CN104529458B - The manufacture method of high-performance SiC ceramic based composites blade of aviation engine - Google Patents

The manufacture method of high-performance SiC ceramic based composites blade of aviation engine Download PDF

Info

Publication number
CN104529458B
CN104529458B CN201410721023.1A CN201410721023A CN104529458B CN 104529458 B CN104529458 B CN 104529458B CN 201410721023 A CN201410721023 A CN 201410721023A CN 104529458 B CN104529458 B CN 104529458B
Authority
CN
China
Prior art keywords
sic
pcs
blade
sic ceramic
carbon fiber
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201410721023.1A
Other languages
Chinese (zh)
Other versions
CN104529458A (en
Inventor
鲁中良
曹继伟
白树钊
李涤尘
卢秉恒
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Xian Jiaotong University
Original Assignee
Xian Jiaotong University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Xian Jiaotong University filed Critical Xian Jiaotong University
Priority to CN201410721023.1A priority Critical patent/CN104529458B/en
Publication of CN104529458A publication Critical patent/CN104529458A/en
Application granted granted Critical
Publication of CN104529458B publication Critical patent/CN104529458B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/60Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
    • C04B2235/602Making the green bodies or pre-forms by moulding
    • C04B2235/6026Computer aided shaping, e.g. rapid prototyping

Landscapes

  • Ceramic Products (AREA)

Abstract

本发明公开一种高性能SiC陶瓷基复合材料航空发动机叶片的制造方法,采用3D打印技术制备了航空发动机叶片模具,再通过凝胶注模法制备出加入碳纤维的SiC陶瓷素坯件,经过冷冻干燥、脱脂等工艺得到多孔SiC陶瓷预制件,然后多次浸渍裂解有机物前驱体,利用裂解产物填充预制件的孔隙,使其达到初步致密,为了保证制件强度与致密度,最终使用热等静压方法制造出高性能SiC陶瓷基复合材料航空发动机叶片。该方法结合多种近净成型技术克服了SiC材料加工困难等缺点,与传统的合金叶片相比较,SiC陶瓷基复合材料航空发动机叶片具有质量轻、耐高温的优势,是未来航空发动机叶片发展的趋势。The invention discloses a method for manufacturing a high-performance SiC ceramic-based composite material aero-engine blade. The aero-engine blade mold is prepared by using 3D printing technology, and then a SiC ceramic blank with carbon fiber is prepared by gel injection molding. After freezing Porous SiC ceramic preforms are obtained by drying, degreasing and other processes, and then the organic precursor is impregnated and cracked multiple times, and the cracked products are used to fill the pores of the preforms to achieve initial densification. In order to ensure the strength and density of the parts, hot isostatic High-performance SiC ceramic matrix composite aeroengine blades were manufactured by pressing method. This method combines a variety of near-net shape technologies to overcome the shortcomings of SiC material processing difficulties. Compared with traditional alloy blades, SiC ceramic matrix composite aero-engine blades have the advantages of light weight and high temperature resistance, and are the future development of aero-engine blades. trend.

Description

高性能SiC陶瓷基复合材料航空发动机叶片的制造方法Manufacturing method of high-performance SiC ceramic matrix composite aeroengine blade

【技术领域】【Technical field】

本发明属于陶瓷基复合材料复杂零件制造技术领域,涉及一种高性能SiC陶瓷基复合材料航空发动机叶片的制造方法。The invention belongs to the technical field of manufacturing complex parts of ceramic matrix composite materials, and relates to a method for manufacturing high-performance SiC ceramic matrix composite material aeroengine blades.

【背景技术】【Background technique】

叶片是航空发动机的关键部件,为了不断提高航空发动机的综合性能,则需要提高航空发动机的燃气温度,这就要求叶片有足够高的承热能力。传统采用的高温合金使用温度有限,且密度较高(8.03-8.06g/cm3),制约了航空发动机性能的进一步提升。Blades are the key components of aero-engines. In order to continuously improve the overall performance of aero-engines, it is necessary to increase the gas temperature of aero-engines, which requires the blades to have a high enough heat-bearing capacity. Traditionally used superalloys have limited service temperature and high density (8.03-8.06g/cm 3 ), which restricts the further improvement of aero-engine performance.

【发明内容】【Content of invention】

本发明的目的在于提供一种高性能SiC陶瓷基复合材料航空发动机叶片的制造方法,该方法基于3D打印技术,经过凝胶注模、热等静压工艺制造出高性能SiC陶瓷基复合材料航空发动机叶片,该叶片耐高温且密度低,有利于提高航空发动机的综合性能。The purpose of the present invention is to provide a method for manufacturing high-performance SiC ceramic matrix composite aeroengine blades. The method is based on 3D printing technology and produces high-performance SiC ceramic matrix composite aviation Engine blades, which are high-temperature-resistant and low-density, are conducive to improving the overall performance of the aero-engine.

为了实现上述目的,本发明采用如下技术方案:In order to achieve the above object, the present invention adopts the following technical solutions:

高性能SiC陶瓷基复合材料航空发动机叶片的制造方法,包括以下步骤:A method for manufacturing a high-performance SiC ceramic matrix composite aeroengine blade, comprising the following steps:

1)制备航空发动机叶片的树脂模具;1) Prepare a resin mold for an aeroengine blade;

2)制备固相颗粒分散均匀的SiC悬浮浆料;2) preparing a SiC suspension slurry in which the solid phase particles are uniformly dispersed;

3)采用真空注型技术将SiC悬浮浆料浇入树脂模具内,得到SiC陶瓷素坯;3) Pouring the SiC suspension slurry into the resin mold by vacuum injection molding technology to obtain the SiC ceramic green body;

4)将得到的SiC陶瓷素坯进行冷冻干燥处理,去除坯体内的结晶水得到干燥的生坯;并使用液氮将其树脂模具去除;4) subjecting the obtained SiC ceramic green body to freeze-drying treatment, removing crystal water in the green body to obtain a dried green body; and using liquid nitrogen to remove the resin mold;

5)在气氛保护下对干燥的生坯进行脱脂工艺,将坯体内部有机物烧蚀,得到多孔的SiC陶瓷叶片;5) Degreasing the dried green body under the protection of the atmosphere, ablation of the organic matter inside the green body to obtain porous SiC ceramic blades;

6)通过进行多次前驱体浸渍裂解工艺,将多孔的SiC陶瓷叶片初步致密化;6) Preliminary densification of porous SiC ceramic blades by performing multiple precursor dipping and cracking processes;

7)利用等静压技术,将初步致密化的SiC陶瓷叶片烧结,最终制造出致密度大于或等于95%的SiC陶瓷基复合材料叶片。7) Using isostatic pressing technology to sinter the pre-densified SiC ceramic blade, and finally manufacture a SiC ceramic matrix composite material blade with a density greater than or equal to 95%.

