Rapid synthesis of Mo_5Si_3-Al_2O_3 nanocomposite powders by mechanochemical reduction method

Mo5Si3-20%Al2O3 （mass fraction） nanocomposite was synthesized by mechanical alloying （MA） of mixture of MoO3,Mo,Si and Al powders.The structural evolutions of powder particles during mechanical alloying were studied by X-ray diffractometry （XRD）,scanning electron microscopy （SEM）,transmission electron microscopy （TEM） and differential thermal analysis （DTA）.Results show that Mo5Si3-20%Al2O3 was obtained after 10 h of milling.The spontaneous reaction of powders takes place in an explosive mode.The crystallite sizes of Mo5Si3 and Al2O3 after milling for 30 h were 36.3 nm and 21.9 nm,respectively.With longer milling time,the intensities of Mo5Si3 and Al2O3 peaks decreased and became broad due to the decrease in crystallite size.Thermal analysis results and XRD analysis results show that the Mo5Si3-Al2O3 nanocomposite powders are very stable during milling （up to 30 h） and heating （up to 1 000℃） and no transformation takes place.

Modification of Nano-α-Al2O3 and Its Influence on the Surface Properties of Waterborne Polyurethane Resin Composite Passivation Films

Silane coupling agent KH560 was used to modify the surface of nano-α-Al2O3 in ethanol-aqueous solution with different proportions. The particle size of nano-α-Al2O3 was determined by nano-particle size analyzer, and the effects of nano-α-Al2O3 content, ethanol-aqueous solution ratio and KH560 dosage on the dispersion and particle size of nano-α-Al2O3 were investigated. The material structure before and after modification was determined by Fourier transform infrared spectroscopy (FTIR). Aqueous polyurethane resin and inorganic components are combined with modified nano-α-Al2O3 dispersion to form chromium-free passivation solution. The solution is coated on the galvanized sheet, the adhesion and surface hardness are tested, the bonding strength of the coating and the surface hardness of the substrate are discussed. The corrosion resistance and surface morphology of the matrix were investigated by electrochemical test, neutral salt spray test and scanning electron microscope test. The chromium-free passivation film formed after the modification of nano-α-Al2O3 increases the surface hardness of galvanized sheet by about 85%. The corrosion resistance of the film is better than that of a single polyurethane film. The results show that the surface hardness and corrosion resistance of polyurethane resin composite passivation film are significantly improved by the introduction of nano-α-Al2O3.

关于NaNO_2-Al(NO_3)_3-NaOH比色法测定总黄酮方法的探讨

目的:探讨NaNO_2-Al(NO_3)_3-NaOH定量方法的专属性。方法:选用多种黄酮及非黄酮化合物,与NaNO_2、Al(NO_3)_3、NaOH试剂反应后测定400～700nm吸收曲线。结果:有些黄酮类物质在500nm处无最大吸收或吸收很弱,而有些非黄酮类物质在500nm处有最大吸收或有较强吸收。结论:以芦丁为对照品,NaNO_2-Al(NO_3)_3-NaOH比色法测定总黄酮方法专属性差。

NaNO_2-Al(NO_3)_3显色分光光度法测定香椿叶总黄酮的含量

采用NaNO2-Al(NO3)3显色分光光度法测定香椿叶提取液中总黄酮含量,并对测定条件进行研究。结果表明:以芦丁为标样,以NaNO2-Al(NO3)3为显色剂,碱性条件下在510nm处测定显色液的吸光度确定总黄酮的含量,黄酮含量在12.032mg/L～96.256mg/L范围内,服从比耳定律,回归方程A=0.0119C—0.0084,相关系数R2=0.9998,方法的回收率为96.33%～101.20%,相对标准偏差(RSD)为1.26%;本方法简便、快速。

Ni-P—Nano-Al_2O_3化学复合镀层的磨损机理

通过摩擦磨损试验和扫描电镜分析等手段对Ni P—Nano Al2 O3化学复合镀层的摩擦磨损性能进行了研究 ,分析了Ni P—Nano Al2 O3复合镀层的磨损机理。结果表明 ,在干摩擦条件下 ,Ni P—Nano Al2 O3复合镀层中的Nano Al2 O3微粒能够有效地降低摩擦副之间的犁沟效应和粘着效应 。

