NiMoO4/g-C3N4的制备及电化学性能研究

超级电容器具有比电容高、循环寿命长和绿色无污染的特点,其优异的电化学性能备受关注。本文水热合成了NiMoO₄/g-C₃N₄复合粉体,并将粉体涂覆在泡沫镍上制备了NiMoO₄/g-C₃N₄电极材料。结果表明,NiMoO₄/g-C₃N₄粉体形貌主要为NiMoO₄纳米棒和团状g-C₃N₄,且NiMoO₄纳米棒生长在g-C₃N₄纳米片上。在NiMoO₄中加入30at%的g-C₃N₄能降低电容体系的等效串联电阻和扩散阻抗,有利于氧化还原反应的进行。相比于其他g-C₃N₄含量的电极材料,g-C₃N₄含量为30at%的NiMoO₄/g-C₃N₄电极材料具有更高的比电容(584.3F/g)和更好的倍率特性。     

Characteristics of N-doped TiO2 nanotube arrays by N2-plasma for visible light-driven photocatalysis

N-doped TiO₂ nanotube arrays were prepared by electrochemical anode oxidation of Ti foil followed by treatment with N₂-plasma and subsequent annealed under Ar atmosphere. The morphologies, composition and optical properties of N-doped TiO₂ nanotube arrays were characterized using field-emission scanning electron microscope (FE-SEM), transmission electron microscope (TEM), X-ray photoelectron spectroscopy (XPS), X-ray diffraction spectrometer (XRD), Photoluminescence (PL) and UV-vis diffusion reflection spectroscopy (UV-vis DRS). Methylene blue (MB) solution was utilized as the degradation model to evaluate the photocatalytic activity of the samples under visible light irradiation. The results suggested N₂-plasma treatment created doping of nitrogen onto the surface of photoelectrodes successfully and the N-doped TiO₂ nanotube arrays display a significantly enhancement of the photocatalytic activity comparing with the pure TiO₂ nanotube arrays under the visible light irradiation.     

SiC_w/Si_3N_4复合陶瓷的制备及介电性能的研究

采用凝胶注模成型工艺制备了SiC_w/Si_3N_4复合陶瓷,由扫描电镜(SEM)可以看出,随热处理温度升高,碳化硅晶须的长径比逐渐减小;随烧结温度升高,复合陶瓷开孔率降低,密度随晶须含量的增加而增加。研究表明,SiC_w/Si_3N_4复合陶瓷的介电常数实部和虚部随碳化硅晶须含量的增加而升高,当烧结温度为1600℃,晶须含量从5%增加到15%时,8 GHz时介电常数实部从13.4增加到22.8,虚部从0.67增加到4.86;当烧结温度为1750℃时,8 GHz时介电常数实部从9.2增加到21.7,虚部从0.51增加到3.02。由反射率曲线可以看出,烧结温度为1750℃比1600℃时反射衰减随晶须含量的增加向低频移动的更快,频宽更宽。     

采用Ag-Cu-Ti+Mo复合钎料钎焊Si3N4陶瓷

采用Ag-Cu-Ti+Mo复合钎料连接Si3N4陶瓷,利用SEM,TEM,Nanoindentation研究了钎料内钼颗粒含量对接头组织和力学性能的影响.结果表明,在Si3N4/钎料界面处形成了一层致密的反应层,该反应层由TiN和Ti5Si3组成.接头的中间部分由银基固溶体、铜基固溶体、钼颗粒和Ti-Cu金属间化合物组成.借助于纳米压痕技术测定了接头内Ti-Cu化合物以及钎料金属的弹性模量和硬度值.随着钎料内钼颗粒含量的提高,母材/钎料界面反应层厚度逐渐降低;钎料金属中Ti-Cu化合物数量增多;此外,银和铜基固溶体组织逐渐变得细小.当添加5%Mo时,得到最高的接头强度429.4 MPa,该强度相比合金钎料提高了114.7%.     

