CN100522887C - 具有对潮湿暴露的增强的抵抗力的用于碳-碳刹车材料的抗氧化*** - Google Patents
具有对潮湿暴露的增强的抵抗力的用于碳-碳刹车材料的抗氧化*** Download PDFInfo
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- CN100522887C CN100522887C CNB2005800299027A CN200580029902A CN100522887C CN 100522887 C CN100522887 C CN 100522887C CN B2005800299027 A CNB2005800299027 A CN B2005800299027A CN 200580029902 A CN200580029902 A CN 200580029902A CN 100522887 C CN100522887 C CN 100522887C
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- boracic
- graphite
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- CREMABGTGYGIQB-UHFFFAOYSA-N carbon carbon Chemical compound C.C CREMABGTGYGIQB-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 239000011203 carbon fibre reinforced carbon Substances 0.000 title claims abstract description 19
- 230000003078 antioxidant effect Effects 0.000 title claims abstract description 14
- 239000003963 antioxidant agent Substances 0.000 title claims abstract description 13
- 239000000463 material Substances 0.000 title description 14
- 239000002131 composite material Substances 0.000 claims abstract description 42
- 239000011521 glass Substances 0.000 claims abstract description 40
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 29
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 19
- 239000004917 carbon fiber Substances 0.000 claims abstract description 19
- 239000010439 graphite Substances 0.000 claims abstract description 18
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 18
- 229910052582 BN Inorganic materials 0.000 claims abstract description 15
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 14
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052796 boron Inorganic materials 0.000 claims abstract description 13
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 11
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- 239000011153 ceramic matrix composite Substances 0.000 claims abstract description 8
- 229910052915 alkaline earth metal silicate Inorganic materials 0.000 claims abstract description 6
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 17
- 229910052728 basic metal Inorganic materials 0.000 claims description 13
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- 150000003016 phosphoric acids Chemical class 0.000 claims description 6
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 claims description 2
- 229910019142 PO4 Inorganic materials 0.000 abstract description 8
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- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 abstract 1
