Drying process in a solvent-based paint analyzed by phase-shifting digital holography and an estimation of time for tack free

A technique to study the drying of paints, based on phase-shifting digital holography, is presented. The technique is applied to the drying process of solvent-based paint on a three-dimensional surface at different substrate temperatures. For processing the data, a cross-correlation function and phase change derived from reconstructed complex amplitudes are calculated to visualize and to evaluate the local variations in the dryness of paint. The relationship between the optical signal obtained by the holographic method and the actual microscopic variations occurring in the paint film is also investigated using the gravimetric technique and a microscope. It is shown that the holographic technique can determine the stationary state of a painted surface corresponding to the end of the falling rate period in the drying process. The holographic technique detects mainly the activity on the surface and is applicable to assessment of the early drying process of paint.     

Improvement of minimum paint film thickness for THz paint meters by multiple-regression analysis

We propose a numerical parameter fitting method to determine the time delay between two temporally overlapped echo pulses in terahertz (THz) tomography measurements. The method is based on multiple-regression analysis with the least-squares method and is applied to decrease the minimum paint film thickness for THz paint meters. Applying multiple-regression analysis to paint thickness measurements is five times more sensitive with regard to the minimum thickness than numerical Fourier deconvolution. We apply the proposed method to determine the optical thickness, geometrical thickness, and group refractive index of dry paint film and wet paint film. The proposed method is useful for decreasing the minimum thickness for a THz paint meter and other THz tomography measurements.     

Terahertz paintmeter for noncontact monitoring of thickness and drying progress in paint film

We propose a paintmeter for noncontact and remote monitoring of the thickness and drying progress of a paint film based on the time-of-flight measurement of the echo signal of a terahertz (THz) electromagnetic pulse. The proposed method is effectively applied to two-dimensional mapping of the painting thickness distribution for single-layer and multilayer paint films. Furthermore, adequate parameters for the drying progress are extracted from the THz pulse-echo signal and effectively applied to monitor the wet-to-dry transformation. The THz paintmeter can be a powerful tool for quality control of the paint film on the in-process monitoring of car body painting.     

Preparation and characterisation of thickness dependent nano-structured ZnS thin films by sol–gel technique

Zinc sulfide (ZnS) thin films of different thickness were coated on glass substrates by the sol–gel dip-coating technique. Thickness dependent structural and optical properties of the films were studied in detail. X-ray diffraction (XRD) analysis indicated that the films had mixture of cubic (β) and hexagonal (α) phases with cubic (β) phase being predominant. Scanning electron microscope (SEM) showed that the film surfaces were smooth and crack free. Energy dispersive X-ray (EDX) measurement showed no impurity in the ZnS compound with elemental concentration of Zn/S being 50.38/49.62. Optical measurements showed that optical transmittance of the films were decreased in the visible range as the film thickness increased and band gap of the thin films were estimated to be about 3.61, 3.56, and 3.39?eV for the films with thickness of 100, 220, and 360?nm, respectively. Reactive indices and extinction coefficients of the films were measured by Spectroscopic Ellipsometer. Both the refractive index (n) and extinction coefficient (k) of the films were increased as the film thickness decreased. Electrical measurements showed that the resistivity of the films were decreased as the substrate temperature and film thickness increased.     

新型表面可修饰性有机硅密封材料的制备及应用

制备了一种单组分室温硫化表面可修饰性有机硅密封材料。在通用的酮肟型有机硅密封材料组分中,添加自制的含有氰基、仲胺基的硅烷改性剂,可明显改善油溶性醇酸漆和聚氨酯漆对有机硅密封材料的可涂覆性及储存稳定性。添加甲基丙烯酰丙基三甲氧基硅烷,同时在水溶性丙烯酸乳胶漆中添加适量的硅丙乳胶,可显著改善水性丙烯酸乳胶漆对有机硅密封材料的表面可修饰性。表面可修饰性有机硅密封材料可用作普通有机硅密封胶的底涂。     

Photocatalytic oxidation of alkyd paint films measured by FTIR analysis of UV generated carbon dioxide

