CN110483086B - Preparation method of carbon-ceramic brake disc - Google Patents

Preparation method of carbon-ceramic brake disc Download PDF

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CN110483086B
CN110483086B CN201910803674.8A CN201910803674A CN110483086B CN 110483086 B CN110483086 B CN 110483086B CN 201910803674 A CN201910803674 A CN 201910803674A CN 110483086 B CN110483086 B CN 110483086B
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brake disc
carbon
parts
preparing
ceramic brake
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CN110483086A (en
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刘汝强
杨川
李宗乐
何留阳
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Shandong Stopart Brake Materials Co ltd
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Shandong Stopart Brake Materials Co ltd
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    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16DCOUPLINGS FOR TRANSMITTING ROTATION; CLUTCHES; BRAKES
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Abstract

The invention relates to a preparation method of a carbon-ceramic brake disc, which comprises the following specific processes: preparing a carbon fiber preform; carrying out chemical vapor deposition on the prefabricated body to prepare a C/C composite material; processing the C/C composite material into unit modules; preparing a C/C brake disc by bonding; the method can improve the material utilization rate, avoid the waste and the loss of materials for processing the carbon/ceramic brake disc, and shorten the processing time, thereby greatly reducing the production cost of the carbon/ceramic brake disc.

Description

Preparation method of carbon-ceramic brake disc
Technical Field
The invention relates to a preparation method of a carbon fiber toughened ceramic-based (carbon ceramic for short) brake disc, in particular to a preparation method of a carbon fiber toughened SiC-based brake disc, and belongs to the field of carbon ceramic composite material braking.
Background
Carbon fiber toughened SiC base (C)fthe/SiC) friction material has the advantages of low density, abrasion resistance, high friction coefficient, no heat fading and the like. C compared with the traditional metal or semi-metal friction materialfthe/SiC has the advantages of low density, high temperature resistance, small abrasion, stable friction performance, excellent oxidation resistance, insensitivity of the friction performance to external environments (oil stain, moisture, seawater and the like) and the like. At present, Cfthe/SiC is the key point of light-weight, high-braking-efficiency and full-environment service friction materialThe research direction is recognized as the latest generation of brake materials.
Patent No. CN109095929A discloses a method for preparing a carbon-ceramic brake disc, which comprises preparing a low-density C/C composite material by a vapor deposition method, preparing a carbon/ceramic brake disc by a precursor impregnation cracking method and a melt siliconizing method, and finally processing and molding the carbon-ceramic composite material to obtain the carbon-ceramic brake disc. However, the carbon-ceramic brake material has high hardness, which results in time-consuming processing, severe cutter loss and extremely high processing cost. In addition, the post-processing belongs to material reduction manufacturing, so that the material utilization rate is reduced, and the cost of the brake disc is increased. Based on the above, the invention provides a preparation method of a carbon ceramic disc, which can improve the material utilization rate and avoid processing the carbon ceramic brake disc, so that the production cost of the carbon ceramic brake disc is greatly reduced.
Disclosure of Invention
The invention relates to a preparation method of a carbon-ceramic brake disc, which comprises the following specific processes: (1) preparing a carbon fiber preform; (2) carrying out chemical vapor deposition on the prefabricated body to prepare a C/C composite material; (3) processing the C/C composite material into unit modules; (4) preparing a C/C brake disc by bonding; (5) and (4) infiltrating the reaction melt to prepare the carbon/ceramic brake disc. The invention can improve the material utilization rate and avoid processing the carbon/ceramic brake disc, thereby greatly reducing the production cost of the carbon/ceramic brake disc.
