relative to the carbon fiber reinforced resin matrix composite, are not mutually adhered with resin after solidification, and can form cavities by utilizing the volume of the polytetrafluoroethylene particles and the silicon dioxide particles, so that the effect of prefabricating the pores is achieved as the effect and the pores of the formed polytetrafluoroethylene particle cavities or silicon dioxide particle cavities are the same, and the pore defects in the carbon fiber reinforced resin matrix composite can be researched in a targeted manner in the later stage.
The glass transition temperature of the pore defect prefabricated filling particles selected by the invention is higher than the highest temperature in the component forming process, so that the pore defect prefabricated filling particles cannot be vitrified in the component forming process, and the interference to pore defect research due to vitrification is avoided.
The invention adopts an ultrasonic vibration mode to solve the problem of agglomeration of pore defect prefabricated filling particles, and reduces the waste of purchased particle raw materials, thereby reducing the cost for preparing the pore defects.
According to the invention, the carbon fiber reinforced resin matrix composite material is subjected to vibration precompaction treatment, so that the influence of natural pore defects in the process of preparing the composite material with specific pore defects can be effectively reduced, and the interference factors in the research of the pore defects of the composite material are reduced.
According to the invention, the pore defects generated in the actual molding process of the carbon fiber reinforced resin matrix composite are generally pore defects with the size of 10-500 mu m, and the particle size of the selected pore defect prefabricated filling particles is 2-700 mu m, so that the requirements of research can be fully met.
In addition to the objects, features and advantages described above, the present invention has other objects, features and advantages. The present invention will be described in further detail with reference to the drawings.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention. In the drawings:
FIG. 1 is a microscopic view of the depth of field of a laminate made in accordance with the present invention after cutting and polishing.
Detailed Description
The following detailed description of embodiments of the invention, taken in conjunction with the accompanying drawings, is provided to illustrate and not to limit the invention.
A method for prefabricating a composite void defect, comprising the steps of:
step 1, selecting pore defect prefabricated filling particles according to a molding process of a carbon fiber reinforced resin matrix composite member and the size requirement of prefabricated pore defects, wherein the pore defect prefabricated filling particles meet the size requirement of the prefabricated pore defects, the glass transition temperature of the pore defect prefabricated filling particles is higher than the highest temperature in the molding process of the member, and the pore defect prefabricated filling particles are not adhered with resin used in the carbon fiber reinforced resin matrix composite member; the particle size of the selected pore defect prefabricated filling particles is 2-700 mu m. The pore defect pre-filling particles comprise polytetrafluoroethylene particles or/and silica particles, preferably polytetrafluoroethylene particles.
Step 2, uniformly spreading a proper amount of pore defect prefabricated filling particles on an ultrasonic vibration platform, sealing the upper part of the ultrasonic vibration platform by using sealant and a isolating film, and then performing ultrasonic vibration treatment; the ultrasonic vibration treatment time is more than 1min. Screening the pore defect prefabricated filling particles; when screening, screening the pore defect prefabricated filling particles by using a standard screen with screening size larger than the required size, removing the particles with oversized size, and then screening the obtained pore defect prefabricated filling particles by using a standard screen with screening size smaller than the required size, and removing the particles with undersize.
And 3, converting the pore defect prefabricated filling particles with corresponding volumes into corresponding masses according to a density formula according to the porosity required by the prefabricated pore defects, and weighing the pore defect prefabricated filling particles with the screened corresponding masses by adopting a milligram-scale electronic scale.
And 4, carrying out ultrasonic vibration treatment on the screened and weighed particles again. Adopting glass rod electrostatic adsorption to dip pore defect prefabricated filling particles, uniformly placing the pore defect prefabricated filling particles at positions where the pore defects need to be prefabricated, and bonding the pore defect prefabricated filling particles with a composite material layer into a whole; before electrostatic adsorption dipping of the glass rod, firstly carrying out friction electrification treatment on the glass rod on silk; when placing the glass stick and adsorbing the pore defect prefabricated filling particles that dips in, heat the combined material in order to improve desorption effect, if desorption effect is not good, once place and can not accomplish the desorption, then carry out hot-blast heating to the combined material and reach the temperature that once places and accomplish the desorption.
