CN1077444A - 涂层陶瓷制品 - Google Patents
涂层陶瓷制品 Download PDFInfo
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Abstract
一种用于高温和腐蚀环境中的陶瓷制品,包括一
种陶瓷基体,在该基体上沉积了一层基本上无孔的一
种或多种贵金属或其合金的涂层。
Description
本发明涉及涂层耐火陶瓷制品。
在许多工业以及各种应用领域中,通常是在高温和腐蚀的环境中使用耐火陶瓷,如在玻璃原料,产品和组分的制备中使用的陶瓷热电偶保护套管,鼓泡管,出料口,搅拌器和其它工艺设备。
例如,热的熔融玻璃的温度是通过保护在保护套管中的热电偶测定的。温度的这种测定存在着许多问题,它们包括熔融玻璃的高粘度和磨损,玻璃的化学反应性和加热时的燃烧气氛。保护套管的作用是防止热电偶在这样的环境下受到机械的和化学的损坏。保护套管一般为氧化铝的。但是,这类保护套管在高温下比较易脆。另外,它们受到熔融玻璃的严重侵蚀,造成迅速的破裂,同时完全失去了对热电偶的保护。
至于氧化锆颗粒稳定的ZGS类合金,铂族金属(PGM)和铂族金属合金已经被用作为替代的保护材料。这些套管的最大完整结构要求金属厚度为0.5~0.8mm,这样,套管的花费是很昂贵的。陶瓷管的内部支承使该厚度降低到约0.3mm的目前使用水平。但是需要考虑到套的机械设计配合,实质上,其费用仍然是很高的。
用铂族金属涂层或包层金属基体制造的装置能起到保护作用并延长其使用寿命,但使用温度受到基体熔点的限制。例如,使用Ni合金基体时,其工作温度应限定在1300℃以下,大多数情况下,限定在1200℃以下。使用耐火合金可以将工作温度提高到1600℃,但是为此所付出的代价是必须保护所有的表面,该表面可能比可见温度高400~600℃。陶瓷基体提供了一个特别是在高温下使用的替代载体。
铂族金属包层陶瓷已经满足这种温度场合。可是,金属包层和陶瓷之间存在的空气间隙降低了密封式热电偶对温度变化的响应,所形成的套的耐热和机械冲击性差。包层陶瓷为两片结构,其部件具有金属用于包层,陶瓷用于基体的特征。
传统上,直接用铂族金属涂层陶瓷,不能经济的生产适于在高温下和腐蚀环境下使用的具有耐久性的制品。传统的涂层工艺在喷涂时产生应力,由于特殊的使用方式一般限制了涂层厚度。这样的厚度通常不足以达到所需的保护。当涂层工艺能够形成满意厚度的涂层时,其它问题就暴露出来,如附着力,和/或机械强度,和/或完整性,和/或气孔率。
GB1242996(康宁玻璃)公开了一种用等离子喷涂在陶瓷上形成铂涂层的方法。据说火焰喷涂法不能形成附着的、无孔的涂层。我们从末注意到按照GB1242996的工艺或其它工艺制备的涂层陶瓷成功地商业化。
本发明的目的是提供一种陶瓷制品,该制品适用于任何高温和/或腐蚀环境的领域,本发明的制品至少克服了现有技术中的一些问题。
因此,本发明提供了一种在高温下和腐蚀环境中使用的陶瓷制品,该制品包括耐火陶瓷基体,在该基体上沉积了一种或多种贵金属或其合金的涂层,所说涂层的厚度为50~350微米,并且基本上是无孔的。
本发明进一步提供了在高温下和腐蚀环境中使用的陶瓷制品的制造方法,该方法包括采用火焰喷涂法将一种或多种贵金属或其合金涂层到耐火陶瓷基体上,其涂层厚度为50~350微米,制造基本上是无气孔的涂层。
基体可以是任何合适的氧化物或非氧化物技术或耐火陶瓷材料,如氧化铝,硅酸铝,锆莫来石,氧化锆,莫来石,二氧化硅,氧化钛。基体优选的为氧化铝或氧化锆基材料,或莫来石基材料。更重要的是,为了避免制品在使用中产生不希望的应力,陶瓷和涂层系统的热膨胀系数应该是匹配的。
实质上无孔的涂层选自一种或多种贵金属。优选的涂层为铂或铂合金,如含5%金的铂合金、含10%铱的铂合金,含5%钌的铂合金,含10%铑的铂合金,或含1%以下锆的铂合金。使用的合金的,百分数可低可高,也包括传统上难以制造成适用于包层形式的组份。其它可使用的铂族金属为钯和钯合金。
涂层是通过火焰喷涂沉积的,例如,用高速氧化燃料气体喷涂。在一个优选的火焰喷涂工艺中,贵金属源为丝状的,而不是其它技术中所需的粉未状。合适的设备可从市场上获得。涂层的外表面在沉积后经处理如喷射硬化火焰抛光或机械打磨,基本上是无孔的。涂层厚度一般为50~350μm,如100~350μm,优选的至少为125μm。
