WO2017107735A1 - Method for preparing carbon-ceramic brake material and method for preparing carbon-ceramic brake disc - Google Patents

Method for preparing carbon-ceramic brake material and method for preparing carbon-ceramic brake disc Download PDF

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WO2017107735A1
WO2017107735A1 PCT/CN2016/107047 CN2016107047W WO2017107735A1 WO 2017107735 A1 WO2017107735 A1 WO 2017107735A1 CN 2016107047 W CN2016107047 W CN 2016107047W WO 2017107735 A1 WO2017107735 A1 WO 2017107735A1
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carbon
ceramic
ceramic powder
phenolic resin
fiber preform
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刘军
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深圳市勒马制动科技有限公司
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    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/71Ceramic products containing macroscopic reinforcing agents
    • C04B35/78Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
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    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/80After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
    • C04B41/81Coating or impregnation
    • C04B41/85Coating or impregnation with inorganic materials
    • C04B41/87Ceramics
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16DCOUPLINGS FOR TRANSMITTING ROTATION; CLUTCHES; BRAKES
    • F16D65/00Parts or details
    • F16D65/02Braking members; Mounting thereof
    • F16D65/12Discs; Drums for disc brakes
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16DCOUPLINGS FOR TRANSMITTING ROTATION; CLUTCHES; BRAKES
    • F16D65/00Parts or details
    • F16D65/02Braking members; Mounting thereof
    • F16D65/12Discs; Drums for disc brakes
    • F16D65/125Discs; Drums for disc brakes characterised by the material used for the disc body
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    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/48Organic compounds becoming part of a ceramic after heat treatment, e.g. carbonising phenol resins
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16DCOUPLINGS FOR TRANSMITTING ROTATION; CLUTCHES; BRAKES
    • F16D2200/00Materials; Production methods therefor
    • F16D2200/0034Materials; Production methods therefor non-metallic
    • F16D2200/0039Ceramics
    • F16D2200/0047Ceramic composite, e.g. C/C composite infiltrated with Si or B, or ceramic matrix infiltrated with metal

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Abstract

Provided is a method for preparing a carbon-ceramic brake material, comprising the following steps: 1) preparing a first carbon fibre preform; 2) preparing a phenolic resin solution; 3) preparing a mixed slurry of the phenolic resin and a ceramic powder; 4) preparing a second carbon fibre preform; 5) drying the second carbon fibre preform; 6) hot pressing and curing the dried preform; 7) cracking a carbon/phenolic-ceramic composite material; and 8) processing a first porous carbon/carbon-ceramic powder composite material at high temperature. Provided is a method for preparing a carbon-ceramic brake disc, further comprising, in addition to the above 8 steps, the following steps: 9) pre-processing; 10) silicon infiltration processing a first brake disc; and 11) final processing.

Description

一种碳陶刹车材料的制备方法和一种碳陶刹车盘的制备方法Method for preparing carbon ceramic brake material and preparation method of carbon ceramic brake disc 技术领域Technical field
本发明涉及刹车材料技术领域,具体涉及一种碳陶刹车材料和刹车盘的制备方法。The invention relates to the technical field of brake materials, in particular to a method for preparing a carbon ceramic brake material and a brake disc.
背景技术Background technique
碳陶刹车材料作为一种新型刹车材料,与传统的金属和半金属刹车材料相比,其具有密度低、摩擦系数稳定、制动比大、不锈蚀和使用寿命长等优点,尤其是长时间连续刹车时不会产生热衰退。而与碳碳刹车材料相比,其具有优良的抗氧化性能及湿态摩擦性能衰减小、静摩擦系数高以及寿命长等突出优点,大大提高了刹车的安全性。其在飞机、坦克、高速列车以及高档轿车等刹车领域具有广泛的应用前景。As a new type of brake material, carbon ceramic brake material has the advantages of low density, stable friction coefficient, large braking ratio, no corrosion and long service life compared with traditional metal and semi-metal brake materials, especially for long time. There is no thermal decay when braking continuously. Compared with the carbon-carbon brake material, it has excellent oxidation resistance, low attenuation of wet friction performance, high static friction coefficient and long service life, which greatly improves the safety of the brake. It has broad application prospects in the field of braking such as airplanes, tanks, high-speed trains and high-end cars.
目前,德国SGL公司的碳陶刹车材料已成功应用于高档轿车,其寿命是钢刹车材料的4倍多,可满足轿车全寿命(行驶30多万公理)行驶无需更换刹车盘的需要。西北工业大学和西安航空制动科技有限公司的碳陶刹车盘已成功应用于军用飞机,大幅提高了刹车盘使用寿命,解决了碳碳刹车材料静刹车力矩低和湿态摩擦性能严重衰减的问题,提高了飞机刹车安全性。对高速列车来说,相对传统刹车材料不仅可以提高使用安全性和寿命,而且可显著降低列车的重量(约5吨/列),节约能源。 At present, the German SGL carbon-ceramic brake material has been successfully applied to high-end cars, and its life span is more than four times that of steel brake materials, which can meet the needs of the car's full life (driving more than 300,000 agong) without the need to replace the brake disc. The carbon ceramic brake discs of Northwestern Polytechnical University and Xi'an Aviation Brake Technology Co., Ltd. have been successfully applied to military aircraft, which greatly improved the service life of brake discs and solved the problem of low static braking torque and wet friction performance of carbon-carbon brake materials. Improve the safety of aircraft brakes. For high-speed trains, the use of conventional brake materials not only improves the safety and longevity of the use, but also significantly reduces the weight of the train (about 5 tons / column), saving energy.
碳陶刹车材料有以上优异性能,但应用推广速度很慢,主要原因是成本过高。目前碳陶刹车材料的制备方法有两种:一种是通常是通过短纤维预浸料热压裂解,再渗硅得到;但是在此工艺中,纤维首先浸树脂、烘干、短切,然后热压裂解,其制备工序复杂,而且得到的是短纤维增强的碳陶刹车材料,其性能较低,可靠性不及三维针刺结构的。另外一种是通过三维针刺预制体经化学气相沉积热解碳,再渗硅得到;但是此工艺的生产周期长,成本高,难以推广。Carbon ceramic brake materials have the above excellent performance, but the application promotion speed is very slow, mainly because the cost is too high. At present, there are two methods for preparing carbon ceramic brake materials: one is usually obtained by hot pressing cracking of short fiber prepreg, and then silicon is obtained; but in this process, the fiber is first impregnated with resin, dried, chopped, and then Hot pressing cracking, the preparation process is complicated, and the short fiber reinforced carbon ceramic brake material is obtained, and the performance is low, and the reliability is not as good as the three-dimensional needling structure. The other is obtained by chemical vapor deposition of pyrolysis carbon through three-dimensional acupuncture preforms, and then silicon is obtained; however, the production cycle of the process is long, the cost is high, and it is difficult to promote.
