亲水性无定型TiO_2/SiO_2薄膜及其强化传热性能研究

采用溶胶-凝胶技术在传热管表面涂覆TiO2/SiO2复合溶胶涂层,并通过优化热处理温度和干湿交替处理工艺,提升涂层的亲水性能和强化传热性能。试验结果显示,在热处理温度为200℃时,凝胶涂层以无定型结构为主;热处理试样经过6次干湿交替处理后,即可使表面接触角降低到10°左右;传热管表面较好的润湿性能,可显著提升降膜式换热器的换热效率。     

Fabrication of fluorocarbon terminated DLC thin film using soft X-ray

The control of wettability on a diamond-like carbon (DLC) thin film was carried out by exposing the film to synchrotron radiation (SR) ranging 50–1000 e V under perfluorohexane (C₆F₁₄) gas atmosphere. The contact angle of the DLC surface with a water droplet was found to increase from 73° to 114° by the SR irradiation under C₆F₁₄ gas atmosphere. The chemical components variations of the DLC surface were studied using X-ray photoelectron spectroscopy and the modified DLC film with F was studied using near-edge X-ray absorption fine structure spectroscopy. By mounting the new sample holder for the parallel SR irradiation, we succeeded in preventing secondary reaction of deposited material and controlling the contact angle of the fluorocarbon modified DLC surface.     

Preparation of hydrophobic SiO<Subscript>2</Subscript>@(TiO<Subscript>2</Subscript>/MoS<Subscript>2</Subscript>) composite film and its self-cleaning properties

TiO₂/MoS₂ composite was encapsulated by hydrophobic SiO₂ nanoparticles using a sol–gel hydrothermal method with methyltriethoxysilane (MTES), titanium tetrachloride (TiCl₄), and molybdenum disulfide (MoS₂) as raw materials. Then, a novel dual functional composite film with hydrophobicity and photocatalytic activity was fabricated on a glass substrates via the combination of polydimethylsiloxane adhesives and hydrophobic SiO₂@(TiO₂/MoS₂) composite particles. The influence of the mole ratios of MTES to TiO₂/MoS₂ (M:T) on the wettability and photocatalytic activity of the composite film was discussed. The surface morphology, chemical compositions, and hydrophobicity of the composite film on the glass substrate were investigated by scanning electron microscopy, transmission electron microscopy, X-ray powder diffraction, Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy, and water contact angle (water CA) measurements. The results indicated that the composite film exhibited stable superhydrophobicity and excellent photocatalytic activity for degradation of methyl orange (MO) even after five continuous cycles of photocatalytic reaction when M/T was 7:1. The water CA and degradation efficiency for MO remained at 154° and 94%, respectively. Further, the composite film showed a good non-sticking characteristic with the water sliding angle (SA) at about 4°. The SiO₂@(TiO₂/MoS₂) composite consisting of hydrophobic SiO₂ nanoparticles and TiO₂/MoS₂ heterostructure could provide synergistic effects for maintaining long-term self-cleaning performance.     

Synthesis and characterisation of chemical bath deposited TiO2 thin-films

A series of titania thin films was prepared by chemical bath deposition (CBD) of TiCl₃ on indium tin oxside (ITO) glass at room temperature, followed by calcinations at 500 °C for 4 h. The effect of cyclic deposition on phase composition, microstructure and electrical resistivity of TiO₂ thin films was characterised using X-ray diffraction, scanning electron microscopy and four-point probe respectively. Results showed that TiO₂ films produced by single deposition cycle were amorphous. In contrast, those produced by 5 and 6 deposition cycles were partly amorphous and partly crystalline with the formation of rutile. Both the film thickness and electrical resistivity increased with an increase in the number of deposition cycles.     