FTIR assay of UV generated gaseous CO₂ has been used to monitor the photo-degradation of alkyd paint films in oxygen of controlled humidity. The three contributions to CO₂ evolution from such paint films are (a) a dark reaction associated with the drying process, (b) direct photochemical reaction, and (c) photocatalysis by the TiO₂ opacifier. As this paper is focused on the photocatalysis by TiO₂, the dark reaction has been minimized by accelerated drying of the paint films and the photocatalytic component has been emphasised by studying films pigmented with TiO₂ that has not been surface treated. This methodology allows the UV stability of alkyd paints to be monitored rapidly by an FTIR measurement of the UV-generated carbon dioxide. CO₂ evolution was greater for films made with high (35%) than for low (15%) TiO₂ pigment volume concentration (p.v.c.) paints. This behaviour, which parallels weight losses from similar films exposed in conventional accelerated weathering equipment, shows that photocatalysis by the TiO₂ is dominant. The CO₂ evolution rates from films opacified with different grades of rutile pigment correlate with weight loss measurements made from identical paints exposed to glass-filtered carbon arc irradiation in conventional accelerated weathering equipment. These two comparisons confirm the relevance, to conventional accelerated testing, of paint durability of the FTIR assay of carbon dioxide evolution from alkyd paints. Because the experimental procedure allows the ready interposition of suitable optical filters, the method is well suited to studies of e.g., incident wavelength & intensity. In addition, deliberate variations in the humidity of the atmosphere in the FTIR cell were monitored by using the i.r. absorption of water vapour. Not only did the observed rates of carbon dioxide evolution decrease with decreasing humidity, they extrapolated to zero at zero humidity. This is consistent with mechanisms, derived from studies of model systems, that identify hydroxyl radicals as the key catalytic intermediate in photocatalytic oxidation of TiO₂ pigmented paint.     

Infrared spectroscopic evaluation of the photodegradation of paint Part I The UV degradation of acrylic films pigmented with titanium dioxide

In situ, quantitative infrared spectrometry has been used to measure the evolution of carbon dioxide during the photo-degradation of pigmented and unpigmented acrylic-emulsion paint films. It is demonstrated that the method permits a fast and convenient way of assessing the resistance of such paints to UV degradation. However, it is also shown that valid comparisons of paints prepared with different grades of titanium dioxide, but with the same acrylic emulsion, require careful selection and control of the experimental conditions. Thus, the relative importance of (a) direct photochemical oxidation of the binder and (b) indirect photo-catalysed oxidation (mediated by titanium dioxide) depend not only on the spectral distribution of the radiation source, particularly the output between 300 and 400 nm, but also on the humidity of the ambient atmosphere. The increased rate of oxidation with increased humidity is not unexpected, but the size of the effect is unexpectedly high. In addition, there is some carbon dioxide formation during irradiation of the paint film in nitrogen and further investigation of this phenomenon is in hand. For both pigmented and unpigmented films, the rate of carbon dioxide evolution is sensitive to the film thickness. The dependence of the oxidation rate on the thickness of clear, unpigmented films is consistent with the measured UV absorption. However, for pigmented films, this dependence extends over greater film thicknesses than predicted by a simple model based on paint film optics.     

Effect of annealing on the structural and optical properties of InSe bilayer thin films

InSe bilayer thin films with different thickness were prepared on to a glass substrate by sequential thermal evaporation. Preparation and post deposition treatment conditions were optimized in order to achieve effective bilayer mixing. The influence of bilayer film thickness and annealing temperature on the structural and optical properties was investigated. The prepared films were characterized by X-ray diffraction analysis, scanning electron microscopy, energy dispersive X-ray analysis, UV-Visible spectroscopy, photoconduction and resistivity measurement. Structural studies show that the material undergoes phase transition with thickness, due to co-existence of many phases. Morphological analysis revealed that Se content plays an important role in determining the surface morphology of the film. It has been observed that grain growth and grain splitting phenomena depend on film thickness and annealing temperature. From the photoconduction measurements, the photocurrent increases rapidly when the sample is illuminated using 135 K Lux of white light. Absorption coefficient is in the order of 10⁴ cm⁻¹, makes the InSe thin film useful for the preparation of absorber layer in hybrid solar cell.     

Synergism in anticorrosive paints

The present work depicts synergism anticorrosive behaviour between zinc hypophosphite and zinc phosphate in a commercial pigment mixture. Also, the performance of anticorrosive paints was evaluated. Synergism anticorrosive behaviour was evaluated by corrosion potential and linear polarization measurements in pigment suspensions. The protective layer obtained with this pigment mixture was investigated by scanning electron microscopy (SEM). Then, the anticorrosive properties of the pigment were assessed by incorporating it into alkyd and epoxy paints which were evaluated by salt spray test and electrochemical noise technique. The morphology and the nature of the protective layer grown under the paint film were also studied by SEM. Experimental results showed that improved anticorrosion protection is achieved in paints with reduced zinc phosphate contents as a consequence of the synergistic interaction between zinc hypophosphite and the other components of the pigment mixture. The electrochemical noise technique proved to be adequate to monitor corrosion in painted panels and is able to detect corrosion under the paint film from very early stages. This paper identified the need to study synergism between anticorrosive pigments to try to reduce the phosphate content in anticorrosive paints.     

