CN107043923A - 含氮化硅的热化学气相沉积涂层 - Google Patents
含氮化硅的热化学气相沉积涂层 Download PDFInfo
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Abstract
本发明公开了具有含氮化硅的热化学气相沉积涂层的表面、制品和方法。方法包括在腔室内的表面上制备含氮化硅的热化学气相沉积涂层。在所述表面上制备含氮化硅的热化学气相沉积涂层的过程中,流入和流出所述腔室是受限的或暂停的。表面包含含氮化硅的热化学气相沉积涂层。所述表面至少具有被遮挡而无法看见的隐蔽部分。制品包含在腔室内的表面上的含氮化硅的热化学气相沉积涂层。所述表面至少具有被遮挡而无法看见的隐蔽部分。
Description
技术领域
本发明涉及含氮化硅的热化学气相沉积涂层。更具体而言,本发明涉及与这样的涂层相关的表面、制品和方法。
背景技术
通常,基材的表面不具有期望的性能特征。不具有特定期望的性能特征会导致在某些环境中的表面劣化,不能满足某些性能要求,或这些情况的组合。例如,在某些环境中,金属、玻璃和陶瓷表面可能会经受磨损和其它不期望的表面活动如化学吸附、催化活性、腐蚀侵蚀、氧化、副产品积聚或静摩擦,和/或其它不期望的表面活动。
不期望的表面活动会引起其它分子的化学吸附、其它分子的可逆和不可逆的物理吸附、与其它分子的催化反应、外来物质的侵蚀、表面的分子崩解、基材的物理损失或其组合。
为了提供某些所需的性能特性,涂料可通过各种涂覆沉积技术施用至表面,以赋予其更好的耐腐蚀性、改进的化学惰性、更好的耐磨性和增强的抗摩擦特性。这些技术可包括浸涂、喷涂、旋涂、印刷、电镀和/或物理气相沉积(PVD)。浸涂、喷涂、旋涂、印刷、电镀和PVD可限于特定的表面和/或不能提供准确的三维涂覆能力。例如,管内表面的涂覆可尤其是成问题的,因为涂料可累积在管的入口,在整个管中,涂层可具有不同的厚度,和/或所述施用方法不能将涂料施用在管内。
化学气相沉积通过将材料在高于该材料的热分解温度的温度下进行沉积已被用于制备具有改进特性的涂层。然而,还需要进一步的改进。
在本领域中,期望一种与现有技术相比显示出一项或多项改进的表面、制品和方法。
发明内容
在一个实施方案中,方法包括在腔室内的表面上制备含氮化硅的热化学气相沉积涂层。在所述表面上制备含氮化硅的热化学气相沉积涂层的过程中,流入和流出所述腔室是受限的或暂停的。
在另一个实施方案中,表面包括含氮化硅的热化学气相沉积涂层。所述表面至少具有被遮挡而无法看见的隐蔽部分。
在另一个实施方案中,制品包括在腔室内的表面上的含氮化硅的热化学气相沉积涂层。所述表面至少具有被遮挡而无法看见的隐蔽部位。
本发明的其他特征和优点根据以下更详细的描述并结合附图是明白易懂的,该更详细的描述和附图以示例的方式阐述了本发明的原理。
附图说明
图1为在本发明公开的一个实施方案中的方法中所用的化学气相沉积体系的透视图。
在整个附图中,尽可能采用相同的附图标记代表相同的部位。
具体实施方式
本发明提供了一种具有含氮化硅的热化学气相沉积(CVD)涂层的表面、制品和方法。例如,与不包括本发明公开的一个或多个特征的概念相比,本发明公开的实施方案允许下述效果:改进的耐腐蚀性、更好的耐磨性、增强的化学惰性、提高的抗静摩擦特性以及对于具有复杂几何形状的物体而言准确的三维涂覆能力,或者允许其效果的组合。
根据一个实施方案,所述方法包括:在CVD体系100的封闭CVD腔室105和/或封闭CVD容器111内,在制品102的表面103上制备含氮化硅的热CVD涂层101。如本文中所使用的,术语“热CVD”是指不包括非热能量源的热应用,所述非热能量源为例如光能、等离子体、动能和/或化学能辅助技术。
