A TiN-SiN2O ceramic modified C / C-SiC brake material and preparation method thereof

Abstract

The present invention discloses a TiN-SiN2O ceramic-modified C / C-SiC brake material and a preparation method thereof, belonging to the technical field of friction brake material preparation. The material uses TiN-SiN2O ceramic to modify C / C-SiC material. By adding Si and TiSi₂ powders to the raw materials, TiN-SiN₂O and SiC ceramic phases are generated by reaction, so that carbonization-ceramicization-densification are completed in a single heat treatment, thereby shortening the preparation cycle, while improving mechanical properties and reducing wear rate, and is expected to reduce costs, so as to solve the problem that the excellent friction and wear performance and mechanical properties of existing C / C-SiC cannot be taken into account at the same time with a short preparation cycle.

Description

Technical Field

[0001] The invention belongs to the technical field of friction brake material preparation, and particularly relates to a TiN-SiN2O ceramic modified C / C-SiC brake material and a preparation method thereof. Background Art

[0002] With the advancement of science and technology, the speed of modern transportation vehicles is increasing, placing increasingly stringent demands on braking systems. Braking materials for vehicles with frequent braking, such as cars, airplanes, high-speed trains, and trucks, have undergone several generations of development. Initially, asbestos friction materials offered the advantages of lightweight and low cost, but were gradually replaced due to asbestos being a carcinogen. Subsequent powder metallurgy friction materials offered long service life and high reliability, but their high density and tendency to stick at high temperatures limited their operating conditions. C / C-SiC friction material is a new type of friction material, boasting a range of excellent properties, including high strength, high thermal conductivity, excellent mechanical properties, and strong environmental adaptability. It inherits the advantages of existing friction materials while addressing their shortcomings, and has attracted widespread attention.

[0003] Traditional C / C-SiC materials, composed of carbon fibers, matrix carbon, and SiC, suffer from insufficient toughness and high wear rates due to their exclusive SiC ceramic phase. Furthermore, their high cost and complex preparation process limit their widespread application. Currently, the main methods for preparing C / C-SiC materials include chemical vapor infiltration, polymer impregnation and pyrolysis, and reactive melt infiltration. Chemical vapor infiltration and polymer impregnation and pyrolysis utilize a continuous fiber mat as reinforcement, resulting in products with excellent mechanical properties. However, due to the alternating arrangement of the mat / weft-free fabric, materials reinforced with a continuous fiber mat exhibit relatively low friction stability, and the preparation cycle can exceed 150 hours. Furthermore, the raw material cost of continuous fiber mats is high. In contrast, reactive melt infiltration offers a simpler process, allowing the use of either a continuous fiber mat or short fibers as reinforcement. The preparation cycle can be shortened to 72 hours compared to chemical vapor infiltration and polymer impregnation and pyrolysis. However, products prepared by reactive melt infiltration contain 5%-15% residual silicon by mass, which negatively impacts the overall friction, wear, and mechanical properties of the material. Therefore, developing a method that can significantly improve the friction and wear performance of the material and has a shorter preparation cycle is crucial to promoting the large-scale application of C / C-SiC brake materials.

[0004] For example, Chinese patent publication number CN116354735A discloses a method for rapidly preparing AlN-modified C / C-SiC friction materials. This method involves pressing a uniform mixture of short carbon fibers, phenolic resin, industrial silicon powder, and aluminum powder into a fiber-reinforced resin block. This block is then carbonized and ceramicized to produce the C / C-AlN-SiC friction material. This method has a short densification cycle and low production costs, but the material still has a wear rate of 1.277×10 -15 m 3 N -1 m -1 -34.765×10 - 15 m 3 N -1 m -1 The carbon fiber preform is still high, and the modified component AlN ceramic is easily hydrolyzed, which limits its operating conditions. A Chinese patent with patent publication number CN101493126A discloses a method for manufacturing carbon / ceramic brake linings for industrial brakes. The method first uses a needle-punching method to prepare a carbon fiber preform, which is subjected to high-temperature heat treatment and then chemical vapor infiltration to obtain a low-density C / C composite material. The C / C composite material is subjected to high-temperature heat treatment and then machined. The C / C material is then melt-siliconized in a high-temperature vacuum furnace, and Si reacts with C to form SiC to obtain a C / C-SiC brake material. This method combines chemical vapor infiltration and reactive infiltration. The prepared C / C-SiC brake material has high mechanical properties, but the material still contains a small amount of residual silicon, which affects its friction and wear performance. The preparation cycle is as long as 130-300 hours, and the cost of the raw material continuous fiber is relatively high.