The technical scheme of the invention is as follows:
a preparation method of a carbon-ceramic brake disc comprises the following steps:
(1) preparing a carbon fiber preform; preparing unidirectional non-dimensional cloth and a short fiber net tire by using carbon fiber bundles, then circularly layering a layer of non-dimensional cloth, a layer of net tire and a layer of non-dimensional cloth, and finally needling to prepare a three-dimensional needling structure carbon fiber preform;
(2) preparing a C/C composite material by chemical vapor deposition; putting the carbon fiber preform into a CVI furnace, and carrying out isothermal and isobaric chemical vapor deposition, wherein the deposition gases are natural gas and ethylene, so as to obtain a C/C composite material;
(3) processing the C/C composite material into a fan-shaped unit module and a circular unit module as required;
(4) after coating adhesives on the upper surface and the lower surface of the fan-shaped unit module, adhering the fan-shaped unit module and the annular unit module to prepare a C/C brake disc; the adhesive mainly has a shaping function, namely, the brake disc unit module is fixed, so that the transportation and the furnace charging are convenient;
(5) and (3) putting silicon powder in a BN crucible, putting the bonded C/C brake disc on the silicon powder, putting the crucible into a siliconizing furnace for melt infiltration, and preparing the carbon/ceramic brake disc by the reaction melt infiltration.
According to the present invention, it is preferable that the carbon fiber preform in step (1) is laid to a thickness of 14 to 16 layers/cm and the carbon fiber preform has a density of 0.4 to 0.6g/cm3The needling density is 25-30 needles/cm3
According to the present invention, preferably, the deposition temperature in step (2) is 950-1100 ℃, the natural gas purity is 99.9%, the ethylene purity is 99.5%, wherein the natural gas flow is 40-80SLM, the ethylene flow is 40-80SLM, and the deposition time is 300-400h, such that the density is 1.0-1.4g/cm3The C/C composite material of (1).
According to the present invention, it is preferable that the number of the sector unit modules in the step (3) is 6 to 8, the number of the circular unit modules is 2, and the sector unit module is disposed between the two circular unit modules.
According to the invention, preferably, in the step (4), the fan-shaped unit module and the circular unit module are bonded and then placed into an oven for curing, the curing temperature is 200 ℃ and 250 ℃, and the heat preservation time is 1-2 h.
According to the present invention, preferably, the adhesive in the step (4) is selected from one of the following:
A. the adhesive is prepared from the following raw materials in parts by mass: 30 parts of phenolic resin, 40 parts of absolute ethyl alcohol and 30 parts of C powder;
B. the adhesive is prepared from the following raw materials in parts by mass: 40 parts of phenolic resin, 40 parts of absolute ethyl alcohol and 20 parts of SiC powder;
C. the adhesive is prepared from the following raw materials in parts by mass: 30 parts of furfuryl ketone resin, 40 parts of absolute ethyl alcohol and 20 parts of SiC powder;
putting the raw materials of the adhesive into a ball milling tank, and carrying out ball milling and mixing for more than 2 hours.
According to the invention, it is further preferable that the phenolic resin used in the step (4) is 2123 type, the purity of the C powder is more than 99%, and the particle size is 1 um; the granularity of the SiC is 0.5um, and the purity is more than 98 percent; the furfuryl ketone resin is KT-1 produced by Shandong Yongchuang GmbH.
According to the invention, in the step (5), the crucible is placed in a siliconizing furnace, then the crucible is vacuumized to be below 500pa, the temperature is raised to 1500 ℃ for melt infiltration, and the heat preservation time is 15-30 min. During the infiltration of the reaction melt, the liquid silicon bonds the two materials.
According to the invention, the granularity of the silicon powder in the step (5) is preferably 200 meshes, and the purity is more than or equal to 99.9%.
According to the invention, the adding amount of the silicon powder in the step (5) is preferably 1-2.5 times of the mass of the bonded C/C brake disc.
The invention has the following beneficial effects:
according to the invention, after C/C is processed into unit modules, the C/C brake disc is prepared in a bonding mode and reaction melt infiltration is carried out, and each C/C unit module is vitrified into SiC while SiC is generated by reaction of Si and C, so that the bonding effect is achieved. Compared with the method for processing the integral C/C blank, the method has the advantages of improving the utilization rate of the C/C material, simplifying the processing flow, shortening the processing period and reducing the production cost of the carbon-ceramic brake disc.