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- ZOXJGFHDIHLPTG-BJUDXGSMSA-N Boron-10 Chemical compound [10B] ZOXJGFHDIHLPTG-BJUDXGSMSA-N 0.000 description 5
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- 229910052700 potassium Inorganic materials 0.000 description 3
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- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 description 2
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- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
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- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
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- 208000034189 Sclerosis Diseases 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
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- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- 150000001639 boron compounds Chemical class 0.000 description 1
- 229910052810 boron oxide Inorganic materials 0.000 description 1
- -1 boron oxide compound Chemical class 0.000 description 1
- 125000000707 boryl group Chemical group B* 0.000 description 1
- 238000009954 braiding Methods 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 150000001721 carbon Chemical class 0.000 description 1
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- 238000003763 carbonization Methods 0.000 description 1
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- 230000008595 infiltration Effects 0.000 description 1
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- 229910000464 lead oxide Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
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- 229920003986 novolac Polymers 0.000 description 1
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- 239000000047 product Substances 0.000 description 1
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- 230000000630 rising effect Effects 0.000 description 1
- 229910052701 rubidium Inorganic materials 0.000 description 1
- IGLNJRXAVVLDKE-UHFFFAOYSA-N rubidium atom Chemical compound [Rb] IGLNJRXAVVLDKE-UHFFFAOYSA-N 0.000 description 1
- 239000005368 silicate glass Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000013517 stratification Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000007669 thermal treatment Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- LRXTYHSAJDENHV-UHFFFAOYSA-H zinc phosphate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O LRXTYHSAJDENHV-UHFFFAOYSA-H 0.000 description 1
- 229910000165 zinc phosphate Inorganic materials 0.000 description 1
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- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
