CN117923939A - Method for preparing carbon ceramic brake disc by combining porous carbon/carbon blank with RMI - Google Patents
Method for preparing carbon ceramic brake disc by combining porous carbon/carbon blank with RMI Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 178
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 170
- 238000000034 method Methods 0.000 title claims abstract description 48
- 239000000919 ceramic Substances 0.000 title claims abstract description 47
- 229920005989 resin Polymers 0.000 claims abstract description 42
- 239000011347 resin Substances 0.000 claims abstract description 42
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 30
- 238000006243 chemical reaction Methods 0.000 claims abstract description 21
- 239000003054 catalyst Substances 0.000 claims abstract description 19
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000005336 cracking Methods 0.000 claims abstract description 17
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 16
- 239000004917 carbon fiber Substances 0.000 claims abstract description 16
- 238000000626 liquid-phase infiltration Methods 0.000 claims abstract description 14
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000003960 organic solvent Substances 0.000 claims abstract description 11
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 238000012545 processing Methods 0.000 claims abstract description 3
- 238000000498 ball milling Methods 0.000 claims description 20
- 239000000463 material Substances 0.000 claims description 17
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 16
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical group C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims description 16
- 238000005470 impregnation Methods 0.000 claims description 16
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 15
- 229920001568 phenolic resin Polymers 0.000 claims description 15
- 239000005011 phenolic resin Substances 0.000 claims description 15
- 239000011863 silicon-based powder Substances 0.000 claims description 14
- 239000002243 precursor Substances 0.000 claims description 11
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 10
- HYBBIBNJHNGZAN-UHFFFAOYSA-N furfural Chemical compound O=CC1=CC=CO1 HYBBIBNJHNGZAN-UHFFFAOYSA-N 0.000 claims description 8
- 235000010299 hexamethylene tetramine Nutrition 0.000 claims description 8
- 239000004312 hexamethylene tetramine Substances 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- XWHPIFXRKKHEKR-UHFFFAOYSA-N iron silicon Chemical compound [Si].[Fe] XWHPIFXRKKHEKR-UHFFFAOYSA-N 0.000 claims description 7
- 238000007598 dipping method Methods 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 6
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- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 2
- 229920000647 polyepoxide Polymers 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 abstract description 14
- 238000005087 graphitization Methods 0.000 abstract description 13
- 230000009286 beneficial effect Effects 0.000 abstract description 10
- 239000011521 glass Substances 0.000 abstract description 9
- 230000001737 promoting effect Effects 0.000 abstract description 2
- 238000001723 curing Methods 0.000 description 33
- 239000011148 porous material Substances 0.000 description 11
- 238000009826 distribution Methods 0.000 description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 8
- 238000001816 cooling Methods 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 239000002904 solvent Substances 0.000 description 7
- 238000005475 siliconizing Methods 0.000 description 5
- 239000004677 Nylon Substances 0.000 description 4
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- 229910052757 nitrogen Inorganic materials 0.000 description 4
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 4
- 229910010271 silicon carbide Inorganic materials 0.000 description 4
- 238000002791 soaking Methods 0.000 description 4
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- 238000001878 scanning electron micrograph Methods 0.000 description 2
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- 229910001018 Cast iron Inorganic materials 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 239000002419 bulk glass Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
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- 239000003153 chemical reaction reagent Substances 0.000 description 1
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- 239000011856 silicon-based particle Substances 0.000 description 1
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Abstract
The invention discloses a method for preparing a carbon ceramic brake disc by combining porous carbon/carbon blank with RMI, which comprises the following steps: mixing resin, an organic solvent, a curing agent, a catalyst and/or a pore-forming agent to prepare a resin-based solution; immersing the carbon fiber three-dimensional needling preform in a resin-based solution, and then curing and cracking to obtain a porous carbon/carbon blank; finally, after mechanical processing, ceramic is carried out by a reaction melt infiltration method, and the ceramic is prepared. The preparation method has the advantages of simple preparation process, short period and low cost, and the problems of high carbon residue rate, poor mechanical property, low graphitization degree, poor uniformity and the like of the carbon ceramic brake disc in the preparation process are solved by adding the nickel source catalyst in the PIP process, catalyzing the large glass generated by high-temperature cracking of the organic resin to be converted into carbon with higher graphitization degree, promoting the glass carbon to be converted into a porous carbon structure by adding the pore-forming agent, and being more beneficial to the subsequent RMI.