发明内容Summary of the invention
本发明为了避免现有技术的不足之处而提供了一种碳陶刹车材料和刹车盘的制备方法,该方法工艺简单,能大幅度降低材料的制造成本,生产出的碳陶刹车材料具有良好的力学、热物理、摩擦磨损性能。In order to avoid the deficiencies of the prior art, the present invention provides a method for preparing a carbon ceramic brake material and a brake disc, which has a simple process and can greatly reduce the manufacturing cost of the material, and the carbon ceramic brake material produced has good performance. Mechanics, thermophysics, friction and wear properties.
本发明的第一个目的可以通过采取如下技术方案达到:The first object of the present invention can be achieved by adopting the following technical solutions:
一种碳陶刹车材料的制备方法,包括以下步骤:A method for preparing a carbon ceramic brake material, comprising the following steps:
1)第一碳纤维预制体的制备:将若干层的单层0°无纬布、胎网、90°无纬布、胎网依次循环叠加至预设厚度,得到第一碳纤维预制体;1) preparation of the first carbon fiber preform: a plurality of layers of a single layer of 0° non-woven fabric, a tire mesh, a 90° laid fabric, and a tire mesh are sequentially cycled to a predetermined thickness to obtain a first carbon fiber preform;
2)酚醛树脂溶液的制备:将热塑性酚醛树脂、乙醇、丙酮和六次甲基四胺按重量份比1~2:1~3:1~3:0.1~0.2的比例进行混合,配制成酚醛树脂溶液;2) Preparation of phenolic resin solution: mixing thermoplastic phenolic resin, ethanol, acetone and hexamethylenetetramine in a ratio of 1 to 2:1 to 3:1 to 3:0.1 to 0.2 by weight to prepare phenolic resin Resin solution;
3)酚醛树脂与陶瓷粉混合浆料的制备:往所述酚醛树脂溶液中添加陶瓷粉,获得混合料,其中陶瓷粉的量为酚醛树脂溶液量的 20-50wt%;调节所述混合料的pH值为9-11后,球磨24-48h,配制成酚醛树脂与陶瓷粉混合浆料;3) Preparation of mixed slurry of phenolic resin and ceramic powder: adding ceramic powder to the phenolic resin solution to obtain a mixture, wherein the amount of the ceramic powder is the amount of the phenolic resin solution 20-50wt%; adjusting the pH of the mixture to 9-11, ball milling for 24-48h, formulated into a mixture of phenolic resin and ceramic powder;
4)第二碳纤维预制体的制备:在真空条件下,将所述第一碳纤维预制体浸入所述酚醛树脂与陶瓷粉混合浆料中,浸渗10-30min后,通过惰性气体加压,压力为1-2MPa,保压10-30min后;泄压,取出浸有酚醛树脂和陶瓷粉混合浆料的第一碳纤维预制体,获得第二碳纤维预制体;4) Preparation of a second carbon fiber preform: under vacuum, the first carbon fiber preform is immersed in the mixed slurry of the phenolic resin and the ceramic powder, impregnated for 10-30 minutes, and then pressurized by an inert gas, pressure After 1-2 MPa, after holding pressure for 10-30 min; releasing pressure, taking out the first carbon fiber preform impregnated with the mixed slurry of phenolic resin and ceramic powder to obtain a second carbon fiber preform;
5)第二碳纤维预制体烘干:将所述第二碳纤维预制体烘干,获得烘干预制体;烘干温度为40-60℃,干燥时间为12-24h;5) drying of the second carbon fiber preform: drying the second carbon fiber preform to obtain a dried preform; drying temperature is 40-60 ° C, drying time is 12-24 h;
6)烘干预制体热压固化:将所述烘干预制体在温度为150-180℃,压力为10-30MPa的条件下,保温15-30min后,固化得到碳/酚醛-陶瓷复合材料;6) drying the preform to be hot-pressed: the dried preform is cured at a temperature of 150-180 ° C and a pressure of 10-30 MPa for 15-30 min to obtain a carbon/phenolic-ceramic composite;
7)碳/酚醛-陶瓷复合材料裂解:将所述碳/酚醛-陶瓷复合材料在惰性气体保护的条件下进行裂解处理,得到第一多孔碳/碳-陶瓷粉复合材料;7) carbon/phenolic-ceramic composite cracking: the carbon/phenolic-ceramic composite material is subjected to cracking treatment under inert gas protection to obtain a first porous carbon/carbon-ceramic powder composite material;
8)第一多孔碳/碳-陶瓷粉复合材料进行高温处理:将所述第一多孔碳/碳-陶瓷粉复合材料在惰性气体保护的条件下进行高温处理,得到第二多孔碳/碳-陶瓷粉复合材料,即最终的碳陶刹车材料。8) The first porous carbon/carbon-ceramic powder composite material is subjected to high temperature treatment: the first porous carbon/carbon-ceramic powder composite material is subjected to high temperature treatment under inert gas protection to obtain a second porous carbon. / Carbon-ceramic powder composite, the ultimate carbon ceramic brake material.
优选地,步骤1)中采用接力式针刺方法制备所述第一碳纤维预制体。Preferably, the first carbon fiber preform is prepared in a step 1) by a relay needle punching method.
优选地,步骤1)中针刺密度为30针/cm2,体积密度为0.3-0.45g/cm3,其中胎网层与无纬布层的体积比为1:1-2。 Preferably, the needle density in step 1) is 30 needles/cm 2 and the bulk density is 0.3-0.45 g/cm 3 , wherein the volume ratio of the tire web layer to the non-woven fabric layer is 1:1-2.
优选地,步骤3)中所述陶瓷粉的主要成分为SiC、B4C或BN;所述陶瓷粉的粒度为0.5-5μm。Preferably, the main component of the ceramic powder in the step 3) is SiC, B 4 C or BN; and the ceramic powder has a particle size of 0.5-5 μm.
优选地,步骤3)中滴入氨水和盐酸调节所述混合料的pH值。Preferably, ammonia and water are added dropwise in step 3) to adjust the pH of the mixture.
优选地,步骤3)中在球磨机上对所述混合料进行球磨。Preferably, the mixture is ball milled in a ball mill in step 3).
优选地,步骤4)中真空压力为1000Pa。Preferably, the vacuum pressure in step 4) is 1000 Pa.
优选地,步骤4)、步骤7)和步骤8)中所述惰性气体为氩气或氮气。Preferably, the inert gas in step 4), step 7) and step 8) is argon or nitrogen.
优选地,步骤7)中所述碳/酚醛-陶瓷复合材料裂解处理时,裂解升温速度为1-5℃/min,最高裂解温度为900-1100℃;步骤8)中将所述第一多孔碳/碳-陶瓷粉复合材料进行高温处理时,所述热处理温度为1800-2000℃,保温1h。Preferably, in the cracking treatment of the carbon/phenolic-ceramic composite in step 7), the pyrolysis heating rate is 1-5 ° C / min, the highest cracking temperature is 900-1100 ° C; the first plurality in step 8) When the pore carbon/carbon-ceramic powder composite material is subjected to high temperature treatment, the heat treatment temperature is 1800-2000 ° C, and the temperature is kept for 1 h.
