CN115536419A - Aviation carbon-ceramic brake material and preparation method thereof - Google Patents
Aviation carbon-ceramic brake material and preparation method thereof Download PDFInfo
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- C04B2235/9607—Thermal properties, e.g. thermal expansion coefficient
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
- F16D—COUPLINGS FOR TRANSMITTING ROTATION; CLUTCHES; BRAKES
- F16D2200/00—Materials; Production methods therefor
- F16D2200/0034—Materials; Production methods therefor non-metallic
- F16D2200/0039—Ceramics
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
- F16D—COUPLINGS FOR TRANSMITTING ROTATION; CLUTCHES; BRAKES
- F16D2200/00—Materials; Production methods therefor
- F16D2200/0082—Production methods therefor
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Abstract
The invention discloses a preparation method of an aviation carbon ceramic brake material, which comprises the steps of enabling the centers of N hollow disc-shaped carbon fiber preforms to penetrate through an internal heat source heater to be stacked to form a material column, placing the material column in a chemical vapor deposition furnace, controlling the distance between any two adjacent carbon fiber preforms to be 0.4-3.5mm, sealing the periphery of the upper end of the material column by using a hollow sealing material, enabling an air outlet to be only located in the middle of the upper end of the material column, uniformly arranging at least 6 air inlets on the side face of the lower end of the material column, using propylene as a carbon source gas and nitrogen as a diluent gas to carry out chemical vapor deposition, enabling the temperature of the chemical vapor deposition to be 1020-1100 ℃, gradually decreasing the temperature of the chemical vapor deposition along with the increase of deposition time, forming a carbon blank after the chemical vapor deposition, carrying out heat treatment to obtain a carbon porous body, and carrying out ceramic treatment to obtain the aviation carbon ceramic brake material.
Description
Technical Field
The invention relates to a preparation method of an aviation carbon-ceramic brake material, and belongs to the technical field of brake material preparation.
Background
The C/C composite material is mostly adopted as a matrix of the aviation carbon-ceramic brake material, the density control, the pore distribution and the material microstructure of the matrix can directly influence the performance of a brake pair of the aviation carbon-ceramic material, and carbon-ceramic materials with large performance differences, such as small friction coefficient, abnormal friction curve during loading and the like, can be obtained by different matrix structures of the carbon-ceramic brake material under the same siliconizing process condition, which is also a main reason that many carbon-ceramic brake materials cannot be directly applied to the aviation brake material.
Disclosure of Invention
Aiming at the defects of the prior art, the first purpose of the invention is to provide a preparation method of an aviation carbon-ceramic brake material.
The second purpose of the invention is to provide the aviation carbon ceramic brake material prepared by the preparation method, and the density of the obtained aviation carbon ceramic brake material can reach 2.20g/cm at most 3 The brake curve is good, the abrasion is low,
in order to achieve the purpose, the invention adopts the following technical scheme:
the invention relates to a preparation method of an aviation carbon ceramic brake material, which comprises the steps of enabling the centers of N hollow disc-shaped carbon fiber preforms to penetrate through an internal heat source heater to be stacked to form a material column, placing the material column in a chemical vapor deposition furnace, controlling the distance between any two adjacent carbon fiber preforms to be 0.4-3.5mm, sealing the periphery of the upper end of the material column by using a hollow sealing material, enabling an air outlet to be only located in the middle of the upper end of the material column, uniformly arranging at least 6 air inlets on the side face of the lower end of the material column, using propylene as a carbon source gas and nitrogen as a diluent gas to carry out chemical vapor deposition, enabling the temperature of the chemical vapor deposition to be 1020-1100 ℃, gradually decreasing the temperature of the chemical vapor deposition along with the increase of deposition time, forming a carbon blank after the chemical vapor deposition, carrying out heat treatment to obtain a carbon body, and carrying out ceramic treatment to obtain the aviation carbon ceramic porous body.
The preparation method of the invention adopts a resistance heating mode for the inner diameter, and adopts the prefabricated bodies to pass through the inner heat source heater for stacking, and controls the space between any adjacent carbon fiber prefabricated bodies to be 0.4-3.5mm, so that the formed inner ring and outer ring are emptyThe upper end of the material column is sealed by adopting a hollow sealing material, so that the gas outlet is arranged in the middle of the upper end of the material column, and the gas inlet is uniformly arranged on the side surface of the lower end of the material column, so that the carbon fiber preform forms a thermal gradient from inside to outside, in the chemical deposition process, propylene is used as a carbon source gas, the temperature of chemical vapor deposition is gradually reduced along with the deposition process, and finally a structure with a carbon matrix, uniformly distributed holes and almost through holes can be formed, so that the highest density of the aviation carbon ceramic brake material obtained after ceramic treatment can reach 2.20g/cm 3 Meanwhile, more than 80% of the materials are in a rough layer structure from inside to outside, and the carbon-ceramic brake material plays an important role in mechanical property, frictional wear property and heat conductivity.
Preferably, the carbon fiber preform is obtained by the following steps: alternately laminating the carbon fiber laid cloth and the carbon fiber mesh fabric, and continuously needling the carbon fibers to obtain the carbon fiber preform, wherein the mass ratio of the carbon fiber laid cloth to the mesh fabric is 1.
Preferably, the density of the carbon fiber preform is 0.45g/cm 3 -0.60g/cm 3 。
In a preferred scheme, the carbon fiber preform is subjected to heat treatment at 2100-2300 ℃ for 2-3h.
The carbon fiber preform is subjected to heat treatment, organic matters on the surface of the carbon fiber are volatilized through the heat treatment, the specific surface area is increased, the interface bonding strength of the pyrolytic carbon and the carbon fiber is increased in the later Chemical Vapor Deposition (CVD) densification process, and the strength of the material is increased.
In a preferred scheme, the internal heat source heater is positioned in the center of the chemical vapor deposition furnace, and the chemical vapor deposition furnace is in a cylindrical shape.
Preferably, the number of the air inlets is 6-10, preferably 8. The inventors have found that the number of air inlets is controlled within the preferred range, and the final deposition effect is optimal.
According to the preferable scheme, during chemical vapor deposition, temperature is controlled through 4 temperature measuring points, namely a main control temperature measuring point, an upper temperature measuring point, a middle temperature measuring point and a lower temperature measuring point, wherein the main control temperature measuring point is axially positioned in the middle of the stock column and is 18-25mm away from the outer diameter of the inner heat source heater in the radial direction, the upper temperature measuring point is axially positioned at the upper part of the stock column and is radially positioned at the outer edge of the stock column, the middle temperature measuring point is axially positioned in the middle of the stock column and is radially positioned at the outer edge of the stock column, and the lower temperature measuring point is axially positioned at the lower part of the stock column and is radially positioned at the outer edge of the stock column. By adopting the temperature control mode, the thermal gradient in the invention can be effectively monitored, and the effective operation of the CVI process is ensured.