[0005] In summary, how to improve the friction and wear properties and mechanical properties of C / C-SiC materials while shortening the preparation cycle and reducing costs is a technical problem to be solved by those skilled in the art. Summary of the Invention

[0006] In order to overcome the shortcomings of the above-mentioned prior art, the purpose of the present invention is to provide a TiN-SiN2O ceramic modified C / C-SiC brake material and a preparation method thereof. By adding Si and TiSi2 powders to the raw materials, TiN-SiN2O and SiC ceramic phases are generated by reaction, so that carbonization-ceramicization-densification are completed in one heat treatment, thereby shortening the preparation cycle, while improving mechanical properties and reducing wear rate, and is expected to reduce costs, so as to solve the problem that the excellent friction and wear performance and mechanical properties of existing C / C-SiC cannot be taken into account at the same time with a shorter preparation cycle.

[0007] In order to achieve the above object, the present invention adopts the following technical solutions:

[0008] On one hand, the present invention provides a TiN-SiN2O ceramic modified C / C-SiC brake material, wherein the TiN-SiN2O ceramic modified C / C-SiC brake material uses TiN-SiN2O ceramic to modify the C / C-SiC material.

[0009] The TiN-SiN2O ceramic modified C / C-SiC brake material is made of the following raw materials by volume percentage: 10-20% TiSi2 powder, 7-20% graphite powder, 15-20% phenolic resin powder, 10-13% SiC powder, 20-30% Si powder and 15-20% chopped carbon fiber.

[0010] In one embodiment, the TiN-SiN2O ceramic modified C / C-SiC brake material includes TiN ceramic, SiN2O ceramic and SiC ceramic. The TiN-SiN2O ceramic modified C / C-SiC brake material has a compressive strength of 270-290 MPa, a flexural strength of 120-130 MPa, and a wear rate reduced to 2.05×10 -16 m 3 N -1 m -1 .

[0011] The present invention also provides a method for preparing a TiN-SiN2O ceramic modified C / C-SiC brake material, comprising the following steps:

[0012] TiSi2 powder, graphite powder, phenolic resin powder, SiC powder and Si powder are uniformly mixed to obtain a mixed powder; short carbon fibers are added into anhydrous ethanol, stirred, dispersed, and dried to obtain dispersed fibers;

[0013] The mixed powder and the fiber are uniformly mixed to obtain a fiber mixed powder; the fiber mixed powder is molded to obtain a fiber reinforced resin block;

[0014] curing the fiber-reinforced resin block to obtain a cured fiber-reinforced resin block;

[0015] The cured fiber reinforced resin block is heat treated in a nitrogen atmosphere to obtain a TiN-SiN2O ceramic modified C / C-SiC brake material.

[0016] In one embodiment, the TiSi2 powder, graphite powder, phenolic resin powder, SiC powder and Si powder are ball-milled in a planetary ball mill at a rotation speed of 300-400 r / min for 2-3 h.

[0017] In one embodiment, the dispersion is performed under an ultrasonic power of 60-100 W, and the dispersion time is 10-15 min.

[0018] In one embodiment, the drying is performed at a temperature of 50-80° C., and the drying time is 2-4 hours.

[0019] In one embodiment, the molding temperature is 160-190° C., the molding pressure is 7-10 MPa, and the molding time is 60-120 min.

[0020] In one embodiment, the curing process is a step-by-step curing process, and the specific process is as follows: heating to 160° C. and keeping warm for 3 hours, then heating to 180° C. and keeping warm for 3 hours, and finally heating to 220° C. and keeping warm for 2 hours.

[0021] In one embodiment, the heat treatment is performed under a carrier gas atmosphere, the carrier gas atmosphere is a nitrogen atmosphere, and the flow rate of the carrier gas is 80-120 mL / min.

[0022] In one embodiment, the heat treatment process is as follows: heating to 900-1000°C at a heating rate of 1-5°C / min, keeping warm for 1-2 hours, then heating to 1400-1500°C at a heating rate of 1-5°C / min, keeping warm for 2-3 hours, then cooling to 250-300°C at a cooling rate of 7-10°C / min and then cooling to room temperature with the furnace.

[0023] Compared with the prior art, the present invention has the following beneficial effects:

[0024] On one hand, the present invention provides a TiN-SiN2O ceramic modified C / C-SiC brake material, in which TiSi2 powder and Si powder in the raw materials react with carrier gas N2 to generate ceramics such as TiN and SiN2O, which can fill the pores generated by resin carbonization and improve the density of the material, which is equivalent to the density of the material prepared by the reactive infiltration method; and because there are multiple ceramics such as TiN, SiN2O and SiC, the shortcomings of a single SiC ceramic are compensated, TiN and SiN2O ceramics have higher toughness and lower hardness than SiC, and the addition of TiN and SiN2O is beneficial to reducing excessive abrasive wear of the material caused by excessive hardness during the friction process, and the improvement of toughness is beneficial to improving the mechanical properties of the material; and TiN and SiN2O ceramics have higher thermal stability than SiC, which is beneficial to reducing oxidative wear and fatigue wear of the material at high temperatures. SiC powder is added to the raw materials. It acts as a sintering aid, facilitating reactions during heat treatment. It reduces resin carbonization and volume shrinkage from the silicon-carbon reaction, preventing significant internal stress in the material. It also acts as an inert filler, maintaining stability within the material. It bonds well with the SiC formed by the silicon-carbon reaction, acting as a ceramic phase that enhances performance. Graphite powder, with its low hardness, acts as a lubricant, modulating the material's friction coefficient and preventing high wear rates caused by excessive hardness and friction. It also serves as a carbon source for the Si-C reaction, minimizing the carbon fiber-Si reaction and thus reducing damage. The material reinforcement utilizes short carbon fibers, which are uniformly distributed and randomly oriented throughout the material. Compared to materials reinforced with fiber-blanketed felts, which have relatively low friction stability due to the alternating arrangement of mesh and non-woven fabrics, short carbon fibers exhibit superior friction stability due to their uniform distribution and random orientation. Furthermore, the cost of short carbon fibers is only 30% of that of continuous fiber-blanketed felts.

