CN106966751A - High-performance and low-cost C/C SiC ceramic matrix composite material brake discs and preparation method and application - Google Patents
High-performance and low-cost C/C SiC ceramic matrix composite material brake discs and preparation method and application Download PDFInfo
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Abstract
本发明涉及一种高性能低成本C/C‑SiC复合材料制动盘及其制备方法与应用,制备方法包括:将制动盘预制体碳化,采用化学气相渗积法将碳化后的制动盘预制体致密化得到C/C复合材料;然后在惰性气氛中进行热处理,以提高复合材料的石墨化度;再进行机械加工,得到C/C复合材料坯体;利用熔融渗硅法处理C/C复合材料坯体,得到C/C‑SiC复合材料制动盘;再利用化学气相渗积法或先驱体浸渍裂解法对C/C‑SiC复合材料制动盘进行处理;将得到的产品机械加工成最终的设计尺寸,即得复合材料制动盘成品。本发明提供的C/C‑SiC复合材料制动盘及其制备方法,可以降低制备成本,提高制动盘的力学性能、导热性能和摩擦磨损性能。The invention relates to a high-performance and low-cost C/C‑SiC composite brake disc and its preparation method and application. The disc preform is densified to obtain a C/C composite material; then heat treatment is performed in an inert atmosphere to increase the degree of graphitization of the composite material; then mechanical processing is performed to obtain a C/C composite material green body; the C/C composite material is processed by fusion siliconization /C composite material green body to obtain a C/C-SiC composite material brake disc; then use the chemical vapor infiltration method or the precursor impregnation cracking method to process the C/C-SiC composite material brake disc; the obtained product Machining to the final design size, that is, the finished product of the composite material brake disc. The C/C-SiC composite brake disc and the preparation method thereof provided by the invention can reduce the preparation cost and improve the mechanical properties, thermal conductivity and friction and wear properties of the brake disc.
Description
技术领域technical field
本发明涉及复合材料制备技术领域,具体涉及一种高性能低成本C/C-SiC复合材料制动盘及其制备方法与应用。The invention relates to the technical field of composite material preparation, in particular to a high-performance and low-cost C/C-SiC composite brake disc and its preparation method and application.
背景技术Background technique
高速铁路(以下称“高铁”)是世界轨道交通发展的潮流,目前我国高铁投入运营的里程已达到10000公里,正在建设中的高速铁路10000多公里,预计到2021年中国高铁总里程将超过30000公里,居世界第一。高铁快速发展的同时,其安全性也备受瞩目,其中制动技术对于列车安全运行至关重要。目前,高铁采用的制动方式主要包括电制动和空气制动,此外还有涡流制动、磁轨制动和风阻制动等制动方式。其中空气制动作为一种紧急制动手段,当高速列车遭遇地震、停电或列车故障等紧急情况时,必须确保高速的列车能够在规定的距离之内停车,保证列车运行的安全,因此空气制动又称“基础制动”,是高铁制动系统中不可或缺的重要组成部分。High-speed railway (hereinafter referred to as "high-speed railway") is the trend of the world's rail transit development. At present, the mileage of my country's high-speed railway has reached 10,000 kilometers, and the high-speed railway under construction is more than 10,000 kilometers. It is estimated that by 2021, the total mileage of China's high-speed railway will exceed 30,000 kilometers, ranking first in the world. With the rapid development of high-speed rail, its safety has also attracted much attention, among which braking technology is crucial to the safe operation of trains. At present, the braking methods used by high-speed rail mainly include electric braking and air braking, and there are also braking methods such as eddy current braking, magnetic rail braking and wind resistance braking. Among them, air braking is an emergency braking method. When a high-speed train encounters an emergency such as an earthquake, a power outage, or a train failure, it must be ensured that the high-speed train can stop within a specified distance to ensure the safety of the train. Therefore, air braking Braking, also known as "basic braking", is an indispensable and important part of the high-speed rail braking system.
空气制动主要采用轴盘制动和轮盘制动两种盘形制动方式,其区别主要在于轴盘制动是在车轴上安装制动盘,而轮盘制动是在车轮辐板侧面安装制动盘。当前制动盘材料主要以铸铁、铸钢和锻钢为主,其优点主要是制造技术成熟,性能可以满足速度较低列车的制动要求。然而随着列车不断向“高速化”和“重载化”方向发展,对制动盘提出了既具有较高制动能量又要有较轻质量的要求,但是现有制动盘材料耐磨性差,磨损较快,散热效果不佳,容易产生热裂纹,重量较重,摩擦产生较大的噪音,因而不能很好的满足列车速度需要不断提高的发展需求。The air brake mainly adopts two disc brake methods: shaft disc brake and wheel disc brake. Install the brake disc. At present, the materials of brake discs are mainly cast iron, cast steel and forged steel. The main advantages are that the manufacturing technology is mature, and the performance can meet the braking requirements of low-speed trains. However, with the continuous development of trains in the direction of "high speed" and "heavy load", the brake discs are required to have both high braking energy and light weight, but the existing brake disc materials are wear-resistant Poor performance, fast wear, poor heat dissipation, prone to thermal cracks, heavy weight, and high noise caused by friction, so it cannot well meet the development needs of trains with continuously increasing speed.
发明内容Contents of the invention
针对现有技术中的缺陷,本发明目的在于提供一种高性能低成本C/C-SiC复合材料制动盘及其制备方法与应用,以降低制备成本,提高制动盘的力学性能、导热性能和摩擦磨损性能。Aiming at the defects in the prior art, the purpose of the present invention is to provide a high-performance and low-cost C/C-SiC composite brake disc and its preparation method and application, so as to reduce the preparation cost and improve the mechanical properties and thermal conductivity of the brake disc. performance and friction and wear properties.