Preferably, the chemical vapor deposition is divided into three sections, the temperature of the first section of chemical vapor deposition is 1060-1085 ℃, the temperature is firstly raised to 1080-1085 ℃, then the temperature is lowered to 1060-1065 ℃ at 15-22 ℃/80h, the time of the first section of chemical vapor deposition is controlled to be 80-110h, the pressure during the first section of chemical vapor deposition is 0.8-1.2kPa, the temperature of the second section of chemical vapor deposition is 1060-1040 ℃, the temperature is firstly raised to 1055-1060 ℃, then the temperature is lowered to 1040-1045 ℃ at 10-20 ℃/40h, the time of the second section of chemical vapor deposition is controlled to be 55-65h, the pressure of the second section of chemical vapor deposition is 0.60-1.2kPa, the temperature of the third section of chemical vapor deposition is constantly set to 1030-1040 ℃, the time of the third section of chemical vapor deposition is controlled to be 20-60h, and the pressure of the third section of chemical vapor deposition is 0.60-1.2kPa.
In the practical operation of 25392f, the temperature of the chemical vapor deposition is the temperature of a main control temperature measuring point, when the main control temperature measuring point reaches the set temperature of the chemical vapor deposition, gas is introduced to carry out deposition, and the temperatures of an upper temperature measuring point, a middle temperature measuring point and a lower temperature measuring point in any chemical vapor deposition stage are controlled to be more than or equal to 920 ℃ in the deposition process.
According to the invention, propylene is used as a nitrogen gas source and nitrogen is used as a diluent gas in three stages of chemical vapor deposition, then the temperature gradients of the three stages are controlled within the range, and the processing time of each stage is coordinated, so that the deposition is uniform, almost all pores are through holes, the efficiency of post-ceramic processing is greatly improved, the final density of the final aviation carbon-ceramic brake material is improved, more than 80% of carbon can be in a rough layer structure, the carbon-ceramic brake material can obtain a stable and proper friction coefficient, the heat conduction is improved, and meanwhile, a small amount of smooth layer carbon has high hardness and high strength, and can better effectively support silicon carbide, so that the abrasion is reduced to the lowest under the coordination of the structure.
Further preferably, in the first-stage chemical vapor deposition, the mass ratio of propylene to nitrogen is 1.8-2.2, and the ratio of the total volume of the carbon fiber preform into which propylene and nitrogen are introduced per minute is 1.2-1.3.
Further preferably, in the second-stage chemical vapor deposition, the mass ratio of propylene to nitrogen is 1.8-2.2.
Further preferably, in the third stage of chemical vapor deposition, the mass ratio of propylene to nitrogen is 1.8-2.2, and the ratio of the total volume of the carbon fiber preform into which propylene and nitrogen are introduced per minute is 0.8-0.9.
In the three-stage deposition process, the flow rates of the carbon source gas and the nitrogen gas are controlled within the preferable range, and the structure of the finally obtained carbon matrix is optimal.
Preferably, during the loading of the first stage of chemical vapor deposition, the N carbon fiber preforms are sequentially numbered from small to large or from large to small from bottom to top, the distance between any two adjacent carbon fiber preforms is controlled to be 2-3mm, during the loading of the second stage of chemical vapor deposition, all carbon blanks are firstly divided into two sections B and A from bottom to top, when the first chemical vapor deposition is numbered from small to large in sequence, the number of the section B is from middle to large, the number of the section A is from small to middle, when the first chemical vapor deposition charging is carried out in the order of large to small, the number of the section B is from middle to small, the number of the section A is from large to middle, the distance between any two adjacent carbon fiber preforms is controlled to be 1.5-2.5mm when the second chemical vapor deposition charging is carried out, and the first removal density is more than 1.42g/cm when the third chemical vapor deposition charging is carried out 3 Then dividing the rest M carbon-carbon blanks into the carbon-carbon blanks from bottom to topD and C, when the materials are numbered in sequence from small to large in the first chemical vapor deposition charging process, the number of the D section is from middle to large, the number of the C section is from small to middle, when the materials are numbered in sequence from large to small in the first chemical vapor deposition charging process, the number of the D section is from middle to small, the number of the C section is from large to middle, meanwhile, the distance between two adjacent carbon blanks with the density lower than the middle value is controlled to be 1.3-1.6mm, and the density is controlled to be 1.4g/cm at the middle value 3 The space between two adjacent carbon-carbon blanks is 0.7-1.1mm, and the density is 1.4g/cm 3 The distance between the two adjacent carbon-carbon green bodies is 0.4-0.6mm.
The inventor finds that through the numbering mode of the invention and the control of the thickness of the gasket in the above mode, the density of a single carbon-carbon blank can be uniform finally, and the density among different carbon-carbon blanks can also be kept to be very high, and particularly in the third chemical vapor deposition, the control of the thickness of the gasket has obvious effects of distribution and fashion control of a convection field, high thickening speed of the thickness and the thickening speed of the thickness relative to the thickness of the gasket are low, so that the uniformity of the density of the material can be controlled.
In the actual operation process, the carbon-carbon green body obtained after the first-stage chemical vapor deposition is machined for the first time, the surface of the green body is machined and peeled, the size of the carbon-carbon green body is controlled to be about 50% of the total machining allowance, the carbon-carbon green body is machined for the second time after the second-stage chemical vapor deposition, the surface of the green body is machined and peeled, the size of the carbon-carbon green body is controlled to be about 30% of the total machining allowance, and the blank body volume density of the prefabricated body can be reduced after the peeling process, wherein the maximum reduction amplitude is generally 0.04g/mm 3 After the third stage of chemical vapor deposition, the carbon blank is firstly subjected to heat treatment and then subjected to third machining, the size of the carbon blank accounts for 20 percent of the total machining allowance, and the carbon blank can be reduced in volume density after being peeled in the process, and the reduction amplitude is generally 0.03g/mm 3 -0.05g/mm 3 The larger the decrease of the density is.
In a preferred embodiment, the bulk density of the carbon-carbon blank obtained after the first-stage chemical vapor deposition is 0.85g/mm 3 -1.15g/mm 3 The volume density of the carbon-carbon blank obtained after the second-stage chemical vapor deposition is 1.25g/mm 3 -1.45g/mm 3 The volume density of the carbon-carbon blank obtained after the third-stage chemical vapor deposition is 1.38g/cm 3 -1.48g/cm 3 。
In a preferable scheme, the heat treatment temperature is 2000-2100 ℃, and the heat treatment time is 1-3h.
