N,N 0 -Bis(benzoyl) suberic acid dihydrazide (NA) as nucleating agent for poly(L-lactic acid) (PLLA) was synthesized from benzoyl hydrazine and suberoyl chloride, which was deprived from suberic acid via acylation. PLLA/NA samples were prepared by melt blending and a hot-press forming process. The nonisothermal and isothermal crystallization, spherulite morphology, and melting behavior of PLLA/NA with different contents of NA were investigated with differential scanning calorimetry, depolarized-light intensity measurement, scanning electron microscopy, polarized optical microscopy, and wide-angle X-ray diffraction. With the incorporation of NA, the crystallization peak became sharper and shifted to a higher temperature as the degree of supercooling decreased at a cooling rate of 1 C/min from the melt. Nonisothermal crystallization indicated that the presence of NA accelerated the overall PLLA crystallization. In isothermal crystallization from the melt, the presence of NA affected the isothermal crystalline behaviors of PLLA remarkably. The addition of NA led to a shorter crystallization time and a faster overall crystallization rate; this meant that there was a heterogeneous nucleation effect of NA on the crystallization of PLLA. With the addition of 0.8% NA, the crystallization half-time of PLLA/NA decreased from 26.5 to 1.4 min at 115 C. The Avrami theory was used to describe the kinetics of isothermal crystallization of the PLLA/NA samples. Also, with the presence of NA, the spherulite number of PLLA increased, and the spherulite size decreased significantly.
Transition metal oxides (TMOs) have attracted extensive research attentions as promising electrocatalytic materials. Despite low cost and high stability, the electrocatalytic activity of TMOs still cannot satisfy the requirements of applications. Inspired by kinetics, the design of hollow porous structure is considered as a promising strategy to achieve superior electrocatalytic performance. In this work, cubic NiO hollow porous architecture (NiO HPA) was constructed through coordinating etching and precipitating (CEP) principle followed by post calcination. Being employed to detect glucose, NiO HPA electrode exhibits outstanding electrocatalytic activity in terms of high sensitivity (1323 μA mM−1 cm−2) and low detection limit (0.32 μM). The excellent electrocatalytic activity can be ascribed to large specific surface area (SSA), ordered diffusion channels, and accelerated electron transfer rate derived from the unique hollow porous features. The results demonstrate that the NiO HPA could have practical applications in the design of nonenzymatic glucose sensors. The construction of hollow porous architecture provides an effective nanoengineering strategy for high-performance electrocatalysts.Electronic supplementary materialThe online version of this article (10.1186/s11671-017-2406-0) contains supplementary material, which is available to authorized users.
Molybdenum (Mo) doped BiVO4 was fabricated via a simple electrospun method. Morphology, structure, chemical states and optical properties of the obtained catalysts were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), UV-vis diffuse reflectance spectroscopy (DRS), N2 adsorption–desorption isotherms (BET) and photoluminescence spectrum (PL), respectively. The photocatalytic properties indicate that doping Mo into BiVO4 can enhance the photocatalytic activity and dark adsorption ability. The photocatalytic test suggests that the 1% Mo-BiVO4 shows the best photocatalytic activity, which is about three times higher than pure BiVO4. Meanwhile, 3% Mo-BiVO4 shows stronger dark adsorption than pure BiVO4 and 1% Mo-BiVO4. The enhancement in photocatalytic property should be ascribed to that BiVO4 with small amount of Mo doping could efficiently separate the photogenerated carries and improve the electronic conductivity. The high concentration doping would lead the crystal structure transformation from monoclinic to tetragonal phase, as well as the formation of MoO3 nanoparticles on the BiVO4 surface, which could also act as recombination centers to decrease the photocatalytic activity.
Crystallization and melting behavior of Poly(L-lactic acid)(PLLA)/Talc composites with different talc content were investigated in detail. The addition of talc can increase the overall crystallization rate of PLLA, 5%talc makes the melt-crystallization peak temperature of PLLA increase from 96.28 °C to 105.22 °C, and the crystallization enthalpy increases from 1.379 J•g-1to 28.99 J•g-1. The melting behavior of PLLA/5%talc composites at a different heating rate during non-isothermal crystallization at different cooling rate shows that heating rate can affect the melting behavior of PLLA, with increasing of heating rate, the double melting peak degenerates to single melting peak. Melting behavior after isothermal crystallization and after cold isothermal crystallization and hot isothermal crystallization indicates that the double-melting peak of PLLA/5%talc composites results from melting-recrystallization.
Adding a nucleating agent is one of the best ways to accelerate the crystallization rate of poly(L-lactic acid) (PLLA) so as to obtain a high degree of crystallinity during the process, which will improve the heat distortion temperature of final products. In the work reported, N, N -bis(benzoyl)sebacic acid dihydrazide (BSAD) was synthesized and used as a nucleating agent for PLLA. Isothermal and non-isothermal crystallization behaviors were investigated using differential scanning calorimetry (DSC). The addition of BSAD successfully enhances the crystallization rate of PLLA. A unique phase separation behavior of PLLA/BSAD blends is found from DSC as well as from polarized optical microscopy, which explains the difference of optimal BSAD concentration between isothermal and non-isothermal crystallization. This is the first recording of a phase separation peak in PLLA/nucleating agent blends using DSC. In thermogravimetric analysis, the enhanced thermal stability indicates that there are strong hydrogen bonds between BSAD and PLLA matrix. BSAD can dissolve in PLLA melt below its melting point through intermolecular hydrogen bonding with PLLA and self-assemble upon cooling, leading to the surface being capable of nucleating PLLA. Different phase separation temperatures can be used to control the morphology of BSAD, which finally determines the crystallite morphology of PLLA.
N,N,N 0 -Tris(1H-benzotriazole) trimesinic acid acethydrazide (BD) was synthesized from 1H-benzotriazole acetohydrazide and trischloride to serve as an organic nucleating agent for the crystallization of poly(L-lactic acid) (PLLA). First, the thermogravimetric analysis of BD exhibited a high thermal decomposition temperature; this indicated that BD maybe used as a heterogeneous nucleating agent of PLLA. Then, the effect of BD on the crystallization and melting behavior of PLLA was investigated through differential scanning calorimetry, depolarized light intensity measurements, and wide-angle X-ray diffraction. The appearance of a nonisothermal crystallization peak and increases in the glass-transition temperature and the intensity of the diffraction peak suggested that the presence of BD accelerated the overall PLLA crystallization. Upon cooling at a rate of 18C/min, the addition of just 0.5 wt % BD to PLLA increased the onset crystallization temperature from 101.4 to 111.38C, and the nonisothermal crystallization enthalpy increased from 0.1 to 38.6 J/g. The isothermal crystallization behavior showed that the crystallization half-time of PLLA with 0.5 wt % BD (PLLA/0.5% BD) decreased from 49.9 to 1.1 min at 1058C. However, the equilibrium melting point of PLLA/0.5% BD was lower than that of the pristine PLLA; this resulted from the increasing nucleating density of PLLA. The melting behavior of PLLA/ 0.5% BD further confirmed that BD improved the crystallization of PLLA, and the double-melting peaks of PLLA/0.5% BD were assigned to melting-recrystallization.
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