为实现上述目的,本发明提供的技术方案为:To achieve the above object, the technical solution provided by the invention is:
第一方面,本发明提供了一种复合材料制动盘的制备方法,包括如下步骤:In a first aspect, the present invention provides a method for preparing a composite material brake disc, comprising the following steps:
S1:将制动盘预制体碳化,然后采用化学气相渗积法将碳化后的制动盘预制体致密化,得到C/C复合材料;其中,制动盘预制体是采用聚丙烯腈基预氧丝纤维以三维针刺而成;S2:将C/C复合材料在惰性气氛中进行热处理,得到C/C复合材料坯体;S3:利用熔融渗硅法处理C/C复合材料坯体,得到C/C-SiC复合材料制动盘;S4:将C/C-SiC复合材料制动盘利用化学气相渗积法或先驱体浸渍裂解法进行处理;其中,化学气相渗积法的先驱体为三氯甲基硅烷,先驱体浸渍裂解法的先驱体溶液为聚碳硅烷与二乙烯基苯的混合溶液;S5:将步骤S4得到的产品机械加工成最终的设计尺寸,即得复合材料制动盘成品。S1: Carbonize the brake disc prefabricated body, and then use the chemical vapor deposition method to densify the carbonized brake disc prefabricated body to obtain a C/C composite material; wherein, the brake disc prefabricated body is made of polyacrylonitrile-based prefabricated Oxygen silk fibers are formed by three-dimensional needle punching; S2: heat-treating the C/C composite material in an inert atmosphere to obtain a C/C composite material green body; S3: treating the C/C composite material green body by fusion siliconizing method, Obtain the C/C-SiC composite brake disc; S4: process the C/C-SiC composite brake disc using chemical vapor deposition or precursor impregnation cracking; wherein, the precursor of chemical vapor deposition It is trichloromethylsilane, and the precursor solution of the precursor dipping and cracking method is a mixed solution of polycarbosilane and divinylbenzene; S5: the product obtained in step S4 is mechanically processed into the final design size to obtain a composite material. Finished disc.
需要说明的是,三维针刺法是将单层0°无纬布、胎网、90°无纬布和胎网依次循环叠加,然后采用接力式针刺的方法在垂直于铺层方向引入聚丙烯腈基预氧丝纤维,制成制动盘预制体。在步骤S3的熔融渗硅过程中,熔硅与基体C反应生成碳化硅,冷却至室温后体积收缩导致微裂纹的产生;复合材料在熔融渗硅的高温逐渐冷却至室温的过程中,由于复合材料中纤维、热解碳、碳化硅和残余硅的热膨胀系数存在差异,使得冷却过程中产生应力,在应力的作用下产生微裂纹。步骤S4是为了填封C/C-SiC复合材料制动盘的裂纹,降低复合材料中Si的残余量,提高复合材料的抗蠕变性能。It should be noted that in the three-dimensional acupuncture method, a single layer of 0° no-weft fabric, tire mesh, 90° no-weft fabric and tire mesh are stacked in sequence, and then the relay-type acupuncture method is used to introduce polyacrylamide in the direction perpendicular to the laying layer. Acrylonitrile-based pre-oxygenated silk fibers are used to make brake disc preforms. During the molten siliconizing process of step S3, the molten silicon reacts with the matrix C to form silicon carbide, and the volume shrinks after cooling to room temperature, resulting in the generation of microcracks; The thermal expansion coefficients of fiber, pyrolytic carbon, silicon carbide, and residual silicon are different in the material, which causes stress during the cooling process, and microcracks are generated under the action of stress. Step S4 is to fill the cracks of the C/C-SiC composite brake disc, reduce the residual amount of Si in the composite material, and improve the creep resistance of the composite material.
在本发明的进一步实施方式中,步骤S1中,化学气相渗积法具体为:以丙烷、天然气和丙烯中的一种或几种为碳源气体,氮气和/或氢气为稀释气体,渗积温度为900~1200℃,渗积压力为1000~5000Pa,渗积时间为50~200h;其中,碳源气体和稀释气体的体积比为1:(1~4)。In a further embodiment of the present invention, in step S1, the chemical vapor deposition method is specifically: using one or more of propane, natural gas and propylene as the carbon source gas, nitrogen and/or hydrogen as the dilution gas, and the infiltration The temperature is 900-1200°C, the infiltration pressure is 1000-5000Pa, and the infiltration time is 50-200h; wherein, the volume ratio of carbon source gas and dilution gas is 1:(1-4).
在本发明的进一步实施方式中,步骤S2中,热处理的处理温度为1800~2400℃,处理时间1~5h,惰性气氛为氩气和/或氮气。热处理是为了提高复合材料的石墨化程度。In a further embodiment of the present invention, in step S2, the heat treatment temperature is 1800-2400° C., the treatment time is 1-5 hours, and the inert atmosphere is argon and/or nitrogen. Heat treatment is to improve the degree of graphitization of composite materials.
在本发明的进一步实施方式中,步骤S3中,熔融渗硅法具体为:在真空条件下,将C/C复合材料坯体置于粒径为100~300目的硅粉中,然后1500~1700℃保温1.5~3.5h,再1750~2050℃保温5~60min。In a further embodiment of the present invention, in step S3, the molten siliconizing method is specifically: under vacuum conditions, the C/C composite body is placed in silicon powder with a particle size of 100-300 mesh, and then 1500-1700 mesh Keep warm at ℃ for 1.5~3.5h, then keep warm at 1750~2050℃ for 5~60min.
需要说明的是:为了满足反应比需要,可以根据C/C-SiC复合材料制动盘的预期密度和C/C复合材料坯体密度之差计算出熔融渗硅过程中需要生成的SiC的含量,从而计算出Si、C反应中理论需要的Si量,称取理论需要Si的量的2.2~5倍Si粉置于石墨坩埚中,Si粉的纯度优选大于或等于99%,并将C/C制动盘坯体掩埋于Si粉中,然后放入高温炉中进行熔融渗硅,制得的C/C-SiC复合材料制动盘,密度优选为1.8~2.2g/cm3。为了节约生产成本,还可以将多个装有Si粉和C/C复合材料坯体的石墨坩埚同时叠置于高温炉中进行熔融渗硅。熔融渗硅过程中,熔融硅在毛细管力和重力的共同作用下由C/C复合材料坯体的孔隙渗入到材料内部,同时与接触到的热解碳发生反应生成SiC基体相,得到C/C-SiC复合材料制动盘,少量未反应的熔融Si残留在C/C-SiC复合材料制动盘中。It should be noted that in order to meet the requirements of the reaction ratio, the content of SiC that needs to be generated during the molten siliconizing process can be calculated according to the difference between the expected density of the C/C-SiC composite brake disc and the density of the C/C composite body , so as to calculate the theoretically required amount of Si in the reaction of Si and C, take 2.2 to 5 times Si powder of the theoretically required amount of Si and place it in a graphite crucible. The purity of the Si powder is preferably greater than or equal to 99%, and the C/ The C brake disc green body is buried in Si powder, and then placed in a high temperature furnace for molten silicon infiltration, and the prepared C/C-SiC composite brake disc has a density of preferably 1.8-2.2 g/cm 3 . In order to save production costs, multiple graphite crucibles filled with Si powder and C/C composite body can also be stacked in a high-temperature furnace at the same time for fusion siliconization. During the fusion siliconizing process, the molten silicon infiltrates into the interior of the material from the pores of the C/C composite body under the combined action of capillary force and gravity, and reacts with the pyrolytic carbon in contact to form a SiC matrix phase, resulting in a C/C composite material. C-SiC composite brake disc, a small amount of unreacted molten Si remains in the C/C-SiC composite brake disc.