[0025] The material has excellent mechanical properties and low wear rate. The compressive strength of the material is increased to 270-290 MPa, the bending strength is increased to 120-130 MPa, and the wear rate is reduced to 2.05×10 -16 m 3 N -1 m -1 .

[0026] On the other hand, the present invention also provides a preparation method of TiN-SiN2O ceramic modified C / C-SiC brake material, which uses the above raw materials to perform curing treatment and heat treatment in sequence, and the carbonization-ceramicization-densification process is completed in one heat treatment. Compared with the existing process, compared with the existing technology, the cycle can be shortened from more than 150 hours to about 30 hours, and no more complicated steps are required, which significantly reduces the cost of manpower and equipment use. BRIEF DESCRIPTION OF THE DRAWINGS

[0027] Figure 1 The cross-sectional SEM images of TiN-SiN2O ceramic modified C / C-SiC brake material are shown in Figure 1. (a) is a low magnification image, and (b) is a high magnification image.

[0028] Figure 2 1 is an XRD pattern of TiN-SiN2O ceramic modified C / C-SiC brake material; wherein (a) is Example 1 and Example 2; (b) is Example 3 and Comparative Example 1;

[0029] Figure 3 are the mechanical properties of TiN-SiN2O ceramic modified C / C-SiC brake materials; (a) is the bending strength; (b) is the compressive strength;

[0030] Figure 4 The tribological properties of TiN-SiN2O ceramic modified C / C-SiC brake material; (a) is a comparison chart of friction coefficient changes; (b) is the friction coefficient and wear rate. DETAILED DESCRIPTION

[0031] To facilitate understanding of the features and effects of the present invention by those skilled in the art, the following provides a general description and definition of the terms and expressions used in the specification and claims. Unless otherwise indicated, all technical and scientific terms used herein have the ordinary meanings as understood by those skilled in the art regarding the present invention. In the event of conflict, the definitions in this specification shall prevail.

[0032] The theories or mechanisms described and disclosed herein, whether correct or incorrect, should not limit the scope of the present invention in any way, that is, the present invention can be implemented without being limited by any specific theory or mechanism.

[0033] All features, such as values, amounts, contents, and concentrations, described herein as numerical ranges or percentage ranges are provided for simplicity and convenience only. Accordingly, the description of numerical ranges or percentage ranges should be considered to include and specifically disclose all possible subranges and individual values ​​within the range (including integers and fractions).

[0034] In this document, unless otherwise specified, “include,” “including,” “contains,” “has” or similar terms cover the meanings of “consisting of” and “mainly consisting of,” for example, “A includes a” covers the meanings of “A includes a and other” and “A only includes a.”

[0035] In this document, for the sake of brevity, not all possible combinations of the various technical features in each embodiment or example are described. Therefore, as long as there are no contradictions in the combination of these technical features, the various technical features in each embodiment or example can be combined in any way, and all possible combinations should be considered to be within the scope of this specification.

[0036] The present invention provides a TiN-SiN2O ceramic-modified C / C-SiC brake material and a preparation method thereof. TiSi2 powder and Si powder added to the raw materials react with carrier gas N2 to generate ceramics such as TiN and SiN2O, thereby increasing the density of the material and reducing its porosity, thereby obtaining a multi-component ceramic co-modified C / C-SiC composite material, thereby reducing the wear rate and improving the mechanical properties of the material. Secondly, a preform is prepared by rapid molding, and the carbonization-ceramicization-densification process of the preform into the product is completed in a single heat treatment. Compared with existing processes, this significantly shortens the cycle time and reduces labor and equipment costs.

[0037] In one aspect, the present invention provides a TiN-SiN2O ceramic-modified C / C-SiC brake material. The TiN-SiN2O ceramic-modified C / C-SiC brake material uses TiN-SiN2O ceramic to modify C / C-SiC material. The raw materials for preparing the TiN-SiN2O ceramic-modified C / C-SiC brake material are as follows, by volume percentage: 10-20% TiSi2 powder, 7-20% graphite powder, 15-20% phenolic resin powder, 10-13% SiC powder, 20-30% Si powder and 15-20% chopped carbon fiber.