本发明的第二个目的可以通过采取如下技术方案达到:The second object of the present invention can be achieved by adopting the following technical solutions:
一种碳陶刹车盘的制备方法,包括以下步骤:A method for preparing a carbon ceramic brake disc comprises the following steps:
1)第一碳纤维预制体的制备:将若干层的单层0°无纬布、胎网、90°无纬布、胎网依次循环叠加至预设厚度,得到第一碳纤维预制体;1) preparation of the first carbon fiber preform: a plurality of layers of a single layer of 0° non-woven fabric, a tire mesh, a 90° laid fabric, and a tire mesh are sequentially cycled to a predetermined thickness to obtain a first carbon fiber preform;
2)酚醛树脂溶液的制备:将热塑性酚醛树脂、乙醇、丙酮和六次甲基四胺按重量份比1~2:1~3:1~3:0.1~0.2的比例进行混合,配制成酚醛树脂溶液;2) Preparation of phenolic resin solution: mixing thermoplastic phenolic resin, ethanol, acetone and hexamethylenetetramine in a ratio of 1 to 2:1 to 3:1 to 3:0.1 to 0.2 by weight to prepare phenolic resin Resin solution;
3)酚醛树脂与陶瓷粉混合浆料的制备:往所述酚醛树脂溶液中添加陶瓷粉,获得混合料,其中陶瓷粉的量为酚醛树脂溶液量的20-50wt%;调节所述混合料的pH值为9-11后,球磨24-48h,配制成酚醛树脂与陶瓷粉混合浆料; 3) preparation of a mixed slurry of a phenolic resin and a ceramic powder: adding a ceramic powder to the phenolic resin solution to obtain a mixture, wherein the amount of the ceramic powder is 20-50% by weight of the amount of the phenolic resin solution; adjusting the mixture After the pH value is 9-11, the ball mill is used for 24-48 hours, and is prepared into a mixed slurry of phenolic resin and ceramic powder;
4)第二碳纤维预制体的制备:在真空条件下,将所述第一碳纤维预制体浸入所述酚醛树脂与陶瓷粉混合浆料中,浸渗10-30min后,通过惰性气体加压,压力为1-2MPa,保压10-30min后;泄压,取出浸有酚醛树脂和陶瓷粉混合浆料的第一碳纤维预制体,获得第二碳纤维预制体;4) Preparation of a second carbon fiber preform: under vacuum, the first carbon fiber preform is immersed in the mixed slurry of the phenolic resin and the ceramic powder, impregnated for 10-30 minutes, and then pressurized by an inert gas, pressure After 1-2 MPa, after holding pressure for 10-30 min; releasing pressure, taking out the first carbon fiber preform impregnated with the mixed slurry of phenolic resin and ceramic powder to obtain a second carbon fiber preform;
5)第二碳纤维预制体烘干:将所述第二碳纤维预制体烘干,获得烘干预制体;烘干温度为40-60℃,干燥时间为12-24h;5) drying of the second carbon fiber preform: drying the second carbon fiber preform to obtain a dried preform; drying temperature is 40-60 ° C, drying time is 12-24 h;
6)烘干预制体热压固化:将所述烘干预制体在温度为150-180℃,压力为10-30MPa的条件下,保温15-30min后,固化得到碳/酚醛-陶瓷复合材料;6) drying the preform to be hot-pressed: the dried preform is cured at a temperature of 150-180 ° C and a pressure of 10-30 MPa for 15-30 min to obtain a carbon/phenolic-ceramic composite;
7)碳/酚醛-陶瓷复合材料裂解:将所述碳/酚醛-陶瓷复合材料在惰性气体保护的条件下进行裂解处理,得到第一多孔碳/碳-陶瓷粉复合材料;7) carbon/phenolic-ceramic composite cracking: the carbon/phenolic-ceramic composite material is subjected to cracking treatment under inert gas protection to obtain a first porous carbon/carbon-ceramic powder composite material;
8)第一多孔碳/碳-陶瓷粉复合材料进行高温处理:将所述第一多孔碳/碳-陶瓷粉复合材料在惰性气体保护的条件下进行高温处理,得到第二多孔碳/碳-陶瓷粉复合材料;8) The first porous carbon/carbon-ceramic powder composite material is subjected to high temperature treatment: the first porous carbon/carbon-ceramic powder composite material is subjected to high temperature treatment under inert gas protection to obtain a second porous carbon. /carbon-ceramic powder composite;
9)预加工:将所述第二多孔碳/碳-陶瓷粉复合材料按照刹车盘的预设图纸进行加工,获得第一刹车盘;9) pre-processing: processing the second porous carbon/carbon-ceramic powder composite material according to a preset drawing of the brake disc to obtain a first brake disc;
10)第一刹车盘的渗硅处理:将所述第一刹车盘在真空炉中进行渗硅处理,获得第二刹车盘;浸渗温度为1600-1800℃,保温时间为1~5h;10) siliconizing treatment of the first brake disc: the first brake disc is subjected to siliconizing treatment in a vacuum furnace to obtain a second brake disc; the infiltration temperature is 1600-1800 ° C, and the holding time is 1 to 5 h;
11)终加工:将所述第二刹车盘的两摩擦面按照预设要求进行磨 削加工,得到碳陶刹车盘。11) Final processing: grinding the two friction surfaces of the second brake disc according to preset requirements Cutting, get carbon ceramic brake discs.
其中,碳陶刹车盘也可以称为碳陶刹车片。Among them, carbon ceramic brake discs can also be called carbon ceramic brake pads.
优选地,步骤9)中将所述第二多孔碳/碳-陶瓷粉复合材料按照刹车盘的预设图纸进行加工时,其中摩擦面的厚度方向单面预留0.3-1mm的加工余量。Preferably, in the step 9), when the second porous carbon/carbon-ceramic powder composite material is processed according to a preset drawing of the brake disc, a machining allowance of 0.3-1 mm is reserved on one side of the thickness direction of the friction surface. .
本发明所提供的技术方案可以包括以下有益效果:The technical solution provided by the present invention may include the following beneficial effects:
(1)本发明所提供的制备方法其制备周期短,成本低。浸渍浆料采用酚醛树脂和陶瓷粉混合浆料,并采用热压固化,在材料裂解时提高固相产率,能保证一次浸渍裂解就能达到渗硅需要的预制体密度要求,降低制备周期。因为如果采用纯酚醛树脂溶液为浸渍液,常压固化,裂解这样的工艺,通常需要3-4次浸渍裂解过程才能达到要求。(1) The preparation method provided by the present invention has a short preparation cycle and low cost. The impregnating slurry adopts a mixed slurry of phenolic resin and ceramic powder, and adopts hot pressing curing to improve the solid phase yield during material cracking, which can ensure the requirement of preform density required for silicon infiltration by one impregnation cracking, and reduce the preparation cycle. Because if a pure phenolic resin solution is used as the impregnation liquid, the atmospheric pressure solidification, and the cracking process, it usually takes 3-4 times of the impregnation cracking process to meet the requirements.
