CN101253004B - 涂层制品 - Google Patents

涂层制品 Download PDF

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CN101253004B
CN101253004B CN2006800313635A CN200680031363A CN101253004B CN 101253004 B CN101253004 B CN 101253004B CN 2006800313635 A CN2006800313635 A CN 2006800313635A CN 200680031363 A CN200680031363 A CN 200680031363A CN 101253004 B CN101253004 B CN 101253004B
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oxide ceramic
layer
ceramic layer
rotor
metal
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CN101253004A (zh
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M·弗罗伊茨海姆
J·黑珀考森
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Leybold GmbH
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Oerlikon Leybold Vacuum GmbH
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    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
    • B05D7/24—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials for applying particular liquids or other fluent materials
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F04—POSITIVE - DISPLACEMENT MACHINES FOR LIQUIDS; PUMPS FOR LIQUIDS OR ELASTIC FLUIDS
    • F04D—NON-POSITIVE-DISPLACEMENT PUMPS
    • F04D29/00—Details, component parts, or accessories
    • F04D29/02—Selection of particular materials
    • F04D29/023—Selection of particular materials especially adapted for elastic fluid pumps
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D1/00—Processes for applying liquids or other fluent materials
    • B05D1/60—Deposition of organic layers from vapour phase
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/448—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials
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    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
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    • C25D11/026—Anodisation with spark discharge
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    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
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    • C25D11/24—Chemical after-treatment
    • C25D11/246—Chemical after-treatment for sealing layers
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    • F04—POSITIVE - DISPLACEMENT MACHINES FOR LIQUIDS; PUMPS FOR LIQUIDS OR ELASTIC FLUIDS
    • F04D—NON-POSITIVE-DISPLACEMENT PUMPS
    • F04D19/00—Axial-flow pumps
    • F04D19/02—Multi-stage pumps
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    • F04D19/042—Turbomolecular vacuum pumps
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    • B05D2202/00—Metallic substrate
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    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D2350/00—Pretreatment of the substrate
    • B05D2350/60—Adding a layer before coating
    • B05D2350/63—Adding a layer before coating ceramic layer
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F05—INDEXING SCHEMES RELATING TO ENGINES OR PUMPS IN VARIOUS SUBCLASSES OF CLASSES F01-F04
    • F05D—INDEXING SCHEME FOR ASPECTS RELATING TO NON-POSITIVE-DISPLACEMENT MACHINES OR ENGINES, GAS-TURBINES OR JET-PROPULSION PLANTS
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    • F05D2230/30—Manufacture with deposition of material
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    • F05—INDEXING SCHEMES RELATING TO ENGINES OR PUMPS IN VARIOUS SUBCLASSES OF CLASSES F01-F04
    • F05D—INDEXING SCHEME FOR ASPECTS RELATING TO NON-POSITIVE-DISPLACEMENT MACHINES OR ENGINES, GAS-TURBINES OR JET-PROPULSION PLANTS
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    • F05D2230/90—Coating; Surface treatment
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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    • F05D—INDEXING SCHEME FOR ASPECTS RELATING TO NON-POSITIVE-DISPLACEMENT MACHINES OR ENGINES, GAS-TURBINES OR JET-PROPULSION PLANTS
    • F05D2300/00—Materials; Properties thereof
    • F05D2300/10—Metals, alloys or intermetallic compounds
    • F05D2300/17—Alloys
    • F05D2300/173—Aluminium alloys, e.g. AlCuMgPb
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    • F05D2300/00—Materials; Properties thereof
    • F05D2300/20—Oxide or non-oxide ceramics
    • F05D2300/21—Oxide ceramics
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F05—INDEXING SCHEMES RELATING TO ENGINES OR PUMPS IN VARIOUS SUBCLASSES OF CLASSES F01-F04
    • F05D—INDEXING SCHEME FOR ASPECTS RELATING TO NON-POSITIVE-DISPLACEMENT MACHINES OR ENGINES, GAS-TURBINES OR JET-PROPULSION PLANTS
    • F05D2300/00—Materials; Properties thereof
    • F05D2300/40—Organic materials
    • F05D2300/43—Synthetic polymers, e.g. plastics; Rubber
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F05—INDEXING SCHEMES RELATING TO ENGINES OR PUMPS IN VARIOUS SUBCLASSES OF CLASSES F01-F04
    • F05D—INDEXING SCHEME FOR ASPECTS RELATING TO NON-POSITIVE-DISPLACEMENT MACHINES OR ENGINES, GAS-TURBINES OR JET-PROPULSION PLANTS
    • F05D2300/00—Materials; Properties thereof
    • F05D2300/60—Properties or characteristics given to material by treatment or manufacturing
    • F05D2300/611—Coating
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/26—Web or sheet containing structurally defined element or component, the element or component having a specified physical dimension
    • Y10T428/263—Coating layer not in excess of 5 mils thick or equivalent
    • Y10T428/264—Up to 3 mils
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract

本发明涉及一种用氧化物陶瓷层对由选自铝、镁、钛、铌、和/或锆、及其合金的阀用金属制成的制品进行涂布的方法，该氧化物陶瓷层由具有薄阻挡层作为朝向金属的边界层的金属形成，其表面已经涂有聚合物，其特征在于，所述聚合物通过真空涂布然后使二聚体聚合而以通式I的二聚体或卤代二聚体形式引入氧化物陶瓷层的毛细管系统中：
Figure B2006800313635A00011
其中，R1代表一个或多个氢或卤素残基；每个R2代表氢或卤素；且R3通常代表完成二聚结构的相应亚二甲苯基残基。

Description

涂层制品
发明领域
本发明涉及一种由选自Al、Mg、Ti、Nb和/或Zr或其合金的阀用金属(valve metal)制成的制品的涂布方法，以及由此得到的制品。
背景技术
EP 0 545 230 A1涉及一种在形成阻挡层(barrier-layer)的金属上产生任选改性的氧化物陶瓷层的方法以及得到的产品。为了增加形成阻挡层的金属上的氧化物陶瓷层的厚度和耐磨性，在至少1A/dm2的恒定电流密度下在pH值为2至8的无氯电解质浴中进行等离子体-化学阳极氧化，直至电压达到终值。在铝或铝合金制品上，可以产生由刚玉组成的氧化物陶瓷层。在镁和钛上，也可以达到至多150μm的层厚。
对于许多应用来说，高负载的阀用金属部件即使在极端条件下也必须耐腐蚀并且耐磨。这可以通过下述方式实现：提供带有具有粗筛互连毛细管系统的氧化物陶瓷层的制品，引入在至少一个维度上小于毛细管直径的含氟聚合物颗粒，并且将具有预填毛细管系统的制品暴露于变化的压力条件。
DE 41 24 730 C2涉及一种将含氟聚合物加入通过阳极氧化制备的由铝或其合金制成的制品的微孔表面中的方法，其特征在于将粒径为1至50 nm的含氟聚合物或其前体的水相悬浮液加入到垂直于金属的阳极化硬铝层毛细管中。
DE 42 39 391 C2涉及具有填有含氟聚合物的氧化物陶瓷层的铝、镁或钛的制品，及其制造方法。描述了由形成阻挡层的金属制成的制品，其在形成阻挡层的金属上具有叠加有烧结致密氧化物陶瓷层的附着阻挡薄层，并在其顶上具有带有实质上填有含氟氧化物的粗筛互连毛细管系统的氧化物陶瓷层。具体地说，氧化物陶瓷层的厚度为40至150μm。这些制品的例子是用于涡轮-分子泵的转子、用于柴油或汽油发动机的涡轮增压机、用于真空或等离子体技术的部件、用于冠状放电的辊、以及超声焊极(sonotrode)、各种铝或铝合金。据说明，除非是液体，否则结合到外部氧化物陶瓷层中的含氟聚合物或其前体的颗粒作为适当溶剂中的溶液或悬浮液而引入。该描述的本质核心是将含氟聚合物颗粒在适当的溶剂中承受适合浸渍系统的变化的压力条件，其中首先使用真空从氧化物陶瓷层的毛细管系统中除去空气，随后颗粒在真空作用下进入孔隙，并且在解除真空之后被大气压压入孔隙内，从而也达到微细分支(ramification)。
作为特别合适的含氟聚合物，具体描述了四氟乙烯、六氟丙烯、二氟乙烯、偏二氟乙烯、和三氟氯乙烯的聚合物和共聚物。这些含氟聚合物已知事实上不溶于任何溶剂，因此根据DE 42 39 391 C2，应当视为这些聚合物以分散体的形式被引入表面。
日本专利JP 2,913,537中描述了类似方法。耐腐蚀结构的特征在于，在半导体制造装置中用于释放氯气的涡轮-分子泵的铝/合金部件上配置了厚度为大约20μm的Ni-P合金的镀金属层(plated layer)，该部件与氯气接触，并且通过将所述涡轮-分子泵的转子或定子浸泡在用于形成含氟树脂层的液体中然后干燥而在所述镀金属层上形成含氟树脂保护层。
EP1485 622 B1涉及一种用薄阻挡层对由选自铝、镁、钛、铌和/或锆及其合金的阀用金属制成的制品进行涂布的方法，该薄阻挡层由由金属和其上配置的氧化物陶瓷层组成，该氧化物陶瓷层的表面已经涂有含氟聚合物，其特征在于，含氟聚合物以溶液形式通过下述方法引入氧化物陶瓷层的毛细管系统中：真空浸渍，然后除去溶液的未润湿部分，并干燥。
上述现有技术文献的共同特征在于含氟聚合物实质上配置在氧化物陶瓷层的外表面上，但仅以很低的程度进入分支中。
因此，本发明的目的是改善涂层的均匀性，从而改善制品特别是氧化物陶瓷层的密封特性。
发明内容
在第一实施方式中，上述目的通过用氧化物陶瓷层对由选自铝、镁、钛、铌、和/或锆、及其合金的阀用金属制成的制品进行涂布的方法来实现，该氧化物陶瓷层由具有薄阻挡层作为朝向金属的边界层的金属形成，其表面已经涂有聚合物，其特征在于，所述聚合物通过真空涂布然后使二聚体聚合而以通式I的二聚体或卤代二聚体形式引入氧化物陶瓷层的毛细管系统中：
Figure S2006800313635D00031
其中，
R1代表一个或多个氢或卤素残基；
每个R2代表氢或卤素；且
R3通常代表完成二聚结构的相应亚二甲苯基残基。
通式(I)代表二聚结构的单体。
具体实施方式
通过氧化物或陶瓷层、特别是阳极产生的氧化物或陶瓷层的后处理，通过用二聚体或卤代二聚体进行真空涂布，保护层的致密性特性相对于现有技术可以大大提高。应用该聚合物的另一优点在于，其对于侵蚀性和腐蚀性介质具有极高的耐受性。这些介质可以是气态的，例如用于等离子体蚀刻器中的涡轮分子泵，但是也可以包括酸或碱的液体或蒸汽。