- C03C1/006—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels to produce glass through wet route
- C03C1/008—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels to produce glass through wet route for the production of films or coatings
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- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
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- Materials Engineering (AREA)
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- Structural Engineering (AREA)
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- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- General Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Composite Materials (AREA)
- Mechanical Engineering (AREA)
- Paints Or Removers (AREA)
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- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Application Of Or Painting With Fluid Materials (AREA)
Abstract
改进涂覆制品(19)内潮湿抵抗力的方法,该涂覆制品(19)包括碳-碳复合材料部件(10),石墨部件(10),或基于碳纤维和/或石墨的陶瓷基体复合材料部件(10)。部件(10)优选地配置为航空器着陆***刹车盘。该方法包括以下步骤:(A)提供碳-碳复合材料部件(10),石墨部件(10),或基于碳纤维和/或石墨的陶瓷基体复合材料部件(10);(B)使用含磷的具有约1-10密耳厚度的内涂层(11)覆盖所述部件(10);及(C)使用含硼的具有约1-10密耳厚度的玻璃外涂层(12)覆盖因此产生的内涂覆部件(10,11)。外涂层含20-50wt%的碱金属或碱土金属硅酸盐,3-25wt%的碱金属氢氧化物,高达10wt%的氮化硼,及5-40wt%的元素硼和5-40wt%的碳化硼的一种或两者。外涂层基本上没有磷酸和磷酸盐。以及用规定的内涂层/外涂层的组合涂覆的制品。
Description
发明领域
本发明涉及用于碳-碳复合材料和诸如石墨之类的其他碳材料的新颖的抗氧化涂层***,及涉及氧化保护复合材料的制备方法。该发明在航空器刹车***领域特别有用。
发明背景
例如在飞机刹车***中使用的碳纤维或C-C复合材料遭受氧化和因此造成的重量损失(即,质量损失)。这些碳复合材料的氧化重量损失通常通过由具有抗氧化涂层的碳复合材料制成的涂覆制品延缓。
美国专利No.6,737,120 B1涉及在各种应用中使用的碳纤维或C-C复合材料。该专利教授了通过把这些复合材料涂覆流态化的玻璃类型的混合物保护复合材料免受氧化的方法。流态化的玻璃混合物保持为液体前体,并且施加到由碳纤维或C-C复合材料形成的部件。一旦涂覆前体,涂覆的C-C部件通过一系列的逐渐加热和冷却步骤热处理或退火一个或更多个循环。这产生了具有约1-10密耳厚度的玻璃涂层。该玻璃涂层的厚度可以通过改变流态化的玻璃前体混合物的组成,应用循环的数量,和/或退火参数而改变。
US 6,737,120教导了可以包括诸如硼酸盐玻璃(硼氧化物)、磷酸盐玻璃(磷氧化物)、硅酸盐玻璃(硅氧化物)及高铅酸盐玻璃(铅氧化物)之类的材料的流态化的玻璃材料。这些玻璃可以含锰,镍,钒,铝和锌的磷酸盐,和/或碱金属和碱土金属诸如锂,钠,钾,铷,镁,和钙之类,及它们的氧化物,及元素硼和/或诸如BN,B4C,B2O3,和H3BO3之类的硼化合物。作为例子,US 6,737,120披露了含硼的液体流态化的玻璃前体混合物,其含29wt%的磷酸,2wt%的磷酸锰,3wt%的氢氧化钾,1wt%的氮化硼,10wt%的硼和55wt%的水。
美国专利No.6,455,159 B1同样涉及碳-碳复合材料和石墨材料。US 6,455,159把在高达并且超过850℃的升高的温度下的碳/碳复合材料或石墨的保护和在正常运转温度下的催化氧化的减少作为目标。US6,455,159通过采用渗透剂盐(penetrant salt)溶液达到这些目标,该盐溶液含由10-80wt%的H2O,20-70wt%的H3PO4,0.1-25wt%的碱金属单,双,或三碱式磷酸盐,及高达2wt%的B2O3形成的离子。它们的渗透剂盐溶液还含MnHPO4·1.6H2O,AlPO4,及Zn3(PO4)2中的至少一种,重量百分数分别高达25wt%,30wt%,及10wt%。
2002年8月20日提交(H0003342)的申请系列No.10/223,946,批露了当制品遭受800℃或更高的温度时,受到保护免于催化氧化的涂覆制品。该制品包括由在1600-2600℃退火的碳纤维或碳-碳复合材料制成的部件。该部件被含磷的内涂层覆盖,该内涂层含由10-80wt%的H2O,20-70wt%的H3PO4,0.1-25wt%的碱金属单,双,或三碱式磷酸盐,及0-2wt%的B2O3,0-25wt%的MnHPO4·1.6H2O,0-30wt%的AlPO4,及0-10wt%的Zn3(PO4)2形成的离子,假如AlPO4,MnHPO4·1.6H2O和Zn3(PO4)2中的至少一种存在的话。内涂层被含硼的玻璃外涂层覆盖。SN10/223,946的涂层***同时提供在高温下和催化氧化条件下的高水平的氧化保护。然而,这些涂层***在长期潮湿暴露后在外观上变得有些“浑浊”。这使得它们对于现场使用是不令人满意的。