[0038] The compressive strength of the TiN-SiN2O ceramic modified C / C-SiC brake material is 270-290 MPa, the bending strength is 120-130 MPa, and the wear rate is reduced to 2.05×10 -16 m 3 N -1 m -1 .

[0039] Another aspect of the present invention provides a method for preparing a TiN-SiN2O ceramic modified C / C-SiC brake material, comprising the following steps:

[0040] TiSi2 powder, graphite powder, phenolic resin powder, SiC powder and Si powder are uniformly mixed to obtain a mixed powder; short carbon fibers are added into anhydrous ethanol, stirred, dispersed, and dried to obtain dispersed fibers;

[0041] The mixed powder and the fiber are uniformly mixed to obtain a fiber mixed powder; the fiber mixed powder is molded to obtain a fiber reinforced resin block;

[0042] curing the fiber-reinforced resin block to obtain a cured fiber-reinforced resin block;

[0043] The cured fiber reinforced resin block is heat treated to obtain a TiN-SiN2O ceramic modified C / C-SiC brake material.

[0044] In one embodiment, the above preparation method comprises the following steps:

[0045] Step 1: Weigh TiSi2 powder A, graphite powder B, phenolic resin powder C, SiC powder D, Si powder E, and chopped carbon fiber F.

[0046] Step 2: Mix TiSi2 powder A, graphite powder B, phenolic resin powder C, SiC powder D, and Si powder E evenly to obtain mixed powder G.

[0047] Step 3: Add the chopped carbon fiber F into anhydrous ethanol, stir thoroughly, disperse, and dry to obtain dispersed fiber H.

[0048] Step 4: Mix the mixed powder G and the fiber H in a high-speed grinder to obtain fiber mixed powder I.

[0049] Step 5: Add the fiber mixed powder I into a homemade mold and perform molding in a molding press to obtain a fiber reinforced resin block J.

[0050] Step 6: The block J is cured in an oven to obtain a cured fiber reinforced resin block K.

[0051] Step 7: Heat-treating the block J in a carrier gas atmosphere, and heating and cooling according to a heating curve to obtain a C / C-TiN-SiN2O-SiC composite material.

[0052] In the above step 1, by volume percentage: TiSi2 powder A accounts for 10-20%; graphite powder B accounts for 7-20%; phenolic resin powder C accounts for 15-20%; SiC powder D accounts for 10-13%; Si powder E accounts for 20-30%; and chopped carbon fiber F accounts for 15-20%.

[0053] In the above step 2, the mixing is to place TiSi2 powder A, graphite powder B, phenolic resin powder C, SiC powder D, and Si powder E in a planetary ball mill and mix them at a ball milling speed of 300-400 r / min and a ball milling time of 2-3 h.

[0054] In the above step 3, the dispersion is carried out at an ultrasonic power of 60-100 W for 10-15 minutes; and the drying / stoving is carried out at 50-80° C. for 2-4 hours.

[0055] In the above step 4, the mixing times are 6-10 times.

[0056] In the above step 5, the molding temperature is 160-190° C., the molding pressure is 7-10 MPa, and the molding time is 60-120 min.

[0057] In the above step 6, the curing process is a step-by-step curing process, and the specific process is as follows: heating to 160°C and keeping it for 3 hours, then heating to 180°C and keeping it for 3 hours, and finally heating to 220°C and keeping it for 2 hours.

[0058] In step 7, the heat treatment carrier gas is N2 at a flow rate of 80-120 mL / min. The heating curve is as follows: heating to 900-1000°C, holding for 1-2 hours, then heating to 1400-1500°C, holding for 2-3 hours, cooling to 250-300°C, and then cooling to room temperature in the furnace. The heating rate is 1-5°C / min, and the cooling rate is 7-10°C / min.

[0059] Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiments are only used to illustrate the present invention and are not used in limiting the scope of the present invention.In addition, should be understood that after reading the content taught by the present invention, those skilled in the art can make various changes or modifications to the present invention, and these equivalent forms fall equally within the scope limited by the appended claims of the application.

[0060] The following examples were prepared using conventional instruments and equipment in the art. Experimental methods in the following examples, where specific conditions are not specified, were generally performed under conventional conditions or according to the conditions recommended by the manufacturer. The various raw materials used in the following examples, unless otherwise specified, were conventional commercially available products, with specifications conventional in the art. In the present specification and the following examples, unless otherwise specified, "%" indicates percentage by weight, "part" indicates parts by weight, and "ratio" indicates weight ratio.

