CN115536419B - 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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- CN115536419B CN115536419B CN202211257275.4A CN202211257275A CN115536419B CN 115536419 B CN115536419 B CN 115536419B CN 202211257275 A CN202211257275 A CN 202211257275A CN 115536419 B CN115536419 B CN 115536419B
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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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 stacking N hollow disc-shaped carbon fiber preforms through an internal heat source heater to form a material column, placing the material column in a chemical vapor deposition furnace, controlling the interval 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 positioned in the middle of the upper end of the material column, uniformly arranging at least 6 air inlets on the side surface of the lower end of the material column, taking propylene as carbon source gas, taking nitrogen as diluent gas, performing chemical vapor deposition, wherein the temperature of the chemical vapor deposition is 1020-1100 ℃, the temperature of the chemical vapor deposition gradually decreases along with the increase of deposition time, forming a carbon blank after the chemical vapor deposition, obtaining a carbon-carbon porous body through heat treatment, and performing 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 aviation carbon ceramic brake material mostly adopts a C/C composite material as a matrix, the density control, pore distribution and material microstructure of the matrix can directly influence the performance of an aviation carbon ceramic brake pair, and carbon ceramic materials with larger performance difference, such as small friction coefficient, abnormal friction curve under load and the like, can be obtained under the same siliconizing process condition by different carbon ceramic brake material matrix structures, which is also a main reason that many carbon ceramic brake materials cannot be directly applied to aviation brake materials.
Disclosure of Invention
Aiming at the defects of the prior art, the first aim 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, wherein the density of the obtained aviation carbon ceramic brake material can reach 2.20g/cm at most 3 The braking curve is good, the abrasion is low,
in order to achieve the above purpose, the present 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 stacking N hollow disc-shaped carbon fiber preforms through an internal heat source heater to form a material column, placing the material column in a chemical vapor deposition furnace, controlling the interval 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 positioned in the middle of the upper end of the material column, uniformly arranging at least 6 air inlets on the side surface of the lower end of the material column, taking propylene as carbon source gas and nitrogen as diluent gas, performing chemical vapor deposition, wherein the temperature of the chemical vapor deposition is 1020-1100 ℃, the temperature of the chemical vapor deposition gradually decreases along with the increase of deposition time, forming a carbon-carbon blank after the chemical vapor deposition, performing heat treatment to obtain a carbon-carbon porous body, and performing ceramic treatment to obtain the aviation carbon ceramic brake material.
The preparation method of the invention adopts a resistance heating mode, stacks the carbon fiber prefabricated bodies through an internal heat source heater, controls the interval between any adjacent carbon fiber prefabricated bodies to be 0.4-3.5mm, forms an inner ring and an outer ring space, seals the upper end of a material column by adopting a hollow sealing material, ensures that an air outlet is arranged in the middle of the upper end of the material column, and an air inlet is uniformly arranged on the side surface of the lower end of the material column, so that the carbon fiber prefabricated bodies form a thermal gradient from inside to outside, in the chemical deposition process, propylene is used as carbon source gas, the chemical vapor deposition temperature gradually decreases along with the deposition process, and finally, a carbon matrix, uniformly distributed holes and almost through-hole structure can be formed, so that the density of the aviation carbon ceramic brake material obtained after the ceramic treatment is realizedUp to 2.20g/cm 3 Meanwhile, more than 80% of the material is of a coarse layer structure from inside to outside, and plays an important role in the mechanical property, friction and wear performance and heat conduction performance of the carbon ceramic brake material.
Preferably, the carbon fiber preform obtaining process includes: the carbon fiber non-woven cloth and the carbon fiber mesh fabric are alternately laminated, and the carbon fiber preform is obtained by continuous carbon fiber needling, wherein the mass ratio of the carbon fiber non-woven cloth to the mesh fabric is 1:0.20-0.30, and the interlayer density of the carbon fiber non-woven cloth is 10-16 layers/cm.
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 2-3 hours.
According to the invention, 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 pyrolytic carbon and the carbon fiber is increased in the late 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 at the center of the chemical vapor deposition furnace, and the chemical vapor deposition furnace is cylindrical.
Preferably, the number of the air inlets is 6-10, preferably 8. The inventors found that the number of air inlets is controlled to be within this preferred range and that the final deposition effect is optimal.
In the preferred scheme, during chemical vapor deposition, temperature control is performed 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 located in the middle of the material column and is 18-25mm away from the outer diameter of the internal heat source heater in the radial direction, the upper temperature measuring point is axially located in the upper part of the material column and is radially located at the outer edge of the material column, the middle temperature measuring point is axially located in the middle of the material column and is radially located at the outer edge of the material column, and the lower temperature measuring point is axially located at the lower part of the material column and is radially located at the outer edge of the material 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.
In a preferred scheme, the chemical vapor deposition is divided into three sections, wherein the temperature of the first section is 1060-1085 ℃, the temperature is firstly increased to 1080-1085 ℃, then the temperature is reduced to 1060-1065 ℃ at 15-22 ℃/80h, the time of the first section is controlled to 80-110h, the pressure of the first section is 0.8-1.2kPa, the temperature of the second section is 1060-1040 ℃, the temperature is firstly increased to 1055-1060 ℃, then the temperature is reduced to 1040-1045 ℃ at 10-20 ℃/40h, the time of the second section is controlled to 55-65h, the pressure of the second section is controlled to 0.60-1.2kPa, the temperature of the third section is constant to 1030-1040 ℃, the time of the third section is controlled to 20-60h, and the pressure of the third section is 0.60-1.2kPa.