本发明的制品得益于特征范围。它具有良好的防止氧化剂扩散到由高纵横尺寸比微结构涂层保护的基体上的倾向,所需要的贵金属比现有技术的制品少许多。陶瓷基体和金属涂层之间的紧密接触消除了由于考虑到空气间隙而对热电偶的任何限制。高质量的结构和其固有的热和电特性使得铂族金属和合金涂层起着热电偶的电磁保护的作用,因而减少了噪音水平,改善了它们的信号质量。由声音界面特性的产生所获得的复合构件与基体表面状态有关,小心地控制涂层沉积参数,使得金属沉积到陶瓷上形成金属涂层,反之易然,其结果是构件材料比现有技术的包层陶瓷好。这就允许使用先前热应力和机械应力太大的部件。声音界面的获得是由基体的前期准备,化学、机械或热处理造成的。这类处理可包括机加工,喷砂,脱脂,或酸侵蚀。
用于该用途的方法具有较低的应力积聚,必要时该应力可被积聚到构件厚度上。不易于包层的形状复杂的构件可以被保护。在部件的不同区域上,实质上可改变涂层的厚度以确保得到保护的标准水准。另外,一旦获得标准的界面特性,相同的或不同的PGMS和合金的进一步沉积在局部区域可减少。
在本发明的涂层中,可以使用氧化物或惰性颗粒牵制颗粒界面。长时间处于高温下的铂族金属合金,特别是纯金属能呈现出大范围的结构变化和颗粒生长。这些特征致使使用时毁坏。牵制颗粒界面能抵消或抑制这类微结构变化。惰性颗粒,如ZGS合金中的氧化锆,可以直接包括在沉积涂层中,或经后沉积处理产生,这取决于组成,尺寸和分布方面的需要而定。习惯上是制备ZGS合金的包层,但是需要将这些包层结合成复杂的形状。在任何情况下这种结合可能是弱的,因此使用涂层技术的一个显著的进步是避免了必须的结合。
必要时可以在基体和贵金属涂层之间增加一个附加涂层,该附加涂层或者为单个组分或者为一种或多种陶瓷和一种或多种贵金属或其合金的混合物。可由热喷涂如火焰或真空或空气等离子喷涂,或一层或多层的沉积形成附加的涂层。可以使多层涂层形成陶瓷与金属比的逐步渐变。通过传统技术可将习惯上制备的PGM产品如片、条,管,丝结合到涂层的部件上。这类技术包括电弧焊接,锻焊,激光或离子束接合,和喷涂接合。这能同时利用两种工艺的最好特征。
本发明将通过实施例得到描述。实施例13描述了涂层制品的工业使用试验。
实施例
实施例1-4
在每种情况下,套管通过火焰喷涂法直接向基体上喷涂一层铂涂层。采用一种工业火焰喷涂装置,用丙烯和氧气形成火焰,压缩空气使铂形成雾化状态。将卷筒中的铂丝送入火焰中。进行喷射硬化后处理,将测试的涂层试样部分浸入标称温度为1350℃的火石玻璃中保持100小时。
试样 涂层 厚度 基体 结果
E1 Pt 100μm 莫来石 在高于玻璃处涂层有针眼
其它良好
E2 Pt 250μm 莫来石 性能良好,涂层起了保护作用
E3 Pt 100μm 抗渗氧化铝瓷 在高于玻璃液面以上涂层有
针眼
E4 Pt 250μm 抗渗氧化铝瓷 性能良好,涂层起了保护作用
实施例5和6
在每种情况下,通过火焰喷涂直接将铂涂层到基体上使套管被涂层。进行喷射硬化后处理。
将直接沉积,涂层的试样部分浸入标称温度为1350℃的琥珀色玻璃中进行测示。
试样 涂层 厚度 基体 测试 结果
E5 Pt 175μm 莫来石 200小时 轻微的颗粒生长涂
层起了保护作用
E6 Pt 400μm 莫来石 400小时 颗粒生长,涂层起
了保护作用并支承
了碎裂的基体
实施例7-9
在每种情况下,一种氧化铝套管,由Morgan Matroc Limited提供的Development试样号MX3是通过火焰喷涂直接将铂涂层到该氧化铝制品上涂层的。进行喷射硬化后处理。将涂层试样部分地浸入标称温度为1250℃的火石玻璃中保持300小时进行测示。
试样 涂层 厚度 结果
E7 Pt 186μm 涂层充分地起到了保护作用
E8 Pt 165μm 涂层充分地起到了保护作用
E9 Pt 178μm 涂层充分地起到了保护作用
实施例10
涂层是直接地火焰喷涂到莫来石套管上的,进行喷射硬化后处理。将试样部分浸入1250℃的琥珀色玻璃中300小时进行试验。
试样 涂层 厚度 结果
E10 10%Ir/Pt 200μm 涂层腿色但起到了保护作用
实施例11
涂层被直接地火焰喷涂到莫来石的套管上。将试样在空气中于1200℃热处理一小时,并进行喷射硬化后处理。在1250℃的琥珀色玻璃中进行试验300小时。
试样 涂层 厚度 结果
E11 Pt-Zr 200μm 基体受到保护