在本发明的进一步实施方式中,步骤S4中,化学气相渗积法具体为:以三氯甲基硅烷为先驱体(CH3SiCl3,MTS),氢气为载气,氩气为稀释气,渗积温度为900~1400℃,渗积压力为300~1200Pa,渗积时间为15~25h;其中,三氯甲基硅烷、氢气和氩气的体积比为1:(7~10):(3~5)。需要说明的是,MTS为液态先驱体原料,氢气为载气,通过鼓泡方式将气态MTS带入反应室,采用惰性气体氩气作为稀释气体以调节MTS的热解反应速率。In a further embodiment of the present invention, in step S4, the chemical vapor deposition method is specifically: using trichloromethylsilane as a precursor (CH 3 SiCl 3 , MTS), hydrogen as a carrier gas, and argon as a diluent gas, The infiltration temperature is 900~1400℃, the infiltration pressure is 300~1200Pa, and the infiltration time is 15~25h; among them, the volume ratio of trichloromethylsilane, hydrogen and argon is 1:(7~10):( 3~5). It should be noted that MTS is a liquid precursor raw material, and hydrogen is used as a carrier gas. The gaseous MTS is brought into the reaction chamber by bubbling, and the inert gas argon is used as a diluent gas to adjust the pyrolysis reaction rate of MTS.
在本发明的进一步实施方式中,步骤S4中,先驱体浸渍裂解法具体为:将C/C-SiC复合材料制动盘浸渍于聚碳硅烷与二乙烯基苯的混合溶液30~60min,浸渍温度为60~100℃,浸渍压力为1~2MPa,然后110~200℃固化交联2~3.5h,再1100~1300℃裂解0.5~2h;重复先驱体浸渍裂解法的步骤直至裂纹被完全填封;其中,聚碳硅烷与二乙烯基苯的混合溶液中聚碳硅烷的质量分数为40%~60%。In a further embodiment of the present invention, in step S4, the precursor immersion cracking method specifically includes: immersing the C/C-SiC composite brake disc in a mixed solution of polycarbosilane and divinylbenzene for 30-60 minutes, then immersing The temperature is 60-100°C, the impregnation pressure is 1-2MPa, then curing and cross-linking at 110-200°C for 2-3.5 hours, and then cracking at 1100-1300°C for 0.5-2 hours; repeat the steps of the precursor impregnation cracking method until the cracks are completely filled seal; wherein, the mass fraction of polycarbosilane in the mixed solution of polycarbosilane and divinylbenzene is 40% to 60%.
在本发明的进一步实施方式中,步骤S1中,碳化的温度为1000~1400℃,时间为45~75h,碳化在真空条件下进行。In a further embodiment of the present invention, in step S1, the carbonization temperature is 1000-1400° C., the time is 45-75 hours, and the carbonization is carried out under vacuum conditions.
在本发明的进一步实施方式中,在步骤S2的热处理之后,得到C/C复合材料坯体之前,还包括机械加工的步骤,具体包括:将热处理后的C/C复合材料表面加工出螺栓孔和定位孔;和/或对C/C复合材料四周的尺寸进行加工,并在厚度方向留出1~2mm的后续加工余量。需要说明的是:将热处理后的C/C复合材料进行机械加工,可以是根据制动盘的孔径尺寸要求,在热处理后的C/C复合材料表面加工出螺栓孔和定位孔;按制动盘尺寸的负公差要求,对C/C复合材料四周的尺寸进行加工,并在厚度方向留出1~2mm的后续加工余量。步骤S5的机械加工可以是根据制动盘的尺寸进行一次性的彻底加工,也可以是在此步机械加工的基础上,将制得的C/C-SiC复合材料制动盘在磨床上采用金刚石砂轮对摩擦面进行表面加工,去除之前预留的1~2mm的后续加工余量。In a further embodiment of the present invention, after the heat treatment in step S2, before obtaining the C/C composite body, a step of mechanical processing is also included, specifically including: machining bolt holes on the surface of the C/C composite material after heat treatment and positioning holes; and/or process the dimensions around the C/C composite material, and leave a subsequent processing allowance of 1 to 2 mm in the thickness direction. It should be noted that: machining the heat-treated C/C composite material can be based on the aperture size requirements of the brake disc, machining bolt holes and positioning holes on the surface of the heat-treated C/C composite material; Negative tolerance requirements of the disk size, the size around the C/C composite material is processed, and a subsequent processing allowance of 1 to 2 mm is left in the thickness direction. The mechanical processing in step S5 can be a one-time thorough processing according to the size of the brake disc, or it can be based on this step of mechanical processing, and the prepared C/C-SiC composite brake disc is used on a grinding machine. The diamond grinding wheel performs surface processing on the friction surface, and removes the previously reserved 1-2mm subsequent processing allowance.
第二方面,本发明提供了根据上述任一项的方法制备得到的复合材料制动盘。In a second aspect, the present invention provides a composite brake disc prepared according to any one of the above methods.
第三方面,本发明提供了上述复合材料制动盘在制造列车尤其是制造高铁中的应用。In a third aspect, the present invention provides the application of the above-mentioned composite material brake disc in the manufacture of trains, especially in the manufacture of high-speed rail.