优选的,步骤2)具体包括:Preferably, step 2) specifically includes:

2.1)按照具有PCS涂层的松散单丝短碳纤维:纳米SiC:预混液=1:(5~15):45的体积比将具有PCS涂层的松散单丝短碳纤维和纳米SiC加入到配置好的预混液当中,并进行超声分散得到分散好的预混液;2.1) Add the loose monofilament short carbon fiber with PCS coating and nano SiC to the configured Among the premixed liquids, ultrasonic dispersion is carried out to obtain dispersed premixed liquids;

2.2)将微米SiC混合粉末加入步骤2.1)分散好的预混液中得到混合浆料,然后加入混合浆料中固相成分0.5~2wt%的聚丙烯酸钠作为分散剂;然后把混合浆料置入机械搅拌器内搅拌均匀,最终得到固相颗粒分散均匀的SiC悬浮浆料;其中,微米SiC混合粉末的加入量与步骤2.1)中所使用的预混液的体积比为(39~49):45;2.2) Add the micron SiC mixed powder into the dispersed premix in step 2.1) to obtain a mixed slurry, then add sodium polyacrylate with a solid phase content of 0.5 to 2wt% in the mixed slurry as a dispersant; then put the mixed slurry into Stir evenly in a mechanical stirrer, and finally obtain a SiC suspension slurry with uniformly dispersed solid phase particles; wherein, the volume ratio of the added amount of micron SiC mixed powder to the premixed liquid used in step 2.1) is (39-49):45 ;

所述预混液的制备方法为:将有机单体丙烯酰胺和交联剂N,N′-亚甲基双丙烯酰胺,按照质量比(6~24):1混合,然后在室温下溶解到去离子水中,配制成质量分数为15~25%的预混液;The preparation method of the premixed solution is as follows: the organic monomer acrylamide and the crosslinking agent N,N'-methylenebisacrylamide are mixed according to the mass ratio (6-24): 1, and then dissolved at room temperature until In deionized water, prepare a premix solution with a mass fraction of 15-25%;

所述具有PCS涂层的松散单丝短碳纤维的制备方法为:将固态PCS研磨成粉末,溶于二甲苯中,配制成质量分数的20wt%~25wt%的PCS/Xylene浸渍液;将长度为0.5~4mm短碳纤维加入浸渍液中,超声波处理排除短碳纤维表面沟壑中的气泡;静置1h后取出,于140℃保温8h使PCS与空气中的氧发生氧化自交联反应;然后将完成交联的短碳纤维在二甲苯中超声分散5min,取出后烘干;循环上述操作1~2次,得到表面具有均匀而光滑的PCS涂层的松散单丝短碳纤维;The preparation method of the loose monofilament short carbon fiber with PCS coating is: solid PCS is ground into powder, is dissolved in xylene, is mixed with the PCS/Xylene dipping liquid of 20wt%~25wt% of mass fraction; 0.5-4mm short carbon fibers are added to the impregnating solution, and the air bubbles in the surface grooves of the short carbon fibers are removed by ultrasonic treatment; they are taken out after standing for 1 hour, and kept at 140°C for 8 hours to allow the oxidation and self-crosslinking reaction of PCS and oxygen in the air to occur; then the crosslinking is completed The combined short carbon fibers were ultrasonically dispersed in xylene for 5 minutes, taken out and then dried; the above operation was repeated 1 to 2 times to obtain loose monofilament short carbon fibers with a uniform and smooth PCS coating on the surface;

微米SiC混合粉末由粗SiC粉和细SiC粉以质量比(3~5):1混合而成,所述粗SiC粉的粒径为40~60um,细SiC粉的粒径为2~10μm。The micron SiC mixed powder is formed by mixing coarse SiC powder and fine SiC powder at a mass ratio (3-5): 1, the particle size of the coarse SiC powder is 40-60um, and the particle size of the fine SiC powder is 2-10μm.

优选的,步骤3)具体包括以下步骤:将SiC悬浮浆料置入真空注型机内,先后加入催化量的催化剂和引发剂,搅拌均匀后开始向树脂模具内浇注悬浮浆料,同时开启振动台,排尽树脂模具内气泡;待真空浇注完成后,在大气环境常温静置彻底完成单体交联固化得到凝胶后的叶片素坯;其中,所述催化剂为质量分数为25%的四甲基乙二胺溶,所述引发剂为质量分数为30%过硫酸铵溶液,催化剂的质量与引发剂的质量比为1:6-7。Preferably, step 3) specifically includes the following steps: placing the SiC suspension slurry into a vacuum injection molding machine, adding catalytic amounts of catalyst and initiator successively, stirring evenly and starting to pour the suspension slurry into the resin mold, and simultaneously starting the vibration platform to exhaust the air bubbles in the resin mold; after the vacuum pouring is completed, stand at room temperature in the atmospheric environment to completely complete the monomer cross-linking and solidification to obtain the green blade green body after the gel; wherein the catalyst is 25% four Methylethylenediamine is dissolved, the initiator is ammonium persulfate solution with a mass fraction of 30%, and the mass ratio of the catalyst mass to the initiator is 1:6-7.

优选的,步骤4)具体包括:将凝胶后的叶片素坯放置于-60℃冻柜内,冷冻3~5h,使生坯中的水分完全冷冻结晶;然后使用液氮剥离树脂模具,再将生坯放入冷冻干燥机的真空负压舱内,持续抽真空至真空度保持在0.1Pa~10Pa,使得生坯内的结晶水完全升华得到干燥的生坯。Preferably, step 4) specifically includes: placing the gelled blade blank in a freezer at -60°C, freezing for 3 to 5 hours, so that the water in the green blank is completely frozen and crystallized; then using liquid nitrogen to peel off the resin mold, and then Put the green body into the vacuum negative pressure chamber of the freeze dryer, and continue to vacuum until the vacuum degree is kept at 0.1Pa-10Pa, so that the crystal water in the green body is completely sublimated to obtain a dried green body.

优选的,步骤5)具体包括:将干燥的生坯在气氛箱式炉内完成脱脂工艺,以氩气为保护气体,脱脂升温工艺:以5℃/min的升温速率从室温升温至200℃,然后以1℃/min的升温速率从200℃升温至700℃,然后以2℃/min的升温速率从700℃升温至~900℃并保温1h;脱脂后,得到多孔的SiC陶瓷叶片。Preferably, step 5) specifically includes: completing the degreasing process of the dried green body in an atmosphere box furnace, using argon as a protective gas, and the degreasing and heating process: raising the temperature from room temperature to 200 °C at a heating rate of 5 °C/min, Then the temperature was raised from 200°C to 700°C at a heating rate of 1°C/min, and then from 700°C to ~900°C at a heating rate of 2°C/min and kept for 1 hour; after degreasing, porous SiC ceramic blades were obtained.