(2)采用本发明所提供的方法制备的三维针刺碳纤维预制体,其中的胎网体积含量较目前市场上使用的三维针刺碳纤维预制体的体积大1倍多,使最终的碳陶刹车材料中陶瓷含量提高,从而大幅提高了材料的耐摩擦磨损性能。(2) A three-dimensional needle-punched carbon fiber preform prepared by the method provided by the present invention, wherein the volume of the tire mesh is more than twice as large as that of the three-dimensional needle-punched carbon fiber preform currently used on the market, so that the final carbon ceramic brake The ceramic content of the material is increased, which greatly improves the friction and wear resistance of the material.
(3)本发明所提供的碳陶刹车盘制备方法中,对碳陶刹车材料进行预加工后再进行渗硅处理,大大降低加工难度和加工成本。因为渗硅前材料强度低,易加工,渗硅后材料硬度和强度增大,难加工。(3) In the method for preparing a carbon ceramic brake disc provided by the present invention, the carbon ceramic brake material is pre-processed and then subjected to siliconizing treatment, thereby greatly reducing processing difficulty and processing cost. Because the material strength is low and easy to process before siliconizing, the hardness and strength of the material after siliconizing increase, which is difficult to process.
(4)本发明所提供碳陶刹车材料和刹车盘的制备方法工艺过程简单、可重复性好,适于工业化批量生产。 (4) The preparation method of the carbon ceramic brake material and the brake disc provided by the invention is simple in process, good in repeatability, and suitable for industrial mass production.
具体实施方式detailed description
下面,结合附图以及具体实施方式,对本发明做进一步描述:The present invention will be further described below in conjunction with the drawings and specific embodiments.
实施例1Example 1
步骤1,第一碳纤维预制体的制备;将若干层的单层0°无纬布、胎网、90°无纬布、胎网依次循环叠加至设计厚度,采用接力式针刺方法制备得到;针刺密度为30针/cm2,体积密度约为0.3g/cm3,其中胎网层与无纬布层的体积比约为1:1。Step 1, the preparation of the first carbon fiber preform; a plurality of layers of a single layer of 0° non-woven fabric, a tire mesh, a 90° non-woven fabric, and a tire mesh are sequentially cycled to a design thickness, and are prepared by a relay acupuncture method; The needle density is 30 needles/cm 2 and the bulk density is about 0.3 g/cm 3 , wherein the volume ratio of the tire web layer to the non-woven fabric layer is about 1:1.
步骤2,酚醛树脂溶液的制备;将热塑性酚醛树脂、乙醇、丙酮和六次甲基四胺按重量份比1:1:1:0.1比例进行混合,配制成酚醛树脂溶液。Step 2: preparation of a phenolic resin solution; mixing a thermoplastic phenolic resin, ethanol, acetone and hexamethylenetetramine in a ratio of 1:1:1:0.1 by weight to prepare a phenolic resin solution.
步骤3,酚醛树脂和陶瓷粉混合浆料的制备;往步骤2制备的酚醛树脂溶液中添加主要成分为SiC、粒度为1μm的陶瓷粉,陶瓷粉的量为酚醛树脂溶液量的35wt%;然后滴入氨水和盐酸调节该混合料的pH值为11;将混合料在球磨机上球磨48h,配制成酚醛树脂和陶瓷粉混合浆料。Step 3, preparing a mixed slurry of a phenolic resin and a ceramic powder; adding a ceramic powder having a main component of SiC and a particle size of 1 μm to the phenolic resin solution prepared in the step 2, wherein the amount of the ceramic powder is 35 wt% of the amount of the phenolic resin solution; Aqueous ammonia and hydrochloric acid were added dropwise to adjust the pH of the mixture to 11; the mixture was ball milled in a ball mill for 48 hours to prepare a mixed slurry of a phenol resin and a ceramic powder.
步骤4,第二碳纤维预制体的制备;在真空条件(1000Pa)下将步骤1的第一碳纤维预制体浸入步骤3的酚醛树脂和陶瓷粉混合浆料中,浸渗10min;对浸有预制体的浆料通过氮气加压,压力为1MPa,保压30min;泄压并取出浸有酚醛树脂及陶瓷粉的第一碳纤维预制体,获得第二碳纤维预制体。Step 4, preparation of the second carbon fiber preform; the first carbon fiber preform of the step 1 is immersed in the mixed slurry of the phenol resin and the ceramic powder of the step 3 under vacuum condition (1000 Pa), impregnated for 10 min; The slurry was pressurized by nitrogen, the pressure was 1 MPa, and the pressure was maintained for 30 minutes; the first carbon fiber preform impregnated with the phenol resin and the ceramic powder was taken out and the second carbon fiber preform was obtained.
步骤5,第二碳纤维预制体烘干;将步骤4的第二碳纤维预制体置于烘箱内烘干,获得烘干预制体;烘干温度为40℃,干燥时间为 24h。Step 5, the second carbon fiber preform is dried; the second carbon fiber preform of step 4 is dried in an oven to obtain a dried preform; the drying temperature is 40 ° C, and the drying time is 24h.
步骤6:烘干预制体的热压固化;将步骤5的烘干预制体在150℃,压力30MPa的条件下,保温30min,固化得到碳/酚醛-陶瓷复合材料。Step 6: drying the preform by hot pressing; the dried preform of step 5 is heated at 150 ° C under a pressure of 30 MPa for 30 min to obtain a carbon/phenolic-ceramic composite.
步骤7:碳/酚醛-陶瓷复合材料裂解;将步骤6制备的碳/酚醛-陶瓷复合材料进行裂解处理,升温速度为5℃/min,最高裂解温度为1000℃,用氩气作为保护性气体,得到第一多孔C/C-SiC复合材料。Step 7: Cleavage of carbon/phenolic-ceramic composite; the carbon/phenolic-ceramic composite prepared in step 6 is subjected to cracking treatment at a heating rate of 5 ° C/min, a maximum cracking temperature of 1000 ° C, and argon gas as a protective gas. The first porous C/C-SiC composite material is obtained.
步骤8:第一多孔C/C-SiC复合材料进行高温处理;将步骤7制备的第一多孔C/C-SiC复合材料在氩气下进行高温处理,得到第二多孔C/C-SiC复合材料;热处理温度为1800℃,保温时间1h。Step 8: The first porous C/C-SiC composite material is subjected to high temperature treatment; the first porous C/C-SiC composite material prepared in the step 7 is subjected to high temperature treatment under argon to obtain a second porous C/C. - SiC composite material; heat treatment temperature is 1800 ° C, holding time 1 h.