本发明提供的复合材料制动盘及其制备方法,有如下积极效果:(1)本发明首次提出用聚丙烯腈基预氧丝纤维作为高铁用碳陶双基复合材料制动盘的增强体,提供了一种可批量生产的制造技术。预氧丝纤维相对碳纤维价格非常低廉,制备预制体时大大降低了制备成本;预氧丝纤维断裂延伸率高,柔韧性好,适合针刺,而碳纤维为脆性材料,且表面为沟槽结构,针刺时纤维受到的阻力大,易从勾刺上脱落或断裂滑出,因此预氧丝预制体较碳纤维预制体表面平整,Z向纤维的引入数量和长度高,所制备得到的碳陶双基复合材料Z向导热系数高,层间结合力强,摩擦磨损性能优异,特别适合做列车尤其是高铁制动盘材料。(2)本发明采用化学气相渗积法(CVI)或先驱体浸渍裂解法(PIP)对熔融渗硅后的C/C-SiC复合材料制动盘进行填封裂纹处理,处理后的C/C-Si复合材料制动盘几乎不含裂纹,提高了其力学性能;而且PIP法处理所产生的多余C还可以与熔融渗硅处理后材料中残余的Si进行反应生成SiC,降低了复合材料中Si的残余量,提高了复合材料的抗蠕变性能。(3)本发明选择在两个不同的高温环境下进行熔融渗硅,这种反应方式可以使Si与基体中的C反应的更加充分,减少C/C-SiC复合材料中的闭孔数量和残余硅的含量,提高复合材料抗蠕变性能、均匀性和力学性能,减少摩擦磨损量。(4)当基体中热解碳含量过高时会导致力学性能降低,过低时则会导致陶瓷基体含量过高,制动盘脆性高,同时摩擦系数过高。本发明通过调节基体中的热解碳的含量,实现对复合材料中基体碳与碳化硅含量的控制,从而使复合材料的力学性能和摩擦磨损性能达到均衡的效果。The composite material brake disc provided by the invention and the preparation method thereof have the following positive effects: (1) the present invention proposes to use polyacrylonitrile-based pre-oxidized silk fiber as the reinforcing body of the carbon-ceramic double-base composite brake disc for high-speed rail for the first time, providing A manufacturing technique that can be mass-produced. Compared with carbon fiber, the price of pre-oxidized silk fiber is very low, and the preparation cost is greatly reduced when preparing the preform; the pre-oxidized silk fiber has a high elongation at breakage, good flexibility, and is suitable for acupuncture, while carbon fiber is a brittle material with a grooved surface. When needling, the fiber is subjected to great resistance, and it is easy to fall off or break off from the hook. Therefore, the surface of the pre-oxidized fiber preform is smoother than that of the carbon fiber preform, and the number and length of the Z-direction fibers are higher. The prepared carbon-ceramic double-matrix composite Material Z has high thermal conductivity, strong interlayer bonding, and excellent friction and wear properties, and is especially suitable for trains, especially high-speed rail brake disc materials. (2) The present invention adopts chemical vapor infiltration (CVI) or precursor impregnated cracking method (PIP) to carry out sealing crack treatment to the C/C-SiC composite material brake disk after molten siliconizing, the C/C after processing The C-Si composite brake disc has almost no cracks, which improves its mechanical properties; and the excess C produced by the PIP method can also react with the residual Si in the material after the molten siliconizing treatment to form SiC, which reduces the composite material. The residual amount of Si improves the creep resistance of the composite material. (3) The present invention chooses to carry out fusion siliconizing under two different high-temperature environments, and this reaction mode can make Si and the C reaction in the matrix more fully, reduce the number of closed cells and the number of closed cells in the C/C-SiC composite material The content of residual silicon improves the creep resistance, uniformity and mechanical properties of the composite material, and reduces the amount of friction and wear. (4) When the pyrolytic carbon content in the matrix is too high, the mechanical properties will be reduced, and if it is too low, the content of the ceramic matrix will be too high, the brake disc will be highly brittle, and the friction coefficient will be too high. The invention controls the content of matrix carbon and silicon carbide in the composite material by adjusting the content of pyrolytic carbon in the matrix, so that the mechanical properties and friction and wear properties of the composite material can be balanced.
本发明的附加方面和优点将在下面的描述中部分给出,部分将从下面的描述中变得明显,或通过本发明的实践了解到。Additional aspects and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention.
附图说明Description of drawings
图1为本发明实施例中的熔融渗硅示意图。Fig. 1 is a schematic diagram of fused siliconization in an embodiment of the present invention.
附图标记:Reference signs:
1-高温加热炉;2-感应加热体;3-硅粉;4-石墨坩埚;5-C/C复合材料坯体。1-High temperature heating furnace; 2-Induction heating body; 3-Silicon powder; 4-Graphite crucible; 5-C/C composite material green body.
具体实施方式detailed description
下面将结合本发明实施例中的附图,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。The following will clearly and completely describe the technical solutions in the embodiments of the present invention with reference to the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only some, not all, embodiments of the present invention. Based on the embodiments of the present invention, all other embodiments obtained by persons of ordinary skill in the art without making creative efforts belong to the protection scope of the present invention.
下述实施例中的实验方法,如无特殊说明,均为常规方法。The experimental methods in the following examples are conventional methods unless otherwise specified.
下述实施例中所用的试验材料,如无特殊说明,均为自常规试剂商店购买得到的。The test materials used in the following examples, unless otherwise specified, were purchased from conventional reagent stores.
以下实施例中的定量试验,均设置三次重复实验,数据为三次重复实验的平均值或平均值±标准差。In the quantitative experiments in the following examples, three repeated experiments were set up, and the data were the mean value or mean ± standard deviation of the three repeated experiments.