优选的,步骤6)具体包括:将得到的多孔的SiC陶瓷叶片放置真空罐内,抽真空后吸入SiC/PCS/xylene浸渍浆料,真空度为8×10-2,保压浸渍30min;将浸渍后的制件,于80℃下干燥2~4h,然后升温到150℃完成氧化交联;然后在Ar气保护下,以5℃/min的速度升温至1300℃进行裂解,并在1300℃保温1~1.5h;然后将浸渍剂更换为PCS/xylene溶液,重复上述浸渍裂解工艺得到初步致密化的SiC陶瓷叶片;SiC/PCS/xylene浸渍浆料中SiC的质量分数为10%,PCS的质量分数为40%,SiC为纳米颗粒;PCS/xylene浸渍浆料中PCS的质量分数为40%。Preferably, step 6) specifically includes: placing the obtained porous SiC ceramic blade in a vacuum tank, sucking in the SiC/PCS/xylene impregnation slurry after vacuuming, with a vacuum degree of 8×10 -2 , and impregnating for 30 minutes under pressure; The impregnated parts are dried at 80°C for 2 to 4 hours, and then heated to 150°C to complete oxidative cross-linking; then under the protection of Ar gas, the temperature is raised to 1300°C at a speed of 5°C/min for cracking, and at 1300°C Insulate for 1 to 1.5 hours; then replace the impregnating agent with PCS/xylene solution, repeat the above dipping and cracking process to obtain a preliminary densified SiC ceramic blade; the mass fraction of SiC in the SiC/PCS/xylene impregnating slurry is 10%, and the The mass fraction is 40%, and SiC is nanoparticles; the mass fraction of PCS in the PCS/xylene impregnation slurry is 40%.

优选的,步骤7)具体包括:将初步致密化的SiC陶瓷叶片从室温以5℃/min的升温速率进行升温至1500℃,并在1500℃保温时间1.5~2h进行热等静压烧结,热等静压烧结以氩气为传压介质,压力100MPa;热等静压烧结完成后随炉冷却至室温,得到所要制备的高性能SiC陶瓷基复合材料航空发动机叶片。Preferably, step 7) specifically includes: heating the pre-densified SiC ceramic blade from room temperature to 1500°C at a heating rate of 5°C/min, and performing hot isostatic pressing sintering at 1500°C for 1.5-2 hours. The isostatic sintering uses argon as the pressure transmission medium, and the pressure is 100 MPa; after the hot isostatic sintering is completed, it is cooled to room temperature with the furnace to obtain the high-performance SiC ceramic matrix composite aero-engine blade to be prepared.

优选的,步骤2)具体包括:Preferably, step 2) specifically includes:

2.1)按照具有PCS涂层的松散单丝短碳纤维:预混液=(5~15):45的体积比将具有PCS涂层的松散单丝短碳纤维加入到配置好的预混液当中,并进行超声分散得到分散好的预混液;2.1) According to the volume ratio of loose monofilament short carbon fiber with PCS coating: premix solution = (5 ~ 15): 45, add loose monofilament short carbon fiber with PCS coating into the prepared premix solution, and perform ultrasonic Disperse to obtain a dispersed premix;

2.2)再以石墨:硅粉:SiC:预混液=6:14:(20~30):45的体积将石墨、硅粉和SiC粉末加入分散好的预混液中得到混合浆料,然后加入混合浆料中固相成分0.5~2wt%的分散剂;然后把浆料置入机械搅拌器内搅拌均匀,最终得到固相颗粒分散均匀的SiC悬浮浆料;石墨粒径为15~25um,硅粉粒径为5um,SiC粉末粒径为40~60um;2.2) Then add graphite, silicon powder and SiC powder into the dispersed premix with the volume of graphite: silicon powder: SiC: premix = 6: 14: (20-30): 45 to obtain a mixed slurry, then add and mix A dispersant with 0.5-2wt% solid phase component in the slurry; then put the slurry into a mechanical stirrer and stir evenly, and finally obtain a SiC suspension slurry with uniformly dispersed solid phase particles; graphite particle size is 15-25um, silicon powder The particle size is 5um, and the SiC powder particle size is 40-60um;

所述预混液的制备方法为:将有机单体丙烯酰胺和交联剂N,N′-亚甲基双丙烯酰胺,按照质量比(6~24):1混合,然后在室温下溶解到去离子水中,配制成质量分数为15~25%的预混液;The preparation method of the premixed solution is as follows: the organic monomer acrylamide and the crosslinking agent N,N'-methylenebisacrylamide are mixed according to the mass ratio (6-24): 1, and then dissolved at room temperature until In deionized water, prepare a premix solution with a mass fraction of 15-25%;

所述具有PCS涂层的松散单丝短碳纤维的制备方法为:将固态PCS研磨成粉末,溶于二甲苯中,配制成质量分数的20wt%~25wt%的PCS/Xylene浸渍液;将长度为0.5~4mm短碳纤维加入浸渍液中,超声波处理排除短碳纤维表面沟壑中的气泡;静置1h后取出,于140℃保温8h使PCS与空气中的氧发生氧化自交联反应;然后将完成交联的短碳纤维在二甲苯中超声分散5min,取出后烘干;循环上述操作1~2次,得到表面具有均匀而光滑的PCS涂层的松散单丝短碳纤维。The preparation method of the loose monofilament short carbon fiber with PCS coating is: solid PCS is ground into powder, is dissolved in xylene, is mixed with the PCS/Xylene dipping liquid of 20wt%~25wt% of mass fraction; 0.5-4mm short carbon fibers are added to the impregnating solution, and the air bubbles in the surface grooves of the short carbon fibers are removed by ultrasonic treatment; they are taken out after standing for 1 hour, and kept at 140°C for 8 hours to allow the oxidation and self-crosslinking reaction of PCS and oxygen in the air to occur; then the crosslinking is completed The linked short carbon fibers were ultrasonically dispersed in xylene for 5 minutes, taken out and then dried; the above operation was repeated 1 to 2 times to obtain loose monofilament short carbon fibers with a uniform and smooth PCS coating on the surface.

优选的,步骤1)具体包括:使用三维建模软件构建航空发动机叶片三维原型,然后对原型抽壳得到叶片模具,将其导出为stl格式,再将其导入分层软件Magics中,对叶片模具模型进行分层处理;将Magics处理数据导入光固化快速成型机中,启动程序,完成叶片光固化树脂模具的制造;扫描参数:光斑大小为0.14mm,激光功率为300mw,扫描速度为5500mm/s,层厚0.1mm。Preferably, step 1) specifically includes: using 3D modeling software to build a 3D prototype of an aeroengine blade, then extracting the shell of the prototype to obtain a blade mold, exporting it to stl format, and then importing it into the layered software Magics, and then performing the blade mold The model is layered and processed; the Magics processing data is imported into the light-cured rapid prototyping machine, and the program is started to complete the manufacture of the blade light-cured resin mold; scanning parameters: the spot size is 0.14mm, the laser power is 300mw, and the scanning speed is 5500mm/s , layer thickness 0.1mm.

与现有技术相比,本发明具有以下有益的技术效果:Compared with the prior art, the present invention has the following beneficial technical effects:

本发明提供一种高性能SiC陶瓷基复合材料航空发动机叶片的制造方法,采用3D打印技术制备出光固化叶片负型模具,使用凝胶注模法得到SiC陶瓷素坯,然后经过冷冻干燥、脱脂等工艺得到的SiC零件,然而其致密度低,难以实现SiC陶瓷在高性能航空发动机上的应用。本发明结合先驱体浸渍裂解法和热等静压技术克服了其致密度低的缺陷,得到了韧性、结构性好,致密度高SiC陶瓷基航空发动机叶片。The invention provides a method for manufacturing a high-performance SiC ceramic-based composite material aeroengine blade, which uses 3D printing technology to prepare a light-cured blade negative mold, uses a gel injection molding method to obtain a SiC ceramic green body, and then undergoes freeze-drying, degreasing, etc. However, the SiC parts obtained by the process have low density, which makes it difficult to realize the application of SiC ceramics in high-performance aero-engines. The invention combines the precursor impregnation cracking method and the hot isostatic pressing technology to overcome the defect of low density, and obtains SiC ceramic-based aeroengine blades with good toughness and structure and high density.