步骤9:预加工;将步骤8制备的第二多孔C/C-SiC复合材料按照刹车盘的产品图纸进行加工,其中摩擦面的厚度方向单面预留0.5mm加工余量,其余尺寸按图纸加工到产品尺寸要求,获得第一刹车盘。Step 9: Pre-processing; the second porous C/C-SiC composite material prepared in the step 8 is processed according to the product drawing of the brake disc, wherein the thickness of the friction surface is reserved for 0.5 mm machining allowance on one side, and the remaining dimensions are The drawings are machined to the product size requirements to obtain the first brake disc.
步骤10:第一刹车盘渗硅处理;将步骤9加工好的第一刹车盘在真空炉中进行渗硅处理,获得第二刹车盘;浸渗温度为1650℃,保温5h。Step 10: The first brake disc is siliconized; the first brake disc processed in step 9 is subjected to siliconizing treatment in a vacuum furnace to obtain a second brake disc; the infiltration temperature is 1650 ° C, and the heat is kept for 5 h.
步骤11:终加工。将步骤10的第二刹车盘的两摩擦面按照产品要求进行磨削加工,得到碳陶刹车盘。Step 11: Final processing. The two friction surfaces of the second brake disc of step 10 are ground according to the product requirements to obtain a carbon ceramic brake disc.
实施例2Example 2
步骤1,第一碳纤维预制体的制备;将若干层的单层0°无纬布、胎网、90°无纬布、胎网依次循环叠加至设计厚度,采用接力式针刺 方法制备得到;针刺密度为30针/cm2,体积密度约为0.45g/cm3,其中胎网层与无纬布层的体积比约为1:2。Step 1, the preparation of the first carbon fiber preform; a plurality of layers of a single layer of 0° non-woven fabric, a tire mesh, a 90° non-woven fabric, and a tire mesh are sequentially cycled to a design thickness, and are prepared by a relay acupuncture method; The needle density is 30 needles/cm 2 and the bulk density is about 0.45 g/cm 3 , wherein the volume ratio of the tire web layer to the non-woven fabric layer is about 1:2.
步骤2,酚醛树脂溶液的制备;将热塑性酚醛树脂、乙醇、丙酮和六次甲基四胺按重量份比2:1:1:0.2比例进行混合,配制成酚醛树脂溶液。Step 2: preparation of a phenolic resin solution; mixing a thermoplastic phenolic resin, ethanol, acetone and hexamethylenetetramine in a ratio of 2:1:1:0.2 by weight to prepare a phenolic resin solution.
步骤3,酚醛树脂和陶瓷粉混合浆料的制备;往步骤2制备的酚醛树脂溶液中添加主要成分为B4C、粒度为5μm的陶瓷粉,陶瓷粉的量为酚醛树脂溶液量的50wt%;然后滴入氨水和盐酸调节该混合料的pH值为11;将混合料在球磨机上球磨48h,配制成酚醛树脂和陶瓷粉混合浆料。Step 3, preparing a mixed slurry of a phenolic resin and a ceramic powder; adding a ceramic powder having a main component of B 4 C and a particle size of 5 μm to the phenolic resin solution prepared in the step 2, the amount of the ceramic powder being 50% by weight of the amount of the phenolic resin solution Then, ammonia water and hydrochloric acid were added dropwise to adjust the pH of the mixture to 11; the mixture was ball milled in a ball mill for 48 hours to prepare a mixed slurry of a phenol resin and a ceramic powder.
步骤4,第二碳纤维预制体的制备;在真空条件(1000Pa)下将步骤1的第一碳纤维预制体浸入步骤3的酚醛树脂和陶瓷粉混合浆料中,浸渗10min;对浸有预制体的浆料通过氮气加压,压力为1.5MPa,保压30min;泄压并取出浸有酚醛树脂及陶瓷粉的第一碳纤维预制体,获得第二碳纤维预制体。Step 4, preparation of the second carbon fiber preform; the first carbon fiber preform of the step 1 is immersed in the mixed slurry of the phenol resin and the ceramic powder of the step 3 under vacuum condition (1000 Pa), impregnated for 10 min; The slurry was pressurized by nitrogen, the pressure was 1.5 MPa, and the pressure was maintained for 30 minutes; the first carbon fiber preform impregnated with the phenol resin and the ceramic powder was taken out and the second carbon fiber preform was obtained.
步骤5,第二碳纤维预制体烘干;将步骤4的第二碳纤维预制体置于烘箱内烘干,获得烘干预制体;烘干温度为60℃,干燥时间为12h。Step 5, the second carbon fiber preform is dried; the second carbon fiber preform of step 4 is dried in an oven to obtain a dried preform; the drying temperature is 60 ° C, and the drying time is 12 h.
步骤6:烘干预制体的热压固化;将步骤5的烘干预制体在180℃,压力10MPa的条件下,保温15min,固化得到碳/酚醛-陶瓷复合材料。Step 6: drying the preform by hot pressing; the dried preform of step 5 is heated at 180 ° C under a pressure of 10 MPa for 15 min to obtain a carbon/phenolic-ceramic composite.
步骤7:碳/酚醛-陶瓷复合材料裂解;将步骤6制备的碳/酚醛-陶瓷复合材料进行裂解处理,升温速度为2℃/min,最高裂解温度为 1100℃,用氩气作为保护性气体,得到第一多孔C/C-B4C复合材料。Step 7: Carbon/phenolic-ceramic composite cracking; the carbon/phenolic-ceramic composite prepared in step 6 is subjected to cracking treatment at a heating rate of 2 ° C/min, a maximum cracking temperature of 1100 ° C, and argon gas as a protective gas. The first porous C/CB 4 C composite was obtained.
步骤8:第一多孔C/C-B4C复合材料进行高温处理;将步骤7制备的第一多孔C/C-B4C复合材料在氩气下进行高温处理,得到第二多孔C/C-B4C复合材料;热处理温度为2000℃,保温时间1h。Step 8: The first porous C/CB 4 C composite material is subjected to high temperature treatment; the first porous C/CB 4 C composite material prepared in the step 7 is subjected to high temperature treatment under argon to obtain a second porous C/CB. 4 C composite material; heat treatment temperature is 2000 ° C, holding time 1 h.
步骤9:预加工;将步骤8制备的第二多孔C/C-B4C复合材料按照刹车盘的产品图纸进行加工,其中摩擦面的厚度方向单面预留0.3mm加工余量,其余尺寸按图纸加工到产品尺寸要求,获得第一刹车盘。Step 9: Pre-processing; the second porous C/CB 4 C composite material prepared in the step 8 is processed according to the product drawing of the brake disc, wherein a 0.3 mm machining allowance is reserved on one side of the thickness direction of the friction surface, and the remaining dimensions are The drawings are machined to the product size requirements to obtain the first brake disc.