在一个实施方案中,在表面103上制备含氮化硅的热CVD涂层101的过程中,流入CVD腔室104且从封闭CVD腔室105和/或封闭CVD容器111流过流出物路径119的过程是受限的或暂停的,例如,使得所述方法作为一种静态热CVD技术区别于用于视线(line-of-sight)沉积的流过型(flow-through)方法。
在热CVD方法中使用的封闭CVD腔室105和/或封闭CVD容器111的合适尺寸包括但不限于,最小宽度为大于5cm、大于10cm、大于20cm、大于30cm、大于100cm、大于300cm、大于1000cm、10cm至100cm、100cm至300cm、100cm至1000cm、300cm至1000cm,任何能够均匀或基本均匀加热的其他最小宽度,或其任何合适的组合、子组合、范围或子范围。合适的体积包括但不限于,至少1000cm3、大于3000cm3、大于5000cm3、大于10000cm3、大于20000cm3、3000cm3至5000cm3、5000cm3至10000cm3、5000cm3至20000cm3、10000cm3至20000cm3,任何能够均匀或基本均匀加热的其他体积,或其任何合适的组合、子组合、范围或子范围。
含氮化硅的热CVD涂层101通过将一种或多种合适的含氮物质107和/或含硅物质109引入封闭CVD腔室105和/或位于封闭CVD腔室105内的封闭容器111中而制备。合适的含氮物质包括但不限于氨、氮、肼、任何其他合适的物质及其组合。合适的含硅物质包括但不限于硅烷、三甲硅烷基胺(也称为TSA;硅烷胺;N,N-二甲硅烷基-二硅氮烷;2-甲硅烷基-;硅烷、次氨基三;或3SA)、双(叔丁基氨基)硅烷、1,2-双(二甲基氨基)四甲基二硅烷、二氯硅烷、六氯二硅烷、任何其他合适的物质及其组合。在引入多于一种物质的实施方案中,这些物质同时或相继(先引入任一物质)引入。
在一个实施方案中,所述物质的引入产生包含纯或基本上纯的氮化硅、氧氮化硅、一个或多个官能化层或其组合的含氮化硅的热CVD涂层101。如本文中所使用的,术语“官能化(functionalized)”及其语法变体是指端基与表面的键合。
在其他实施方案中,包括一个或多个额外的含氮化硅的热CVD涂层113。这种额外的含氮化硅的热CVD涂层113的厚度大于、小于或基本上等于含氮化硅的热CVD涂层101的厚度,例如为至少100nm、200nm、50至500nm,或其任何合适的组合、子组合、范围或子范围。所述额外的含氮化硅的热CVD涂层113可具有在本文中参考含氮化硅的热CVD涂层101所述的任何特性或特征。
热CVD在允许形成所需特性如提高的压缩性/密度的任何合适的条件下进行。合适的温度范围包括但不限于100℃至700℃、100℃至450℃、100℃至300℃、200℃至500℃、300℃至600℃、325℃至600℃、450℃至600℃、550℃至600℃、450℃至700℃、700℃、450℃、100℃、200℃至600℃、300℃至600℃、400℃至500℃、300℃、400℃、500℃、600℃,或其任何合适的组合、子组合、范围或子范围。
合适的压力范围包括但不限于0.01psia至200psia、1.0psia至100psia、5psia至40psia、20psia至25psia、大于25psia、大于20psia、小于20psia、小于15psia、1.0psia、5psia、20psia、23psia、25psia、40psia、100psia、200psia,或其任何合适的组合、子组合、范围或子范围。