Description of the drawings:
FIG. 1 is a schematic view of a bonded C/C brake disc;
FIG. 2 is a schematic illustration of brake disc siliconizing;
FIG. 3 is a SEM of a low-power carbon ceramic brake disc section;
FIG. 4 is a high-power carbon-ceramic brake disc cross-section SEM;
FIG. 5 is a schematic flow chart of the method of the present invention;
FIG. 6 is a graph comparing the shear strength of a carbon/ceramic brake disc prepared in comparative example and example 3.
Wherein: 1. 2, a unit module, 3, a BN crucible, 4, a C/C brake disc, 5 and silicon powder.
Detailed Description
The present invention will be further described by way of examples, but not limited thereto, with reference to the accompanying drawings.
Example 1
A preparation method of a carbon-ceramic brake disc comprises the following steps:
(1) preparation of carbon fiber preform
Preparing unidirectional non-woven cloth and short fiber net tire by Dongli T700-12K carbon fiber bundles, performing cyclic layering to 1cm according to 0-degree non-woven cloth, short fiber net tire and 90-degree non-woven cloth, performing needling, repeating the steps to prepare a carbon fiber preform with the size of 40cm x 3cm, and ensuring the density of the carbon fiber preform to be 0.45g/cm314-16 layers/cm.
(2) Preparation of C/C composite material by chemical vapor deposition
Putting the carbon fiber preform into a CVI furnace, carrying out isothermal and isobaric chemical vapor deposition at the deposition temperature of 1100 ℃, wherein the deposition gases are natural gas and ethylene, the natural gas flow is 80SLM, the ethylene gas flow is 40SLM, and the deposition time is 340h, thus obtaining the carbon fiber preform with the density of 1.40g/cm3C/C composite material.
(3) Processing the C/C composite material into unit modules, wherein the unit modules comprise 6 fan-shaped unit modules and 2 circular unit modules;
(4) the unit modules are bonded to prepare a C/C brake disc;
putting 30 parts of phenolic resin, 40 parts of absolute ethyl alcohol and 30 parts of C powder into a ball milling tank, and performing ball milling mixing for more than 2 hours to ensure that the adhesive is uniformly mixed;
coating an adhesive with the thickness of 0.5-1.0mm on the upper surface and the lower surface of the fan-shaped unit module, then bonding the fan-shaped unit module and the annular unit module, assembling to prepare a C/C brake disc, and then putting the C/C brake disc into an oven for curing, wherein the curing temperature is 250 ℃, and the heat preservation time is 2 hours;
(5) preparation of carbon/ceramic brake disc by infiltration of reaction melt
Placing silicon powder in a BN crucible, then placing the bonded C/C brake disc on the silicon powder, wherein the amount of the silicon powder is 2 times of the weight of the C/C brake disc, then placing the bonded C/C brake disc in a silicon infiltration furnace, vacuumizing to below 500pa, heating to 1500 ℃ for melt infiltration, and keeping the temperature for 30 min.
Example 2
A preparation method of a carbon-ceramic brake disc comprises the following steps:
(1) preparation of carbon fiber preform
Preparing unidirectional non-woven cloth and short fiber net tire by Dongli T700-12K carbon fiber bundles, performing cyclic layering to 1cm according to 0-degree non-woven cloth, short fiber net tire and 90-degree non-woven cloth, performing needling, repeating the steps to prepare a carbon fiber preform with the size of 40cm x 3cm, and ensuring the density of the carbon fiber preform to be 0.45g/cm314-16 layers/cm.
(2) Preparation of C/C composite material by chemical vapor deposition
Putting the carbon fiber preform into a CVI furnace, performing chemical vapor deposition at 1100 ℃, wherein the deposition gas comprises natural gas and ethylene, the natural gas flow is 80SLM, the ethylene gas flow is 40SLM, and the deposition time is 340h, so that the density of the carbon fiber preform is 1.40g/cm3C/C composite material.