Further preferably, the density obtained after the second stage of chemical vapor deposition is more than 1.42g/cm 3 And carrying out heat treatment on the carbon-carbon blank and the carbon-carbon blank subjected to the third-stage chemical vapor deposition.
Preferably, the density of the carbon-carbon porous body is 1.35g/cm 3 -1.45g/cm 3 。
Preferably, the ceramic treatment mode is reaction melt siliconizing, the reaction melt siliconizing is carried out in an argon atmosphere, the temperature of the reaction melt siliconizing is 1550-1650 ℃, the time of the reaction melt siliconizing is 2-4h, and the pressure is 0.1-0.15Pa.
The aviation carbon-ceramic brake material prepared by the preparation method is provided by the invention.
Principles and advantages
The preparation method of the aviation carbon-ceramic brake material provided by the invention realizes effective control of gap distribution, density control and microstructure of a base material structure through design of a loading mode, process temperature field design control, design flow field distribution, pressure design control and the like by using a TG-CVI process method, and further obtains the carbon-ceramic brake pair after the base material is obtained through mechanical processing and the technological processes of a siliconizing process and the like, and meets various index requirements of an unmanned aircraft of a certain model on brake performance through tests of various indexes of the material, an inertial table test and the like, and the preparation method is practically applied to the carbon-ceramic brake pair of the unmanned aircraft of the certain model.
Compared with the prior art, the invention has the following advantages:
1. the process method is suitable for large-scale production and manufacturing processes, and the rejection rate formed in the manufacturing process is very low.
2. Adjustment of CVI time and adjustment of charging by the method of the inventionThe volume density of the material is controlled by the thickness of the gasket, the density qualified rate of the densified preform is effectively guaranteed, the consistency and the stability of the material preparation are improved, and the material can be controlled to be 1.35g/cm finally 3 -1.45g/cm 3 In the meantime. The density distribution difference of the material is less than 0.10g/cm 3 。
3. The porosity of the composite material prepared by the invention is controlled, and the formation form and the hole sealing degree of the material porosity are controlled by gradually decreasing the main control temperature and controlling the deposition rate in the deposition process in the CVI process. The microstructure of the material shows that the radius size of the outer diameter of the deposited carbon growing around the carbon fiber is controlled within the range of 0.6-0.9 μm, which is beneficial to the formation of through holes in pores and the densification of a siliconizing melting process.
4. The process control of temperature, flow and pressure in the CVI process is adopted to control the material structure, more than 80% of carbon materials are in a rough layer structure from inside to outside, and the carbon materials play an important role in the mechanical property, the frictional wear property and the heat conductivity of the carbon ceramic brake material.
5. The material has strong infiltration capacity: the material has the highest density of 2.20g/cm after subsequent siliconizing 3 。
6. The aviation carbon-ceramic brake material provided by the invention has the advantages that the mechanical property, the heat conductivity and the dynamic friction coefficient all meet the brake performance requirements of an unmanned aerial vehicle, and the deceleration rate is more than 3.05m/s in an inertia test 2 The dynamic friction coefficient is 0.29-0.37, the braking curve has good performance, the average wear rate is about 0.42 mu m/time surface, other technical indexes meet the requirements, and the brake is already applied to a carbon ceramic braking pair of an unmanned aerial vehicle.
Drawings
FIG. 1 is a schematic view of a chemical vapor deposition material column, a thermal field and a flow field.
Fig. 2 is a microstructure diagram of the carbon-carbon body obtained in example 1.
Fig. 3 is a microstructure diagram of the carbon-carbon green body obtained in example 1.
Fig. 4 is a microstructure diagram of the carbon-carbon body obtained in example 1.
Fig. 5 shows a carbon-ceramic brake byproduct of an unmanned aerial vehicle assembled by the aviation carbon-ceramic brake material obtained in example 1.
Detailed Description
In the following embodiments, the loading space during chemical vapor deposition is a cylindrical space, the upper end of the cylinder is an air outlet, the side surface of the cylinder is provided with air inlets, the air inlets are distributed at the lower end of the cylinder, eight points are uniformly distributed based on the side area of the lower cylinder, and the upper end of the material column is sealed by a sealing material, so that the material column airflow directional diagram 1 is shown.
The inner diameter adopts a resistance heating mode, the center of the carbon fiber prefabricated body passes through the inner heat source heater to be stacked, and an inner ring space and an outer ring space are formed, so that the prefabricated body forms a thermal gradient from inside to outside.
During charging, a 4-point temperature control method is adopted to monitor a temperature field, the temperature field is divided into a main control temperature, upper, middle and lower temperatures are monitored, and the measurement positions are as follows: the main control temperature measuring position is 20mm away from the outer diameter of the heater and the middle position of the material column. The upper monitoring temperature measuring position is located at the outer edge of the material column, and the upper-most monitoring temperature measuring position is located at the outer edge of the material column and the middle end of the material column. The temperature measuring position is located at the outer edge of the material column and the lowest end of the material column under monitoring. The temperature control structure is beneficial to monitoring a temperature field and ensuring the effective operation of the CVI process.
Example 1
Step one, preparation of carbon fiber preform
Alternately laminating the carbon fiber non-woven cloth and the carbon fiber mesh fabric, continuously needling the carbon fiber to obtain a carbon fiber preform, controlling the mass ratio of the carbon fiber non-woven cloth to the mesh fabric to be 1 3 -0.60g/cm 3 Of size of
The carbon fiber preform of (1).
Step two high temperature heat treatment
The carbon fiber preform was heat-treated at 2100 ℃ under vacuum for 3 hours.
Step three CVD1
A preform of 16 carbon fibers was charged and charged into a TG-CVI furnace from small to large in the number of 1 to 16. The thickness of the gasket was controlled to be 2.5mm.
The process control parameters are that the master control temperature is 1060-1080 ℃, and the upper, middle and lower temperature of the monitoring is more than or equal to 900 ℃.
The temperature control mode is as follows: and (3) introducing air to start deposition when the master control temperature reaches 1080 ℃, and reducing the temperature to 1060 ℃ in a temperature reduction range of 20 ℃/80 hours in the deposition process. Introducing gas in a mass ratio: propylene: nitrogen =2, with a ratio of gas flow volume per minute to total preform volume of 1.2. The pressure of the first stage chemical vapor deposition is 0.80-1.2kPa, the deposition time: for 100 hours. The density of the material blank after the stage is finished is 0.85g/mm 3 -1.1g/mm 3 In the meantime. The blank surface is machined and peeled, the size is controlled to be about 50 percent of the total machining allowance, the process is carried out according to the machined size and the weight of the measured material blank, the volume density is measured, and the volume density is 0.85g/mm 3 -1.15g/mm 3 In the meantime.
