CN106676497A - 热化学气相沉积分离官能化的方法、产品和涂层 - Google Patents

热化学气相沉积分离官能化的方法、产品和涂层 Download PDF

Info

Publication number
CN106676497A
CN106676497A CN201610969416.3A CN201610969416A CN106676497A CN 106676497 A CN106676497 A CN 106676497A CN 201610969416 A CN201610969416 A CN 201610969416A CN 106676497 A CN106676497 A CN 106676497A
Authority
CN
China
Prior art keywords
functionalization
chemical vapor
thermal chemical
product
range
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201610969416.3A
Other languages
English (en)
Inventor
M·袁
P·H·西尔维斯
D·A·史密斯
J·B·马特泽拉
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Silcotek Corp
Original Assignee
Silcotek Corp
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Silcotek Corp filed Critical Silcotek Corp
Publication of CN106676497A publication Critical patent/CN106676497A/zh
Pending legal-status Critical Current

Links

Classifications

    • 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
    • C23C16/455—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 introducing gases into reaction chamber or for modifying gas flows in reaction chamber
    • C23C16/45557—Pulsed pressure or control pressure
    • 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
    • C23C16/52—Controlling or regulating the coating process
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/4505—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements characterised by the method of application
    • C04B41/455—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements characterised by the method of application the coating or impregnating process including a chemical conversion or reaction
    • C04B41/4558—Coating or impregnating involving the chemical conversion of an already applied layer, e.g. obtaining an oxide layer by oxidising an applied metal layer
    • C04B41/456—Coating or impregnating involving the chemical conversion of an already applied layer, e.g. obtaining an oxide layer by oxidising an applied metal layer the conversion only taking place under certain conditions, e.g. avoiding damage of underlaying layers or parts of the substrate
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/52—Multiple coating or impregnating multiple coating or impregnating with the same composition or with compositions only differing in the concentration of the constituents, is classified as single coating or impregnation
    • C04B41/524—Multiple coatings, comprising a coating layer of the same material as a previous coating layer
    • 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
    • C23C16/22—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 deposition of inorganic material, other than metallic material
    • C23C16/24—Deposition of silicon only
    • 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
    • C23C16/22—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 deposition of inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • 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
    • C23C16/22—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 deposition of inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/40—Oxides
    • C23C16/401—Oxides containing silicon
    • 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
    • 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
    • C23C16/4488—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 by in situ generation of reactive gas by chemical or electrochemical reaction
    • 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
    • C23C16/56—After-treatment
    • 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
    • C23C2222/00—Aspects relating to chemical surface treatment of metallic material by reaction of the surface with a reactive medium
    • C23C2222/20—Use of solutions containing silanes

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Inorganic Chemistry (AREA)
  • Ceramic Engineering (AREA)
  • Structural Engineering (AREA)
  • Electrochemistry (AREA)
  • Chemical Vapour Deposition (AREA)

Abstract

本发明公开了一种热化学气相沉积分离官能化的方法，涂层和产品。所述热化学气相沉积分离官能化的方法包括：将制品定位在封闭室内，在第一温度范围内官能化所述制品第一段时间，然后在第二温度范围内进一步官能化所述制品第二段时间。热化学气相沉积分离官能化产品的包括：在第一温度范围内官能化第一段时间的官能作用，和在第二温度范围内进一步官能化第二段时间的进一步官能作用。

