Characterization of PTFE Using Advanced Thermal Analysis Techniques

Polytetrafluoroethylene (PTFE) is a synthetic fluoropolymer used in numerous industrial applications. It is often referred to by its trademark name, Teflon. Thermal characterization of a PTFE material was carried out using various thermal analysis and thermophysical properties test techniques. The transformation energetics and specific heat were measured employing differential scanning calorimetry. The thermal expansion and the density changes were determined employing pushrod dilatometry. The viscoelastic properties (storage and loss modulus) were analyzed using dynamic mechanical analysis. The thermal diffusivity was measured using the laser flash technique. Combining thermal diffusivity data with specific heat and density allows calculation of the thermal conductivity of the polymer. Measurements were carried out from − 125 °C up to 150 °C. Additionally, measurements of the mechanical properties were carried out down to − 170 °C. The specific heat tests were conducted into the fully molten regions up to 370 °C.     

Optical and dielectric properties of nitrophenolate based nonlinear optical crystal

A semi-organic nonlinear optical (NLO) material, lithium-p-nitrophenolate trihydrate (LPNP) was synthesized. Single crystals of dimensions 20 × 7 × 3 mm³ were harvested following the solvent evaporation technique. The functional groups present in the compound were identified from FT-IR and FT-Raman spectral analyses, and its molecular structure was confirmed. Identification of the compound was accomplished by X-ray diffraction technique (powder and single crystal XRD). The unit-cell dimensions and the morphology of the grown crystals were identified from single crystal XRD measurements. The thermal transport properties, thermal effusivity (e), thermal diffusivity (α), thermal conductivity (k) and heat capacity (C _p) were measured by the photopyroelectric technique at room temperature. Dielectric constant and dielectric loss were also measured as a function of frequency between 42 Hz and 5 MHz, and temperature between 32 and 100 °C. From optical transmittance measurements, the direct optical band gap of the LPNP crystal was estimated to be 2.47 eV. Laser damage threshold is 60.91 GW cm⁻². Powder second harmonic generation (SHG) measurement was carried out using a modified Kurtz–Perry technique. Third order nonlinear response was studied using Z-scan technique with a He–Ne laser (632.8 nm, 35 mW). The magnitude and the sign of the nonlinear absorption and nonlinear refraction are derived from a transmittance curve. The NLO parameters Intensity dependent refractive index n ₂, nonlinear absorption coefficient β and third order susceptibility χ⁽³⁾ were estimated.     

Size and defect related broadening of photoluminescence spectra in ZnO:Si nanocomposite films

Nanocomposite films of zinc oxide and silicon were grown by thermal evaporation technique using varying ratios of ZnO:Si in the starting material. Structural analyses reveal the role of ZnO and amorphous silicon interface in contributing to the relatively less common blue photoluminescence emissions (at ～410 and 470 nm). These blue peaks are observed along with the emissions resulting from band edge transition (370 nm) and those related to defects (520 nm) of ZnO. Careful analysis shows that along with the grain size of ZnO, a suitable compositional ratio of ZnO to silicon is critical for the coexistence of all the four peaks. Proper selection of conditions can give comparable photoluminescence peak intensities leading to broad-band emission.     

碳纤维层合板低速冲击后的红外热波检测分析

采用红外热波无损检测技术对低速冲击后的碳纤维层合板进行检测和分析, 研究了损伤面积与冲击能量之间的关系。对比发现, 实验结果与文献结果一致; 实验结果说明红外热波不仅可以检测冲击损伤的大小, 还可以确定损伤在材料内部绕冲击点沿纤维方向呈旋转方式进行扩展的损伤模式。采用超声C扫描对相同复合材料层合板进行了检测, 详细对比了2种检测方法的优缺点, 发现对于碳纤维层合板的低速冲击损伤, 红外热波检测技术是一种快速、 有效、 可靠的无损检测技术和评估手段。      

Synthesis and characterisation of styrene butadiene styrene-g-acrylic acid for potential use in biomedical applications