Description
Technical Field
The invention relates to the technical field of brake materials, in particular to a method for preparing a carbon ceramic brake disc by combining porous carbon/carbon blank with RMI.
Background
Brake materials have undergone development from cast iron, composite materials, powder metallurgy materials to carbon/carbon composites and carbon/ceramic composites. The carbon/silicon carbide ceramic matrix composite is a high-performance brake material developed in recent years after powder metallurgy materials and carbon/carbon composite materials, adopts pyrolytic carbon, silicon carbide and the like as matrixes, adopts high-strength carbon fiber as a reinforcing body and adopts a hard ceramic material silicon carbide as a matrix on the basis of the carbon/carbon composite materials, thereby realizing the characteristics of low density, high temperature resistance, high strength, stable friction performance, small abrasion loss, large brake ratio and long service life, meeting the brake requirements in a plurality of fields of airplanes, high-speed rails, civil vehicles and the like, and having wide application prospect.
The existing preparation methods of the carbon/silicon carbide composite brake material mainly comprise a chemical vapor infiltration method (CVI), a precursor impregnation cracking method (PIP), a reaction melt infiltration method (RMI) and the like. The Chemical Vapor Infiltration (CVI) method has the advantages of less damage to the carbon fiber, uniform matrix and good mechanical property, but has long preparation period and high cost; the precursor impregnation cracking method (PIP) has the advantages of simple process, short preparation period, large porosity and large volume deformation; the Reactive Melt Infiltration (RMI) method has the advantages of simple operation, short implementation period, low cost, high density and capability of preparing components with complex shapes, but meanwhile, the siliconizing uniformity is difficult to control, part of silicon can remain after the reaction, and the silicon reacts with carbon fibers to reduce the strength of the carbon fibers, thereby affecting the performance of the material. The method has certain limitations, and a single method is difficult to meet the use requirement of the severe service environment of the brake material and is also difficult to meet the requirement of industrial production.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a method for preparing a carbon ceramic brake disc by combining a porous carbon/carbon blank body with RMI, so as to solve the problems of high carbon residue rate, poor mechanical property, uneven structure and the like in the preparation process of the existing carbon ceramic brake disc material.
The technical scheme for solving the technical problems is as follows:
A method for preparing a carbon ceramic brake disc by combining porous carbon/carbon blank with RMI comprises the following steps:
(1) Mixing resin, an organic solvent, a curing agent, a catalyst and/or a pore-forming agent to prepare a resin-based solution;
(2) Immersing the carbon fiber three-dimensional needling preform into the resin-based solution prepared in the step (1), and then solidifying and cracking to prepare a porous carbon/carbon blank;
(3) And (3) mechanically processing the porous carbon/carbon blank obtained in the step (2), and then performing ceramization through a reaction melt infiltration method to obtain the porous carbon/carbon blank.
The beneficial effects of the invention are as follows: in the process of precursor impregnation cracking (PIP), the invention converts bulk glass carbon into carbon with higher graphitization degree in small blocks through the actions of organic resin cracking and nickel source catalyst introduction, and the pore-forming agent is added to promote the glass carbon to be in a porous carbon structure, which is more beneficial to the subsequent Reaction Melt Impregnation (RMI) process, so as to solve the problems of low graphitization degree, poor uniformity and the like in the preparation process of the carbon ceramic brake disc.
Further, in the step (1), the mass ratio of the resin to the organic solvent is 5-70:30-95; the addition amount of the curing agent is 5-15% of the mass of the resin; the addition amount of the catalyst is 1-5% of the mass of the resin; the addition amount of the pore-forming agent is 1-5% of the mass of the resin.