硅酸盐粘结剂组合物已经长期众所周知。例如参看US 4,504,314;4,391,642;4,329,177及2,995,453。然而,以前硅酸盐粘结剂并未使用在本发明使用它们的环境中。
上面描述的涂层***向碳复合材料提供显著的抗氧化保护。然而,依然存在对提供改进的潮湿抵抗力的抗氧化涂层***的需要。
发明内容
本发明提供包括碳-碳复合材料部件,石墨部件,或基于碳纤维和/或石墨的陶瓷基体复合材料部件的涂覆制品。在优选的实施方案中,该部件为航空器着陆***刹车盘。根据本发明,该部件被内涂层覆盖,内涂层又被外涂层覆盖。
本发明的一个实施方案为涂覆制品。该涂覆制品的开始点可以为碳-碳复合材料部件,石墨部件,或基于碳纤维和/或石墨的陶瓷基体复合材料部件。在该实施方案优选的方面中,部件配置为航空器着陆***刹车盘。该部件被含磷的具有约1-10密耳厚度的内涂层覆盖。
本发明的内涂层为含磷的抗氧化涂层。该内涂层可以由渗透剂溶液制成,该渗透剂溶液含5-80wt%的H2O,10-70wt%的H3PO4,高达25wt%的碱金属单,双,或三碱式磷酸盐,高达2wt%的B2O3,及高达25wt%的MnHPO4·1.6H2O,高达80wt%的AlPO4,及高达10wt%的Zn3(PO4)2,假如AlPO4,MnHPO4·1.6H2O和Zn3(PO4)2中的至少一种存在的话。
根据本发明,内涂覆部件被含硼的具有约1-10密耳厚度的玻璃外涂层覆盖。
本发明的外涂层,基于固相,含,20-50wt%(优选地为35-50%)的碱金属或碱土金属硅酸盐,3-25wt%(优选地为4-20wt%)的碱金属氢氧化物,高达10wt%(优选地为1-6wt%)的氮化硼,及5-40wt%的元素硼和5-40wt%的碳化硼(优选地为25-40wt%的元素硼)中的一种或两者。根据本发明,这样的含硼的玻璃外涂层基本上没有磷酸和磷酸盐。
在本发明的制品方面的优选的特别实施方案中,含硼的玻璃外涂层含40wt%的碱金属硅酸盐,19wt%的碱金属氢氧化物,3wt%的氮化硼,及38wt%的元素硼。
本发明的另一个实施方案为改进涂覆制品内潮湿抵抗力的方法。该涂覆制品可以包括碳-碳复合材料部件、石墨部件、或基于碳纤维和/或石墨的陶瓷基体复合材料部件,并且最优选地为航空器着陆***刹车盘。该方法包括使用含磷的具有约1-10密耳厚度的内涂层覆盖部件,该内涂层含5-80wt%的H2O,10-70wt%的H3PO4,高达25wt%的碱金属单,双,或三碱式磷酸盐,高达2wt%的B2O3,及高达25wt%的MnHPO4·1.6H2O,高达80wt%的AlPO4,及高达10wt%的Zn3(PO4)2,假如AlPO4,MnHPO4·1.6H2O和Zn3(PO4)2中的至少一种存在的话,随后使用含硼的具有约1-10密耳厚度的玻璃外涂层覆盖因此产生的内涂覆部件,所述外涂层含20-50wt%的碱金属或碱土金属硅酸盐,3-25wt%的碱金属氢氧化物,高达10wt%的氮化硼,及5-40wt%的元素硼和5-40wt%的碳化硼中的一种或两者,应理解含硼的玻璃外涂层基本上没有磷酸和磷酸盐。在该方法中,内涂层可以在250-900℃的温度下退火成碳复合材料,并且玻璃外涂层可以在环境温度下干燥至少一小时到内涂层上。
附图说明
图1为具有根据本发明形成的涂层***的碳纤维或C-C基底的示意图。
具体实施方式
本发明通过涂覆两层抗氧化***的碳纤维或C-C复合材料部件具体化。为了更好地理解本发明,关注图1,其中涂覆碳纤维或C-C制品部件总地在19说明。部件10被保护性内涂层11(含磷的玻璃)覆盖,并且内涂层11被保护性外涂层12(含硼、硅酸盐及氢氧化物的玻璃)覆盖。
部件10
在第一个流态化的玻璃配方施加到C-C复合材料部件之前,该部件可以制造为几乎任何需要的形状。当C-C复合材料部件为航空器着陆***刹车盘时,本发明尤其有价值。
碳-碳复合材料通常由碳预成型坯制备。碳预成型坯由碳纤维制成,碳纤维例如由预氧化的聚丙烯腈(PAN)形成。这些纤维可以一起成层,以形成诸如摩擦刹车盘的形状,该形状随后加热并渗透甲烷或另一种可热解的碳源以形成C-C复合材料预成型坯。根据本发明的有用的碳-碳复合材料典型地具有从约1.6g/cm3到2.0g/cm3范围的密度。制造C-C复合材料的方法对于本领域内的普通技术人员通常是所熟知的。在该领域内好的参考为:Buckley等人,碳-碳材料和复合材料,Noyes出版,1993。该出版的完整的内容通过参考因此特意引入。
仅仅为了说明的目的,C-C复合材料部件10可以由沥青基AmocoP30X碳纤维束的编织纤维方格以综缎编织制造,或由沥青基的NipponXNC25以平纹编织制造。纤维束通过诸如酚醛环氧树脂之类的含一些wt%的碳的树脂刚性化。该材料随后在800-1000℃的范围内的温度下碳化,并通过碳CVD致密。因此产生的材料随后在在1600-2600℃的范围内的温度下在惰性气体内退火。该方法产生C-C复合材料部件,当该部件适当地被保护免于氧化时,其适于在高温环境中使用。应理解本发明的氧化保护性涂层***可应用于C-C复合材料部件,不管C-C复合材料部件如何制造。
内涂层11
C-C部件10全部浸入或部分浸入液体渗透剂溶液中几分钟。根据本发明,在应用内涂层中使用的优选的前体为磷酸基的渗透剂盐溶液,其在美国专利No.6,455,159中详细地描述,该专利的完整的披露通过参考因此特意引入。此处可以用来形成内涂层的典型的渗透剂盐溶液可以含5-80wt%的H2O,10-70wt%的H3PO4,高达25wt%的碱金属单,双,或三碱式磷酸盐,及高达2wt%的B2O3。典型的渗透剂盐溶液还含MnHPO4·1.6H2O,AlPO4和Zn3(PO4)2中的至少一种,其重量百分数分别高达25wt%,30wt%,及10wt%。
根据本发明,碳-碳复合材料或石墨材料的表面通过涂抹,浸入,或其他传统施加技术使用渗透剂溶液处理。接着,表面处理的材料在250-900℃的范围内的温度下硬化。典型地,表面使用一层至三层渗透剂溶液处理,并且峰值温度通常保持一至六小时。
