CN1712167A - 用硅基组合物密封的复合材料部件的钎焊方法 - Google Patents
用硅基组合物密封的复合材料部件的钎焊方法 Download PDFInfo
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- CN1712167A CN1712167A CNA2005100791121A CN200510079112A CN1712167A CN 1712167 A CN1712167 A CN 1712167A CN A2005100791121 A CNA2005100791121 A CN A2005100791121A CN 200510079112 A CN200510079112 A CN 200510079112A CN 1712167 A CN1712167 A CN 1712167A
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- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
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- B23K1/19—Soldering, e.g. brazing, or unsoldering taking account of the properties of the materials to be soldered
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Abstract
为了阻止钎焊组合物(40)与两个要通过钎焊装配在一起的由热结构复合材料制成的部件(20,30)的材料中存在的硅(21,31)或其它元素接触,至少在所述部件的待接合表面(S20,S30)上形成耐火陶瓷材料层(22,32),所述耐火陶瓷材料在钎焊温度下与硅不反应。
Description
技术领域
本发明涉及通过钎焊(brazing)装配热结构(thermostructural)复合材料部件。
背景技术
由热结构复合材料制成的具有复杂形状的结构难于直接制成一个部件。通常优选使用形状简单的元件通过装配来构建特定结构,特别是通过钎焊来构建结构。
一般而言,钎焊是一种包括使金属基组合物在需要装配于一起的部件之间熔化的装配技术。钎焊的主要优点是与焊接(welding)不同,它能够在不熔化构成所述部件的材料的情况下装配需要装配于一起的部件。举例来说,在通常用于将热结构复合材料部件装配在一起的钎焊组合物或合金中包括:硅+金属硅化物、硅+任选合金化的镓等合金,以及商标名为Cusil-ABA、Ticusil、Incusil和Brasic的金属组合物。
热结构复合材料因其良好的机械性质并能够在高温下保持这些性质而著称。它们包括通过耐火基质增加密度并使用耐火纤维作为增强体(reinforcement)的复合材料。作为非穷举的实例,所述材料包括碳-碳(C/C)复合材料(使用碳基质增加密度并使用碳纤维作为增强体(reinforcement));以及陶瓷基质复合材料(CMC),例如C/SiC复合材料(由碳制成的增强体和由碳化硅制成的基质)、SiC/SiC复合材料(纤维和基质均由碳化硅制成)、C/C-SiC复合材料(用碳纤维作为增强体,并且基质包括碳相(通常接近所述碳纤维)和碳化硅相);用气态SiO、液态Si等硅化的C/C复合材料。
获得由热结构复合材料制成的部件的常用方法包括液相技术和气相技术。
液相技术包括制造基本上具有要制造的部件形状并且构成复合材料的增强体的纤维预制件,以及用包含基质材料前体的液体组合物浸渍所述预制件。所述前体通常是聚合物形式,例如树脂,其可以在溶剂中稀释。在去除任何溶剂后,并且在固化聚合物后,通过热处理将所述前体转变成耐火相。为了实现所需的致密度,可以实施多次连续的浸渍循环。举例来说,碳的液体前体可以是具有较高焦炭含量的树脂(例如酚醛树脂),而陶瓷(特别是SiC)的液体前体可以是多碳硅烷(polycarbosilane)(PCS)型或者多钛碳硅烷(polytitanocarbosilane)(PTCS)型或者聚硅氨烷(PSZ)型树脂。
气相技术包括化学气相渗入。将相应于待制造部件的纤维预制件被放在允许反应气体进入的加热炉中。为了使沉积的固体材料与所述增强纤维接触,从而在预制件中形成基质,选择加热炉内的压力和温度以能使气体在预制件的孔内扩散,并使气体组分分解或者在多种气体组分之间发生反应。举例来说,碳的气体前体可以是通过裂解得到的碳的烃例如甲烷,并且陶瓷(特别是SiC)的气体前体可以是甲基三氯硅烷(MTS),通过分解MTS(例如在氢的存在下)可以得到SiC。