The work undertaken investigates the mechanical and thermal properties of styrene butadiene styrene (SBS) grafted with acrylic acid (AA) for use as a potential biomedical material. SBS-g-AA was synthesised by UV polymerisation and analytical techniques such as differential scanning calorimetry (DSC), attenuated total reflectance infrared Fourier transform spectrometry (ATR-FTIR), dynamic mechanical thermal analysis (DMTA) and tensile tests were used to characterise the grafted copolymers. From the DSC analysis, the glass transitions of polystyrene (PS) and polybutadiene (PB) domains present in the SBS copolymer were detected at 67 °C and ? 90 °C respectively. ATR-FTIR spectral analysis was used in conjunction with the DSC thermographs to analyse the grafted copolymers. The peak (1711 cm^? 1 ) associated with CO stretching in poly acrylic acid was located at 1725 cm^? 1 on the grafted SBS-g-AA copolymer which confirmed grafting took place. Mechanical testing was carried out to analyse the physical attributes of the grafted copolymers. It was found that a decrease in Young's modulus and stress at break occurred for SBS-g-AA copolymers which were soxhlet extracted using chloroform (washed). It was evident from the DMTA results that the glass transition values for each of the washed grafted samples increased, thus establishing that grafting had occurred onto the various butadiene segments along the SBS backbone. The results showed that the hydrophilic monomer was successfully grafted onto a hydrophobic polymer and the mechanical and thermal properties were in the useful range for biomedical applications.     

Application of band-target entropy minimization to infrared emission spectroscopy and the reconstruction of pure component emissivities from thin films and liquid samples

Thermal emission spectral data sets were collected for a thin solid film (parafilm) and a thin liquid film (isopropanol) on the interval of 298-348 K. The measurements were performed using a conventional Fourier transform infrared (FT-IR) spectrometer with external optical bench and in-house-designed emission cell. Both DTGS and MCT detectors were used. The data sets were analyzed with band-target entropy minimization (BTEM), which is a pure component spectral reconstruction program. Pure component emissivities of the parafilm, isopropanol, and thermal background were all recovered without any a priori information. Furthermore, the emissivities were obtained with increased signal-to-noise ratios, and the signals due to absorbance of thermal radiation by gas-phase moisture and CO2 were significantly reduced. As expected, the MCT results displayed better signal-to-noise ratios than the DTGS results, but the latter results were still rather impressive given the low temperatures used in this study. Comparison is made with spectral reconstruction using the orthogonal projection approach-alternating least squares (OPA-ALS) technique. This contribution introduces the primary equation for emission spectral reconstruction using BTEM and discusses some of the unusual characteristics of thermal emission and their impact on the analysis.     

Growth,structural, optical,DFT, thermal and dielectric studies of N-Benzyl-3-nitroaniline (B3NA): a promising nonlinear optical crystal

The non-linear optical material N-Benzyl-3-nitroaniline was synthesized and grown through an aqueous solution using a low temperature solution growth technique. This conforming monoclinic crystal structure with the P2₁ space group was established by the characterization study of single crystal X-ray diffraction. A powder X-ray diffraction analysis was performed to confirm crystalline nature. As one of the functioning groups of nitro-aniline revealed using the Fourier transform infrared spectrum and the prominent spectral band seen at 3404 cm^?1 is caused by stretching vibrations of the N–H group. The lower cut-off wavelength of the ultra violet-visible absorption and emission spectrum was found to be about 320 nm as the excitation of fluorescence and the emission of blue and red colors are expected at 459 nm and 688 nm. To determine the difference in energy between HOMO and LUMO by 9.6258, using the B3LYP/6-311G++ (d,p) method. The time-based DFT technique was used to calculate the first-order hyperpolarization (β)?=?1.214?×?10^–30 esu. Thermo gravimetric and differential thermal analysis measurements were used to determine the crystal’s moisturing toughness up to 282.87 °C. The relative dielectric constant changes with frequency. Kurtz Perry’s method confirmed 1.66 times the efficiency of second harmonic generation to this present crystal comparing KDP crystal. This data shows that there is a significant amount of promise that is used in optoelectronic materials.