外涂层12
载有内涂层11的复合材料部件10浸入或浸泡在流态化的玻璃前体中以使用外涂层12覆盖内涂覆的部件。根据本发明,外涂层12含20-50wt%的碱金属或碱土金属硅酸盐,3-20wt%的碱金属氢氧化物,高达10wt%的氮化硼,及5-40wt%的元素硼和5-40wt%的碳化硼的一种或两者。另外,在本发明中,玻璃外涂层12基本上没有磷酸和磷酸盐。在上下文中术语“基本上没有”意味着外涂层的抗氧化效果不会依赖于组成中磷酸或磷酸盐的存在。
C-C部件10和它的固体玻璃内涂层11全部浸入或部分浸入含硼的流态化的玻璃液体溶池前体中几分钟。液体前体维持在约20-90℃范围内的温度。部件10可以相对液体前体旋转以改进涂层的润湿特性和均匀性。
流态化的含硼-硅酸盐-氢氧化物的玻璃转化为固体玻璃涂层12,涂层12完全覆盖并形成固体玻璃涂层11,其为抵抗C-C部件10不希望的氧化的保护屏障。换句话说,在这个阶段,复合材料部件10永久地涂覆有流态化的玻璃保护性涂层***(11,12)。涂层***(11,12)包括玻璃材料,该玻璃材料能够至少部分流动,使得在C-C部件内可能存在的任何先前发生的裂缝至少部分密封。
可变性
玻璃材料11和12的性能可以根据如下的温度范围和/或氧化催化剂而定制,在该温度范围和/或氧化催化剂的作用下,涂层***(11,12)被设计为保护复合材料部件10免受破坏氧化。同样,施加到部件10的玻璃涂层的厚度和数量将依赖于施加涂层的方法和涂覆的制品19的所计划的使用。如果涂覆制品遭受持续或反复的高温,可以应用许多分开的底层来组成内涂层11和/或外涂层12。这样的抗氧化涂层***可以用在大量碳纤维或碳-碳复合材料制品上,包括但不限于航空器着陆***刹车盘。
潮湿抵抗力
本发明提供具有增强的湿气抵抗力的碳-碳刹车材料和相似的材料,增强的湿气抵抗力归因于硼基外涂层内的含硅酸盐的粘结剂的使用。
制备具有下面成分(重量为克)的外涂层配方。在下面所有的情况下,采用的粘结剂为Cerama-Bind 830粘结剂溶液,并且KOH指的是氢氧化钾。Cerama-Bind 830是可以从Aremco Product,Inc.of ValleyCottage,New York得到的硅酸盐粘结剂溶液。Cerama-Bind 830具有11.4的pH值和25wt%的固体含量。
成分 | #1<sup>*</sup> | #2<sup>*</sup> | #3<sup>*</sup> | #4 |
硼 | 10 | 10 | 10 | 10 |
氮化硼 | ||||
粘结剂 | 40 | 40 | 40 | 40 |
KOH | 0.1 | 1 | 5 | |
蒸馏水 |
成分 | #5 | #6<sup>*</sup> | #7<sup>*</sup> | #8<sup>*</sup> |
硼 | 10 | 10 | 10 | 10 |
氮化硼 | 0.92 | 0.92 | 0.92 | |
粘结剂 | 40 | 40 | 40 | 40 |
KOH | 10 | 0.1 | 1 | |
蒸馏水 |
成分 | #9 | #10 | #11<sup>*</sup> | #12 |
硼 | 10 | 10 | 10 | 10 |
氮化硼 | 0.92 | 0.92 | ||
粘结剂 | 40 | 40 | 40 | 40 |
KOH | 5 | 10 | 1.5 | 2 |
蒸馏水 |
成分 | #13 | #14 | #15<sup>*</sup> | #16 |
硼 | 10 | 10 | 10 | 10 |
氮化硼 | 0.92 | 0.92 | ||
粘结剂 | 40 | 40 | 40 | 40 |
KOH | 3 | 4 | 1.5 | 2 |
蒸馏水 |
成分 | #17 | #18 | #9A<sup>*</sup> | #21 |
硼 | 10 | 10 | 10 | 10 |
氮化硼 | 0.92 | 0.92 | 0.92 | 0.92 |
粘结剂 | 40 | 40 | 25 | 40 |
KOH | 3 | 4 | 4 | |
蒸馏水 | 10 | 10 |
所有含低于3wt%的氢氧化钾的这些配方不构成本发明的一部分。此处为了比较的目的包括这些配方。
上面的配方的每个作为外涂层施加到碳-碳复合材料上,复合材料预先已经被磷基的抗氧化内涂层涂覆。
上面的配方的每个,如所指示涂覆在C-C复合材料上,在可见性测试中测试。可见性测试研究抗氧化外涂层抵抗“泥裂”结果的能力,在硬化或干燥过程期间观察到一些配方的结果。“好”等级指示当样本在光学显微镜下检查时没有观察到泥裂。“坏”等级指示当样本在光学显微镜下检查时观察到泥裂。
#1<sup>*</sup> | #2<sup>*</sup> | #3<sup>*</sup> | #4 | |
可见性评级 | 坏 | 坏 | 坏 | 好 |
#5 | #6<sup>*</sup> | #7<sup>*</sup> | #8<sup>*</sup> | |
可见性评级 | 好 | 坏 | 坏 | 坏 |
#9 | #10 | #11<sup>*</sup> | #12 | |
可见性评级 | 好 | 好 | 坏 | 坏 |
#13 | #14 | #15<sup>*</sup> | #16 | |
可见性评级 | 坏 | 好 | 好 | 坏 |
#17 | #18 | #9A<sup>*</sup> | #21 | |
可见性评级 | 好 | 好 | 坏 | 好 |
在上面的报告中可以看到,本发明新颖的配方通常提供“好”的结果,而对比配方通常提供“坏”的结果。尽管在“泥裂”测试中本发明的一些组合物(#12,#13)不提供最优的可见性结果,这可以从下面展示的数据看出,但它们在氧化和潮湿抵抗力方面的性能依然很好。
上面配方中的一些,如上面所指示的涂覆在C-C复合材料上,在潮湿抵抗力测试中进行测试。潮湿抵抗力测试研究当涂覆有抗氧化外涂层的表面受到指状物或织物重击时,抗氧化外涂层抵抗变脏的能力。测试在已经在潮湿箱内(95%湿度,84℉)保持10天的涂覆的碳-碳复合材料片段上进行。下面的评级***用于评估外涂层配方对潮湿的抵抗力:
●“1”=差的抵抗力;当受到指状物或织物重击时变脏;