还存在使用液体技术和气体技术的组合技术。
但是,无论使用哪种致密化方法,由于纤维预制件致密化的不可避免的不完全性质,由热结构复合材料制成的部件总是存在残余孔隙。典型地,在致密化期间没有特别处理的情况,所得部件存在最小体积含量约为10%的孔。所述孔隙度表示存在较大或较小尺寸的孔和/或裂纹,其彼此相通,并且向部件的表面开放。
如图1中所例示,通过在待接合部件的表面S1和S2之间插入钎焊层3来钎焊,从而将由热结构复合材料M制成的部件1和2装配在一起。但是,因为制造所述部件的材料的多孔性质,部分夹在部件1和2之间的钎焊组合物3沿向部件表面开放的孔而渗入材料的孔P内,从而在两个表面之间形成没有任何钎焊组合物的局部4。缺乏钎焊组合物会导致在两个部件之间有缺陷的结合,并导致装配质量的降低。
上述问题公知的解决方法包括通过硅化,即通过向材料内引入基于熔融硅的组合物而填充热结构复合材料部件的孔隙。这种硅化方法本身是已知的,并且具体地说在下面的文献中描述:FR 2 653 763、US 4 626 516、EP 0 636 700和FR 03/01871。
但是,尽管可以认为以上述方式硅化的热结构复合材料足以不会渗透,从而在表面上保留钎焊组合物,但是在材料中存在一种或多种硅化物相会导致其它问题。
大多数用于钎焊目的的合金,以及上述组合物都包含显著量的金属组分,相应于与硅反应的过渡金属(例如Cu、Fe、Ni、Mn等),这会导致在粘结中形成易碎的金属硅化物。
此外,当使用非反应性的或者具有控制反应性的在BraSic技术中实现的钎焊组合物时,在钎焊温度(约1400℃)下,在所述钎焊组合物和所述材料的孔中存在的硅之间发生相互扩散,以至于在部件之间形成粘结的预期物理化学转变不再受控。由于在钎焊期间在液态中的扩散,所述材料中的硅与钎焊组合物之间的直接接触会改变钎焊组合物的组成比例,从而改变其性质。
另外,在通过钎焊装配在一起的硅化热结构复合材料的情况中,在重新加工或者重新修复粘结时出现另一个问题。如果两个硅化热结构复合材料部件装配不良,或者最初或者随后削弱,或者攻击钎焊接点,必须可以除去残留的钎焊材料,从而清洁所述部件,然后再次适当地将其钎焊到一起。除去钎焊组合物并清洁所述部件需要在腐蚀性的浴(酸或碱)中处理,其会攻击硅化部分残留的硅。在这些条件下,两个硅化热结构复合材料部件之间钎焊粘结的拆卸导致所述部件不可再用,这就造成费用和/或再循环。
发明内容
本发明寻求提供一种能够通过钎焊将热结构复合材料部件装配在一起的方法,其中至少接触表面通过用硅基组合物浸渍而密封,从而避免了上述缺点,并且特别是阻止了钎焊组合物和部件材料中存在的硅之间的任何反应或扩散。
根据本发明,通过如下方法实现其目标:在密封步骤后和钎焊步骤前,至少在待接合部件的表面上形成耐火陶瓷材料层,所述陶瓷材料在钎焊温度下与硅不反应。具体地说,这种材料可以选自含硅陶瓷,例如氮化硅(Si3N4)或碳化硅(SiC)。
因此,因为耐火陶瓷层保护了待钎焊材料的表面,所以钎焊组合物不会与所述材料中存在的硅或者其它元素接触。
因此,可以避免钎焊组合物和所述材料中的硅之间反应或扩散的危险,从而可以更好地控制钎焊,并在两个部件之间形成均匀且优质的粘结。
此外,所述陶瓷(例如碳化硅)的耐腐蚀性很好,所以在重新加工或者重新修复粘结的情况中,可以用腐蚀性化学试剂攻击钎焊组合物而不会伤害部件材料。
所述陶瓷层可以通过化学气相沉积或者化学气相渗入来形成。
所述部件表面上形成的陶瓷层表面在钎焊前可以重叠。所述陶瓷层的平均厚度优选在1微米(μm)至100μm的范围内,例如约为50μm。
所用的钎焊组合物优选基于对于覆盖待接合部件表面的陶瓷为非反应性的或者具有控制反应性的金属。
在一个具体的实施方案中,在钎焊步骤前,在待钎焊到一起的部件上部分施用抗湿润剂,以使钎焊组合物仅润湿需要装配在一起的那些表面部分。
在另一个实施方案中,为了通过两个待接合部件之间的毛细作用来传输钎焊组合物,使用芯(wick)(例如由碳纤维构成的芯)借助毛细作用将液态钎焊组合物传输到待接合部件之间。
附图说明
参考附图,本发明的其它特征和优点将从下面以非限制性实施例给出的本发明具体实施方案的说明中变得明显,附图中:
如上所述,图1是当钎焊两个多孔热结构复合材料部件时所得结果的示意图;
图2是表示实施本发明方法的连续步骤的流程图;
图3表示通过硅化密封并且已经在其表面上沉积了碳化硅层后的热结构复合材料部件的一部分;
图4是图3所示相同部分在碳化硅层经过磨光(lap)后的图;