     

Glottal closure instant and voice source analysis using time-scale lines of maximum amplitude

¹Time-scale representation of voiced speech is applied to voice quality analysis, by introducing the Line of Maximum Amplitude (LoMA) method. This representation takes advantage of the tree patterns observed for voiced speech periods in the time-scale domain. For each period, the optimal LoMA is computed by linking amplitude maxima at each scale of a wavelet transform, using a dynamic programming algorithm. A time-scale analysis of the linear acoustic model of speech production shows several interesting properties. The LoMA points to the glottal closure instants. The LoMA phase delay is linked to the voice open quotient. The cumulated amplitude along the LoMA is related to voicing amplitude. The LoMA spectral centre of gravity is an indication of voice spectral tilt. Following these theoretical considerations, experimental results are reported. Comparative evaluation demonstrates that the LoMA is an effective method for the detection of Glottal Closure Instants (GCI). The effectiveness of LoMA analysis for open quotient, amplitude and spectral tilt estimations is also discussed with the help of some examples.     

Synthesis and characterization of zirconium oxynitride ZrOxNy coatings deposited via unbalanced DC magnetron sputtering

A study of structure, morphology, and corrosion resistance was performed on zirconium oxynitride thin films deposited on 304 and 316 stainless steels by the DC sputtering magnetron unbalance technique. Structural analysis was carried out using X-ray diffraction (XRD), while morphological analysis was performed by scanning electron microscopy (SEM), atomic force microscopy (AFM), and transmission electron microscopy (TEM). These studies were performed as a function of deposition time via DC sputtering at room temperature (287 K) with an Ar/air flow ratio of 3.0 and a total deposition time of 30 min. The oxynitride films were grown with cubic crystalline structures Zr₂ON₂ and preferentially oriented along the (222) plane. Chemical analysis determined that in the last 5.0 nm, the Zr coatings present the following spectral lines: Zr3d_3/2 (184.6 eV) and 3d_5/2 (181.7 eV), O1s (531.3 eV), and N1s (398.5 eV).     

Growth and characterization of a new semi-organic nonlinear optical sodium paranitrophenolate paranitrophenol dihydrate single crystal

A new semi-organic nonlinear optical sodium paranitrophenolate paranitrophenol dihydrate single crystal is grown successfully using methanol as solvent by slow evaporation technique to dimensions of 14 × 5 × 4 mm³ in a period of 7 days. The grown crystal is characterized by X-ray diffractometry and UV-Visible spectral analysis. X-ray diffraction data reveals that the crystal belongs to monoclinic system with space group C2. Optical absorption studies illustrate low absorption in the entire UV and Visible region. The second harmonic generation (SHG) efficiency of the crystal measured by Kurtz's powder technique infers that the crystal has NLO coefficient 5 times greater than that of KDP crystal. Remarkable mechanical strength with the work hardening coefficient less than 2 and thermal stability up to 120 °C of the grown crystal is reported.     

Growth and characterization of an organic nonlinear optical material: l-alanine alaninium nitrate

l-alanine alaninium nitrate (LAAN), an organic nonlinear optical material was grown by slow evaporation technique at room temperature from its aqueous solution at pH value of 2.5. As grown single crystals were characterized for its spectral, thermal, linear and second order nonlinear optical properties. LAAN crystallizes in monoclinic system with space group P₂₁ and cell parameters a = 7.846 Å, b = 5.431 Å, c = 12.806 Å and β = 94.65°. The mode of vibrations of different molecular groups present in LAAN were identified by FTIR studies. The thermal behaviour of the crystals has been investigated using thermogravimetry (TG) and differential thermal analysis (DTA), which indicates that the material does not decompose before melting. Transmittance spectrum reveals that the crystal has a low UV cut-off of 320 nm and has a good transmittance in the entire visible region. NLO property of the crystal was confirmed by Kurtz SHG powder technique.     

Cryogenic helium gas circulation system for advanced characterization of superconducting cables and other devices

A versatile cryogenic test bed, based on circulating cryogenic helium gas, has been designed, fabricated, and installed at the Florida State University Center for Advanced Power Systems (FSU-CAPS). The test bed is being used to understand the benefits of integrating the cryogenic systems of multiple superconducting power devices. The helium circulation system operates with four sets of cryocooler and heat exchanger combinations. The maximum operating pressure of the system is 2.1 MPa. The efficacy of helium circulation systems in cooling superconducting power devices is evaluated using a 30-m-long simulated superconducting cable in a flexible cryostat. Experiments were conducted at various mass flow rates and a variety of heat load profiles. A 1-D thermal model was developed to understand the effect of the gas flow parameters on the thermal gradients along the cable. Experimental results are in close agreement with the results from the thermal model.     