水热法制备C3N4/CuGaO2 复合物及其气敏性能

采用简单水热法合成了一系列C₃N₄/CuGaO₂复合材料。采用XRD、SEM、TEM和XPS对制备的样品进行了表征。研究了一系列C₃N₄/CuGaO₂复合材料的气敏性能。结果表明,基于C₃N₄/CuGaO₂-0.3复合材料（C₃N₄与CuGaO₂的摩尔比为0.3:1）的气体传感器对甲苯的传感性能优于CuGaO₂传感器。相比较于CuGaO₂传感器的工作温度（140 ℃）,C₃N₄/CuGaO₂-0.3复合材料传感器的最佳工作温度仅为25 ℃,对100 μL/L甲苯气体的响应达到28,检出限低至0.01 μL/L。对100 μL/L甲苯气体的响应时间和恢复时间分别为114.2和27.4 s。此外,用于检测甲苯的C₃N₄/CuGaO₂-0.3复合材料传感器还具有优异的长期稳定性、良好的重复性和优异的抗湿性能。     

Deposition and characterization of CrN/Si3N4 and CrAlN/Si3N4 nanocomposite coatings prepared using reactive DC unbalanced magnetron sputtering

Nanocomposite coatings of CrN/Si₃N₄ and CrAlN/Si₃N₄ with varying silicon contents were synthesized using a reactive direct current (DC) unbalanced magnetron sputtering system. The Cr and CrAl targets were sputtered using a DC power supply and the Si target was sputtered using an asymmetric bipolar-pulsed DC power supply, in Ar + N₂ plasma. The coatings were approximately 1.5 μm thick and were characterized using X-ray diffraction (XRD), nanoindentation, X-ray photoelectron spectroscopy and atomic force microscopy. Both the CrN/Si₃N₄ and CrAlN/Si₃N₄ nanocomposite coatings exhibited cubic B1 NaCl structure in the XRD data, at low silicon contents (< 9 at.%). A maximum hardness and elastic modulus of 29 and 305 GPa, respectively were obtained from the nanoindentation data for CrN/Si₃N₄ nanocomposite coatings, at a silicon content of 7.5 at.%. (cf., 24 and 285 GPa, respectively for CrN). The hardness and elastic modulus decreased significantly with further increase in silicon content. CrAlN/Si₃N₄ nanocomposite coatings exhibited a hardness and elastic modulus of 32 and 305 GPa, respectively at a silicon content of 7.5 at.% (cf., 31 and 298 GPa, respectively for CrAlN). The thermal stability of the coatings was studied by heating the coatings in air for 30 min in the temperature range of 400-900 °C. The microstructural changes as a result of heating were studied using micro-Raman spectroscopy. The Raman data of the heat-treated coatings in air indicated that CrN/Si₃N₄ and CrAlN/Si₃N₄ nanocomposite coatings, with a silicon content of approximately 7.5 at.% were thermally stable up to 700 and 900 °C, respectively.     

Fast fabrication of Co3O4 and CuO/BiVO4 composite photocatalysts with high crystallinity and enhanced photocatalytic activity via ultrasound irradiation

A facile and efficient approach for the fabrication of Co₃O₄ and CuO/BiVO₄ composite photocatalysts was developed by intense ultrasound irradiation at room temperature. The as-synthesized samples were characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), photoluminescence (PL) spectroscopy, UV-vis diffuse reflectance spectra (UV-vis DRS), and Brunauer-Emmett-Teller (BET) surface areas. The photocatalytic activity of the composite catalysts was evaluated by photocatalytic degradation of acid orange II under visible light (λ > 420 nm) irradiation. Results showed that under intense ultrasonic irradiation, the precursors of copper acetate and cobaltous acetate could transform into CuO and Co₃O₄, respectively and the amorphous BiVO₄ can easily crystallize to highly crystalline BiVO₄. The composite photocatalysts exhibited much higher photocatalytic activity than that of pure BiVO₄. The enhanced photocatalytic performance could be attributed to the high crystallinity of BiVO₄ and the formed p-n heterojunction of Co₃O₄/BiVO₄ or CuO/BiVO₄. These two factors can effectively suppress the recombination of photogenerated hole-electron pairs.     