In the actual operation , the temperature of the chemical vapor deposition is the temperature of the main control temperature measuring point, when the main control temperature measuring point reaches the set temperature of the chemical vapor deposition, the gas is introduced to deposit at the beginning, and the temperatures of the upper temperature measuring point, the middle temperature measuring point and the lower temperature measuring point at 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 taken as a nitrogen source and nitrogen is taken as diluent gas in all three stages of chemical vapor deposition, then the temperature gradient of the three stages is controlled within the range, and the processing time of the three stages is coordinated, so that the deposition is uniform, almost all pores are through holes, the efficiency of the post-ceramic treatment is greatly improved, the final density of the final aviation carbon ceramic brake material is improved, more than 80% of carbon is in a coarse 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 silicon carbide is better and effectively supported, so that the abrasion is reduced to the minimum under the coordination of the structure.
Further preferably, during the first stage chemical vapor deposition, the mass ratio of propylene to nitrogen is 1.8-2.2:3, and the total volume ratio of the total carbon fiber preform into which propylene and nitrogen are introduced per minute is 1.2-1.3:1.
Further preferably, during the second stage chemical vapor deposition, the mass ratio of propylene to nitrogen is 1.8-2.2:3, and the total volume ratio of the total carbon fiber preform into which propylene and nitrogen are introduced per minute is 1-1.1:1.
Further preferably, during the third stage chemical vapor deposition, the mass ratio of propylene to nitrogen is 1:1.8-2.2, and the total volume ratio of the total carbon fiber preform into which propylene and nitrogen are introduced per minute is 0.8-0.9:1.
In the three-stage deposition process, the flow rates of the carbon source gas and the nitrogen are controlled within the above preferred ranges, and the structure of the finally obtained carbon matrix is optimal.
Further preferably, in the 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, and the interval between any two adjacent carbon fiber preforms is controlled to be 2-3mm, in the second stage of chemical vapor deposition, all carbon preforms are first divided into two sections B and a from bottom to top, in the first stage of chemical vapor deposition, the number of the section B is from the middle to large, the number of the section a is from the small to the middle, in the first stage of chemical vapor deposition, the number of the section B is from the middle to small, in the number of the section a is from the large to the middle, in the second stage of chemical vapor deposition, the interval between any two adjacent carbon fiber preforms is controlled to be 1.5-2.5mm, and in the third stage of chemical vapor deposition, the density is removed to be greater than 1.42g/cm 3 Dividing the M carbon blanks into two sections D and C from bottom to top, numbering the section D from middle to large when the chemical vapor deposition is carried out in sequence from large to small when the chemical vapor deposition is carried out for the first time, numbering the section C from small to small when the chemical vapor deposition is carried out for the first time, numbering the section D from large to small when the chemical vapor deposition is carried out in sequence from large to small when the chemical vapor deposition is carried out for the first time, numbering the section C from large to small, and simultaneously controlling the interval between two adjacent carbon blanks with the density lower than the intermediate value to be 1.3-1.6mm and the density to be between the intermediate value and 1.4g/cm 3 Adjacent to each otherThe distance between two carbon bodies is 0.7-1.1mm, and the density is 1.4g/cm 3 The spacing between the two adjacent carbon-carbon green bodies is 0.4-0.6mm.
The inventor finds that the thickness of the gasket is controlled in the mode according to the numbering mode, so that the density of a single carbon-carbon blank body can be uniform, the density among different carbon-carbon blank bodies can also keep very high uniformity, particularly, the thickness of the gasket is controlled in the third chemical vapor deposition process, the distribution and popularity control effect of a convection field is obvious, the thickness densification speed is high, and the densification speed is low relative to the thickness of the gasket, so that the uniformity of the density of a material can be controlled.
In the actual operation process, the carbon blank obtained after the first stage of chemical vapor deposition is subjected to first machining, the surface of the blank is machined and peeled, the dimension is controlled to be about 50% of the total machining allowance, the second stage of chemical vapor deposition is carried out, the surface of the blank is machined and peeled, the dimension is about 30% of the total machining allowance, the volume density of the blank body of the preform is reduced after the process of peeling, and the maximum reduction 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 is subjected to third machining, wherein the dimension accounts for 20 percent of the total machining allowance, and the volume density of the carbon blank is reduced, and the reduction is generally 0.03g/mm after peeling 3 -0.05g/mm 3 The greater the density is reduced.
Preferably, the volume density of the 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 section of chemical vapor deposition is 1.38g/cm 3 -1.48g/cm 3 。
In a preferred scheme, the temperature of the heat treatment is 2000-2100 ℃, and the time of the heat treatment is 1-3h.
Further preferably, the density obtained after the second stage chemical vapor deposition is greater than 1.42g/cm 3 Carbon blank of (2) and after the third stage chemical vapor depositionIs subjected to heat treatment.
Preferably, the density of the carbon-carbon porous body is 1.35g/cm 3 -1.45g/cm 3 。
In a preferred scheme, the ceramic treatment mode is reactive infiltration siliconizing, the reactive infiltration siliconizing is carried out under the argon atmosphere, the temperature of the reactive infiltration siliconizing is 1550-1650 ℃, the time of the reactive infiltration siliconizing is 2-4h, and the pressure is 0.1-0.15Pa.
