CN116238095A - Preparation method of carbon cylinder column - Google Patents
Preparation method of carbon cylinder column Download PDFInfo
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- CN116238095A CN116238095A CN202310139296.4A CN202310139296A CN116238095A CN 116238095 A CN116238095 A CN 116238095A CN 202310139296 A CN202310139296 A CN 202310139296A CN 116238095 A CN116238095 A CN 116238095A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 18
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- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
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Images
Classifications
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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
- B29C45/00—Injection moulding, i.e. forcing the required volume of moulding material through a nozzle into a closed mould; Apparatus therefor
- B29C45/14—Injection moulding, i.e. forcing the required volume of moulding material through a nozzle into a closed mould; Apparatus therefor incorporating preformed parts or layers, e.g. injection moulding around inserts or for coating articles
-
- 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
- B29C45/00—Injection moulding, i.e. forcing the required volume of moulding material through a nozzle into a closed mould; Apparatus therefor
- B29C45/0005—Injection moulding, i.e. forcing the required volume of moulding material through a nozzle into a closed mould; Apparatus therefor using fibre reinforcements
-
- 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
- B29C45/00—Injection moulding, i.e. forcing the required volume of moulding material through a nozzle into a closed mould; Apparatus therefor
- B29C45/0053—Injection moulding, i.e. forcing the required volume of moulding material through a nozzle into a closed mould; Apparatus therefor combined with a final operation, e.g. shaping
-
- 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
- B29C45/00—Injection moulding, i.e. forcing the required volume of moulding material through a nozzle into a closed mould; Apparatus therefor
- B29C45/14—Injection moulding, i.e. forcing the required volume of moulding material through a nozzle into a closed mould; Apparatus therefor incorporating preformed parts or layers, e.g. injection moulding around inserts or for coating articles
- B29C45/1418—Injection moulding, i.e. forcing the required volume of moulding material through a nozzle into a closed mould; Apparatus therefor incorporating preformed parts or layers, e.g. injection moulding around inserts or for coating articles the inserts being deformed or preformed, e.g. by the injection pressure
-
- 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
- B29C45/00—Injection moulding, i.e. forcing the required volume of moulding material through a nozzle into a closed mould; Apparatus therefor
- B29C45/17—Component parts, details or accessories; Auxiliary operations
- B29C45/26—Moulds
- B29C45/34—Moulds having venting means
-
- 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
- B29C45/00—Injection moulding, i.e. forcing the required volume of moulding material through a nozzle into a closed mould; Apparatus therefor
- B29C45/17—Component parts, details or accessories; Auxiliary operations
- B29C45/76—Measuring, controlling or regulating
-
- 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
- B29C45/00—Injection moulding, i.e. forcing the required volume of moulding material through a nozzle into a closed mould; Apparatus therefor
- B29C45/17—Component parts, details or accessories; Auxiliary operations
- B29C45/76—Measuring, controlling or regulating
- B29C45/78—Measuring, controlling or regulating of temperature
Abstract
The application relates to the technical field of carbon-carbon composite materials, and particularly discloses a preparation method of a carbon-carbon cylindrical column, which comprises the following steps: s1, uniformly mixing a reinforcing material and thermosetting resin to obtain a compression injection material; s2, fixing a plurality of carbon ropes in a forming die at intervals, arranging the carbon ropes along the axial direction of the forming die, pressurizing and injecting a pressure injection material into an inner cavity of the forming die from a feeding hole below the forming die, discharging air from an exhaust hole at the top of the forming die, and sealing the feeding hole and keeping the exhaust hole in an open state after the pressure injection is finished; s3, heating the forming die to solidify the injection material and the carbon rope, and demolding to obtain a resin-based column; and S4, sequentially carrying out densification treatment and graphitization treatment on the resin-based column, and finally carrying out mechanical processing to obtain the carbon-carbon cylindrical column. The preparation method has the advantages of reducing raw material waste, reducing cost and improving the production efficiency and mechanical property of the carbon cylinder column.
Description
Technical Field
The invention relates to the technical field of carbon-carbon composite materials, in particular to a preparation method of a carbon-carbon cylinder column.
Background
The carbon-carbon composite material is more applied to the fields of aerospace, semiconductor thermal fields and the like due to the excellent performances of high temperature resistance, mechanical strength, service life and the like. The carbon-carbon cylinder column structure is extremely widely applied to the aspects of brake discs, throat liners, spray pipes, thermal fields and the like.
The related art discloses a preparation method of a carbon ceramic composite material, which comprises the following steps: s1, yarn is put, a fiber shaft is put on a creel, and each yarn shaft is provided with a tension system; s2, soaking yarns, namely pulling the fibers through a resin tank to enable the fibers to be completely soaked in resin; s3, winding the fiber yarn soaked with the resin on the surface of a prepared preform die, winding the fiber yarn on the surface of the preform die into a net, and needling; s4, curing, namely heating to cure the resin; s5, demolding to obtain a preform blank; s6, cutting, namely cutting the carbon cylinder column into a plurality of sections along the axial direction of the prefabricated body according to the designed specific specification thickness, so as to obtain the prefabricated body, carrying out multiple vapor deposition densification and liquid phase impregnation densification, carrying out graphitization treatment, and finally carrying out mechanical processing to obtain the carbon cylinder column.
Aiming at the related technology, as more carbon cylinders have larger wall thickness or outer diameter, more than 5 densification is generally needed in the preparation process to reach the target density, the densification efficiency is low, and the period is long; in addition, in the preparation process of the carbon fiber preform, a large amount of carbon fiber leftover materials are generated by cutting, the carbon fiber leftover materials are in a net tire or carbon cloth state, the carbon fiber leftover materials are difficult to reuse, and raw materials are seriously wasted.