颗粒生长受到限制
实施例12
涂层被直接地火焰喷涂到一种氧化铝瓷套管上,进行喷射硬化后处理。将试样部分浸入标称温度为1430℃的火石玻璃中保持40小时进行试验。
试样 涂层 厚度 结果
E12 Pt 150μm Pt涂层具有保护作用
实施例13
使用试验
情形1
将10%Rh/Pt直接地火焰喷涂到莫来石套管上,并且将其在玻璃液面处局部加厚到250μm,而玻璃液面以下处为200μm,液面以上处为175μm。进行喷射硬化后处理。
将涂层制品在1140~1220℃的工业工作带中的琥珀,火石和绿色玻璃中,以不同的时间进行试验。总的使用寿命超过8个月,而在该阶段涂层制品仍在进行试验中。
情形2
将颗粒稳定铂上的双层铂直接火焰喷涂到莫来石套管上,并进行喷射硬化。涂层厚度为225μm和275μm之间。试验是在制备琥珀玻璃瓶的工作带中进行的,使用寿命为1000小时。然后将试样移出进行检测。基体基本上受到了保护。
情形3
将一种经1400℃热处理约1小时的二氧化硅球直接地火焰喷涂上250μm厚的Pt涂层。对其进行喷射硬化后处理。
将涂层制品在1430℃下试验1.75小时。将温度循环到估计1200℃每分钟循环一次约100次。
涂层性能良好,但由于基体的多处损坏造成破裂。
情形4
将一种经1400℃热处理约1小时的硅酸铝球直接火焰喷涂上标称厚度为250μm的Pt涂层。进行喷射硬化后处理。
将涂层制品在1340℃(最大)下进行试验72小时以上,在最大温度和估计温度1000℃之间每分钟重复循环。
然后将涂层制品冷却到定温并再加热到操作温度。
还在1300℃或700℃下进行若干过夜保温。涂层性能极好,基体基本上受到了保护。
情形5
涂层/包层焊接
在莫来石管上直接火焰喷涂上300μm的Pt涂层。将一个0.5mm厚的Pt管套在该试样上,采用标准的钨惰性焊接(TIG)工艺焊接。结合是完整的。
将该整体在上升到1300℃进一步试验1小时,然后冷却到室温。涂层或结合处没有观察到损坏的迹象。
Claims (9)
1、一种高温下和腐蚀环境中使用的陶瓷制品,包括一种耐火陶瓷基体,在该基体上沉积了一种或多种贵金属或合金基本涂层,所述的涂层的厚度为50~350微米,并且基本上是无孔的。
2、根据权利要求1的一种制品,其中基体包括氧化铝或氧化锆。
3、根据权利要求1的一种制品,其中基体包括莫来石。
4、根据权利要求1,2或3的一种制品,其中涂层包括铂或铂合金。
5、根据权利要求4的一种制品,其中该涂层由铂,5%金的铂合金,5%钌的铂合金,10%铑的铂合金和ZGS铂或铂合金中的至少一种构成。
6、根据上述任一权利要求的一种制品,其中涂层的厚度至少为125μm。
7、根据上述任一权利要求的一种制品,其中将一种包括一种或多种陶瓷和一种或多种贵金属或其合金的混合物的附加涂层沉积在基体和贵金属涂层之间。
8、一种用于高温和腐蚀环境中的陶瓷制品的制造方法,包括向一种耐火陶瓷基体上火焰喷涂上一层一种或多种贵金属或其合金的涂层,涂层的厚度为50~350微米,并且处理涂层使之基本上无孔。
9、根据权利要求8的方法,其中涂层的处理包括喷射硬化,火焰抛光或机械打磨。
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GB9203394.3 | 1992-02-18 | ||
GB929203394A GB9203394D0 (en) | 1992-02-18 | 1992-02-18 | Coated article |
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CN93102943A Pending CN1077444A (zh) | 1992-02-18 | 1993-02-18 | 涂层陶瓷制品 |
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US (1) | US5437933A (zh) |
EP (1) | EP0559330B1 (zh) |
JP (1) | JP3151778B2 (zh) |
KR (1) | KR100237966B1 (zh) |
CN (1) | CN1077444A (zh) |
AT (1) | ATE126550T1 (zh) |
AU (1) | AU659712B2 (zh) |