Further, the resin is phenolic resin or epoxy resin; the organic solvent is ethanol, furfural or glycol; the catalyst is a nickel source catalyst; the pore-forming agent is ferric salt; the curing agent is hexamethylenetetramine.
The beneficial effects of adopting the further technical scheme are as follows: according to the invention, the nickel source catalyst is added into the preparation process of the resin-based solution, so that the large glass carbon blocks after high-temperature cracking of the organic resin can be effectively catalyzed to be converted into carbon blocks with higher graphitization degree; meanwhile, the ferric salt pore-forming agent is also beneficial to promoting the large glass carbon generated after the high-temperature cracking of the organic resin to be converted into a porous carbon structure, and is beneficial to the subsequent Reaction Melt Infiltration (RMI) process.
Further, the mixing conditions are: firstly, placing the catalyst and/or pore-forming agent into an organic solvent, carrying out ultrasonic treatment until the catalyst and/or pore-forming agent are completely dissolved, then sequentially adding resin and curing agent, and carrying out ball milling.
Further, the ball milling conditions are as follows: ball-to-material ratio 3-10:1, the ball milling speed is 50-300r/min, and the time is 2-12h.
Preferably, the ball milling conditions are: ball-to-material ratio 3:1, the ball milling speed is 50r/min, and the time is 12h.
The beneficial effects of adopting the further technical scheme are as follows: according to the invention, the introduced catalyst and/or pore-forming agent are ultrasonically dissolved in the organic solvent, and then the resin and the curing agent are added, so that the dispersion efficiency and the dispersion effect of the catalyst and/or pore-forming agent in the organic solvent can be greatly improved, the preparation time of the resin-based solution is shortened, and the uniformity of the resin-based solution is improved.
Further, the conditions of the impregnation in the step (2) are as follows: the dipping temperature is 30-80 ℃, the vacuum dipping time is 0.5-5h, and then the pressure dipping is 0.5-1h.
Preferably, the conditions of the impregnation in step (2) are: the impregnation temperature is 55 ℃, the vacuum impregnation is carried out for 30min, then the pressure impregnation is carried out for 30min, and the air pressure of the pressure impregnation is 8kPa.
Further, the curing temperature in the step (2) is 60-150 ℃ and the curing time is 4-8h.
Further, the curing condition in the step (2) is that the curing is performed for 0.5 to 1.5 hours at the temperature of between 60 and 90 ℃, then for 0.5 to 1.5 hours at the temperature of between 100 and 120 ℃ and finally for 2 to 5 hours at the temperature of between 130 and 150 ℃.
Preferably, the curing conditions in step (2) are curing for 1 hour at 80 ℃, then for 1 hour at 100 ℃ and finally for 4 hours at 150 ℃.
The beneficial effects of adopting the further technical scheme are as follows: according to the three-section curing method, the impregnated carbon fiber three-dimensional needled preform can be cured more thoroughly, and the phenomenon of uneven curing of partial areas is avoided.
Further, the temperature of the cleavage in the step (2) is 800-1200 ℃.
Further, the reaction precursor of the reaction melt infiltration method in the step (3) is at least one of silicon powder and iron-silicon powder, the temperature is 1500-1800 ℃ and the time is 2-6h.
Preferably, the reaction precursor of the reaction melt infiltration method in the step (3) is mixed powder composed of silicon powder and iron silicon powder, and the temperature is 1600 ℃ and the time is 4 hours.
The invention has the following beneficial effects:
(1) According to the invention, a carbon ceramic brake disc is prepared by combining a precursor impregnation cracking method (PIP) and a reactive melt infiltration method (RMI), a nickel source catalyst is added in a PIP process, and large glass carbon generated after high-temperature cracking of catalytic organic resin is converted into carbon with higher graphitization degree, and a pore-forming agent is added to promote the glass carbon to be converted into a porous carbon structure, so that the preparation method is more beneficial to the subsequent RMI, and the problems of high carbon residue rate, poor mechanical property, low graphitization degree, poor uniformity and the like of the carbon ceramic brake disc in the preparation process are solved.