Disclosure of Invention
In order to improve the production efficiency of the carbon-carbon cylindrical column and reduce raw material waste, the application provides a preparation method of the carbon-carbon cylindrical column.
The preparation method of the carbon-carbon cylindrical column adopts the following technical scheme:
the preparation method of the carbon cylinder column comprises the following steps:
s1, uniformly mixing a reinforcing material and thermosetting resin to obtain a compression injection material;
s2, fixing a plurality of carbon ropes in a forming die at intervals, arranging the carbon ropes along the axial direction of the forming die, pressurizing and injecting a pressure injection material into an inner cavity of the forming die from a feeding hole below the forming die, discharging air from an exhaust hole at the top of the forming die, and sealing the feeding hole and keeping the exhaust hole in an open state after the pressure injection is finished;
s3, heating the forming die to solidify the injection material and the carbon rope, and demolding to obtain a resin-based column;
and S4, sequentially carrying out densification treatment and graphitization treatment on the resin-based column, and finally carrying out mechanical processing to obtain the carbon-carbon cylindrical column.
By adopting the technical scheme, the prefabricated body prepared by the existing needling molding densification process has large porosity, and generally needs to be densified for 5 times or more to reach the target density when a carbon cylinder column with larger wall thickness or outer diameter is produced, and vapor deposition, resin impregnation solidification and carbonization are needed to be sequentially carried out, and the steps of vapor deposition are repeated for a plurality of times, so that the temperature is required to be raised to 900-1000 ℃ stepwise and then to be lowered to normal temperature, the period of one vapor deposition densification step needs about 26 days, the period of one liquid phase impregnation densification step needs about 5 days, and the period of 5 times densification needs at least about 90 days, thereby seriously reducing the production efficiency; according to the method, the carbon ropes are used as main framework materials, the reinforcing materials and the thermosetting resin are mixed to obtain the pressure injection materials, and the pressure injection process is adopted to produce the resin-based column, so that on one hand, the pores in the resin-based column are greatly reduced, only one-time vapor deposition densification or one-time vapor deposition plus one-time liquid phase impregnation densification are needed, the time period of each densification is shortened, the total densification time is reduced to about 30 days, and the production efficiency of the carbon-carbon column is greatly improved; on the other hand, as the pressure injection process adopts the forming die to form, the size of the resin-based column body is more accurate, the turning amount during machining is reduced, the machining efficiency is improved, the carbon fiber leftover materials are greatly reduced, and the production cost is reduced.
Optionally, the pressure in the pressurizing injection in the step S2 is 0.1-0.5MPa.
By adopting the technical scheme, as the injection material is viscous fluid, the injection pressure is too small, and the cavity of the forming die is difficult to be filled with the injection material; the injection pressure is too high, burrs are easily generated, and demolding is difficult, so the pressure at the time of pressure injection is preferably 0.1 to 0.5MPa.
Optionally, the injection speed during the pressurizing injection in the S2 is 1-3m 3 /h。
By adopting the technical scheme, too slow injection speed can lead to overlong injection time and incomplete filling, too fast injection speed is easy to generate burrs, and air is difficult to discharge to lead to higher porosity, so the injection speed is preferably 1-3m 3 /h。
Optionally, heating the forming die in S3 specifically includes:
s31, heating the forming die to 70-90 ℃ at a heating rate of 8-12 ℃/min, and keeping the temperature for 20-40min;
s32, heating the forming die to 110-130 ℃ at a heating rate of 4-6 ℃/min, and keeping the temperature for 10-20min;
s33, heating the forming die to 150-180 ℃ at a heating rate of 8-12 ℃/min, and keeping the temperature for 50-70min.
By adopting the technical scheme, the thermosetting resin contains the solvent, so that the solvent can be fully volatilized by sectional heating and curing, and the porosity is reduced; the S31 is used for quickly reaching the curing temperature, the S32 is used for accelerating the exhaust while the thermosetting resin is cured, reducing the probability of sealing the gas in the thermosetting resin, reducing the porosity, improving the density and reducing the time and the times of subsequent densification; the temperature rising speed of the S33 is increased because the solvent is basically volatilized completely in the S32 stage, so that the thermosetting resin, the reinforcing material and the carbon ropes can be fully cured and crosslinked, the interlayer binding force is improved, and the mechanical property of the carbon-carbon cylindrical column is improved.
Optionally, the reinforcing material in the step S1 comprises carbon black powder and chopped carbon fibers, and the mass ratio of the carbon black powder to the chopped carbon fibers to the thermosetting resin is (1-2): (5-7): (1-4).
Through adopting above-mentioned technical scheme, functional groups such as hydroxyl on carbon black powder surface can form the hydrogen bond with thermosetting resin's molecule, and carbon black powder and chopped carbon fiber evenly distributed are inside thermosetting resin, and carbon black powder and chopped carbon fiber form crosslinked network inside thermosetting resin, play the effect of supplementary reinforcing, cooperate with the carbon rope and improve the mechanical properties of carbon cylinder post.
Optionally, the preparation method of the chopped carbon fiber comprises the following steps: soaking the carbon fiber multifilament in a strong oxidizing solution with the mass fraction of 1% -10% for 10-300min, taking out, washing with water, drying, and cutting to obtain the chopped carbon fiber with the length of 10-60 mm.
Optionally, the carbon rope is subjected to surface activation treatment before being fixed on a forming die: soaking the carbon rope in a strong oxidizing solution with the mass fraction of 1% -10% for 10-300min, taking out, washing with water, and drying to obtain the surface activated carbon rope.