据推测，二聚体首先被单体化(monomerize)，然后是由此形成的自由基的聚合。
类似地，也可以直接使用单体或卤代单体，而不必应用预先涂布的氧化物或陶瓷类涂层。由此处理的表面的特征还在于特别的特性，例如抗污性或抗尘粒性，以及不被例如水、油或其它液体的介质润湿。
使用本发明，相对于现有技术可以显著提高多孔表面涂层的均匀性。为实现这一点，特别有帮助的是在真空下进行上述层的涂布，其中气态的单体或卤代单体进入层中的孔隙或微观小空腔，并在其中聚合。
一方面，根据本发明的涂层的优点在于表面能非常低，另一方面，其优点在于对几乎所有溶剂和气体具有最佳的耐受性和不渗透性，这些溶剂和气体具体包括溶剂、油、(以及硅氧烷油)和水基液体。固体也可以沉积在薄膜表面，但有困难。此外，聚合的特性导致对上述阀用金属以及其氧化物陶瓷层的粘附非常好。进一步指出的是，其化学、热和电稳定性很高，在处理过的表面所暴露的一般工作条件下保持不受影响。
在本发明的意义内，使用铝、镁、钛、铌、或钛、及其合金作为阀用金属。
在此要特别指出的是铝和铝合金，其经常用于制备涡轮分子泵中的转子。
本发明中所用的术语“铝及其合金”是指根据DIN EN5731-4的超纯铝以及2xxx、3xxx、5xxx、6xxx和7xxx组的合金，以及根据DINEN1706的铸造合金。
除纯镁之外，其它适用于本发明的目的的还有，具体的说，ASTM命名为AS41、AM60、AZ61、AZ63、AZ81、AZ91、AZ92、HK31、QE22、ZE41、ZH62、ZK51、ZK61、EZ33、HZ32的镁铸造合金，以及捏和合金AZ31、AZ61、AZ80、M1 ZK60、ZK40。
而且，也可以使用纯钛或其它钛合金，例如TiAl6V4、TiAl5Fe2.5和其它。
根据本发明，特别优选地，氧化物陶瓷层由或多或少分级(graded)的材料制备，其中氧化物陶瓷层包括致密的阻挡层作为朝向阀用金属的边界层，之后是微孔层结构，其朝向表面变为粗筛互连毛细管结构。相应的氧化物陶瓷层由例如DE 42 39 391 C2可知。
另外，根据本发明，等离子体-化学氧化物陶瓷层、以及其它氧化层如通过电化学阳极化涂布的氧化层，以10至50μm、特别是20至40μm的厚度使用，这也可以从DE 42 39 391C2中得知。
根据本发明可以使用的单体或卤代单体优选选自通式I的对亚二甲苯基的二聚体或卤代对亚二甲苯基的二聚体。
名为“ParyleneTM”的亚二甲苯基衍生物由Parylene Coating ServicesInc.或Uniglobal Kisco Inc.出售，作为用途广泛的涂层材料。ParyleneTM是一种在真空下通过从气相中缩合到基质上成为无孔透明聚合物薄膜来涂布的涂层。实际上，任何基质材料如金属、玻璃、纸、涂料、塑料、陶瓷、铁氧体和硅氧烷均可以用ParyleneTM涂层。在一利方式中，可以使用应用0.1至50μm的涂层厚度。ParyleneTM涂层是疏水、耐化学性涂层，对无机和有机介质如强酸、碱液、气体和水蒸汽均具有良好的阻挡作用。它们具有优异的电绝缘性，耐电压性高，且介电常数低。涂层从0.2μm的厚度起不含微孔和针孔。具有高裂缝进入性能(crevice access)的透明薄涂层适合用于结构复杂的基质，甚至是边缘。基质的涂层在真空下在没有温度负荷的情况下、尤其是在室温下进行。涂层耐温高达220℃。
起始原料通常是二聚体的形式(二对亚二甲苯基)，将其加热至大约150℃，以使其转变成相应的气态单体。层的厚度和均匀性通过所用二聚体的量和纯度来控制。
优选地，根据本发明，应用厚度为0.5至15μm、特别是5至10μm的聚-对亚二甲苯基层。
在另一个实施方式中，本发明包括由阀用金属制成的制品，其可以通过上述方法得到。根据本发明特别优选的是，这些制品用于涡轮-分子泵的部件，尤其是转子或定子，其最优选由铝或铝合金制备。
通过本发明，可以得到如下特征的制品：表面导纳(admittance)极低，这可以通过未处理氧化物层和真空浸渍氧化物层的导纳测量结果的比较而显示出。
在真空涂布中，确保了氧化层中的孔隙的完全涂布以及由此导致的整个表面的完全涂布。对于通过等离子体化学产生的层以及阳极氧化物层的孔隙尺寸，该方法特别有利。
经典的浸泡处理仅仅到达可润湿的表面，但不能进入孔隙(特别是硬阳极层的孔隙)。在这一方面，在等离子体氧化层上进行测试，并显示出如下差异：
常规涂层的导纳确认为42μS，与之相比较，根据本发明的真空涂层的导纳为7μS。
实施例
实施例1
根据通常用于聚对二甲苯的制备方法，将具有Kepla Coat涂层(25μm)且导纳为55μS的2xxx合金组试样片用＜10μm的ParyleneTM C涂布。
真空涂布之后，产生的导纳不再能测出。
对于导纳的测定，使用接触面积直径为2.3mm的测量池。使用硫酸钾溶液作为辅助电解质。测量本身使用Fischer公司的“Anotest YD”。