(3) Processing the C/C composite material into 8 fan-shaped unit modules and 2 circular unit modules
(4) The unit modules are bonded to prepare a C/C brake disc;
putting 40 parts of phenolic resin, 40 parts of absolute ethyl alcohol and 20 parts of SiC into a ball milling tank, and carrying out ball milling mixing for more than 2 hours to ensure that the adhesive is uniformly mixed;
coating an adhesive with the thickness of 0.5-1.0mm on the upper surface and the lower surface of the fan-shaped unit module, then bonding the fan-shaped unit module and the annular unit module, assembling to prepare a C/C brake disc, and then putting the C/C brake disc into an oven for curing, wherein the curing temperature is 250 ℃, and the heat preservation time is 2 hours;
(5) preparation of carbon/ceramic brake disc by infiltration of reaction melt
Placing silicon powder in a BN crucible, then placing the bonded C/C brake disc on the silicon powder, wherein the amount of the silicon powder is 2 times of the weight of the C/C brake disc, then placing the bonded C/C brake disc in a siliconizing furnace, vacuumizing to below 500pa, heating to 1500 ℃ for melt infiltration, and keeping the temperature for 30 min;
example 3
A preparation method of a carbon-ceramic brake disc comprises the following steps:
(1) preparation of carbon fiber preform
Preparing unidirectional non-woven cloth and short fiber net tire by Dongli T700-12K carbon fiber bundles, performing cyclic layering to 1cm according to 0-degree non-woven cloth, short fiber net tire and 90-degree non-woven cloth, performing needling, repeating the steps to prepare a carbon fiber preform with the size of 40cm x 3cm, and ensuring the density of the carbon fiber preform to be 0.45g/cm314-16 layers/cm.
(2) Preparation of C/C composite material by chemical vapor deposition
Putting the carbon fiber preform into a CVI furnace, performing chemical vapor deposition at 1100 ℃, wherein the deposition gas comprises natural gas and ethylene, the natural gas flow is 80SLM, the ethylene gas flow is 40SLM, and the deposition time is 340h, thus obtaining the carbon fiber preform with the density of 1.4g/cm3C/C composite material.
(3) Processing the C/C composite material into 6 fan-shaped unit modules and 2 circular unit modules
(4) The unit modules are bonded to prepare a C/C brake disc;
40 parts of phenolic resin, 40 parts of absolute ethyl alcohol and 20 parts of SiC are put into a ball milling tank for ball milling and mixing for more than 2 hours, so that the adhesive is uniformly mixed;
coating an adhesive with the thickness of 0.5-1.0mm on the upper surface and the lower surface of the fan-shaped unit module, then bonding the fan-shaped unit module and the annular unit module, assembling to prepare a C/C brake disc, and then putting the C/C brake disc into an oven for curing, wherein the curing temperature is 250 ℃, and the heat preservation time is 2 hours;
(5) preparation of carbon/ceramic brake disc by infiltration of reaction melt
Placing silicon powder in a BN crucible, then placing the bonded C/C brake disc on the silicon powder, wherein the amount of the silicon powder is 2 times of the weight of the C/C brake disc, then placing the bonded C/C brake disc in a silicon infiltration furnace, vacuumizing to below 500pa, heating to 1500 ℃ for melt infiltration, and keeping the temperature for 30 min.
The brake disc prepared by the method of the embodiment has the cross-section SEM microscopic views as shown in fig. 3 and fig. 4, as can be seen from fig. 3, the bonding layer is formed at the positions of the fan-shaped unit module (left) and the annular unit module (right) in the infiltration process of the reaction melt through the adhesive, the bonding layer is uniform and compact and has no air holes and macrocracks, the bonding layer is composed of SiC and Si phases, as can be seen from the partial enlarged view of fig. 4, the bonding layer reacts with the unit modules to generate a SiC transition layer, the macrocracks are avoided, and the bonding layer has excellent mechanical properties.