TiZrNiCu钎焊Si3N4-MoSi2复合陶瓷与Nb接头组织与力学性能

采用高温活性钎料TiZrNiCu对Si₃N₄-MoSi₂复合陶瓷和金属Nb进行真空钎焊试验,研究了其典型界面组织组成及形成机理,分析了钎焊温度和保温时间对钎焊接头界面组织及力学性能的影响规律。结果表明,接头典型界面结构为Nb/β-Ti/(Ti. Zr)₂(Cu, Ni)+β-Ti+(Ti, Zr)₅Si₃/TiN+(Ti, Zr)₅Si₃+MoSi₂/Si₃N₄-MoSi₂。钎焊温度和保温时间主要通过控制Si₃N₄-MoSi₂复合陶瓷母材中Si原子向钎料中扩散程度,来影响钎缝中(Ti, Zr)₅Si₃化合物的数量及分布,进而影响钎焊接头的抗剪强度。在920 ℃/10 min的工艺参数下,Si₃N₄-MoSi₂/Nb接头的室温抗剪强度最高达到112 MPa,选择最优参数条件下的Nb/Si₃N₄-MoSi₂钎焊接头在500 ℃和600 ℃条件下进行高温剪切实验,其高温抗剪强度分别达到123 MPa和131 MPa。     

N-doped TiO2/ZnO composite powder and its photocatalytic performance for degradation of methyl orange

The N-doped TiO₂/ZnO composite powder with a molar ratio of Ti to Zn of 3/1 was prepared via sol–gel process and then ammonia treated with NH₃ mass fractions of 0%, 7%, and 28% for 24 h at room temperature followed by thermal calcinations in air for 2 h at various temperatures of 500, 600, and 700 °C. The as-prepared composite powder was characterized in detail through thermo-gravimetric analyzer, X-ray diffraction, Fourier transform infrared spectroscopy, scanning electron microscopy, and high-resolution transmission electron microscopy. The results showed that the phase transformation of anatase to rutile has been successfully retarded via the ammonia treating process, leading to the presence of anatase phase in the composite. The particle crystallization of the composite powder was significantly promoted with the increase of the calcining temperature. The photocatalysis evaluation through MO degradation revealed an enhanced photocatalytic activity for the composite powder that might be related to the good crystallization, the presence of anatase phase, and the particle size reduction of the powder.     

Mechanical properties and microstructure of Ti(C,N) based cermets reinforced by nano-Si3N4 particles

Titanium carbonitride (Ti(C,N)) matrix cermets with different contents of nano-Si₃N₄ particles have been fabricated by microwave sintering in nitrogen atmosphere. The addition of nano-Si₃N₄ particle has important effect on the property of this cermet. Hardness and transverse rupture strength of the cermet are improved to about 1.3% and 25.2%, respectively, when the content of nano-particles is 2.0% in weight. Scanning electron microscopy (SEM) in combination with energy dispersive X-ray analysis (EDX) reveals that various cermets with or without nano-Si₃N₄ present quite different morphological and structural characteristics. It may be because that the addition of nano-Si₃N₄ particles inhibits the dissolution of Ti(C,N), and promotes the dissolution of WC and Mo₂C in binder phase and the formation of the inner rim. The modified microstructure by the addition of nano-Si₃N₄ particles results in the high mechanical properties of the cermet.     