本发明提供一种复合材料制动盘的制备方法,其特征在于,包括如下步骤:The invention provides a method for preparing a composite material brake disc, which is characterized in that it comprises the following steps:
S1:将制动盘预制体碳化,然后采用化学气相渗积法将碳化后的制动盘预制体致密化,得到C/C复合材料;其中,制动盘预制体是采用聚丙烯腈基预氧丝纤维以三维针刺而成;碳化的温度为1000~1400℃,时间为45~75h,碳化在真空条件下进行;化学气相渗积法具体为:以丙烷、天然气和丙烯中的一种或几种为碳源气体,氮气和/或氢气为稀释气体,渗积温度为900~1200℃,渗积压力为1000~5000Pa,渗积时间为50~200h;其中,碳源气体和稀释气体的体积比为1:(1~4)。S1: Carbonize the brake disc prefabricated body, and then use the chemical vapor deposition method to densify the carbonized brake disc prefabricated body to obtain a C/C composite material; wherein, the brake disc prefabricated body is made of polyacrylonitrile-based prefabricated Oxygen silk fibers are formed by three-dimensional needle punching; the carbonization temperature is 1000-1400°C, the time is 45-75h, and the carbonization is carried out under vacuum conditions; the chemical vapor deposition method is specifically: one of propane, natural gas and propylene or several kinds of carbon source gas, nitrogen and/or hydrogen as dilution gas, infiltration temperature is 900-1200°C, infiltration pressure is 1000-5000Pa, and infiltration time is 50-200h; among them, carbon source gas and dilution gas The volume ratio is 1:(1~4).
S2:将C/C复合材料在惰性气氛中进行热处理,提高复合材料的石墨化度;热处理的处理温度为1800~2400℃,处理时间1~5h,惰性气氛为氩气和/或氮气。将热处理后的C/C复合材料进行机械加工得到C/C复合材料坯体,具体包括:将热处理后的C/C复合材料表面加工出螺栓孔和定位孔;和/或对C/C复合材料四周的尺寸进行加工,并在厚度方向留出1~2mm的后续加工余量。S2: Heat-treat the C/C composite material in an inert atmosphere to increase the degree of graphitization of the composite material; the heat treatment temperature is 1800-2400°C, the treatment time is 1-5h, and the inert atmosphere is argon and/or nitrogen. Machining the heat-treated C/C composite material to obtain a C/C composite material green body, specifically including: machining bolt holes and positioning holes on the surface of the heat-treated C/C composite material; and/or machining the C/C composite material The dimensions around the material are processed, and a subsequent processing allowance of 1 to 2 mm is left in the thickness direction.
S3:利用熔融渗硅法处理C/C复合材料坯体,得到C/C-SiC复合材料制动盘;熔融渗硅法具体为:在真空条件下,将C/C复合材料坯体置于粒径为100~300目的硅粉中,然后1500~1700℃保温1.5~3.5h,再1750~2050℃保温5~60min。S3: process the C/C composite material green body by the molten siliconizing method to obtain a C/C-SiC composite material brake disc; the molten siliconizing method is specifically: under vacuum conditions, place the C/C composite material green body The particle size is 100-300 mesh silicon powder, then keep warm at 1500-1700°C for 1.5-3.5h, and then keep warm at 1750-2050°C for 5-60min.
S4:利用化学气相渗积法或先驱体浸渍裂解法对C/C-SiC复合材料制动盘进行填封微裂纹处理;其中,化学气相渗积法的先驱体为三氯甲基硅烷,先驱体浸渍裂解法的先驱体溶液为聚碳硅烷与二乙烯基苯的混合溶液;化学气相渗积法具体为:以三氯甲基硅烷(CH3SiCl3,MTS)为先驱体,氢气为载气,氩气为稀释气,渗积温度为900~1400℃,渗积压力为300~1200Pa,渗积时间为15~25h;其中,三氯甲基硅烷、氢气和氩气的体积比为1:(7~10):(3~5);先驱体浸渍裂解法具体为:在真空条件下,将C/C-SiC复合材料制动盘浸渍于聚碳硅烷与二乙烯基苯的混合溶液30~60min,浸渍温度为60~100℃,浸渍压力为1~2MPa,然后110~200℃固化交联2~3.5h,再1100~1300℃裂解0.5~2h;重复先驱体浸渍裂解法直至裂纹被完全填封;其中,聚碳硅烷与二乙烯基苯的混合溶液中聚碳硅烷的质量分数为40%~60%。S4: Use the chemical vapor deposition method or the precursor impregnation cracking method to seal the microcracks of the C/C-SiC composite brake disc; wherein, the precursor of the chemical vapor deposition method is trichloromethylsilane, the precursor The precursor solution of the bulk impregnation cracking method is a mixed solution of polycarbosilane and divinylbenzene; the chemical vapor deposition method is specifically: trichloromethylsilane (CH 3 SiCl 3 , MTS) as the precursor, hydrogen as the carrier Gas, argon is the dilution gas, the infiltration temperature is 900-1400°C, the infiltration pressure is 300-1200Pa, and the infiltration time is 15-25h; among them, the volume ratio of trichloromethylsilane, hydrogen and argon is 1 :(7~10):(3~5); Precursor impregnation cracking method is specifically: under vacuum conditions, the C/C-SiC composite brake disc is immersed in the mixed solution of polycarbosilane and divinylbenzene 30-60min, impregnation temperature is 60-100°C, impregnation pressure is 1-2MPa, then curing and crosslinking at 110-200°C for 2-3.5h, and then cleavage at 1100-1300°C for 0.5-2h; repeat the precursor immersion cracking method until the crack It is completely sealed; wherein, the mass fraction of polycarbosilane in the mixed solution of polycarbosilane and divinylbenzene is 40% to 60%.
S5:将步骤S4得到的产品机械加工成最终的设计尺寸,即得复合材料制动盘成品。S5: Machining the product obtained in step S4 into the final design size to obtain the finished composite brake disc.
下面结合具体实施例对本发明提供的本发明提供的复合材料制动盘及其制备方法作进一步说明。The composite material brake disc provided by the present invention and the preparation method thereof will be further described below in conjunction with specific examples.
