适用于微传感器的纳米多孔铝膜的制备研究

在单晶硅表面溅射铝,采用两步阳极氧化法制备纳米多孔铝膜。研究了电解液种类、阳极氧化时间、扩孔时间对孔的结构与形貌的影响。结果表明,与硫酸和磷酸相比,草酸是制备纳米孔阵列的相对方便与可靠的电解液;第二步阳极氧化时间对孔的均匀性及孔深度影响较大,对平均孔径的影响较小;扩孔时间的长短对孔径大小及孔的均匀性均影响显著。     

多孔型阳极氧化铝膜的制备及微观分析

在硫酸电解液、草酸和磷酸电解液中,采用阳极氧化方法制备多孔型氧化铝膜。通过扫描电子显微镜对多孔型氧化铝膜进行形貌表征。根据试验得到:当0.3mol/L硫酸中,恒压25V阳极氧化1h可得到孔径约为40～60nm多孔氧化铝膜。在电解液为10.0g/L草酸与3.0ml/L磷酸混合液中,恒压140V二次阳极氧化可得到孔径为160～190nm多孔氧化铝膜。讨论了高温退火及磷酸处理对多孔氧化铝膜的影响,并进行了机理分析。     

多通孔阳极氧化铝膜的制备

通过两步阳极氧化法由铝片制得高度有序的多孔氧化铝膜（PAA）,采用高电压瞬时脉冲法分离出完整而独立的多通孔氧化铝模板.用SEM对其表面进行分析,结果表明用瞬时电压脉冲法可以很好地分离出完整的通孔膜,且膜质量很高.孔直径为40～50 nm,孔间距为90～ 105 nm,膜厚度为25μm左右,孔密度高达1.34×10^10个/cm2.通过4次阳极氧化的时间电流密度曲线对比,表明两步阳极氧化可以制得高度有序的PAA膜.     

玻璃基底上多孔氧化铝模板的制备

利用磁控溅射在玻璃基底上直接溅射一层铝薄膜,然后利用阳极氧化制备了多孔氧化铝模板,扫描电子显微镜图片显示在195V、60s的条件下获得的多孔氧化铝模板孔道排列规则,且双向贯通。这种方法为在玻璃等硬质基底上制备规则的纳米结构提供了一种有效途径。     

阳极氧化工艺对氧化铝模板孔径的影响

为了能制备出有序的纳米线阵列，采用一次阳极氧化的方法，制备出了孔径在12．8～43．5nm之间的多孔有序的氧化铝模板．通过改变氧化液浓度、氧化电压、氧化温度等条件，可对氧化铝模板的孔径大小进行控制，对各阳极氧化工艺因数对模板孔径的影响机理也进行了分析讨论．结果表明，在较低的氧化液浓度，氧化电压和氧化温度条件下，氧化铝膜的孔径较小；而在高的氧化液浓度，氧化电压和氧化温度条件下，氧化铝膜的孔径较大．     

Bioactive titanium metal surfaces with antimicrobial properties prepared by anodic oxidation treatment

In order to endow titanium metals with bioactivity and antimicrobial properties, titanium plates were subjected to anodic oxidation treatment in NaCl solutions in this study. The treated titanium metals could induce apatite formation in the fast calcification solution, and osteoblasts on the treated titanium surfaces proliferated well as those on the untreated titanium metal surfaces. The treated metals could inhibit S. aureus growth in the microbial culture experiments. It was assumed that Ti-OH groups and Ti-Cl groups formed on the treated titanium surface were responsible for the bioactivity and antimicrobial properties of the metals. The anodic oxidation treatment was an effective way to prepare bioactive titanium surfaces with antimicrobial properties. Supported by the National Natural Science Foundation of China (Grant Nos. 50672062 and 30870615), Key Programs for Science and Technology Development of Sichuan Province, China (Grant No. 2008SZ0104) and Sichuan Youth Science & Technology Foundation, China (Grant No. 09ZQ026-033)     