Description

热化学气相沉积分离官能化的方法、产品和涂层
技术领域
本发明涉及一种热化学气相沉积方法，和由该方法生产的产品。更具体而言，本发明涉及一种具有多重官能化的方法和产品。
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的不利之处会导致在某些环境中的表面劣化，不能满足某些性能要求，或这些情况的综合。例如，在某些环境中，基材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、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性，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。
样品容器的表面，例如样品圆柱体的内表面，可以与在该样品容器内存储或收集的气体样品相互作用。例如，当含有硫化氢、甲硫醇和硫化羰的气体样品在具有一定内部涂层的样品容器中储存一段时间时，可回收的甲硫醇的量实质上低于原始量。
因此，本领域期望一种热化学气相沉积分离官能化(split-functionalization)的方法，涂层和产品，它们与现有技术相比可以展示出一种或多种改进。
发明内容
在一个实施方案中，热化学气相沉积分离官能化的方法包括：将制品定位在封闭室内，在第一温度范围内官能化该制品第一段时间，然后在第二温度范围内进一步官能化该制品持续第二段时间。
在另一个实施方案中，热化学气相沉积分离官能化的方法包括：将制品定位在封闭室内，在高于二甲基硅烷分解条件的条件下将该制品暴露于二甲基硅烷以产生表面，在封闭室内氧化该制品以产生氧化表面，在第一温度范围内使该氧化表面暴露于三甲基硅烷而被官能化第一段时间；然后在第二温度范围内进一步被官能化第二段时间。第一温度范围和第二温度范围在400℃和500℃的范围内。
在另一个实施方案中，热化学气相沉积分离官能化的产品包括：在第一温度范围内官能化第一段时间的官能作用；和在第二温度范围内进一步官能化第二段时间的进一步官能作用。
本发明的其它特征和优点根据以下的更详细描述是显而易见的，该更详细的描述以示例的方式展示了本发明的原理。
具体实施方式
本发明提供了一种热化学气相沉积(CVD)分离官能化的方法、涂层和产品。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在某些环境中增加对表面劣化的抵抗力、允许降低磨损和其它不期望的表面活动(例如化学吸附、催化活性、氧化、副产品积聚和/或静摩擦)、允许降低或消除与其它分子的催化反应性、允许减少或消除外来物质的侵蚀、允许降低或消除分子崩解、允许减少或消除基材的物理损失、允许较高的甲硫醇回收率、允许在没有辅助非热技术(例如等离子体、射频、催化剂、辐射)或其组合的情况下的涂布。
热CVD产品包括基材和分离官能化的表面，例如基材的表面或涂层。如本发明所使用的，短语“热CVD”是指不包括等离子体辅助技术的热应用。热CVD产品是能够通过热CVD涂布的任何合适制品。分离官能化的表面包括在第一温度范围内官能化第一段时间的官能作用，和在第二温度范围内进一步官能化第二段时间的进一步官能作用。如本发明所用的，术语“官能化(functionalized)”及其语法变体是指端基与表面的键合。
用于生产热CVD分离官能化的产品的合适制品包括但不限于管(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。
这种结构可以是锻造结构、模制结构、附加制造的结构或任何其它合适的结构。在一个实施方案中，表面是或者包括：不锈钢表面(马氏体或奥氏体)、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；和/或等轴晶粒的、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。
在另一个实施方案中，表面由硅烷基材料形成，例如由二甲基硅烷(例如气态形式的)、三甲基硅烷、二烷基甲硅烷基二氢化物、烷基甲硅烷基三氢化物、非自燃物质(例如二烷基甲硅烷基二氢化物和/或烷基甲硅烷基三氢化物)、热反应材料(例如，碳硅烷和/或羧基硅烷，例如非晶碳硅烷和/或非晶羧基硅烷)、能够重组碳硅基的物质(二甲硅烷基或三甲硅烷基片段)，和/或任何其它合适的硅烷基材料。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吹扫(例如，氮气，氦气和/或氩气，作为分压力稀释剂)。这种材料的厚度在100nm和10,000nm之间、在100nm和5000nm之间、在200nm和5000nm之间、在100nm和3000nm之间、在300nm和1500nm之间，或其任何组合、子组合、范围、子范围。
另外，在另外的实施方案中，表面被处理。合适的处理包括但不限于暴露于水(单独，与零空气的或与惰性气体的)、氧气(例如，以至少50重量％的浓度)、空气(例如，单独、不单独、和/或零空气的)、一氧化二氮、臭氧、过氧化物，或其组合。如本发明所用，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％至76％)，并且氧的浓度是至少20重量％(例如，23％至24％)。
根据本发明公开的内容，分离官能化包括通过在一个或两个封闭室和/或容器中使气体热反应来重复改性表面，以在该表面上形成热CVD分离官能化。使用术语“封闭”意在包括静态CVD技术，并且区别于恒流CVD技术。气体选自三甲基硅烷、甲基三甲氧基硅烷、甲基三乙氧基硅烷、二甲基二甲氧基硅烷、二甲基二乙氧基硅烷、三甲基甲氧基硅烷、三甲基乙氧基硅烷，能够在本发明公开的条件下官能化的任何其它气体，及其组合。
在一个实施方案中，分离官能化包括引入合适的有机硅烷试剂。一种合适的有机硅烷试剂是由通式RR’R”Si-H表示的三官能团有机硅烷，其中R，R’，R”是有机官能团。有机官能团的例子是烷基、芳基、卤代烷基和芳基、酮基、醛基、酰基、醇基、环氧基和硝基-有机基团，以及有机金属官能团。在一个实施方案中，有机硅烷是三甲基硅烷。
