Polyethers with pendent phenylvinyl substituted carbazole rings as polymers for hole transporting layers of OLEDs

Polyethers containing pendent 3-(2-phenylvinyl)carbazole moieties have been synthesized by the multi-step synthetic routes. Full characterization of their structures is presented. The polymers represent materials of high thermal stability with initial thermal degradation temperatures exceeding 370 °C. The glass transition temperatures of the amorphous materials were in the range of 56–658 °C. The electron photoemission spectra of thin layers of the polymers showed ionization potentials of about 5.6 eV. Hole-transporting properties of the polymeric materials were tested in the structures of organic light emitting diodes with Alq₃ as the green emitter and electron transporting layer. The device containing hole-transporting layers of poly{9-[6-(3-methyloxetan-3-ylmethoxy)hexyl]-3-(2-phenylvinyl)carbazole} exhibited the best overall performance with a maximum photometric efficiency of about 4.0 cd/A and maximum brightness exceeding 6430 cd/m².     

Syntheses and characterization of 6,6′-diaryl-9,9′-dialkyl[3,3′]bicarbazoles as materials for electroluminescent devices

Electro-active materials containing 6,6′-diaryl-substituted [3,3′]bicarbazole core were synthesized by multistep synthetic rote and characterized. The derivatives were examined by differential scanning calorimetry and demonstrated formation of amorphous materials with rather high glass transition temperatures. The synthesized compounds have been tested as hole transporting layers in simple OLED devices with Alq₃ as the emitter/electron transporting layer. The green devices containing hole transporting films of diphenyl-9,9′-diethyl-[3,3′]bicarbazole exhibited the best overall performance (turn-on voltage: 3.5 V, maximum photometric efficiency: 4.2 cd/A, maximum brightness: ∼12,200 cd/m²).     

Electronic and thermal properties of compounds bearing diimide,azomethine and triphenylamine units

New triphenylamine containing azomethine diimides and two kinds of poly(azomethine imide)s, i.e., linear and branched were synthesized. These compounds were prepared from two diamines, that is, N,N′-bis(4-amino-2,3,5,6-tetramethylphenyl)phtalene-1,2,4,5-dicarboximide (DAPhDI), N,N′-bis(5-aminonaphtalen)naphthalene-1,4,5,8-dicarboxyimide (DANDI-2) and 4-formyltriphenylamine, 4,4′-diformyltriphenylamine and 4,4′,4″-triformyltriphenylamine. The structures of the compounds were characterized by means of FTIR, ¹H NMR spectroscopy and elemental analysis; the results show an agreement with the proposed structure. Thermal properties of prepared azomethine diimides and polymers were evaluated by thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC). Obtained compounds exhibited high thermal stability with 5% weight-loss temperatures above 390 °C. Azomethine diimides exhibited glass-forming properties with high glass-transition temperatures 216 and 308 °C. Optical properties of the prepared compounds were investigated by UV–vis and photoluminescence (PL) measurements. All compounds emitted blue light in NMP solution and in solid state as blend with PMMA. The electrochemical properties, that is, orbital energies and resulting energy gap were estimated based on cyclic voltammetry (CV). All synthesized material showed reversible reduction process, furthermore AzPhDI and AzNDI showed partially reversible oxidation process. Electrochemical band gap was found in the range 1.23–1.70 eV. Low molecular weight model compounds were tested as bipolar host materials in blue phosphorescent organic light emitting diodes (OLEDs). The devices exhibited turn-on voltages of about 5.5 V and maximum brightness of 40–220 cd/m².     

Effects of organo-modified montmorillonite on the tribology performance of bismaleimide-based nanocomposites

Poly(allyl condensed polynuclear aromatic-bismaleimide) (ACOPNA–BMI) with different loadings of an organo-modified montmorillonite (OMMT) nanocomposites were successfully prepared via in situ suspension polymerization. Exfoliation/intercalation phenomena were detected using transmission electron microscopy (TEM) and X-ray diffraction (XRD). Positive effects of the exfoliated platelets on the wearable and thermal behaviours were achieved by varying the OMMT load. The lowest friction coefficient of ACOPNA–BMI/2.0 wt.% OMMT was 0.46 at a wear rate of 0.508 × 10^− 6 mm³/Nm, which was superior to that of pure ACOPNA–BMI copolymer resin. The thermostabilities of the materials were assessed by thermogravimetric analysis (TGA). The temperature at the maximum rate of thermal decomposition of ACOPNA–BMI/3 wt.% OMMT was 480 °C, which was much higher than that of the pure ACOPNA–BMI copolymer (436 °C). The nanocomposite obtained, which is a suitable wearable material, can be widely used for protecting drilling tools in petroleum engineering applications due to its thermostability and good self-lubrication properties.     