Thermal Diffusivity Measurement for Titanium Thin Films on Copper Substrate by Laser Produced Plasmas

The transport properties of condensed phase materials are, in principle, dependent on the local structure and composition of the specimen. This is particularly evident near the free surface of a solid alloy specimen where the morphology, composition, and thermal diffusivity exhibit significant depth dependence, as demonstrated in an earlier study of the depth-resolved thermal diffusivity of a galvanized steel specimen. A new non-contact method was used, based on time-resolved, spectroscopic measurement of the total mass removed from the specimen surface representatively in elemental composition by a high-power laser pulse. A new study of a titanium thin film of varying thickness deposited on a copper substrate is presented. The titanium thin film is first fabricated in a vacuum and then immediately analyzed for composition and thermophysical properties in situ, both by the method of representative laser-produced plasmas (LPP). Successive ablation layers of the thin film, as exposed by LPP ablation, have revealed the dependence of the thermophysical properties on film thickness as well as on depth. The existence of a characteristic length over which the substrate influences the dynamics of thermal transport in the titanium thin film has also been observed.     

Structural, optical and electrical characterization of selenium sulphide nanostructured thin film

Thin film of selenium sulphide (Se₇₅S₂₅) has been prepared using inert-gas consolidation (IGC) method and micro-structural, optical and electrical measurements were carried out on the film. Scanning electron microscopy (SEM) studies show that the deposited film is well adherent and grains are uniformly distributed over the surface of the substrate. X-ray diffraction (XRD) analysis shows that the film is polycrystalline nature with single phase and crystallizes in the orthorhombic structure. The field emission transmission electron microscope (FETEM) revealed the uniform dispersion and an average particle size of 20 nm. Analysis of the optical absorption data indicates that the optical band gap E_opt of this film obeys Tauc's relation for the allowed non-direct transition with energy gap is 2.48 eV. Electrical conduction measurements also show the presence of two distinct phases of the materials and characteristic changes in transport properties due to the nanosize of the materials.     

“Thermal Prism” Method for Measuring Thermophysical Properties of Thin Films

Theoretical principles underlying the photothermal method for measuring the thickness and thermal properties of a thin film located between two optical elements (“sandwich”) are analyzed. The method is based on the irradiation of the assembly by repetitive pulse laser radiation. Radiation is absorbed in the film and causes heating of the optical elements by heat conduction. The element is monitored by a narrow beam of a second low-power laser propagating through the heated region. The beam is deflected due to the spatial variation of the refractive index, and the magnitude of the deflection angle as a function of time contains the relaxation and “wave” components. It is shown that the phase of the “wave” component depends on the thickness and thermophysical properties of the film. The thermophysical properties of the film can be determined, provided that the analogous properties of the optical element are measured previously or otherwise known, by comparing experimentally measured values of the phase shift with theoretical values obtained from the analytical solution of the non-stationary two-dimensional heat conduction equation.     

立方相Y掺杂ZrO2纳米晶薄膜的制备与辐照效应研究

采用溶胶-凝胶结合旋涂法在单晶Si衬底上制备了立方相Y掺杂ZrO₂纳米晶薄膜(YSZ), 并分析了制备工艺参数对YSZ成膜的影响。采用光学显微镜、扫描电子显微镜、X射线衍射和透射电镜等手段对样品进行了表征和分析。结果表明, 加入PVA作为分散剂、采用分级干燥工艺以及提高匀胶转速可大大提高YSZ薄膜的成膜质量, 制备的YSZ薄膜表面十分平整, 没有出现裂纹。YSZ薄膜为立方相结构, 没有出现其它相。薄膜由平均晶粒尺寸为9.4 nm的纳米晶组成, 薄膜的厚度约为60 nm。在室温条件下, 低剂量的Xe离子辐照YSZ薄膜后出现微裂纹, 而当辐照剂量比较高时, 由于热峰效应, 辐照引起的微裂纹逐渐发生愈合。并且, 随着辐照剂量的增加, YSZ薄膜的平均晶粒尺寸增大。     

Thermophysical Properties of 1,1,1,3,3-Pentafluorobutane (R365mfc)