为了获得所需压力,在一个实施方案中,含氮物质107(例如氨)的引入包括:当封闭CVD腔室105和/或封闭CVD容器111处于第一选定压力(例如0.0001psia至10psia)时,打开与包括含氮物质107的第一容器117(例如圆柱状物)连接的第一流量控制装置115,然后当封闭CVD腔室105和/或封闭CVD容器111内的压力处于第二选定压力(例如0.01psia至50psia)时,关闭和/或限制在第一流量控制装置115中的流动。
在一个实施方案中,重复(例如反复地)引入含氮物质107和/或含硅物质109的顺序,以获得在CVD涂层101内的硅和氮的所需比例。此外或可选地,在一个实施方案中,含氮物质107和含硅物质109例如通过使用平行填充方式、预混合方式(例如包括在引入至CVD容器111之前以预定比例混合前体的配置)或其组合而同时引入。
此外或可选地,在另一个实施方案中,含硅物质109(例如三甲硅烷基胺)的引入包括:当封闭CVD腔室105和/或封闭CVD容器111处于第三选定压力(例如0.01psia至10psia)时,打开与包括含硅物质109的第二容器123(例如圆柱状物)连接的第二流量控制装置121,然后当封闭CVD腔室105和/或封闭CVD容器111内的压力处于第四选定压力(例如0.01psia至50psia)时,关闭和/或限制在第二流量控制装置121中的流动。
合适的持续时间(例如,在引入开始之后、在引入完成之后或在引入的开始和完成之间,但在允许或促进排空CVD腔室105之前)允许形成CVD涂层101的所需特性。这样合适的持续时间包括但不限于10分钟至24小时、1小时至10小时、2小时至10小时、4小时至6小时、4小时至8小时、至少10分钟、至少1小时、至少4小时、至少10小时、小于10小时、小于8小时、小于6小时、小于4小时,或其任何合适的组合、子组合、范围或子范围。
在一个实施方案中,含氮化硅的热CVD涂层101为或包含通过在合适的条件下氧化制备的氧化涂层。合适的条件包括但不限于在预定氧化条件下暴露于能够将活性氧物质供给到涂层中的任何合适的化学物质。通常,氧化是影响涂层主体的本体反应。用于氧化的合适化学物质包括例如水、氧气、空气、一氧化二氮、臭氧、过氧化物及其组合。在一个实施方案中,用水作为氧化剂进行氧化(例如,在100℃至600℃的温度范围内,在300℃至600℃的温度范围内,或在325℃或450℃的温度下)。在一个实施方案中,用空气和水进行氧化(例如,在100℃至600℃的温度范围内、在300℃至600℃的温度范围内,或在325℃或450℃的温度下)。在一个实施方案中,仅用空气进行氧化(例如,在100℃至600℃的温度范围内、在300℃至600℃的温度范围内,或在325℃或450℃的温度下)。在一个实施方案中,用一氧化二氮(N2O)进行氧化。具体地,在加热(例如约325℃或450℃)条件下,在基本上纯N2O的压力下,在具有涂覆碳硅烷样品的容器中,施用N2O。
这样的材料可以反复使用,和/或在两次使用之间采用例如惰性气体(例如,氮气、氦气和/或氩气,作为分压力稀释剂)吹扫。这种材料的厚度为100nm至10000nm、100nm至5000nm、200nm至5000nm、100nm至3000nm、300nm至1500nm,或其任何组合、子组合、范围或子范围。
此外,在其他实施方案中,处理表面103。合适的处理包括但不限于暴露于水(单独的,含有零空气或含有惰性气体的)、氧气(例如,在至少50重量%的浓度下)、空气(例如,单独、非单独和/或零空气的)、一氧化二氮、臭氧、过氧化物,或其组合。如本文中所使用的,术语“零空气”是指具有小于0.1ppm总烃的大气空气。术语“空气”通常是指在重量上主要为氮气的气态流体,其中氧气是浓度第二高的物质。例如,在一个实施方案中,氮的浓度是至少70重量%(例如,75重量%至76重量%),并且氧的浓度是至少20重量%(例如,23重量%至24重量%)。