Example 4
The preparation method of the carbon-ceramic brake disc comprises the following steps of 1, except that in the step (4), the adhesive is prepared from the following raw materials in parts by mass: 30 parts of furfuryl ketone resin, 40 parts of absolute ethyl alcohol and 20 parts of SiC powder; putting the raw materials of the adhesive into a ball milling tank, and carrying out ball milling and mixing for more than 2 hours.
Example 5
A preparation method of a carbon-ceramic brake disc comprises the steps of embodiment 1, except that in the step (4), a fan-shaped unit module and a circular unit module are bonded and then placed in an oven to be cured, the curing temperature is 200 ℃, and the heat preservation time is 1 h.
Example 6
The preparation method of the carbon-ceramic brake disc comprises the steps as described in example 1, except that in the step (5), the adding amount of silicon powder is 1 time of the mass of the bonded C/C brake disc; and (3) placing the crucible into a siliconizing furnace, vacuumizing to below 500pa, heating to 1500 ℃ for melt infiltration, and keeping the temperature for 30 min.
Example 7
The preparation method of the carbon-ceramic brake disc comprises the steps as described in example 1, except that in the step (5), the adding amount of silicon powder is 2.5 times of the mass of the bonded C/C brake disc; and (3) placing the crucible into a siliconizing furnace, vacuumizing to below 500pa, heating to 1500 ℃ for melt infiltration, and keeping the temperature for 15 min.
Example 8
A method for preparing a carbon-ceramic brake disc, which comprises the following steps of example 1, except that the deposition temperature in the step (2) is 950 ℃, the purity of natural gas is 99.9%, the purity of ethylene is 99.5%, wherein the flow rate of the natural gas is 40SLM, the flow rate of the ethylene is 80SLM, and the deposition time is 300h, so that the C/C composite material can be obtained.
Example 9
A preparation method of a carbon-ceramic brake disc comprises the steps of example 8, except that the C/C composite material can be obtained after deposition time in the step (2) is 400 hours.
Example 10
The preparation method of the carbon-ceramic brake disc comprises the steps of example 1, except that in the step (4), the fan-shaped unit module and the circular unit module are bonded and then placed in an oven for curing, the curing temperature is 200 ℃, and the heat preservation time is 1 hour.
Comparative example 1
The preparation method of the conventional carbon-ceramic brake disc comprises the following steps: preparing a carbon fiber preform, preparing a C/C composite material by chemical vapor deposition, preparing a carbon/ceramic composite material by infiltration of a reaction melt, and processing the prepared carbon/ceramic composite material into a carbon/ceramic brake disc according to a drawing. When the carbon/ceramic composite material is processed, a diamond milling cutter with the diameter of 8mm is used for processing the carbon/ceramic, the milling amount in the whole process is 3423cm3, the cutter loss is 6, the processing time is 350min, the ratio of the volume of the brake disc to the volume of the carbon/ceramic composite material blank is 0.331, and the material utilization rate is 33.1%.
When carbon ceramics were prepared using the method steps of example 3, C/C was machined using the same diamond milling cutter with a diameter of 8mm, and the milling amount in the whole process was 1397cm3The cutter is not worn, the processing time is 60 mm, the ratio of the volume of the brake disc to the volume of the carbon/ceramic composite material blank is 0.548, and the material utilization rate is 54.8 percent.
The shear strength stress strain of the materials prepared in the example 3 and the comparative example is shown in fig. 6, and it can be seen that the shear strength difference between the example 3 and the comparative example is not large, and the stress strain curves are jagged, which indicates that the fracture modes are ductile fractures, so that it can be inferred that the strength of the carbon ceramic brake disc prepared in the example 3 and the comparative example is equivalent, and the service life difference is not large, but the method has great advantages in material utilization, tool loss and processing time.