本发明制造的SiC陶瓷基复合材料航空发动机叶片,采用浸渍先驱体(聚碳硅烷),在纤维表面裂解生成表面完整SiC界面层,有效防止纤维与基体反应,并提高了其与陶瓷基体的结合强度。The SiC ceramic matrix composite aero-engine blade manufactured by the present invention adopts the impregnated precursor (polycarbosilane) to crack and generate a complete SiC interface layer on the surface of the fiber, effectively preventing the fiber from reacting with the matrix, and improving its bonding with the ceramic matrix strength.

【具体实施方式】【detailed description】

下面结合具体的实施例对本发明做进一步的详细说明,所述是对本发明的解释而不是限定。The present invention will be further described in detail below in conjunction with specific embodiments, which are explanations of the present invention rather than limitations.

下面具体以航空发动机叶片的制备来进行具体的说明。The preparation of an aeroengine blade will be specifically described below.

实施例1Example 1

一种高性能SiC陶瓷基复合材料航空发动机叶片的制备方法,包括以下步骤:A method for preparing a high-performance SiC ceramic matrix composite material aeroengine blade, comprising the following steps:

1.航空发动机叶片负型模具设计与制造1. Design and manufacture of aero-engine blade negative mold

1.1使用三维建模软件(UG、ProE等)构建航空发动机叶片三维原型,然后对原型抽壳(抽壳厚度为0.5-1.0mm)得到叶片模具,将其导出为stl格式,再将其导入分层软件Magics中,对叶片模具模型进行分层处理。1.1 Use 3D modeling software (UG, ProE, etc.) to build a 3D prototype of an aero-engine blade, then shell the prototype (the thickness of the shell is 0.5-1.0mm) to get the blade mold, export it to stl format, and then import it into the In the layer software Magics, the blade mold model is layered.

1.2将Magics处理数据导入光固化快速成型机(SPS600)RP制造程序内,启动程序,完成叶片光固化树脂模具的制造。扫描参数:光斑大小为0.14mm,激光功率为300mw,扫描速度为5500mm/s,层厚0.1mm。1.2 Import the Magics processing data into the RP manufacturing program of the light-curing rapid prototyping machine (SPS600), start the program, and complete the manufacture of the blade light-curing resin mold. Scanning parameters: the spot size is 0.14mm, the laser power is 300mw, the scanning speed is 5500mm/s, and the layer thickness is 0.1mm.

2.浆料的制备2. Preparation of Slurry

2.1预混液的制备2.1 Preparation of master mix

将有机单体丙烯酰胺AM和交联剂N,N′-亚甲基双丙烯酰胺MBAM,按照质量比(6~24):1混合,然后在室温下(25℃)溶解到去离子水中,配制成质量分数为15~25%的预混液。The organic monomer acrylamide AM and the crosslinking agent N,N'-methylenebisacrylamide MBAM are mixed according to the mass ratio (6~24): 1, and then dissolved in deionized water at room temperature (25°C), Prepare a premix solution with a mass fraction of 15-25%.

2.2纤维涂层制备2.2 Fiber coating preparation

将固态PCS(聚碳硅烷)研磨成粉末,溶于二甲苯(Xylene)中,配制成质量分数的20wt%~25wt%的PCS/Xylene浸渍液。将长度为0.5~4mm短碳纤维加入浸渍液中,超声波处理(28Hz)30min,以排除短碳纤维表面沟壑中的气泡。静置1h,取出后于140℃保温8h使PCS与空气中的氧发生氧化自交联反应;然后将完成交联的短碳纤维在二甲苯中超声分散5min,取出后烘干。循环上述操作1~2次,即可得到表面具有均匀而光滑的PCS涂层的松散单丝短碳纤维。Solid PCS (polycarbosilane) is ground into powder, dissolved in xylene (Xylene), and prepared into a PCS/Xylene impregnating solution with a mass fraction of 20wt%-25wt%. Add short carbon fibers with a length of 0.5 to 4 mm into the impregnation solution, and perform ultrasonic treatment (28Hz) for 30 minutes to remove air bubbles in the grooves on the surface of the short carbon fibers. Let it stand for 1 hour, take it out and keep it warm at 140°C for 8 hours to make PCS oxidize and self-crosslink with the oxygen in the air; then ultrasonically disperse the crosslinked short carbon fiber in xylene for 5 minutes, take it out and dry it. By repeating the above operation for 1-2 times, the loose monofilament short carbon fiber with a uniform and smooth PCS coating on the surface can be obtained.

2.3固相组分制备2.3 Preparation of solid phase components

固相成份为:步骤2.2制备的具有PCS涂层的松散单丝短碳纤维、纳米SiC(平均粒径50nm,形状为球形)和微米级α-SiC混合粉末;其中微米级α-SiC混合粉末的纯度99.8%,并由粗SiC和细SiC组成,粗SiC粉的粒径为40~60um、细SiC粉的粒径为2~10μm,粗SiC:细SiC的质量比为(3~5):1,混合均匀形成微米级α-SiC混合粉末。The solid phase components are: the loose monofilament short carbon fiber with PCS coating prepared in step 2.2, nano-SiC (average particle diameter 50nm, spherical shape) and micron α-SiC mixed powder; wherein the micron α-SiC mixed powder The purity is 99.8%, and it is composed of coarse SiC and fine SiC. The particle size of coarse SiC powder is 40-60um, the particle size of fine SiC powder is 2-10μm, and the mass ratio of coarse SiC: fine SiC is (3-5): 1. Mix evenly to form micron-sized α-SiC mixed powder.

2.3.1按照具有PCS涂层的松散单丝短碳纤维:纳米SiC:预混液=1:(5~15):45的体积比将上述短碳纤维和纳米SiC加入到配置好的预混液当中,并进行5min的超声分散得到分散好的预混液。2.3.1 According to the volume ratio of PCS-coated loose monofilament short carbon fiber: nano-SiC: premix solution = 1: (5-15): 45, add the above-mentioned short carbon fiber and nano-SiC into the prepared premix solution, and Ultrasonic dispersion was carried out for 5 min to obtain a well-dispersed premix.

2.3.2将微米SiC混合粉末加入步骤2.3.1分散好的预混液中,然后加入固相成分0.5~2wt%的聚丙烯酸钠作为分散剂。然后把浆料置入机械搅拌器内搅拌,搅拌时间设定为20~45min,最终得到固相颗粒分散均匀的SiC悬浮浆料。微米SiC混合粉末的加入量与步骤2.3.1中所使用的预混液的体积比为(39~49):45。2.3.2 Add the micron SiC mixed powder into the premix solution dispersed in step 2.3.1, and then add 0.5-2 wt% sodium polyacrylate as a dispersant in the solid phase. Then put the slurry into a mechanical stirrer and stir, the stirring time is set at 20-45min, and finally obtain the SiC suspension slurry with uniformly dispersed solid phase particles. The volume ratio of the added amount of micron SiC mixed powder to the premix solution used in step 2.3.1 is (39-49):45.