在其他实施方案中,热CVD方法包括任何合适的附加步骤。合适的附加步骤包括但不限于清洗、吹扫、预沉积处理(例如,加热基材和/或冷填充),和/或氧化(例如,引入氧化剂)。
热CVD方法的吹扫是从封闭CVD腔室105和/或封闭CVD容器111排空或基本上排空气体。通常,热CVD方法的任何部分都可以在选择性地施加吹扫气体至封闭CVD腔室105和/或封闭CVD容器111之前或之后进行。吹扫气体是氮气、氦气、氩气或任何其他合适的惰性气体。吹扫是一个吹扫循环、两个吹扫循环、三个吹扫循环、多于三个吹扫循环,或允许封闭CVD腔室105和/或封闭CVD容器111变为化学惰性环境的任何合适数量的吹扫循环。
热CVD方法的清洁是从表面103上除去不需要的材料。通常,CVD方法的任何部分都可以在该清洁之前或之后进行。
在一个实施方案中,预沉积处理、官能化或其组合包括冷填充操作。例如,在另一个实施方案中,在预沉积处理期间的冷填充操作包括在低于所要分解气体的热分解温度的亚分解温度下引入分解气体。如本文中所用的,术语“亚分解温度”是指分解气体不会明显热分解的条件。根据所使用的物质,合适的冷填充操作温度包括但不限于低于30℃、低于60℃、低于100℃、低于150℃、低于200℃、低于250℃、低于300℃、低于350℃、低于400℃、低于440℃、低于450℃、100℃至300℃、125℃至275℃、200℃至300℃、230℃至270℃,或其任何合适的组合、子组合、范围或子范围。
在引入分解气体期间和/或之后,封闭CVD腔室105和/或封闭CVD容器111的操作包括加热至等于或高于所要分解气体的热分解温度的超分解温度。如本文中所用的,术语“超分解温度”是指分解气体明显热分解的条件。封闭CVD腔室105和/或封闭CVD容器111的加热是在从亚分解温度到超分解温度的任何合适的加热速率下进行的。
在一个实施方案中,接收含氮化硅的热CVD涂层101的制品102为或包括但不限于管(例如,内表面和/或外表面)、平面几何结构、非平面几何结构、复杂几何结构、金属性结构、金属结构和/或陶瓷结构。在一个实施方案中,制品102包括位于被遮挡而无法看见的隐蔽部分106(例如,该部分不能通过视线技术接收涂料)上的含氮化硅的热CVD涂层101。
具体的实施方案包括制品102为下述的一种或多种:配件(例如,管接头、连接器、适配器、两个或多个管的其他连接物如能够具有无泄漏的或基本上无泄漏的密封件)、螺纹管件(例如,套管如前套管和后套管)、管(例如,松散的或绑紧的连续管,如在金属线轴中,用防水夹套组装并密封,预弯的、直的和/或易弯曲的)、阀门(例如,具有破裂片、转子、多位置构型、大于5000psia的压力等级、按钮的把手或把柄、球柄零件、球阀零件、止回阀零件、弹簧、多个实体、密封件、针阀零件、密封垫圈和/或柄)、快速连接件、圆柱体样品、调节器和/或流量控制器(例如,包括O型环、密封件和/或隔膜)、注入口(例如,用于气相色谱仪)、串联过滤器(例如,包括弹簧、扳手平坦部、网筛和/或焊接件)、玻璃衬里、气相色谱仪组件、试样探针、控制探针(例如,包括盒子、抽吸管、抽吸过滤器和/或稀释盒)、井下取样容器,或其组合。
制品102可为锻造结构、模制结构、附加制造的结构或任何其他合适的结构。在一个实施方案中,表面103是或包括:不锈钢表面(马氏体或奥氏体的)、镍基合金、金属表面、金属性表面(铁的或非铁的;回火或非回火的;和/或等轴的、定向凝固的或单晶的)、陶瓷表面、陶瓷基复合材料表面、玻璃表面、陶瓷基复合材料表面、复合金属表面、涂布的表面、纤维表面、箔表面、膜、聚合物表面(例如聚醚醚酮),和/或能够承受热CVD方法的操作条件的任何其它合适表面。在其他实施方案中,所述结构中Cu的浓度为26至34重量%,和/或Ni的浓度为50至67重量%。