A capric–palmitic–stearic acid ternary eutectic mixture/expanded graphite composite phase change material for thermal energy storage

This paper demonstrated a capric acid–palmitic acid–stearic acid ternary eutectic mixture/expanded graphite (CA–PA–SA/EG) composite phase change material (PCM) for low-temperature heat storage. The CA–PA–SA ternary eutectic mixture with a mass ratio of CA:PA:SA = 79.3:14.7:6.0 was prepared firstly, and its mass ratio in the CA–PA–SA/EG composite can reach as high as 90%. The melting and freezing temperatures of CA–PA–SA/EG composite were 21.33 °C and 19.01 °C, and the corresponding latent heat were 131.7 kJ kg⁻¹ and 127.2 kJ kg⁻¹. The CA–PA–SA/EG composite powders can be formed into round blocks by dry pressing easily, with much higher thermal conductivity than CA–PA–SA. Thermal performance test showed that the increasing thermal conductivity of CA–PA–SA could obviously decrease the melting/cooling time. Thermal property characterizations after 500 heating/cooling cycles test indicated that CA–PA–SA/EG composite PCM had excellent thermal reliability. Based on all these results, CA–PA–SA/EG composite PCM is a promising material for low-temperature thermal energy storage applications.     

An innovative process to fabricate copper/diamond composite films for thermal management applications

Diamond dispersed copper matrix (Cu/D) composite films with strong interfacial bonding were produced by tape casting and hot pressing without carbide forming additives. The tape casting process offers an original solution to obtain laminated materials with accurate thickness control, smooth surface finish, material net-shaping, scalability, and low cost. This study presents an innovative process of copper submicronic particles deposition onto diamond reinforcements prior to densification by hot pressing. Copper particles act as chemical bonding agents between the copper matrix and the diamond reinforcements during hot pressing, thus offering an alternative solution to traditionnal carbide-forming materials in order to get efficient interfacial bonding and heat-transfer in Cu/D composites. It allows high thermal performances with low content of diamond, thus enhancing the cost-effectiveness of the materials. Microstructural study of composites by scanning electron microscopy (SEM) was correlated with thermal conductivity and thermal expansion coefficient measurements. The as-fabricated films exhibit a thermal conductivity of 455 W m^?1 K^?1 associated to a coefficient of thermal expansion of 12 × 10^?6 °C^?1 and a density of 6.6 g cm^?3 with a diamond volume fraction of 40%, which represents a strong enhancement relative to pure copper properties (λ_Cu = 400 W m^?1 K^?1, α_Cu = 17 × 10^?6 °C^?1, ρ_Cu = 8.95 g cm^?3). The as-fabricated composite films might be useful as heat-spreading layers for thermal management of power electronic modules.     

Effect of the thermal cycle on the hot ductility and fracture mechanisms of a C–Mn steel

Transverse cracking on the surface of continuously cast steel products has been one of the main problems of this stage in steelmaking for many years. The incidence of this problem has been found in microalloyed steels as well as in some plain carbon steels containing residual elements. In this work, the hot ductility and fracture mechanisms of a C–Mn steel containing 0.6%Cu and 0.053%Sn as residual elements have been evaluated. To simulate the thermo-mechanical conditions of the straightening operation, tensile tests were carried out at temperatures ranging from 700 to 1100 °C with an initial strain rate of 5 × 10⁻³ s⁻¹. Specimens were subjected to three different reheating temperatures prior to the hot ductility test, including 1100 °C, 1330 °C and melting. After each test, the reduction in area of the samples tested to fracture was used as a measure of the hot ductility. The fracture surfaces were then examined by scanning electron microscopy. The widest and deepest ductility trough was obtained for the specimens tested after melting; for these conditions brittle fractures are interdendritic showing very low ductility. After reheating at 1330 °C, fracture features showed intergranular fracture combined with some plastic deformation corresponding to the test temperature. Reheating at 1100 °C produced a finer microstructure and the fracture features showed a mixture of intergranular with some interdendritic features. Also, ductile behaviours were associated with void coalescence. The different results obtained depending on the thermal cycle can be attributed to the presence of the residual elements in the steel through different segregation and precipitation patterns.     