[0061] Example 1:

[0062] A method for preparing a TiN-SiN2O ceramic modified C / C-SiC brake material comprises the following steps:

[0063] Step 1: Calculated by volume percentage, TiSi2 powder accounts for 20%, graphite powder accounts for 10%, phenolic resin powder accounts for 20%, SiC powder accounts for 10%, Si powder accounts for 20%, and chopped carbon fiber accounts for 20%. The corresponding weights are as follows: Weigh 27.10g of TiSi2 powder, 6.78g of graphite powder, 10.16g of phenolic resin powder, 10.85g of SiC powder, 15.85g of Si powder, and 11.86g of chopped carbon fiber and set aside.

[0064] Step 2: Put the weighed TiSi2 powder, graphite powder, phenolic resin powder, SiC powder and Si powder into a ball mill, set the speed to 400r / min, and mix the powders with a planetary ball mill for 2h and set aside.

[0065] Step 3: Add the weighed chopped carbon fibers to 100 mL of anhydrous ethanol and stir for 15 minutes. Set the ultrasonic disperser power to 100 W. After dispersing for 10 minutes, place the mixture in an oven at 50°C and dry for 4 hours for later use.

[0066] Step 4: Mix the powder processed in step 2 with the chopped carbon fiber processed in step 3 in a high-speed mill set at a speed of 23,000 r / min, and repeat 6 times with an interval of 10 minutes each time.

[0067] Step 5: The powder processed in step 4 is molded on a molding machine with a molding pressure of 10 MPa, a molding temperature of 160°C, and a holding time of 60 min to obtain a density of 2.2 g / cm 3 Fiber reinforced resin composite blocks.

[0068] Step 6: Place the block obtained in step 5 into an oven for curing. The curing process is to keep the temperature at 160°C for 3 hours, then heat it to 180°C for 3 hours, and finally heat it to 220°C for 2 hours to obtain a cured fiber reinforced resin block.

[0069] Step 7: Place the block obtained in step 6 in a tubular heat treatment furnace for heat treatment. The heat treatment carrier gas is N2, and the carrier gas flow rate is 120 mL / min. The heating curve is to increase the temperature from room temperature to 900°C at a heating rate of 1°C / min, keep it warm for 2 hours, so that the phenolic resin in the material is converted into resin carbon, increase the temperature from 900°C to 1400°C at a heating rate of 5°C / min, keep it warm for 3 hours, and cool it from 1400°C to 300°C at a cooling rate of 7°C / min. Then cool it to room temperature with the furnace to convert the TiSi2 powder and Si powder in the material into TiN, SiN2O and SiC ceramics, and obtain a C / C-TiN-SiN2O-SiC composite material with a material density of 2.29 g / cm 3 .

[0070] See also Figure 1 , the cross-sectional SEM image of TiN-SiN2O ceramic modified C / C-SiC brake material, as can be seen from the figure, the different phases are evenly distributed on the cross section, among which the black and dark gray phases are graphite, resin carbon and carbon fiber, the medium gray phase is SiC, the light gray is TiN, and the white is SiN2O. There are no crack defects on the cross section. Figure 2(a) XRD pattern of TiN-SiN2O ceramic modified C / C-SiC brake material. It can be seen that C, TiN, SiN2O and SiC were detected in the material, indicating that the C / C-TiN-SiN2O-SiC composite material was successfully prepared. Figure 3 and Figure 4 The bending strength of the material is 130.88 MPa, the compressive strength is 292.56 MPa, the dynamic friction coefficient is 0.553, and the wear rate is 25.24×10 -16 m 3 N -1 m -1 .

[0071] Example 2:

[0072] A method for preparing a TiN-SiN2O ceramic modified C / C-SiC brake material comprises the following steps:

[0073] Step 1: Calculated by volume percentage, TiSi2 powder accounts for 15%, graphite powder accounts for 15%, phenolic resin powder accounts for 20%, SiC powder accounts for 10%, Si powder accounts for 20%, and chopped carbon fiber accounts for 20%. The corresponding weights are as follows: Weigh 20.33g of TiSi2 powder, 10.16g of graphite powder, 10.16g of phenolic resin powder, 10.85g of SiC powder, 15.85g of Si powder, and 11.86g of chopped carbon fiber and set aside.

[0074] Step 2: Put the weighed TiSi2 powder, graphite powder, phenolic resin powder, SiC powder and Si powder into a ball mill, set the speed to 400r / min, and mix the powders with a planetary ball mill for 2h and set aside.

[0075] Step 3: Add the weighed chopped carbon fibers to 100 mL of anhydrous ethanol and stir for 15 minutes. Set the ultrasonic disperser power to 100 W. After dispersing for 10 minutes, place the mixture in an oven at 50°C and dry for 4 hours for later use.

[0076] Step 4: Mix the powder processed in step 2 with the chopped carbon fiber processed in step 3 in a high-speed mill set at a speed of 23,000 r / min, and repeat 6 times with an interval of 10 minutes each time.

[0077] Step 5: The powder processed in step 4 is molded on a molding machine with a molding pressure of 10 MPa, a molding temperature of 160°C, and a holding time of 60 min to obtain a density of 2.18 g / cm 3 Fiber reinforced resin composite blocks.