图5表示在使用毛细芯时怎样在两个部件之间实施钎焊;及
图6是表示根据本发明方法将两个部件钎焊在一起后所得结构的图。
具体实施方式
本发明的钎焊装配方法适用于任何类型的硅化热结构复合材料,即任何包括耐火纤维增强体并通过耐火基质增加密度的材料,例如C/C材料,或者CMC材料,并且特别是C/SiC、SiC/SiC、C/C-SiC等材料。
参照图2,实施根据本发明的钎焊两个已经通过硅化密封的由热结构复合材料制成的部件的方法包括下面的步骤。
第一个步骤(步骤10)包括密封所述部件的热结构复合材料,至少密封待接合的材料表面,通过用基于熔融硅的组合物浸渍所述热结构复合材料而填充其中的孔隙。硅基组合物可以由硅或者由硅合金(例如SiGe)和至少一种其它材料来构成,具体地说所述其它材料选自:铁、钴、钛、锆、钼、钒、碳和硼。用硅基组合物浸渍热结构复合材料是一种本身已知的技术,并且具体地说在下面的文献中描述:FR 2653 763、US 4 626 516、EP 0 636 700和FR 03/01871。
第二个步骤(步骤11)包括对两个要置于一起的部件的表面进行处理。为此,加工部件的接触表面,使之适合两个部件之间对接平面的形状。
一旦完成对所述表面的处理,在至少一个待钎焊的表面上沉积耐火陶瓷(步骤12)。所述耐火陶瓷选自在钎焊温度下与硅不反应的材料。一般而言,任何相应于硅衍生物(例如Si3N4或SiC)的陶瓷都可以用来保护需要钎焊在一起的部件的表面。在本文公开的实施例中,沉积SiC。所述沉积可以通过化学气相沉积(CVD)或者通过化学气相渗入(CVI)来实施。在任一情况下,在允许碳化硅的气态前体(例如甲基三氯硅烷(MTS))进入,从而可以在气态氢气(H2)的存在下,通过MTS的分解得到碳化硅的加热炉中发生沉积。通过化学气相沉积或者化学气相渗入获得碳化硅所需的反应气体的性质及压力和温度条件都是公知的。
图3显示了由热结构复合材料M制成的部件20的一部分,其中孔隙例如已经通过用硅基熔融组合物21浸渍而填充,需要与另一部件的相应表面钎焊的部件20的表面S20被覆盖在碳化硅层22中。
这就在每个待钎焊部件的表面上形成了一层保护层,该层在随后的钎焊操作期间用来阻止钎焊组合物与部件表面上存在的硅接触。
尽管用于沉积陶瓷的方法(化学气相沉积或者化学气相渗入)容易控制所得沉积物的厚度,但是可能发生在以这种方法形成的碳化硅层22的表面上出现微起伏222(表面不规则的球粒)的情况。
在这种情况下,一旦已经沉积了陶瓷层,为了通过研磨消除较大的粗糙度,可以对其表面进行磨光(步骤13),但是对陶瓷致密层的攻击并不足以穿透它。如图4所示,得到基本上是平面的碳化物层,优选所述碳化物层的平均厚度e在10μm至100μm的范围内,例如约为50μm。在SiC的情况中,通过控制沉积的陶瓷的质量来获得所述厚度,如果使用磨光还要考虑磨光对厚度的影响。
此后,通过钎焊将这两个部件装配到一起。在常规方式中,钎焊操作包括两个主要步骤,即在需要彼此接合到一起的部件表面之间夹入钎焊组合物(步骤14),并进行热处理(步骤15),以将温度升高到钎焊组合物的熔点之上。
在第一种钎焊技术中,组合物可以直接沉积在待接合的表面上。在另一种技术中,可以通过毛细作用在部件之间传输组合物。为此,如图5所示,将“干的”(即未浸渍的)芯50(例如碳纤维形成的引流芯)插在两个表面S20和S30分别覆盖在碳化硅层22和32中的热结构复合材料部件20和30之间。所述芯的一端浸在含有钎焊组合物61的坩埚60中。然后,升高温度,直至钎焊组合物61变成流体,通过毛细作用沿所述芯吸入,并且分布在与所述芯接触的两个部件之间用于钎焊的整个表面上。
如图6所示,由此在两个部件20和30之间提供用于将它们粘结在一起的钎焊组合物接合40。因为根据本发明,在钎焊前部件20和30的表面S20和S30分别覆盖在碳化硅层22和32中,所以钎焊组合物与部件20和30表面上存在的硅21、31之间没有直接接触。
当将存在不连续或者复杂形状的接触表面的两个部件装配到一起时,可以在不需要钎焊的部件区域上沉积抗湿润剂,从而控制钎焊组合物的流动,使其仅润湿需要钎焊的部件区域。举例来说,所用的抗湿润剂可以是以气溶胶喷雾形式制备的氮化硼(BN),或者所谓的“Stop-Off”产品,例如由供应商Wesgo Metals销售的抗湿润剂Stopyt,或者由供应商Wall Colmonoy Limited销售的Nicrobraz物品。
