CN113817933A - 陶瓷增强钛基复合材料、其制备方法及应用 - Google Patents
陶瓷增强钛基复合材料、其制备方法及应用 Download PDFInfo
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- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 80
- 239000010936 titanium Substances 0.000 title claims abstract description 70
- 239000000919 ceramic Substances 0.000 title claims abstract description 69
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 68
- 239000002131 composite material Substances 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000011159 matrix material Substances 0.000 claims abstract description 24
- 239000002245 particle Substances 0.000 claims abstract description 19
- 238000005245 sintering Methods 0.000 claims abstract description 19
- 239000011573 trace mineral Substances 0.000 claims abstract description 16
- 235000013619 trace mineral Nutrition 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 14
- 239000000956 alloy Substances 0.000 claims abstract description 13
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 12
- 239000010949 copper Substances 0.000 claims abstract description 10
- 229910052684 Cerium Inorganic materials 0.000 claims abstract description 8
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 8
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 8
- 229910052802 copper Inorganic materials 0.000 claims abstract description 8
- 229910052718 tin Inorganic materials 0.000 claims abstract description 8
- 229910052746 lanthanum Inorganic materials 0.000 claims abstract description 6
- 229910052727 yttrium Inorganic materials 0.000 claims abstract description 4
- 239000000843 powder Substances 0.000 claims description 27
- 238000010438 heat treatment Methods 0.000 claims description 24
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 12
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 11
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 11
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 10
- 239000011651 chromium Substances 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 8
- 239000011135 tin Substances 0.000 claims description 8
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000003825 pressing Methods 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 6
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims description 5