A mechanical and modelling study of magnetron sputtered cerium-titanium oxide film coatings on Si (100)

Ce/Ti mixed metal oxide thin films have well known optoelectrical properties amongst several other physio-chemical properties. Changes in the structural and mechanical properties of magnetron sputtered Ce/Ti oxide thin films on Si (100) wafers with different Ce:Ti ratios are investigated experimentally and by modelling. X-ray Photoemission Spectroscopy (XPS) and X-ray diffraction (XRD) confirm the primary phases as trigonal Ce₂O₃ and rutile form of TiO₂ with SiO₂ present in all prepared materials. FESEM imaging delivers information based on the variation of grain size, the mixed Ce/Ti oxides providing much smaller grain sizes in the thin film/substrate composite. Nanoindentation analysis concludes that the pure cerium oxide film has the highest hardness value (20.1?GPa), while the addition of excess titanium oxide decreases the hardness of the film coatings. High temperature in-situ XRD (up to 1000?°C) results indicate high thermal phase stability for all materials studied. The film with Ce:Ti?=?68%:32% has a new additional minor oxide phase above 800?°C. Contact angle experiments suggest that the chemical composition of the surface is insignificant affecting the water contact angle. Results show a narrow band of 87.7–95.7° contact angle. The finite element modelling (FEM) modelling of Ce/Ti thin film coatings based on Si(100); Si(110); silica and steel substrates shows a variation in stress concentration.     

Fabrication of superhydrophobic TiO2 quadrangular nanorod film with self-cleaning,anti-icing properties

Superhydrophobic TiO₂ quadrangular nanorod film was fabricated by hydrothermal reaction and stearic acid modification. X-ray diffractometer and Fourier transform infrared spectrometer were employed to characterize the surface crystal structures and chemical compositions of the superhydrophobic TiO₂ film, respectively. The effects of the titanium source (titanium tetraisopropoxide (TTIP)) amount and reaction time on the morphology and wettability of the TiO₂ film were studied by scanning electron microscope and contact angle meter. The results show that the diameter of the TiO₂ quadrangular nanorods increases and then the water contact angle on modified TiO₂ film decreases with the increase of the reaction time and TTIP amount. Moreover, when the TTIP amount is 0.3?mL and solvent is 30?mL, the wetted state of the superhydrophobic TiO₂ film surface conforms to an improved Cassie model. Besides, the superhydrophobic TiO₂ film shows good low adhesion, self-cleaning and anti-icing properties. Particularly, the anti-icing property decreases with the increase of the reaction time and TTIP amount.     

Growth behavior of titanium dioxide thin films at different precursor temperatures

The hydrophilic TiO₂ films were successfully deposited on slide glass substrates using titanium tetraisopropoxide as a single precursor without carriers or bubbling gases by a metal-organic chemical vapor deposition method. The TiO₂ films were employed by scanning electron microscopy, Fourier transform infrared spectrometry, UV-Visible [UV-Vis] spectroscopy, X-ray diffraction, contact angle measurement, and atomic force microscopy. The temperature of the substrate was 500°C, and the temperatures of the precursor were kept at 75°C (sample A) and 60°C (sample B) during the TiO₂ film growth. The TiO₂ films were characterized by contact angle measurement and UV-Vis spectroscopy. Sample B has a very low contact angle of almost zero due to a superhydrophilic TiO₂ surface, and transmittance is 76.85% at the range of 400 to 700 nm, so this condition is very optimal for hydrophilic TiO₂ film deposition. However, when the temperature of the precursor is lower than 50°C or higher than 75°C, TiO₂ could not be deposited on the substrate and a cloudy TiO₂ film was formed due to the increase of surface roughness, respectively.     

Superhydrophilic Cu-doped TiO2 thin film for solar-driven photocatalysis

Nanosized Cu-doped TiO₂ film was prepared by the sol–gel spin coating technique. XPS analysis showed that Cu atoms had been successfully doped into TiO₂ lattice, which hence modified the surface chemical composition. As a result, the Cu-doped TiO₂ thin film possessed a superhydrophilic surface with a water contact angle (WCA) only 5.1° and exhibited excellent anti-fogging behavior. The Cu-doped TiO₂ thin film also exhibited a much better photocatalytic activity than the reference TiO₂ thin film, as evaluated by the degradation of 10 mg/L methylene blue (MB) solution under simulated solar-driven irradiation.     

Low-temperature fabrication of TiO<Subscript>2</Subscript> film on flexible substrate by atmospheric roll-to-roll CVD

Titanium dioxide (TiO₂) thin film was fabricated using titanium isopropoxide as a precursor through an atmospheric low-temperature roll-to-roll chemical vapor deposition method. TiO₂ was deposited on the PET substrate in the temperature range of room temperature to 100°C, and the working pressure was 740 Torr. The surface morphology of TiO₂ thin film was analyzed by field emission scanning electron microscopy and a 2D surface profiler. The results revealed that the growth rate of TiO₂ film was 31 nm/min at 100°C, and it also showed that the surface is uniform and smooth. Moreover, the lowest root mean square roughness (R _q) value of 1.87 nm was obtained for TiO₂ film prepared at 100°C. The composition of TiO₂ film was confirmed by X-ray photoelectron spectroscopy (XPS) analysis. The film showed very good chemical and optical properties while increasing the substrate deposition temperature. The UV–Vis spectroscopy analysis revealed that TiO₂ films exhibited excellent optical transmittance, more than 91% observed in the visible region.     