步骤10:第一刹车盘渗硅处理;将步骤9加工好的第一刹车盘在真空炉中进行渗硅处理,获得第二刹车盘;浸渗温度为1700℃,保温2h。Step 10: The first brake disc is siliconized; the first brake disc processed in step 9 is subjected to siliconizing treatment in a vacuum furnace to obtain a second brake disc; the infiltration temperature is 1700 ° C, and the heat is kept for 2 h.
步骤11:终加工。将步骤10的第二刹车盘的两摩擦面按照产品要求进行磨削加工,得到碳陶刹车盘。Step 11: Final processing. The two friction surfaces of the second brake disc of step 10 are ground according to the product requirements to obtain a carbon ceramic brake disc.
实施例3Example 3
步骤1,第一碳纤维预制体的制备;将若干层的单层0°无纬布、胎网、90°无纬布、胎网依次循环叠加至设计厚度,采用接力式针刺方法制备得到;针刺密度为30针/cm2,体积密度约为0.4g/cm3,其中胎网层与无纬布层的体积比约为1:1.5。Step 1, the preparation of the first carbon fiber preform; a plurality of layers of a single layer of 0° non-woven fabric, a tire mesh, a 90° non-woven fabric, and a tire mesh are sequentially cycled to a design thickness, and are prepared by a relay acupuncture method; The needle density is 30 needles/cm 2 and the bulk density is about 0.4 g/cm 3 , wherein the volume ratio of the tire web layer to the non-woven fabric layer is about 1:1.5.
步骤2,酚醛树脂溶液的制备;将热塑性酚醛树脂、乙醇、丙酮和六次甲基四胺按重量份比1.5:2:2:0.15比例进行混合,配制成酚醛树脂溶液。 Step 2: preparation of a phenolic resin solution; mixing a thermoplastic phenolic resin, ethanol, acetone and hexamethylenetetramine in a ratio of 1.5:2:2:0.15 by weight to prepare a phenolic resin solution.
步骤3,酚醛树脂和陶瓷粉混合浆料的制备;往步骤2制备的酚醛树脂溶液中添加主要成分为BN、粒度为0.5μm的陶瓷粉,陶瓷粉的量为酚醛树脂溶液量的35wt%;然后滴入氨水和盐酸调节该混合料的pH值为9;将混合料在球磨机上球磨24h,配制成酚醛树脂和陶瓷粉混合浆料。Step 3, the preparation of the mixed slurry of the phenolic resin and the ceramic powder; adding the ceramic powder having a main component of BN and a particle size of 0.5 μm to the phenolic resin solution prepared in the step 2, the amount of the ceramic powder being 35 wt% of the amount of the phenolic resin solution; Then, ammonia water and hydrochloric acid were added dropwise to adjust the pH of the mixture to 9; the mixture was ball milled in a ball mill for 24 hours to prepare a mixed slurry of a phenol resin and a ceramic powder.
步骤4,第二碳纤维预制体的制备;在真空条件(1000Pa)下将步骤1的第一碳纤维预制体浸入步骤3的酚醛树脂和陶瓷粉混合浆料中,浸渗30min;对浸有预制体的浆料通过氮气加压,压力为1MPa,保压10min;泄压并取出浸有酚醛树脂及陶瓷粉的第一碳纤维预制体,获得第二碳纤维预制体。Step 4, preparation of the second carbon fiber preform; the first carbon fiber preform of the step 1 is immersed in the mixed slurry of the phenol resin and the ceramic powder of the step 3 under vacuum condition (1000 Pa), impregnated for 30 min; The slurry was pressurized by nitrogen, the pressure was 1 MPa, and the pressure was maintained for 10 minutes; the first carbon fiber preform impregnated with the phenol resin and the ceramic powder was taken out and the second carbon fiber preform was obtained.
步骤5,第二碳纤维预制体烘干;将步骤4的第二碳纤维预制体置于烘箱内烘干,获得烘干预制体;烘干温度为45℃,干燥时间为20h。Step 5, the second carbon fiber preform is dried; the second carbon fiber preform of step 4 is dried in an oven to obtain a dried preform; the drying temperature is 45 ° C, and the drying time is 20 h.
步骤6:烘干预制体的热压固化;将步骤5的烘干预制体在160℃,压力20MPa的条件下,保温20min,固化得到碳/酚醛-陶瓷复合材料。Step 6: drying the preform by hot pressing; the dried preform of step 5 is heated at 160 ° C under a pressure of 20 MPa for 20 min to obtain a carbon/phenolic-ceramic composite.
步骤7:碳/酚醛-陶瓷复合材料裂解;将步骤6制备的碳/酚醛-陶瓷复合材料进行裂解处理,升温速度为3℃/min,最高裂解温度为900℃,用氩气作为保护性气体,得到第一多孔C/C-BN复合材料。Step 7: carbon/phenolic-ceramic composite cracking; the carbon/phenolic-ceramic composite prepared in step 6 is subjected to cracking treatment at a heating rate of 3 ° C/min, a maximum cracking temperature of 900 ° C, and argon gas as a protective gas. The first porous C/C-BN composite material was obtained.
步骤8:第一多孔C/C-BN复合材料进行高温处理;将步骤7制备的第一多孔C/C-BN复合材料在氩气下进行高温处理,得到第二多孔C/C-BN复合材料;热处理温度为1900℃,保温时间1h。Step 8: The first porous C/C-BN composite material is subjected to high temperature treatment; the first porous C/C-BN composite material prepared in the step 7 is subjected to high temperature treatment under argon to obtain a second porous C/C. -BN composite material; heat treatment temperature is 1900 ° C, holding time 1 h.
步骤9:预加工;将步骤8制备的第二多孔C/C-BN复合材料按 照刹车盘的产品图纸进行加工,其中摩擦面的厚度方向单面预留1mm加工余量,其余尺寸按图纸加工到产品尺寸要求,获得第一刹车盘。Step 9: pre-processing; the second porous C/C-BN composite material prepared in step 8 is pressed According to the product drawings of the brake disc, the machining surface of the friction surface is reserved with a machining allowance of 1 mm on one side, and the remaining dimensions are processed according to the drawings to obtain the first brake disc.
步骤10:第一刹车盘渗硅处理;将步骤9加工好的第一刹车盘在真空炉中进行渗硅处理,获得第二刹车盘;浸渗温度为1800℃,保温1h。Step 10: The first brake disc is siliconized; the first brake disc processed in step 9 is subjected to siliconizing treatment in a vacuum furnace to obtain a second brake disc; the infiltration temperature is 1800 ° C, and the heat is kept for 1 h.
步骤11:终加工。将步骤10的第二刹车盘的两摩擦面按照产品要求进行磨削加工,得到碳陶刹车盘。Step 11: Final processing. The two friction surfaces of the second brake disc of step 10 are ground according to the product requirements to obtain a carbon ceramic brake disc.