8407模具钢表面渗铝后的常温硬质阳极氧化

为了防止模具钢表面产生热熔损失效,对渗铝后的8407钢表面进行常温硬质阳极氧化实验,使试样表面形成了氧化膜．着重研究了电流密度和氧化时间对氧化膜厚度和硬度的影响．实验结果确定适宜的氧化条件是：电流密度为2．5A／dm^2左右,氧化时间在60min左右,氧化温度在25℃左右．     

烘烤对重铬酸盐封闭膜形貌和腐蚀行为的影响

铝合金阳极氧化后需进行封孔处理,烘烤极大的影响铝合金氧化膜的形貌和耐蚀性。本实验对2024铝合金阳极氧化经过重铬酸钾封孔处理后的膜进行烘烤研究。对烘烤过的试片与未烘烤的试片做电子显微镜表面形貌、激光共聚焦显微镜三维形貌及膜层的表面轮廓、膜的孔隙分布测试,且比较烘烤前后膜层的极化曲线。结果如下:铝合金阳极氧化重铬酸钾封闭后未烘烤膜的表面轮廓有很多非常深(深达18μm)、窄而细的孔,孔隙分布广而且密集;烘烤后封孔膜的孔隙深度降低,多孔层收缩变薄,孔隙分布稀疏。烘烤降低了重铬酸钾封闭膜的粗糙度且膜表面的凹坑有一定程度减少。从极化曲线看,烘烤后重铬酸钾封孔阳极钝化电流比未烘烤时低了几个数量级,说明烘烤提高了重铬酸钾封孔的铝合金的耐蚀能力。     

H2SO4浓度对6061硬质阳极氧化膜层质量的影响

针对低浓度硫酸进行硬质阳极氧化膜层厚度、硬度不均匀,以及膜层致密度较低等现象,研究了H2SO4浓度对铝合金6061硬质阳极氧化膜层均匀性和致密度的影响。结果表明：H2SO4浓度对铝合金6061硬质阳极氧化膜层的均匀性起到很大的影响作用,硬质氧化膜的硬度均匀性、膜厚均匀性随着H2SO4浓度（1～20％）的提高而改善;6061在低H2SO4浓度中通过硬质阳极氧化获得的氧化膜有部分孔蚀残缺现象,而在高H2SO4浓度中获得的氧化膜不存在此种缺陷,并且在高H2SO4浓度中获得的氧化膜较低浓度的更致密。     

Highly Ordered Carbon Nanotube Arrays with Open Ends Grown in Anodic Alumina Nanoholes

Highly ordered rmdtiwalled carbon nanotube arrays were fabricated by pyrolysis of acetylene within anodic alumina templates. Nanotubes are very uniform irt diameter and open at both ends. High resolution transmission electron microscopy and electron diffraction analysis show that the carbon nanotubes are well graphi-tized. These standing and open carbon nattotubes are possible to offer a potential elegant technique for electron emitting devices, chemical functionalization and nanotube composites.     

High-temperature oxidation behavior of Al<Subscript>2</Subscript>O<Subscript>3</Subscript>/TiAl matrix composite in air

The oxidation behavior of Al₂O₃/TiAl in situ composites fabricated by hot-pressing technology was investigated at 900° in static air. The results indicate that the mass gains of the composites samples decrease gradually with increasing Nb₂O₅ content and the inert Al₂O₃ dispersoids effectively increase the oxidation resistance of the composites. The higher the Al₂O₃ dispersoids content, the more pronounced the effect. The primary oxidation precesses obey approximately the linear laws, and the cyclic oxidation precesses follow the parabolic laws. The oxidized sample containing Ti₂AlN and TiAl phases in the scales exhibits excellent oxidation resistance. The oxide scale formed after exposure at 900°C for 120 h is multiple-layered, consisting mainly of an outer TiO₂ layer, an intermediate Al₂O₃ layer, and an inner TiO₂+Al₂O₃ mixed layer. From the outer layer to the inner layer, TiO₂+Al₂O₃ mixed layer presents the transit of Al-rich oxide to Ti-rich oxide mixed layer. Near the substrate, cross-section micrograph shows a relatively loose layer, and micro- and macro-pores remain on this layer, which is a transition layer and transferres from Al₂O₃+TiO₂ scale to substrate. The thickness of oxide layer is about 20 μm. It is also found that continuous protective alumina scales can not be observed on the surface of oxidation scales. Ti ions diffuse outwardly to form the outer TiO₂ layer, while oxygen ions transport inwardly to form the inner TiO₂+Al₂O₃ mixed layer. Under long-time intensive oxidation exposure, the internal Al₂O₃ scale has a good adhesiveness with the outer TiO₂ scale. No obvious spallation of the oxide scales occurs. The increased oxidation resistance by the presence of in situ Al₂O₃ particulates is attributed to the enhanced alumina-forming tendency and thin and dense scale formation. Al₂O₃ particulates enhance the potential barrier of Ti ions from M/MO interface to O/MO interface, thereby the TiO₂ growth rate decreases, which is also beneficial to improve the oxidation resistance. Moreover, the multi-structure of the TiO₂+Al₂O₃ mixed layer decreases the indiffusion of oxygen ions and also avails to improve the high temperature oxidation resistance of the as-sintered composites. Supported by the Special Program for Education Bureau of Shaanxi Province, China (Grant No. 08JK240) and Scientific Research Startup Program for Introduced Talents of Shaanxi University of Technology, China (Grant No. SLGQD0751)     