[0078] Step 6: Place the block obtained in step 5 into an oven for curing. The curing process is to keep the temperature at 160°C for 3 hours, then heat it to 180°C for 3 hours, and finally heat it to 220°C for 2 hours to obtain a cured fiber reinforced resin block.

[0079] Step 7: Place the block obtained in step 6 in a tubular heat treatment furnace for heat treatment. The heat treatment carrier gas is N2 and the carrier gas flow rate is 120 mL / min. The heating curve is to increase the temperature from room temperature to 900°C at a heating rate of 1°C / min and keep it warm for 2 hours to convert the phenolic resin in the material into resin carbon, increase the temperature from 900°C to 1400°C at a heating rate of 5°C / min and keep it warm for 3 hours, and then cool it from 1400°C to 300°C at a cooling rate of 7°C / min. Then cool it to room temperature with the furnace to convert the TiSi2 powder and Si powder in the material into TiN, SiN2O and SiC ceramics, and obtain a C / C-TiN-SiN2O-SiC composite material with a material density of 2.22 g / cm 3 .

[0080] See also Figure 2 (a) XRD pattern of TiN-SiN2O ceramic modified C / C-SiC brake material. It can be seen that C, TiN, SiN2O and SiC were detected in the material, indicating that the C / C-TiN-SiN2O-SiC composite material was successfully prepared. Figure 3 and Figure 4 The bending strength of the material is 101.13 MPa, the compressive strength is 271.36 MPa, the dynamic friction coefficient is 0.356, and the wear rate is 2.05×10 -16 m 3 N -1 m -1 .

[0081] Example 3:

[0082] A method for preparing a TiN-SiN2O ceramic modified C / C-SiC brake material comprises the following steps:

[0083] Step 1: Calculated by volume percentage, TiSi2 powder accounts for 10%, graphite powder accounts for 20%, phenolic resin powder accounts for 20%, SiC powder accounts for 10%, Si powder accounts for 20%, and chopped carbon fiber accounts for 20%. The corresponding weights are as follows: Weigh 13.55g of TiSi2 powder, 13.56g of graphite powder, 10.16g of phenolic resin powder, 10.85g of SiC powder, 15.85g of Si powder, and 11.86g of chopped carbon fiber and set aside.

[0084] Step 2: Put the weighed TiSi2 powder, graphite powder, phenolic resin powder, SiC powder and Si powder into a ball mill, set the speed to 400r / min, and mix the powders with a planetary ball mill for 2h and set aside.

[0085] Step 3: Add the weighed chopped carbon fibers to 100 mL of anhydrous ethanol and stir for 15 minutes. Set the ultrasonic disperser power to 60 W. After dispersing for 15 minutes, place the mixture in an oven at 80°C and dry for 2 hours for later use.

[0086] Step 4: Mix the powder processed in step 2 with the chopped carbon fiber processed in step 3 in a high-speed mill set at a speed of 23,000 r / min, and repeat 6 times with an interval of 10 minutes each time.

[0087] Step 5: The powder processed in step 4 is molded on a molding machine with a molding pressure of 10 MPa, a molding temperature of 160°C, and a holding time of 60 min to obtain a density of 2.15 g / cm 3 Fiber reinforced resin composite blocks.

[0088] Step 6: Place the block obtained in step 5 into an oven for curing. The curing process is to keep the temperature at 160°C for 3 hours, then heat it to 180°C for 3 hours, and finally heat it to 220°C for 2 hours to obtain a cured fiber reinforced resin block.

[0089] Step 7: Place the block obtained in step 6 in a tubular heat treatment furnace for heat treatment. The heat treatment carrier gas is N2 and the carrier gas flow rate is 120 mL / min. The heating curve is to increase the temperature from room temperature to 900°C at a heating rate of 1°C / min and keep it warm for 2 hours to convert the phenolic resin in the material into resin carbon, increase the temperature from 900°C to 1400°C at a heating rate of 5°C / min and keep it warm for 3 hours, and then cool it from 1400°C to 300°C at a cooling rate of 7°C / min. Then cool it to room temperature with the furnace to convert the TiSi2 powder and Si powder in the material into TiN, SiN2O and SiC ceramics, and obtain a C / C-TiN-SiN2O-SiC composite material with a material density of 2.14 g / cm 3 .

[0090] See also Figure 2 (b) XRD pattern of TiN-SiN2O ceramic modified C / C-SiC brake material. It can be seen that C, TiN, SiN2O and SiC were detected in the material, indicating that the C / C-TiN-SiN2O-SiC composite material was successfully prepared. Figure 3 and Figure 4 The bending strength of the material is 120.13 MPa, the compressive strength is 221.24 MPa, the dynamic friction coefficient is 0.274, and the wear rate is 14.64×10 -16 m 3 N -1 m -1 .