(2) Compared with a pure CVI process, the PIP process has the advantages that the preparation process is simpler, the period is shorter, and the cost is lower.
Drawings
FIG. 1 is an SEM micrograph of a carbon/carbon blank of comparative example 1;
FIG. 2 is an SEM micro-topography of a carbon ceramic brake disc made in accordance with comparative example 1;
FIG. 3 is a graph showing pore size distribution of the carbon/carbon green body produced in comparative example 1;
FIG. 4 is an SEM micrograph of a carbon/carbon blank of example 3;
FIG. 5 is an SEM micro-topography of a carbon ceramic brake disc prepared in example 3;
FIG. 6 is a graph showing pore size distribution of the carbon/carbon green body obtained in example 3.
Detailed Description
The principles and features of the present invention are described below with reference to the drawings, the examples are illustrated for the purpose of illustrating the invention and are not to be construed as limiting the scope of the invention. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
Example 1:
A method for preparing a carbon ceramic brake disc by combining porous carbon/carbon blank with RMI comprises the following steps:
(1) Weighing the following components in percentage by mass: 50 a phenolic resin and a furfural solvent, wherein the mass fraction of the phenolic resin is 2% of Ni (NO 3)2·6H2 O and the mass fraction of the phenolic resin is 10% of hexamethylenetetramine;
(2) Placing Ni (NO 3)2·6H2 O in a furfural solvent, performing ultrasonic treatment until the Ni (NO 3)2·6H2 O is completely dissolved, and then sequentially adding phenolic resin and hexamethylenetetramine;
(3) Placing the sizing agent prepared in the step (2) into a nylon ball milling tank, wherein the ball-to-material ratio is 3:1, the mass ratio of the large ball to the medium ball is 1:1:1, ball milling is carried out on a horizontal ball mill, the ball milling rotating speed is 50r/min, and the time is 12h, so as to prepare resin-based solution;
(4) Soaking the three-dimensional needled carbon fiber preform in clear water, ultrasonically cleaning for 1h, and drying in a blast oven at 80 ℃ for 12h;
(5) Placing the three-dimensional needled carbon fiber preform dried in the step (4) into a vacuum impregnation tank added with the resin-based solution prepared in the step (3), heating the resin-based solution to 55 ℃ in a water bath, vacuum impregnating for 30min, then introducing nitrogen, and maintaining the pressure for 30min after the air pressure reaches 8 kPa;
(6) Taking out the immersed preform in the step (5) for curing, curing for 1h at 80 ℃, curing for 1h at 100 ℃, and curing for 4h at 150 ℃ to finish curing;
(7) Cracking the preform obtained after solidification in the step (6) in a high-temperature furnace at 1000 ℃, and then cooling along with the furnace to obtain a carbon/carbon blank;
(8) After the density of the carbon/carbon blank reaches 1.3g/cm 3, machining to obtain the carbon/carbon brake disc;
(9) And (3) taking silicon powder and iron silicon powder as reaction precursors, adopting a reaction melt infiltration method to carry out ceramic treatment on the carbon/carbon brake disc obtained in the step (8), carrying out siliconizing at 1600 ℃, carrying out ceramic treatment for 4 hours, and then cooling along with a furnace to obtain the carbon ceramic brake disc.
