CN114436670A - Winding forming-based high-strength carbon-carbon cylinder preparation method - Google Patents

Winding forming-based high-strength carbon-carbon cylinder preparation method Download PDF

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CN114436670A
CN114436670A CN202210221002.8A CN202210221002A CN114436670A CN 114436670 A CN114436670 A CN 114436670A CN 202210221002 A CN202210221002 A CN 202210221002A CN 114436670 A CN114436670 A CN 114436670A
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carbon
winding
cylinder
temperature
strength
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魏益强
侯光远
杨浩
李志保
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Xi'an Meilan New Material Co ltd
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Xi'an Meilan New Material Co ltd
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    • C04B35/71Ceramic products containing macroscopic reinforcing agents
    • C04B35/78Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
    • C04B35/80Fibres, filaments, whiskers, platelets, or the like
    • C04B35/83Carbon fibres in a carbon matrix
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    • C04B35/52Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
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Abstract

The invention discloses a preparation method of a high-strength carbon-carbon cylinder based on winding forming, which relates to the technical field of carbon-carbon composite materials, and comprises the following steps: preparing a cylinder winding mold, preparing a colloidal solution to prepare carbon fibers with glue, circularly winding the carbon fibers with glue on the cylinder winding mold to obtain a cylindrical winding body, carrying out rotary curing on the cylindrical winding body to obtain a high-strength carbon fiber composite material winding cylinder, carrying out impregnation carbonization to obtain a carbon-carbon cylinder blank, carrying out high-temperature graphitization treatment on the carbon-carbon cylinder blank, carrying out mechanical processing to obtain a carbon-carbon cylinder semi-finished product, putting the carbon-carbon cylinder semi-finished product into a deposition furnace, and carrying out surface coating treatment to obtain the carbon-carbon cylinder; compared with a net tire and carbon cloth composite forming process, the method reduces the generation of carbon fiber leftover materials and greatly reduces the cost of raw materials.

Description

Winding forming-based high-strength carbon-carbon cylinder preparation method
Technical Field
The invention belongs to the technical field of carbon-carbon composite materials, and particularly relates to a preparation method of a high-strength carbon-carbon cylinder based on winding forming.
Background
The carbon-carbon composite material is used as a novel structural material, and has the characteristics of high specific strength, high temperature resistance, excellent thermal shock resistance, good ablation resistance, low thermal expansion coefficient and the like, which completely meet the requirements of a single crystal thermal field, and can be rapidly developed along with market demands, particularly in the aspects of carbon-carbon crucibles, carbon-carbon heat shields, carbon-carbon heat-preservation barrels and the like;
however, the current process route of carbon-carbon composite material thermal field products is mainly that carbon fiber plain cloth and a net tire are needled to form a prefabricated body, then densification and high-temperature graphitization treatment are carried out, and finally finished product manufacturing is finished through machining.
Disclosure of Invention
The invention aims to provide a preparation method of a high-strength carbon-carbon cylinder based on winding forming, so as to solve the problems in the background technology.
The technical scheme adopted by the invention is as follows:
a preparation method of a high-strength carbon-carbon cylinder based on winding forming comprises the following steps:
step 1, preparing a cylinder winding mould.
And 2, mounting the cylinder winding mould on a winding machine.
And 3, coating the surface of the cylinder winding mould with tetrafluoro cloth.
And 4, preparing a colloidal solution, namely mixing the phenolic resin, the graphite powder and the curing agent to prepare the colloidal solution.
And 5, placing the colloidal solution prepared in the step 4 into a colloidal solution tank, heating by adopting a constant-temperature water bath heating tank, and simultaneously starting an ultrasonic transducer.
And 6, dipping the carbon fiber into glue, namely dipping the carbon fiber on the carbon fiber tow hub into a colloidal solution in a colloidal solution tank after passing through a yarn spreading roller, and then, passing the carbon fiber from the colloidal solution through two continuous groups of glue squeezing press rollers to obtain the carbon fiber with glue, wherein the mass fraction of the colloidal solution is 30-35%.
And 7, winding and forming the cylinder, namely enabling the carbon fiber with the adhesive in the step 6 to penetrate out of the screw nozzle, and then circularly winding on a cylinder winding mould to obtain the cylindrical winding body.
And 8, curing the cylindrical winding body, namely performing rotary curing on the cylindrical winding body in the step 7 at a linear speed of 2-5m/min, and removing the winding mold of the cylinder body after curing to obtain the high-strength carbon fiber composite material winding cylinder.