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims description 4
- 230000001681 protective effect Effects 0.000 claims description 3
- 150000001247 metal acetylides Chemical class 0.000 claims description 2
- 150000004767 nitrides Chemical class 0.000 claims description 2
- 229910021332 silicide Inorganic materials 0.000 claims description 2
- -1 borides Chemical class 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 9
- 238000010924 continuous production Methods 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 4
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- 229910000765 intermetallic Inorganic materials 0.000 abstract description 3
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 abstract description 2
- 238000002485 combustion reaction Methods 0.000 abstract description 2
- 239000013078 crystal Substances 0.000 abstract description 2
- 239000003063 flame retardant Substances 0.000 abstract description 2
- 238000002844 melting Methods 0.000 abstract description 2
- 230000008018 melting Effects 0.000 abstract description 2
- 229910044991 metal oxide Inorganic materials 0.000 abstract description 2
- 150000004706 metal oxides Chemical class 0.000 abstract description 2
- 230000003647 oxidation Effects 0.000 abstract description 2
- 238000007254 oxidation reaction Methods 0.000 abstract description 2
- 238000007670 refining Methods 0.000 abstract description 2
- 239000006104 solid solution Substances 0.000 abstract description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical group [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 14
- 239000011812 mixed powder Substances 0.000 description 12
- 229910001069 Ti alloy Inorganic materials 0.000 description 11
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 9
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- 229910052581 Si3N4 Inorganic materials 0.000 description 2
- 229910010039 TiAl3 Inorganic materials 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 2
- 229910010271 silicon carbide Inorganic materials 0.000 description 2