Structure and mechanical properties of TiAlSiN/Si3N4 multilayer coatings

TiAlSiN/Si₃N₄ multilayer coatings which have different separate layer thicknesses of TiAlSiN or Si₃N₄ were deposited onto glass sheets, single-crystal silicon wafers and polished WC-Co substrates by reactive magnetron co-sputtering. The morphology, crystalline structure and thickness of the as-prepared multilayer coatings were characterized by TEM, SEM, XRD and film thickness measuring instrument. The mechanical properties of the coatings were evaluated by a nanoindenter. The effects of monolayer thickness on the microstructure and properties of TiAlSiN/Si₃N₄ multilayer coatings were explored. The coatings showed the highest hardness when the thickness of Si₃N₄ and TiAlSiN monolayers was 0.33 nm and 5.8 nm, respectively. The oxidation characteristics of the coatings were studied at temperatures ranging from 700 °C to 900 °C for oxidation time up to 20 h in air. It was found that the coatings displayed good oxidation resistance.     

Fe3O4/SiO2/Bi2WO6磁性复合光催化剂的制备及其光催化性能

钨酸铋(Bi₂WO₆),结构最简单的Aurivillius相化合物,是近期受到研究者关注的新型光催化材料。然而,光催化剂粉末在反应介质中难被回收,工业化应用成本较高。本文用三步方法合成了可回收的Fe₃O₄/SiO₂/Bi₂WO₆磁性复合光催化剂,通过溶剂热法合成具有磁性的Fe₃O₄,用溶胶凝胶法在Fe₃O₄表面覆盖SiO₂层,后将磁性颗粒与Bi₂WO₆纳米片相结合。光催化剂的形貌结构及性能通过XRD、SEM、PL、UV-vis进行表征测试。结果表明,直径约500 nm的Fe₃O₄微球附着在边长约500 nm的Bi₂WO₆纳米片的表面,SiO₂在两者之间起到了粘连作用。光催化剂Fe₃O₄/SiO₂/Bi₂WO₆对于罗丹明B的光降解活性较好,且有一定磁性,可以通过外加磁场将其从溶液中分离,有较大的应用潜力。     

g-C3N4/MoS2纳米片异质复合物的球磨法制备及可见光催化性能研究

采用球磨法制备g-C₃N₄/MoS₂纳米片异质复合物,运用X-射线衍射仪、高分辨透射电镜、紫外可见漫反射光谱和荧光发射光谱对异质复合物的结构和形貌进行了表征。结果表明：MoS₂纳米片可进入g-C₃N₄的层间形成异质复合物。以罗丹明B为模拟污染物,在可见光照射下考察了复合物的光催化特性。结果显示,含有2%的MoS₂纳米片与g-C₃N₄形成的异质复合物在120min内对罗丹明B降解率为98%,其降解动力学常数是体相g-C₃N₄为的4.3倍。g-C₃N₄/MoS₂纳米片异质复合物具有十分优良的光催化特性。其催化活性的提高主要归因于光生电子和空穴的有效分离和传输,并根据光捕获实验提出复合物可能的光催化机理。     

Performance of single Si3N4 and mixed Si3N4+PCBN wiper cutting tools applied to high speed face milling of cast iron

In this work two face milling cutter systems were used in high speed cutting of gray cast iron under cutting condition encountered in the shop floor. The first system, called ‘A’, has 24 Si₃N₄ ceramic inserts all with square wiper edges. The second system, called ‘B’, is a mixed tool material system, having 24 wiper inserts, 20 of them are Si₃N₄ intercalated by four PCBN inserts. Cutting speed (v_c), depth of cut (doc) and feed rate per tooth (f_z) were kept constant. Surface roughness (R_a and R_t) and waviness (W_t), tool life (based on flank wear, VB_Bmax) and burr formation (length of the burr, h) were the parameters considered to compare the two systems. System ‘B’ presented better performance according to all parameters, although only end of life criterion based on R_t parameter has been reached.     

