End-Blocked Silanization of Side-Chain Fluoroalkyl Oligoether and its Surface Properties

2018 ◽  
Vol 71 (11) ◽  
pp. 855
Author(s):  
Lei Wang ◽  
Lei Chen ◽  
Zhanxiong Li

In this study, three novel side-chain fluoroalkyl oligoethers with different molecular weights were synthesised via a ring-opening reaction of 2,2,3,3,4,4,5,5,5-nonafluoropentyloxirane. The fluorooligoethers were then silanized and characterised by FT-IR,1H, and 19F NMR spectroscopies. These silanlized fluorooligoethers were used to fabricate hydrophobic coatings on silicon substrates, which were pre-treated with O2 plasma, by the method of liquid phase deposition. The chemical compositions and structures of the film surfaces were analysed by X-ray photoelectron spectroscopy and the results showed that silanized fluorooligoethers formed self-assembled films on the silicon wafer. The surface wettability of the coatings was measured by water contact angles. It is noted that the annealing process can improve the hydrophobicity with the highest water contact angle being 115.2 ± 1° and hexadecane contact angle being 67.2 ± 1°. The surface morphologies and roughness of the self-assembled films were measured by atomic force microscopy (AFM), as a result, the surface was found to be rougher with the increment of the molecular weight of the fluorooligoethers.

2017 ◽  
Vol 95 (5) ◽  
pp. 605-611 ◽  
Author(s):  
Lei Wang ◽  
Shaoqing Wen ◽  
Zhanxiong Li

A series of novel amphiphilic ABA-type poly(tridecafluorooctylacrylate)-poly(ethylene glycol)-poly(tridecafluorooctylacrylate) (henceforth referred to as p-TDFA-PEG-p-TDFA) triblock oligomers were successfully synthesized via atom transfer radical polymerization (ATRP) using well-defined Br-PEG-Br as macroinitiator and copper as catalyst. The block oligomers were characterized by Fourier transform infrared (FTIR) spectroscopy and 1H and 19F nuclear magnetic resonances (NMR). Gel permeation chromatography (GPC) showed that the block oligomers have been obtained with narrow molecular weight distributions of 1.22–1.33. X-ray photoelectron spectroscopy (XPS) was carried out to confirm the attachment of p-TDFA-PEG-p-TDFA onto the silicon substrate, together with the chemical compositions of p-TDFA-PEG-p-TDFA. The wetabilities of the oligomer films were measured by water contact angles (CAs). Water CAs of p-TDFA-PEG-p-TDFA film were measured and their morphologies were tested by atomic force microscopy (AFM). The result showed that the CAs of the oligomer films, which possess fluoroalkyl groups assembled on the outer surface, increase after heating due to the migration of fluoroalkyl groups and the resulted microphase separation of the p-TDFA-PEG-p-TDFA.


1995 ◽  
Vol 383 ◽  
Author(s):  
M. R. Houston ◽  
R. T. Howe ◽  
K Komvopoulos ◽  
R. Maboudian

ABSTRACTThe surface properties of diamond-like carbon (DLC) films deposited by a vacuum arc technique on smooth silicon wafers are presented with specific emphasis given to stiction reduction in microelectromechanical systems (MEMS). The low deposition temperatures afforded by the vacuum arc technique should allow for easy integration of the DLC films into the current fabrication process of typical surface micromachines by means of a standard lift-off processing technique. Using X-ray photoelectron spectroscopy (XPS), contact angle analysis, and atomic force microscopy (AFM), the surface chemistry, microroughness, hydrophobicity, and adhesion forces of DLC-coated Si(100) surfaces were measured and correlated to the measured water contact angles. DLC films were found to be extremely smooth and possess a water contact angle of 87°, which roughly corresponds to a surface energy of 22 mJ/m2. It is shown that the pull-off forces measured by AFM correlate well with the predicted capillary forces. Pull-off forces are reduced on DLC surfaces by about a factor of five compared to 10 nN pull-off forces measured on the RCA-cleaned silicon surfaces. In the absence of meniscus forces, the overall adhesion force is expected to decrease by over an order of magnitude to the van der Waals attractive force present between two DLC-coated surfaces- To further improve the surface properties of DLC, films were exposed to a fluorine plasma which increased the contact angle to 99° and lowered the pull-off force by approximately 20% over that obtained with as-deposited DLC. The significance of these results is discussed with respect to stiction reduction in micromachines.


Micromachines ◽  
2019 ◽  
Vol 10 (2) ◽  
pp. 121 ◽  
Author(s):  
Jianbing Meng ◽  
Xiaojuan Dong ◽  
Yugang Zhao ◽  
Rufeng Xu ◽  
Xue Bai ◽  
...  

A superhydrophobic surface with low adhesion and good wear resistance was fabricated on Ti6Al4V substrates via TiO2/Ni composite electrodeposition, and subsequently modified with a fluoroalkylsilane (FAS) film. Scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), and optical contact angle measurements were used to characterize the surface morphologies, chemical compositions, and surface wettability. The superhydrophobicity of the as-prepared surface results from the fabrication of a hierarchical structure and the assembly of low-surface energy fluorinated components. The as-prepared surface had a water contact angle as high as 162.6° and a sliding angle close to 1.8°. Scratch and abrasion tests showed that the superhydrophobic coating provided a superior wear resistance and stable mechanical abrasion protection. In addition, the influence of processing conditions, such as working voltage, deposited time, pH value, and TiO2 concentration, was also investigated.