Step four CVD2
And (3) evenly dividing the blank after the machining 1 into A/B sections according to the numbers from small to large, wherein the numbers of the A sections are 1 to 8, the numbers of the B sections are 9 to 16, and loading the prefabricated bodies into a TG-CVI furnace according to the sequence from B to A (the sequence is 9-16 and 1-8).
The thickness of the gasket is controlled to be 2.0mm.
The control parameters are that the master control temperature is 1060-1040 ℃, and the monitoring upper, middle and lower temperatures are more than or equal to 920 ℃.
The temperature control mode is as follows: aeration was started when the master temperature reached 1060 ℃ and the temperature was lowered to 1040 ℃ in 20 ℃/40 hour temperature ramp.
Introducing gas in a mass ratio: propylene: nitrogen =2, and the ratio of the gas flow volume per minute to the total preform volume was 1.1.
The pressure of the second-stage chemical vapor deposition is 0.60-1.2kPa, and the deposition time is as follows: 60 hours
The density of the blank body after the stage is finished is 1.25g/mm 3 -1.45g/mm 3 Between
Machining 2, peeling the surface in the process, wherein the size of the peel accounts for about 30 percent of the total machining allowance. After the process of peeling, the volume density of the preform body is reduced, and the maximum reduction amplitude is generally 0.04g/mm 3 The higher the density, the larger the reduction.
Bulk density measurement 2
The process comprises measuring bulk density according to the processing size and the weight of the blank, and if the bulk density is more than 1.42g/cm 3 Then the heat treatment process is carried out.
Step five CVD3
And (3) evenly dividing the prefabricated body after machining 2 into A/B sections according to the number from small to large, wherein the number of the A section is from small to medium, the number of the B section is from medium to large, and the prefabricated body is loaded into a TG-CVI furnace according to the sequence from B to A according to the loading control configuration.
The thickness of the gasket is selected according to the following conditions: dividing the material into 3 intervals by taking the intermediate value of the designed volume density of the material as a reference, wherein the gasket control conditions are as follows in the following table 1:
TABLE 1
| Density (g/mm) 3 ) | Pad thickness (mm) |
| Below the median value | 1.5 |
| Median value-1.40 | 0.8 |
| 1.4-1.42 | 0.5 |
The control parameters are that the master control temperature is 1040 ℃, and the upper, middle and lower temperature is not less than 920 ℃.
Temperature control mode: aeration starts to aerate deposition when the master temperature reaches 1040 ℃.
Introducing gas in a mass ratio: propylene: nitrogen =1, and propylene was fed at a ratio of gas flow volume per minute to total preform volume of 0.9.
The pressure of the third stage chemical vapor deposition is 0.60-1.2kPa, the deposition time is as follows: 38 hours
The bulk density of the material after this stage fell to 1.38g/cm 3 -1.48g/cm 3 In between.
Step six heat treatment
The density obtained after the second stage of chemical vapor deposition is more than 1.42g/cm 3 And carrying out heat treatment on the carbon-carbon blank and the carbon-carbon blank subjected to the third-stage chemical vapor deposition. Post heat treatment machining 3
The size accounts for 20 percent of the total processing allowance, and the volume density of the preform body is reduced after peeling in the process, and the reduction amplitude is generally 0.03g/mm 3 -0.05g/mm 3 The higher the density, the larger the reduction amplitude. Bulk density measurement 3 the process was based on the dimensions after heat treatment and on the weight of the green body of the material, and a bulk density measurement was carried out, the bulk density being 1.35g/cm 3 -1.45g/cm 3 The difference of the density distribution of the materials is less than 0.10g/cm 3 。
The bulk density of the sample plate is 1.39g/cm 3 The density distribution of the material is shown in Table 2 below using a local sampling.
TABLE 2
| Position of | Inner diameter | Pitch diameter | Outer diameter |
| On the upper part | 1.41g/cm 3 | 1.40g/cm 3 | 1.37g/cm 3 |
| In | 1.39g/cm 3 | 1.39g/cm 3 | 1.37g/cm 3 |
| Lower part | 1.42g/cm 3 | 1.40g/cm 3 | 1.38g/cm 3 |
Step seven reaction infiltration of silicon
And (3) carrying out reaction, melting and siliconizing on the carbon-carbon porous body obtained by heat treatment to obtain the aviation carbon ceramic brake material.
The reaction melt infiltration is carried out in the argon atmosphere, the temperature of the reaction melt infiltration is 1600 ℃, the time of the reaction melt infiltration is 4h, and the pressure is 0.1-0.15MPa.
The carbon-carbon green body obtained in this example 1, as shown in fig. 2, shows that the radius size of the outer diameter of the deposited carbon growing around the carbon fiber is controlled within the range of 0.6 μm to 0.9 μm, which is beneficial to the formation of through holes in pores and the densification of the siliconizing melting process.
More than 80% of the materials shown in the figures 3 and 4 are in a rough layer structure from inside to outside, and play an important role in the mechanical property, the frictional wear property and the heat conductivity of the carbon-ceramic brake material.
The densities of the carbon porous body and the final product obtained in example 1 are shown in table 3:
TABLE 3
| Density (g/cm) of carbon blank 3 ) | Density after infiltration (g/cm) 3 ) |
| 1.37 | 2.20 |
| 1.40 | 2.20 |
| 1.40 | 2.19 |
| 1.39 | 2.18 |
In the inertia test, the deceleration rate is more than 3.05m/s 2 The brake curve with the dynamic friction coefficient of 0.29-0.37 has good performance, the average wear rate is about 0.42 mu m/time surface, and other technical indexes meet the requirements, so the brake shoe is already applied to a carbon-ceramic brake pair of an unmanned aerial vehicle.
Example 2
Step one, preparation of carbon fiber preform
Alternately laminating the carbon fiber laid fabric and the carbon fiber mesh fabric, continuously needling the carbon fibers to obtain a carbon fiber preform, controlling the mass ratio of the carbon fiber laid fabric to the mesh fabric to be 1 3 -0.60g/cm 3 Of a size of
The carbon fiber preform of (1).
Step two high temperature heat treatment
And (3) carrying out heat treatment on the carbon fiber preform at the temperature of 2200 ℃ under the vacuum condition, wherein the heat treatment time is 2.5 hours.