The aviation carbon ceramic brake material prepared by the preparation method disclosed by the invention is prepared.
Principle and advantages
According to the preparation method of the aviation carbon ceramic brake material, through the design and manufacture of a prefabricated body, the heat treatment of a process, the processing design of the process, the design of a charging mode by using a TG-CVI (glass fiber reinforced composite metal composite) process method, the design control of a process temperature field, the design of a flow field distribution, the design of a pressure design and the like, the effective control of the void distribution, the density control and the microstructure of a matrix material structure is realized, the matrix material obtained after mechanical processing is subjected to the technological processes of a siliconizing process and the like, and a carbon ceramic brake pair is obtained after the technological processes of the material index test, the inertia table test and the like, so that the requirements of a certain model of unmanned aircraft on various indexes of brake performance are met, and the preparation method is practically applied to a certain model of unmanned aircraft carbon ceramic brake pair.
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. The method of the invention adjusts CVI time and gasket thickness during charging to control the bulk density of the material, effectively ensures the density qualification rate of the densified preform, increases the consistency and stability of material preparation, and finally can control the material to be 1.35g/cm 3 -1.45g/cm 3 Between them. 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, the deposition rate in the deposition process is controlled by gradually decreasing the main control temperature in the CVI process, and the pore formation form and the sealing degree of the material are controlled. The microstructure of the material shows that the outer diameter radius of the deposited carbon growing around the carbon fiber is controlled within the range of 0.6-0.9 mu m, which is favorable for the formation of through holes in pores and densification of siliconizing fusion process.
4. The material structure is controlled by the temperature, flow and pressure of the CVI process, and more than 80% of the carbon material is of a coarse layer structure from inside to outside, so that the carbon ceramic brake material plays an important role in the mechanical property, friction and wear performance and heat conduction performance.
5. The material has strong infiltration capacity: the density of the material after subsequent siliconizing can reach 2.20g/cm at most 3 。
6. The aviation carbon ceramic brake material provided by the invention has the mechanical property, the heat conduction property and the dynamic friction coefficient which all meet the brake performance requirement of a certain 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 brake curve has good performance, the average wear rate is about 0.42 mu m/time per surface, and other technical indexes meet the requirements, and the brake curve has been applied to a carbon ceramic brake pair of a certain unmanned aerial vehicle.
Drawings
FIG. 1, schematic diagram of a material column, thermal field, flow field of chemical vapor deposition.
FIG. 2 shows a microstructure of the carbon body obtained in example 1.
FIG. 3 shows a microstructure of the carbon body obtained in example 1.
FIG. 4 shows a microstructure of the carbon body obtained in example 1.
Fig. 5, an unmanned aerial vehicle carbon ceramic brake byproduct assembled from the aviation carbon ceramic brake material obtained in example 1.
Detailed Description
In the following embodiment, 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 an air inlet, the air inlet is distributed at the lower end of the cylinder and is uniformly distributed at eight points based on the side area of the cylinder at the lower end, and the air inlet is positioned at the upper end of the material column and is sealed by adopting a sealing material, so that the air flow direction of the material column is shown in fig. 1.
The inner diameter adopts a resistance heating mode, and the center of the carbon fiber preform passes through an internal heat source heater to be stacked, so that an inner ring and an outer ring space are formed, and the preform forms a thermal gradient from inside to outside.
The temperature field is monitored by a 4-point temperature control method during charging and is divided into main control temperatures, upper, middle and lower temperatures are monitored, and the measuring positions are as follows: the main control temperature measuring position is positioned at the middle position of the material column which is 20mm away from the outer diameter of the heater. The upper temperature measuring position is monitored and located at the outer edge of the material column, and the lower temperature measuring position is monitored and located at the middle end of the material column. The temperature measuring position under the control is located at the outer edge of the material column and at the lowest end of the material column. The temperature control structure is beneficial to monitoring the temperature field and guaranteeing the effective operation of the CVI process.
Example 1
Step one, preparation of carbon fiber preform
Alternately laminating carbon fiber non-woven cloth and carbon fiber mesh fabric, and performing continuous carbon fiber needling to obtain a carbon fiber preform, wherein the mass ratio of the carbon fiber non-woven cloth to the mesh fabric is controlled to be 1:0.20-0.30, the interlayer density of the carbon fiber non-woven cloth is 14 layers/cm, and the density is 0.45g/cm 3 -0.60g/cm 3 The size isIs a carbon fiber preform of (a).
Step two high temperature heat treatment
And (3) carrying out heat treatment on the carbon fiber preform under the vacuum condition at the temperature of 2100 ℃ for 3 hours.
Step three CVD1
And loading 16 carbon fiber preforms, and loading the preforms into a TG-CVI furnace according to the number of 1-16 from small to large. The thickness of the spacer was controlled to 2.5mm.
The process control parameters are that the main control temperature is 1060-1080 ℃, and the upper, middle and lower temperatures are monitored to be more than or equal to 900 ℃.