Facile fabrication of superhydrophobic polysiloxane/magnetite nanocomposite coatings with electromagnetic shielding property

Superhydrophobic coatings, with a water contact angle (WCA) of 158.3° and a sliding angle of 4.3°, were readily prepared by mixing silicone resin, aminopropyltriethoxysilane and Fe₃O₄ nanoparticles, and subsequently curing at an ambient temperature. The surface wettability, surface morphology and composition, and long-term durability of the coatings were investigated by WCA analysis, field emission scanning electron microscopy, atomic force microscopy, X-ray photoelectron spectroscopy, and QUV accelerated weathering tests, respectively. The results show that the coatings display a pencil hardness of B, excellent weatherability, and electromagnetic shielding effectiveness beyond 60% in the frequency range of 10–3000 MHz.     

The effect of TiO2 morphology on the surface modification of poly (ethylene terephthalate) for electroless plating

In this study, a surface modification of the poly (ethylene terephthalate) (PET) film using TiO₂ photocatalytic treatment was investigated. In order to enhance the adhesion strength between the PET film and the electroless copper film, the effects of TiO₂ crystal forms, TiO₂ particle sizes, and TiO₂ content, as well as treatment condition, upon the surface contact angle, surface characterization, and adhesion strength were investigated. Anatase TiO₂ with a particle size of 5 nm had a high catalytic activity and dispersibility in aqueous solution. After the optimal photocatalytic treatment, the surface contact angle of the PET film decreased from 84.4° to 19.8°, and the surface roughness of the PET film increased from 36 to 117 nm. The adhesion strength between the PET film and the electroless copper film reached 0.89?KN?m^?1. X-ray photoelectron spectroscopy analyses indicated the carbonyl group was formed on the PET surface after photocatalytic treatment, and the surface hydrophilicity was improved. Consequently, TiO₂ photocatalytic treatment is an environmentally friendly and effective method for the surface modification of the PET film.     

Facile synthesis of Sm2S3 diffused nanoflakes and their pseudocapactive behavior

The Sm₂S₃ thin films with diffused nanoflakes morphology are prepared by an environment-friendly facile chemical synthesis method and used in electrochemical supercapacitors. The structural, elemental and surface morphological characterization are carried out using X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), field emission scanning electron microscopy (FESEM) and wettability techniques. The FESEM images show tree root like distribution of flakes with average flake width of about 80 nm. The film surface is lyophilic with propylene carbonate contact angle of 21°. The supercapacitive measurements are carried out through cyclic voltammetry, galvanostatic charge-discharge and electrochemical impedance spectroscopy (EIS) techniques. The Sm₂S₃ film electrode exhibited a highest specific capacitance (C_s) of 213 Fg⁻¹ at 5 mVs⁻¹ scan rate in LiClO₄-propylene carbonate electrolyte. Asymmetric nature of charge–discharge curves confirmed pseudocapacitive behavior of electrode with energy and power densities of 39.39 Whkg⁻¹ and 4.33 kWkg⁻¹, respectively. An equivalent series resistance of 0.44 Ωcm⁻² indicated negligible ohmic losses in charge storage. An electrochemical stability of 81.47% is retained after 1000 cycles indicating that Sm₂S₃ is a promising candidate for supercapacitor application.     