实施例一Embodiment one
将单层0°无纬布、胎网、90°无纬布、胎网依次循环叠加,然后采用接力式针刺的方法在垂直于铺层方向引入聚丙烯腈(PAN)基预氧丝纤维,制成制动盘预制体;在真空条件下,将制动盘预制体在1200℃温度下进行碳化处理,碳化时间60小时;再利用化学气相渗积法将碳化后的制动盘预制体致密化,以丙烷为碳源气体,氮气为稀释气体,丙烷与氮气的体积比为1:2,渗积温度为1150℃,渗积压力为3000Pa,渗积时间为120h,得到密度为1.3g/cm3的C/C复合材料。The single-layer 0° no-weft cloth, tire net, 90° no-weft cloth, and tire net are superimposed in sequence, and then the polyacrylonitrile (PAN)-based pre-oxidized silk fiber is introduced in the direction perpendicular to the lay-up direction by the relay-type needling method. , to make a brake disc prefabricated body; under vacuum conditions, the brake disc prefabricated body was carbonized at a temperature of 1200 ° C for 60 hours; and then the carbonized brake disc prefabricated body was Densification, using propane as the carbon source gas, nitrogen as the diluent gas, the volume ratio of propane to nitrogen is 1:2, the infiltration temperature is 1150°C, the infiltration pressure is 3000Pa, the infiltration time is 120h, and the obtained density is 1.3g /cm 3 of C/C composites.
将C/C复合材料在氩气的保护下,于2200℃进行高温热处理,处理时间为2h;然后进行机械加工,根据制动盘的孔径尺寸要求,在所述热处理后的C/C复合材料表面加工出螺栓孔和定位孔;按制动盘尺寸的负公差要求,对所述热处理后的C/C复合材料四周的尺寸进行加工,并在厚度方向留出1mm的后续加工余量,得到C/C复合材料坯体。Under the protection of argon, the C/C composite material is subjected to high-temperature heat treatment at 2200 ° C for 2 hours; then it is machined, and according to the pore size requirements of the brake disc, the C/C composite material after the heat treatment Bolt holes and positioning holes are processed on the surface; according to the negative tolerance requirements of the brake disc size, the dimensions around the heat-treated C/C composite material are processed, and a subsequent machining allowance of 1 mm is left in the thickness direction to obtain C/C composite body.
将C/C复合材料坯体置于装有硅粉的石墨坩埚中,放入高温炉中进行熔融渗硅,如图1所示,具体为:在真空条件下,将C/C复合材料坯体掩埋于粒径为300目的硅粉中,然后1650℃保温2.5h,再1850℃保温10min,得到密度为1.95g/cm3的C/C-SiC复合材料制动盘;其中硅粉纯度为99.5%,硅粉的量为4倍于反应理论需要量。Put the C/C composite body in a graphite crucible filled with silicon powder, put it into a high-temperature furnace for molten siliconization, as shown in Figure 1, specifically: under vacuum conditions, put the C/C composite body The body was buried in silicon powder with a particle size of 300 mesh, and then kept at 1650°C for 2.5h, and then kept at 1850°C for 10min to obtain a C/C-SiC composite brake disc with a density of 1.95g/cm 3 ; the purity of the silicon powder was 99.5%, the amount of silicon powder is 4 times the theoretical requirement of the reaction.
利用化学气相渗积法对得到的C/C-SiC复合材料制动盘进行填封裂纹处理,以三氯甲基硅烷(CH3SiCl3,MTS)为液态先驱体原料,氢气为载气,通过鼓泡方式将气态MTS带入反应室,采用惰性气体氩气作为稀释气体以调节MTS的热解反应速率,渗积温度为1150℃,渗积压力为500Pa,渗积时间为20h,三氯甲基硅烷、氢气和氩气的体积比为1:9:3,得到密度为1.97g/cm3的C/C-SiC复合材料制动盘;然后将得到的产品进行机械加工成最终的设计尺寸,在磨床上采用金刚石砂轮对摩擦面进行表面加工,去除之前预留的1mm的后续加工余量,得到复合材料制动盘成品。The obtained C/C-SiC composite brake disc was crack-filled by chemical vapor deposition method, using trichloromethylsilane (CH 3 SiCl 3 , MTS) as the liquid precursor raw material, hydrogen as the carrier gas, The gaseous MTS is brought into the reaction chamber by bubbling, and the inert gas argon is used as the diluent gas to adjust the pyrolysis reaction rate of MTS. The infiltration temperature is 1150°C, the infiltration pressure is 500Pa, and the infiltration time is 20h. The volume ratio of methylsilane, hydrogen and argon was 1:9:3 to obtain a C/C-SiC composite brake disc with a density of 1.97 g/ cm3 ; the resulting product was then machined into the final design Dimensions, using a diamond grinding wheel on the grinding machine to process the surface of the friction surface, remove the previously reserved 1mm subsequent processing allowance, and obtain the finished composite material brake disc.
实施例二Embodiment two
将单层0°无纬布、胎网、90°无纬布、胎网依次循环叠加,然后采用接力式针刺的方法在垂直于铺层方向引入聚丙烯腈(PAN)基预氧丝纤维,制成制动盘预制体;在真空条件下,将制动盘预制体在1200℃温度下进行碳化处理,碳化时间60小时;再利用化学气相渗积法将碳化后的制动盘预制体致密化,以丙烷为碳源气体,氮气为稀释气体,丙烷与氮气的体积比为1:2,渗积温度为1150℃,渗积压力为3000Pa,渗积时间为120h,得到密度为1.3g/cm3的C/C复合材料。The single-layer 0° no-weft cloth, tire net, 90° no-weft cloth, and tire net are superimposed in sequence, and then the polyacrylonitrile (PAN)-based pre-oxidized silk fiber is introduced in the direction perpendicular to the lay-up direction by the relay-type needling method. , to make a brake disc prefabricated body; under vacuum conditions, the brake disc prefabricated body was carbonized at a temperature of 1200 ° C for 60 hours; and then the carbonized brake disc prefabricated body was Densification, using propane as the carbon source gas, nitrogen as the diluent gas, the volume ratio of propane to nitrogen is 1:2, the infiltration temperature is 1150°C, the infiltration pressure is 3000Pa, the infiltration time is 120h, and the obtained density is 1.3g /cm 3 of C/C composites.
将C/C复合材料在氩气的保护下,于2200℃进行高温热处理,处理时间为2h;然后进行机械加工,根据制动盘的孔径尺寸要求,在所述热处理后的C/C复合材料表面加工出螺栓孔和定位孔;按制动盘尺寸的负公差要求,对所述热处理后的C/C复合材料四周的尺寸进行加工,并在厚度方向留出1mm的后续加工余量,得到C/C复合材料坯体。Under the protection of argon, the C/C composite material is subjected to high-temperature heat treatment at 2200 ° C for 2 hours; then it is machined, and according to the pore size requirements of the brake disc, the C/C composite material after the heat treatment Bolt holes and positioning holes are processed on the surface; according to the negative tolerance requirements of the brake disc size, the dimensions around the heat-treated C/C composite material are processed, and a subsequent machining allowance of 1 mm is left in the thickness direction to obtain C/C composite body.