Optionally, the strong oxidizing solution is a nitric acid solution or a hydrogen peroxide solution.
By adopting the technical scheme, the short carbon fiber and the carbon rope have fewer surface functional groups, and when the short carbon fiber and the carbon rope are directly solidified together with thermosetting resin, the interlayer binding force is lower, so that the mechanical property of the carbon cylinder column can be reduced; nitric acid solution or hydrogen peroxide solution is used as strong oxidizing solution, so that the surfaces of inert chopped carbon fibers and carbon ropes can be etched, and oxygen active functional groups such as hydroxyl, carboxyl and the like are added; and the surface roughness of the chopped carbon fiber and the carbon rope is increased, so that the interlayer binding force among the chopped carbon fiber, the carbon rope and the thermosetting resin is improved, a stronger anchoring effect is shown, and finally the mechanical property of the carbon-carbon cylindrical column is improved.
Optionally, the surface activated carbon rope is further subjected to a pre-impregnation treatment: and (3) immersing the surface activated carbon rope in thermosetting resin for 30-60min, taking out and drying to obtain the pre-impregnated carbon rope.
By adopting the technical scheme, after the carbon rope is subjected to presoaked treatment, thermosetting resin is facilitated to enter the tiny pores in the carbon rope, the carbon rope and the thermosetting resin are pre-crosslinked, the porosity is reduced, interlayer binding force between the carbon rope and the injection material is facilitated to be improved, and further the mechanical property of the carbon-carbon cylinder column is improved.
Optionally, the thermosetting resin is water-soluble thermosetting phenolic resin or water-soluble thermosetting epoxy resin, the solid content is more than or equal to 80%, and the viscosity is less than or equal to 600 mPa.s at 25 ℃.
By adopting the technical scheme, the thermosetting resin is controlled to keep higher solid content, the shrinkage after curing is smaller, and the thermosetting resin can be fully crosslinked with the carbon ropes and the reinforcing materials to form a resin-based column body; the viscosity of the thermosetting resin is controlled so as to adapt to the injection molding process of the present application.
In summary, the present application has the following beneficial effects:
1. according to the method, the carbon ropes are used as main framework materials, the reinforcing materials and the thermosetting resin are mixed to obtain the compression injection materials, and the resin-based column is produced by adopting a compression injection process, so that on one hand, the pores in the resin-based column are greatly reduced, and therefore, only 1-2 times of densification are needed, the time length of each densification is shortened, the total densification time is reduced to about 30 days, and the production efficiency of the carbon-carbon column is greatly improved; on the other hand, as the pressure injection process adopts the forming die to form, the size of the resin-based column body is more accurate, the turning amount during machining is reduced, the machining efficiency is improved, the carbon fiber leftover materials are greatly reduced, and the production cost is reduced.
2. The method is characterized in that the method is preferably used for segmented heating and curing, solvent can be fully volatilized, exhaust is promoted while thermosetting resin is cured, the probability of sealing gas in the thermosetting resin is reduced, the porosity is reduced, the density is improved, the time and the times of subsequent densification are reduced, the thermosetting resin, reinforcing materials and carbon ropes are fully cured and crosslinked, the interlayer bonding force is improved, and the mechanical property of the carbon-carbon cylindrical column is improved.
3. The application preferably carries out oxidation treatment on the chopped carbon fiber and the carbon rope, and the strong oxidizing solution can etch the surfaces of the inert chopped carbon fiber and the carbon rope to increase oxygen active functional groups such as hydroxyl, carboxyl and the like; and the surface roughness of the chopped carbon fiber and the carbon rope is increased, so that the interlayer binding force among the chopped carbon fiber, the carbon rope and the thermosetting resin is improved, a stronger anchoring effect is shown, and finally the mechanical property of the carbon-carbon cylindrical column is improved.
Drawings
Fig. 1 is a schematic structural view of example 1 of a molding die in the present application.
Fig. 2 is a schematic view of an exploded structure of example 1 of the molding die in the present application.
Fig. 3 is a schematic view of an exploded structure of example 2 of the molding die in the present application.
Reference numerals illustrate: 1. a cylinder; 101. an upper arc plate; 102. a lower arc plate; 2. a left sealing plate; 3. a right sealing plate; 4. a left cover; 5. a right cover; 6. a feeding plug; 7. an exhaust plug; 8. threading the rope hole; 9. a feed hole; 10. an exhaust hole; 11. a left seal groove; 12. a left seal ring; 13. a right seal groove; 14. a right seal ring; 15. a limit groove; 16. a lining rod; 17. and a connection hole.
Detailed Description
The present application is described in further detail below in conjunction with figures 1-3 and the examples.