Research on the Temperature and Emissivity Measurement of the Metallic Thermal Protection Blanket

The temperatures and emissivities of the metallic thermal protection blanket at (900–1,300) °C are investigated experimentally by using a multi-wavelength pyrometer. A linear relation between the emissivity and true temperature at different wavelengths is assumed. Based on this assumption, the true temperatures and spectral emissivities of the metallic thermal protection blanket at the two temperature measurement points can be calculated simultaneously. Some experimental results for the practical data processing of measurements performed on the metallic thermal protection blanket show that the difference between the calculated temperature and the temperature measured by a standard thermocouple is within  ±  10°C.     

Growth and characterization of 4-methyl benzene sulfonamide single crystals

Single crystals of 4-methyl benzene sulfonamide (4MBS) were successfully grown from aqueous solution by low temperature solution growth technique. The grown crystal was characterized by single crystal XRD and powder XRD methods to obtain the lattice parameters and the diffraction planes of the crystal. UV–vis–NIR absorption spectrum was used to measure the range of optical transmittance and optical band gap energy. The optical transmission range was measured as 250–1200 nm. FTIR spectral studies were carried out to identify the presence of functional groups in the grown crystal. The thermal behavior of the crystal was investigated from thermo gravimetric analysis (TGA) and differential scanning calorimetry (DSC) study. The absence of SHG was noticed by Kurtz and Perry powder technique. The third order NLO behavior of the material was confirmed by measuring the nonlinear optical properties using Z-scan technique and it was found that the crystal is capable of exhibiting saturation absorption and self-defocusing performance.     

Variational-asymptotic modeling of the thermoelastic behavior of composite beams

This paper deals with steady state thermoelastic problems in composite beam structure by using variational-asymptotic method. First, the original three-dimensional heat conduction problem is reduced to be a two-dimensional thermal cross-sectional analysis along with an optional one-dimensional heat conduction analysis. The one-dimensional heat conduction analysis exists only if the temperature is not prescribed at any point of the cross-section along the span except the end surfaces. Then we reduce the one-way coupled, three-dimensional thermoelasticity problem into a two-dimensional, one-way coupled thermoelastic cross-sectional analysis and a one-dimensional, one-way coupled, thermoelastic beam analysis. The present theory is implemented into the computer program, variational-asymptotic beam sectional analysis (VABS). Several examples are studied using the present theory and the results from VABS are compared with available analytical solutions and the three-dimensional analysis using the commercial finite element package ANSYS.     

Film thickness dependence on the optical properties of sputtered and UHV deposited Ti thin films

Titanium films of different thicknesses were deposited on glass substrates, using planar magnetron sputtering at 313 K substrate temperature. Their optical properties were measured by spectrophotometry in the spectral range of 200-2500 nm. Kramers-Kronig method was used for the analysis of the reflectivity curves of Ti films to obtain the optical constants of the films. In order to compare the influence of thickness of Ti films prepared using two different PVD methods, namely sputtering and electron gun depositions on the optical properties of Ti films, the optical results of Savaloni and Kangarloo (2007) for Ti films produced using electron gun deposition under UHV condition at 313 K substrate temperature are incorporated in this work.The analysis of the residual stress in the sputter deposited films using sin² ψ technique and the nano-strain in the E. Gun deposited films obtained from X-ray diffraction line broadening analysis (Warren-Averbach method) showed consistency with the results obtained for optical functions and agreed well with the predictions of both structural zone model (SZM) and effective medium approximation (EMA) results. Therefore, a direct correlation between the optical properties and the processes involved in the evolution of thin films is established.The optical data, in particular the conductivity results for sputter deposited Ti films show more agreement with those of bulk sample (Lynch et al., 1975), while those of UHV E. Gun deposited films are more consistent with those of thin film sample (Johnson and Christy, 1974).     