3.凝胶注模成型3. Gel injection molding

将SiC悬浮浆料置入真空注型机内(真空度为8×10-2),先后加入催化量的催化剂(质量分数为25%的四甲基乙二胺溶液)和引发剂(质量分数为30%过硫酸铵溶液),继续搅拌。1min后开始向叶片模具内浇注悬浮浆料,同时开启振动台,排尽模具内气泡保证充型完整。待真空浇注完成后,在大气环境常温静置30min彻底完成单体交联固化得到凝胶后的叶片素坯。其中,催化剂的质量与引发剂的质量比为1:6-7。Put the SiC suspension slurry into a vacuum injection molding machine (vacuum degree is 8×10 -2 ), and add a catalytic amount of catalyst (a solution of tetramethylethylenediamine with a mass fraction of 25%) and an initiator (mass fraction 30% ammonium persulfate solution), continue stirring. After 1 minute, start pouring the suspension slurry into the blade mold, and at the same time turn on the vibrating table to exhaust the air bubbles in the mold to ensure the complete filling. After the vacuum pouring is completed, stand still at room temperature in the atmosphere for 30 minutes to completely complete the monomer cross-linking and solidification to obtain the green blade green body after gelation. Wherein, the mass ratio of the mass of the catalyst to the initiator is 1:6-7.

4.冷冻干燥4. Freeze drying

将凝胶后的叶片素坯放置于-60℃冻柜内,冷冻3~5h,使生坯中的水分完全冷冻结晶。然后使用液氮将生坯的树脂模具剥离,再将其放入冷冻干燥机的真空负压舱内,持续抽真空(真空度保持在0.1Pa~10Pa),使得生坯内的结晶水完全升华,从而达到干燥的目的以得到干燥的生坯。Place the gelled leaf green body in a freezer at -60°C for 3-5 hours, so that the moisture in the green body is completely frozen and crystallized. Then use liquid nitrogen to peel off the resin mold of the green body, then put it into the vacuum negative pressure chamber of the freeze dryer, and keep vacuuming (the vacuum degree is kept at 0.1Pa ~ 10Pa), so that the crystal water in the green body is completely sublimated , so as to achieve the purpose of drying to obtain a dry green body.

5.真空脱脂5. Vacuum degreasing

将干燥的生坯在气氛箱式炉内完成脱脂工艺,以氩气为保护气体,脱脂升温工艺:室温~200℃(升温速率5℃/min);200~700℃(升温速率1℃/min);700~900℃(升温速率2℃/min);900℃保温1h。脱脂后,得到孔径在5um左右的多孔SiC陶瓷基复合材料叶片。Complete the degreasing process of the dried green body in the atmosphere box furnace, using argon as the protective gas, degreasing and heating process: room temperature ~ 200 ° C (heating rate 5 ° C / min); 200 ~ 700 ° C (heating rate 1 ° C / min ); 700~900°C (heating rate 2°C/min); keep at 900°C for 1h. After degreasing, a porous SiC ceramic matrix composite material blade with a pore diameter of about 5um is obtained.

6.有机物前驱体的浸渍与裂解6. Impregnation and pyrolysis of organic precursors

6.1配制两种浸渍剂:配置SiC/PCS/xylene浆料(浆料中SiC的质量分数为10%,PCS的质量分数为40%,SiC为纳米颗粒)与PCS/xylene溶液(PCS的质量分数为40%)。6.1 Prepare two kinds of impregnating agents: configure SiC/PCS/xylene slurry (the mass fraction of SiC in the slurry is 10%, the mass fraction of PCS is 40%, and SiC is nanoparticles) and PCS/xylene solution (the mass fraction of PCS is 40%).

6.2将得到的多孔SiC陶瓷预制件放置真空罐内,抽真空后吸入SiC/PCS/xylene浸渍浆料。真空度为8×10-2,保压浸渍30min。将浸渍后的制件,于80℃下干燥2~4h,升温到150℃完成氧化交联。在Ar气保护下,以5℃/min的速度升温至1300℃进行裂解,并在1300℃保温1~1.5h。然后将浸渍剂更换为PCS/xylene溶液,重复浸渍-裂解工艺。待裂解工艺完成后得到致密度较高的SiC陶瓷基复合材料航空发动机叶片(其致密度可达85%~90%)。6.2 Place the obtained porous SiC ceramic preform in a vacuum tank, and suck the SiC/PCS/xylene impregnation slurry after vacuuming. The vacuum degree is 8×10 -2 , and the impregnation is held for 30 minutes. Dry the impregnated article at 80°C for 2-4 hours, then raise the temperature to 150°C to complete oxidative cross-linking. Under the protection of Ar gas, the temperature was raised to 1300°C at a rate of 5°C/min for cracking, and the temperature was kept at 1300°C for 1-1.5h. Then the impregnating agent was replaced with PCS/xylene solution, and the impregnating-cracking process was repeated. After the cracking process is completed, a SiC ceramic matrix composite material aero-engine blade with higher density (the density can reach 85% to 90%) is obtained.

7.热等静压7. Hot isostatic pressing

将步骤6.2制备的SiC陶瓷基复合材料航空发动机叶片从室温以5℃/min的升温速率进行升温至1500℃,并在1500℃保温时间1.5~2h进行热等静压烧结,热等静压烧结以氩气为传压介质,压力100MPa。热等静压烧结完成后随炉冷却至室温,取出样件,最终得到密度为2.75-2.82g/cm3,高温(1300℃)抗弯强度为270MPa的SiC陶瓷基复合材料航空发动机叶片。Heat the SiC ceramic matrix composite aero-engine blade prepared in step 6.2 from room temperature to 1500°C at a heating rate of 5°C/min, and conduct hot isostatic pressing sintering at 1500°C for 1.5 to 2 hours. Argon is used as the pressure transmission medium, and the pressure is 100MPa. After the hot isostatic pressing sintering is completed, the furnace is cooled to room temperature, and the sample is taken out to obtain a SiC ceramic matrix composite aero-engine blade with a density of 2.75-2.82g/cm 3 and a high-temperature (1300°C) bending strength of 270MPa.