Examples
Example 1
A preparation method of a carbon cylinder column comprises the following steps:
s1, uniformly mixing and stirring 10kg of graphite powder, 50kg of chopped carbon fibers and 40kg of thermosetting resin to obtain a compression injection material, wherein the expansion degree of the graphite powder is less than 0.0006 times, the particle size is less than or equal to 30 mu m, the chopped carbon fibers are prepared by cutting 12K carbon fiber multifilament, the length is 10-60mm, the thermosetting resin is water-soluble thermosetting phenolic resin, the solid content is more than or equal to 80%, and the viscosity at 25 ℃ is less than or equal to 600 mPa.s;
s2, fixing a plurality of carbon ropes in a forming die at intervals, wherein the carbon ropes are prepared from 3-5 strands of 12K carbon fiber multifilament, the minimum tensile load of the carbon ropes is more than 400N, the carbon ropes are arranged along the axial direction of the forming die, the injection molding material is injected into the inner cavity of the forming die from a feeding hole below the forming die in a pressurizing way, air is discharged from an exhaust hole at the top of the forming die, the pressure during the injection molding is 0.6MPa, and the injection molding speed is 4m 3 After the injection is completed, the feeding hole is closed, and the exhaust hole is kept in an open state;
s3, heating the forming die, heating to 160 ℃ at a heating rate of 10 ℃/min, keeping the temperature for 2 hours, solidifying the injection material and the carbon rope, and demolding to obtain a resin-based column;
s4, sequentially carrying out densification treatment and graphitization treatment on the resin-based column body, wherein the densification treatment comprises the following steps: the first densification is carried out, a resin-based column body is placed in a deposition furnace, propylene gas is introduced at the flow rate of 0.2L/min, the temperature is increased to 1000 ℃ at 40 ℃/h, the deposition is carried out for 600 hours at 1000 ℃, and the density is 0.9-1.2g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the Second densification, the density is 0.9-1.2g/cm 3 The resin-based column is placed in a furan resin impregnation tank, the solid content of furan resin is more than 90%, the furan resin is impregnated for 5 hours under the high pressure condition of 0.2MPa, the furan resin is placed in a curing oven after being taken out, the temperature is raised to 190 ℃ at the heating rate of 40 ℃/h, the resin is kept constant for 0.5 hour, the resin is cured, the resin is placed in a carbonization oven after being cured, the temperature is raised to 900 ℃ at the heating rate of 10 ℃/h, the temperature is kept constant for 3 hours, and the density is more than or equal to 1.6g/cm 3 Obtaining a carbonized column body; the graphitization treatment specifically comprises: heating the carbonization column to 2000 ℃ at a heating rate of 30 ℃/h, keeping the temperature for 20h, wherein the density is more than or equal to 1.55g/cm 3 Ash content is less than or equal to 200ppm; finally, the carbon cylinder column is obtained through mechanical processing.
Example 2
The difference from example 1 is that the pressure at the time of the pressure filling in S2 was 0.5MPa.
Example 3
The difference from example 1 is that the pressure at the time of the pressure filling in S2 was 0.3MPa.
Example 4
The difference from example 1 is that the pressure at the time of the pressure filling in S2 was 0.1MPa.
Example 5
The difference from example 1 is that the pressure at the time of the pressure filling in S2 was 0.05MPa.
Example 6
The difference from example 3 is that the injection speed at the time of pressure injection in S2 was 3m 3 /h。
Example 7
The difference from example 3 is that the injection speed at the time of pressure injection in S2 was 2m 3 /h。
Example 8
The difference from example 3 is that the injection speed at the time of pressure injection in S2 was 1m 3 /h。
Example 9
The difference from example 3 is that the injection speed at the time of pressure injection in S2 was 0.5m 3 /h。
Example 10
The difference from example 7 is that S3 is specifically: the temperature of the forming die is raised,
s31, heating the forming die to 70 ℃ at a heating rate of 8 ℃/min, and keeping the temperature for 40min;
s32, heating the forming die to 110 ℃ at a heating rate of 4 ℃/min, and keeping the temperature for 20min;
s33, heating the forming die to 150 ℃ at a heating rate of 8 ℃/min, keeping the temperature for 70min, solidifying the injection material and the carbon rope, and demolding to obtain the resin-based column.
Example 11
The difference from example 7 is that S3 is specifically: the temperature of the forming die is raised,
s31, heating the forming die to 80 ℃ at a heating rate of 10 ℃/min, and keeping the temperature for 30min;
s32, heating the forming die to 120 ℃ at a heating rate of 5 ℃/min, and keeping the temperature for 15min;
s33, heating the forming die to 165 ℃ at a heating rate of 10 ℃/min, keeping the temperature for 60min, solidifying the injection material and the carbon rope, and demolding to obtain the resin-based column.
Example 12
The difference from example 7 is that S3 is specifically: the temperature of the forming die is raised,
s31, heating the forming die to 90 ℃ at a heating rate of 12 ℃/min, and keeping the temperature for 20min;
s32, heating the forming die to 130 ℃ at a heating rate of 6 ℃/min, and keeping the temperature for 10min;
s33, heating the forming die to 180 ℃ at a heating rate of 12 ℃/min, keeping the temperature for 50min, solidifying the injection material and the carbon rope, and demolding to obtain the resin-based column.
Example 13
The difference from example 11 is that the preparation method of the chopped carbon fiber includes the following steps: soaking the carbon fiber multifilament in 1% nitric acid solution for 300min, taking out, washing with deionized water, drying at 90 deg.C, and cutting to obtain chopped carbon fiber with length of 10-60 mm.
Example 14
The difference from example 13 is that the carbon rope was subjected to surface activation treatment before being fixed on the molding die: soaking the carbon rope in a nitric acid solution with the mass fraction of 5% for 150min, taking out, cleaning with deionized water, and drying at 100 ℃ to obtain the surface activated carbon rope.
Example 15
The difference from example 14 is that the surface activated carbon rope is also subjected to a prepreg treatment: immersing the surface activated carbon rope in thermosetting resin for 30min, wherein the thermosetting resin is water-soluble thermosetting phenolic resin, the solid content is more than or equal to 80%, the viscosity is less than or equal to 600 mPa.s at 25 ℃, and taking out and drying the surface activated carbon rope to obtain the prepreg carbon rope.