Claims (9)

1.一种用氧化物陶瓷层对由选自铝、镁、钛、铌、和/或锆、及其合金的阀用金属制成的涡轮分子泵的转子进行涂布的方法，所述氧化物陶瓷层通过等离子体化学涂布而由具有阻挡层作为朝向金属的边界层的金属形成，其表面已经涂有聚合物，其特征在于，所述聚合物以根据通式I的二聚体或卤代二聚体形式被单体化：
Figure FSB00000441767400011
其中，
R1代表一个或多个氢或卤素残基；
每个R2代表氢或卤素；且
R3代表完成二聚结构的相应亚二甲苯基残基；
并且，单体在真空下被引入所述氧化物陶瓷层的毛细管系统中和表面上，并在那里聚合。
2.根据权利要求1所述的方法，其特征在于，使用这样的氧化物陶瓷层：该氧化物陶瓷层具有阻挡层作为朝向阀用金属的边界层，然后是变为朝向表面的毛细管结构的微孔层状结构。
3.根据权利要求1或2所述的方法，其特征在于，所涂布的涡轮分子泵的转子具有厚度为10至50μm的氧化物陶瓷层。
4.根据权利要求3所述的方法，其特征在于，所涂布的涡轮分子泵的转子具有厚度为20至40μm的氧化物陶瓷层。
5.根据权利要求1或2所述的方法，其特征在于，使用选自二聚氟代亚二甲苯基、氯代亚二甲苯基、和/或氢二亚甲苯基的二聚体。
6.一种通过根据权利要求1-5中任意一项所述的方法得到的由阀用金属组成的涡轮分子泵中的转子。
7.根据权利要求6所述的涡轮分子泵中的转子，其特征在于包括涡轮分子泵的铝或铝合金转子。
8.根据权利要求6或7所述的涡轮分子泵中的转子，其特征在于聚合物的层厚为0.5至15μm。
9.根据权利要求6或7所述的涡轮分子泵中的转子，其特征在于聚合物的层厚为5至10μm。
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