2000 ◽  
Vol 66 (8) ◽  
pp. 3249-3254 ◽  
Author(s):  
Maureen E. Callow ◽  
J. A. Callow ◽  
Linnea K. Ista ◽  
Sarah E. Coleman ◽  
Aleece C. Nolasco ◽  
...  

ABSTRACT We investigated surface selection and adhesion of motile zoospores of a green, macrofouling alga (Enteromorpha) to self-assembled monolayers (SAMs) having a range of wettabilities. The SAMs were formed from alkyl thiols terminated with methyl (CH3) or hydroxyl (OH) groups or mixtures of CH3- and OH-terminated alkyl thiols and were characterized by measuring the advancing contact angles and by X-ray photoelectron spectroscopy. There was a positive correlation between the number of spores that attached to the SAMs and increasing contact angle (hydrophobicity). Moreover, the sizes of the spore groups (adjacent spores touching) were larger on the hydrophobic SAMs. Video microscopy of a patterned arrangement of SAMs showed that more zoospores were engaged in swimming and “searching” above the hydrophobic sectors than above the hydrophilic sectors, suggesting that the cells were able to “sense” that the hydrophobic surfaces were more favorable for settlement. The results are discussed in relation to the attachment of microorganisms to substrata having different wettabilities.


2021 ◽  
Vol 2021 ◽  
pp. 1-11
Author(s):  
Michaela Heier ◽  
Rolf Merz ◽  
Stefan Becker ◽  
Kai Langenbach ◽  
Michael Kopnarski ◽  
...  

Wetting is strongly influenced by adsorbate layers, which are omnipresent on surfaces. The influence of the composition and thickness of adsorbate layers on the water contact angle of sessile drops on different substrates was systematically investigated in the present work. Measurements were carried out for gold-sputtered substrates. These new results are compared to results from a previous study, in which corresponding measurements were carried out for technical steel and titanium substrates. In all experiments, different pretreatments of the samples were used to obtain variations of the adsorbate layer. The samples were either exposed to an oil bath or not, and different cleaning agents were used. The analysis of the adsorbate layer was carried out with X-ray photoelectron spectroscopy (XPS). The results for the different substrates reveal that the water contact angle depends mainly on the composition of the adsorbate layer. The substrate has only an indirect influence, as it influences the composition of the adsorbate layer. The thickness of the adsorbate layers was between 1.4 and 14 nm and was large enough to prevent a direct influence of the substrate on the water contact angle. It is shown that using the information on the adsorbate layer composition from XPS and the results for the water contact angle obtained for the gold samples alone, the water contact angles on the steel and titanium samples can be predicted.


2013 ◽  
Vol 747 ◽  
pp. 178-181 ◽  
Author(s):  
Wasana Kosorn ◽  
Boonlom Thavornyutikarn ◽  
Wanida Janvikul

Polycaprolactone (PCL) was surface modified with alkaline hydrolysis by NaOH and/or low pressure oxygen (O2) plasma treatment. The hydrolysis was conducted in two different stages: one was performed prior to PCL scaffold fabrication by a high pressure supercritical CO2 technique; the other was carried out after the fabrication. The resulting hydrolyzed PCL scaffolds, with pore sizes in the range of 150-250 μm, were denoted as pre-HPCL and post-HPCL, respectively. Both non-hydrolyzed and hydrolyzed PCL scaffolds were subsequently subjected to the plasma treatment, to further enhance the hydrophilicity of the scaffolds. The surface morphology, wettability and chemical composition of all PCL scaffolds were analyzed by scanning electron microscopy (SEM), water contact angle measurement, and X-ray photoelectron spectroscopy (XPS), respectively. It was found that the surface of the scaffolds turned from fairly smooth to highly rough after the hydrolysis and plasma treatment, particularly when both treatments were in use. The post-hydrolysis induced more surface roughness, compared to the pre-hydrolysis. In addition, the water contact angles on the scaffolds enormously reduced after the treatments; plasma treatment, however, showed a more prominent effect than the alkaline hydrolysis. Although expressing a zero-degree contact angle, the plasma-treated pre-HPCL scaffold was wetted more readily than the plasma-treated post-HPCL. These were in good agreement with the XPS results; interestingly, the plasma-treated pre-HPCL scaffold exhibited the greatest O/C atomic ratio among the PCL scaffolds. This indicated its highest extent of PCL chain oxidation, a degradation of ester groups into-COOH and-OH groups.