对本领域的技术人员来说,可根据以上描述的技术方案以及构思,做出其它各种相应的改变以及形变,而所有的这些改变以及形变都应该属于本发明权利要求的保护范围之内。 Various other changes and modifications may be made by those skilled in the art in light of the above-described technical solutions and concepts, and all such changes and modifications are intended to fall within the scope of the appended claims.

Claims (10)

  1. 一种碳陶刹车材料的制备方法,其特征在于,包括以下步骤:A method for preparing a carbon ceramic brake material, comprising the steps of:
    1)第一碳纤维预制体的制备:将若干层的单层0°无纬布、胎网、90°无纬布、胎网依次循环叠加至预设厚度,得到第一碳纤维预制体;1) preparation of the first carbon fiber preform: a plurality of layers of a single layer of 0° non-woven fabric, a tire mesh, a 90° laid fabric, and a tire mesh are sequentially cycled to a predetermined thickness to obtain a first carbon fiber preform;
    2)酚醛树脂溶液的制备:将热塑性酚醛树脂、乙醇、丙酮和六次甲基四胺按重量份比1~2:1~3:1~3:0.1~0.2的比例进行混合,配制成酚醛树脂溶液;2) Preparation of phenolic resin solution: mixing thermoplastic phenolic resin, ethanol, acetone and hexamethylenetetramine in a ratio of 1 to 2:1 to 3:1 to 3:0.1 to 0.2 by weight to prepare phenolic resin Resin solution;
    3)酚醛树脂与陶瓷粉混合浆料的制备:往所述酚醛树脂溶液中添加陶瓷粉,获得混合料,其中陶瓷粉的量为酚醛树脂溶液量的20-50wt%;调节所述混合料的pH值为9-11后,球磨24-48h,配制成酚醛树脂与陶瓷粉混合浆料;3) preparation of a mixed slurry of a phenolic resin and a ceramic powder: adding a ceramic powder to the phenolic resin solution to obtain a mixture, wherein the amount of the ceramic powder is 20-50% by weight of the amount of the phenolic resin solution; adjusting the mixture After the pH value is 9-11, the ball mill is used for 24-48 hours, and is prepared into a mixed slurry of phenolic resin and ceramic powder;
    4)第二碳纤维预制体的制备:在真空条件下,将所述第一碳纤维预制体浸入所述酚醛树脂与陶瓷粉混合浆料中,浸渗10-30min后,通过惰性气体加压,压力为1-2MPa,保压10-30min后;泄压,取出浸有酚醛树脂和陶瓷粉混合浆料的第一碳纤维预制体,获得第二碳纤维预制体;4) Preparation of a second carbon fiber preform: under vacuum, the first carbon fiber preform is immersed in the mixed slurry of the phenolic resin and the ceramic powder, impregnated for 10-30 minutes, and then pressurized by an inert gas, pressure After 1-2 MPa, after holding pressure for 10-30 min; releasing pressure, taking out the first carbon fiber preform impregnated with the mixed slurry of phenolic resin and ceramic powder to obtain a second carbon fiber preform;
    5)第二碳纤维预制体烘干:将所述第二碳纤维预制体烘干,获得烘干预制体;烘干温度为40-60℃,干燥时间为12-24h;5) drying of the second carbon fiber preform: drying the second carbon fiber preform to obtain a dried preform; drying temperature is 40-60 ° C, drying time is 12-24 h;
    6)烘干预制体的热压固化:将所述烘干预制体在温度为150-180℃,压力为10-30MPa的条件下,保温15-30min后,固化得到碳/酚醛-陶瓷复合材料;6) Drying and curing of the preform: the dried preform is cured at a temperature of 150-180 ° C and a pressure of 10-30 MPa for 15-30 min to obtain a carbon/phenolic-ceramic composite. ;
    7)碳/酚醛-陶瓷复合材料裂解:将所述碳/酚醛-陶瓷复合材料在惰性气体保护的条件下进行裂解处理,得到第一多孔碳/碳-陶瓷粉复 合材料;7) Carbon/phenolic-ceramic composite cracking: the carbon/phenolic-ceramic composite is subjected to cracking treatment under inert gas protection to obtain a first porous carbon/carbon-ceramic powder complex. Composite material
    8)第一多孔碳/碳-陶瓷粉复合材料进行高温处理:将所述第一多孔碳/碳-陶瓷粉复合材料在惰性气体保护的条件下进行高温处理,得到第二多孔碳/碳-陶瓷粉复合材料,即最终的碳陶刹车材料。8) The first porous carbon/carbon-ceramic powder composite material is subjected to high temperature treatment: the first porous carbon/carbon-ceramic powder composite material is subjected to high temperature treatment under inert gas protection to obtain a second porous carbon. / Carbon-ceramic powder composite, the ultimate carbon ceramic brake material.
  2. 根据权利要求1所述的碳陶刹车材料的制备方法,其特征在于,步骤1)中采用接力式针刺方法制备所述第一碳纤维预制体。The method for preparing a carbon ceramic brake material according to claim 1, wherein the first carbon fiber preform is prepared by a relay needle punching method in the step 1).
  3. 根据权利要求1所述的碳陶刹车材料的制备方法,其特征在于,步骤1)中针刺密度为30针/cm2,体积密度为0.3-0.45g/cm3,其中胎网层与无纬布层的体积比为1:1-2。The method for preparing a carbon ceramic brake material according to claim 1, wherein the needle density in step 1) is 30 needles/cm 2 and the bulk density is 0.3-0.45 g/cm 3 , wherein the tire mesh layer has no The volume ratio of the weft layer is 1:1-2.
  4. 根据权利要求1所述的碳陶刹车材料的制备方法,其特征在于,步骤3)中所述陶瓷粉的主要成分为SiC、B4C或BN;所述陶瓷粉的粒度为0.5-5μm。The method for preparing a carbon ceramic brake material according to claim 1, wherein the main component of the ceramic powder in the step 3) is SiC, B 4 C or BN; and the ceramic powder has a particle size of 0.5-5 μm.
  5. 根据权利要求1所述的碳陶刹车材料的制备方法,其特征在于,步骤3)中滴入氨水和盐酸调节所述混合料的pH值。The method for preparing a carbon ceramic brake material according to claim 1, wherein the pH of the mixture is adjusted by adding ammonia water and hydrochloric acid to the step 3).
  6. 根据权利要求1所述的碳陶刹车材料的制备方法,其特征在于,步骤4)中真空压力为1000Pa。The method for preparing a carbon ceramic brake material according to claim 1, wherein the vacuum pressure in step 4) is 1000 Pa.
  7. 根据权利要求1所述的碳陶刹车材料的制备方法,其特征在于,步骤4)、步骤7)和步骤8)中所述惰性气体为氩气或氮气。The method for preparing a carbon ceramic brake material according to claim 1, wherein the inert gas in the step 4), the step 7) and the step 8) is argon or nitrogen.