[0091] Example 4:

[0092] A method for preparing a TiN-SiN2O ceramic modified C / C-SiC brake material comprises the following steps:

[0093] Step 1: Calculated by volume percentage, TiSi2 powder accounts for 20%, graphite powder accounts for 7%, phenolic resin powder accounts for 15%, SiC powder accounts for 13%, Si powder accounts for 30%, and chopped carbon fiber accounts for 15%. The corresponding weights are as follows: Weigh 27.10g of TiSi2 powder, 4.74g of graphite powder, 7.62g of phenolic resin powder, 14.09g of SiC powder, 23.78g of Si powder, and 8.89g of chopped carbon fiber and set aside.

[0094] Step 2: Put the weighed graphite powder, phenolic resin powder, SiC powder, and Si powder into a ball mill, set the speed to 300 r / min, and mix the powders with a planetary ball mill for 3 hours for use.

[0095] Step 3: Add the weighed chopped carbon fibers to 100 mL of anhydrous ethanol and stir for 15 minutes. Set the ultrasonic disperser power to 60 W. After dispersing for 15 minutes, place the mixture in an oven at 80°C and dry for 2 hours for later use.

[0096] Step 4: Mix the powder processed in step 2 with the chopped carbon fiber processed in step 3 in a high-speed mill set at a speed of 15,000 r / min, and repeat 10 times with an interval of 10 minutes each time.

[0097] Step 5: The powder processed in step 4 is molded on a molding machine with a molding pressure of 7 MPa, a molding temperature of 190° C., and a holding time of 120 min to obtain a fiber-reinforced resin composite material block.

[0098] Step 6: Place the block obtained in step 5 into an oven for curing. The curing process is to keep the temperature at 160°C for 3 hours, then heat it to 180°C for 3 hours, and finally heat it to 220°C for 2 hours to obtain a cured fiber reinforced resin block.

[0099] Step 7: The block obtained in step 6 is placed in a tubular heat treatment furnace for heat treatment. The heat treatment carrier gas is N2, and the carrier gas flow rate is 80 mL / min. The heating curve is as follows: heating from room temperature to 1000°C at a heating rate of 1°C / min, holding for 1 hour, so that the phenolic resin in the material is converted into resin carbon, heating from 900°C to 1500°C at a heating rate of 5°C / min, holding for 2 hours, and cooling from 1500°C to 250°C at a cooling rate of 10°C / min. Then, the temperature is cooled to room temperature in the furnace to convert the TiSi2 powder and Si powder in the material into TiN, SiN2O and SiC ceramics, thereby obtaining a C / C-TiN-SiN2O-SiC composite material.

[0100] Comparative Example 1:

[0101] A method for preparing a C / C-SiC brake material comprises the following steps:

[0102] Step 1: Calculated by volume percentage, graphite powder accounts for 20%, phenolic resin powder accounts for 20%, SiC powder accounts for 10%, Si powder accounts for 30%, and chopped carbon fiber accounts for 20%. The corresponding weights are as follows: Weigh 13.56g of graphite powder, 10.16g of phenolic resin powder, 10.85g of SiC powder, 23.78g of Si powder, and 11.86g of chopped carbon fiber and set aside.

[0103] Step 2: Put the weighed graphite powder, phenolic resin powder, SiC powder, and Si powder into a ball mill, set the speed to 300 r / min, and mix the powders with a planetary ball mill for 3 hours for use.

[0104] Step 3: Add the weighed chopped carbon fibers to 100 mL of anhydrous ethanol and stir for 15 minutes. Set the ultrasonic disperser power to 60 W. After dispersing for 15 minutes, place the mixture in an oven at 80°C and dry for 2 hours for later use.

[0105] Step 4: Mix the powder processed in step 2 with the chopped carbon fiber processed in step 3 in a high-speed mill set at a speed of 15,000 r / min, and repeat 10 times with an interval of 10 minutes each time.

[0106] Step 5: The powder processed in step 4 is molded on a molding machine with a molding pressure of 7 MPa, a molding temperature of 190°C, and a holding time of 120 min to obtain a density of 2.00 g / cm 3 Fiber reinforced resin composite blocks.

[0107] Step 6: Place the block obtained in step 5 into an oven for curing. The curing process is to keep the temperature at 160°C for 3 hours and then increase the temperature to 180°C for 3 hours to obtain a cured fiber reinforced resin block.

[0108] Step 7: Place the block obtained in step 6 in a tubular heat treatment furnace for heat treatment. The heat treatment carrier gas is N2 and the carrier gas flow rate is 80 mL / min. The heating curve is to increase the temperature from room temperature to 1000°C at a heating rate of 1°C / min and keep it warm for 1 hour to convert the phenolic resin in the material into resin carbon. Then, increase the temperature from 900°C to 1500°C at a heating rate of 5°C / min and keep it warm for 2 hours. Then, cool it from 1500°C to 250°C at a cooling rate of 10°C / min. Then, cool it to room temperature in the furnace to convert the Si powder in the material into SiC ceramics to obtain a C / C-SiC composite material with a material density of 2.03 g / cm 3 .