Step three CVD1
The preform of 18 carbon fibers was charged and charged into a TG-CVI furnace from small to large in the number of 1 to 18. The thickness of the gasket was controlled to be 2.5mm.
The process control parameters are that the master control temperature is 1060-1080 ℃, and the upper, middle and lower temperature of the monitoring is more than or equal to 900 ℃.
Temperature control mode: and (3) ventilating to start deposition when the master control temperature reaches 1085 ℃, and reducing the temperature to 1065 ℃ according to the temperature reduction amplitude of 20 ℃/80 hours in the deposition process. Introducing gas in a mass ratio: propylene: nitrogen =2, with a ratio of gas flow volume per minute to total preform volume of 1.2. The pressure of the first stage chemical vapor deposition is 0.8-1.2kPa, the deposition time is: for 80 hours. The density of the material blank after the stage is finished is 0.90g/mm 3 -1.15g/mm 3 In between. Peeling the blank surface by machining, controlling the size to be about 50% of the total machining allowance, and measuring the volume density according to the machined size and the weight of the blank of the measured material, wherein the volume density is 0.90g/mm 3 -1.14g/mm 3 In between.
Step four CVD2
And (3) evenly dividing the carbon after machining 1 into A/B sections according to the numbers from small to large, wherein the numbers of the A sections are 1 to 9, the numbers of the B sections are 10 to 18, and loading the prefabricated bodies into a TG-CVI furnace according to the sequence from B to A (10-19 and 1-9 in sequence).
The thickness of the gasket is controlled to be 2.0mm.
The control parameters are that the master control temperature is 1060-1040 ℃, and the upper, middle and lower temperature is monitored to be more than or equal to 920 ℃.
The temperature control mode is as follows: aeration is started when the master control temperature reaches 1065 ℃, and the temperature is reduced to 1040 ℃ in a temperature reduction range of 20 ℃/40 hours.
Introducing gas in a mass ratio: propylene: nitrogen =2, the ratio of the gas flow volume per minute to the total preform volume was 1.1.
The pressure of the second-stage chemical vapor deposition is 0.60-1.2kPa, and the deposition time is as follows: 55 hours
The density of the blank body after the stage is finished is 1.28g/mm 3 -1.46g/mm 3 Between
And 2, machining, namely peeling the surface in the process, wherein the size of the product accounts for about 30% of the total machining allowance. After the process of peeling, the volume density of the preform body is reduced, and the maximum reduction amplitude is generally 0.04g/mm 3 The higher the density, the larger the amplitude decrease.
Bulk density measurement 2
The process is based on the machining size and the weight of the blank, and the bulk density is measured, if the bulk density is more than 1.42g/cm 3 Then the heat treatment process is carried out.
Step five CVD3
And (3) evenly dividing the prefabricated body after machining 2 into A/B sections according to the number from small to large, wherein the number of the A section is from small to medium, the number of the B section is from medium to large, and the prefabricated body is loaded into a TG-CVI furnace according to the sequence from B to A according to the loading control configuration.
The thickness of the gasket is selected according to the following conditions: dividing the material into 3 intervals by taking the intermediate value of the designed volume density as a reference, and controlling the gasket as the following table 4:
TABLE 4
The control parameters are that the master control temperature is 1040 ℃, and the upper, middle and lower temperature is not less than 920 ℃.
Temperature control mode: aeration starts to aerate when the master temperature reaches 1040 ℃.
Introducing gas in a mass ratio: propylene: nitrogen =1, and propylene was fed at a ratio of gas flow volume per minute to total preform volume of 0.9.
The pressure of the third-stage chemical vapor deposition is 0.60-1.2kPa, and the deposition time is as follows: 28 hours
The bulk density of the material after this stage fell to 1.39g/cm 3 -1.47g/cm 3 In the meantime.
Step six heat treatment
The density obtained after the second stage of chemical vapor deposition is more than 1.42g/cm 3 And carrying out heat treatment on the carbon-carbon blank and the carbon-carbon blank subjected to the third-stage chemical vapor deposition. Post heat treatment machining 3
The size accounts for 20 percent of the total processing allowance, and the volume density of the preform body is reduced after peeling in the process, and the reduction amplitude is generally 0.02g/mm 3 -0.05g/mm 3 The larger the decrease of the density is. Bulk density measurement 3 the process is based on the dimensions after heat treatment and the weight of the green body of the material, and bulk density measurements are made, with a bulk density of 1.35g/cm 3 -1.45g/cm 3 The difference of the density distribution of the materials is less than 0.10g/cm 3 。
The bulk density of the sample plate is 1.43g/cm 3 The density distribution of the material was measured by local sampling as shown in Table 5 below.
TABLE 5
Step seven reaction infiltration of silicon
And (3) carrying out reaction, melting and siliconizing on the carbon-carbon porous body obtained by heat treatment to obtain the aviation carbon ceramic brake material.
The reaction melt infiltration is carried out under the argon atmosphere, the temperature of the reaction melt infiltration is 1650 ℃, the time of the reaction melt infiltration is 2h, and the pressure is 0.1-0.15MPa.
The carbon-carbon blank obtained in example 2, the size of the radius of the outer diameter of the deposited carbon growing around the carbon fiber is controlled within the range of 0.7 μm to 0.9 μm, which is beneficial to the densification of the siliconizing melting process.
More than 83% of the material is in a rough layer structure from inside to outside, and plays an important role in the mechanical property, the frictional wear property and the heat-conducting property of the carbon-ceramic brake material.
The densities of the carbon porous body and the final product obtained in example 2 are shown in table 6:
TABLE 6
| Density (g/cm) of carbon blank 3 ) | Density after infiltration (g/cm) 3 ) |
| 1.38 | 2.19 |
| 1.42 | 2.20 |
| 1.40 | 2.19 |
| 1.37 | 2.18 |
In the inertia test, the deceleration rate is more than 3.05m/s 2 The dynamic friction coefficient is 0.28-0.36, the braking curve has good performance, the average wear rate is about 0.43 mu m/time surface, other technical indexes meet the requirements, and the brake is already applied to a carbon ceramic braking pair of an unmanned aerial vehicle.
Example 3
Step one, preparation of carbon fiber preform
Alternately laminating the carbon fiber non-woven cloth and the carbon fiber mesh fabric, continuously needling the carbon fiber to obtain a carbon fiber preform, controlling the mass ratio of the carbon fiber non-woven cloth to the mesh fabric to be 1 3 -0.60g/cm 3 Of a size of
The carbon fiber preform of (1).
Step two high temperature heat treatment
The carbon fiber preform was heat-treated at 2300 ℃ for 2 hours under vacuum.