固相-水热法制备LiFePO4-Li3V2（PO4）3复合材料及其电化学性能（英文）

分别采用固相-水热法和球磨法制备磷酸亚铁锂-磷酸钒锂复合正极材料(LiFePO4-Li3V2(PO4)3)。电化学性能测试表明,LiFePO4-Li3V2(PO4)3复合正极材料的电化学性能远远高于 LiFePO4和 Li3V2(PO4)3单独作为正极材料的性能,并且以固相-水热法制备的复合材料性能优于以球磨法制得的复合材料。研究发现 LiFePO4-Li3V2(PO4)3复合材料有 4 个氧化还原峰,相当于 LiFePO4 和 Li3V2(PO4)3 氧化还原峰的叠加。采用固相-水热法制备的LiFePO4-Li3V2(PO4)3 复合材料形貌较为规则,且有新相物质产生,这是导致其电化学性能较好的原因。     

Preparation and characteristic of spherical Li3V2(PO4)3

Spherical Li₃V₂(PO₄)₃ was synthesized by using N₂H₄ as reducer. The products were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM). The results show that single-phase, spherical and well-dispersed Li₃V₂(PO₄)₃ has been successfully synthesized in our experimental process. Electrochemical behaviors have been characterized by charge/discharge measurements. The initial discharge capacities of Li₃V₂(PO₄)₃ were 123 mAh g⁻¹ in the voltage range of 3.0–4.3 V and 132 mAh g⁻¹ in the voltage range of 3.0–4.8 V.     

N, Fe and WO3 modified TiO2 for degradation of formaldehyde

Butyltitanate, ethanol and glacial acetic acid were chosen as titanium source, solvent and chelating agent, respectively, via a sol-gel method combined impregnation method to prepare N, Fe co-doped and WO₃ compounded photocatalyst TiO₂ powder. The synthesized products were characterized by X-ray diffraction (XRD), diffuse reflectance UV-Vis spectra (UV-DRS), scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS). Photocatalytic degradation of formaldehyde was employed to investigate the catalytic activity. The results show that the degradation rate is 77.61% in 180 min under UV light irradiation when the concentration of N is fixed on, and the optimum proportioning ratio of n(Fe):n(W):n(Ti) is 0.5:2:100.     

Thermal shock behavior of Si3N4-TiN nano-composites

Si₃N₄-TiN nano-composites were fabricated by hot press sintering nano-sized Si₃N₄ and TiN powders. The microstructure, mechanical properties and thermal shock behavior of Si₃N₄-TiN nano-composites were investigated. The addition of proper amount TiN particles can significantly increase the flexural strength and the fracture toughness. Si₃N₄-TiN nano-composites showed both higher critical temperature difference and higher residual strength compared with those of monolithic silicon nitride nano-ceramic when the amount of TiN is less than 15 wt.%. But a further increase in the amount of TiN leaded to a decrease in the thermal shock resistance.     

钎料中Ti元素含量对Si3N4/Si3N4接头界面结构及性能的影响

在900℃保温10 min的工艺条件下采用Ti含量不同的AgCu+Ti+nano-Si₃N₄复合钎料（AgCu_C）实现了Si₃N₄陶瓷自身的钎焊连接,并对不同Ti元素含量的接头界面组织及性能进行了分析.结果表明,接头典型界面结构为Si₃N₄/TiN+Ti₅Si₃/Ag_（s,s）+Cu_（s,s）+TiN_P+Ti₅Si_3P/TiN+Ti₅Si₃/Si₃N₄.随着复合钎料中Ti元素含量的增加,钎缝中团聚的纳米Si₃N₄颗粒逐渐减少,母材侧的反应层厚度逐渐增加后趋于稳定.当Ti元素含量高于4%时,钎缝中形成了类似于颗粒增强金属基复合材料的界面组织;当Ti元素含量达到10%时,有少量Ti-Cu金属间化合物在钎缝中形成;钎焊接头的抗剪强度随着Ti元素含量的增加而呈现先增加后降低的变化趋势,当Ti元素含量为6%时接头的抗剪强度达到最高值,即75 MPa.