High thermal stability fluorene-based hole-injecting material for organic light-emitting devices

Novel N¹,N³,N⁵-tris(9,9-diphenyl-9H-fluroen-2-yl)-N¹,N³,N⁵-triphenylbenzene-1,3,5-triamine (TFADB) was synthesized and characterized as a hole-injecting material (HIM) for organic light-emitting devices (OLEDs). By incorporating fluorene group TFADB shows a high glass-transition temperature T_g > 168 °C, indicative of excellent thermal stability. TFADB-based devices exhibited the highest performance in terms of the maximum current efficiency (6.0 cd/A), maximum power efficiency (4.0 lm/W), which is improved than that of the standard device based on 4-4′-4″Tris(N-(naphthalene-2-yl)-N-phenyl-amino)triphenylamine (2T-NATA) (5.2 cd/A, 3.6 lm/W). This material could be a promising hole-injecting material, especially for the high temperature applications of OLEDs and other organic electronic devices.     

Structural transformation and photoluminescence behavior during calcination of the layered europium-doped yttrium hydroxide intercalate with organic-sensitizer

We report, for the first time, structural transformation and photoluminescence behavior by calcination of layered europium-doped yttrium hydroxide (LYH:Eu) intercalate with organic sensitizer terephthalate (TA). The calcined samples displayed tunable luminescent performance dependent on calcined temperatures. Calcination under low temperatures (200 and 300 °C) retained layered structure, while high temperatures (>400 °C) yielded oxide phase. The optimal fluorescence occurred in 200 °C-calcination, possibly resulting from an optimal arrangement of TA. Above 200 °C, the luminescence intensity was first weakened and then enhanced, due to gradual departure of TA and following occurrence of oxide phase. The energy transfer presented an intrinsic transition from TA-to-Eu³⁺ in the organic intercalate to O²⁻-to-Eu³⁺ charge transfer in as-transformed oxide. The predominant luminescence property of the hybrid material can provide valuable guide for developing tunable luminescent materials, especially flexible materials resulting from the containing organic component.     

Solution combustion synthesis of LiMn2O4 fine powders for lithium ion batteries

In this work, fine powders of spinel-type LiMn₂O₄ as cathode materials for lithium ion batteries (LIBs) were produced by a facile solution combustion synthesis using glycine as fuel and metal nitrates as oxidizers. Single phase of LiMn₂O₄ products were successfully prepared by SCS with a subsequent calcination treatment at 600–1000 °C. The structure and morphology of the powders were studied in detail by X-ray diffraction, scanning electron microscopy and transmission electron microscopy. The electrochemical properties were characterized by galvanostatic charge–discharge cycling and cyclic voltammetry. The crystallinity, morphology, and size of the products were greatly influenced by the calcination temperature. The sample calcined at 900 °C had good crystallinity and particle sizes between 500 and 1000 nm. It showed the best performance with an initial discharge capacity of 115.6 mAh g⁻¹ and a capacity retention of 93% after 50 cycles at a 1 C rate. In comparison, the LiMn₂O₄ sample prepared by the solid-state reaction showed a lower capacity of around 80 mAh g⁻¹.     