实施例2Example 2

一种高性能SiC陶瓷基复合材料航空发动机叶片的制备方法,包括以下步骤:A method for preparing a high-performance SiC ceramic matrix composite material aeroengine blade, comprising the following steps:

1.与实例1的步骤1相同;1. Same as Step 1 of Example 1;

2.浆料的配制2. Preparation of slurry

2.1.与实例1步骤2.1相同2.1. Same as Step 2.1 of Example 1

2.2.与实例1步骤2.2相同2.2. Same as Step 2.2 of Example 1

2.3.按照具有PCS涂层的松散单丝短碳纤维:预混液=(5~15):45的体积比将其混合,并进行5min的超声分散。再以石墨:硅粉:SiC:预混液=6:14:(20~30):45的体积将石墨、硅粉和SiC粉末加入分散好的预混液中,然后加入整个固相成分0.5~2wt%的聚丙烯酸钠作为分散剂。然后把浆料置入机械搅拌器内搅拌,搅拌时间设定为20~45min,最终得到固相颗粒分散均匀的SiC悬浮浆料。石墨粒径为15~25um,Si粉粒径为5um,SiC粉末粒径为40~60um。2.3. Mix them according to the volume ratio of loose monofilament short carbon fibers with PCS coating: premix solution = (5-15): 45, and perform ultrasonic dispersion for 5 minutes. Then add graphite, silicon powder and SiC powder into the dispersed premix with the volume of graphite: silicon powder: SiC: premix = 6:14: (20-30): 45, and then add 0.5-2wt of the entire solid phase component % sodium polyacrylate as a dispersant. Then put the slurry into a mechanical stirrer and stir, the stirring time is set at 20-45min, and finally obtain the SiC suspension slurry with uniformly dispersed solid phase particles. The graphite particle size is 15-25um, the Si powder particle size is 5um, and the SiC powder particle size is 40-60um.

3.凝胶注模成型3. Gel injection molding

将SiC悬浮浆料置入真空注型机内(真空度为8×10-2),先后加催化量的催化剂(质量分数为25%的四甲基乙二胺溶液)和引发剂(质量分数为30%过硫酸铵溶液),继续搅拌。1min后开始向叶片模具内浇注悬浮浆料,同时开启振动台,排尽模具内气泡以保证充型完整。待真空浇注完成后,在大气环境常温静置30min彻底完成单体交联固化得到凝胶后的叶片制件。其中,催化剂的质量与引发剂的质量比为1:6-7。Put the SiC suspension slurry into a vacuum injection molding machine (vacuum degree is 8×10 -2 ), add a catalytic amount of catalyst (a solution of tetramethylethylenediamine with a mass fraction of 25%) and an initiator (mass fraction 30% ammonium persulfate solution), continue stirring. After 1 minute, start pouring the suspension slurry into the blade mold, and at the same time turn on the vibrating table to exhaust the air bubbles in the mold to ensure the complete filling. After the vacuum pouring is completed, let it stand at room temperature in the atmosphere for 30 minutes to completely complete the monomer cross-linking and solidification to obtain the gelled blade parts. Wherein, the mass ratio of the mass of the catalyst to the initiator is 1:6-7.

4.冷冻干燥4. Freeze drying

将凝胶后的叶片制件放置于-60℃冻柜内,冷冻3~5h,使生坯中的水分完全冷冻结晶。然后使用液氮将生坯的树脂模具剥离,再将其放入冷冻干燥机的真空负压舱内,持续抽真空(真空度保持在0.1Pa~10Pa),使得生坯内的结晶水完全升华,从而达到干燥的目的,以得到干燥的生坯。Place the gelled leaf parts in a -60°C freezer and freeze for 3 to 5 hours to completely freeze and crystallize the moisture in the green body. Then use liquid nitrogen to peel off the resin mold of the green body, then put it into the vacuum negative pressure chamber of the freeze dryer, and keep vacuuming (the vacuum degree is kept at 0.1Pa ~ 10Pa), so that the crystal water in the green body is completely sublimated , so as to achieve the purpose of drying to obtain a dry green body.

5.真空脱脂5. Vacuum degreasing

在气氛箱式炉内完成脱脂工艺,以氩气为保护气体,脱脂升温工艺:室温~200℃(升温速率5℃/min);200~700℃(升温速率1℃/min);700~900℃(升温速率2℃/min);900℃保温1h。脱脂后,得到孔径在5um左右的多孔SiC陶瓷。The degreasing process is completed in the atmosphere box furnace, with argon as the protective gas, and the degreasing heating process: room temperature ~ 200 ° C (heating rate 5 ° C / min); 200 ~ 700 ° C (heating rate 1 ° C / min); 700 ~ 900 °C (heating rate 2 °C/min); keep at 900 °C for 1 h. After degreasing, a porous SiC ceramic with a pore size of about 5um is obtained.

6.有机物前驱体的浸渍与裂解6. Impregnation and pyrolysis of organic precursors

6.1配制两种浸渍剂,配置SiC/PCS/xylene浆料(浆料中SiC的质量分数为10%,PCS的质量分数为40%,SiC为纳米颗粒)与PCS/xylene溶液(PCS的质量分数为40%)。6.1 Prepare two kinds of impregnating agents, configure SiC/PCS/xylene slurry (the mass fraction of SiC in the slurry is 10%, the mass fraction of PCS is 40%, and SiC is nanoparticles) and PCS/xylene solution (the mass fraction of PCS is 40%).

6.2将得到的多孔SiC陶瓷预制件放置真空罐内,抽真空后吸入SiC/PCS/xylene浸渍浆料。真空度为8×10-2,保压浸渍30min。将浸渍后的制件,于80℃下干燥2~4h,升温到150℃完成氧化交联。在Ar气保护下,以5℃/min的速度从室温升温至1300℃进行裂解,并在1300℃保温1~1.5h。然后将浸渍剂更换为PCS/xylene溶液,重复浸渍-裂解工艺。待裂解工艺完成后得到致密度较高的SiC复合材料叶片。6.2 Place the obtained porous SiC ceramic preform in a vacuum tank, and suck the SiC/PCS/xylene impregnation slurry after vacuuming. The vacuum degree is 8×10 -2 , and the impregnation is held for 30 minutes. Dry the impregnated article at 80°C for 2-4 hours, then raise the temperature to 150°C to complete oxidative cross-linking. Under the protection of Ar gas, the temperature was raised from room temperature to 1300°C at a rate of 5°C/min for cracking, and kept at 1300°C for 1-1.5h. Then the impregnating agent was replaced with PCS/xylene solution, and the impregnating-cracking process was repeated. After the cracking process is completed, a SiC composite material blade with higher density is obtained.

7.热等静压7. Hot isostatic pressing

将步骤6.2制备的SiC陶瓷基复合材料航空发动机叶片从室温以5℃/min的升温速率进行升温至1500℃,并在1500℃保温时间1.5~2h进行热等静压烧结,热等静压烧结以氩气为传压介质,压力100MPa。热等静压烧结完成后随炉冷却至室温,取出样件,最终得到密度为2.75-2.82g/cm3,高温(1300℃)抗弯强度为270MPa的SiC陶瓷基复合材料航空发动机叶片。Heat the SiC ceramic matrix composite aero-engine blade prepared in step 6.2 from room temperature to 1500°C at a heating rate of 5°C/min, and conduct hot isostatic pressing sintering at 1500°C for 1.5 to 2 hours. Argon is used as the pressure transmission medium, and the pressure is 100MPa. After the hot isostatic pressing sintering is completed, the furnace is cooled to room temperature, and the sample is taken out to obtain a SiC ceramic matrix composite aero-engine blade with a density of 2.75-2.82g/cm 3 and a high-temperature (1300°C) bending strength of 270MPa.