将C/C复合材料坯体置于装有硅粉的石墨坩埚中,放入高温炉中进行熔融渗硅,如图1所示,具体为:在真空条件下,将C/C复合材料坯体掩埋于粒径为300目的硅粉中,然后1650℃保温2.5h,再1850℃保温10min,得到密度为1.95g/cm3的C/C-SiC复合材料制动盘;其中硅粉纯度为99.5%,硅粉的量为4倍的反应理论需要量。Put the C/C composite body in a graphite crucible filled with silicon powder, put it into a high-temperature furnace for molten siliconization, as shown in Figure 1, specifically: under vacuum conditions, put the C/C composite body The body was buried in silicon powder with a particle size of 300 mesh, and then kept at 1650°C for 2.5h, and then kept at 1850°C for 10min to obtain a C/C-SiC composite brake disc with a density of 1.95g/cm 3 ; the purity of the silicon powder was 99.5%, the amount of silicon powder is 4 times the theoretical requirement of the reaction.
利用先驱体浸渍裂解法对得到的C/C-SiC复合材料制动盘进行填封裂纹处理,以聚碳硅烷(PCS)和二乙烯基苯的混合溶液作为先驱体溶液,其中聚碳硅烷与二乙烯基苯的混合溶液中聚碳硅烷的质量分数为45%,将C/C-SiC复合材料制动盘浸渍于聚碳硅烷与二乙烯基苯的混合溶液中30min,浸渍温度为70℃,浸渍压力为1.5MPa,然后在150℃下固化交联3h,再在1200℃高温下裂解1h;重复上述先驱体浸渍裂解法5次,得到密度为1.96g/cm3的C/C-SiC复合材料制动盘。然后将得到的产品进行机械加工成最终的设计尺寸,在磨床上采用金刚石砂轮对摩擦面进行表面加工,去除之前预留的1mm的后续加工余量,得到复合材料制动盘成品。The cracks of the obtained C/C-SiC composite brake disc were filled by the precursor impregnation cracking method, and the mixed solution of polycarbosilane (PCS) and divinylbenzene was used as the precursor solution, in which polycarbosilane and The mass fraction of polycarbosilane in the mixed solution of divinylbenzene is 45%, the C/C-SiC composite brake disc is immersed in the mixed solution of polycarbosilane and divinylbenzene for 30min, and the immersion temperature is 70°C , the immersion pressure is 1.5MPa, then curing and crosslinking at 150°C for 3h, and then cracking at 1200°C for 1h; repeat the above precursor dipping and cracking method 5 times to obtain C/C-SiC with a density of 1.96g/cm 3 Composite brake discs. Then, the obtained product is machined into the final design size, and the friction surface is processed on the grinding machine with a diamond grinding wheel, and the 1 mm subsequent processing allowance reserved before is removed to obtain the finished composite material brake disc.
将本发明实施例一和实施例二制备得到的复合材料制动盘进行性能测定,具体测试方法和测试结果如下。The performance of the composite brake discs prepared in Examples 1 and 2 of the present invention was tested, and the specific test methods and test results are as follows.
测试方法:对实施例一和实施例二制备得到的复合材料制动盘分别进行1:1动力台架试验,确认其摩擦磨损性能。试验条件为在400km/h的速度下反复进行40次紧急制动(在干态和湿态条件下各进行20次),并对制动盘摩擦表面的摩擦磨损性能进行测试。Test method: 1:1 dynamic bench test was carried out on the composite brake discs prepared in Example 1 and Example 2, respectively, to confirm their friction and wear properties. The test conditions are repeated emergency braking 40 times at a speed of 400km/h (20 times under dry and wet conditions), and the friction and wear performance of the friction surface of the brake disc is tested.
测试结果:具体结果如下表1所示。Test results: the specific results are shown in Table 1 below.
表1复合材料制动盘性能测试结果Table 1 Performance test results of composite brake discs
实施例一和实施例二制备得到的复合材料制动盘在湿态刹车试验中都表现出了优异的性能,其中实施例一制备得到的复合材料制动盘的干湿态摩擦系数变化率仅为2.6%,实施例二制备得到的复合材料制动盘的干湿态摩擦系数变化率仅为2.7%,因此都几乎不存在湿态摩擦性能衰减的问题。The composite brake discs prepared in Example 1 and Example 2 all showed excellent performance in the wet braking test, and the change rate of the dry and wet friction coefficient of the composite brake disc prepared in Example 1 was only is 2.6%, and the change rate of the dry and wet friction coefficient of the composite brake disc prepared in Example 2 is only 2.7%, so there is almost no problem of attenuation of wet friction performance.
需要说明的是,除了上述实施例一和实施例二列举的情况,选用其他的制备方法参数也是可行的。It should be noted that, in addition to the cases listed in the first and second examples above, it is also feasible to select other parameters of the preparation method.
本发明提供的C/C-SiC复合材料制动盘及其制备方法,可以降低制备成本,提高制动盘的力学性能、导热性能和摩擦磨损性能。The C/C-SiC composite material brake disk and the preparation method thereof provided by the invention can reduce the preparation cost and improve the mechanical performance, thermal conductivity and friction and wear performance of the brake disk.