●“2”=好的抵抗力;重击后在指状物或织物上观察到很少的材料;
●“3”=极好的抵抗力;没有变脏。
#1<sup>*</sup> | #2<sup>*</sup> | #3<sup>*</sup> | #4 | |
潮湿评级 | 没有测试 | 没有测试 | 没有测试 | 2 |
#5 | #6<sup>*</sup> | #7<sup>*</sup> | #8<sup>*</sup> | |
潮湿评级 | 1 | 没有测试 | 没有测试 | 没有测试 |
#9 | #10 | #11<sup>*</sup> | #12 | |
潮湿评级 | 2 | 1 | 1 | 3 |
#13 | #14 | #15<sup>*</sup> | #16 | |
潮湿评级 | 3 | 2 | 1 | 2 |
#17 | #18 | #9A<sup>*</sup> | #21 | |
潮湿评级 | 3 | 3 | 1 | 2 |
在上面的报告中可以看到,本发明新颖的配方通常提供好的或极好的结果,而对比配方通常提供坏的结果。
氧化重量损失
本发明的配方#17或#18作为外涂层使用在具有磷基的抗氧化内涂层的碳-碳复合材料上。在这些例子中使用的内涂层,下面称作P13K(-50)和P39,为含磷酸和磷酸盐的抗氧化组合物。P13K(-50)为51.27wt%的磷酸(85%的水溶液),14.17wt%的一元磷酸铝(50%的水溶液),12.41wt%的蒸馏水,3.56wt%的磷酸锌,2.96wt%的磷酸锰,1.63wt%的硼酸,及12.23wt%的磷酸二氢钾。P39为11.08wt%的磷酸(85%水溶液),66.76%一元磷酸铝(50%的水溶液),8.08wt%的蒸馏水,2.58wt%的磷酸锰,0.8wt%的硼酸酐,及10.7wt%的磷酸二氢钾。通过在1600℉,在每小时3立方英尺的速率的气流中加热6小时的时段,测试外涂覆的C-C复合材料氧化重量损失,获得下面的结果。
内涂层/外涂层 | 制造的重量(克) | 氧化后的重量(克) | 重量损失(百分数) | |
1 | P13K(-50)/#17 | 20.8836 | 26.7704 | 0.54 |
2 | P13K(-50)/#17 | 20.8139 | 20.8183 | (0.02) |
3 | P13K(-50)/#17 | 20.9163 | 20.8581 | 0.23 |
4 | P13K(-50)/#17 | 20.6344 | 20.6384 | (0.02) |
5 | P13K(-50)/#17 | 20.6322 | 20.6519 | (0.10) |
6 | P13K(-50)/#17 | 20.7957 | 20.7721 | 0.11 |
7 | P13K(-50)/#17 | 20.7137 | 20.7391 | (0.12) |
8 | P13K(-50)/#17 | 20.8348 | 20.8778 | (0.21) |
9 | P13K(-50)/#17 | 20.7272 | 20.7354 | (0.04) |
10 | P13K(-50)/#17 | 20.9431 | 20.9645 | (0.10) |
平均 | 20.7895 | 20.7836 | 0.03 |
内涂层/外涂层 | 制造的重量(克) | 氧化后的重量(克) | 重量损失(百分数) | |
1 | P13K(-50)/#18 | 20.6496 | 20.6600 | (0.05) |
2 | P13K(-50)/#18 | 20.7909 | 20.7837 | 0.04 |
3 | P13K(-50)/#18 | 20.8758 | 20.7591 | 0.56 |
4 | P13K(-50)/#18 | 20.6188 | 20.4855 | 0.65 |
5 | P13K(-50)/#18 | 20.7341 | 20.6790 | 0.27 |
6 | P13K(-50)/#18 | 20.9985 | 20.9561 | 0.15 |
7 | P13K(-50)/#18 | 21.1190 | 20.1359 | (0.08) |
8 | P13K(-50)/#18 | 20.9577 | 20.9162 | 0.20 |
9 | P13K(-50)/#18 | 20.9008 | 20.8573 | 0.21 |
10 | P13K(-50)/#18 | 20.8276 | 20.7877 | 0.19 |
平均 | 20.8473 | 20.8030 | 0.21 |
内涂层/外涂层 | 制造的重量(克) | 氧化后的重量(克) | 重量损失(百分数) | |
1 | P39/#17 | 20.4855 | 20.5097 | (0.12) |
2 | P39/#17 | 20.7300 | 20.7624 | (0.16) |
3 | P39/#17 | 20.4841 | 20.5239 | (0.19) |
4 | P39/#17 | 20.7053 | 20.7072 | (0.01) |
5 | P39/#17 | 20.5505 | 20.3700 | 0.88 |
6 | P39/#17 | 20.6222 | 20.6225 | 0.00 |
7 | P39/#17 | 20.4038 | 20.4353 | (0.15) |
8 | P39/#17 | 20.5815 | 20.6121 | (0.15) |
9 | P39/#17 | 20.9072 | 20.9412 | (0.16) |
10 | P39/#17 | 20.6681 | 20.6855 | (0.08) |
平均 | 20.6138 | 20.6170 | (0.02) |
内涂层/外涂层 | 制造的重量(克) | 氧化后的重量(克) | 重量损失(百分数) | |
1 | P39/#18 | 20.1782 | 20.2095 | (0.16) |
2 | P39/#18 | 19.9074 | 19.9499 | (0.21) |
3 | P39/#.18 | 20.5795 | 20.6127 | (0.16) |