DE (2) | DE9321489U1 (zh) |
DK (1) | DK0559330T3 (zh) |
ES (1) | ES2075758T3 (zh) |
GB (1) | GB9203394D0 (zh) |
TW (1) | TW313563B (zh) |
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-
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- 1993-02-02 US US08/012,442 patent/US5437933A/en not_active Expired - Fee Related
- 1993-02-04 AT AT93300823T patent/ATE126550T1/de not_active IP Right Cessation
- 1993-02-04 DE DE9321489U patent/DE9321489U1/de not_active Expired - Lifetime
- 1993-02-04 DE DE69300369T patent/DE69300369T2/de not_active Expired - Fee Related
- 1993-02-04 DK DK93300823.7T patent/DK0559330T3/da active
- 1993-02-04 ES ES93300823T patent/ES2075758T3/es not_active Expired - Lifetime
- 1993-02-04 EP EP93300823A patent/EP0559330B1/en not_active Revoked
- 1993-02-08 AU AU32889/93A patent/AU659712B2/en not_active Ceased
- 1993-02-18 KR KR1019930002234A patent/KR100237966B1/ko not_active IP Right Cessation
- 1993-02-18 TW TW082101132A patent/TW313563B/zh active
- 1993-02-18 CN CN93102943A patent/CN1077444A/zh active Pending
- 1993-02-18 JP JP02880093A patent/JP3151778B2/ja not_active Expired - Lifetime
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Also Published As
Publication number | Publication date |
---|---|
DE9321489U1 (de) | 1998-08-13 |
GB9203394D0 (en) | 1992-04-01 |
EP0559330B1 (en) | 1995-08-16 |
KR100237966B1 (ko) | 2000-02-01 |
EP0559330A1 (en) | 1993-09-08 |
KR930017843A (ko) | 1993-09-20 |
DE69300369T2 (de) | 1996-02-29 |
DE69300369D1 (de) | 1995-09-21 |
JPH05339082A (ja) | 1993-12-21 |
US5437933A (en) | 1995-08-01 |
ES2075758T3 (es) | 1995-10-01 |
AU3288993A (en) | 1993-08-19 |
ATE126550T1 (de) | 1995-09-15 |
DK0559330T3 (da) | 1995-10-02 |
JP3151778B2 (ja) | 2001-04-03 |
TW313563B (zh) | 1997-08-21 |
AU659712B2 (en) | 1995-05-25 |
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