[0109] See also Figure 2 (b) XRD pattern of C / C-SiC brake material. It can be seen that C and SiC are detected in the material, indicating that the C / C-SiC composite material is successfully prepared. Figure 3 and Figure 4 The bending strength of the material is 45.87 MPa, the compressive strength is 188.31 MPa, the dynamic friction coefficient is 0.264, and the wear rate is 28.91×10 -16 m 3 N -1 m -1 Compared with Examples 1, 2, and 3, which produced TiN-SiN2O ceramics, Comparative Example 1, which did not produce TiN-SiN2O ceramics, exhibited lower compressive and flexural strengths, a lower dynamic friction coefficient, and a higher wear rate. Its overall performance significantly differed from that of Examples 1, 2, and 3. Therefore, the TiN-SiN2O ceramic-modified C / C-SiC composite material provided by the present invention exhibits superior performance.

[0110] The above content is only for explaining the technical idea of ​​the present invention and cannot be used to limit the protection scope of the present invention. Any changes made on the basis of the technical solution in accordance with the technical idea proposed by the present invention shall fall within the protection scope of the claims of the present invention.

Claims

1. A TiN-SiN2O ceramic modified C / C-SiC brake material, characterized in that: The TiN-SiN2O ceramic modified C / C-SiC brake material uses TiN-SiN2O ceramic to modify the C / C-SiC material; The TiN-SiN2O ceramic modified C / C-SiC brake material is made of the following raw materials by volume percentage: 10-20% TiSi2 powder, 7-20% graphite powder, 15-20% phenolic resin powder, 10-13% SiC powder, 20-30% Si powder and 15-20% chopped carbon fiber.

2. The TiN-SiN2O ceramic modified C / C-SiC brake material according to claim 1, characterized in that: The TiN-SiN2O ceramic modified C / C-SiC brake material has a compressive strength of 270-290 MPa, a bending strength of 120-130 MPa, and a minimum wear rate of 2.05×10 -16 m 3 N -1 m -1 .

3. A method for preparing a TiN-SiN2O ceramic modified C / C-SiC brake material according to any one of claims 1 to 2, characterized in that: The following steps are involved: TiSi2 powder, graphite powder, phenolic resin powder, SiC powder and Si powder are uniformly mixed to obtain a mixed powder; short carbon fibers are added into anhydrous ethanol, stirred, dispersed, and dried to obtain dispersed fibers; mixing the mixed powder and the fiber to obtain a fiber mixed powder; The fiber mixed powder is molded to obtain a fiber reinforced resin block; curing the fiber-reinforced resin block to obtain a cured fiber-reinforced resin block; The cured fiber reinforced resin block is heat treated in a nitrogen atmosphere to obtain a TiN-SiN2O ceramic modified C / C-SiC brake material.

4. The method for preparing the TiN-SiN2O ceramic modified C / C-SiC brake material according to claim 3, characterized in that: The TiSi2 powder, graphite powder, phenolic resin powder, SiC powder and Si powder are ball-milled and mixed in a planetary ball mill at a rotation speed of 300-400 r / min and a ball-milling time of 2-3 h.

5. The method for preparing the TiN-SiN2O ceramic modified C / C-SiC brake material according to claim 3, characterized in that: The dispersion is performed under an ultrasonic power of 60-100 W, and the dispersion time is 10-15 minutes.

6. The method for preparing the TiN-SiN2O ceramic modified C / C-SiC brake material according to claim 3, characterized in that: The drying is carried out at a temperature of 50-80° C. and the drying time is 2-4 hours.

7. The method for preparing the TiN-SiN2O ceramic modified C / C-SiC brake material according to claim 3, characterized in that: The molding temperature is 160-190° C., the molding pressure is 7-10 MPa, and the molding time is 60-120 min.

8. The method for preparing the TiN-SiN2O ceramic modified C / C-SiC brake material according to claim 3, characterized in that: The curing process is a step-by-step curing process, and the specific process is as follows: heating to 160° C. and keeping it for 3 hours, then heating to 180° C. and keeping it for 3 hours, and finally heating to 220° C. and keeping it for 2 hours.

9. The method for preparing the TiN-SiN2O ceramic modified C / C-SiC brake material according to claim 3, characterized in that: The flow rate of the nitrogen gas is 80-120 mL / min.

10. The method for preparing the TiN-SiN2O ceramic modified C / C-SiC brake material according to claim 3, characterized in that: The heat treatment process is as follows: heating to 900-1000°C at a heating rate of 1-5°C / min, keeping warm for 1-2 hours, then heating to 1400-1500°C at a heating rate of 1-5°C / min, keeping warm for 2-3 hours, then cooling to 250-300°C at a cooling rate of 7-10°C / min, and then cooling to room temperature with the furnace.

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