Solving the Inverse Heat Conduction Problem in Using Long Square Pulse Thermography to Estimate Coating Thickness by Using SVR Models Based on Restored Pseudo Heat Flux (RPHF) In-Plane Profile

This research develops a method to estimate opaque coating thickness based on time-and-space-resolved thermography. Thermography is a viable technique for measuring coating thickness. However, time-resolved thermography becomes unreliable when uncontrolled constant thermal stimulation amplitude appears. Therefore, a time- and space-resolved thermography technique for coating thickness measurement called restored pseudo heat flux (RPHF) has been developed by using Fourier–Hankel transform. A non-dimensional analysis was conducted and the results show RPHF curves with different coating thicknesses converging as the thermal diffusivity ratio or thermal conductivity ratio goes to one. For large thermal conductivity ratio values, the RPHF curves have two inflection points along the non-dimensional radius. Fifty-nine samples were tested using the proposed method. Support vector regression (SVR) models were constructed with the in-plane distribution of RPHF and the temporal distribution of the measured surface temperature as inputs. To avoid overfitting, cross validation was applied to all the models. Later, another twenty-eight samples were tested to validate the SVR models. The results suggest that a support vector regression model with in-plane profiles of RPHF handles uncontrolled heat flux variation better and yields a better performance in coating thickness measurement than the temporal profile does. With in-plane RPHF profile as input, the SVR model can evaluate coating thickness with a relative root mean square error at 25.3% even when heat amplitude varies 50%.     

Thermal characterization of polyamide 11/nanographene platelet nanocomposites

The objective of this study is to evaluate thermal properties of polyamide 11 (PA11)/nanographene platelet (NGP) nanocomposites. Samples were prepared using 1 wt%, 3 wt%, and 5 wt% of NGPs. Isopropyl alcohol (IPA) was used as a solvent to assist in dispersion of the NGPs within the PA11 powder. The NGPs were hand mixed evenly into the PA11 powder using a wooden dowel. Morphological characterization of the PA11/NGP nanocomposite was conducted using scanning electron microscopy. Thermal characterization of nanocomposites includes thermogravimetric analysis, differential scanning calorimetry and thermomechanical analysis. Results indicate that the addition of NGPs shows an initial increase in thermal stability and crystallization temperature (T(c)) along with a decrease in glass transition temperature (T(g)) and no improvement in coefficient of thermal expansion (alpha). These results are attributed to improved interfacial adhesion between NGPs and PA11, restricting polymer chain mobility.     

Use of a High-Temperature Integrating Sphere Reflectometer for Surface-Temperature Measurements

The National Institute of Standards and Technology (NIST) has developed a new facility for the characterization of the infrared spectral emissivity of samples between 150 and 1,000°C. For accurate measurement of the sample surface temperatures above 150°C, the system employs a high-temperature reflectometer to obtain the surface temperature of the sample. This technique is especially useful for samples that have significant temperature gradients due to the thermal conductivity of the sample and the heating mechanism used. The sample temperature is obtained through two measurements: (a) an indirect sample emissivity measurement with an integrating sphere reflectometer and (b) a relative radiance measurement (at the same wavelengths as in (a)) of the sample as compared to a blackbody source. The results are combined with a knowledge of the blackbody temperature and Planck’s law to obtain the sample temperature. The reflectometer’s integrating sphere is a custom design that accommodates the sample and heater to allow reflectance measurements at temperature. The sphere measures the hemispherical-near- normal (8°) reflectance factor of the sample compared relative to a previously calibrated room-temperature reference sample. The reflectometer technique of sample temperature measurement is evaluated with several samples of varying reflectance. Temperature results are compared with values simultaneously obtained from embedded thermocouples and temperature-drop calculations using a knowledge of the sample’s thermal conductivity.     

Young’s modulus evolution at high temperature of SiC refractory castables

The evolution of Young’s modulus versus temperature has been evaluated in SiC-based hydraulically bonded refractories used in waste-to-energy (WTE) plants. Two types of low cement castables (LCC) with 60 and 85 wt% of SiC aggregates have been considered. The study was conducted by the way of a high temperature ultrasonic pulse-echo technique which allowed in situ measurement of Young’s modulus during heat treatment starting from the as-cured state up to 1400 °C in air or in neutral atmosphere (Ar) and during thermal cycles at intermediate temperatures (1000 and 1200 °C). For comparison in order to facilitate interpretation, thermal expansion has also been followed by dilatometry performed in the same conditions. Results are discussed in correlation with phase transformations occurring in the oxide matrix (dehydration at low temperature, crystallization of phases in the CaO–Al₂O₃–SiO₂ system) above 800 °C and damage occurring when cooling. The influence of oxidation of SiC aggregates on elastic properties is also discussed.