NaNO_2-Al(NO_3)_3显色分光光度法测定萼翅藤叶总黄酮的含量

采用NaNO2-Al(NO3)3显色分光光度法测定萼翅藤叶提取液中总黄酮含量,并对测定条件进行研究。结果表明:以芦丁为标样,以NaNO2-Al(NO3)3为显色剂,碱性条件下在508 nm处测定显色液的吸光度确定总黄酮的含量,回归方程A=0.523C-0.0122,相关系数R=0.9998,方法的回收率为90.28%～99.73%,相对标准偏差(RSD)为1.57%;本方法简便、快速。

微波辐射KF/nano-γ-Al_2O_3催化的Gewald反应研究

以KF/nano-γ-Al2O3为碱性催化剂,在微波辐射作用下发生三组分Gewald反应,合成了一类2-氨基噻吩类化合物,并探索了不同反应条件对收率的影响。实验结果表明,该方法具有催化剂廉价高效、反应时间短、产品收率高、后处理简便等优点。

Synthesis of nanocrystalline γ-Al_2O_3 by sol-gel and precipitation methods for methanol dehydration to dimethyl ether

The capability of sol-gel and conventional precipitation techniques for the synthesis of nanocrystalline γ-alumina was investigated. These catalysts were used for vapor-phase dehydration of methanol to dimethyl ether in a fixed-bed reactor under the same operating conditions （T = 300 ？C, P = 1 bar, LHSV = 2.8, 11.7, 26.1 h？1） and characterized by means of N2 adsorption-desorption, NH3-TPD, XRD, TGA and SEM techniques. According to the experimental results, the catalysts prepared using sol-gel method in non-aqueous medium showed better performance compared with those prepared by other methods.

Structure and mechanical properties of ZrO_2-mullite nano-ceramics in SiO_2-Al_2O_3-ZrO_2 system

ZrO2-mullite nano-ceramics were fabricated by in-situ controlled crystallizing from SiO2-Al2O3-ZrO2 amorphous bulk. The thermal transformation sequences of the SiO2-Al2O3-ZrO2 amorphous bulk were investigated by X-ray diffraction, infrared spectrum, scanning electron microscope and differential scanning calorimetric. And the mechanical properties of the nano-ceramics were studied. The results show that the bulks are still in amorphous state at 900 ℃ and the t-ZrO2 forms at about 950 ℃ with a faint spinel-like phase which changes into mullite on further heating. ZrO2 and mullite become major phases at 1 100 ℃ and an amount of m-ZrO2 occur at the same time. The sample heated at 950 ℃ for 2 h and then at 1 100 ℃ for 1 h shows very dense and homogenous microstructure with ball-like grains in size of 20-50 nm. With the increase of crystallization temperature up to 1 350 ℃, the grains grow quickly and some grow into lath-shaped grains with major diameter of 5 μm. After two-step treatment the highest micro-hardness, flexural strength and fracture toughness of the samples are 13.72 GPa, 520 MPa and 5.13 MPa·m1/2, respectively.

Effect of anions on preparation of ultrafine α-Al_2O_3 powder

Ultrafine alumina power was obtained by calcining the precursor at 1 200 ℃ for 2 h, which was prepared by homogeneous precipitation method using aluminium salts and urea as raw materials. The effects of anions on the morphology, particle size, surface area and configuration of the precursors were studied. The results show that the reactions of urea with aluminium nitrate and aluminium chloride result in agglomerates gels with bad filtering performance, the morphology is fibrillar. Aluminium sulphate-urea reactions result in the direct formation of amorphous powders with good filtering performance, of which morphology are regular spherical particles with larger granularity and smaller surface area. The reaction of mutual compound of aluminium sulphate and aluminium nitrate with molar ratio of 40:60 with urea can produce precursor with good filtering performance, spherical morphology, and uniform granularity distribution in the particle size range of 2-3 μm.