Example 16
The difference from example 15 is that a method for preparing a carbon-carbon cylindrical column comprises the following steps:
s1, uniformly mixing and stirring 10kg of graphite powder, 50kg of chopped carbon fibers and 40kg of thermosetting resin to obtain a compression injection material, wherein the expansion degree of the graphite powder is less than 0.0006 times, the particle size is less than or equal to 30 mu m, the chopped carbon fibers are prepared by cutting 12K carbon fiber multifilament, the length is 10-60mm, the thermosetting resin is water-soluble thermosetting epoxy resin, the solid content is more than or equal to 80%, and the viscosity at 25 ℃ is less than or equal to 600 mPa.s; the preparation method of the chopped carbon fiber comprises the following steps: soaking the carbon fiber multifilament in a hydrogen peroxide solution with the mass fraction of 10% for 10min, taking out, cleaning with deionized water, drying at 80 ℃, and cutting to obtain chopped carbon fibers with the length of 10-60 mm;
s2, uniformly fixing a plurality of carbon ropes in a forming die at intervals, wherein the carbon ropes are prepared from 3-5 strands of 24K carbon fiber multifilament, the minimum tensile load of the carbon ropes is more than 400N, and the carbon ropes are arranged along the forming dieAxially arranging, namely pressurizing and injecting the injection material into the inner cavity of the forming die from a feeding hole below the forming die to discharge air from an exhaust hole at the top of the forming die, wherein the pressure during pressurizing and injecting is 0.6MPa, and the injection speed is 4m 3 After the injection is completed, the feeding hole is closed, and the exhaust hole is kept in an open state;
wherein, the carbon rope is subjected to surface activation treatment and presoaking treatment before being fixed on a forming die: soaking the carbon rope in a hydrogen peroxide solution with the mass fraction of 10% for 10min, taking out, cleaning with deionized water, and drying at 100 ℃ to obtain a surface activated carbon rope; dipping the surface activated carbon rope in thermosetting resin for 60min, wherein the thermosetting resin is water-soluble thermosetting phenolic resin, the solid content is more than or equal to 80%, the viscosity is less than or equal to 600 mPa.s at 25 ℃, taking out and drying to obtain the prepreg carbon rope;
s3, heating the forming die, S31, heating the forming die to 80 ℃ at a heating rate of 10 ℃/min, and keeping the temperature for 30min; s32, heating the forming die to 120 ℃ at a heating rate of 5 ℃/min, and keeping the temperature for 15min; s33, heating the forming die to 165 ℃ at a heating rate of 10 ℃/min, keeping the temperature for 60min, solidifying the injection material and the carbon rope, and demolding to obtain a resin-based column;
s4, sequentially carrying out densification treatment and graphitization treatment on the resin-based column body, wherein the densification treatment comprises the following steps: the first densification is carried out, a resin-based column body is placed in a deposition furnace, propylene gas is introduced at the flow rate of 0.2L/min, the temperature is increased to 1000 ℃ at 40 ℃/h, the deposition is carried out for 600h at 1000 ℃, and the density is more than or equal to 1.6g/cm 3 Obtaining a carbonized column body; the graphitization treatment specifically comprises: heating the carbonization column to 2000 ℃ at a heating rate of 30 ℃/h, keeping the temperature for 20h, wherein the density is more than or equal to 1.55g/cm 3 Ash content is less than or equal to 200ppm; finally, the carbon cylinder column is obtained through mechanical processing.
Comparative example
Comparative example 1
The preparation method of the carbon cylinder column comprises the following steps:
step 1: three-dimensional woven carbon fiber preform: (1) 300g/m 2 Carbon cloth and 40g/m 2 Is compounded with the net tyre to manufacture composite cloth for standby; (2) 70g/m 2 Laying the net tyre on a wood mould with EVA plate adhered on the surface for backing needling, and EVAThe thickness of the plate is controlled to be 11mm, and the needling density is controlled to be 25 needles/cm 2 The method comprises the steps of carrying out a first treatment on the surface of the (3) Spreading the prepared composite cloth on the surface of the net tire layer, and continuously needling for 2 times after spreading; (4) Winding carbon fiber wires on the surface of the needled composite cloth, wherein the distance between the fiber wires is 2cm, the above (1) - (4) are standard unit layers, and repeating the actions of net tire-composite cloth-wire winding on the unit layers until reaching the preset thickness of the preform;
step 2: curing the preform: placing a carbon fiber preform in an oven, placing a graphite mold at the inner side of the preform, reserving a gap of 4mm between the graphite mold and the preform, coating a prepared resin solution (the weight ratio of resin powder to alcohol is 1:2) on the outer surface of the preform, and then heating the oven to 200 ℃ for heat curing for 2 hours;
step 3: deposition densification: heating a deposition furnace to 1000 ℃ at 40 ℃/h, introducing precursor mixed gas (the volume ratio of natural gas to propane is 10:1) under the pressure of 10KPa, and depositing for 800 hours to finally prepare a carbon-carbon blank;
step 4: machining a blank, wherein the inner diameter remains 10mm, and the outer diameter is machined to be 5mm smaller than the size of a finished drawing;
step 5: and winding fiber yarns on the outer side of the machined carbon-carbon product, wherein the fiber yarn part is 1/3 of the volume of the whole product, a multi-tow synchronous spiral wet winding process is adopted, the winding angle is easy to control at 30 degrees, the winding tension is easy to control at 110N, and when the outer diameter of a winding piece is consistent with the outer diameter of a product drawing, the winding is finished:
step 6: winding the fiber filaments, densifying by impregnating, impregnating with asphalt, controlling the pressure of the impregnating at 2MPa and the temperature of 180 ℃, curing after impregnating, carbonizing, heating to 1000 ℃ at the heating rate of 10 ℃/h, maintaining the temperature for 3 hours, repeating the impregnating and carbonizing process for 4 times, wherein the density of the carbonized product is more than or equal to 1.6g/cm 3 The total time of soaking, carbonization and densification is 60 days; step 7: high-temperature graphitization treatment: placing the carbonized product meeting the density requirement in a high-temperature graphitization furnace, heating to 1900 ℃ under negative pressure, preserving heat for 3 hours, and then cooling;
step 8: and (5) machining to a size of a product meeting the drawing requirement, and obtaining the carbon cylinder column.