Synthesis and magnetic properties of CuFe2O4 nanotube arrays

CuFe2O4 nanotube arrays with different outer diameters were synthesized in anodic aluminum oxide templates through sol-gel techniques followed by heating treatment processes. The morphology of the nanotube arrays was investigated by field emission scanning electron microscope and transmission electron microscopy, suggesting that the nanotube arrays are ordered and uniform. The X-ray diffraction results indicate that the crystal structure of the nanotube arrays is polycrystalline with a spinel-type structure. The measurements of magnetic properties indicate that CuFe2O4 nanotube arrays with outer diameter of 200 nm exhibit magnetic anisotropy with easy magnetization direction along the axis of nanotubes.     

AC7A新型铝合金硫酸草酸阳极氧化研究

为了提高铝合金阳极氧化膜的性能,采用硫酸和草酸的混合溶液(质量浓度比10:1)对AC7A铝合金进行了阳极氧化处理,并对阳极氧化的工艺参数进行了优化。实验结果表明:AC7A铝合金硫酸草酸阳极氧化的氧化膜为多孔蜂窝状结构,其硬度和厚度均随温度的升高而减小;在电流密度3.0 A/dm2、电解液温度2℃、氧化时间1 h的工艺参数下,AC7A硫酸草酸阳极氧化膜层硬度可达471 HV50,厚度可达75μm。说明采用质量浓度比10∶1的硫酸草酸混合溶液对AC7A铝合金进行阳极氧化处理,可保证氧化膜的硬度和厚度满足使用要求,提高铝合金构件的使用寿命。     

H_2SO_4浓度对6061硬质阳极氧化膜层质量的影响

针对低浓度硫酸进行硬质阳极氧化膜层厚度、硬度不均匀,以及膜层致密度较低等现象,研究了H2SO4浓度对铝合金6061硬质阳极氧化膜层均匀性和致密度的影响.结果表明:H2SO4浓度对铝合金6061硬质阳极氧化膜层的均匀性起到很大的影响作用,硬质氧化膜的硬度均匀性、膜厚均匀性随着H2SO4浓度(1-20%)的提高而改善;6061在低H2SO4浓度中通过硬质阳极氧化获得的氧化膜有部分孔蚀残缺现象,而在高H2SO4浓度中获得的氧化膜不存在此种缺陷,并且在高H2SO4浓度中获得的氧化膜较低浓度的更致密.     

Preparation of uitrafine α-Al2O3 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-Al2 O3 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-Al2 O3 seeds and the mixture of α-Al2 O3 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.     