4 | P39/#18 | 20.7570 | 20.7383 | 0.09 |
5 | P39/#18 | 20.5825 | 20.5433 | 0.19 |
6 | P39/#18 | 20.3384 | 20.3767 | (0.19) |
7 | P39/#18 | 21.7465 | 20.7617 | (0.07) |
8 | P39/#18 | 20.8360 | 20.8698 | (0.16) |
9 | P39/#18 | 20.5003 | 20.5141 | (0.07) |
10 | P39/#18 | 20.5862 | 20.6089 | (0.11) |
平均 | 20.5012 | 20.5185 | (0.09) |
应注意上文所报导的许多“重量损失”数字为负数。在这些情况下,涂覆的C-C复合材料事实上在氧化测试期间增加重量。
在下面的条件下,使用P13K(-50)内涂层和配方#6外涂层进行催化氧化抵抗力测试。涂覆的样本在醋酸钾溶液中浸泡30分钟,随后在80℃干燥最少8小时。它们随后在1200℉在3 SCFH的气流速率下氧化24小时。获得了下面的结果:
内涂层/外涂层 | 制造的重量(克) | 氧化后的重量(克) | 重量损失(百分数) | |
1 | P13K(-50)/#6 | 20.7734 | 20.5908 | 0.88 |
2 | P13K(-50)/#6 | 20.7286 | 20.4931 | 1.14 |
3 | P13K(-50)/#6 | 20.7386 | 20.6312 | 0.49 |
4 | P13K(-50)/#6 | 20.6880 | 21.5420 | 0.71 |
5 | P13K(-50)/#6 | 21.2424 | 21.2164 | 0.12 |
6 | P13K(-50)/#6 | 21.0690 | 21.0095 | 0.28 |
7 | P13K(-50)/#6 | 20.7900 | 20.7256 | 0.31 |
8 | P13K(-50)/#6 | 21.1210 | 21.0918 | 0.14 |
9 | P13K(-50)/#6 | 20.9741 | 20.9204 | 0.26 |
10 | P13K(-50)/#6 | 21.0940 | 20.8233 | 1.28 |
平均 | 20.9213 | 20.8044 | 0.56 |
上面的结果提供了使用本发明的涂层配方在氧化时不造成过多的重量损失的证明(并且在一些情况下,涂覆本发明配方的复合材料事实上在氧化时增加重量)。
Claims (14)
1.一种涂覆制品(19),包括碳-碳复合材料部件(10)、石墨部件(10)或基于碳纤维和/或石墨的陶瓷基体复合材料部件(10),所述部件被具有1-10密耳厚度的含磷抗氧化内涂层(11)覆盖,所述内涂层被含硼的具有1-10密耳厚度的玻璃外涂层(12)覆盖,所述外涂层含20-50wt%的碱金属或碱土金属硅酸盐,3-25wt%的碱金属氢氧化物,不超过10wt%的氮化硼,及5-40wt%的元素硼和5-40wt%的碳化硼中的一种或两者,所述含硼的玻璃外涂层基本上不含磷酸和磷酸盐。
2.根据权利要求1所述的制品,其配置为航空器着陆***刹车盘。
3.根据权利要求1所述的制品,其中所述含硼的玻璃外涂层(12)含:35-50wt%的碱金属硅酸盐;4-20wt%的碱金属氢氧化物;1-6wt%的氮化硼,及25-40wt%的元素硼。
4.根据权利要求3所述的制品,其中所述含硼的玻璃外涂层(12)含40wt%的碱金属硅酸盐。
5.根据权利要求3所述的制品,其中所述含硼的玻璃外涂层(12)含19wt%的碱金属氢氧化物。
6.根据权利要求3所述的制品,其中所述含硼的玻璃外涂层(12)含3wt%的氮化硼。
7.根据权利要求3所述的制品,其中所述含硼的玻璃外涂层(12)含38wt%的元素硼。
8.根据权利要求1所述的制品,其中所述含磷的抗氧化内涂层(11)由渗透剂盐溶液形成,该渗透剂盐溶液含5-80wt%的H2O,10-70wt%的H3PO4,高达25wt%的碱金属单,双或三碱式磷酸盐,高达2wt%的B2O3,及MnHPO4·1.6H2O,AlPO4和Zn3(PO4)2中的至少一种,其重量百分数分别高达25wt%,30wt%及10wt%。
9.根据权利要求1所述的制品,其中内涂层(11)在250-900℃的温度范围内退火成碳复合材料(10),并且外涂层(12)在环境温度下在内涂层(11)上被干燥至少一小时。
10.改进涂覆制品(19)内潮湿抵抗力的方法,该涂覆制品(19)包括碳-碳复合材料部件(10)、石墨部件(10)或基于碳纤维和/或石墨的陶瓷基体复合材料部件(10),所述方法包括以下步骤:
(a)提供碳-碳复合材料部件(10)、石墨部件(10)或基于碳纤维和/或石墨的陶瓷基体复合材料部件(10);
(b)使用含磷的具有1-10密耳厚度的抗氧化内涂层(11)覆盖所述部件(10);及
(c)使用含硼的具有1-10密耳厚度的玻璃外涂层(12)覆盖所产生的内涂覆的部件,所述外涂层含20-50wt%的碱金属或碱土金属硅酸盐,3-25wt%的碱金属氢氧化物,高达10wt%的氮化硼,及5-40wt%的元素硼和5-40wt%的碳化硼中的一种或两者,所述含硼的玻璃外涂层基本上不含磷酸和磷酸盐。
11.根据权利要求10所述的方法,其中所述部件(10)配置为航空器着陆***刹车盘。
12.根据权利要求10所述的方法,其中所述含磷的抗氧化内涂层(11)由渗透剂盐溶液形成,该渗透剂盐溶液含5-80wt%的H2O,10-70wt%的H3PO4,高达25wt%的碱金属单,双或三碱式磷酸盐,高达2wt%的B2O3,及MnHPO4·1.6H2O,AlPO4和Zn3(PO4)2中的至少一种,其重量百分数分别高达25wt%,30wt%及10wt%。
13.根据权利要求10所述的方法,其中在步骤(b)中,内涂层(11)在250-900℃的温度范围内退火成碳复合材料(10)。
14.根据权利要求10所述的方法,其中在步骤(c)中,外涂层(12)在环境温度下在内涂层(11)上被干燥至少一小时上。