Comparative example 2
The difference from example 1 is that S2 is specifically: the injection material is injected into the inner cavity of the forming die from the feeding hole below the forming die in a pressurizing way, so that air is discharged from the exhaust hole at the top of the forming die, the pressure during the injection is 0.6MPa, and the injection speed is 4m 3 After the injection is completed, the feeding hole is closed, and the exhaust hole is kept in an open state;
s3, heating the forming die, heating to 160 ℃ at a heating rate of 10 ℃/min, keeping the temperature for 2 hours, solidifying the injection material, and demolding to obtain a resin-based column;
comparative example 3
The difference from example 1 is that 10kg of graphite powder and 50kg of chopped carbon fibers are replaced with 60kg of a water-soluble thermosetting phenol resin.
Performance test
Detection method
(1) The shear strength of the carbon-carbon cartridge columns of examples 1-16 and comparative examples 1-3 was tested according to the GB/T30969-2014 polymer matrix composite short beam shear strength test method, and the results are recorded in Table 1;
(2) Tensile strength of the carbon-carbon cartridge columns of examples 1 to 16 and comparative examples 1 to 3 was measured according to the GB/T33501-2017 tensile property test method, and the results are recorded in Table 1;
(3) According to GB/T40398.2-2021 carbon-carbon composite carbon material test method part 2: flexural performance test the flexural strength of the carbon-carbon cartridge columns of examples 1-16 and comparative examples 1-3 was measured and the results are recorded in Table 1.
TABLE 1 mechanical test results
| Examples/comparative example numbering | Shear Strength/MPa | Tensile Strength/MPa | Flexural Strength/MPa |
| Example 1 | 90.5 | 81.3 | 136.8 |
| Example 2 | 91.3 | 82.5 | 138.3 |
| Example 3 | 92.3 | 82.8 | 138.7 |
| Example 4 | 91.1 | 82.2 | 138.0 |
| Example 5 | 90.1 | 81.0 | 136.1 |
| Example 6 | 93.5 | 84.1 | 140.8 |
| Example 7 | 94.0 | 84.5 | 141.3 |
| Example 8 | 93.3 | 83.8 | 140.5 |
| Example 9 | 92.5 | 83.1 | 139.0 |
| Example 10 | 98.5 | 88.5 | 146.0 |
| Example 11 | 99.8 | 89.2 | 146.5 |
| Example 12 | 99.1 | 88.9 | 146.3 |
| Example 13 | 106.5 | 92.7 | 150.4 |
| Example 14 | 112.4 | 96.5 | 155.6 |
| Implementation of the |
117.8 | 100.0 | 160.5 |
| Example 16 | 115.6 | 98.7 | 158.1 |
| Comparative example 1 | 75.8 | 60.3 | 110.4 |
| Comparative example 2 | 71.5 | 55.6 | 104.7 |
| Comparative example 3 | 68.7 | 54.8 | 106.1 |
As can be seen from the combination of examples 1 to 16 and comparative examples 1 to 3 and the combination of table 1, comparative example 1 adopts a three-dimensional woven carbon fiber preform for 5 times densification, the total densification time is about 90 days, the efficiency is low, a large amount of leftover materials are wasted in machining, the target density can be achieved by performing densification for 2 times in example 1, the total densification time is about 30 days, the production efficiency of the carbon cylinder column is greatly improved, the carbon fiber leftover materials are greatly reduced, and the production cost is reduced; comparative example 2, which was a compression injection process but did not incorporate a carbon rope, resulted in lower shear strength, tensile strength and flexural strength than comparative example 1, indicating that the carbon rope was able to increase the shear strength, tensile strength and flexural strength of the carbon-carbon column; comparative example 3, which was a compression injection process but did not add reinforcing materials, resulted in lower shear strength, tensile strength and flexural strength than comparative example 1, indicating that the reinforcing materials were able to increase the shear strength, tensile strength and flexural strength of the carbon-carbon column; in the embodiment 1, the compression injection process is adopted, and the carbon ropes and the reinforcing materials are added at the same time, so that the shearing strength, the tensile strength and the bending strength are greatly improved, and the mechanical properties of the carbon drum column can be improved by compounding the carbon ropes, the reinforcing materials and the thermosetting resin.