The temperature control mode is as follows: and (3) ventilation is carried out when the main control temperature reaches 1080 ℃, and the temperature is reduced to 1060 ℃ according to the temperature reduction of 20 ℃/80 hours in the deposition process. And (3) introducing gas mass ratio: propylene: nitrogen = 2:3, on per minuteThe ratio of the inlet gas flow volume to the total preform volume was 1.2. The pressure is 0.80-1.2kPa during the first stage chemical vapor deposition, and the deposition time is as follows: and 100 hours. The density of the blank of the material after the stage is finished is 0.85g/mm 3 -1.1g/mm 3 Between them. Machining and peeling the surface of the blank, controlling the size to be about 50% of the total machining allowance, measuring the volume density according to the machined size and the weight of the measured material blank, and measuring the volume density to be 0.85g/mm 3 -1.15g/mm 3 Between them.
Step four CVD2
Dividing the blank body after machining 1 into A/B sections with the number of 1 to 8 and the number of 9 to 16 according to the number of the sections from small to large, and loading the prefabricated body into a TG-CVI furnace according to the sequence from B to A (the sequence of 9 to 16 and 1 to 8 in turn) according to the loading control configuration.
The thickness of the spacer was controlled to 2.0mm.
The control parameters are that the main control temperature is 1060-1040 ℃, and the upper, middle and lower temperatures are more than or equal to 920 ℃ after monitoring.
The temperature control mode is as follows: ventilation deposition is started when the main control temperature reaches 1060 ℃, and the temperature is reduced to 1040 ℃ according to the temperature reduction of 20 ℃/40 hours.
And (3) introducing gas mass ratio: propylene: nitrogen=2:3, 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 which are located
Machining 2, removing the skin on the surface, wherein the size of the skin accounts for about 30% of the total machining allowance. After the peeling process, the volume density of the preform body is reduced, and the maximum reduction is 0.04g/mm 3 The higher the density, the greater the drop in amplitude.
Bulk Density measurement 2
The process is based on the processing size and the weight of the measured material blank, and the bulk density is measured if the bulk density is more than 1.42g/cm 3 Then the process is shifted to a heat treatment process.
Step five CVD3
And (3) dividing the machined 2-step preform into A/B sections from small to large, wherein the A section is from small to medium, the B section is from medium to large, and the preform is loaded into a TG-CVI furnace according to the sequence from B to A according to a loading control configuration.
The thickness of the gasket is selected according to the following steps: based on the intermediate value of the designed bulk density of the material, the material is divided into 3 sections, and the control conditions of the gaskets are shown in the following table 1:
TABLE 1
| Density (g/mm) 3 ) | Thickness of gasket (mm) |
| Below the intermediate value | 1.5 |
| Intermediate value-1.40 | 0.8 |
| 1.4-1.42 | 0.5 |
The control parameters are that the main control temperature is 1040 ℃, and the upper, middle and lower temperatures are more than or equal to 920 ℃ after monitoring.
The temperature control mode is as follows: aeration starts aeration deposition when the main control temperature reaches 1040 ℃.
And (3) introducing gas mass ratio: propylene: nitrogen=1:2, the ratio of the volume of gas flow per minute to the total preform volume introduced by propylene was 0.9.
The pressure of the third stage chemical vapor deposition is 0.60-1.2kPa, and the deposition time is as follows: 38 hours
The bulk density of the material at the end of this stage falls at 1.38g/cm 3 -1.48g/cm 3 Between them.
Step six heat treatment
The density obtained after the second stage of chemical vapor deposition is more than 1.42g/cm 3 And (3) carrying out heat treatment on the carbon blank body subjected to the third-stage chemical vapor deposition. Machining 3 after heat treatment
The size accounts for 20 percent of the total processing allowance, and after peeling, the volume density of the preform body is reduced, and the width is generally reduced to 0.03g/mm 3 -0.05g/mm 3 The greater the density is reduced. Bulk Density measurement 3 bulk Density measurement was performed according to the size after heat treatment and the weight of the measured material blank, with a bulk Density of 1.35g/cm 3 -1.45g/cm 3 The difference of the density distribution of the material is less than 0.10g/cm 3 。
The bulk density of the sample tray is 1.39g/cm 3 The material density distribution is shown in Table 2 below by means of local sampling.
TABLE 2
| Position of | Inner diameter of | Pitch diameter | Outer diameter of |
| Upper part | 1.41g/cm 3 | 1.40g/cm 3 | 1.37g/cm 3 |
| In (a) | 1.39g/cm 3 | 1.39g/cm 3 | 1.37g/cm 3 |
| Lower part(s) | 1.42g/cm 3 | 1.40g/cm 3 | 1.38g/cm 3 |
Step seven, reaction and siliconizing
And (3) carrying out reactive fusion siliconizing on the carbon-carbon porous body obtained by heat treatment to obtain the aviation carbon ceramic brake material.
The reaction and the infiltration are carried out under the argon atmosphere, the temperature of the reaction and the infiltration is 1600 ℃, the time of the reaction and the infiltration is 4 hours, and the pressure is 0.1-0.15MPa.
The carbon-carbon green body obtained in this example 1, from the outer diameter radius size of the deposited carbon grown around the carbon fiber shown in fig. 2, was controlled to be in the range of 0.6 μm to 0.9 μm, which is advantageous for the formation of through holes in pores and for densification of siliconizing fusion process.
More than 80% of the materials shown in fig. 3 and 4 are of coarse layer structures from inside to outside, and play an important role in the mechanical property, friction and wear property and heat conduction property of the carbon ceramic brake material.