  8. 根据权利要求1所述的碳陶刹车材料的制备方法,其特征在于,步骤7)中所述碳/酚醛-陶瓷复合材料裂解处理时,裂解升温速度为1-5℃/min,最高裂解温度为900-1100℃;步骤8)中将所述第一多孔碳/碳-陶瓷粉复合材料进行高温处理时,所述热处理温度为 1800-2000℃,保温1h。The method for preparing a carbon ceramic brake material according to claim 1, wherein in the cracking treatment of the carbon/phenolic-ceramic composite material in the step 7), the pyrolysis heating rate is 1-5 ° C / min, and the highest cracking temperature is obtained. When the first porous carbon/carbon-ceramic powder composite material is subjected to high temperature treatment in 900-1100 ° C; in step 8), the heat treatment temperature is 1800-2000 ° C, heat preservation 1h.
  9. 一种根据权利要求1-8任意一项所述的碳陶刹车材料的制备方法的碳陶刹车盘的制备方法,其特征在于,包括以下步骤:A method for preparing a carbon ceramic brake disc according to a method for preparing a carbon ceramic brake material according to any one of claims 1-8, characterized in that it comprises the following steps:
    1)第一碳纤维预制体的制备:将若干层的单层0°无纬布、胎网、90°无纬布、胎网依次循环叠加至预设厚度,得到第一碳纤维预制体;1) preparation of the first carbon fiber preform: a plurality of layers of a single layer of 0° non-woven fabric, a tire mesh, a 90° laid fabric, and a tire mesh are sequentially cycled to a predetermined thickness to obtain a first carbon fiber preform;
    2)酚醛树脂溶液的制备:将热塑性酚醛树脂、乙醇、丙酮和六次甲基四胺按重量份比1~2:1~3:1~3:0.1~0.2的比例进行混合,配制成酚醛树脂溶液;2) Preparation of phenolic resin solution: mixing thermoplastic phenolic resin, ethanol, acetone and hexamethylenetetramine in a ratio of 1 to 2:1 to 3:1 to 3:0.1 to 0.2 by weight to prepare phenolic resin Resin solution;
    3)酚醛树脂与陶瓷粉混合浆料的制备:往所述酚醛树脂溶液中添加陶瓷粉,获得混合料,其中陶瓷粉的量为酚醛树脂溶液量的20-50wt%;调节所述混合料的pH值为9-11后,球磨24-48h,配制成酚醛树脂与陶瓷粉混合浆料;3) preparation of a mixed slurry of a phenolic resin and a ceramic powder: adding a ceramic powder to the phenolic resin solution to obtain a mixture, wherein the amount of the ceramic powder is 20-50% by weight of the amount of the phenolic resin solution; adjusting the mixture After the pH value is 9-11, the ball mill is used for 24-48 hours, and is prepared into a mixed slurry of phenolic resin and ceramic powder;
    4)第二碳纤维预制体的制备:在真空条件下,将所述第一碳纤维预制体浸入所述酚醛树脂与陶瓷粉混合浆料中,浸渗10-30min后,通过惰性气体加压,压力为1-2MPa,保压10-30min后;泄压,取出浸有酚醛树脂和陶瓷粉混合浆料的第一碳纤维预制体,获得第二碳纤维预制体;4) Preparation of a second carbon fiber preform: under vacuum, the first carbon fiber preform is immersed in the mixed slurry of the phenolic resin and the ceramic powder, impregnated for 10-30 minutes, and then pressurized by an inert gas, pressure After 1-2 MPa, after holding pressure for 10-30 min; releasing pressure, taking out the first carbon fiber preform impregnated with the mixed slurry of phenolic resin and ceramic powder to obtain a second carbon fiber preform;
    5)第二碳纤维预制体烘干:将所述第二碳纤维预制体烘干,获得烘干预制体;烘干温度为40-60℃,干燥时间为12-24h;5) drying of the second carbon fiber preform: drying the second carbon fiber preform to obtain a dried preform; drying temperature is 40-60 ° C, drying time is 12-24 h;
    6)烘干预制体的热压固化:将所述烘干预制体在温度为150-180℃,压力为10-30MPa的条件下,保温15-30min后,固化得到碳/酚醛-陶瓷复合材料; 6) Drying and curing of the preform: the dried preform is cured at a temperature of 150-180 ° C and a pressure of 10-30 MPa for 15-30 min to obtain a carbon/phenolic-ceramic composite. ;
    7)碳/酚醛-陶瓷复合材料裂解:将所述碳/酚醛-陶瓷复合材料在惰性气体保护的条件下进行裂解处理,得到第一多孔碳/碳-陶瓷粉复合材料;7) carbon/phenolic-ceramic composite cracking: the carbon/phenolic-ceramic composite material is subjected to cracking treatment under inert gas protection to obtain a first porous carbon/carbon-ceramic powder composite material;
    8)第一多孔碳/碳-陶瓷粉复合材料进行高温处理:将所述第一多孔碳/碳-陶瓷粉复合材料在惰性气体保护的条件下进行高温处理,得到第二多孔碳/碳-陶瓷粉复合材料;8) The first porous carbon/carbon-ceramic powder composite material is subjected to high temperature treatment: the first porous carbon/carbon-ceramic powder composite material is subjected to high temperature treatment under inert gas protection to obtain a second porous carbon. /carbon-ceramic powder composite;
    9)预加工:将所述第二多孔碳/碳-陶瓷粉复合材料按照刹车盘的预设图纸进行加工,获得第一刹车盘;9) pre-processing: processing the second porous carbon/carbon-ceramic powder composite material according to a preset drawing of the brake disc to obtain a first brake disc;
    10)第一刹车盘的渗硅处理:将所述第一刹车盘在真空炉中进行渗硅处理,获得第二刹车盘;浸渗温度为1600-1800℃,保温时间为1-5h;10) siliconizing treatment of the first brake disc: the first brake disc is subjected to siliconizing treatment in a vacuum furnace to obtain a second brake disc; the infiltration temperature is 1600-1800 ° C, and the holding time is 1-5 h;
    11)终加工:将所述第二刹车盘的两摩擦面按照预设要求进行磨削加工,得到碳陶刹车盘。11) Final processing: the two friction surfaces of the second brake disc are ground according to a preset requirement to obtain a carbon ceramic brake disc.
  10. 根据权利要求9所述的碳陶刹车盘的制备方法,其特征在于,步骤9)中将所述第二多孔碳/碳-陶瓷粉复合材料按照刹车盘的预设图纸进行加工时,其中摩擦面的厚度方向单面预留0.3-1mm的加工余量。 The method for preparing a carbon ceramic brake disc according to claim 9, wherein in the step 9), the second porous carbon/carbon-ceramic powder composite material is processed according to a preset drawing of the brake disc, wherein A machining allowance of 0.3-1 mm is reserved on one side in the thickness direction of the friction surface.
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