2019 ◽  
Vol 97 (2) ◽  
pp. 147-153 ◽  
Author(s):  
Lei Chen ◽  
Yanhua Yuan ◽  
Zhanxiong Li

In this study, three types of fluorinated polyacrylates (PBFB, PBFS, and PMFA) were synthesized by 4-gem-bis(2,2,3,3,4,4,5,5,5-nonafluoropentyl)-1-butene, 4-gem-bis(2,2,3,3,4,4,5,5,5-nonafluoropentyl)-methine-1-styrene, and 3,3,4,4,5,5,6,6,6-nonafluorohexyl acrylate, respectively, as monomers via emulsion polymerization. Particle size, particle size distribution, and zeta potential were tested to assess the emulsion stability. Afterwards, the latexes were coated onto fabrics to obtain gem-bis(fluoroalkyl)-cotton. The surface properties of the treated cotton fabrics were analyzed by X-ray photoelectron spectroscopy and water contact angle. It was found that, when controlling the fluorine content level to be similar, the water contact angles of gem-bis(fluoroalkyl)-cottons were 127° ± 0.5° and 134.9° ± 0.7°, respectively, which were both higher than that of mono-fluoroalkyl-cotton (PMFA-cotton of 125.2° ± 0.2°). This showed that gem-bis-fluoroalkyl groups could provide better hydrophobic performance than the mono-fluoroalkyl group, especially when the rigid benzene was used as a side-chain bridged group.


Nanomaterials ◽  
2019 ◽  
Vol 9 (5) ◽  
pp. 706 ◽  
Author(s):  
Chaoqun Wu ◽  
Yudan Zhou ◽  
Haitao Wang ◽  
Jianhua Hu

Zwitterionic polymers are suitable for replacing poly(ethylene glycol) (PEG) polymers because of their better antifouling properties, but zwitterionic polymers have poor mechanical properties, strong water absorption, and their homopolymers should not be used directly. To solve these problems, a reversible-addition fragmentation chain transfer (RAFT) polymerization process was used to prepare copolymers comprised of zwitterionic side chains that were attached to an ITO glass substrate using spin-casting. The presence of 4-vinylpyridine (4VP) and zwitterion chains on these polymer-coated ITO surfaces was confirmed using 1H NMR, FTIR, and GPC analyses, with successful surface functionalization confirmed using water contact angle, X-ray photoelectron spectroscopy (XPS), and atomic force microscopy (AFM) studies. Changes in water contact angles and C/O ratios (XPS) analysis demonstrated that the functionalization of these polymers with β-propiolactone resulted in hydrophilic mixed 4VP/zwitterionic polymers. Protein adsorption and cell attachment assays were used to optimize the ratio of the zwitterionic component to maximize the antifouling properties of the polymer brush surface. This work demonstrated that the antifouling surface coatings could be readily prepared using a “P4VP-modified” method, that is, the functionality of P4VP to modify the prepared zwitterionic polymer. We believe these materials are likely to be useful for the preparation of biomaterials for biosensing and diagnostic applications.


2014 ◽  
Vol 1061-1062 ◽  
pp. 170-174
Author(s):  
Jian Li

The effects of surface treatment of a carbon fiber (CF) by Polyethylene-polyamine (PEPA) on the interfacial adhesion behavior and morphology of polypropylene/polystyrene (PP/PS) matrix blends filled CF composites were investigated. Effects of surface treated a commercial CF on mechanical properties are studied. Contact angle was measured to examine the changes in wettability of the carbon fiber. The chemical and morphological changes were characterized by using X-ray photoelectron spectroscopy (XPS). PP/PS/CF composites were fabricated with and without PEPA treatment, and their interlaminar fracture toughnesses were compared. The results showed that the interlaminar shear strength (ILSS) of composites has been greatly improved filled PEPA modification CF. The water contact angle of resin sample decreased 50% after addition of PEPA surface treated CF.


Polymers ◽  
2021 ◽  
Vol 13 (13) ◽  
pp. 2058
Author(s):  
Kyutae Seo ◽  
Hyo Kang

We synthesized a series of polystyrene derivatives modified with precursors of liquid crystal (LC) molecules via polymer modification reactions. Thereafter, the orientation of the LC molecules on the polymer films, which possess part of the corresponding LC molecular structure, was investigated systematically. The precursors and the corresponding derivatives used in this study include ethyl-p-hydroxybenzoate (homopolymer P2BO and copolymer P2BO#, where # indicates the molar fraction of ethylbenzoate-p-oxymethyl in the side chain (# = 20, 40, 60, and 80)), n-butyl-p-hydroxybenzoate (P4BO), n-hexyl-p-hydroxybenzoate (P6BO), and n-octyl-p-hydroxybenzoate (P8BO). A stable and uniform vertical orientation of LC molecules was observed in LC cells fabricated with P2BO#, with 40 mol% or more ethylbenzoate-p-oxymethyl side groups. In addition, the LC molecules were oriented vertically in LC cells fabricated with homopolymers of P2BO, P4BO, P6BO, and P8BO. The water contact angle on the polymer films can be associated with the vertical orientation of the LC molecules in the LC cells fabricated with the polymer films. For example, vertical LC orientation was observed when the water contact angle of the polymer films was greater than ~86°. Good orientation stability was observed at 150 °C and with 20 J/cm2 of UV irradiation for LC cells fabricated with the P2BO film.


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