And 9, dipping and carbonizing, namely dipping the high-strength carbon fiber composite material winding barrel belt upper tool obtained in the step 8 in furan resin for 2-5h, and then raising the temperature to 850-1000 ℃ at the heating rate of 10-20 ℃/h for carbonizing treatment to obtain a carbon-carbon barrel blank.
Step 10, repeating the step 9 until the density of the carbon-carbon cylinder blank in the step 9 is more than 1.4g/cm3
And 11, performing high-temperature graphitization treatment, namely putting the carbon-carbon cylinder blank obtained in the step 10 into a high-temperature furnace to complete the high-temperature graphitization treatment.
And 12, machining, namely removing the tool from the carbon-carbon cylinder blank obtained in the step 11, and machining the inner surface, the outer surface and the port of the carbon-carbon cylinder blank to obtain a high-strength carbon-carbon cylinder semi-finished product.
And step 13, surface treatment, namely putting the semi-finished product of the high-strength carbon-carbon cylinder obtained in the step 12 into a deposition furnace, and carrying out surface coating treatment to obtain the carbon-carbon cylinder which is formed by winding and has the hoop tensile strength of more than or equal to 500 MPa.
Preferably, in the colloidal solution in step 4:
the phenolic resin is thermosetting phenolic resin with the solid content of more than 50 percent and the viscosity of 150-1000 MPa-s/25 ℃;
the graphite powder is 1000nm of 100-inch sand-doped nano graphite powder with carbon content more than 99.99 percent, and the mass ratio of the nano graphite powder to the thermosetting phenolic resin is 10 to 25 percent;
the curing agent is a special curing agent for thermosetting phenolic resin, and the mass ratio of the curing agent to the thermosetting phenolic resin is 3-5%.
Preferably, in the step 5, the temperature of the constant temperature water bath heating tank is controlled to be 40-80 ℃.
Preferably, in step 7, the winding tension of the carbon fiber with glue by the filament nozzle is 55-75N at the initial value, the winding speed is 30-60m/min, the winding speed is 0.5-0.2N progressively decreased every 1-3 layers, and 1-3 layers of hoop winding and 1-3 layers of spiral winding form a repeating unit.
Preferably, in the step 8, the rotational curing is performed by four-stage heating, the first stage is performed by heating to 70-90 ℃ at a heating rate of 10-40 ℃/h for pre-curing, the second stage is performed by constant-temperature curing at 70-90 ℃ for 1-3h, the third stage is performed by heating to 120-.
Preferably, in step 11, the vacuum degree in the high temperature furnace is less than 100pa, and the temperature of the high temperature furnace is kept constant for 2-4h after the temperature rise rate of the high temperature furnace is increased to 1900-2500 ℃ at a speed of 10-100 ℃/h.
In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that:
compared with a carbon fiber needling process, the method better reserves the excellent mechanical property of the carbon fiber;
compared with a net tire and carbon cloth composite forming process, the method reduces the generation of carbon fiber leftover materials, greatly reduces the cost of raw materials, also avoids the problem of uneven density caused by uneven distribution of the net tire, improves the utilization rate of carbon fibers and improves the consistency of the density of carbon products;
the carbon-carbon cylinder prepared by the preparation method has low surface and internal porosity, is more resistant to ablation, corrosion and oxidation, and has wider application range in the preparation of single crystal thermal field components.
Drawings
FIG. 1 is a block flow diagram of the present invention;
FIG. 2 is a schematic structural view of a carbon fiber running of the present invention;
in the figure: 1. a carbon fiber tow hub; 2. a yarn spreading roller; 3. an ultrasonic transducer; 4. a constant-temperature water bath heating tank; 5. a colloidal solution tank; 6. extruding glue and pressing rollers; 7. a nipple; 8. the cylinder body is wound on the die.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example one
Referring to fig. 1-2, a method for manufacturing a high-strength carbon-carbon cylinder based on winding molding comprises the following steps:
step 1, preparing a cylinder winding mold 8, wherein the cylinder winding mold 8 is formed by sealing a wood keel and a wood board with the water content of less than 14%, machining, splicing, assembling and polishing.
And 2, mounting a flange at the center of the sealing end of the cylinder winding mold 8 in the step 1, connecting the shaft core and the cylinder winding mold 8 into a whole through a coaxial flange, and mounting the cylinder winding mold 8 with the shaft core on a winding machine.
And 3, wrapping the surface of the barrel winding mold 8 in the step 2 with the tetrafluoro cloth to obtain the barrel winding mold 8 tightly wrapped with the tetrafluoro cloth.