Example 2:
A method for preparing a carbon ceramic brake disc by combining porous carbon/carbon blank with RMI comprises the following steps:
(1) Weighing the following components in percentage by mass: 80, wherein the mass fraction of the phenolic resin is 2% of FeCl 2·4H2 O of the phenolic resin, and the mass fraction of the ethylene glycol solvent is 10% of hexamethylenetetramine of the phenolic resin;
(2) Placing FeCl 2·4H2 O in an ethylene glycol solvent, performing ultrasonic treatment until Ni (NO 3)2·6H2 O is completely dissolved, and then sequentially adding phenolic resin and hexamethylenetetramine;
(3) Placing the sizing agent prepared in the step (2) into a nylon ball milling tank, wherein the ball-to-material ratio is 3:1, the mass ratio of the large ball to the medium ball is 1:1:1, ball milling is carried out on a horizontal ball mill, the ball milling rotating speed is 50r/min, and the time is 12h, so as to prepare resin-based solution;
(4) Soaking the three-dimensional needled carbon fiber preform in clear water, ultrasonically cleaning for 1h, and drying in a blast oven at 80 ℃ for 12h;
(5) Placing the three-dimensional needled carbon fiber preform dried in the step (4) into a vacuum impregnation tank added with the resin-based solution prepared in the step (3), heating the resin-based solution to 55 ℃ in a water bath, vacuum impregnating for 1h, then introducing nitrogen, and maintaining the pressure for 1h after the air pressure reaches 8 kPa;
(6) Taking out the immersed preform in the step (5) for curing, curing for 1h at 80 ℃, curing for 1h at 120 ℃, and curing for 2h at 150 ℃ to finish curing;
(7) Cracking the preform obtained after solidification in the step (6) in a high-temperature furnace at 1200 ℃, and then cooling along with the furnace to obtain a carbon/carbon blank;
(8) After the density of the carbon/carbon blank reaches 1.3g/cm 3, machining to obtain the carbon/carbon brake disc;
(9) And (3) taking silicon powder and iron silicon powder as reaction precursors, adopting a reaction melt infiltration method to carry out ceramic treatment on the carbon/carbon brake disc obtained in the step (8), carrying out siliconizing at 1600 ℃, carrying out ceramic treatment for 4 hours, and then cooling along with a furnace to obtain the carbon ceramic brake disc.
Example 3:
A method for preparing a carbon ceramic brake disc by combining porous carbon/carbon blank with RMI comprises the following steps:
(1) Weighing the following components in percentage by mass: 80 of phenolic resin and ethylene glycol solvent, wherein the mass fraction of the phenolic resin is 1% of Ni (NO 3)2·6H2 O, the mass fraction of the phenolic resin is 3% of FeCl 2·4H2 O and the mass fraction of the phenolic resin is 10% of hexamethylenetetramine;
(2) Placing Ni (NO 3)2·6H2 O and FeCl 2·4H2 O in an ethylene glycol solvent, performing ultrasonic treatment until the Ni (NO 3)2·6H2 O is completely dissolved, and then sequentially adding phenolic resin and hexamethylenetetramine;
(3) Placing the sizing agent prepared in the step (2) into a nylon ball milling tank, wherein the ball-to-material ratio is 3:1, the mass ratio of the large ball to the medium ball is 1:1:1, ball milling is carried out on a horizontal ball mill, the ball milling rotating speed is 50r/min, and the time is 12h, so as to prepare resin-based solution;
(4) Soaking the three-dimensional needled carbon fiber preform in clear water, ultrasonically cleaning for 1h, and drying in a blast oven at 80 ℃ for 12h;
(5) Placing the three-dimensional needled carbon fiber preform dried in the step (4) into a vacuum impregnation tank added with the resin-based solution prepared in the step (3), heating the resin-based solution to 55 ℃ in a water bath, vacuum impregnating for 30min, then introducing nitrogen, and maintaining the pressure for 30min after the air pressure reaches 8 kPa;
(6) Taking out the immersed preform in the step (5) for curing, curing for 1h at 80 ℃, curing for 1h at 100 ℃, and curing for 4h at 150 ℃ to finish curing;
(7) Cracking the preform obtained after solidification in the step (6) in a high-temperature furnace at 1200 ℃, and then cooling along with the furnace to obtain a carbon/carbon blank;
(8) After the density of the carbon/carbon blank reaches 1.3g/cm 3, machining to obtain the carbon/carbon brake disc;
(9) And (3) taking silicon powder and iron silicon powder as reaction precursors, adopting a reaction melt infiltration method to carry out ceramic treatment on the carbon/carbon brake disc obtained in the step (8), carrying out siliconizing at 1600 ℃, carrying out ceramic treatment for 4 hours, and then cooling along with a furnace to obtain the carbon ceramic brake disc.