The densities of the carbon-carbon porous body and the final product obtained in this example 1 are shown in table 3:
TABLE 3 Table 3
| Density (g/cm) of carbon green body 3 ) | Density after infiltration (g/cm) 3 ) |
| 1.37 | 2.20 |
| 1.40 | 2.20 |
| 1.40 | 2.19 |
| 1.39 | 2.18 |
In inertial test, the deceleration rate is more than 3.05m/s 2 The dynamic friction coefficient is 0.29-0.37, the brake curve has good performance, the average wear rate is about 0.42 mu m/time per surface, and other technical indexes meet the requirements, and the brake curve has been applied to a carbon ceramic brake pair of a certain unmanned aerial vehicle.
Example 2
Step one, preparation of carbon fiber preform
Alternately laminating carbon fiber non-woven cloth and carbon fiber mesh fabric, and performing continuous carbon fiber needling to obtain a carbon fiber preform, wherein the mass ratio of the carbon fiber non-woven cloth to the mesh fabric is controlled to be 1:0.20-0.30, the interlayer density of the carbon fiber non-woven cloth is 15 layers/cm, and the density is 0.45g/cm 3 -0.60g/cm 3 The size isIs a carbon fiber preform of (a).
Step two high temperature heat treatment
The carbon fiber preform was heat-treated at a temperature of 2200 c for 2.5 hours under vacuum.
Step three CVD1
And charging 18 carbon fiber preforms, and charging the preforms into a TG-CVI furnace according to the number of 1-18 from small to large. The thickness of the spacer was controlled to 2.5mm.
The process control parameters are that the main control temperature is 1060-1080 ℃, and the upper, middle and lower temperatures are monitored to be more than or equal to 900 ℃.
Temperature (temperature)The control mode is as follows: and (3) ventilation is carried out when the main control temperature reaches 1085 ℃, and the temperature is reduced to 1065 ℃ according to the temperature reduction of 20 ℃/80 hours in the deposition process. And (3) introducing gas mass ratio: propylene: nitrogen=2:3, the ratio of the gas flow volume per minute to the total preform volume was 1.2. The pressure is 0.8-1.2kPa during the first stage chemical vapor deposition, and the deposition time is as follows: 80 hours. The density of the blank body of the material after the stage is finished is 0.90g/mm 3 -1.15g/mm 3 Between them. Machining and peeling the surface of the blank, controlling the size to be about 50% of the total machining allowance, measuring the volume density according to the machined size and the weight of the measured material blank, and measuring the volume density to be 0.90g/mm 3 -1.14g/mm 3 Between them.
Step four CVD2
The carbon and carbon after machining 1 is equally divided into A/B sections from small to large, the A sections are numbered 1 to 9, the B sections are numbered 10 to 18, and the prefabricated body is filled into a TG-CVI furnace according to the sequence from B to A (the sequence 10-19 and 1-9 in sequence) according to the charge control configuration.
The thickness of the spacer was controlled to 2.0mm.
The control parameters are that the main control temperature is 1060-1040 ℃, and the upper, middle and lower temperatures are more than or equal to 920 ℃ after monitoring.
The temperature control mode is as follows: aeration deposition is started when the main control temperature reaches 1065 ℃, and the temperature is reduced to 1040 ℃ according to the temperature reduction of 20 ℃/40 hours.
And (3) introducing gas mass ratio: propylene: nitrogen=2:3, 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 which are located
Machining 2, removing the skin on the surface, wherein the size of the skin accounts for about 30% of the total machining allowance. After the peeling process, the volume density of the preform body is reduced, and the maximum reduction is 0.04g/mm 3 The higher the density, the greater the drop in amplitude.
Bulk Density measurement 2
The process is based on the dimensions of the work and the measurement of the material blankBody weight, bulk density measurement, if the bulk density is greater than 1.42g/cm 3 Then the process is shifted to a heat treatment process.
Step five CVD3
And (3) dividing the machined 2-step preform into A/B sections from small to large, wherein the A section is from small to medium, the B section is from medium to large, and the preform is loaded into a TG-CVI furnace according to the sequence from B to A according to a loading control configuration.
The thickness of the gasket is selected according to the following steps: based on the intermediate value of the designed bulk density of the material, the material is divided into 3 sections, and the control conditions of the gaskets are shown in the following table 4:
TABLE 4 Table 4
The control parameters are that the main control temperature is 1040 ℃, and the upper, middle and lower temperatures are more than or equal to 920 ℃ after monitoring.
The temperature control mode is as follows: aeration starts aeration deposition when the main control temperature reaches 1040 ℃.
And (3) introducing gas mass ratio: propylene: nitrogen=1:2, the ratio of the volume of gas flow per minute to the total preform volume introduced by propylene was 0.9.
The pressure of the third stage chemical vapor deposition is 0.60-1.2kPa, and the deposition time is as follows: for 28 hours
The bulk density of the material at the end of this stage falls at 1.39g/cm 3 -1.47g/cm 3 Between them.
Step six heat treatment
The density obtained after the second stage of chemical vapor deposition is more than 1.42g/cm 3 And (3) carrying out heat treatment on the carbon blank body subjected to the third-stage chemical vapor deposition. Machining 3 after heat treatment
The size accounts for 20 percent of the total processing allowance, the volume density of the preform body is reduced after peeling, and the width is generally reduced to 0.02g/mm 3 -0.05g/mm 3 The greater the density is reduced. Bulk Density measurement 3 bulk Density measurement was performed according to the size after heat treatment and the weight of the measured material blank, with a bulk Density of 1.35g/cm 3 -1.45g/cm 3 The difference of the density distribution of the material is less than 0.10g/cm 3 。
The bulk density of the sample tray is 1.43g/cm 3 The material density distribution was measured by local sampling as shown in table 5 below.