Step 4, preparing a colloidal solution, wherein the colloidal solution is a mixed solution of phenolic resin, graphite powder and a curing agent; the phenolic resin in the colloidal solution is water-soluble thermosetting phenolic resin with the solid content of 75 percent and the viscosity of 200-; the graphite powder in the colloidal solution is nano graphite powder with the granularity of 100-1000nm and the carbon content of more than 99.99 percent, and the mass ratio of the nano graphite powder to the water-soluble thermosetting phenolic resin is 25 percent; the curing agent in the colloidal solution is a special curing agent for water-soluble thermosetting phenolic resin, and the mass ratio of the curing agent to the water-soluble thermosetting phenolic resin is 5%.
And 5, placing the colloidal solution prepared in the step 4 in a colloidal solution tank 5, starting a constant temperature water bath heating tank 4 to heat at 50 ℃, and simultaneously starting an ultrasonic transducer 3.
And 6, dipping the carbon fiber in glue, namely, passing the carbon fiber on the carbon fiber tow hub 1 through four groups of winding machine yarn spreading rotating rollers 2 and then dipping the carbon fiber into the colloidal solution in the step 5, continuously passing the carbon fiber out of the colloidal solution through two groups of glue squeezing press rollers 6, and adjusting the pressure of the glue squeezing press rollers 6 to obtain the carbon fiber with glue with the mass fraction of the colloidal solution of 30-35%.
And 7, winding and molding the cylinder, namely, enabling the carbon fiber with the glue in the step 6 to penetrate out of a wire nozzle 7 of a winding machine, gradually decreasing by 0.5N every 3 layers with the initial value of winding tension of 60N, enabling the winding speed to be 50m/min, enabling 1 layer of circumferential winding and 1 layer of spiral winding to be a repeating unit, and circularly winding on a cylinder winding mold 8 to obtain the cylindrical winding body.
Step 8, curing the cylindrical winding body, namely performing rotary curing on the cylindrical winding body in the step 7 at a linear speed of 4 m/min; the rotary curing adopts a four-section heating scheme, the temperature is raised to 80 ℃ at the heating rate of 20 ℃/h for precuring, the curing is carried out at the constant temperature of 80 ℃ for 2h, the temperature is raised to 150 ℃ at the heating rate of 20 ℃/h for curing, and the curing is carried out at the constant temperature of 150 ℃ for 3 h; and after rotary curing, removing the cylinder winding mould 8 to obtain the high-strength carbon fiber composite material winding cylinder.
And 9, resin impregnation and curing, namely immersing the carbon fiber composite material winding barrel belt upper tool in the step 8 in furan resin for 3 hours under the pressure of 1.8MPa, heating to 180 ℃ at the heating rate of 20 ℃/h, and preserving the heat at 180 ℃ for 2 hours to complete resin curing, so as to obtain the furan resin densified barrel resin material.
And step 10, carbonizing resin, namely putting the barrel resin material obtained in the step 9 into a carbonization furnace, and raising the temperature to 900 ℃ at a heating rate of 10 ℃/h for carbonization treatment to obtain a carbon-carbon barrel blank.
Step 11, repeating the step 9 and the step 10 until the density of the carbon cylinder blank is more than 1.4g/cm in the step 103
And 12, performing high-temperature graphitization treatment, namely putting the carbon-carbon cylinder blank obtained in the step 11 into a high-temperature furnace, heating to 2100 ℃ at the heating rate of 50 ℃/h under the condition that the vacuum degree is less than 100pa, and keeping the temperature for 4h to complete the high-temperature graphitization treatment.
And step 13, machining, namely removing the tool from the carbon-carbon cylinder blank obtained in the step 12, and machining the inner surface, the outer surface and the port of the carbon-carbon cylinder blank to obtain a high-strength carbon-carbon cylinder semi-finished product.
And 14, performing surface treatment, namely putting the semi-finished product of the high-strength carbon-carbon cylinder obtained in the step 13 into a deposition furnace, and performing surface coating treatment to obtain the high-strength carbon-carbon cylinder based on winding forming.
Example two
Referring to fig. 1-2, a method for manufacturing a high-strength carbon-carbon cylinder based on winding molding comprises the following steps:
step 1, preparing a cylinder winding mold 8, wherein the cylinder winding mold 8 is a splicing type cylinder winding mold 8 made of high-strength alloy materials.
And 2, mounting the spliced cylinder winding mould 8 in the step 1 on a winding machine, and uniformly coating a release agent on the surface of the cylinder winding mould 8.