Effect of sputtering parameters on the self-cleaning properties of amorphous titanium dioxide thin films

The aim of this work was to assess the effect of the direct current magnetron sputtering parameters on the photocatalytic activity and photoinduced wettability of amorphous TiO₂ films. TiO₂ films were deposited on glass using the direct current magnetron sputtering technique, without heating, at different total working pressures. Qualitative analysis using in situ X-ray photoelectron spectroscopy confirmed the TiO₂ stoichiometry of the deposited films. Surface structure was studied as a function of working pressure using scanning electron microscopy. The hydrophilicity of the TiO₂ surfaces was investigated macroscopically using measurements of the water contact angle. A threshold working pressure was observed, with a strong dependence on the film thickness. A super hydrophilic surface was observed after less than 1 h of UV irradiation. The photocatalytic activity of the films was evaluated under UV light through the degradation of methylene blue (\(\lambda_{\hbox{max} } \approx 660\;{\text{nm}}\)). The effect of UV irradiation on the photocatalytic activity was rapid, strong, and dependent on film thickness and total working pressure. Fifty percent of organic compounds were photodegraded by films with a thickness of 60 nm deposited at 10 mTorr.     

Photo-Generated Activities of Nanocrystalline TiO<Subscript>2</Subscript> Thin Films

Transparent nanocrystalline TiO₂ thin films with high photocatalytic activity and photo-induced wettability were successfully deposited on a glass slide. Crystal phase transformations and particle size of TiO₂ were investigated. Structural and morphological properties of the films were investigated. The photocatalytic activity of the TiO₂ films was evaluated. It is found that the photocatalytic activity of TiO₂ thin films is significantly decreased by increasing the annealing temperature, which results in a decrease in BET surface area and an increase in crystal size. In addition, increasing film thickness within a certain range significantly improves the photocatalytic activity without causing crack formation of the TiO₂ films. Photocatalytic oxidation and photo-induced wettability conversion on the films were investigated. It is found that photo-induced hydrophilic conversion is observed even on the samples annealed at high temperature. The best photo-generated activities are obtained by optimization of dip-coating cycles and annealing temperatures.     

Experimental investigation on high temperature wettability and structural behaviour of SAW fluxes using MgO–TiO2–SiO2 and Al2O3–MgO–SiO2 flux system

To establish the relationship between wettability and structure with the change in SAW flux composition, the contact angle measurement study was performed at 1700 K. For MgO–TiO₂–SiO₂ and Al₂O₃–MgO–SiO₂ flux system the wetting behaviour was studied by evaluating the contact angle as well as surface tension properties. Sessile drop method was used to determine the wetting properties of SAW fluxes. Twenty-one SAW fluxes were designed & developed by applying mixture design approach of design of experiments. Chemical, phase and structural properties of SAW fluxes were measured using modern techniques such as X-ray fluorescence (XRF), X-ray diffraction (XRD) & Fourier Transform Infra-red spectroscopy (FTIR). As per the calculated contact angle value, different surface tension values for MgO–TiO₂–SiO₂ and Al₂O₃–MgO–SiO₂ flux system was calculated using Young's & Boni's equations. Using Dupre's equation the adhesion energy for twenty-one basic fluxes was also calculated. Measured contact angle value increased with increase in the TiO₂/MgO & TiO₂/Al₂O₃ flux ratio. Lower contact angle gives higher wettability between the flux and the heating substrate. With increase of TiO₂/SiO₂ ratio up to 1.5 to 2.0 the calculated surface tension value is decreasing while after that it is increased with increase in TiO₂/SiO₂ ratio.     

Effects of surface modification by Ar+ irradiation on wettability of surfaces of poly(ethylene terephthalate) films

Surfaces of poly(ethylene terephthalate); PET, films were irradiated with Ar⁺ at 1 keV using various ion doses (ID) from 10¹⁴ to 10¹⁷ ions/cm² (isc) with and without an O₂ environment. The wettability of the modified surfaces of PET was determined by measuring the contact angle between water droplets and the modified surfaces. The modified surfaces were also characterized by AFM (atomic force microscopy) and XPS (X-ray photoelectron spectroscopy) for changes in the surface morphology, and the chemical composition and molecular structure, respectively. The contact angle decreased from 70° for unmodified surfaces to 45° for modified surface with ID = 10¹⁴ isc without O₂ and remained relatively constant with higher ID. The contact angle, however, reached a minimum value of 8° for modified surfaces with ID = 10¹⁶ isc with O₂. The improved wettability may be due to a combination of the formation of hydrophilic groups, chemical and molecular structural changes, physical structural or morphological changes, and increased roughness of the surface. The wettability of the modified surfaces also depended on the time of exposure to air. The wettability worsened with exposure time to air, but was revived by immersing the films into water. Possible mechanisms for the change of the wettability of the modified surfaces are given.     