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US6884467B2 (en) * | 2002-08-20 | 2005-04-26 | Honeywell International Inc. | Method for simultaneously protecting carbon-containing components against catalytic oxidation and high temperature non-catalytic oxidation |
US7241476B2 (en) * | 2004-09-16 | 2007-07-10 | Honeywell International Inc. | Airflow masking of carbon-carbon composites for application of antioxidants |
US20070262200A1 (en) * | 2006-05-15 | 2007-11-15 | Honeywell International Inc. | Extra long life carbon-carbon friction material |
EP1889822A3 (en) * | 2006-08-18 | 2009-03-04 | Honeywell International Inc. | Two piece carbon-carbon pressure plate design for aircraft brakes |
US20080220256A1 (en) * | 2007-03-09 | 2008-09-11 | Ues, Inc. | Methods of coating carbon/carbon composite structures |
US8003026B2 (en) | 2008-05-28 | 2011-08-23 | Honeywell International Inc. | Pitch-only densification of carbon-carbon composite materials |
CN101328077B (zh) * | 2008-07-17 | 2011-11-09 | 居小平 | 碳/碳复合材料航空刹车件的氧化防护空气阻断层涂料 |
US8801981B2 (en) * | 2008-11-25 | 2014-08-12 | Honeywell International Inc. | Preventing carbon AO migration by limiting surface porosity |
FR2944010B1 (fr) * | 2009-04-02 | 2012-07-06 | Snecma Propulsion Solide | Procede pour le lissage de la surface d'une piece en materiau cmc |
US8383197B2 (en) * | 2009-05-28 | 2013-02-26 | Honeywell International Inc. | Titanium carbide or tungsten carbide with combustion synthesis to block porosity in C-C brake discs for antioxidation protection |
US20110033623A1 (en) * | 2009-08-05 | 2011-02-10 | Honeywell International Inc. | Method of preventing carbon friction material anti oxidation system migration by utilizing carbon vapor deposition |
JP5528227B2 (ja) * | 2009-10-16 | 2014-06-25 | 曙ブレーキ工業株式会社 | 固体潤滑材、その製造方法および用途 |
US9085991B2 (en) * | 2009-11-06 | 2015-07-21 | Honeywell International Inc. | Protective coatings for ceramic matrix composite substrates and methods for improving the wear resistance thereof and coated articles produced therefrom |
FR2983192B1 (fr) * | 2011-11-25 | 2014-05-23 | Commissariat Energie Atomique | Procede pour revetir une piece d'un revetement de protection contre l'oxydation par une technique de depot chimique en phase vapeur, et revetement et piece |
CN103032499B (zh) * | 2012-12-19 | 2015-03-04 | 重庆红宇摩擦制品有限公司 | 六方晶系氮化硼汽车制动器摩擦片及其制备方法 |
US9409823B2 (en) | 2013-02-15 | 2016-08-09 | Deborah D. L. Chung | Microstructured high-temperature hybrid material, its composite material and method of making |
CN105090038A (zh) * | 2015-08-20 | 2015-11-25 | 无锡中强电碳有限公司 | 一种汽车用刹车泵旋片 |
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