Alkaline aluminum phosphate glasses for thermal ion-exchanged optical waveguide

Alkaline aluminum phosphate glasses (NMAP) with excellent chemical durability for thermal ion-exchanged optical waveguide have been designed and investigated. The transition temperature Tg (470 °C) is higher than the ion-exchange temperature (390 °C), which is favorable to sustain the stability of the glass structure for planar waveguide fabrication. The effective diffusion coefficient D_e of K⁺–Na⁺ ion exchange in NMAP glasses is 0.110 μm²/min, indicating that ion exchange can be achieved efficiently in the optical glasses. Single-mode channel waveguide has been fabricated on Er³⁺/Yb³⁺ doped NMAP glass substrate by standard micro-fabrication and K⁺–Na⁺ ion exchange. The mode field diameter is 9.6 μm in the horizontal direction and 6.0 μm in the vertical direction, respectively, indicating an excellent overlap with a standard single-mode fiber. Judd–Ofelt intensity parameter Ω₂ is 5.47 × 10⁻²⁰ cm², implying a strong asymmetrical and covalent environment around Er³⁺ in the optical glasses. The full width at half maximum and maximum stimulated emission cross section of the ⁴I_13/2 → ⁴I_15/2 are 30 nm and 6.80 × 10⁻²¹ cm², respectively, demonstrating that the phosphate glasses are potential glass candidates in developing compact optoelectronic devices. Pr³⁺, Tm³⁺ and Ho³⁺ doped NMAP glasses are promising candidates to fabricate waveguide amplifiers and lasers operating at special telecommunication windows.     

Thermal expansion of hydroxyapatite between − 100 °C and 50 °C

Hydroxy apatite (HAp) ceramic was synthesized using traditional sintering. Dilatometric and lattice thermal expansion properties of a HAp ceramic were evaluated at temperatures of ? 100–50 °C. In that temperature range, the dilatometric thermal expansion coefficient and the lattice thermal expansion coefficient of the HAp ceramic were, respectively, 10.6 × 10^? 6/°C and 9.9 × 10^? 6/°C. Furthermore, thermal expansion properties of a human tooth were measured. The thermal expansion coefficient of the horizontal direction perpendicular to the growing direction of a tooth was 15.5 × 10^? 6/°C; that of the vertical direction along with the direction of tooth growth was 18.9 × 10^? 6/°C at the temperature range described above.     

An investigation on the tribological behavior of AZ91 and AZ91 + 3 wt% RE magnesium alloys at elevated temperatures

The wear behavior of AZ91 and AZ91 + 3 wt% RE magnesium alloys was investigated under a normal load of 20 N at the wear testing temperatures of 25–250 °C and sliding speeds of 0.4 and 1 m s⁻¹. As the sliding speed increased from 0.4 to 1 m s⁻¹ at the wear temperature of 25 °C, the wear rates of AZ91 and AZ91 + 3 wt% RE alloys decreased by about 8% and 60%, respectively. With an increase in the wear temperature to 100 °C, the wear rate of AZ91 alloy was reduced by 58% at a sliding speed of 0.4 m s⁻¹, while the wear rate was sharply increased at a sliding speed of 1 m s⁻¹. At higher wear temperatures, the wear of the AZ91 alloy at both sliding speeds soared as a result of the softening of β-Mg₁₇Al₁₂ phase. However, the wear rate of AZ91 + 3 wt% RE alloy showed a minimum at the wear temperatures of 100 and 200 °C at sliding speeds of 1 and 0.4 m s⁻¹, respectively. Superior wear behavior of AZ91 + 3 wt% RE at the elevated temperatures could be attributed to its higher thermal stability and strength. Furthermore, a rise in sliding speed led to a 55% reduction in the wear rate of AZ91 + 3 wt% RE alloy at the wear temperature of 100 °C due to the formation of stable oxide layers on the wear surface.     

Elevated temperature low cycle fatigue of grey cast iron used for automotive brake discs

This paper evaluates the fatigue life properties of low carbon grey cast iron (EN-GJL-250), which is widely used for automotive brake discs. Although several authors have examined mechanical and fatigue properties at room temperatures, there has been a lack of such data regarding brake discs operating temperatures. The tension, compression and low cycle fatigue properties were examined at room temperature (RT) and at brake discs’ working temperatures: 500 °C, 600 °C and 700 °C. The microstructure of the material was documented and analysed. Tensile stress–strain curves, cyclic hardening/softening curves, stress–strain hysteresis loops, and fatigue life curves were obtained for all the above-mentioned temperatures. It was concluded, that Young’s modulus is comparable with both tension and compression, but yield its strength and ultimate strength are approximately twice as great in compression than in tension. All the mechanical properties remained quite stable until 500 °C, where at 700 °C all deteriorated drastically. During fatigue testing, the samples endured at 500 °C on average at around 50% of cycles at room temperature. Similar to other materials’ properties, the cycles to failure have dropped significantly at 700 °C.     