TABLE 1 comparison of the effects
Preparation scheme Milling amount/cm3 Material utilization ratio% Tool holder Processing time/min
Comparative example 3423 33.1 6 350
Example 3 1397 54.8 0 60

Claims (6)

1. The preparation method of the carbon-ceramic brake disc is characterized by comprising the following steps of:
(1) preparing a carbon fiber preform; preparing unidirectional non-dimensional cloth and a short fiber net tire by using carbon fiber bundles, then circularly layering a layer of non-dimensional cloth, a layer of net tire and a layer of non-dimensional cloth, and finally needling to prepare a three-dimensional needling structure carbon fiber preform;
(2) preparing a C/C composite material by chemical vapor deposition; putting the carbon fiber preform into a CVI furnace, and carrying out isothermal and isobaric chemical vapor deposition, wherein the deposition gases are natural gas and ethylene, so as to obtain a C/C composite material;
(3) processing the C/C composite material into a fan-shaped unit module and a circular unit module as required;
the number of the fan-shaped unit modules is 6-8, the number of the circular unit modules is 2, and the fan-shaped unit modules are arranged between the two circular unit modules;
(4) after coating adhesives on the upper surface and the lower surface of the fan-shaped unit module, adhering the fan-shaped unit module and the annular unit module to prepare a C/C brake disc;
after being bonded, the fan-shaped unit module and the circular unit module are put into an oven for curing, wherein the curing temperature is 200-250 ℃, and the heat preservation time is 1-2 h;
the adhesive is selected from one of the following:
A. the adhesive is prepared from the following raw materials in parts by mass: 30 parts of phenolic resin, 40 parts of absolute ethyl alcohol and 30 parts of C powder;
B. the adhesive is prepared from the following raw materials in parts by mass: 40 parts of phenolic resin, 40 parts of absolute ethyl alcohol and 20 parts of SiC powder;
C. the adhesive is prepared from the following raw materials in parts by mass: 30 parts of furfuryl ketone resin, 40 parts of absolute ethyl alcohol and 20 parts of SiC powder;
putting the raw materials of the adhesive into a ball milling tank, and carrying out ball milling mixing for more than 2 hours; the phenolic resin is 2123 type, the purity of C powder is more than 99 percent, and the granularity is 1 mu m; the granularity of the SiC is 0.5 mu m, and the purity is more than 98 percent; the furfuryl ketone resin is KT-1 type;
(5) putting silicon powder in a BN crucible, putting the bonded C/C brake disc on the silicon powder, putting the crucible into a siliconizing furnace for melt infiltration, and preparing the carbon/ceramic brake disc by the melt infiltration reaction.
2. The method for preparing a carbon-ceramic brake disc as claimed in claim 1, wherein the carbon fiber preform is laid in the thickness of 14-16 layers/cm in step (1), and the density of the carbon fiber preform is 0.4-0.6g/cm3The needling density is 25-30 needles/cm3
3. The method for preparing a carbon-ceramic brake disc as claimed in claim 1, wherein the deposition temperature in the step (2) is 950-1100 ℃ per dayThe purity of natural gas is 99.9 percent, the purity of ethylene is 99.5 percent, wherein the flow rate of natural gas is 40SLM-80SLM, the flow rate of ethylene is 40SLM-80SLM, the deposition time is 300h-400h, and the density is 1.0-1.4g/cm3The C/C composite material of (1).
4. The preparation method of the carbon-ceramic brake disc as claimed in claim 1, wherein in the step (5), the crucible is placed in a siliconizing furnace, then the crucible is vacuumized to be below 500P a, the temperature is raised to 1500 ℃ for melt infiltration, and the heat preservation time is 15min to 30 min.
5. The preparation method of the carbon-ceramic brake disc as claimed in claim 1, wherein the silicon powder in the step (5) has a particle size of 200 meshes and a purity of not less than 99.9%.
6. The preparation method of the carbon-ceramic brake disc as claimed in claim 1, wherein the silicon powder is added in the step (5) in an amount of 1-2.5 times the mass of the bonded C/C brake disc.
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