Step 3, preparing a colloidal solution, wherein the colloidal solution is a mixed solution of phenolic resin and graphite powder; the phenolic resin in the colloidal solution is alcohol-soluble thermosetting phenolic resin with the solid content of 75 percent and the viscosity of 400-1000MPa & s/25 ℃; the graphite powder in the colloidal solution is nano graphite powder with the granularity of 100-1000nm and the carbon content of more than 99.99 percent, and the mass ratio of the nano graphite powder to the alcohol-soluble thermosetting phenolic resin is 15 percent.
And 4, placing the colloidal solution prepared in the step 3 in a colloidal solution tank 5, starting the constant-temperature water bath heating tank 4 to heat at 40 ℃ and starting the ultrasonic transducer 3 at the same time.
And 5, dipping the carbon fiber in glue, namely, passing the carbon fiber on the carbon fiber tow hub 1 through four groups of winding machine yarn spreading rotating rollers 2 and then dipping the carbon fiber into the colloidal solution in the step 4, continuously passing the carbon fiber from the colloidal solution through two groups of glue squeezing press rollers 6, and adjusting the pressure of the glue squeezing press rollers 6 to obtain the carbon fiber with glue, the mass fraction of which is 30-35%, of the colloidal solution.
And 6, winding and molding the cylinder, namely enabling the carbon fiber with the glue in the step 5 to penetrate out of a wire nozzle 7 of a winding machine, enabling the winding tension to be 75N at an initial value, decreasing by 0.2N for each layer, enabling the winding speed to be 40m/min, enabling 4 layers of circumferential winding and 2 layers of spiral winding to be a repeating unit, and circularly winding on a cylinder winding mold 8 to obtain the cylindrical winding body.
Step 7, curing the cylindrical winding body, namely performing rotary curing on the cylindrical winding body in the step 6 at a linear speed of 4 m/min; the rotary curing adopts a four-section heating scheme, the temperature is increased to 90 ℃ at the heating rate of 15 ℃/h for precuring, the temperature is constant at 90 ℃ for curing for 2h, the temperature is increased to 160 ℃ at the heating rate of 20 ℃/h for curing, and the temperature is constant at 160 ℃ for curing for 3 h; and after rotary curing, removing the cylinder winding mould 8 to prepare the high-strength carbon fiber reinforced resin matrix composite winding cylinder.
And 8, resin impregnation and curing, namely putting the carbon fiber reinforced resin matrix composite material winding barrel belt on the tool in the step 7 into an impregnation curing furnace, impregnating the carbon fiber reinforced resin matrix composite material winding barrel belt for 3 hours under the pressure condition of 1.8MPa with furan resin, then discharging residual resin, raising the temperature to 180 ℃ at the heating rate of 20 ℃/h, and preserving the temperature at 180 ℃ for 2 hours to finish resin curing, so as to obtain the furan resin densified barrel resin material.
And 9, carbonizing resin, namely putting the cylinder body resin material obtained in the step 8 into a carbonization furnace, and raising the temperature to 900 ℃ at the heating rate of 10 ℃/h for carbonization treatment to obtain a carbon cylinder body blank.
Step 10, repeating the step 8 and the step 9 until the density of the carbon-carbon cylinder blank in the step 9 is more than 1.4g/cm3
And 11, performing high-temperature graphitization, namely putting the carbon-carbon cylinder blank obtained in the step 10 into a high-temperature furnace, heating to 2100 ℃ at a heating rate of 50 ℃/h under the condition that the vacuum degree is less than 100pa, and keeping the temperature for 4h to complete the high-temperature graphitization.
And 12, machining, namely removing the tool from the carbon-carbon cylinder blank obtained in the step 11, and machining the inner surface, the outer surface and the port of the carbon-carbon cylinder blank to obtain a high-strength carbon-carbon cylinder semi-finished product.
And step 13, surface treatment, namely putting the semi-finished product of the high-strength carbon-carbon cylinder obtained in the step 12 into a deposition furnace, and carrying out surface coating treatment to obtain the high-strength carbon-carbon cylinder based on winding forming.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.