Step three CVD1
A preform of 20 carbon fibers was charged and charged into a TG-CVI furnace from small to large in accordance with the number of 1 to 20. The thickness of the gasket was controlled to be 2.5mm.
The process control parameters are that the master control temperature is 1060-1080 ℃, and the upper temperature, the middle temperature and the lower temperature are monitored to be more than or equal to 900 ℃.
Temperature control mode: and (3) ventilating to start deposition when the master control temperature reaches 1083 ℃, and reducing the temperature to 1063 ℃ according to the temperature reduction amplitude of 20 ℃/80 hours in the deposition process. Introducing gas in a mass ratio: propylene: nitrogen =2, the ratio of the gas flow volume per minute to the total preform volume was 1.2. The pressure of the first stage chemical vapor deposition is 0.8-1.2kPa, the deposition time is: for 110 hours. The density of the material blank after the stage is finished is 0.92g/mm 3 -1.18g/mm 3 In the meantime. Peeling the blank surface by machining, controlling the size to be about 50% of the total machining allowance, and measuring the volume density according to the machined size and the weight of the blank of the measured material, wherein the volume density is 0.93g/mm 3 -1.17g/mm 3 In between.
Step four CVD2
And (3) evenly dividing the carbon after machining 1 into A/B sections according to the numbers from small to large, wherein the numbers of the A sections are 1 to 9, the numbers of the B sections are 10 to 18, and loading the prefabricated bodies into a TG-CVI furnace according to the sequence from B to A (the sequence is 11-20 and 1-10).
The thickness of the gasket is controlled to be 2.0mm.
The control parameters are that the master control temperature is 1060-1040 ℃, and the upper, middle and lower temperature is monitored to be more than or equal to 920 ℃.
Temperature control mode: aeration is started when the master control temperature reaches 1063 ℃, and the temperature is reduced to 1040 ℃ in a temperature reduction range of 20 ℃/40 hours.
Introducing gas in a mass ratio: propylene: nitrogen =2, the ratio of the gas flow volume per minute to the total preform volume was 1.1.
The pressure of the second-stage chemical vapor deposition is 0.60-1.2kPa, and the deposition time is as follows: 65 hours
The density of the blank body after the stage is finished is 1.29g/mm 3 -1.47g/mm 3 Between
And 2, machining, wherein the surface is peeled in the process, and the size of the peeled product accounts for about 30% of the total machining allowance. After peeling in the process, the volume density of the preform body is reduced, and the maximum reduction amplitude is generally 0.05g/mm 3 The higher the density, the larger the reduction.
Bulk density measurement 2
The process is based on the machining size and the weight of the blank, and the bulk density is measured, if the bulk density is more than 1.42g/cm 3 Then the heat treatment process is carried out.
Step five CVD3
And (3) evenly dividing the prefabricated body after machining 2 into A/B sections according to the number from small to large, wherein the number of the A section is from small to medium, the number of the B section is from medium to large, and the prefabricated body is loaded into a TG-CVI furnace according to the sequence from B to A according to the loading control configuration.
The thickness of the gasket is selected according to the following conditions: dividing the material into 3 intervals by taking the intermediate value of the designed volume density as a reference, and controlling the gasket as the following table 7:
TABLE 7
| Density (g/mm) 3 ) | Pad thickness (mm) |
| Below the median value | 1.3 |
| Intermediate value-1.40 | 0.7 |
| 1.4-1.42 | 0.5 |
The control parameters are that the master control temperature is 1040 ℃, and the upper, middle and lower temperature is not less than 920 ℃.
Temperature control mode: aeration starts to aerate deposition when the master temperature reaches 1040 ℃.
Introducing gas in a mass ratio: propylene: nitrogen =1, and propylene was fed at a ratio of gas flow volume per minute to total preform volume of 0.9.
The pressure of the third stage chemical vapor deposition is 0.60-1.2kPa, the deposition time is as follows: 48 hours
The bulk density of the material after the end of this stage fell to 1.39g/cm 3 -1.47g/cm 3 In between.
Step six heat treatment
The density obtained after the second stage of chemical vapor deposition is more than 1.42g/cm 3 And carrying out heat treatment on the carbon-carbon blank and the carbon-carbon blank subjected to the third-stage chemical vapor deposition. Post heat treatment machining 3
The size accounts for 20 percent of the total processing allowance, and the volume density of the preform body is reduced after peeling in the process, and the reduction amplitude is generally 0.02g/mm 3 -0.05g/mm 3 The larger the decrease of the density is. Bulk density measurement 3 the process is based on the dimensions after heat treatment and the weight of the green body of the material, and bulk density measurements are made, with a bulk density of 1.35g/cm 3 -1.45g/cm 3 The difference of the density distribution of the materials is less than 0.10g/cm 3 。
The bulk density of the sample plate is 1.36g/cm 3 The density distribution of the material was measured by local sampling as shown in Table 8 below.
TABLE 8
| Position of | Inner diameter | Pitch diameter | Outer diameter |
| Upper part of | 1.40g/cm 3 | 1.36g/cm 3 | 1.33g/cm 3 |
| In (1) | 1.39g/cm 3 | 1.34g/cm 3 | 1.32g/cm 3 |
| Lower part | 1.40g/cm 3 | 1.37g/cm 3 | 1.33g/cm 3 |
Step seven reaction infiltration of silicon
And (3) carrying out reaction, melting and siliconizing on the carbon-carbon porous body obtained by heat treatment to obtain the aviation carbon ceramic brake material.
The reaction melt infiltration is carried out in the argon atmosphere, the temperature of the reaction melt infiltration is 1550 ℃, the time of the reaction melt infiltration is 3h, and the pressure is 0.1-0.15MPa.
The carbon-carbon green body obtained in the embodiment 3 has the advantages that the size of the radius of the outer diameter of the deposited carbon growing around the carbon fiber is controlled within the range of 0.6-0.9 μm, and the densification of the siliconizing melting process is facilitated.
More than 80% of the material is in a rough layer structure from inside to outside, and plays an important role in the mechanical property, the frictional wear property and the heat-conducting property of the carbon-ceramic brake material.
The densities of the carbon porous body and the final product obtained in example 3 are shown in table 9:
TABLE 9
| Density (g/cm) of carbon blank 3 ) | Density after infiltration (g/cm) 3 ) |
| 1.35 | 2.18 |
| 1.42 | 2.19 |
| 1.40 | 2.19 |
| 1.38 | 2.19 |
In the inertia test, the deceleration rate is more than 3.05m/s 2 The brake curve with the dynamic friction coefficient of 0.27-0.37 has good performance, the average wear rate is about 0.45 mu m/time surface, and other technical indexes meet the requirements, so the brake shoe is already applied to a carbon-ceramic brake pair of an unmanned aerial vehicle.