- OCKGFTQIICXDQW-ZEQRLZLVSA-N 5-[(1r)-1-hydroxy-2-[4-[(2r)-2-hydroxy-2-(4-methyl-1-oxo-3h-2-benzofuran-5-yl)ethyl]piperazin-1-yl]ethyl]-4-methyl-3h-2-benzofuran-1-one Chemical compound C1=C2C(=O)OCC2=C(C)C([C@@H](O)CN2CCN(CC2)C[C@H](O)C2=CC=C3C(=O)OCC3=C2C)=C1 OCKGFTQIICXDQW-ZEQRLZLVSA-N 0.000 description 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 229910009871 Ti5Si3 Inorganic materials 0.000 description 1
- 238000012669 compression test Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000010406 interfacial reaction Methods 0.000 description 1
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- B22F3/10—Sintering only
- B22F3/1003—Use of special medium during sintering, e.g. sintering aid
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Abstract
本申请涉及陶瓷增强钛基复合材料、其制备方法及应用。该陶瓷增强钛基复合材料,采用较低熔点的元素(Al、Cu、Cr、Sn中的至少一种)作为主要合金元素,采用Ce、Y、La中的至少一种作为微量元素,这些元素能与钛形成固溶体,降低烧结温度,同时生成金属间化合物,减少烧结过程中陶瓷颗粒与钛基体的界面反应,并且微量元素还起到细化晶粒的作用,各元素协调一致,提高了材料强度,降低了能耗与成本,适合工业化连续生产,且这些元素在摩擦制动时能在摩擦表面形成金属氧化物,减少钛的氧化燃烧,具有一定的阻燃效果,适用于交通运输领域里的高速摩擦制动。
Description
技术领域
本发明涉及复合材料技术领域,特别是涉及陶瓷增强钛基复合材料、其制备方法及应用。
背景技术
钛及钛合金不仅具有很高的比强度和比刚度,而且具有优异的耐高温性能以及抗腐蚀性能,在航空航天、汽车制造、体育器材和医疗器械等领域的应用前景非常广泛。但是由于钛合金本身具有不耐磨、硬度偏低及生产成本高等弱点,严重阻碍了它在工程中的大量应用。通过在钛基体中添加相应的增强相制备钛基复合材料已成为钛合金的一种发展趋势。陶瓷增强钛基复合材料是以高强度和高模量陶瓷颗粒或晶须为增强相,以钛或钛合金为基体而制备的一种材料,具有比钛合金更高的比强度和比模量,极佳的抗疲劳和抗蠕变性能,以及优异的耐高温性能和耐蚀性能,并克服了钛合金不耐磨、硬度偏低等缺点。
目前,制备陶瓷增强钛基复合材料的方法主要有熔铸法和粉末冶金法两大类。熔铸法存在易产生缺陷,成分易于偏析、组织不均匀、生产效率低、增强相含量受限等问题。与熔铸法相比,粉末冶金具有能耗低、材料利用率高、微观组织细小、成分均匀可控、易实现近净成形等优点。然而,粉末冶金法在制备陶瓷增强钛基复合材料时,由于热动力学稳定的陶瓷增强相很难与高活性的钛合金基体形成良好的化学和冶金结合,因此烧结通常需要在真空或惰性气氛及较高的温度条件下进行,增加了能耗与成本,使连续化生产变得困难,且钛基体非常活跃,在上述烧结条件下容易与陶瓷增强相发生界面反应。影响材料强度。此外,由于钛金属非常活跃,在高速摩擦制动的温度压力和空气流速下能够燃烧而产生危险,限制了其在高速摩擦制动领域里的应用。
发明内容
基于此,有必要提供一种能够降低烧结温度,减少陶瓷增强相与钛基体在烧结时的界面反应,适用于高速摩擦制动领域的陶瓷增强钛基复合材料,具体方案如下:
一种陶瓷增强钛基复合材料,以质量百分含量计,由5%~25%的主要合金元素、≤1.5%的微量元素、10%~40%的陶瓷颗粒及余量的钛元素组成,其中,主要合金元素选自铝(Al)、铜(Cu)、铬(Cr)、锡(Sn)中的至少一种;微量元素选自铈(Ce)、钇(Y)、镧(La)中的至少一种。
在其中一个实施例中,上述陶瓷增强钛基复合材料,以质量百分含量计,由5%~20%的铝、1%~6%的铬、0.5%~10%的铜、0.5%~5%的锡、≤1.5%的上述微量元素、10%~40%的上述陶瓷颗粒及余量的钛元素组成。
在其中一个实施例中,上述陶瓷增强钛基复合材料,以质量百分含量计,由8%~15%的铝、2.5%~4%的铬、1.5%~6%的铜、1%~3%的锡、≤1.5%的所述微量元素、10%~40%的所述陶瓷颗粒及余量的钛元素组成。
在其中一个实施例中,上述陶瓷颗粒选自碳化物(如TiC、SiC、B4C等)、硼化物(如TiB、TiB2等)、氮化物(如Si3N4)及硅化物(如Ti5Si3)中的至少一种。
在本实施方式中,上述陶瓷颗粒为碳化钛(TiC)。
在其中一个实施例中,上述陶瓷增强钛基复合材料的密度为3.86g/cm3~4.32g/cm3。
上述陶瓷增强钛基复合材料,采用较低熔点的元素(Al、Cu、Cr、Sn中的至少一种)作为主要合金元素,采用Ce、Y、La中的至少一种作为微量元素,这些元素能与钛形成固溶体,降低烧结温度,同时可生成部分金属间化合物,减少烧结过程中陶瓷颗粒与钛基体的界面反应,并且微量元素还起到细化晶粒的作用,各元素协调一致,提高了材料强度,降低了能耗与成本,适合工业化连续生产,且这些元素在摩擦制动时能在摩擦表面形成金属氧化物,减少钛的氧化燃烧,具有一定的阻燃效果,适用于交通运输领域里的高速摩擦制动。