Claims (6)

1. A preparation method of a high-strength carbon-carbon cylinder based on winding forming is characterized by comprising the following steps: the method comprises the following steps:
step 1, preparing a cylinder winding mould (8);
step 2, mounting a cylinder winding mould (8) on a winding machine;
step 3, coating the surface of the cylinder winding die (8) with tetrafluoro cloth;
step 4, preparing a colloidal solution, namely mixing phenolic resin, graphite powder and a curing agent to prepare the colloidal solution;
step 5, placing the colloidal solution prepared in the step 4 into a colloidal solution tank (5), heating by adopting a constant-temperature water bath heating tank (4), and simultaneously starting an ultrasonic transducer (3);
step 6, carbon fiber gum dipping, namely, after carbon fibers on a carbon fiber tow hub (1) pass through a yarn spreading rotating roller (2), soaking the carbon fibers into a colloidal solution in a colloidal solution tank (5), and then, passing the carbon fibers from the colloidal solution through two continuous groups of gum squeezing press rollers (6) to prepare carbon fibers with gum, the mass fraction of which is 30-35%, of the colloidal solution;
step 7, winding and forming the cylinder, namely enabling the carbon fiber with the adhesive in the step 6 to penetrate out of the screw nozzle (7), and then circularly winding on a cylinder winding die (8) to obtain a cylinder winding body;
8, curing the cylindrical winding body, namely performing rotary curing on the cylindrical winding body in the step 7 at a linear speed of 2-5m/min, and removing a cylinder winding mold (8) after curing to obtain a high-strength carbon fiber composite material winding cylinder;
step 9, dipping and carbonizing, namely dipping the high-strength carbon fiber composite material winding barrel belt upper tool obtained in the step 8 in furan resin for 2-5h, and then raising the temperature to 850-1000 ℃ at the heating rate of 10-20 ℃/h for carbonizing treatment to obtain a carbon-carbon barrel blank;
step 10, repeating the step 9 until the density of the carbon-carbon cylinder blank in the step 9 is more than 1.4g/cm3
Step 11, performing high-temperature graphitization treatment, namely putting the carbon-carbon cylinder blank obtained in the step 10 into a high-temperature furnace to complete the high-temperature graphitization treatment;
step 12, machining, namely removing a tool from the carbon-carbon cylinder blank obtained in the step 11, and machining the inner surface, the outer surface and the port of the carbon-carbon cylinder blank to obtain a high-strength carbon-carbon cylinder semi-finished product;
and step 13, surface treatment, namely putting the semi-finished product of the high-strength carbon-carbon cylinder obtained in the step 12 into a deposition furnace, and carrying out surface coating treatment to obtain the carbon-carbon cylinder which is formed by winding and has the hoop tensile strength of more than or equal to 500 MPa.
2. The preparation method of the high-strength carbon-carbon cylinder based on winding forming as claimed in claim 1, wherein: in the colloidal solution in step 4:
the phenolic resin is thermosetting phenolic resin with the solid content of more than 50 percent and the viscosity of 150-1000 MPa-s/25 ℃;
the graphite powder is 1000nm of 100-inch sand-doped nano graphite powder with carbon content more than 99.99 percent, and the mass ratio of the nano graphite powder to the thermosetting phenolic resin is 10 to 25 percent; the curing agent is a special curing agent for thermosetting phenolic resin, and the mass ratio of the curing agent to the thermosetting phenolic resin is 3-5%.
3. The preparation method of the high-strength carbon-carbon cylinder based on winding forming as claimed in claim 1, wherein: in the step 5, the temperature of the constant-temperature water bath heating tank (4) is controlled to be 40-80 ℃.
4. The preparation method of the high-strength carbon-carbon cylinder based on winding forming as claimed in claim 1, wherein: in the step 7, the initial value of the winding tension of the carbon fiber with the adhesive of the silk nozzle (7) is 55-75N, the winding speed is 30-60m/min, the winding tension of every 1-3 layers of the carbon fiber with the adhesive is gradually reduced by 0.5-0.2N, and 1-3 layers of the hoop winding and 1-3 layers of the spiral winding are a repeating unit.
5. The preparation method of the high-strength carbon-carbon cylinder based on winding forming as claimed in claim 1, wherein: in the step 8, the rotary curing adopts four-section temperature rise, the first section is pre-cured by raising the temperature to 70-90 ℃ at the temperature rise rate of 10-40 ℃/h, the second section is cured at the constant temperature of 70-90 ℃ for 1-3h, the third section is cured by raising the temperature to 200 ℃ at the temperature rise rate of 15-30 ℃/h, and the fourth section is cured at the constant temperature of 120 ℃ to 200 ℃ for 2-4 h.
6. The preparation method of the high-strength carbon-carbon cylinder based on winding forming as claimed in claim 1, wherein: in step 11, the vacuum degree in the high temperature furnace is less than 100pa, and the temperature of the high temperature furnace is kept constant for 2-4h after being increased to 1900-.
CN202210221002.8A 2022-03-09 2022-03-09 Winding forming-based high-strength carbon-carbon cylinder preparation method Pending CN114436670A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115259882A (en) * 2022-08-02 2022-11-01 内蒙古康碳复合材料科技有限公司 Production process of composite fiber filament winding carbon-carbon composite material

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Application publication date: 20220506