Comparative example 1
A method of making a carbon ceramic brake disc comprising the steps of:
(1) Weighing the following components in percentage by mass: 80 and absolute ethanol solvent, and placing the mixture in a nylon ball milling tank, wherein the ball-to-material ratio is 3:1, the mass ratio of the large ball to the medium ball is 1:1:1, ball milling is carried out on a horizontal ball mill, the ball milling rotating speed is 50r/min, and the time is 12h, so as to prepare resin-based solution;
(2) Soaking the three-dimensional needled carbon fiber preform in clear water, ultrasonically cleaning for 1h, and drying in a blast oven at 80 ℃ for 12h;
(3) Placing the three-dimensional needled carbon fiber preform dried in the step (2) into a vacuum impregnation tank added with the resin-based solution prepared in the step (1), heating the resin-based solution to 55 ℃ in a water bath, vacuum impregnating for 30min, then introducing nitrogen, and maintaining the pressure for 30min after the air pressure reaches 8 kPa;
(4) Taking out the immersed preform in the step (3) for curing, curing for 1h at 80 ℃, curing for 1h at 100 ℃, and curing for 4h at 150 ℃ to finish curing;
(5) Cracking the preform obtained after solidification in the step (4) in a high-temperature furnace at 1200 ℃, and then cooling along with the furnace to obtain a carbon/carbon blank;
(6) After the density of the carbon/carbon blank reaches 1.3g/cm 3, machining to obtain the carbon/carbon brake disc;
(7) And (3) taking silicon powder and iron silicon powder as reaction precursors, adopting a reaction melt infiltration method to carry out ceramic treatment on the carbon/carbon brake disc obtained in the step (8), carrying out siliconizing at 1600 ℃, carrying out ceramic treatment for 4 hours, and then cooling along with a furnace to obtain the carbon ceramic brake disc.
Test example:
The carbon/carbon green body and the carbon ceramic brake disc prepared in example 3 and comparative example 1 were subjected to experiments, the surface microscopic morphology thereof was observed by a scanning electron microscope, and the pore size distribution diagram was drawn, and the graphitization degree of the carbon/carbon green body was measured by an X-ray diffractometer.
The experimental results are shown in FIGS. 1-6 and Table 1.
TABLE 1 graphitization degree of carbon/carbon bodies
| Sample preparation | 2θ | Spacing d of graphite layers 002 | Degree of graphitization G |
| Example 3 | 26.280 | 0.33884 | 60％ |
| Comparative example 1 | 26.009 | 0.34230 | 19.8％ |
The microscopic morphologies of the carbon/carbon blank body and the carbon ceramic brake disc manufactured in the comparative example 1 are respectively shown in fig. 1 and 2, and as can be seen from the figures, large glass carbon blocks are distributed among the carbon/carbon blank body fibers, the distribution is extremely uneven, silicon particles can be adhered to the surface of a material and are subject to segregation, the structure is uneven in the microscopic morphology of the carbon ceramic brake disc, and as can be seen from the figure, the figure 3 is a pore diameter distribution diagram of the carbon/carbon blank body manufactured in the comparative example 1, the nanoscale peaks represent the pore diameters in the blank body, the distribution is mainly between 3 and 100 mu m, the median pore diameter is 38 mu m, and the pore diameter distribution is uneven; from the data in table 1 above, the graphitization degree is also relatively low, which is only 19.8%, which directly affects the subsequent ceramization process and the performance of the manufactured carbon ceramic brake disc.