PREPARATION OF NANOMETER ZrO_2-8% Y_2O_3 POWDERS BY AZEOTROPIC DISTILLATION PROCESSING

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Effect of NH_4F and Nano-SiO_2 on Morphological Control of α-Al_2O_3 Platelets via Solid-state Reaction

Alpha-alumina(α-Al_2O_3) platelets were prepared via solid-state reaction using pseudo-boehmite as the starting material, while NH_4F and nano-SiO_2 were used as additives, and nitric acid was used as the binder. The effect of these additives on properties of the alumina platelets was determined via scanning electron microscopy, X-ray diffraction, and measurements of the surface area and silicon content. A mechanism governing their role in the synthesis process was proposed. The results indicated that NH_4F could promote the formation of highly crystalline platelets. Addition of nano-SiO_2 could lead to increase in the diameter and reduction in the thickness of the platelets, and could also prevent their transformation to α-Al_2O_3. This addition weakened the effect of NH_4F because of the reaction of nano-SiO_2 with F-species and the formation of volatile SiF_4.

Effects of drying method on preparation of nanometer α-Al_2O_3

Ammonium aluminum carbonate hydroxide (AACH) precursor was synthesized by the precipitation reaction of aluminum sulfate and ammonium carbonate. Then the precursor was dealt with five drying methods including ordinary drying, alcohol exchange, vacuum freeze-drying, glycol distillation, n-butanol azeotropic distillation respectively and calcined at 1 200 ℃ for 2 h to get α-Al2O3. The effects of drying methods on preparation of nanometer α-Al2O3 were discussed, and the optimal drying method was confirmed. The structural properties of powders were characterized by XRD, SEM and BET measurements. The results show that vacuum freeze-drying, glycol distillation and n-butanol azeotropic distillation can prevent the powders from aggregating, and among them the n-butanol azeotropic distillation is the best method. The nanometer α-Al2O3 powder with non-aggregation can be manufactured using n-butanol azeotropic distillation and the average particle size is about 40 nm.

Phase Transition Behavior of Nanocrystalline Al₂O₃Powders

Alumina (Al2O3) has been synthesized through combustion synthesis (CS) technique. The calcined products were characterized using X-ray diffractional analysis (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and thermo-gravimetric analysis (TGA). TG-DTA results reveal the various stages involved in transition from γ-phase to α-Al2O3 phase. The first phase γ-Al2O3 was presented in the temperature range from 600°C-875°C as deduced from the XRD patterns with cubic crystal structure. The second stage occurs in the temperature range from 900°C-1000°C. In the final step, above 1000°C, the aluminium oxide appears completely as α-Al2O3, showing high crystallinity. The particle sizes are closely related to γ- to α-Al2O3 phase transition.

Preparation of ultrafine α-Al_2O_3 powders by catalytic sintering of ammonium aluminum carbonate hydroxide at low temperature

The precursor of ammonium aluminum carbonate hydroxide was synthesized by using aluminum sulfate（Al2（SO4）3） and ammonium carbonate（（NH4）2CO3）. The effects of α-Al2O3 seeds and mixture composed of α-Al2O3 and ammonium nitrate, as well as multiplex catalysts （AT） on phase transformation of alumina in sintering process were investigated respectively. The results show that the α-Al2O3 seeds and the mixture of α-Al2O3 and ammonium nitrate can lower the phase transformation temperature of α-Al2O3 to different extents while the particles obtained agglomerate heavily. AT has great potential synergistic effects on the phase transformation of alumina and reduces the phase transformation temperature of α-Al2O3 and the trends of necking-formation between particles. Therefore the dispersion of powder particles is improved significantly.

Synthesis of γ-Al_2O_3 nanoparticles by chemical precipitation method

Highly pure active γ-Al2O3 nanoparticles were synthesized from aluminum nitrate and ammonium carbonate with a little surfactant by chemical precipitation method. The factors affecting the synthesis process were studied. The properties of γ-Al2O3 nanoparticles were characterized by DTA, XRD, BET, TEM, laser granularity analysis and impurity content analysis. The results show that the amorphous precursor AI（OH）3 sols are produced by using 0.1 mol/L Al（NO3）3·9H2O and 0.16 mol/L （NH4）2CO3·H2O reaction solutions, according to the volume ratio 1.33, adding 0.024%（volume fraction） surfactant PEG600, and reacting at 40℃, 1000 r/min stirring rate for 15min. Then, after stabilizing for 24 h, the precursors were extracted and filtrated by vacuum, washed thoroughly with deionized water and dehydrated ethanol, dried in vacuum at 80℃ for 8h, final calcined at 800℃ for 1h in the air, and high purity active γ-Al2O3 nanoparticles can be prepared with cubic in crystal system, OH^7-FD3M in space group, about 9 nm in crystal grain size, about 20 nm in particle size and uniform size distribution, 131.35 m^2/g in BET specific surface area, 7 - 11 nm in pore diameter, and not lower than 99.93% in purity.