Comparative example 1
The other conditions were the same as in example 1 except that the carbon fiber preforms were not numbered and were not charged according to the numbering convention. The uniformity of the batch density is not good, and the density is more than 1.50g/mm at most 3 。
Comparative example 2
The other conditions were the same as in example 1 except that the deposition temperature was kept constant at 1010 ℃ in three chemical vapor deposition processes. When the deposition temperature is less than 1020 ℃, the proportion of the rough layer is about 40-60%.
Comparative example 3
The other conditions were the same as in example 1, except that deposition was carried out at the temperature in CVD2 in three chemical vapor deposition processes. Density less than 1.35g/mm 3 The proportion is about 35 percent.
Comparative example 4
The other conditions were the same as in example 1, and the thickness of the gasket at CVD3 was 1.7mm. If the thickness of the gasket exceeds 1.6mm,1.38g/mm 3 -1.42g/mm 3 The green body is more than 1.45g/mm in the range 3 The probability of the surface tension is 80 percent and can reach 1.52g/mm at most 3 。
Claims (10)
1. A preparation method of an aviation carbon-ceramic brake material is characterized by comprising the following steps: the method comprises the steps of enabling the centers of N hollow disc-shaped carbon fiber preforms to penetrate through an internal heat source heater to be stacked to form a material column, placing the material column in a chemical vapor deposition furnace, controlling the distance between any two adjacent carbon fiber preforms to be 0.4-3.5mm, sealing the periphery of the upper end of the material column by using a hollow sealing material, enabling a gas outlet to be only located in the middle of the upper end of the material column, enabling at least 6 gas inlets to be uniformly arranged on the side face of the lower end of the material column, performing chemical vapor deposition by using propylene as a carbon source gas and nitrogen as a diluent gas, enabling the temperature of the chemical vapor deposition to be 1020-1100 ℃, enabling the temperature of the chemical vapor deposition to gradually decrease along with the increase of deposition time, forming a carbon blank after the chemical vapor deposition, obtaining a carbon porous body through heat treatment, and then performing ceramic treatment to obtain the aviation carbon ceramic brake material.
2. The preparation method of the aviation carbon-ceramic brake material as claimed in claim 1, wherein the preparation method comprises the following steps: the carbon fiber preform obtaining process comprises the following steps: alternately laminating the carbon fiber laid cloth and the carbon fiber mesh fabric, and carrying out continuous carbon fiber needling to obtain a carbon fiber preform, wherein the mass ratio of the carbon fiber laid cloth to the mesh fabric is 1;
the density of the carbon fiber preform is 0.45g/cm 3 -0.60g/cm 3 ；
The carbon fiber preform is subjected to heat treatment at 2100-2300 ℃ for 2-3h.
3. The preparation method of the aviation carbon-ceramic brake material as claimed in claim 1, wherein the preparation method comprises the following steps: the internal heat source heater is positioned in the center of the chemical vapor deposition furnace, and the chemical vapor deposition furnace is cylindrical;
the number of the air inlets is 6-10.
And during the chemical vapor deposition, controlling the temperature through 4 temperature measuring points, namely a main control temperature measuring point, an upper temperature measuring point, a middle temperature measuring point and a lower temperature measuring point respectively, wherein the main control temperature measuring point is axially positioned in the middle of the stock column and is 18-25mm away from the outer diameter of the inner heat source heater in the radial direction, the upper temperature measuring point is axially positioned at the upper part of the stock column and is radially positioned at the outer edge of the stock column, the middle temperature measuring point is axially positioned in the middle of the stock column and is radially positioned at the outer edge of the stock column, and the lower temperature measuring point is axially positioned at the lower part of the stock column and is radially positioned at the outer edge of the stock column.
4. The preparation method of the aviation carbon-ceramic brake material as claimed in claim 1, wherein the preparation method comprises the following steps: the chemical vapor deposition is divided into three sections, the temperature of the first section of chemical vapor deposition is 1060-1085 ℃, the temperature is firstly raised to 1080-1085 ℃, then the temperature is lowered to 1060-1065 ℃ at 15-22 ℃/80h, the time of the first section of chemical vapor deposition is controlled to be 80-110h, the pressure of the first section of chemical vapor deposition is 0.8-1.2kPa, the temperature of the second section of chemical vapor deposition is 1060-1040 ℃, the temperature is firstly raised to 1055-1060 ℃, then the temperature is lowered to 1040-1045 ℃ at 10-20 ℃/40h, the time of the second section of chemical vapor deposition is controlled to be 55-65h, the pressure of the second section of chemical vapor deposition is 0.60-1.2kPa, the temperature of the third section of chemical vapor deposition is constantly 1030-1040 ℃, the time of the third section of chemical vapor deposition is controlled to be 20-60h, and the pressure of the third section of chemical vapor deposition is 0.60-1.2kPa.
5. The preparation method of the aviation carbon-ceramic brake material as claimed in claim 4, wherein the preparation method comprises the following steps:
during the first-stage chemical vapor deposition, the mass ratio of propylene to nitrogen is 1.8-2.2, and the ratio of the total volume of propylene and nitrogen introduced per minute to the total volume of the carbon fiber preform is 1.2-1.3;
during the second-stage chemical vapor deposition, the mass ratio of propylene to nitrogen is 1.8-2.2, and the ratio of the total volume of propylene and nitrogen introduced per minute to the total volume of the carbon fiber preform is 1-1.1;
and during the third-stage chemical vapor deposition, the mass ratio of the propylene to the nitrogen is 1.8-2.2, and the ratio of the total volume of the propylene and the nitrogen introduced per minute to the total volume of the carbon fiber preform is 0.8-0.9.
6. The preparation method of the aviation carbon-ceramic brake material as claimed in claim 4, wherein the preparation method comprises the following steps: during loading of a first stage of chemical vapor deposition, N carbon fiber preforms are sequentially numbered from small to large or from large to small from bottom to top, the distance between any two adjacent carbon fiber preforms is controlled to be 2-3mm, during loading of a second stage of chemical vapor deposition, all carbon blanks are firstly divided into two sections from bottom to top, A, when the carbon fiber blanks are numbered in sequence from small to large during first chemical vapor deposition, the number of the section B is from middle to large, the number of the section A is from small to middle, when the carbon fiber blanks are numbered in sequence from large to small during first chemical vapor deposition loading, the number of the section B is from middle to small, the number of the section A is from large to middle, the distance between any two adjacent carbon fiber preforms is controlled to be 1.5-2.5mm during second chemical vapor deposition loading, and during loading of the chemical vapor deposition of a third stage, the carbon fiber blanks with the density of more than 1.42g/cm are firstly removed 3 Then dividing the rest M carbon-carbon blanks into two sections D and C from bottom to top, numbering the sections D and C from middle to big when the first chemical vapor deposition charging is carried out in sequence from small to big, and numbering the sections D and C from small to middleWhen the materials are numbered from large to small in sequence during the first chemical vapor deposition charging, the number of the D section is from middle to small, the number of the C section is from large to middle, and meanwhile, the distance between two adjacent carbon blanks with the density lower than the middle value is controlled to be 1.3-1.6mm, and the density is controlled to be between the middle value and 1.4g/cm 3 The space between two adjacent carbon-carbon blanks is 0.7-1.1mm, and the density is 1.4g/cm 3 The distance between the two adjacent carbon-carbon green bodies is 0.4-0.6mm.