Effect of rapid thermal annealing on the structural and electrical properties of TiO2 thin films prepared by plasma enhanced CVD

Titanium oxide thin films were deposited on p-type Si(100), SiO₂/Si, and Pt/Si substrates by plasma enhanced chemical vapor deposition using high purity Ti(O-i-C₃H₇)₄ and oxygen. As-deposited amorphous TiO₂ thin films were treated by rapid thermal annealing (RTA) in oxygen ambient, and the effects of RTA conditions on the structural and electrical properties of TiO₂ films were studied in terms of crystallinity, microstructure, current leakage, and dielectric constant. The dominant crystalline structures after 600 and 800 ‡C annealing were an anatase phase for the TiO₂ film on SiO₂/Si and a rutile phase for the film on a Pt/Si substrate. The dielectric constant of the as-grown and annealed TiO₂ thin films increased depending on the substrate in the order of Si, SiO₂/Si, and Pt/ Si. The SiO₂ thin layer was effective in preventing the formation of titanium silicide at the interface and current leakage of the film. TEM photographs showed an additional growth of SiO_x from oxygen supplied from both SiO₂ and TiO₂ films when the films were annealed at 1000 ‡C in an oxygen ambient. Intensity analysis of Raman peaks also indicated that optimizing the oxygen concentration and the annealing time is critical for growing a TiO₂ film having high dielectric and low current leakage characteristics.     

Reversible Photocontrol of Wood-Surface Wettability Between Superhydrophilicity and Superhydrophobicity Based on a TiO2 Film

The reversible photocontrol of wood-surface wettability between superhydrophilicity and superhydrophobicity based on a TiO₂ film modified with octadecyl trichlorosilane (OTS) was achieved via a facile hydrothermal method at low temperature. Under UV illumination, the wood surface became superhydrophilic with a water contact angle (WCA) of approximately 0°. However, when placed in the dark, a superhydrophobic wood surface with a WCA of approximately 152° was achieved. The mechanism of the reversible photocontrol of wood-surface wettability is discussed in this article. This photocontrolled wood surface may have potential for wood self-cleaning or manipulation in response to indoor humidity.     

Ag-TiO2多孔薄膜及其非紫外光辐照下的超亲水特性

采用溶胶凝胶法，以钛酸丁酯为前驱体、硝酸银络合物为银源、聚乙二醇2000（PEG2000）作为结构导向剂，制备超亲水多孔Ag-TiO₂复合薄膜。用X射线衍射仪、X射线光电子能谱仪、扫描电镜、原子力显微镜表征薄膜晶相结构、化学成分以及表面形貌。根据静态水接触角、动态润湿时间、超亲水长效稳定性综合评价不同Ag含量及PEG2000添加量薄膜的超亲水性能。研究发现，掺杂Ag与PEG2000对薄膜在非紫外光下的超亲水特性具有协同作用，掺杂Ag明显提高薄膜动态润湿速度及可见光响应，表面粗糙多孔结构有利于避光条件下的长效超亲水特性。Ag含量10%、PEG2000掺杂量5%的Ag-TiO₂复合薄膜在自然光条件下已具备优良的超亲水性能；水滴0.2 s内即可在表面完全铺展到0°；避光条件下保存，超亲水时效性可达到30 d以上。在可见光活化下即可强化超亲水性能，具有良好的防雾效果。     

Improved performance of dense TiO2/CdSe coupled thin films by low temperature process

Dense TiO₂ and TiO₂/CdSe coupled nanocrystalline thin films were synthesized onto ITO coated glass substrate by chemical route at relatively low temperature (≤100 °C). TiO₂ films were nanocrystalline and crystallinity disappears after CdSe deposition as evidenced by X-ray powder diffraction. Surface morphology and physical appearance of films were studied from SEM and actual photo-images, reveals dense nature of TiO₂ (10-12 nm spherical grains, faint violet) and CdSe (80-90 nm spherical grains, deep brown), respectively. Presence of two absorption edges in UV spectra implies existence of separate phases rather than composite formation. TiO₂ film was found to have higher water contact angle (71°) than TiO₂/CdSe (61°) and CdSe (56°). I-V and stability tests of photo-electrochemical cells were performed with TiO₂ and TiO₂/CdSe film electrodes (under light of illumination intensity 80 mW/cm²) in lithium iodide as an electrolyte using two-electrode system.