Step 5, vibrating and pre-compacting the carbon fiber reinforced resin matrix composite member after the paving; the vibration precompaction treatment steps are as follows:
step 5.1, paving the composite material component on a die, sealing by using a vacuum bag, vacuumizing until the pressure in the bag is less than or equal to-0.09 mpa, and closing a vacuum pump to perform pressure maintaining operation to check the air tightness;
step 5.2, measuring an exothermic peak of the resin system in the used composite material by using a DSC differential scanning calorimeter, wherein the temperature corresponding to the measured exothermic peak is the temperature of the resin system for crosslinking and curing reaction, and is marked as K;
and 5.3, placing the vacuum sealed die on a random vibration table, fixedly connecting the die with the random vibration table by using a pressing bar, connecting a vacuum pump, setting the temperature and vibration acceleration in a cavity of the random vibration table, setting the temperature in the cavity of the random vibration table to be less than K, starting the vacuum pump, running a heating program and a vibration program of the vibration table, continuing to run for a period of time after the temperature reaches the set temperature, closing the heating program and the vibration program, taking out after the die and the components are cooled, and completing vibration precompaction treatment.
The vibration acceleration is set to 8-12 g; continuously running for 5-12 min after the temperature of the random vibration table reaches the set temperature;
temperature setting range in cavity of random vibration table: the minimum temperature is the temperature corresponding to the point with the slope larger than-1 in the viscosity-temperature curve of the resin system, the maximum temperature is K-30 ℃, and the viscosity corresponding to the set temperature is smaller than 200 Pa sec.
The vibration precompaction treatment eliminates the influence of the existence of natural pores on the defect research effect of the prefabricated pores of the composite material. The viscosity of the resin is greatly reduced when the resin is heated to a set temperature, the resin is in a viscous state, and the resin is in a vibration auxiliary and vacuum environment, so that gas in the composite material component can be rapidly discharged, most of natural pore defects in the component can be removed through vibration precompaction treatment, and the interference caused by the natural pore defects in subsequent experiments is avoided.
And 6, transferring the carbon fiber reinforced resin matrix composite material component subjected to the vibration precompaction treatment into an autoclave, connecting a vacuum pump, and performing hot pressing, curing and forming. In the hot press solidification forming process, the temperature rising rate, the heat preservation platform and the temperature reducing rate are set according to the solidification characteristics of the resin system.
Examples
The target pore defect size was 30.+ -.10. Mu.m, and polytetrafluoroethylene particles of 35 μm size were selected.
Polytetrafluoroethylene with a density of 2.2g/cm 3 The volume of the prepared member is 15cm 3 The porosity was 1%, and the required poly-tetrafluoroethane was calculatedThe volume of alkene particles is 0.15cm 3 The corresponding weight was 0.33g, and 0.4g of fine particles were weighed by a milligram-scale electronic scale.
Placing the particles on an ultrasonic vibration platform for ultrasonic vibration treatment, then pouring the particles into a 500-mesh standard sieve, placing a milligram-grade electronic scale below, pouring the sieved particles into a 600-mesh standard sieve, and taking the particles on the sieve, thereby obtaining the particles meeting the requirements.
The composite laminate was initially prepared using a selected material of T800/epoxy prepreg with a cure temperature of 130 ℃.
And (3) blanking: the prepreg was cut into a square with a side length of 10 cm.
Paving: 10 layers are paved in total, orthogonal paving is adopted, defect embedding is carried out in the paving, polytetrafluoroethylene particles are dipped by using a glass rod and placed at positions where pore defects are required to be arranged, a milligram-grade electronic scale is observed, and finally, 0.02g of particles are left, so that defect embedding and paving are completed.
Vibration pretreatment: according to the viscosity-temperature curve and the DSC curve, the temperature in the cavity is set to be 70 ℃ during vibration, the vibration acceleration is 10g, and the vibration time is 10min.
And (5) hot pressing and curing: and (3) sealing the bags of the components to be cured after the treatment, and feeding the components to be cured into an autoclave for hot pressing, curing and forming.
The foregoing is a further detailed description of the invention in connection with specific preferred embodiments, and is not intended to limit the practice of the invention to such description. It will be apparent to those skilled in the art that several simple deductions and substitutions can be made without departing from the spirit of the invention, and these are considered to be within the scope of the invention.