热CVD分离官能化的方法是在一个或多个温度范围内使气体热反应，而用于官能化和进一步官能化的温度范围是相同的、重叠的或不同的。合适的温度范围包括但不限于在100℃和700℃之间、在100℃和450℃之间、在100℃和300℃之间、在200℃和500℃之间、在300℃和600℃之间、在450℃和700℃之间、700℃、450℃、100℃、在200℃和600℃之间、在300℃和600℃之间、在400℃和500℃之间、300℃、400℃、500℃、600℃，或其任何合适的组合、子组合、范围或子范围。
热CVD分离官能化的方法是在促进气体热反应的一个或多个压力范围内进行，而用于官能化和进一步官能化的压力范围是相同的、重叠的或不同的。合适的压力范围包括但不限于在0.01psia和200psia之间、在1.0psia和100psia之间、在5psia和40psia之间、在20psia和25psia之间、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。
在热CVD方法中使用的封闭室和/或容器的合适尺寸包括但不限于最小宽度是大于5cm、大于10cm、大于20cm、大于30cm、大于100cm、大于300cm、大于1,000cm、10cm至100cm、100cm至300cm、100cm至1,000cm、300cm至1,000cm，任何能够均匀或基本均匀加热的其它最小宽度，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是至少1,000cm3、大于3,000cm3、大于5,000cm3、大于10,000cm3、大于20,000cm3、3,000cm3至5,000cm3、5,000cm3至10,000cm3、5,000cm3至20,000cm3、10,000cm3至20,000cm3，任何能够均匀或基本均匀加热的其它体积，或其任何合适的组合、子组合、范围或子范围。
官能化和进一步官能化的持续时间是相同的，重叠的或不同的范围。在一个实施方案中，(用于官能化)第一段时间的持续时间是至少2小时、至少3小时、至少4小时、至少5小时、至少7小时、4至10小时、6至8小时或其任何合适的组合、子组合、范围或子范围。另外地或可选地，在一个实施方案中，(用于进一步官能化)第二段时间的持续时间比第一段时间短，例如至少1小时、至少2小时、至少3小时、1至5小时、1至4小时，或其任何合适的组合、子组合、范围或子范围。
可理解的，另外的实施方案包括随后的官能化(例如，第三，第四，第五等)和/或沉积(例如，第二，第三，第四等)，其持续时间大于，等于或者小于上述官能化、进一步官能化和/或沉积的持续时间。用于暴露和/或维持的其它合适的持续时间范围包括但不限于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。
通过热CVD分离官能化的方法，甲硫醇的回收率得到明显改善。在一个实施方案中，在初始时间、24小时和48小时的测试中，甲硫醇的回收率的增加是从40％回收率至80％回收率(超过100％的改善，具体地，200％的改善)。具体地，甲硫醇的回收率的这种增加基于硫化氢、甲硫醇和羰基硫气态组分计。
在进一步的实施方案中，热CVD分离官能化的方法在官能化和进一步官能化之前，之后或之间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室排空或基本上排空气体。通常，在热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室之前或之后进行。吹扫气体是氮气、氦气、氩气或任何其它合适的惰性气体。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，或者允许封闭室变为化学惰性环境的任何合适数量的吹扫循环。
热CVD方法的清洁是从基材上去除不需要的材料。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，进一步官能化或其组合包括冷填充操作。例如，在另一实施方案中，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。如本发明所用，短语“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小于30℃、小于60℃、小于100℃、小于150℃、小于200℃、小于250℃、小于300℃、小于350℃、小于400℃、小于440℃、小于450℃、在100℃和300℃之间、在125℃和275℃之间、在200℃和300℃之间、在230℃和270℃之间，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，封闭室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。如本发明所用，短语“超分解温度”是指分解气体明显热分解的条件。封闭室的加热速率是从亚分解温度到超分解温度的任何合适的加热速率。
氧化包括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，氧化是影响涂层体积的本体反应。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，用水作为氧化剂氧化涂层(例如，在100℃至600℃的温度范围内，在300℃至600℃的温度范围内，或在450℃的温度下)。在一个实施方案中，氧化是用空气和水进行的(例如，在100℃至600℃的温度范围内，在300℃至600℃的温度范围内，或在450℃的温度下)。在一个实施方案中，仅用空气氧化(例如，在100℃至600℃的温度范围内，在300℃至600℃的温度范围内，或在450℃的温度下)。在一个实施方案中，氧化是用一氧化二氮(N2O)。具体地，在加热的条件下(例如约450℃)，在基本上纯N2O的压力下，在具有涂布碳硅烷样品的容器中，施加N2O。
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可以理解，在不脱离本发明的范围的情况下，可以进行各种改变并且可以用等同物替代其成分。另外，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，在详细描述中确认的所有数值都应当被解释为其已经明确确认了精确值和近似值。