7. The preparation method of the aviation carbon-ceramic brake material as claimed in claim 4, wherein the preparation method comprises the following steps: the volume density of the carbon-carbon blank obtained after the first-stage chemical vapor deposition is 0.85g/mm 3 -1.15g/mm 3 The volume density of the carbon-carbon blank obtained after the second-stage chemical vapor deposition is 1.25g/mm 3 -1.45g/mm 3 The volume density of the carbon-carbon blank obtained after the third-stage chemical vapor deposition is 1.38g/cm 3 -1.48g/cm 3 。
8. The preparation method of the aviation carbon-ceramic brake material as claimed in claim 1, wherein the preparation method comprises the following steps: the temperature of the heat treatment is 2000-2100 ℃, and the time of the heat treatment is 1-3h;
the density of the carbon-carbon porous body is 1.35g/cm 3 -1.45g/cm 3 。
9. The preparation method of the aviation carbon-ceramic brake material as claimed in claim 1, wherein the preparation method comprises the following steps: the ceramic treatment mode is reaction melting siliconizing, the reaction melting siliconizing is carried out in an argon atmosphere, the temperature of the reaction melting siliconizing is 1550-1650 ℃, the time of the reaction melting siliconizing is 2-4h, and the pressure is 0.1-0.15Pa.
10. An aviation carbon-ceramic brake material prepared by the preparation method of any one of claims 1 to 9.
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Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5916633A (en) * | 1995-05-19 | 1999-06-29 | Georgia Tech Research Corporation | Fabrication of carbon/carbon composites by forced flow-thermal gradient chemical vapor infiltration |
| CN1350959A (en) * | 2000-10-27 | 2002-05-29 | 西安兰空航空设备公司 | Method and equipment for high-speed gas-phase carbon deposition of braking carbon disk for aircraft |
| TW526544B (en) * | 2002-01-28 | 2003-04-01 | Taiwan Semiconductor Mfg | Method for increasing uniformity of thickness of chemical vapor phase deposition |
| KR20050113090A (en) * | 2004-05-28 | 2005-12-01 | 주식회사 데크 | The method of producing carbon fiber reinforced ceramic matrix composites |
| RU2014115831A (en) * | 2014-04-18 | 2015-10-27 | Открытое Акционерное Общество "Уральский научно-исследовательский институт композиционных материалов" | CARBON-CARBON COMPOSITE MATERIAL AND METHOD FOR PRODUCING FROM IT |
| CN107445638A (en) * | 2016-10-12 | 2017-12-08 | 平顺县西沟龙鼎新材料科技有限公司 | A kind of preparation method of carbon/carbon brake disc |
| CN109400198A (en) * | 2018-12-13 | 2019-03-01 | 上海康碳复合材料科技有限公司 | A kind of carbon/carbon (pottery) composite material brake disc Preparation equipment and preparation method thereof based on quick sedimentation process |
| CN111348931A (en) * | 2020-03-26 | 2020-06-30 | 孚迪斯石油化工（葫芦岛）有限公司 | Gas phase permeation method for annular carbon/carbon composite material |
| CN112624780A (en) * | 2020-11-12 | 2021-04-09 | 湖南世鑫新材料有限公司 | Method for intelligently controlling CVI densified carbon fiber preform in efficient and low-cost matching manner |
| CN112830807A (en) * | 2021-03-19 | 2021-05-25 | 中南大学 | Vapor deposition device and preparation method of carbon/carbon composite material |
-
2022
- 2022-10-14 CN CN202211257275.4A patent/CN115536419B/en active Active
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5916633A (en) * | 1995-05-19 | 1999-06-29 | Georgia Tech Research Corporation | Fabrication of carbon/carbon composites by forced flow-thermal gradient chemical vapor infiltration |
| CN1350959A (en) * | 2000-10-27 | 2002-05-29 | 西安兰空航空设备公司 | Method and equipment for high-speed gas-phase carbon deposition of braking carbon disk for aircraft |
| TW526544B (en) * | 2002-01-28 | 2003-04-01 | Taiwan Semiconductor Mfg | Method for increasing uniformity of thickness of chemical vapor phase deposition |
| KR20050113090A (en) * | 2004-05-28 | 2005-12-01 | 주식회사 데크 | The method of producing carbon fiber reinforced ceramic matrix composites |
| RU2014115831A (en) * | 2014-04-18 | 2015-10-27 | Открытое Акционерное Общество "Уральский научно-исследовательский институт композиционных материалов" | CARBON-CARBON COMPOSITE MATERIAL AND METHOD FOR PRODUCING FROM IT |
| CN107445638A (en) * | 2016-10-12 | 2017-12-08 | 平顺县西沟龙鼎新材料科技有限公司 | A kind of preparation method of carbon/carbon brake disc |
| CN109400198A (en) * | 2018-12-13 | 2019-03-01 | 上海康碳复合材料科技有限公司 | A kind of carbon/carbon (pottery) composite material brake disc Preparation equipment and preparation method thereof based on quick sedimentation process |
| CN111348931A (en) * | 2020-03-26 | 2020-06-30 | 孚迪斯石油化工（葫芦岛）有限公司 | Gas phase permeation method for annular carbon/carbon composite material |
| CN112624780A (en) * | 2020-11-12 | 2021-04-09 | 湖南世鑫新材料有限公司 | Method for intelligently controlling CVI densified carbon fiber preform in efficient and low-cost matching manner |
| CN112830807A (en) * | 2021-03-19 | 2021-05-25 | 中南大学 | Vapor deposition device and preparation method of carbon/carbon composite material |
Non-Patent Citations (1)
| Title |
|---|
| 汤中华等: "用CVI增密技术制备航空刹车用C/C复合材料", 《中南工业大学学报(自然科学版)》 * |
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