Highly efficient blue OLEDs based on diphenylaminofluorenylstyrenes end-capped with heterocyclic aromatics

In this paper, we have designed four diphenylaminofluorenylstyrene derivatives end-capped with heterocyclic aromatic groups, such as 9-phenylcabazole, 4-dibenzofuran, 2-benzoxazole, 2-quinoxaline, respectively. These materials showed blue to red fluorescence with maximum emission wavelengths of 476–611 nm, respectively, which were dependent on the structural and electronic nature of end-capping groups. To explore the electroluminescent properties of these materials, multilayer OLEDs were fabricated in the following sequence: ITO/DNTPD (40 nm)/NPB (20 nm)/2% doped in MADN (20 nm)/Alq₃ (40 nm)/Liq. (1 nm)/Al. Among those, a device exhibited a highly efficient blue emission with the maximum luminance of 14,480 cd/m² at 9 V, the luminous efficiency of 5.38 cd/A at 20 mA/cm², power efficiency of 2.77 lm/W at 20 mA/cm², and CIE_x,y coordinates of (0.147, 0.152) at 8 V, respectively.     

Thermal resistance of indium coated sapphire–copper contacts below 0.1 K

High thermal resistances exist at ultra-low temperatures for solid–solid interfaces. This is especially true for pressed metal–sapphire joints, where the heat is transferred by phonons only. For such pressed joints it is difficult to achieve good physical, i.e. thermal contacts due to surface irregularities in the microscopic or larger scale. Applying ductile indium as an intermediate layer reduces the thermal resistance of such contacts. This could be proven by measurements of several researchers. However, the majority of the measurements were performed at temperatures higher than 1 K. Consequently, it is difficult to predict the thermal resistance of pressed metal–sapphire joints at temperatures below 1 K.In this paper the thermal resistances across four different copper–sapphire–copper sandwiches are presented in a temperature range between 30 mK and 100 mK. The investigated sandwiches feature either rough or polished sapphire discs (Ø 20 mm × 1.5 mm) to investigate the phonon scattering at the boundaries. All sandwiches apply indium foils as intermediate layers on both sides of the sapphire. Additionally to the indium foils, thin indium films are vapour deposited onto both sides of one rough and one polished sapphire in order to improve the contact to the sapphire.Significantly different thermal resistances have been found amongst the investigated sandwiches. The lowest total thermal resistivity (roughly 26 cm² K⁴/W at 30 mK helium temperature) is achieved across a sandwich consisting of a polished sapphire with indium vapour deposition. The thermal boundary resistance between indium and sapphire is estimated from the total thermal resistivity by assuming the scattering at only one boundary, which is the warm sapphire boundary where phonons impinge, and taking the scattering in the sapphire bulk into account. The so derived thermal boundary resistance agrees at low temperatures very well with the acoustic mismatch theory.     

Low-temperature superplasticity of Al2O3(p)/Ni–Co nanocomposites

Nanocomposites of Al₂O₃/Ni–Co prepared using Al₂O₃ of various particle sizes were fabricated by pulse current electrodeposition. Their superplastic tensile deformation was investigated at strain rates of 8.33 × 10⁻⁴ s⁻¹ and 1.67 × 10⁻³ s⁻¹ and temperatures of 723–823 K. The Al₂O₃ particle sizes and the deformation temperature had significant influence on the elongation of the deposited materials. The optimal superplastic condition and the maximum elongation were determined. A low temperature superplasticity with elongation of 632% was achieved at a strain rate of 1.67 × 10⁻³ s⁻¹ and 823 K. Scanning electron microscopy and transmission electron microscopy were used to examine the microstructures of the deposited and deformed samples. The grains grew to a micrometer dimensions and were elongated along the tensile direction after superplastic deformation. Superplasticity in electrodeposited nanocomposites is related to the presence of S at grain boundaries and to deformation twinning.     