Claims (20)

1.一种热化学气相沉积分离官能化的方法，包括：
将制品定位在封闭室内；
在第一温度范围内官能化该制品第一段时间；然后
在第二温度范围内进一步官能化该制品第二段时间。
2.根据权利要求1的热化学气相沉积分离官能化的方法，其中第一温度范围不同于第二温度范围，并且第一段时间不同于第二段时间。
3.根据权利要求1的热化学气相沉积分离官能化的方法，其中第一段时间是至少4小时。
4.根据权利要求1的热化学气相沉积分离官能化的方法，其中第二段时间是至少2小时。
5.根据权利要求1的热化学气相沉积分离官能化的方法，其中第一温度范围和第二温度范围均在400℃至500℃的范围内。
6.根据权利要求1的热化学气相沉积分离官能化的方法，其中在第一压力范围内官能化，并且在第二压力范围内进一步官能化，第一压力范围不同于第二压力范围。
7.根据权利要求1的热化学气相沉积分离官能化的方法，其中在第一压力范围内官能化，在第二压力范围内进一步官能化，第一压力范围大于第二压力范围。
8.根据权利要求1的热化学气相沉积分离官能化的方法，其中在第一压力范围内官能化，在第二压力范围内进一步官能化，第一压力范围与第二压力范围相同。
9.根据权利要求1的热化学气相沉积分离官能化的方法，还包括表面官能化所述制品。
10.根据权利要求9的热化学气相沉积分离官能化的方法，其中表面官能化通过将所述制品暴露于三甲基硅烷进行。
11.根据权利要求1的热化学气相沉积分离官能化的方法，其中官能化针对管的内部。
12.根据权利要求1的热化学气相沉积分离官能化的方法，其中所述制品的官能化是针对预先施加在所述制品基材上的表面。
13.根据权利要求12的热化学气相沉积分离官能化的方法，其中所述表面是金属或金属性基材。
14.根据权利要求12的热化学气相沉积分离官能化的方法，其中所述表面是陶瓷基材。
15.根据权利要求1的热化学气相沉积分离官能化的方法，其中所述制品的官能化是针对所述制品的基材。
16.根据权利要求15的热化学气相沉积分离官能化的方法，其中所述基材是金属或金属性基材。
17.根据权利要求1的热化学气相沉积分离官能化的方法，还包括在封闭室内氧化所述制品。
18.根据权利要求1的热化学气相沉积分离官能化的方法，还包括在高于二甲基硅烷分解条件的条件下将所述制品暴露于二甲基硅烷中。
19.一种热化学气相沉积分离官能化的方法，包括：
将制品定位在封闭室内；
在高于二甲基硅烷分解条件的条件下将所述制品暴露于二甲基硅烷中，以产生表面；
在封闭室内氧化所述制品以产生氧化表面；
使所述氧化表面暴露于三甲基硅烷，以在第一温度范围内官能化第一段时间；然后
在第二温度范围内进一步官能化第二段时间；
其中第一温度范围和第二温度范围在400℃和500℃的范围内。
20.一种热化学气相沉积分离官能化的产品，包括：
在第一温度范围内官能化第一段时间的官能作用；和
在第二温度范围内进一步官能化第二段时间的进一步官能作用。
CN201610969416.3A 2015-11-05 2016-11-01 热化学气相沉积分离官能化的方法、产品和涂层 Pending CN106676497A (zh)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US14/933,295 2015-11-05
US14/933,295 US20170130334A1 (en) 2015-11-05 2015-11-05 Thermal chemical vapor deposition split-functionalization process, product, and coating