本发明提供的复合材料制动盘及其制备方法,有如下积极效果:(1)本发明首次提出用聚丙烯腈基预氧丝纤维作为高铁用碳陶双基复合材料制动盘的增强体,提供了一种可批量生产的制造技术。预氧丝纤维相对碳纤维价格非常低廉,制备预制体时大大降低了制备成本;预氧丝纤维断裂延伸率高,柔韧性好,适合针刺,而碳纤维为脆性材料,且表面为沟槽结构,针刺时纤维受到的阻力大,易从勾刺上脱落或断裂滑出,因此预氧丝纤维预制体较碳纤维预制体表面平整,Z向纤维的引入数量和长度高,所制备得到的碳陶双基复合材料Z向导热系数高,层间结合力强,摩擦磨损性能优异,特别适合做列车尤其是高铁制动盘材料。(2)本发明采用化学气相渗积法(CVI)或先驱体浸渍裂解法(PIP)对熔融渗硅后的C/C-SiC复合材料制动盘进行填封裂纹处理,处理后的C/C-Si复合材料制动盘几乎不含裂纹,提高了其力学性能;而且PIP法处理所产生的多余C还可以与熔融渗硅处理后材料中残余的Si进行反应生成SiC,降低了复合材料中Si的残余量,提高了复合材料的抗蠕变性能。(3)本发明选择在两个不同的高温环境下进行熔融渗硅,这种反应方式可以使Si与基体中的C反应的更加充分,减少C/C-SiC复合材料中的闭孔数量和残余硅的含量,提高复合材料抗蠕变性能、均匀性和力学性能,减少摩擦磨损量。(4)当基体中热解碳含量过高时会导致力学性能降低,过低时则会导致陶瓷基体含量过高,制动盘脆性高,同时摩擦系数过高。本发明通过调节基体中的热解碳的含量,实现对复合材料中基体碳与碳化硅含量的控制,从而使复合材料的力学性能和摩擦磨损性能达到均衡的效果。The composite material brake disc provided by the invention and the preparation method thereof have the following positive effects: (1) the present invention proposes to use polyacrylonitrile-based pre-oxidized silk fiber as the reinforcing body of the carbon-ceramic double-base composite brake disc for high-speed rail for the first time, providing A manufacturing technique that can be mass-produced. Compared with carbon fiber, the price of pre-oxidized silk fiber is very low, and the preparation cost is greatly reduced when preparing the preform; the pre-oxidized silk fiber has a high elongation at breakage, good flexibility, and is suitable for acupuncture, while carbon fiber is a brittle material with a grooved surface. The resistance to the fiber is large during needle punching, and it is easy to fall off or break off from the hook. Therefore, the surface of the pre-oxidized silk fiber preform is smoother than that of the carbon fiber preform, and the number and length of the Z-direction fibers are higher. The prepared carbon-ceramic double-base The composite material Z has high thermal conductivity, strong interlayer bonding, and excellent friction and wear properties, and is especially suitable for trains, especially high-speed rail brake disc materials. (2) The present invention adopts chemical vapor infiltration (CVI) or precursor impregnated cracking method (PIP) to carry out sealing crack treatment to the C/C-SiC composite material brake disk after molten siliconizing, the C/C after processing The C-Si composite brake disc has almost no cracks, which improves its mechanical properties; and the excess C produced by the PIP method can also react with the residual Si in the material after the molten siliconizing treatment to form SiC, which reduces the composite material. The residual amount of Si improves the creep resistance of the composite material. (3) The present invention chooses to carry out fusion siliconizing under two different high-temperature environments, and this reaction mode can make Si and the C reaction in the matrix more fully, reduce the number of closed cells and the number of closed cells in the C/C-SiC composite material The content of residual silicon improves the creep resistance, uniformity and mechanical properties of the composite material, and reduces the amount of friction and wear. (4) When the pyrolytic carbon content in the matrix is too high, the mechanical properties will be reduced, and if it is too low, the content of the ceramic matrix will be too high, the brake disc will be highly brittle, and the friction coefficient will be too high. The invention controls the content of matrix carbon and silicon carbide in the composite material by adjusting the content of pyrolytic carbon in the matrix, so that the mechanical properties and friction and wear properties of the composite material can be balanced.
在本说明书的描述中,参考术语“一个实施例”、“一些实施例”、“示例”、“具体示例”或“一些示例”等的描述意指结合该实施例或示例描述的具体特征、结构、材料或者特点包含于本发明的至少一个实施例或示例中。在本说明书中,对上述术语的示意性表述不必须针对的是相同的实施例或示例。而且,描述的具体特征、结构、材料或者特点可以在任一个或多个实施例或示例中以合适的方式结合。此外,在不相互矛盾的情况下,本领域的技术人员可以将本说明书中描述的不同实施例或示例以及不同实施例或示例的特征进行结合和组合。In the description of this specification, descriptions referring to the terms "one embodiment", "some embodiments", "example", "specific examples" or "some examples" mean specific features described in connection with the embodiment or example, A structure, material or characteristic is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the above terms are not necessarily directed to the same embodiment or example. Furthermore, the described specific features, structures, materials or characteristics may be combined in any suitable manner in any one or more embodiments or examples. In addition, those skilled in the art can combine and combine different embodiments or examples and features of different embodiments or examples described in this specification without conflicting with each other.
尽管上面已经示出和描述了本发明的实施例,可以理解的是,上述实施例是示例性的,不能理解为对本发明的限制,本领域的普通技术人员在本发明的范围内可以对上述实施例进行变化、修改、替换和变型,而并不使相应技术方案的本质脱离本发明各实施例技术方案的范围,其均应涵盖在本发明的权利要求和说明书的范围当中。Although the embodiments of the present invention have been shown and described above, it can be understood that the above embodiments are exemplary and should not be construed as limiting the present invention, those skilled in the art can make the above-mentioned The embodiments are changed, modified, replaced and modified without making the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention, and all of them should be covered by the scope of the claims and description of the present invention.
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| CN113915021A (en) * | 2021-09-29 | 2022-01-11 | 湖北瑞宇空天高新技术有限公司 | Cylindrical prefabricated body, light high-temperature-resistant composite piston and preparation method thereof |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07126089A (en) * | 1993-10-29 | 1995-05-16 | Tokai Carbon Co Ltd | Method for producing oxidation resistant C / C composite material |
| CN105884389A (en) * | 2016-04-19 | 2016-08-24 | 李永军 | Preparation method of C/C-SIC composite with low cost and low density gradient |
-
2016
- 2016-11-21 CN CN201611049125.9A patent/CN106966751B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07126089A (en) * | 1993-10-29 | 1995-05-16 | Tokai Carbon Co Ltd | Method for producing oxidation resistant C / C composite material |
| CN105884389A (en) * | 2016-04-19 | 2016-08-24 | 李永军 | Preparation method of C/C-SIC composite with low cost and low density gradient |
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