本申请还提供一种上述任一项陶瓷增强钛基复合材料的制备方法,具体方案如下:
一种陶瓷增强钛基复合材料的制备方法,包括如下步骤S110~S120:
S110、提供上述陶瓷颗粒及上述钛元素、主要合金元素和微量元素的原料粉体。
在本实施方式中,上述钛元素、主要合金元素和微量元素的原料粉体为单质粉或合金粉。
S120、将上述陶瓷颗粒及上述钛元素、主要合金元素和微量元素的原料粉体按比例混合均匀后,依次进行冷压、烧结,得到陶瓷增强钛基复合材料。
在其中一个实施例中,混合的条件为:转速15r/min~35r/min,时间45~60分钟。
具体的,混合在混料机中进行。
可以理解,混合还可以在其他条件中进行,只要能将上述陶瓷颗粒和各元素的原料粉体混合均匀即可。
在其中一个实施例中,冷压的条件为:加压速率1mm/s~5mm/s,压力300MPa~500MPa,保压3~10s。
具体的,冷压在模具中进行,冷压完成后脱模即可。
在其中一个实施例中,烧结的条件为:在保护性气体氛围中,以8℃/min~15℃/min的加热速率,升温至350℃~450℃,保温15~30分钟,再升温至950℃~980℃,保温45~120分钟,最后降温至200℃以下。
其中,保护性气体氛围为氩气。
上述烧结过程中,升温至350℃~450℃,保温15~30分钟,主要用于除蜡。
上述陶瓷增强钛基复合材料的制备方法简便、成本低,满足工业化连续生产要求,且制备得到的陶瓷增强钛基复合材料,耐磨性能较好,工作温度可达到600℃以上,比传统钢铁制动材料减重40%左右,适用于交通运输领域的高速摩擦制动。
附图说明
图1为实施例1制备的陶瓷增强钛基复合材料不同部位的显微组织图;
图2为实施例2制备的陶瓷增强钛基复合材料与对比例1制备的钛合金的磨损对比实验图;
图3为实施例3制备的陶瓷增强钛基复合材料在650℃环境下的压缩应力应变曲线图。
具体实施方式
为了便于理解本发明,下面将对本发明进行更全面的描述,并给出了本发明的较佳实施例。但是,本发明可以以许多不同的形式来实现,并不限于本文所描述的实施例。相反地,提供这些实施例的目的是使对本发明的公开内容的理解更加透彻全面。
除非另有定义,本文所使用的所有的技术和科学术语与属于本发明的技术领域的技术人员通常理解的含义相同。本文中在本发明的说明书中所使用的术语只是为了描述具体的实施例的目的,不是旨在于限制本发明。
以下为具体实施例。
实施例1
(1)将如下粉体:10g碳化钛粉、33g钛粉、4g铝粉、1.2g铬粉、0.8g铜粉、0.5g锡粉、0.1g铈粉,在混料机中混合均匀得到混合粉体;
(2)将上述混合粉体,填充至模具中在室温下,以5mm/s的加压速率升至400MPa,保压3s,脱模,得到直径12mm,高度约12mm的坯体;
(3)将上述坯体放入烧结炉中,在氩气保护下,以15℃/min的加热速率,先升温至350-450℃,除蜡保温15分钟,再升温至950-980℃,保温120min,最后降温至200℃以下,得到陶瓷增强钛基复合材料。
将实施例1制备的陶瓷增强钛基复合材料试样在室温下打磨抛光后,观察其显微组织,如图1所示。灰色的块状区域a为TiC颗粒增强相,较浅区域b为金属间化合物TiAl3(Cu/Cr)和TiAl3,黑色区域c为孔洞,较暗区域d为复合材料的基体。其主要成份为Ti8Al2.5Cr1.5Cu1Sn+20%TiC,密度为4.02g/cm3。
实施例2
(1)将如下粉体:10g碳化钛粉、33g钛粉、4g铝粉、1.2g铬粉、0.8g铜粉、0.5g锡粉、0.2g钇粉分别在混料机中混合均匀得到混合粉体;
(2)将上述混合粉体,填充至模具中在室温下,以1mm/s的加压速率升至300MPa,保压10s,脱模,得到直径12mm,高度约12mm的坯体;
(3)将上述坯体放入烧结炉中,在氩气保护下,以8℃/min的加热速率,先升温至350-450℃,除蜡保温30分钟,再升温至950-980℃,保温45min,最后降温至200℃以下,得到陶瓷增强钛基复合材料。
实施例2制备的陶瓷增强钛基复合材料的主要成分为Ti8Al2.5Cr1.5Cu1Sn+20%TiC,密度4.01g/cm3。
对比例1
对比例1与实施例2基本相同,不同的是,对比例1在步骤(1)中的粉体组成如下:53g钛粉、0.8g镍粉、1.2g铜粉、0.5g锡粉。
对比例1制备的钛合金的主要成分为Ti2Cu1.5Ni1Sn,密度4.13g/cm3。
将实施例2制备的材料试样和对比例1制备的材料试样在室温下进行80目碳化硅磨料磨损对比实验,结果如图2所示。对比例1制备的材料试样的体积损失比实施例2制备的材料试样的体积损失高出约3.5倍,说明本申请的陶瓷增强钛基复合材料的耐磨性能优于钛合金材料。
实施例3
(1)将如下粉体:10g碳化钛粉、33g钛粉、4g铝粉、1.2g铬粉、0.8g铜粉、0.5g锡粉、0.2g镧粉,在混料机中混合均匀得到混合粉体;
(2)将上述混合粉体,填充至模具中,在室温下,以3mm/s的加压速率升至500MPa,保压5s,脱模,得到直径12mm,高度12mm的坯体;
(3)将上述坯体放入烧结炉中,在氩气保护下,以10℃/min的加热速率,先升温至350-450℃,除蜡保温20分钟,再升温至950-980℃,保温90min,最后降温至200℃以下,得到陶瓷增强钛基复合材料。