Examples 2-5 sequentially reduce the pressure during the compression injection in S2, the shear strength, the tensile strength and the bending strength of examples 2-4 are improved, and the shear strength, the tensile strength and the bending strength of example 5 are reduced, wherein the mechanical properties of example 3 are the best, and the pressure during the compression injection in S2 is preferably 0.1-0.5MPa; examples 6 to 9 successively lower the injection speed during the pressure injection in S2, examples 6 to 8 have improved shear strength, tensile strength and flexural strength, and example 9 has slightly improved shear strength, tensile strength and flexural strength, wherein example 7 has the best mechanical properties, indicating that the injection speed during the pressure injection in S2 is preferably 1 to 3m 3 /h; the embodiment 10-12 changes the one-time heating and curing in the step S3 into three-stage heating and curing, and the shearing strength, the tensile strength and the bending strength of the embodiment 10-12 are greatly improved, wherein the mechanical property of the embodiment 11 is best, which means that the staged heating and curing can promote the exhaust, reduce the porosity, improve the density, improve the interlayer binding force and further improve the mechanical property of the carbon cylinder column; in the embodiment 13, the oxidation treatment is carried out on the carbon fiber multifilament, the shearing strength, the tensile strength and the bending strength are greatly improved, which shows that the oxidation treatment can improve the interlayer binding force between the chopped carbon fiber and the thermosetting resin, and further improve the mechanical property of the carbon cylinder column; example 14 greatly improves the shearing strength, the tensile strength and the bending strength of the carbon rope by oxidation treatment, which shows that the oxidation treatment can improve the interlayer binding force between the carbon rope and the thermosetting resin, thereby improving the mechanical property of the carbon-carbon cylindrical column; EXAMPLE 15 Pre-preg was performed after oxidation treatment of the carbon rope, and the shear strength, tensile strength and flexural strength were all greatThe improvement shows that the prepreg can improve the interlayer binding force between the carbon rope and the thermosetting resin, so as to improve the mechanical property of the carbon cylinder column; the target density can be achieved by 1 densification in example 16, the densification time can be further shortened, and the mechanical properties are better.
Example 1 of Forming die
Referring to fig. 1-2, in order to help a person skilled in the art better understand the present application, the present application further discloses a carbon cylinder column forming mold, which comprises a cylinder 1, a left sealing plate 2, a right sealing plate 3, a left sealing cover 4, a right sealing cover 5, a feeding plug 6 and an exhaust plug 7, wherein the cylinder 1, the left sealing plate 2, the right sealing plate 3, the left sealing cover 4, the right sealing cover 5, the feeding plug 6 and the exhaust plug 7 are all made of 316 stainless steel, the cylinder 1 comprises an upper arc-shaped plate 101 and a lower arc-shaped plate 102, the upper arc-shaped plate 101 and the lower arc-shaped plate 102 are surrounded to form a cylinder 1, the left sealing plate 2 and the right sealing plate 3 are circular plates, circular limiting grooves 15 are formed in the inner walls of two ends of the cylinder 1, the left sealing plate 2 is clamped in the limiting groove 15 of one end of the cylinder 1, and the right sealing plate 3 is clamped in the limiting groove 15 of the other end of the cylinder 1; a plurality of rope penetrating holes 8 are uniformly formed in the left sealing plate 2 and the right sealing plate 3, the rope penetrating holes 8 in the left sealing plate 2 and the right sealing plate 3 are symmetrically arranged, a feeding hole 9 is formed in one side, close to the left sealing plate 2, of the lower arc-shaped plate 102, an exhaust hole 10 is formed in one side, close to the right sealing plate 3, of the upper arc-shaped plate 101, the feeding hole 9 is located at the bottommost end, and the exhaust hole 10 is located at the topmost end, so that sufficient exhaust is facilitated; the outer wall at the two ends of the cylinder 1 is provided with external threads, the left sealing cover 4 and the right sealing cover 5 are provided with internal threads, the left sealing cover 4 and the right sealing cover 5 are in threaded connection with the cylinder 1, the left sealing plate 2 is positioned between the left sealing cover 4 and the cylinder 1, and the right sealing plate 3 is positioned between the right sealing cover 5 and the cylinder 1.
Referring to fig. 1-2, an annular left sealing groove 11 (not shown in the figure) is formed in the edge of one side, close to the left sealing cover 4, of the left sealing plate 2, and a left sealing ring 12 is elastically clamped in the left sealing groove 11; the edge of one side of the right sealing plate 3, which is close to the right sealing cover 5, is provided with a circular right sealing groove 13, and a right sealing ring 14 is elastically clamped in the right sealing groove 13; the left sealing ring 12 is used for sealing a gap between the left sealing plate 2 and the left sealing cover 4, the right sealing ring 14 is used for sealing a gap between the right sealing plate 3 and the right sealing cover 5, and the left sealing ring 12 and the right sealing ring 14 are made of silicon rubber or fluororubber.
Referring to fig. 1-2, in order to conveniently plug the feed hole 9 and the exhaust hole 10, the feed hole 9 is a threaded hole, the feed plug 6 is a bolt, and the feed plug 6 is in threaded connection with the feed hole 9; the exhaust hole 10 is a threaded hole, the exhaust plug 7 is a bolt, the exhaust plug 7 is in threaded connection with the exhaust hole 10, and the diameter of the feeding hole 9 is larger than that of the exhaust hole 10.
When the resin matrix column is required to be produced, the carbon ropes penetrate through the rope penetrating holes 8 of the left sealing plate 2 and the right sealing plate 3, one carbon rope can penetrate through the rope penetrating holes 8 of the left sealing plate 2 and the right sealing plate 3 in sequence, one carbon rope can be penetrated between the two rope penetrating holes 8, two ends of the carbon rope are knotted and fixed, then the upper arc plate 101 and the lower arc plate 102 are encircled to form the cylinder 1, two ends of the cylinder 1 are respectively clamped and fixed with the left sealing plate 2 and the right sealing plate 3, the left sealing cover 4 and the right sealing cover 5 are in threaded connection with the cylinder 1, a pressing injection material is injected into the cylinder 1 from a feed inlet, air is discharged from the air exhaust hole 10, after the injection material is finished, the feed hole 9 and the air exhaust hole 10 are blocked, the pressing injection material is solidified under heating or normal temperature, after solidification, the left sealing cover 4 and the right sealing cover 5 are firstly disassembled, the cylinder 1 is disassembled, the carbon rope is cut off from one side of the left sealing plate 2 and the right sealing plate 3, and the left cylinder 3 are disassembled, and the solid resin matrix column is obtained, and carbon is obtained after processing.