The microscopic morphologies of the carbon/carbon blank and the carbon ceramic brake disc prepared in example 3 are shown in fig. 4 and 5, respectively, and it can be seen from the graph that the large glass carbon among the carbon/carbon blank fibers is converted into carbon with higher graphitization degree of small blocks, and the carbon is uniformly distributed among the fibers; the microscopic morphology of the carbon ceramic brake disc can also be seen that the whole structure is relatively uniform, and the phenomena of segregation and free silicon adhesion are avoided; as can be seen from table 1 above, the graphitization degree of the carbon/carbon green body prepared in example 3 was 60%; according to the pore size distribution of the carbon/carbon green body shown in fig. 6, the nano-scale peaks represent the pore sizes in the green body, which are mainly distributed between 10 and 30nm, the median pore size is 19nm, and the pore size distribution is uniform, so that the porous carbon/carbon green body is formed.
The foregoing description of the preferred embodiments of the invention is not intended to limit the invention to the precise form disclosed, and any such modifications, equivalents, and alternatives falling within the spirit and scope of the invention are intended to be included within the scope of the invention.
Claims (10)
1. A method for preparing a carbon ceramic brake disc by combining porous carbon/carbon blank with RMI, which is characterized by comprising the following steps:
(1) Mixing resin, an organic solvent, a curing agent, a catalyst and/or a pore-forming agent to prepare a resin-based solution;
(2) Immersing the carbon fiber three-dimensional needling preform into the resin-based solution prepared in the step (1), and then solidifying and cracking to prepare a porous carbon/carbon blank;
(3) And (3) mechanically processing the porous carbon/carbon blank obtained in the step (2), and then performing ceramization through a reaction melt infiltration method to obtain the porous carbon/carbon blank.
2. The method for manufacturing a carbon ceramic brake disc by combining a porous carbon/carbon blank with RMI according to claim 1, wherein the mass ratio of the resin to the organic solvent in the step (1) is 5-70:30-95; the addition amount of the curing agent is 5-15% of the mass of the resin; the addition amount of the catalyst is 1-5% of the mass of the resin; the addition amount of the pore-forming agent is 1-5% of the mass of the resin.
3. The method of preparing a carbon ceramic brake disc by combining a porous carbon/carbon blank with RMI according to claim 1 or 2, wherein the resin is a phenolic resin or an epoxy resin; the organic solvent is ethanol, furfural or glycol; the catalyst is a nickel source catalyst; the pore-forming agent is ferric salt; the curing agent is hexamethylenetetramine.
4. The method of preparing a carbon ceramic brake disc with RMI in combination with porous carbon/carbon green body of claim 1, wherein the mixing conditions are: firstly, placing the catalyst and/or pore-forming agent into an organic solvent, carrying out ultrasonic treatment until the catalyst and/or pore-forming agent are completely dissolved, then sequentially adding resin and curing agent, and carrying out ball milling.
5. The method for preparing a carbon ceramic brake disc by combining a porous carbon/carbon blank with RMI according to claim 4, wherein the ball milling conditions are as follows: ball-to-material ratio 3-10:1, the ball milling speed is 50-300r/min, and the time is 2-12h.
6. The method for manufacturing a carbon ceramic brake disc by combining a porous carbon/carbon blank with RMI according to claim 1, wherein the conditions of the impregnation in the step (2) are: the dipping temperature is 30-80 ℃, the vacuum dipping time is 0.5-5h, and then the pressure dipping is 0.5-1h.
7. The method for manufacturing a carbon ceramic brake disc by combining a porous carbon/carbon blank with RMI according to claim 1, wherein the curing temperature in the step (2) is 60-150 ℃ for 4-8 hours.
8. The method for manufacturing a carbon ceramic brake disc by combining a porous carbon/carbon blank with RMI according to claim 1, wherein the cracking temperature in the step (2) is 800-1200 ℃.
9. The method for manufacturing a carbon ceramic brake disc by combining a porous carbon/carbon blank with RMI according to claim 1, wherein the reaction precursor of the reaction melt infiltration method in the step (3) is at least one of silicon powder and iron-silicon powder, and the temperature is 1500-1800 ℃ for 2-6 hours.
10. A carbon ceramic brake disc produced by the method of any one of claims 1 to 9.
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