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首页> 外文学位 >Deposition of thin organic and metal films from carbon dioxide by free meniscus and solvent displacement methods.
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Deposition of thin organic and metal films from carbon dioxide by free meniscus and solvent displacement methods.

机译：用自由弯月面和溶剂置换法从二氧化碳中沉积有机和金属薄膜。

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This thesis investigates the use of liquid carbon dioxide (1-CO2) and supercritical carbon dioxide (scCO2) as coating solvents to deposit small organic molecules, polymers and metal films. The low cost, low toxicity and unique physical properties of 1-CO2 and scCO2, including extremely low surface tension, low viscosity, and tunable density, make them appropriate coating media to overcome some of the constraints associated with traditional coating methods. Two novel pieces of equipment, a high-pressure free meniscus coating (hFMC) apparatus and an apparatus for film deposition by displacement from two immiscible supercritical phases (DISP), were designed and constructed to produce thin films from CO 2 media. It was demonstrated that highly uniform and ultrathin films of sucrose octaacetate (SOA) and poly[(2-perfluorooctyl)ethyl acrylate] (PFOEA) can be formed on substrates consisting of native oxide of silicon (SiOx) using 1-CO2 hFMC. The films deposited from 1-CO2 were much thinner, more uniform, and exhibited much fewer drying defects and lower surface roughness compared to films from typical organic solvents. The unique surface properties of the PFOEA films from 1-CO2 hFMC were also investigated.; The lack of an interfacial boundary associated with the supercritical state of CO2 does not allow its use in traditional liquid-based coating processes. This drawback can be overcome by introducing a fluid such as supercritical He that is not readily miscible with scCO2 to create an interfacial boundary. It has been demonstrated that particles and films of SOA and PFOEA can be deposited on SiOx from the interfacial boundary between a scCO2 phase and a scHe phase using a solvent displacement (DISP) technique. The films deposited from DISP exhibit unique surface morphologies when compared with the films from 1-CO2 hFMC and the films from normal dip coating with organic solvents.; Even though 1-CO2 and scCO2 have valuable properties as coating media, the poor solvent power of CO2 for most of polymeric materials is a major limitation. This limitation can be overcome by depositing polymeric precursors that are soluble in CO2 followed by subsequent polymerization directly on the surface. Ultrathin fluorinated films with optically clear and chemically resistant characteristics were produced by first depositing photocurable perfluoropolyether (alpha-,o-methacryloxy terminated perfluoropolyether) from 1-CO2 hFMC and subsequently curing the deposited films. This deposition/reaction technique can be also utilized in metal film deposition. Nanosize copper particles and copper films were deposited on SiOx or titanium nitride substrates by first producing Cu (II) hexafluoroacetylacetonate hydrate films from DISP and subsequently reducing them in a hydrogen environment. It also has been demonstrated that palladium catalyzed copper deposition using DISP and subsequent reduction can produce highly uniform and ultrathin Cu films.
机译：本文研究使用液态二氧化碳（1-CO2）和超临界二氧化碳（scCO2）作为涂层溶剂来沉积小的有机分子，聚合物和金属膜。 1-CO2和scCO2的低成本，低毒和独特的物理性能，包括极低的表面张力，低粘度和可调的密度，使其成为合适的涂料介质，可以克服传统涂料方法的某些限制。设计并构造了两种新颖的设备，即高压自由弯月面涂层（hFMC）设备和通过从两个不混溶的超临界相（DISP）置换而沉积膜的设备，可从CO 2介质生产薄膜。结果表明，使用1-CO2 hFMC可以在由硅天然氧化物（SiOx）组成的基板上形成蔗糖八乙酸酯（SOA）和聚[（2-全氟辛基）丙烯酸乙酯]（PFOEA）的高度均匀且超薄的薄膜。与来自典型有机溶剂的薄膜相比，由1-CO2沉积的薄膜更薄，更均匀，并且表现出更少的干燥缺陷和更低的表面粗糙度。还研究了由1-CO2 hFMC制成的PFOEA薄膜的独特表面性能。由于缺乏与超临界状态的CO2相关的界面边界，因此无法将其用于传统的基于液体的涂层工艺中。通过引入不易与scCO2混溶的流体（例如超临界He）来创建界面边界，可以克服此缺点。已经证明，可以使用溶剂置换（DISP）技术从scCO2相和scHe相之间的界面边界将SOA和PFOEA的颗粒和薄膜沉积在SiOx上。与1-CO2 hFMC的膜和常规浸涂有机溶剂的膜相比，DISP沉积的膜表现出独特的表面形态。尽管1-CO2和scCO2作为涂层介质具有宝贵的性能，但大多数聚合物材料中CO2的不良溶剂能力仍然是主要限制。可以通过沉积可溶于CO2的聚合物前体，然后直接在表面上进行聚合来克服此限制。通过首先从1-CO2 hFMC沉积可光固化的全氟聚醚（以α,, o-甲基丙烯酰氧基封端的全氟聚醚），然后固化沉积的膜来生产具有光学透明和耐化学腐蚀特性的超薄氟化膜。该沉积/反应技术也可以用于金属膜沉积中。通过首先从DISP生产六氟乙酰丙酮化铜（II）水合物薄膜，然后在氢气环境中对其进行还原，将纳米尺寸的铜颗粒和铜膜沉积在SiOx或氮化钛基板上。还已经证明，使用DISP进行钯催化的铜沉积以及随后的还原可产生高度均匀且超薄的Cu膜。

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