Claims (7)

1. the manufacture method of high-performance SiC ceramic based composites blade of aviation engine, it is characterised in that comprise the following steps:
1) resin die of blade of aviation engine is prepared;
2) solid phase particles finely dispersed SiC suspended nitride is prepared;
3) use type vacuum injecting and forming technology to pour in resin die by SiC suspended nitride, obtain SiC ceramic biscuit;
4) the SiC ceramic biscuit obtained is carried out freeze-drying process, remove the green compact that the crystallization water in base substrate obtains being dried;And use liquid nitrogen to be removed by its resin die;
5) under atmosphere protection, dry green compact are carried out degreasing process, by internal for base substrate organic matter ablation, obtain the SiC ceramic blade of porous;
6) by carrying out repeatedly polymer infiltration and pyrolysis technique, by the SiC ceramic blade initial densification of porous;
7) utilize isostatic pressing technology, the SiC ceramic blade of initial densification is sintered, finally produce the consistency SiC ceramic based composites blade more than or equal to 95%;
Step 3) specifically include following steps: SiC suspended nitride is inserted in type vacuum injecting and forming machine, successively add catalyst and the initiator of catalytic amount, start to pour into a mould suspended nitride after stirring in resin die, open shake table simultaneously, drain bubble in resin die;After vacuum pouring completes, stand at atmospheric environment normal temperature and be properly completed the blade biscuit after monomer crosslinked solidification obtains gel;Wherein, described catalyst be mass fraction be the tetramethylethylenediamine solution of 25%, described initiator be mass fraction be 30% ammonium persulfate solution, the quality of catalyst and the mass ratio of initiator are 1:6-7.
The manufacture method of high-performance SiC ceramic based composites blade of aviation engine the most according to claim 1, it is characterised in that step 2) specifically include:
2.1) according to the loose monofilament short carbon fiber with PCS coating: nano SiC: premixed liquid=1:(5~15): the loose monofilament short carbon fiber and nano SiC with PCS coating are joined in the middle of the premixed liquid configured by the volume ratio of 45, and carry out ultrasonic disperse and obtain scattered premixed liquid;
2.2) micron SiC mixed-powder is added step 2.1) scattered premixed liquid obtains mixed slurry, it is subsequently adding in mixed slurry the Sodium Polyacrylate of solid-phase component 0.5~2wt% as dispersant;Then stir in mixed slurry being inserted mechanical agitator, finally give solid phase particles finely dispersed SiC suspended nitride;Wherein, the addition of micron SiC mixed-powder and step 2.1) volume ratio of scattered premixed liquid is (39~49): 45;
The preparation method of described premixed liquid is: by organic monomer acrylamide and crosslinking agent N, N '-methylene-bisacrylamide, according to mass ratio (6~24): 1 mixing, the most at room temperature it is dissolved in deionized water, is configured to the premixed liquid that mass fraction is 15~25%;
The preparation method of the loose monofilament short carbon fiber of the described PCS of having coating is: by solid-state PCS grind into powder, is dissolved in dimethylbenzene, is configured to the PCS/Xylene maceration extract of 20wt%~25wt% of mass fraction;Adding in maceration extract by a length of 0.5~4mm short carbon fiber, ultrasonic wave processes the bubble got rid of in gully, short carbon fiber surface;Take out after standing 1h, make PCS react with the oxygen generation self-crosslinked oxidation in air in 140 DEG C of insulation 8h;Then will complete short carbon fiber ultrasonic disperse 5min in dimethylbenzene of crosslinking, take out post-drying;Circulation aforesaid operations 1~2 times, must arrive surface and have the loose monofilament short carbon fiber of uniform and smooth PCS coating;
Micron SiC mixed-powder by thick SiC powder and thin SiC powder with mass ratio (3~5): 1 mixes, and the particle diameter of described thick SiC powder is 40~60 μm, and the particle diameter of thin SiC powder is 2~10 μm.
The manufacture method of high-performance SiC ceramic based composites blade of aviation engine the most according to claim 1, it is characterized in that, step 4) specifically include: the blade biscuit after gel is positioned over-60 DEG C and freezes in cabinet, freezing 3~5h, make the complete freezing and crystallizing of the moisture in green compact;Then use liquid nitrogen to peel off resin die, then green compact are put into the negative pressure of vacuum cabin of freeze drier, be persistently evacuated to vacuum and be maintained at 0.1Pa~10Pa so that the crystallization water in green compact distils the green compact obtaining being dried completely.
The manufacture method of high-performance SiC ceramic based composites blade of aviation engine the most according to claim 1; it is characterized in that; step 5) specifically include: dry green compact are completed degreasing process in atmosphere batch-type furnace; with argon gas as protective gas; degreasing heating process: with the heating rate of 5 DEG C/min from room temperature to 200 DEG C; then it is warming up to 700 DEG C with the heating rate of 1 DEG C/min from 200 DEG C, is then warming up to 900 DEG C with the heating rate of 2 DEG C/min from 700 DEG C and is incubated 1h;After degreasing, obtain the SiC ceramic blade of porous.
The manufacture method of high-performance SiC ceramic based composites blade of aviation engine the most according to claim 1, it is characterized in that, step 6) specifically include: the SiC ceramic blade of the porous obtained is placed in vacuum tank, sucking SiC/PCS/xylene dipping sizing agent after vacuumizing, vacuum is 8 × 10-2, pressurize dipping 30min;By the product after dipping, at 80 DEG C, it is dried 2~4h, is then warmed up to 150 DEG C and completes oxidation cross-linked;Then under Ar gas shielded, it is warming up to 1300 DEG C with the speed of 5 DEG C/min and cracks, and be incubated 1~1.5h at 1300 DEG C;Then impregnating agent is replaced by PCS/xylene solution, repeats above-mentioned impregnating cracking technology and obtain the SiC ceramic blade of initial densification;In SiC/PCS/xylene dipping sizing agent, the mass fraction of SiC is 10%, and the mass fraction of PCS is 40%, and SiC is nano particle;In PCS/xylene dipping sizing agent, the mass fraction of PCS is 40%.
The manufacture method of high-performance SiC ceramic based composites blade of aviation engine the most according to claim 1, it is characterized in that, step 7) specifically include: carry out being warming up to 1500 DEG C with the heating rate of 5 DEG C/min from room temperature by the SiC ceramic blade of initial densification, and carry out HIP sintering in 1500 DEG C of temperature retention times 1.5~2h, HIP sintering with argon gas as transmission medium, pressure 100MPa;HIP sintering cools to room temperature with the furnace after completing, and obtains high-performance SiC ceramic based composites blade of aviation engine to be prepared.
The manufacture method of high-performance SiC ceramic based composites blade of aviation engine the most according to claim 1, it is characterised in that step 2) specifically include:
2.1) according to the loose monofilament short carbon fiber with PCS coating: premixed liquid=(5~15): the loose monofilament short carbon fiber with PCS coating is joined in the middle of the premixed liquid configured by the volume ratio of 45, and carry out ultrasonic disperse and obtain scattered premixed liquid;
2.2) again with graphite: silica flour: SiC: premixed liquid=6:14:(20~30): the volume of 45, by obtaining mixed slurry in premixed liquid scattered for the addition of graphite, silica flour and SiC powder, is subsequently adding the dispersant of solid-phase component 0.5~2wt% in mixed slurry;Then stir in slurry being inserted mechanical agitator, finally give solid phase particles finely dispersed SiC suspended nitride;Graphite particle diameter is 15~25 μm, and silica flour particle diameter is 5 μm, and SiC powder particle diameter is 40~60 μm;
The preparation method of described premixed liquid is: by organic monomer acrylamide and crosslinking agent N, N '-methylene-bisacrylamide, according to mass ratio (6~24): 1 mixing, the most at room temperature it is dissolved in deionized water, is configured to the premixed liquid that mass fraction is 15~25%;
The preparation method of the loose monofilament short carbon fiber of the described PCS of having coating is: by solid-state PCS grind into powder, is dissolved in dimethylbenzene, is configured to the PCS/Xylene maceration extract of 20wt%~25wt% of mass fraction;Adding in maceration extract by a length of 0.5~4mm short carbon fiber, ultrasonic wave processes the bubble got rid of in gully, short carbon fiber surface;Take out after standing 1h, make PCS react with the oxygen generation self-crosslinked oxidation in air in 140 DEG C of insulation 8h;Then will complete short carbon fiber ultrasonic disperse 5min in dimethylbenzene of crosslinking, take out post-drying;Circulation aforesaid operations 1~2 times, must arrive surface and have the loose monofilament short carbon fiber of uniform and smooth PCS coating.
CN201410721023.1A 2014-12-01 2014-12-01 The manufacture method of high-performance SiC ceramic based composites blade of aviation engine Active CN104529458B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201410721023.1A CN104529458B (en) 2014-12-01 2014-12-01 The manufacture method of high-performance SiC ceramic based composites blade of aviation engine