Cyclic oxidation behavior of Fe-9Cr-1Mo steel in water vapor atmosphere

The cyclic oxidation behavior of Fe-9Cr-1Mo steel (9Cr-1Mo) in 10%H₂O+90%Ar (volume fraction) atmosphere at 600, 650 and 700 for °C various time was studied. The oxidation mechanism of 9Cr-1Mo steel in 10%H₂O+90%Ar atmosphere was discussed. The thermal stress was evaluated in two oxide layers to illustrate the spallation of the oxide layer. The experimental results indicate that there exists a duplex oxide scale with an outer layer of Fe₂O₃ and an inner layer of mixed (Fe, Cr)₃O₄ formed on 9Cr-1Mo steel during cyclic oxidation. Some cracks generated in both inner and outer oxide layers. Parts of oxide scales spalled from substrate during the cyclic oxidation. A higher tensile stress in the oxide layer is formed at the early oxidation stage than at the later oxidation stage during heating. This tensile stress results in the formation of cracks in the oxide layer. Foundation item: Project(2006–8) supported by the Huadian International Corporation Limited     

Synthesis and performance of mesoporous phosphotungstic acid/alumina composite as a novel oxidative desulfurization catalyst

A series of mesoporous phosphotungstic acid/alumina composites （HPW/Al_2O_3） with various HPW contents were synthesized by evaporation-induced self-assembly method. These composites were characterized by nitrogen adsorption-desorption, TEM, FTIR, and UV-vis, and were tested as catalysts in oxidation desulfurization of model fuel composed of dibenzothiophene （DBT） and hydrocarbon, using H202 as the oxidant. These composites exhibited high activity in catalytic oxidation of DBT in model fuel and good reusing ability. The best performance was achieved by using the mesoporous HPW/Al_2O_3 with 15wt% HPW content, which resulted in a DBT conversion of 98% after 2 h reaction at 343 K, and it did not show significant activity degradation after 3 recycles. Characterization results showed that the mesoporous structure of alumina and the Keggin structure of HPW were preserved in the formed composite. These results suggested that HPW/ Al_2O_3 could be a promising catalyst in oxidative desulfurization process.     

Dissolution rate determination of alumina in molten cryolite-based aluminum electrolyte

Determination of dissolution rate of alumina is one of the classical problems in aluminum electrolysis. A novel method which can measure the dissolution rate of alumina was presented. Effect of factors on dissolution rate of alumina was studied intuitively and roundly using transparent quartz electrobath and image analysis techniques. Images about dissolution process of alumina were taken at an interval of fixed time from transparent quartz electrobath of double rooms. Gabor wavelet transforms were used for extracting and describing the texture features of each image. After subsampling several times, the dissolution rate of alumina was computed using these texture features in local neighborhood of samples. Regression equation of the dissolution rate of alumina was obtained using these dissolution rates. Experiments show that the regression equation of the dissolution rate of alumina is y=−0.000 5x ³+0.024 0x ²−0.287 3x+ 1.276 7 for Na₃AlF₆-AlF₃-Al₂O₃-CaF₂-LiF-MgF₂ system at 920 °C.     

SO2-4对块体纳米晶铜阳极极化行为的影响

为了揭示SO₂^-4对块体纳米晶铜耐蚀性能的影响规律,利用电化学方法,结合X射线衍射、能谱分析、扫描电镜等表面分析技术,研究了惰性气体沉积原位温压法制备的块体纳米晶铜在不同质量分数（0.3%、1.3%、2.3%、3.3%和4.3%）Na₂SO₄溶液中的阳极极化行为.结果表明,随着SO₂^-4的增多,纳米晶铜的致钝电流密度增大,而致钝电位降低.在0.3%的Na₂SO₄溶液中加入1%的NaCl,纳米晶铜阳极极化行为发生明显变化,Cl^-在纳米晶铜表面形成难溶于水的CuCl保护钝化膜,纳米晶铜致钝电流密度降低,活化-钝化过渡区电流密度下降速率显著减小.     

L_2铝H_2SO_4阳极氧化及电解着色的研究

针对Ｌ２铝材研究了化学抛光、电极材料与材料状态对阳极氧化膜质量的影响，试验出适宜于Ｌ２铝制构件的Ｈ２ＳＯ４阳极氧化方法。在获得良好质量的阳极氧化膜基础上，研究了对Ｌ２铝着古铜色、金黄色、黑色以及红褐色的工艺。同时，也探讨了对复杂构件着色以及在同一构件不同部位处着出颜色深线有别的方法。