举例来说,这种抗湿润剂可以在制造热交换器时使用,所述热交换器例如是那些在通过流体循环冷却的推进器喷嘴的扩散部分(diverging portion)的壁中使用的热交换器时使用。这种热交换器可以通过钎焊两个热结构复合材料面板来获得,如同文献FR 03/01039中所述,其至少一个面板具有形成流体循环沟道的沟槽。在钎焊操作之前,将抗湿润剂放在不需要钎焊在一起的面板区域,例如沟槽上。然后,可以将钎焊组合物以大致的方式沉积到待装配于一起的表面上的整个区域上,所述组合物随后迁移到未覆盖抗湿润剂的区域上。在钎焊后,根据抗湿润剂供应商提供的说明,抗湿润剂本身可以通过循环酸或者任何其它试剂来除去。
具体地说根据其与碳化硅的相容性来选择钎焊组合物,即优选选择与碳化硅不反应或者具有可控的反应性的组合物。举例来说,可以使用硅基组合物,例如那些在欧洲专利申请EP 0 806 402或美国专利第5 975 407中公开的组合物;硅+金属硅化物、硅+任选合金化的镓等合金;以及以下列商标名公知的金属组合物:Cusil-ABA、Ticusil、Incusil或Brasic。
因此,本发明的方法能使硅化的热结构复合材料部件钎焊在一起而在没有钎焊组合物和材料中硅之间发生反应或扩散的危险。这就保证了在部件之间形成良好的粘结。
另外,所述耐火陶瓷涂层能够保护部件材料的表面不被氧化,同时不会留下明显的硅。
此外,当沉积在这种部件表面上的陶瓷能承受比硅更高的温度时,可以使用熔化温度高于硅自身直接暴露在部件表面时的熔化温度的钎焊组合物。
Claims (11)
1.一种通过钎焊将两个由热结构复合材料(M)制成的部件(20,30)装配在一起的方法,所述方法包括至少密封所述部件的待接合表面(S20,S30)的在前步骤,其中通过用硅基组合物(21)浸渍所述部件来实施所述的密封,所述方法的特征在于在密封步骤后和钎焊步骤前,至少在所述部件的待接合表面(S20,S30)上形成耐火陶瓷材料层(22,32),所述陶瓷材料在钎焊温度下与硅不反应。
2.根据权利要求1的方法,其特征在于所述陶瓷材料是碳化硅或氮化硅。
3.根据权利要求1或权利要求2的方法,其特征在于在形成所述陶瓷材料层之前,加工待装配在一起的部件(20,30)的表面(S20,S30),以限定两个部件之间的对接区的形状。
4.根据权利要求1至3任何一项的方法,其特征在于所述耐火陶瓷材料层(22,32)通过化学气相沉积来形成。
5.根据权利要求1至3任何一项的方法,其特征在于所述耐火陶瓷材料层(22,32)通过化学气相渗入来形成。
6.根据权利要求1至5任何一项的方法,其特征在于在所述各部件表面上形成的所述耐火陶瓷材料层(22,32)的表面经过磨光。
7.根据权利要求1至6任何一项的方法,其特征在于所述耐火陶瓷材料层(22,32)的平均厚度在1微米至100微米的范围内。
8.根据权利要求7的方法,其特征在于所述耐火陶瓷材料层(22,32)的平均厚度约为50微米。
9.根据权利要求1至8任何一项的方法,其特征在于在所述钎焊步骤中使用的钎焊组合物是不与所述耐火陶瓷材料反应或者具有可控反应性的金属基组合物。
10.根据权利要求1至9任何一项的方法,其特征在于所述方法还包括在钎焊步骤之前,在所述部件的不需要钎焊的部分上施用抗湿润剂。
11.根据权利要求1至10任何一项的方法,其特征在于在所述钎焊步骤之前,借助位于所述部件的待接合表面(S20,S30)之间的芯(50),通过毛细作用来传输所述钎焊组合物。
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FR0406892A FR2872072B1 (fr) | 2004-06-24 | 2004-06-24 | Procede de brasage de pieces en materiau composite thermostructural siliciure |
FR0406892 | 2004-06-24 |
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CN1712167A true CN1712167A (zh) | 2005-12-28 |
CN100525979C CN100525979C (zh) | 2009-08-12 |
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EP (1) | EP1786586B1 (zh) |
JP (2) | JP4991529B2 (zh) |
KR (2) | KR101153560B1 (zh) |
CN (2) | CN100503119C (zh) |
AT (2) | AT502103B8 (zh) |
DE (2) | DE102005025071B4 (zh) |