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201410721023.1A CN104529458B (en) 2014-12-01 2014-12-01 The manufacture method of high-performance SiC ceramic based composites blade of aviation engine

Publications (2)

Publication Number Publication Date
CN104529458A CN104529458A (en) 2015-04-22
CN104529458B true CN104529458B (en) 2016-08-17

Family

ID=52845145

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201410721023.1A Active CN104529458B (en) 2014-12-01 2014-12-01 The manufacture method of high-performance SiC ceramic based composites blade of aviation engine

Country Status (1)

Country Link
CN (1) CN104529458B (en)

Families Citing this family (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104874768B (en) * 2015-04-24 2016-11-23 昆明理工大学 A kind of method that the 3D of utilization print space structure prepares metal-base composites
US10195667B2 (en) 2015-11-23 2019-02-05 Delavan Inc. Powder removal systems
DE102017110362A1 (en) * 2017-05-12 2018-11-15 Psc Technologies Gmbh Process for the production of silicon carbide-containing three-dimensional objects
CN107353008B (en) * 2017-06-20 2020-03-17 西安交通大学 Preparation method of layered metal-ceramic composite material part
CN109516810A (en) * 2018-11-07 2019-03-26 三峡大学 A kind of preparation method of the porous silicon carbide ceramic based on P curved surface
CN111676384B (en) * 2020-07-06 2021-12-14 南阳师范学院 A kind of reinforced magnesium matrix composite material and preparation method thereof
CN111744388A (en) * 2020-07-16 2020-10-09 沈阳九和流体科技有限公司 Carbon fiber silicon carbide composite material stirrer
CN113735590B (en) * 2021-09-29 2022-06-28 北京理工大学 Preparation method and product of high-temperature-resistant electromagnetic wave-absorbing ceramic matrix composite material
CN116425559B (en) * 2023-04-24 2024-07-16 福建立亚新材有限公司 Preparation method of directional porous ceramic matrix composite material
CN120081673A (en) * 2025-04-28 2025-06-03 成都欣然动力科技有限公司 Aeroengine blade and preparation method thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102503503A (en) * 2011-11-07 2012-06-20 西安交通大学 Preparation method of machinable impregnation-reinforced silicon carbide composite ceramic
CN103113123A (en) * 2013-02-04 2013-05-22 西安交通大学 A kind of preparation method of SiCf/SiC ceramic matrix composite material turbine blade

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102503503A (en) * 2011-11-07 2012-06-20 西安交通大学 Preparation method of machinable impregnation-reinforced silicon carbide composite ceramic
CN103113123A (en) * 2013-02-04 2013-05-22 西安交通大学 A kind of preparation method of SiCf/SiC ceramic matrix composite material turbine blade

Also Published As

Publication number Publication date
CN104529458A (en) 2015-04-22

Similar Documents

Publication Publication Date Title
CN104529458B (en) The manufacture method of high-performance SiC ceramic based composites blade of aviation engine
CN104496508B (en) Manufacture method based on the SiC ceramic base turbine blade that photocuring 3D prints
CN103113112B (en) Preparation method of metal toughened ceramic-based composite material turbine blade
CN102875150B (en) Method for preparing silicon carbide ceramic impeller through gel casting and pressureless sintering
CN102964114B (en) Method for preparing composite ceramic material through utilizing ceramic and precursor
CN109320246B (en) A kind of high temperature oxidation resistant graphite ceramic composite material and preparation method thereof
CN104003732B (en) A kind of method of gel injection turbine blade ceramic-mould vacuum degreasing
CN104496507B (en) A kind of labyrinth ceramic part manufacture method towards gas turbine hot-end component
CN103130525B (en) A preparation method of high toughness porous SiC ceramic complex parts
CN105801154A (en) Method for preparing graphene toughened silicon carbide ceramic composite material
CN103288468A (en) A kind of preparation method of fiber reinforced carbon-silicon carbide-zirconium carbide matrix composite material
CN102898141A (en) Preparation method of high-heat-conduction aluminum nitride ceramic shaped part
CN106278335A (en) A kind of manufacture method of fiber alignment toughening ceramic based composites turbo blade
CN107129298B (en) graphene/ZrO2Method for preparing ceramic composite material
CN108658616B (en) ZrO (ZrO)2-SiO2Low-temperature rapid preparation method of base composite material
CN115849928B (en) Injection-molded aluminum oxide fiber reinforced composite material containing lanthanum phosphate interface layer and preparation method thereof
CN106083205B (en) A kind of method that integral alumina base ceramic-mould elevated temperature strength is improved by chemical vapor infiltration
CN103803950B (en) Boron nitride nanotube reinforced ceramic-based composite material and preparation method thereof
WO2007056895A1 (en) Compact foamed thyrite with high intensity and preparation method of the same
CN117658641B (en) Method for preparing high-density SiC ceramic based on selective laser 3D printing and two-step sintering
CN106866156A (en) A kind of low-k α Si3N4The preparation method of porous ceramics
CN112047737A (en) Infiltration method for silicon carbide-based ceramic with microstructure characteristics
CN106187263B (en) The manufacturing method and C/C-SiC composite material component of C/C-SiC composite material component
CN116730736A (en) A method for preparing SiC composite materials based on laser printing and vacuum-pressure-assisted in-situ impregnation of resin
CN105669206B (en) porous silicon carbide ceramic and preparation method thereof

Legal Events

Date Code Title Description
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant