CN103861662B - 带有氧化铝阻隔层的防结焦催化剂涂层 - Google Patents
带有氧化铝阻隔层的防结焦催化剂涂层 Download PDFInfo
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- CN103861662B CN103861662B CN201210541299.2A CN201210541299A CN103861662B CN 103861662 B CN103861662 B CN 103861662B CN 201210541299 A CN201210541299 A CN 201210541299A CN 103861662 B CN103861662 B CN 103861662B
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- 239000000243 solution Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
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- 229910052712 strontium Inorganic materials 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- 229910000601 superalloy Inorganic materials 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- 229910052713 technetium Inorganic materials 0.000 description 1
- GKLVYJBZJHMRIY-UHFFFAOYSA-N technetium atom Chemical compound [Tc] GKLVYJBZJHMRIY-UHFFFAOYSA-N 0.000 description 1
- JBQYATWDVHIOAR-UHFFFAOYSA-N tellanylidenegermanium Chemical compound [Te]=[Ge] JBQYATWDVHIOAR-UHFFFAOYSA-N 0.000 description 1
- FRNOGLGSGLTDKL-UHFFFAOYSA-N thulium atom Chemical compound [Tm] FRNOGLGSGLTDKL-UHFFFAOYSA-N 0.000 description 1
- 229940126680 traditional chinese medicines Drugs 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 1
- NAWDYIZEMPQZHO-UHFFFAOYSA-N ytterbium Chemical compound [Yb] NAWDYIZEMPQZHO-UHFFFAOYSA-N 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
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Abstract
本发明涉及一种工件，该工件包括金属基体、防结焦催化剂层、以及设置在金属基体和防结焦催化剂层之间的氧化铝阻挡层。本发明还涉及制造该工件的工艺方法。
Description
技术领域
本发明一般涉及一种适合用于如重质石油的热裂解反应装置的工件，具体地，涉及一种具有用来防止结焦和堵塞的防结焦催化剂涂层和用来防止该催化剂层钝化的氧化铝阻挡层的工件，以及制造该工件的方法。
背景技术
为了防止在重质石油热裂解过程中使用的工件上形成结焦和堵塞，常用各种防结焦催化剂来减少或防止结焦。比如，研究发现钙钛矿催化剂对于消除和（或）减少热裂解如乙烯裂解工艺中所用的锅炉管上的结焦具有很好的效果。防结焦的催化剂一般镀覆在需要接触高温下被处理的重质石油物料的工件内表面上。对于在重质石油热裂解的工艺中所使用的工件，即便是镀覆有防结焦的催化剂，也需要进行常规的（长期的或重复的）除焦处理，以将堆积在工件壁上的焦炭沉淀物除去。一种典型的除焦过程一般涉及在氧化条件下将焦炭沉淀物氧化形成二氧化碳和其他产物。然而，在所述除焦过程中（氧化条件下）的加热条件下，有些防结焦催化剂，如钙钛矿催化剂可能会与工件基体扩散出来的某些元素发生反应，导致催化剂的催化活性下降。比如，在除焦过程中，由含铬材料制成的锅炉管上的钙钛矿催化剂可能会与从该锅炉管扩散出来的铬发生反应，生成没有催化活性的物质。因此，需要提供一种可用于热裂解工艺的工件，其上有防结焦催化剂层，该催化剂层不会被其所覆盖的基体中扩散出来的元素钝化导致失效。
发明内容
本发明的一方面涉及一种工件，该工件包括金属基体、防结焦催化剂层、以及在该金属基体和防结焦催化剂层之间的氧化铝阻挡层。
本发明的另一方面涉及一种工艺，该工艺包括以下步骤：对金属基体进行镀铝；对镀铝后的金属基体进行热处理以形成覆盖所述金属基体的氧化铝阻挡层；以及在所述氧化铝阻挡层上镀覆防结焦催化剂层。
附图说明
通过结合附图对于本发明的实施例进行描述，可以更好地理解本发明，在附图中：
图1为一个工件的示意图，该工件在其金属基体和催化剂镀层之间有氧化铝阻挡层。
具体实施方式
本文中所使用的近似性的语言可用于定量表述，表明在不改变基本功能的情况下可允许数量有一定的变动。因此，用“大约”、“左右”等语言所修正的数值不限于该准确数值本身。在一些实施例中，“大约”或“左右”表示允许其修正的数值在正负百分之十（10%）的范围内变化，比如，“大约100”表示的可以是90到110之间的任何数值。此外，在“大约第一数值到第二数值”的表述中，“大约”同时修正第一数值和第二数值两个数值。在某些情况下，近似性语言可能与测量仪器的精度有关。
本发明中所提及的数值包括从低到高一个单元一个单元增加的所有数值，此处假设任何较低值与较高值之间间隔至少两个单元。举例来说，如果说了一个组分的数量或一个工艺参数的值，比如，温度，压力，时间等等，是从1到90，20到80较佳，30到70最佳，是想表达15到85，22到68，43到51，30到32等数值都已经明白的列举在此说明书中。对于小于1的数值，0.0001,0.001,0.01或者0.1被认为是比较适当的一个单元。前述例子仅作举例说明之用，实际上，所有在列举的最低到最高值之间的数值组合均被视为以类似方式清楚地列在本说明书中。
除有定义外，本文中所用的技术和科学术语具有与本发明所述领域技术人员普遍理解的相同含义。本文所用的术语“第一”、“第二”等并不表示任何顺序、数量或重要性，而只是用于区别一种元件和另一种元件。并且，所述“一”或“一个”不表示数量的限定，而是表示存在一个的相关项目。
在高温下处理原料的工件，比如，在烃类热裂解过程中使用的工件，其用于接触被处理的烃类原料的内表面上一般镀覆有一层防结焦催化剂，用来防止结焦和堵塞。在本发明的实施例中，在金属基体和防结焦催化剂层之间设置有氧化铝阻挡层，该氧化铝阻挡层可防止一种或多种会导致催化剂失效的元素从所述金属基体扩散到催化剂层中去。
本发明所称“反应装置”是指石化流程中使用的裂解炉管、管路接头、反应容器和辐射管或卷中的至少一种。反应装置可以是一个裂解炉，其包括燃烧室，通过燃烧室运行着一个管阵列。该管阵列和相应的配件总共有几百米。管列阵可包括直管和弯管。
在基体和防结焦催化剂层之间有氧化铝阻挡层的工件可用于应避免焦炭堆积的烃类裂解反应装置中。该反应装置可以是任何可用于烃类裂解的反应装置。在一些实施例中，该反应装置包括裂解炉管、管路接头、反应容器和辐射管或卷中的至少一种。在一些实施例中，反应装置内置有温度在大约500°C到大约1000°C的炉管的燃烧室。
本发明所称“烃类裂解”包括但不限于如乙烷、丙烷、丁烷和石脑油等烃类在水蒸气重量百分比为约30%到约70%时于反应装置中裂解以制取如乙烯和丙烯等低碳烯烃。诸如原油经过常压或减压分馏获得的渣油等烃类有时也在反应装置中裂解，反应温度为约480°C到约600°C，水蒸汽重量百分比为约1%到约2%。
本发明所称“焦炭”包括但不限于来自煤、石油、木材、烃及其他含碳物质的含碳固体或液体或形成含碳固体或液体的微粒或高分子，例如，烃类裂解炉里存在的炭黑、焦油及热解碳。
本发明的一个方面提供了一种包括氧化铝阻挡层的工件。如图1所示，工件100包括金属基体102、防结焦催化剂层104、以及形成于金属基体102和防结焦催化剂层104之间的氧化铝阻挡层106。在所述金属基体102和氧化铝阻挡层106之间可能还会有铝化物层（未图示）。所述金属基体102可以是任何形状。在一个实施例中，所述金属基体为一个管状物，其具有一个用来接触在高温下被处理的氧化性原料的内表面，所述氧化铝阻挡层覆盖管状物的内表面，而防结焦催化剂层形成于所述氧化铝阻挡层上。所述金属基体102可由包括但不限于铁基合金、镍基合金和钴几合金的金属材料制成。对于用于热裂解工艺的工件，其基体可包含铬、镍和铁中的至少一种，在一个具体的实施例中，其基体由一种含铬、镍和铁的金属材料制成。非限制性地举例来说，合适的金属材料包括25Cr20Ni钢、35Cr45Ni钢、以及镍基超合金。在一些实施例中，所述基体中铝的质量百分含量小于3%，或更进一步地，小于0.05%。
所述防结焦催化剂层104中的催化剂可以是化学式为AaBbCcDdO3-δ的钙钛矿材料，其中，0<a<1.2，0≤b≤1.2，0.9<a+b≤1.2，0<c<1.2，0≤d≤1.2，0.9<c+d≤1.2，-0.5<δ<0.5；
A选自钙(Ca)、锶(Sr)、钡(Ba)及其组合；
B选自锂(Li)、钠(Na)、钾(K)、铷(Rb)及其组合；
C选自铈(Ce)、锆(Zr)、锑(Sb)、镨(Pr)、钛(Ti)、铬(Cr)、锰(Mn)、铁(Fe)、钴(Co)、镍(Ni)、镓(Ga)、锡(Sn)、铽(Tb)及其组合；
D选自镧(La)、铈(Ce)、镨(Pr)、钕(Nd)、钷(Pm)、钐(Sm)、铕(Eu)、钆(Gd)、铽(Tb)、镝(Dy)、钬(Ho)、铒(Er)、铥(Tm)、镱(Yb)、镥(Lu)、钪(Sc)、钛(Ti)、钒(V)、铬(Cr)、锰(Mn)、铁(Fe)、钴(Co)、镍(Ni)、铜(Cu)、锌(Zn)、钇(Y)、锆(Zr)、铌(Nb)、钼(Mo)、锝(Tc)、钌(Ru)、铑(Rh)、钯(Pd)、银(Ag)、镉(Cd)、铪(Hf)、钽(Ta)、钨(W)、铼(Re)、锇(Os)、铱(Ir)、铂(Pt)、金(Au)、镓(Ga)、铟(In)、锡(Sn)、锑(Sb)及其组合。
在一些具体的实施例中，所述防结焦催化剂是选自改性LaCrO3、改性LaMnO3、BaCeO3、BaZrO3,BaCexZr(1-x)O3,BaCexY(1-x)O3及其组合，其中0≤x≤1。特别地，所述催化剂可为BaCe0.7Zr0.3O3。
在一些实施例中，所述防结焦催化剂层104中的催化剂为三斜霞石。本发明所称“三斜霞石”包括但不限于具有氧化钠-稳定（或嵌入或富有）的高三斜霞石晶体结构的材料，即拥有一定数量氧化钠嵌入立方主晶格且群体对称为P213或的晶体结构的物质。
所述氧化铝阻挡层106为致密的α-氧化铝阻挡层，可阻止铬等干扰元素从基体102扩散到催化剂层104中。在一些实施例中，所述氧化铝阻挡层106的厚度为约0.01微米到约10微米，或更进一步地，为约1微米到约5微米。
通过对所述金属基体镀铝然后再进行热处理，可形成一层覆盖所述金属基体的氧化铝阻挡层，再往所述氧化铝阻挡层上涂覆防结焦的催化剂，如钙钛矿，可形成一层催化剂层。除了所述氧化铝阻挡层外，所述金属基体和催化剂层之间还可能有其他附加层。比如，在一些实施例中，在形成所述氧化铝阻挡层后，所述在镀铝的过程中形成的铝化物层可能仍然存在，因此在金属基体和氧化铝阻挡层之间还有铝化物层。可通过化学气相沉积法（chemical vapor deposition，CVD）、浆料涂覆法、电镀法、热浸渍法或喷涂法等方法对所述金属基体进行镀铝。
若用化学气相沉积法对所述金属基体进行镀铝，可将所述金属基体放置到一个真空炉中，在约为0.1-5.0Pa的压力和约为800-1200°C或更进一步地约为800-1100°C的温度下焙烧约2-24小时。适合用作镀铝的前体化合物包括气相氯化铝（AlCl3）以及在镀铝的条件下可生成气相AlCl3的材料。气相的镀铝前体化合物可输送到给金属基体镀铝的真空炉中。固相的镀铝前体化合物可与金属基体一起放置到真空炉内。在一个具体的实施例中，气相AlCl3是用氢气为载气输送到所述真空炉的。在一个具体的实施例中，以包括铝、铁和氯化铵（NH4Cl）的固体粉末为镀铝前体化合物，与金属基体一起放置到真空炉中，在真空炉内的条件下，铝和NH4Cl发生反应生成气相AlCl3。所述固体粉末中所含的铁起到缓冲剂的作用，减慢铝和NH4Cl之间的反应。可向真空炉中通入氢气来辅助所述镀铝的过程。所述焙烧的时间取决于所需的阻挡层的厚度，时间越长，产生的涂层越厚。
若用浆料涂覆法对所述金属基体进行镀铝，可将一种含铝的浆料涂覆到金属基体上，再对该涂覆有浆料的金属基体进行热处理。浆料中的铝扩散到所述金属基体的表面区域，在金属基体的表面形成金属铝化物层。在一些具体的实施例中，所述金属基体通过如美国专利US7,569,283、US7,332,024和US7,829,142所描述的浆料涂覆法进行镀铝，该等美国专利US7,569,283、US7,332,024和US7,829,142的内容以引用的方式全部纳入本文。
可使用各种不同成分的浆料。除了上述美国专利US7,569,283、US7,332,024和US7,829,142中所描述的浆料之外，还可使用如美国专利US7,270,852、US7,449,241和US7,896,962中所描述的浆料成分，该等美国专利US7,270,852、US7,449,241和US7,896,962的内容在此以引用的方式全部纳入本文。所述浆料可通过水拭法、油漆法、离心法、喷涂法、填充并排出法、或浸渍法涂覆到所述金属基体上。
在一个具体的实施例中，所述浆料的成分包括铝基粉末、氧化硅（colloidalsilica）和甘油。其中所述铝基粉末可以是任何铝的质量百分含量大于75%的粉末，如铝粉、铝-硅合金粉及其组合。所述涂覆有一层浆料的金属基体在约50-250°C的温度下进行几小时的硬化处理，以干燥所述浆料层，再对其进行一个三阶段加热的焙烧处理和一个两阶段的扩散热处理。在所述扩散热处理过程中，所述浆料中的铝扩散到所述金属基体中以在金属基体表面形成金属铝化物（如FeAl、CrAl和Ni3Al）层。
所述镀铝后的金属基体可在约800°C至约1100°C，或更进一步地，在约900°C至约1000°C的温度下，压力约0.05-0.5Pa的氧化气氛中进行热处理，在该热处理的过程中，所述金属铝化物被氧化，形成一个覆盖所述金属基体的氧化铝阻挡层。可能还会有部分金属铝化物保留在所述金属基体和氧化铝阻挡层之间。
所述防结焦的催化剂可通过等离子喷涂、化学气相沉积或浆料涂覆法等方法涂覆到所述氧化铝阻挡层上。在一些实施例中，可通过浆料涂覆法将一种钙钛矿催化剂涂覆到所述氧化铝阻挡层上。一种通过浆料涂覆法将钙钛矿催化剂涂覆到氧化铝阻挡层上的工艺包括以下步骤：制备一种包含钙钛矿催化剂的浆料；在所述金属基体上涂敷一层所述浆料；然后烧结所述涂覆有浆料的金属基体。所述浆料可用钙钛矿催化剂粉末和有机粘结剂、润湿剂和溶剂中的至少一种制备而成。在烧结所述涂覆有浆料的金属基体之前，可在一个比烧结温度更低的温度下将所述浆料层干燥。在一个具体的实施例中，所述涂覆有浆料的金属基体在约100°C的温度下进行干燥，然后在约900-1100°C的温度下在氩气气氛中烧结约2-5小时。
在一些具体的实施例中，采用了一种如第11/63324号美国专利申请中所描述的浆料成分和浆料涂覆方法，该第11/63324号美国专利申请的内容在此以引用的方式全部纳入本文。一种包括钙钛矿催化剂和一种无机材料的浆料被涂覆到工件（反应装置）的表面，其中所述无机材料包括氧化铈、氧化锌、氧化锡、氧化锆、勃姆石和二氧化硅中的至少一种。在约1000°C的温度下烧结所述浆料涂层，形成一个覆盖所述工件表面的钙钛矿催化剂层。
实例1
在本实例中，以九个25Cr20Ni钢制成的取样片（样品）作基体，其中所述25Cr20Ni钢制成的取样片的以质量百分比表示的成分如下表所示。
| C | Si | Mn | Cr | Ni | Fe |
| 0.13% | 0.48% | 1.35% | 26.25% | 21% | 余量 |
所述取样片先用粗砂纸打磨，再进行Al2O3喷沙处理，然后在酒精中进行超声清洁。然后用化学气相沉积镀铝法对所述清洁后的取样片进行镀铝，镀铝的参数为：
压力：0.8Pa
温度：1050°C
时间：6小时
镀铝过程中以具有下表所示组分（质量百分比）的固体粉末作为前体化合物。
| Al | NH4Cl | Fe |
| 50% | 3% | 余量 |
通过所述化学气相沉积镀铝工艺，在各取样片的表面形成一个铝化物层。将九个镀铝后的取样片清洗之后，将其中的八个（样品1-8）进行热处理以使铝化物氧化形成氧化铝层，而将剩余的一个（样品9）留着用于直接涂覆催化剂层。在热处理过程中，所述八个镀铝后的取样片被放置一个真空炉中，该真空炉在约3小时内被加热到约900°C至约1000°C，然后被充入空气至压力达约0.05Pa至约0.5Pa，保持约20小时到约30小时。基于比较分析的目的，所述八个取样片被分成四组，分别以不同的参数进行热处理，具体的热处理参数如下表所示。
| 样品 | 温度(°C) | 压力(Pa) | 时间(小时) |
| 1 | 1000 | 0.05 | 20 |
| 2 | 1000 | 0.05 | 20 |
| 3 | 900 | 0.05 | 30 |
| 4 | 900 | 0.05 | 30 |
| 5 | 900 | 0.5 | 20 |
| 6 | 900 | 0.5 | 20 |
| 7 | 1000 | 0.5 | 30 |
| 8 | 1000 | 0.5 | 30 |
经过所述热处理之后，在所述八个取样片上分别形成了一个厚度约为1-5微米的氧化铝层。通过比较所述分别形成于样品1-8上的氧化铝层的厚度，发现氧化铝层的厚度随着热处理温度和时间的增大而增大，并随着热处理压力的减小而增大。
再通过浆料涂覆工艺，在样品1-8（镀铝并氧化后的样品）、样品9（镀铝但未氧化的样品）和一个无覆盖的25Cr20Ni钢样品（样品10，既未镀铝也未氧化）上分别形成防结焦催化剂层，该浆料涂覆工艺包括以下步骤：
（1）催化剂（BaCe0.7Zr0.3O3）粉末制备
所述催化剂（BaCe0.7Zr0.3O3）粉末通过固相反应（solid-state reaction）的方法获得。在乙醇中混合高纯度碳酸钡、氧化锆、氧化铈和氧化钇粉末（均来自中国上海国药集团化学试剂有限公司），并球磨12小时。然后将制得的混合物在1450°C下空气中烘干并煅烧6小时，从而制得BaCe0.7Zr0.3O3粉末。将制得的粉末与酒精混合，然后再球磨12小时，等酒精干后，获得了催化剂细粉（d50=1.5um）。
（2）浆料制备
将31.37克用前述方法制得的BaCe0.7Zr0.3O3粉末加到一个塑料罐中；将46.72克CeO2溶胶（在水中的质量百分含量为20%，Alfa Aesar #12730）加入到所述塑料罐中，用作无机粘结剂来提高BaCe0.7Zr0.3O3的涂层强度；添加4.41克甘油，以提高浆料的润湿能力；添加12.63克PVA（质量百分含量为10%的水溶液）以获得良好的以获得良好的生胚涂层强度；再添加10ul的Triton X100，用作消泡剂。具体的配方如下表所示。
| BaCe0.7Zr0.3O3 | 31.37克 |
| CeO2溶液 | 46.72克 |
| 甘油 | 4.41克 |
| PVA | 12.63克 |
| Triton X100 | 10ul |
将所述塑料罐安装到高速混合器中，以2000RPM的转速混合3分钟，获得均匀的浆料。
（3）浆料的涂布
将各样品浸入所述浆料中使其涂上一层浆料，干燥所述浆料层，再将有干燥的浆料层的样品放到烧结炉中，在1000°C下氩气气氛中烧结3小时，再以约1-6℃/分钟的冷却速度将样品冷却，这样，各样品上镀覆上了一层BaCe0.7Zr0.3O3催化剂层。结果发现，与样品9相比，样品1-8上的催化剂层的附着性能明显更好，而样品9上的催化剂层部分剥落。
所述样品10（BaCe0.7Zr0.3O3直接镀覆在无覆盖的25Cr20Ni钢基体上）在900°C下空气氧化气氛中模拟加速除焦试验，试验发现，在空气中氧化8小时之后，样品上的BaCe0.7Zr0.3O3催化剂层转变成黄色（铬酸钡的颜色）。将样品取出做X射线衍射（XRD）显微分析，分析结果显示催化剂层中的主要成分为铬酸钡。BaCe0.7Zr0.3O3已和铬发生反应生成了铬酸钡。XRD分析后，对样品10进行模拟裂解试验，发现在模拟裂解试验中样品10上的催化剂层几乎已经失效。
将样品1-8在900°C下空气中模拟除焦过程进行200小时疲劳测试，其间每隔50小时将样品取出做XRD显微分析。分析结果显示，样品1-8上的催化剂持续了200小时而没有发生退化。此外，实验发现，经过200小时后，样品1-8上的催化剂层与基体之间仍有良好的附着力。再对所述经过200小时疲劳测试后的样品1-8进行了模拟裂解试验，在该模拟裂解试验中样品1-8上的催化剂显示了良好的防结焦性能。
实例2
在本实例中，用35Cr45Ni钢制成的取样片作基体，以实例1中所述的工艺流程制备了样品，其中35Cr45Ni钢制成的取样片的以质量百分比表示的成分如下表所示。
| Ni | Cr | Si | C | Nb | Fe |
| 45% | 35% | 2.5% | 0.45% | 1.5% | 余量 |
通过实例1中所述的工艺流程，在各样品上镀有一层BaCe0.7Zr0.3O3催化剂。
类似地，将获得的样品在900°C下空气中模拟除焦过程进行200小时疲劳测试，其间每隔50小时将样品取出做XRD显微分析。分析结果显示，这些样品上的催化剂持续了200小时而没有发生退化。此外，实验发现，经过200小时后，这些样品上的催化剂层与基体之间仍有良好的附着力。再对所述经过200小时疲劳测试后的样品进行了模拟裂解试验，在该模拟裂解试验中样品上的催化剂显示了良好的防结焦性能。
实例3
在本实例中，以和实例1中成分相同的25Cr20Ni钢制成的取样片作基体，以和实例1类似但镀铝工艺不同的流程制备了样品。本实例中采用了一种与实例1不同的工艺对取样片进行了镀铝。
在本实例的镀铝过程中，对取样片进行Al2O3喷沙处理，然后在约240°C的烤箱中进行约4小时的热脱脂处理。然后在取样片上涂覆一层含铝的浆料，该浆料的以质量百分比表示的成分为：8%的甘油、32%的LP-30氧化硅、45%的铝粉（颗粒尺寸约为10微米）和15%的铝-硅合金粉。在入口空气压力约为40Psi的条件下将所述浆料涂覆到所述取样片上，在各取样片上涂上厚度为约43微米到约89微米的一层浆料。将所述涂有浆料的取样片放入烤箱中进行硬化处理，将烤箱加热到约80°C保持约1小时，再加热到约120°C保持约0.5小时，再加热到约220°C保持约1小时。然后将所述取样片放入一个真空炉中，加热至约649°C保持约15分钟，同时往该真空炉中输入氩气使炉内压力达到0.5托（626.5Pa），然后再加热到约871°C保持约2小时。这样，浆料中的铝扩散到取样片中，在各取样片的表面形成铝化物的涂层。然后，将炉中的取样片冷却后取出并将其上的残渣磨去。
然后再用实例1中的工艺流程对所述取样片进行热处理以形成氧化铝层，并在氧化铝层上涂覆形成BaCe0.7Zr0.3O3催化剂层。
类似地，将获得的样品在900°C下空气中模拟除焦过程进行200小时疲劳测试，其间每隔50小时将样品取出做XRD显微分析。分析结果显示，这些样品上的催化剂持续了200小时而没有发生退化。此外，实验发现，经过200小时后，这些样品上的催化剂层与基体之间仍有良好的附着力。再对所述经过200小时疲劳测试后的样品进行了模拟裂解试验，在该模拟裂解试验中样品上的催化剂显示了良好的防结焦性能。
本发明可用其他的不违背本发明的精神或主要特征的具体形式来概述。因此，无论从哪一点来看，本发明的上述实施方案都只能认为是对本发明的说明而不能限制本发明，本发明的范围是由权利要求书界定，而不是由上述界定的，因此，在与本发明的权利要求书相当的含义和范围内的任何改变，都应认为是包括在权利要求书的范围内。
Claims (20)
1.一种工件，其包括：
金属基体；
防结焦催化剂层；以及
在所述金属基体和防结焦催化剂层之间的氧化铝阻挡层，所述氧化铝阻挡层可阻止干扰元素从所述金属基体扩散到所述防结焦催化剂层，其中所述干扰元素包括铬。
2.如权利要求1所述的工件，其中所述金属基体为管状物，该管状物具有内表面，所述氧化铝阻挡层覆盖所述管状物的内表面，所述防结焦催化剂层形成于所述氧化铝阻挡层上。
3.如权利要求1所述的工件，其中所述金属基体包括镍和铁中的至少一种与铬。
4.如权利要求1所述的工件，其中所述金属基体中铝的质量百分含量小于3％。
5.如权利要求1所述的工件，其中所述金属基体中铝的质量百分含量小于0.05％。
6.如权利要求1所述的工件，其中所述防结焦催化剂包括钙钛矿。