Claims (10)
1. A method for prefabricating a composite void defect, comprising the steps of:
step 1, selecting pore defect prefabricated filling particles according to a molding process of a carbon fiber reinforced resin matrix composite member and the size requirement of prefabricated pore defects, wherein the pore defect prefabricated filling particles meet the size requirement of the prefabricated pore defects, the glass transition temperature of the pore defect prefabricated filling particles is higher than the highest temperature in the molding process of the member, and the pore defect prefabricated filling particles are not adhered with resin used in the carbon fiber reinforced resin matrix composite member;
step 2, screening the pore defect prefabricated filling particles;
step 3, converting the pore defect prefabricated filling particles with corresponding volumes into corresponding masses according to a density formula according to the porosity required by the prefabricated pore defects, and weighing the pore defect prefabricated filling particles with the screened corresponding masses;
step 4, uniformly placing the pore defect prefabrication filling particles at positions where the pore defects need to be prefabricated, and pasting the pore defect prefabrication filling particles and the composite material layering into a whole;
step 5, vibrating and pre-compacting the carbon fiber reinforced resin matrix composite member after the paving;
and 6, transferring the carbon fiber reinforced resin matrix composite material component subjected to the vibration precompaction treatment into an autoclave, connecting a vacuum pump, and performing hot pressing, curing and forming.
2. The method for prefabricating void defects in a composite material according to claim 1, wherein in the step 1, the particle size of the void defect prefabricating and filling particles is selected to be 2-700 μm; the pore defect prefabricated filling particles comprise polytetrafluoroethylene particles or/and silicon dioxide particles.
3. The method for prefabricating void defects in composite materials according to claim 1, wherein in step 2, the void defect prefabricating filling particles are subjected to ultrasonic vibration treatment before being screened; in the step 4, before the pore defect prefabricated filling particles are uniformly placed at the positions where the pore defects are required to be prefabricated, ultrasonic vibration treatment is carried out on the pore defect prefabricated filling particles.
4. The method for prefabricating the pore defects of the composite material according to claim 3, wherein when the pore defect prefabricating and filling particles are subjected to ultrasonic vibration treatment, a proper amount of pore defect prefabricating and filling particles are uniformly paved on an ultrasonic vibration platform, and sealing is performed above the ultrasonic vibration platform by using a sealant and a isolating film, and then the ultrasonic vibration treatment is performed; the ultrasonic vibration treatment time is more than 1min.
5. The method for prefabricating the pore defects of the composite material according to claim 1, wherein in the step 2, the pore defect prefabricating and filling particles are screened by a standard screen with screening size larger than the required size, and the oversized particles are removed; the weighing process in the step 3 adopts a milligram-grade electronic scale as a tool.
6. The method for prefabricating void defects in a composite material according to claim 5, wherein after oversized particles are removed, screening the obtained void defect prefabricating filling particles by using a standard screen with a screening size smaller than the required size, and removing undersized particles.
7. The method for prefabricating void defects in composite materials according to claim 1, wherein in the step 4, the void defect prefabricating and filling particles are uniformly placed at the positions where the void defects are required to be prefabricated, and the void defect prefabricating and filling particles are placed in a manner of dipping the void defects by electrostatic adsorption of glass rods.
8. The method for prefabricating the pore defects of the composite material according to claim 7, wherein before the glass rod is subjected to electrostatic absorption dipping, the glass rod is subjected to frictional electrification treatment on silk; when the glass rod is placed to adsorb and dip the pore defect prefabricated filling particles, the composite material is heated to improve the desorption effect.
9. The method for prefabricating void defects in composite materials according to claim 1, wherein in step 5, the step of vibration precompaction is as follows:
step 5.1, paving the composite material component on a die, sealing by using a vacuum bag, vacuumizing until the pressure in the bag is less than or equal to-0.09 mpa, and closing a vacuum pump to perform pressure maintaining operation to check the air tightness;
step 5.2, measuring an exothermic peak of the resin system in the used composite material by using a DSC differential scanning calorimeter, wherein the temperature corresponding to the measured exothermic peak is the temperature of the resin system for crosslinking and curing reaction, and is marked as K;
and 5.3, placing the vacuum sealed die on a random vibration table, fixedly connecting the die with the random vibration table by using a pressing bar, connecting a vacuum pump, setting the temperature and vibration acceleration in a cavity of the random vibration table, setting the temperature in the cavity of the random vibration table to be less than K, starting the vacuum pump, running a heating program and a vibration program of the vibration table, continuing to run for a period of time after the temperature reaches the set temperature, closing the heating program and the vibration program, taking out after the die and the components are cooled, and completing vibration precompaction treatment.
10. The method for prefabricating void defects in composite materials according to claim 9, wherein in step 5.3, the vibration acceleration is set to 8-12 g; continuously running for 5-12 min after the temperature of the random vibration table reaches the set temperature;
temperature setting range in cavity of random vibration table: the minimum temperature is the temperature corresponding to the point with the slope larger than-1 in the viscosity-temperature curve of the resin system, the maximum temperature is K-30 ℃, and the viscosity corresponding to the set temperature is smaller than 200 Pa sec.
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