CuO/γ-Al_2O_3和CuO-CeO_2-Na_2O/γ-Al_2O_3催化吸附剂的脱硝性能

利用改进的溶胶凝胶法制备CuO／γ-Al2O3和CuO-CeO2-Na2o／γ-Al2O3催化吸附剂颗粒，在固定床上测试其催化脱硝活性。2类催化吸附剂250-400℃范围内脱硝效率稳定在70％以上。在350℃时效率稳定在最高值。利用程序升温方法研究了2类催化剂对NH3和NO的氧化性能，发现NH3在高于400℃下急剧氧化生成N2、NO和N2O，是脱硝效率下降的主要原因。CuO／γ-Al2O3催化剂能将NO氧化生成N02，NO在催化剂上的吸附对脱硝过程有重要作用。改进的CuO-CeO2-Na2o／γ-Al2O3催化剂能使NH3在高温400℃下不被氧化，也促进了NO在催化剂表面的吸附，从而提高了催化剂脱硝效率。催化反应的机理为NO吸附在催化剂表面，氧化生成吸附态的NO2，再与吸附催化剂上的NH3反应。

α-Al_2O_3的晶体结构与价电子结构

对α Al2 O3 的晶体结构进行了详细的讨论 ,通过各种立体插图 ,对比分析了α Al2 O3 的菱面体晶胞和六方晶胞 ,并对每种晶胞中各种原子的排列位置进行了深入分析 ,确定了某一具体位置的O2 -或Al3 + 与其它离子之间的主要键距 ,最后根据“固体与分子经验电子理论 (EET)”计算出了α Al2 O3 晶体的价电子结构 ,并以图示的方式把主要的键及键距标示在图中 ,使能直观地看到α Al2 O3 晶体中最强键及次强键等在晶体中的方位 ,便于分析α Al2 O3 的结构与性能的相互关系。

TiO_2和α-Al_2O_3晶体的生长习性

通过水热法制备粉体的实验观察到金红石、锐钛矿和а－Ａｌ２Ｏ３晶体的生长习性．采用配位多面体生长习性法则合理地解释了ＴｉＯ２和а－Ａｌ２Ｏ３的生长习性．其主要结果为а－Ａｌ２Ｏ３晶体的生长习性为平板｛０００１｝，其各晶面的生长速度为：Ｖ｛０００１｝＜Ｖ｛１１２３｝＜Ｖ｛０１１２｝＝Ｖ｛１１２０｝＜Ｖ｛０１１０｝。金红石的生长习性为柱状，其各晶面的生长速度为：Ｖ＜１１０＞＜Ｖ＜１００＞＜ Ｖ＜１０１＞＜ Ｖ＜００１＞＜ Ｖ＜１１１＞；锐钛矿的生长习性为四面体，其各晶面的生长速度为Ｋ＜０１０＞＝Ｖ＜００１＞＞Ｖ＜０１０＞＞Ｖ＜１１１＞．而ＰＢＣ理论很难合理地解释а－Ａｌ２Ｏ３晶体的生长习性．

纳米α-Al_2O_3在水相介质中的分散性能

在对纳米α-Al2O3粉体的Zeta电位进行测量的基础上,采用无机电解质类分散剂(SHP),阴离子型表面活性剂油酸,阳离子型表面活性剂十六烷基三甲基氯化铵(CTAC)以及非离子型表面活性剂异丙醇胺(DIPA)对纳米α-Al2O3粉体进行了分散实验,系统研究了超声分散时间、表面活性剂种类和浓度对纳米α-Al2O3粉体在水相介质中分散性能的影响。结果表明,随超声时间的延长和分散剂浓度的增加,纳米α-Al2O3粉体的分散性均出现先增后降的变化规律,对于每一种分散剂均存在最佳超声时间和最佳浓度。纳米α-Al2O3粉体在水相介质中的最佳分散工艺为:超声时间40 min,浓度为1.5%的CTAC。