Blue emitting halogen–phenoxy substituted 1,8-naphthalimides for potential organic light emitting diode applications

In this paper, we report the synthesis and characterization of six 1,8-naphthalimides [4a–4c and 5a–5c] obtained by the substitution of electron donating halogen–phenoxy groups at the C-4 position. The derivatives were characterized using ¹H NMR, ¹³C NMR, mass spectra, FT-IR, single crystal XRD; photo-physical, thermal, surface morphological and electrochemical properties were also investigated. The derivatives exhibit deep blue photoluminescence in the range 414–423 nm (in CHCl₃) and 457–466 nm (in thin film state) on UV excitation with high Stokes’ shifts and good chromaticity. The TGA and DSC analysis showed that the derivatives possess good thermal stability (271–284 °C) and melting points (138–201 °C). The HOMO and LUMO energy levels estimated by cyclic voltammetry are in the range 6.21–6.34 eV and 3.31–3.41 eV respectively corresponding to energy band gaps of 2.98–3.15 eV. These energy values are relatively higher than the commonly used electron transporting materials. The optical and electronic properties of the derivatives were tuned by the introduction of different electron donating halogen–phenoxy groups through C-4 position of the naphthalimide moiety. The emissive and electron-transporting properties of the naphthalimide derivative 4a were studied by fabricating a bi-layer and tri-layer devices. Further a phosphorescent device with 4a as electron transport layer (ETL) exhibited superior performance than the device without any ETL and was comparable with the device using standard Alq₃ as ETL. These results indicate that the synthesized naphthalimide derivatives could play an important role in the development of OLEDs.     

Coating and spark plasma sintering of nano-sized TiN on Y-α-sialon

TiN coating on Y-α-sialon was accomplished by depositing TiO₂ on their particle surfaces through controlled hydrolysis of TiCl₄ and Ti(O-i-C₃H₇)₄ and subsequent nitridation with NH₃ gas at 1000 °C. TiN particles covering Y-α-sialon were about 20 nm in size. Spark plasma sintering (SPS) of TiN/Y-α-sialon particles produced composite ceramics with continuous TiN networks at 1400 °C, but with TiN grains isolated in elongated β-sialon grains at 1600 °C. The relative density and Vickers hardness of TiN/sialon ceramics SPSed at 1400–1600 °C containing 25 vol.% TiN were measured. The electrical resistivity was in a wide range of 10⁻⁴ to 10⁰ Ω cm for the ceramics sintered at 1400 °C, but lowered to the order of magnitude of 10⁻¹ and 10⁵ Ω cm at higher temperatures ≥1500 °C. It was found that the complete transition to β-sialon increased the resistivity to 10³ to 10⁵ Ω cm, due to breaking up continuous TiN layers by elongated β-sialon grains.     

Fabrication of asymmetric alumina membranes: I. Effect of SrO addition on thermal stabilization of transition aluminas

The effect of SrO addition on the thermal stabilization of transition aluminas with the aim of producing membrane layers (supported and unsupported) has been investigated. Al₂O₃–x wt.% SrO composite powders (x = 1, 3, 5, 8) were synthesized by co-precipitation of the hydroxides from solutions of AlCl₃ and Sr(NO₃)₂ salts using NH₄OH as a precipitating agent. Optimum SrO dopant concentration regarding the transition aluminas stabilization effect was determined to be 5 wt.% based on XRD analysis. STA analysis showed a 30 °C shift versus higher temperatures in the transformation of final transitional alumina (θ-Al₂O₃) to stable alpha phase due to addition of 5 wt.% SrO. The mechanism of transition aluminas thermal stabilization as a result of SrO addition is thoroughly discussed. Unsupported alumina membranes were prepared by drying boehmite sols at 600, 800, 1000 and 1100 °C. The effect of calcination temperature on surface area, pore size distribution of unsupported membranes containing 5 wt.% SrO has been investigated. The microstructure of unsupported and supported membranes revealed quite different. Smaller grains in the supported layers were attributed to the interaction between support and membrane.