Example 2 of Forming die
Referring to fig. 3, the difference with embodiment 1 of the forming mold is that the forming mold further comprises a lining rod 16, the lining rod 16 is made of 316 stainless steel, the lining rod 16 can be a solid rod or a hollow rod, in this embodiment, the lining rod 16 is a hollow rod, the hollow rod is more material-saving and has light weight, the lining rod 16 is located inside the cylinder 1 and is coaxially arranged with the cylinder 1, threaded connecting holes 17 are formed in centers of opposite sides of the left sealing plate 2 and the right sealing plate 3, the connecting holes 17 are blind holes, external threads are formed at two ends of the lining rod 16, and the lining rod 16 is in threaded connection with the left sealing plate 2 and the right sealing plate 3.
When the cylindrical resin-based column is required to be produced, the two ends of the lining rod 16 are respectively in threaded connection with the left sealing plate 2 and the right sealing plate 3, and after the injection is solidified and molded, the hollow resin-based column can be obtained, and the carbon-carbon column can be obtained through processing.
The present embodiment is merely illustrative of the present application and is not intended to be limiting, and those skilled in the art, after having read the present specification, may make modifications to the present embodiment without creative contribution as required, but is protected by patent laws within the scope of the claims of the present application.
Claims (10)
1. A preparation method of a carbon cylinder column is characterized by comprising the following steps: the method comprises the following steps:
s1, uniformly mixing a reinforcing material and thermosetting resin to obtain a compression injection material;
s2, fixing a plurality of carbon ropes in a forming die at intervals, arranging the carbon ropes along the axial direction of the forming die, pressurizing and injecting a pressure injection material into an inner cavity of the forming die from a feeding hole below the forming die, discharging air from an exhaust hole at the top of the forming die, and sealing the feeding hole and keeping the exhaust hole in an open state after the pressure injection is finished;
s3, heating the forming die to solidify the injection material and the carbon rope, and demolding to obtain a resin-based column;
and S4, sequentially carrying out densification treatment and graphitization treatment on the resin-based column, and finally carrying out mechanical processing to obtain the carbon-carbon cylindrical column.
2. The method for preparing the carbon-carbon cylindrical column according to claim 1, wherein the method comprises the following steps: the pressure during pressurizing and injecting in the S2 is 0.1-0.5MPa.
3. The method for preparing the carbon-carbon cylindrical column according to claim 1, wherein the method comprises the following steps: and (2) the injection speed during the pressurizing injection in the step (S2) is 1-3 m/h.
4. The method for preparing the carbon-carbon cylindrical column according to claim 1, wherein the method comprises the following steps: in the step S3, heating the forming die specifically comprises:
s31, heating the forming die to 70-90 ℃ at a heating rate of 8-12 ℃/min, and keeping the temperature for 20-40min;
s32, heating the forming die to 110-130 ℃ at a heating rate of 4-6 ℃/min, and keeping the temperature for 10-20min;
s33, heating the forming die to 150-180 ℃ at a heating rate of 8-12 ℃/min, and keeping the temperature for 50-70min.
5. The method for preparing the carbon-carbon cylindrical column according to claim 1, wherein the method comprises the following steps: the reinforcing material in the S1 comprises carbon black powder and chopped carbon fibers, wherein the mass ratio of the carbon black powder to the chopped carbon fibers to the thermosetting resin is (1-2): 5-7): 1-4.
6. The method for preparing the carbon-carbon cylindrical column according to claim 5, wherein the method comprises the following steps: the preparation method of the chopped carbon fiber comprises the following steps: soaking the carbon fiber multifilament in a strong oxidizing solution with the mass fraction of 1% -10% for 10-300min, taking out, washing with water, drying, and cutting to obtain the chopped carbon fiber with the length of 10-60 mm.
7. The method for preparing the carbon-carbon cylindrical column according to claim 1, wherein the method comprises the following steps: the carbon rope is subjected to surface activation treatment before being fixed on a forming die: soaking the carbon rope in a strong oxidizing solution with the mass fraction of 1% -10% for 10-300min, taking out, washing with water, and drying to obtain the surface activated carbon rope.
8. The method for preparing the carbon-carbon cylindrical column according to claim 6 or 7, wherein: the strong oxidizing solution is nitric acid solution or hydrogen peroxide solution.
9. The method for preparing the carbon-carbon column according to claim 7, wherein: the surface activated carbon rope is also subjected to a pre-impregnation treatment: and (3) immersing the surface activated carbon rope in thermosetting resin for 30-60min, taking out and drying to obtain the pre-impregnated carbon rope.
10. The method for preparing the carbon-carbon cylindrical column according to claim 1 or 9, wherein: the thermosetting resin is water-soluble thermosetting phenolic resin or water-soluble thermosetting epoxy resin, the solid content is more than or equal to 80 percent, and the viscosity at 25 ℃ is less than or equal to 600 mPa.s.
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Address after: 710600 Factory Building 2, No. 2299 Qinwang Second Road, Weibei New City, Xi'an Economic and Technological Development Zone, Shaanxi Province Applicant after: Shaanxi Meilan New Materials Co.,Ltd. Applicant after: Xi'an Meilan New Material Co.,Ltd. Address before: No. 56, Qinwang Second Road, Lintong District, Xi'an, Shaanxi 710600 Applicant before: SHAANXI MEILANDO CARBON CO.,LTD. Applicant before: Xi'an Meilan New Material Co.,Ltd. |
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