FR (1) | FR2872072B1 (zh) |
GB (1) | GB2415401B (zh) |
IT (1) | ITTO20050443A1 (zh) |
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-
2004
- 2004-06-24 FR FR0406892A patent/FR2872072B1/fr not_active Expired - Lifetime
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- 2005-05-30 DE DE102005025071.8A patent/DE102005025071B4/de active Active
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- 2005-06-17 KR KR1020050052451A patent/KR101153560B1/ko active IP Right Grant
- 2005-06-21 US US11/157,398 patent/US20060006212A1/en not_active Abandoned
- 2005-06-22 WO PCT/FR2005/001566 patent/WO2006010814A1/fr active Application Filing
- 2005-06-22 US US11/630,577 patent/US20080190552A1/en not_active Abandoned
- 2005-06-22 EP EP05778794A patent/EP1786586B1/fr active Active
- 2005-06-22 KR KR1020077001639A patent/KR101092189B1/ko active IP Right Grant
- 2005-06-22 AT AT05778794T patent/ATE424962T1/de active
- 2005-06-22 DE DE602005013245T patent/DE602005013245D1/de active Active
- 2005-06-22 CN CNB2005800242546A patent/CN100503119C/zh active Active
- 2005-06-22 JP JP2007517360A patent/JP4991529B2/ja active Active
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- 2005-06-24 CN CNB2005100791121A patent/CN100525979C/zh active Active
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
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CN102009239A (zh) * | 2010-10-15 | 2011-04-13 | 北京航空航天大学 | 一种用于碳基材料及其制品的连接方法 |
CN102009239B (zh) * | 2010-10-15 | 2012-09-05 | 北京航空航天大学 | 一种用于碳基材料及其制品的连接方法 |
CN116178037A (zh) * | 2014-12-31 | 2023-05-30 | 沃特洛电气制造公司 | 用于连接材料的高温方法及利用该方法的装置 |
CN109071364A (zh) * | 2016-06-13 | 2018-12-21 | 株式会社Ihi | 陶瓷基复合材料部件及其制备方法 |
US11987533B2 (en) | 2016-06-13 | 2024-05-21 | Ihi Corporation | Ceramic matrix composite component and method of producing the same |
CN108274086A (zh) * | 2018-01-24 | 2018-07-13 | 哈尔滨工业大学 | 一种两步法高温钎焊碳纤维增强碳基复合材料的方法 |
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