实施例3制备的陶瓷增强钛基复合材料的主要成分为:Ti8Al2.5Cr1.5Cu1Sn+20%TiC,密度4.02g/cm3。
将实施例3制备的陶瓷增强钛基复合材料试样加热至650℃并在650℃环境下进行热压缩实验。结果如图3所示。复合材料试样在该温度下仍然具有一定的抗压强度。应力-应变曲线显示,复合材料的最大应力达到90MPa以上。高速磨擦制动领域里的最大制动压应力在较高温度时显著低于20MPa。可见,瓷颗粒增强钛基粉末冶金复合材料具有优异的耐磨性能和较好的耐温性能。
实施例4
(1)将如下粉体:20gTiB粉、25.5g钛粉、2.5g铝粉、1.25g铜粉、0.5g锡粉、0.1g铈粉、0.1g钇粉,在混料机中混合均匀得到混合粉体;
(2)将上述混合粉体,填充至模具中在室温下,以2mm/s的加压速率升至300MPa,保压8s,脱模,得到直径12mm,高度约12mm的坯体;
(3)将上述坯体放入烧结炉中,在氩气保护下,以12℃/min的加热速率,先升温至350-450℃,除蜡保温20分钟,再升温至950-980℃,保温80min,最后降温至200℃以下,得到陶瓷增强钛基复合材料,其主要成分为Ti5Al2.5Cu1Sn+40%TiB。
实施例5
(1)将如下粉体:20gSi3N4粉、25g钛粉、2.5g铜粉、2g铬粉、0.1g铈粉,在混料机中混合均匀得到混合粉体;
(2)将上述混合粉体,填充至模具中在室温下,以4mm/s的加压速率升至500MPa,保压5s,脱模,得到直径12mm,高度约12mm的坯体;
(3)将上述坯体放入烧结炉中,在氩气保护下,以15℃/min的加热速率,先升温至350-450℃,除蜡保温15分钟,再升温至950-980℃,保温100min,最后降温至200℃以下,得到陶瓷增强钛基复合材料,其主要成分为Ti5Cu4Cr+40%Si3N4。
实施例6
(1)将如下粉体:20gTi5Si3粉、24.5g钛粉、5g铝粉、0.1g铈粉、0.1g钇粉、0.1g镧粉,在混料机中混合均匀得到混合粉体;
(2)将上述混合粉体,填充至模具中在室温下,以5mm/s的加压速率升至300MPa,保压10s,脱模,得到直径12mm,高度约12mm的坯体;
(3)将上述坯体放入烧结炉中,在氩气保护下,以15℃/min的加热速率,先升温至350-450℃,除蜡保温30分钟,再升温至950-980℃,保温120min,最后降温至200℃以下,得到陶瓷增强钛基复合材料,其主要成分为Ti10Al+40%Ti5Si3。
以上所述实施例仅表达了本发明的几种实施方式,其描述较为具体和详细,但并不能因此而理解为对本发明专利范围的限制。应当指出的是,对于本领域的普通技术人员来说,在不脱离本发明构思的前提下,还可以做出若干变形和改进,这些都属于本发明的保护范围。因此,本发明专利的保护范围应以所附权利要求为准。
Claims (10)
1.一种陶瓷增强钛基复合材料,其特征在于,以质量百分含量计,由5%~25%的主要合金元素、≤1.5%的微量元素、10%~40%的陶瓷颗粒及余量的钛元素组成,所述主要合金元素选自铝、铜、铬、锡中的至少一种;所述微量元素选自铈、钇、镧中的至少一种。
2.根据权利要求1所述的陶瓷增强钛基复合材料,其特征在于,以质量百分含量计,由5%~20%的铝、1%~6%的铬、0.5%~10%的铜、0.5%~5%的锡、≤1.5%的所述微量元素、10%~40%的所述陶瓷颗粒及余量的钛元素组成。
3.根据权利要求2所述的陶瓷增强钛基复合材料,其特征在于,以质量百分含量计,由8%~15%的铝、2.5%~4%的铬、1.5%~6%的铜、1%~3%的锡、≤1.5%的所述微量元素、10%~40%的所述陶瓷颗粒及余量的钛元素组成。
4.根据权利要求1所述的陶瓷增强钛基复合材料,其特征在于,所述陶瓷颗粒选自碳化物、硼化物、氮化物及硅化物中的至少一种。
5.根据权利要求1~4任一项所述的陶瓷增强钛基复合材料,其特征在于,所述陶瓷增强钛基复合材料的密度为3.86g/cm3~4.32g/cm3。
6.一种权利要求1~5任一项所述的陶瓷增强钛基复合材料的制备方法,其特征在于,包括如下步骤:
提供所述陶瓷颗粒及所述钛元素、主要合金元素和微量元素的原料粉体;
将所述陶瓷颗粒和所述钛元素、主要合金元素和微量元素的原料粉体按比例混合均匀后,依次进行冷压、烧结,得到所述陶瓷增强钛基复合材料。
7.根据权利要求6所述的陶瓷增强钛基复合材料的制备方法,其特征在于,所述混合的条件为:转速15r/min~35r/min,时间45~60分钟。
8.根据权利要求6所述的陶瓷增强钛基复合材料的制备方法,其特征在于,所述冷压的条件为:加压速率1mm/s~5mm/s,压力300MPa~500MPa,保压3~10s。
9.根据权利要求6所述的陶瓷增强钛基复合材料的制备方法,其特征在于,所述烧结的条件为:在保护性气体氛围中,以8℃/min~15℃/min的加热速率,升温至350℃~450℃,保温15~30分钟,再升温至950℃~980℃,保温45~120分钟,最后降温至200℃以下。
10.一种权利要求1~5任一项所述的陶瓷增强钛基复合材料或权利要求6~9任一项所述的制备方法制得的陶瓷增强钛基复合材料在摩擦制动领域中的应用。
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