TABLE 5
Step seven, reaction and siliconizing
And (3) carrying out reactive fusion siliconizing on the carbon-carbon porous body obtained by heat treatment to obtain the aviation carbon ceramic brake material.
The reaction and the infiltration are carried out under the argon atmosphere, the temperature of the reaction and the infiltration is 1650 ℃, the time of the reaction and the infiltration is 2 hours, and the pressure is 0.1-0.15MPa.
The carbon-carbon green body obtained in this example 2, in which the outer diameter radius of the deposited carbon grown around the carbon fiber was controlled within the range of 0.7 μm to 0.9. Mu.m, was advantageous for densification of the siliconizing fusion process.
The material has a coarse layer structure with more than 83% from inside to outside, and plays an important role in the mechanical property, friction and wear property and heat conduction property of the carbon ceramic brake material.
The densities of the carbon-carbon porous body and the final product obtained in this example 2 are shown in table 6:
TABLE 6
| Density of charcoal green bodyg/cm 3 ) | Density after infiltration (g/cm) 3 ) |
| 1.38 | 2.19 |
| 1.42 | 2.20 |
| 1.40 | 2.19 |
| 1.37 | 2.18 |
In inertial test, the deceleration rate is more than 3.05m/s 2 The dynamic friction coefficient is 0.28-0.36, the brake curve has good performance, the average wear rate is about 0.43 mu m/time per surface, and other technical indexes meet the requirements, and the dynamic friction coefficient is already applied to a carbon ceramic brake pair of a certain unmanned aerial vehicle.
Example 3
Step one, preparation of carbon fiber preform
Alternately laminating carbon fiber non-woven cloth and carbon fiber mesh fabric, and performing continuous carbon fiber needling to obtain a carbon fiber preform, wherein the mass ratio of the carbon fiber non-woven cloth to the mesh fabric is controlled to be 1:0.20-0.30, the interlayer density of the carbon fiber non-woven cloth is 15 layers/cm, and the density is 0.45g/cm 3 -0.60g/cm 3 The size isIs a carbon fiber preform of (a).
Step two high temperature heat treatment
And (3) carrying out heat treatment on the carbon fiber preform under the vacuum condition at the temperature of 2300 ℃ for 2 hours.
Step three CVD1
And charging 20 carbon fiber preforms, and charging the preforms into a TG-CVI furnace according to the number of 1-20 from small to large. The thickness of the spacer was controlled to 2.5mm.
The process control parameters are that the main control temperature is 1060-1080 ℃, and the upper, middle and lower temperatures are monitored to be more than or equal to 900 ℃.
The temperature control mode is as follows: and (3) ventilation is started when the main control temperature reaches 1083 ℃, and the temperature is reduced to 1063 ℃ according to the temperature reduction of 20 ℃/80 hours in the deposition process. And (3) introducing gas mass ratio: propylene: nitrogen=2:3, the ratio of the gas flow volume per minute to the total preform volume was 1.2. The pressure is 0.8-1.2kPa during the first stage chemical vapor deposition, and the deposition time is as follows: and 110 hours. The density of the blank of the material after the stage is finished is 0.92g/mm 3 -1.18g/mm 3 Between them. Machining and peeling the surface of the blank, controlling the size to be about 50% of the total machining allowance, measuring the volume density according to the machined size and the weight of the measured material blank, and measuring the volume density to be 0.93g/mm 3 -1.17g/mm 3 Between them.
Step four CVD2
The carbon and carbon after machining 1 is equally divided into A/B sections from small to large according to the number, the A sections are numbered from 1 to 9, the B sections are numbered from 10 to 18, and the prefabricated body is filled into a TG-CVI furnace according to the sequence from B to A (the sequence 11-20 and 1-10 in turn) according to the charge control configuration.
The thickness of the spacer was controlled to 2.0mm.
The control parameters are that the main control temperature is 1060-1040 ℃, and the upper, middle and lower temperatures are more than or equal to 920 ℃ after monitoring.
The temperature control mode is as follows: aeration deposition is started when the main control temperature reaches 1063 ℃, and the temperature is reduced to 1040 ℃ according to the temperature reduction of 20 ℃/40 hours.
And (3) introducing gas mass ratio: propylene: nitrogen=2:3, 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 which are located
Machining 2, removing skin on the surface, and making the size about 30% of the total machining allowance. After the peeling process, the volume density of the preform body is reduced, and the maximum reduction is 0.05g/mm 3 The higher the density, the greater the drop in amplitude.
Bulk Density measurement 2
The process is based on the processing size and the weight of the measured material blank, and the bulk density is measured if the bulk density is more than 1.42g/cm 3 Then the process is shifted to a heat treatment process.
Step five CVD3
And (3) dividing the machined 2-step preform into A/B sections from small to large, wherein the A section is from small to medium, the B section is from medium to large, and the preform is loaded into a TG-CVI furnace according to the sequence from B to A according to a loading control configuration.
The thickness of the gasket is selected according to the following steps: based on the intermediate value of the designed bulk density of the material, the material is divided into 3 sections, and the control conditions of the gaskets are shown in the following table 7:
TABLE 7
| Density (g/mm) 3 ) | Thickness of gasket (mm) |
| Below the intermediate value | 1.3 |
| Intermediate value-1.40 | 0.7 |
| 1.4-1.42 | 0.5 |
The control parameters are that the main control temperature is 1040 ℃, and the upper, middle and lower temperatures are more than or equal to 920 ℃ after monitoring.
The temperature control mode is as follows: aeration starts aeration deposition when the main control temperature reaches 1040 ℃.
And (3) introducing gas mass ratio: propylene: nitrogen=1:2, the ratio of the volume of gas flow per minute to the total preform volume introduced by propylene was 0.9.
The pressure of the third stage chemical vapor deposition is 0.60-1.2kPa, and the deposition time is as follows: 48 hours
The bulk density of the material at the end of this stage falls at 1.39g/cm 3 -1.47g/cm 3 Between them.
Step six heat treatment
The density obtained after the second stage of chemical vapor deposition is more than 1.42g/cm 3 And (3) carrying out heat treatment on the carbon blank body subjected to the third-stage chemical vapor deposition. Machining 3 after heat treatment
The size accounts for 20 percent of the total processing allowance, the volume density of the preform body is reduced after peeling, and the width is generally reduced to 0.02g/mm 3 -0.05g/mm 3 The greater the density is reduced. Bulk Density measurement 3 bulk Density measurement was performed according to the size after heat treatment and the weight of the measured material blank, with a bulk Density of 1.35g/cm 3 -1.45g/cm 3 The difference of the density distribution of the material is less than 0.10g/cm 3 。
The bulk density of the sample tray is 1.36g/cm 3 The material density distribution was measured by local sampling as shown in table 8 below.
TABLE 8
| Position of | Inner diameter of | Pitch diameter | Outer diameter of |
| Upper part | 1.40g/cm 3 | 1.36g/cm 3 | 1.33g/cm 3 |
| In (a) | 1.39g/cm 3 | 1.34g/cm 3 | 1.32g/cm 3 |
| Lower part(s) | 1.40g/cm 3 | 1.37g/cm 3 | 1.33g/cm 3 |
Step seven, reaction and siliconizing
And (3) carrying out reactive fusion siliconizing on the carbon-carbon porous body obtained by heat treatment to obtain the aviation carbon ceramic brake material.
The reaction and the infiltration are carried out under the argon atmosphere, the temperature of the reaction and the infiltration is 1550 ℃, the time of the reaction and the infiltration is 3 hours, and the pressure is 0.1-0.15MPa.
The carbon-carbon green body obtained in this example 3, in which the outer diameter radius of the deposited carbon grown around the carbon fiber was controlled within the range of 0.6 μm to 0.9. Mu.m, was advantageous for densification of the siliconizing fusion process.
The material has a coarse layer structure with more than 80% from inside to outside, and plays an important role in the mechanical property, friction and wear property and heat conduction property of the carbon ceramic brake material.
The densities of the carbon-carbon porous body and the final product obtained in this example 3 are shown in table 9:
TABLE 9
| Density (g/cm) of carbon green body 3 ) | Density after infiltration (g/cm) 3 ) |
| 1.35 | 2.18 |
| 1.42 | 2.19 |
| 1.40 | 2.19 |
| 1.38 | 2.19 |
In inertial test, the deceleration rate is more than 3.05m/s 2 The dynamic friction coefficient is 0.27-0.37, the brake curve has good performance, the average wear rate is about 0.45 mu m/time per surface, and other technical indexes meet the requirements, and the dynamic friction coefficient is already applied to a carbon ceramic brake pair of a certain unmanned aerial vehicle.
Comparative example 1
The other conditions were the same as in example 1 except that the carbon fiber preform was not numbered and the charging was not performed according to the numbering rule. The uniformity of the batch density is poor, and the maximum density exceeds 1.50g/mm 3 。
Comparative example 2
Other conditions were the same as in example 1 except that the deposition temperature was constant at 1010 ℃ during the three chemical vapor deposition. When the deposition temperature is less than 1020 ℃, the coarse layer accounts for about 40-60%.
Comparative example 3
Other conditions were the same as in example 1 except that the deposition was performed at the temperature in CVD2 during the three chemical vapor deposition processes. Density of less than 1.35g/mm 3 The ratio is about 35%.
Comparative example 4
Other conditions were the same as in example 1, and the thickness of the spacers 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 exceeds 1.45g/mm in the range 3 The probability of (2) is 80%, and the highest probability can reach 1.52g/mm 3 。
Claims (8)
1. A preparation method of an aviation carbon ceramic brake material is characterized by comprising the following steps: stacking the centers of N hollow disk-shaped carbon fiber preformed bodies through an internal heat source heater to form a material column, placing the material column in a chemical vapor deposition furnace, controlling the interval between any two adjacent carbon fiber preformed bodies 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 positioned in the middle of the upper end of the material column, uniformly arranging at least 6 air inlets on the side surface of the lower end of the material column, performing chemical vapor deposition by taking propylene as carbon source gas and nitrogen as diluent gas, forming a carbon-carbon blank body after chemical vapor deposition, performing heat treatment to obtain a carbon-carbon porous body, and performing ceramic treatment to obtain an aviation carbon ceramic brake material; the chemical vapor deposition is divided into three sections, wherein the temperature of the first section of chemical vapor deposition is 1060-1085 ℃, the temperature is firstly increased to 1080-1085 ℃, then the temperature is reduced to 1060-1065 ℃ at 15-22 ℃/80h, the time of the first section of chemical vapor deposition is controlled to 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 increased to 1055-1060 ℃, then the temperature is reduced to 1040-1045 ℃ at 10-20 ℃/40h, the time of the second section of chemical vapor deposition is controlled to 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 constant to 1030-1040 ℃, the time of the third section of chemical vapor deposition is controlled to 20-60h, and the pressure of the third section of chemical vapor deposition is 0.60-1.2 kPa;
in the first stage of chemical vapor deposition, N carbon fiber preforms are sequentially numbered from bottom to top or from top to bottom, the interval between any two adjacent carbon fiber preforms is controlled to be 2-3mm, and in the second stage of chemical vapor deposition, all carbon preforms are firstly subjected to chemical vapor depositionThe body is divided into two sections B and A from bottom to top, when the first chemical vapor deposition is carried out in sequence from small to large, 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 is carried out in sequence from 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 second chemical vapor deposition is carried out, the distance between any two adjacent carbon fiber preforms is controlled to be 1.5-2.5mm, and when the third chemical vapor deposition is carried out, the density is removed to be more than 1.42g/cm 3 Dividing the M carbon blanks into two sections D and C from bottom to top, numbering the section D from middle to large when the chemical vapor deposition is carried out in sequence from large to small when the chemical vapor deposition is carried out for the first time, numbering the section C from small to small when the chemical vapor deposition is carried out for the first time, numbering the section D from large to small when the chemical vapor deposition is carried out in sequence from large to small when the chemical vapor deposition is carried out for the first time, numbering the section C from large to small, and simultaneously controlling the interval between two adjacent carbon blanks with the density lower than the intermediate value to be 1.3-1.6mm and the density to be between the intermediate value and 1.4g/cm 3 The spacing between two adjacent carbon-carbon blanks is 0.7-1.1mm, and the density is 1.4g/cm 3 The spacing between the two adjacent carbon-carbon green bodies is 0.4-0.6mm.
2. The method for preparing the aviation carbon ceramic brake material according to claim 1, wherein the method comprises the following steps: the carbon fiber preform is obtained through the following steps: the carbon fiber non-woven cloth and the carbon fiber mesh fabric are alternately laminated, and the carbon fiber preform is obtained by continuous carbon fiber needling, wherein the mass ratio of the carbon fiber non-woven cloth to the mesh fabric is 1:0.20-0.30, and the interlayer density of the carbon fiber non-woven cloth is 10-16 layers/cm;
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, wherein the temperature of the heat treatment is 2100-2300 ℃, and the time of the heat treatment is 2-3 hours.
3. The method for preparing the aviation carbon ceramic brake material according to claim 1, wherein the 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;
during chemical vapor deposition, temperature control is performed 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 a material column and is 18-25mm away from the outer diameter of an internal heat source heater in the radial direction, the upper temperature measuring point is axially positioned at the upper part of the material column and is radially positioned at the outer edge of the material column, the middle temperature measuring point is axially positioned in the middle of the material column and is radially positioned at the outer edge of the material column, and the lower temperature measuring point is axially positioned at the lower part of the material column and is radially positioned at the outer edge of the material column.
4. The method for preparing the aviation carbon ceramic brake material according to claim 1, wherein the method comprises the following steps:
during the first-stage chemical vapor deposition, the mass ratio of propylene to nitrogen is 1.8-2.2:3, and the total volume of propylene and nitrogen introduced per minute is 1.2-1.3:1;
during the second-stage chemical vapor deposition, the mass ratio of propylene to nitrogen is 1.8-2.2:3, and the total volume of propylene and nitrogen introduced per minute is 1-1.1:1;
and during the third-stage chemical vapor deposition, the mass ratio of propylene to nitrogen is 1:1.8-2.2, and the total volume of propylene and nitrogen introduced per minute is 0.8-0.9:1 of the total volume of the carbon fiber preform.
5. The method for preparing the aviation carbon ceramic brake material according to claim 1, wherein the 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 third stage is obtained after chemical vapor depositionThe bulk density of the carbon-carbon blank is 1.38g/cm 3 -1.48g/cm 3 。
6. The method for preparing the aviation carbon ceramic brake material according to claim 1, wherein the method comprises the following steps: the temperature of the heat treatment is 2000-2100 ℃, and the time of the heat treatment is 1-3 hours;
the density of the carbon-carbon porous body is 1.35g/cm 3 -1.45g/cm 3 。
7. The method for preparing the aviation carbon ceramic brake material according to claim 1, wherein the method comprises the following steps: the ceramic treatment mode is reactive melt-siliconizing, the reactive melt-siliconizing is carried out under the argon atmosphere, the temperature of the reactive melt-siliconizing is 1550-1650 ℃, the time of the reactive melt-siliconizing is 2-4h, and the pressure is 0.1-0.15Pa.
8. An aviation carbon ceramic brake material prepared by the preparation method of any one of claims 1-7.
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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 (2)
| 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)》.2002,第33卷(第04期),第380-384页. * |
| 用CVI增密技术制备航空刹车用C/C复合材料;汤中华等;《中南工业大学学报(自然科学版)》;第33卷(第04期);第380-384页 * |
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