7.如权利要求6所述的工件，其中所述钙钛矿选自改性LaCrO3、改性LaMnO3、BaCeO3、BaZrO3、BaCexZr(1-x)O3、BaCexY(1-x)O3及其组合，其中0≤x≤1。
8.如权利要求7所述的工件，其中所述钙钛矿为BaCexZr(1-x)O3，其中0≤x≤1。
9.如权利要求7所述的工件，其中所述钙钛矿为BaCe0.7Zr0.3O3。
10.一种工艺，其包括：
对金属基体进行镀铝；
对镀铝后的金属基体进行热处理以形成覆盖所述金属基体的氧化铝阻挡层；以及
在所述氧化铝阻挡层上形成防结焦催化剂层，其中，
所述氧化铝阻挡层可阻止干扰元素从所述金属基体扩散到所述防结焦催化剂层，所述干扰元素包括铬。
11.如权利要求10所述的工艺，其中所述金属基体为管状物，所述氧化铝阻挡层覆盖所述管状物的内表面。
12.如权利要求10所述的工艺，其中金属基体是通过化学气相沉积法、浆料涂覆法、电镀法、热浸渍法或喷涂法进行镀铝的。
13.如权利要求12所述的工艺，其中所述金属基体是通过化学气相沉积法或浆料涂覆法进行镀铝的。
14.如权利要求10所述的工艺，其中所述对镀铝后的金属基体进行热处理的步骤包括在800℃到1100℃的温度下在氧化气氛中加热所述镀铝后的金属基体。
15.如权利要求10所述的工艺，其中所述防结焦催化剂层是通过等离子喷涂法、化学气相沉积法或浆料涂覆法涂覆到所述氧化铝阻挡层上的。
16.如权利要求10所述的工艺，其中所述防结焦催化剂包括钙钛矿。
17.如权利要求16所述的工艺，其中所述钙钛矿选自改性LaCrO3、改性LaMnO3、BaCeO3、BaZrO3、BaCexZr(1-x)O3、BaCexY(1-x)O3及其组合，其中0≤x≤1。
18.如权利要求17所述的工艺，其中所述钙钛矿为BaCexZr(1-x)O3，其中0≤x≤1。
19.一种以权利要求10所述的工艺制备的涂层金属基体。
20.一种包括以权利要求10所述的工艺制备的涂层金属基体的设备。
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| CN106902831A (zh) * | 2015-12-23 | 2017-06-30 | 通用电气公司 | 防结焦的催化材料、保护制品防止结焦的方法以及有防结焦涂层的制品 |
| CN105885486A (zh) * | 2016-06-20 | 2016-08-24 | 天津大学 | 一种抑制炉管结焦的复合涂料、其制备方法和由其制得的复合涂层 |
| JP2022551859A (ja) * | 2019-10-08 | 2022-12-14 | アプライド マテリアルズ インコーポレイテッド | 航空宇宙用部品上に耐コーキング性保護コーティングを堆積させるための方法 |
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| CN114196238B (zh) * | 2021-12-28 | 2022-06-14 | 宜兴瑞泰耐火材料工程有限公司 | 一种防结焦涂料及其使用方法 |
| CN116200743A (zh) * | 2023-04-25 | 2023-06-02 | 鑫鹏源(聊城)智能科技有限公司 | 不锈钢基体用阻氢渗透的复合玻璃质壁垒层及其制备方法和应用 |
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| US9901892B2 (en) | 2018-02-27 |
| MY168293A (en) | 2018-10-23 |
| ES2937243T3 (es) | 2023-03-27 |
| EP2931422A1 (en) | 2015-10-21 |
| KR20150095831A (ko) | 2015-08-21 |
| US20150306558A1 (en) | 2015-10-29 |
| PL2931422T3 (pl) | 2023-02-27 |
| CN103861662A (zh) | 2014-06-18 |
| WO2014092944A1 (en) | 2014-06-19 |
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