This paper presents an experimental study on various thermophysical properties of a new fluoroalkane, 1,1,1,3,3-pentafluorobutane (R365mfc). The thermal conductivity of R365mfc was measured in the liquid phase near saturation conditions at temperatures between 263 and 333 K using a parallel plate instrument with an uncertainty of less than ±5%. For the measurement of the saturated liquid density between 273 and 353 K, a vibrating tube instrument was used. The uncertainty of the density measurements is less than ±0.1%. In addition, experimental data have been obtained for R365mfc under saturation conditions over a wide temperature range from about 253 to 460 K using light scattering techniques. Light scattering from the bulk fluid has been applied for measuring both the thermal diffusivity and the sound speed in the liquid and vapor phases. Light scattering by surface waves on a horizontal liquid–vapor interface has been used for the simultaneous determination of the surface tension and kinematic viscosity of the liquid phase. With the light scattering techniques, uncertainties of less than ±1.0, ±0.5, ±1.0, and ±1.2% have been achieved for the thermal diffusivity, the sound speed, the kinematic viscosity, and the surface tension, respectively.     

光功率热分析仪的温度校准方法研究

薄膜材料相变温度的准确测量是相变材料的应用关键.光功率热分析仪是基于薄膜材料相变前后光反射率发生突变的原理测量相变温度的新型仪器,采用真空红外加热方式达到相变温度.为了测量得到准确可靠的相变温度,通过对光功率热分析仪测量相变温度方式、标准热电偶原位校准仪器测温热电偶方法的研究,实现将相变温度溯源至SI单位,并且对在测温...     

Absolute distance measurement of optically rough objects using asynchronous-optical-sampling terahertz impulse ranging

We report on a real-time terahertz (THz) impulse ranging (IPR) system based on a combination of time-of-flight measurement of pulsed THz radiation and the asynchronous-optical-sampling (ASOPS) technique. The insensitivity of THz radiation to optical scattering enables the detection of various objects having optically rough surfaces. The temporal magnification capability unique to ASOPS achieves precise distance measurements of a stationary target at an accuracy of -551 μm and a resolution of 113 μm. Furthermore, ASOPS THz IPR is effectively applied to real-time distance measurements of a moving target at a scan rate of 10 Hz. Finally, we demonstrate the application of ASOPS THz IPR to a shape measurement of an optically rough surface and a thickness measurement of a paint film, showing the promise of further expanding the application scope of ASOPS THz IPR. The reported method will become a powerful tool for nondestructive inspection of large-scale structures.     

Effect of sample thickness on the extracted near-infrared bulk optical properties of Bacillus subtilis in liquid culture

In order to determine the bulk optical properties of a Bacillus subtilis culture during growth phase we investigated the effect of sample thickness on measurements taken with different measurement configurations, namely total diffuse reflectance and total diffuse transmittance. The bulk optical properties were extracted by inverting the measurements using the radiative transfer theory. While the relationship between reflectance and biomass changes with sample thickness and the intensity (absorbance) levels vary significantly for both reflectance and transmittance measurements, the extracted optical properties show consistent behavior in terms of both the relationship with biomass and magnitude. This observation indicates the potential of bulk optical properties for building models that could be more easily transferable compared to those built using raw measurements.     

Thickness dependence of structural and optical properties of indium tin oxide nanofiber thin films prepared by electron beam evaporation onto quartz substrates

Indium tin oxide (ITO) thin films, produced by electron beam evaporation technique onto quartz substrates maintained at room temperature, are grown as nanofibers. The dependence of structural and optical properties of ITO thin films on the film thickness (99-662 nm) has been reported. The crystal structure and morphology of the films are investigated by X-ray diffraction and scanning electron microscope techniques, respectively. The particle size is found to increase with increasing film thickness without changing the preferred orientation along (2 2 2) direction. The optical properties of the films are investigated in terms of the measurements of the transmittance and reflectance determined at the normal incidence of the light in the wavelength range (250-2500 nm). The absorption coefficient and refractive index are calculated and the related optical parameters are evaluated. The optical band gap is found to decrease with the increase of the film thickness, whereas the refractive index is found to increase. The optical dielectric constant and the ratio of the free carrier concentration to its effective mass are estimated for the films.     

Thickness dependence of structure and optical properties of silver films deposited by magnetron sputtering

A series of silver films with different thickness were prepared under identical conditions by direct current magnetron sputtering. The optical properties of the silver films were measured using spectrophotometric techniques and the optical constants were calculated from reflection and transmission measurements made at near normal incidence. The results show that the optical properties and constants are affected by films' thickness. Below the critical thickness of 17 nm at which Ag film forms a continuous film, the optical properties and constants vary significantly as the thickness of films increases and then tends to a stable value which is reached at 41 nm. X-ray diffraction measurements were carried out to examine the structure and stress evolution of the Ag films as a function of films' thickness. It was found that the interplanar distance of (111) orientation decreases when the film thickness increases and tends to be close to that of bulk material. The compressive strains also decrease with increasing thickness.