Publications (1)

Publication Number Publication Date
CN106676497A true CN106676497A (zh) 2017-05-17

Family

ID=57211410

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201610969416.3A Pending CN106676497A (zh) 2015-11-05 2016-11-01 热化学气相沉积分离官能化的方法、产品和涂层

Country Status (6)

Country Link
US (1) US20170130334A1 (zh)
EP (1) EP3165633A1 (zh)
JP (1) JP2017133096A (zh)
KR (1) KR20170053117A (zh)
CN (1) CN106676497A (zh)
AU (1) AU2016253571A1 (zh)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108546927A (zh) * 2018-07-23 2018-09-18 业成科技（成都）有限公司 以化学气相沉积长碳链硅烷化合物作为气密防水之方法

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US10323321B1 (en) * 2016-01-08 2019-06-18 Silcotek Corp. Thermal chemical vapor deposition process and coated article

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6444326B1 (en) * 1999-03-05 2002-09-03 Restek Corporation Surface modification of solid supports through the thermal decomposition and functionalization of silanes
US11292924B2 (en) * 2014-04-08 2022-04-05 Silcotek Corp. Thermal chemical vapor deposition coated article and process

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108546927A (zh) * 2018-07-23 2018-09-18 业成科技（成都）有限公司 以化学气相沉积长碳链硅烷化合物作为气密防水之方法
CN108546927B (zh) * 2018-07-23 2019-12-03 业成科技（成都）有限公司 以化学气相沉积长碳链硅烷化合物作为气密防水之方法

Also Published As

Publication number Publication date
US20170130334A1 (en) 2017-05-11
JP2017133096A (ja) 2017-08-03
KR20170053117A (ko) 2017-05-15
AU2016253571A1 (en) 2017-05-25
EP3165633A1 (en) 2017-05-10

Similar Documents

Publication Publication Date Title
Lommatzsch et al. Plasma polymerization of HMDSO with an atmospheric pressure plasma jet for corrosion protection of aluminum and low‐adhesion surfaces
TW578214B (en) Method of forming oxynitride film or the like and system for carrying out the same
EP2494087B1 (en) Chemical vapor deposition method
US11131020B2 (en) Liquid chromatography system and component
US20110177349A1 (en) Process for the modification of substrate surfaces through the deposition of amorphous silicon layers followed by surface functionalization with organic molecules and functionalized structures
US10487402B2 (en) Coated article
US10851455B2 (en) Silicon-nitride-containing thermal chemical vapor deposition coating
CN106676497A (zh) 热化学气相沉积分离官能化的方法、产品和涂层
US8993063B2 (en) Low-temperature synthesis of silica
US10323321B1 (en) Thermal chemical vapor deposition process and coated article
US20180163308A1 (en) Fluoro-containing thermal chemical vapor deposition process and article
Hähnel et al. Diagnostics of SiOx‐Containing Layers Deposited on Powder Particles by Dielectric Barrier Discharge
Voss et al. Stability of the surface termination of differently modified ultrananocrystalline diamond/amorphous carbon composite films
Emelyanov et al. The gas‐dynamic synthesis of diamond by thermal activation
JP2017150068A (ja) 拡散律速の熱化学気相成長コーティング
US20190218661A1 (en) Spooled arrangement and process of producing a spooled arrangement
US11161324B2 (en) Corrosion-resistant coated article and thermal chemical vapor deposition coating process
US20190136371A1 (en) Molybdenum substrate with an amorphous chemical vapor deposition coating
US20240117495A1 (en) Cold thermal chemical vapor deposition
US11261524B2 (en) Chemical vapor deposition process and coated article
US20170088947A1 (en) Chemical vapor deposition functionalization
KR20190072264A (ko) 플루오로-함유 열화학 기상 증착 방법 및 물품
Sobiecki et al. The use of trimethylaluminum for producing surface layers by the PACVD method
KR20190062427A (ko) 기재의 소수성화 방법
Xiang et al. Parametric study of ACCVD for controlled synthesis of vertically aligned single-walled carbon nanotubes

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
WD01 Invention patent application deemed withdrawn after publication
WD01 Invention patent application deemed withdrawn after publication

Application publication date: 20170517