虽然已经参考一个或多个实施方案描述了本发明,但是本领域技术人员应理解,在不脱离本发明范围的情况下,可以进行各种改变并且可以用等同物替代其成分。此外,在不脱离本发明的实质范围的情况下,可以进行许多修改以使特定的情况或材料适应本发明的教导。因此,本发明不限于作为实施本发明的最佳模式公开的特定实施方案,而是本发明将包括落入所附权利要求范围内的所有实施方案。此外,在详细描述中的所有数值都应当被解释为精确值和近似值均已明确包括。
Claims (19)
1.一种方法,包括:
在腔室内的表面上制备含氮化硅的热化学气相沉积涂层;
其中,在所述表面上制备含氮化硅的热化学气相沉积涂层的过程中,流入和流出所述腔室是受限的或暂停的。
2.权利要求1的方法,其中制备过程包括将三甲硅烷基胺引入所述腔室中。
3.权利要求2的方法,其中三甲硅烷基胺的引入包括:当所述腔室处于第一压力时,打开与包含所述三甲硅烷基胺的容器连接的流量控制装置,然后当所述腔室内的压力处于第二压力时,闭合流量控制装置,第一压力与第二压力不同。
4.权利要求2的方法,其中制备过程还包括在引入三甲硅烷基胺的同时,将氨引入所述腔室中。
5.权利要求2的方法,其中制备过程还包括在引入三甲硅烷基胺之前,将氨引入所述腔室中。
6.权利要求2的方法,其中制备过程还包括在引入三甲硅烷基胺之后,将氨引入所述腔室中。
7.权利要求2的方法,其中引入过程包括:当所述腔室处于第一压力时,打开与包含所述胺的容器连接的流量控制装置,然后当所述腔室内的压力处于第二压力时,闭合流量控制装置,第一压力与第二压力不同。
8.权利要求1的方法,其中制备过程在至少325℃的温度下进行。
9.权利要求1的方法,其中制备过程包括氧化,所述氧化在至少300℃的温度下进行。
10.权利要求1的方法,其中所述含氮化硅的热化学气相沉积涂层是纯的或基本上纯的氮化硅。
11.权利要求1的方法,其中所述含氮化硅的热化学气相沉积涂层包括氧氮化硅。
12.权利要求1的方法,其中所述含氮化硅的热化学气相沉积涂层是官能化的。
13.权利要求1的方法,其还包括在所述含氮化硅的热化学气相沉积涂层上制备额外的含氮化硅的热化学气相沉积涂层。
14.权利要求13的方法,其中所述额外的含氮化硅的热化学气相沉积涂层具有第一厚度且所述含氮化硅的热化学气相沉积涂层具有第二厚度,第一厚度和第二厚度不同。
15.权利要求1的方法,其中所述表面是金属的或金属性的。
16.权利要求1的方法,其中所述表面至少具有被遮挡而无法看见的隐蔽部分。
17.通过权利要求1的方法制备的表面。
18.一种表面,其包含含氮化硅的热化学气相沉积涂层,其中所述表面至少具有被遮挡而无法看见的隐蔽部分。
19.一种制品,包含:
在腔室内的表面上的含氮化硅的热化学气相沉积涂层;
其中所述表面至少具有被遮挡而无法看见的隐蔽部分。
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EP3192894A1 (en) | 2017-07-19 |
US10851455B2 (en) | 2020-12-01 |
US20190003044A1 (en) | 2019-01-03 |
US10087521B2 (en) | 2018-10-02 |
US20170167015A1 (en) | 2017-06-15 |
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