螯合剂用量对Al2O3-SiO2气凝胶复合材料性能的影响研究

针对Al_2O_3-SiO_2溶胶稳定性差、复合材料结构不稳定等问题,通过溶胶-凝胶和超临界干燥工艺制备出Al_2O_3-SiO_2气凝胶复合材料。采用平板导热仪、SEM、BET等对Al_2O_3-SiO_2气凝胶复合材料在不同工艺参数下的结构和性能进行分析与表征,完成了Al_2O_3-SiO_2溶胶制备工艺参数研究,确定了较佳的Al_2O_3-SiO_2气凝胶复合材料优化工艺参数。结果表明:随着螯合剂与仲丁醇铝物质的量的比增加,气凝胶的孔径分布(30～50 nm)变化不大,复合材料的密度均匀性提高,在微观结构中,气凝胶与纤维的结合程度先增加后减小,其中螯合剂与仲丁醇铝物质的量的比为0. 09时结合较好。     

纤维增强Al2O3-SiO2气凝胶隔热复合材料研究进展

Al₂O₃-SiO₂气凝胶是一种低密度、高比表面积、高孔隙率、低热导率的三维结构纳米多孔材料,在航空航天、建筑保温、石油化工等领域具有广泛的应用前景,是理想的高温隔热基体之一。但纯Al₂O₃-SiO₂气凝胶力学性能和抑制高温辐射传热能力较弱,限制了自身在隔热领域的应用。采用纤维作为增强体,制备的Al₂O₃-SiO₂气凝胶复合材料同时具有较好的力学和隔热性能,是目前国内外高温隔热材料方向的研究热点之一。本文介绍了纤维增强Al₂O₃-SiO₂气凝胶隔热复合材料的制备方法,综述了目前国内外该材料的研究进展,并对其未来发展趋势做了展望。     

Al2O3-SiO2-ZrO2-TiO2溶胶的制备与研究复合

以硝酸铝、正硅酸乙酯、氧氯化锆、钛酸丁酯为前驱体，水和无水乙醇为溶剂，用溶胶-凝胶法制备适合涂膜的复合溶胶。     

金属基表面Al2O3-SiO2涂层耐腐蚀性能的研究

由溶胶完全混合后再制备的Al2O3-SiO2复合涂层在碱性、酸性介质中都表现出更好的耐腐蚀性.     

Sol-Gel-SPD制备超细Al2O3-SiO2二元粉体材料

以硝酸铝(Al(NO3)3·9H2O)和正硅酸乙酯(TEOS)为原料,采用溶胶-凝胶(Sol-Gel)技术并结合喷雾干燥(SPD)技术制得超细Al2O3-SiO2二元复合粉体材料,并分别于400℃、800℃、1000℃、1150℃和1200℃煅烧2 h;采用全自动比表面积与孔隙率分析仪、TEM、TG-DSC及XRD等仪器研究了热处理温度、pH值(分别为5.5、7和8)以及干燥方法对粉体材料的表面性能、显微形貌、物相组成及Al2O3-SiO2二元系晶体转变过程的影响.结果表明由Sol-Gel-SPD制备的超细Al2O3-SiO2二元粉体材料的比表面积＞448 m2·g-1,而经1200℃煅烧2 h后所得的超细莫来石的比表面积34.05m2·g-1;TG-DSC分析表明采用Sol-Gel-SPD制得的Al2O3-SiO2二元粉体材料的质量损失主要发生在500℃之前;XRD分析表明粉体试样的开始莫来石化温度为1000℃,铝硅尖晶石(6Al2O3·SiO2)与非晶态SiO2在1150～1200℃完全转化为莫来石;比较不同pH值试样经1200℃煅烧后的TEM照片发现,当pH=7时,得到的超细莫来石粉体粒径最小,为50 nm.     

溶胶-凝胶法制备Al2O3-ZrO2-SiO2复合薄膜

本文采用溶胶-凝胶法以异丙醇铝、正硅酸乙酯和氧氯化锆为原料，HNO3为催化剂，PVA为成膜助剂，在多孔陶瓷管上制得了Al2O3-ZrO2-SiO2复合薄膜。研究了组分配比对溶胶性质的影响，结果表明Al2O3：ZrO2：SiO2在8：1：2～12：1：2之间时可得到性能符合要求的溶胶。通过扫描电镜可观察到膜的孔径为2～5μm，且膜与基底结合良好。     

Al2O3-SiO2-Na2O体系中制备莫来石连续纤维

以Al2O3、SiO2、Na2CO3粉末为原料,通过熔融拉丝法制备了莫来石连续纤维;通过X-ray衍射、扫描电镜、能谱及差示扫描量热法(DSC)等分析,讨论了莫来石纤维的形成过程及机理.实验表明,采用熔融法,从Si2-Al2O3-Na2O体系中能够制备出组织形态为针状的莫来石连续纤维,纤维的主晶相为莫来石和玻璃相;部分玻璃相在热处理过程中能够转变为莫来石晶相,从而进一步提高了纤维的耐火度.     

Al2O3-SiO2纳米复合粉体材料的超临界制备及其性能

采用sol-gel法和超临界流体干燥技术合成了Al2O3-SiO2纳米复合粉,并研究了该复合粉经不同温度处理后的显微结构形貌、比表面积、孔容分布、物相变化及分形维数等的变化规律.结果表明热处理温度直接影响粉体的显微结构特征,并决定其比表面积、孔容和分形维数;该复合粉体材料的莫来石化温度为1015℃左右.     

Al2O3-SiO2-TiO2复合陶瓷膜的研制

本文用Sol-Gel法制备了掺杂TiO2、SiO2改性的γ-Al2O3膜,Al2O3-SiO2-TiO2混合溶胶的比例为:Al:Si:Ti=1:4:1(mol比),加入硝酸调节其pH值位1.2-2.5,可得到稳定的Al2O3-SiO2-TiO2溶胶。通过XRD分析,膜的相组成为非晶态SiO2、γ-Al2O3和Al4Ti2SiO12及TiO2,SEM分析膜主要特征为层状表面结构,平铺在支撑体上。研究发现添加剂、pH值、膜与基体之间的应力作用、浸渍时间、热处理过程对膜的形成的影响甚大。     

Al2O3-SiO2复合中空微球的制备与表征

复合中空微球材料结合了中空球型材料和复合材料的性质,具有非常显著的优点,以正硅酸乙酯和硫酸铝为主要原料,结合溶胶一凝胶工艺与模板法制备了Al2O3-SiO2复合中空微球。研究表明：复合微球中的Al2O3相对含量随硫酸铝溶液的增大而增大,同时,中空微球表面变得不光滑。     

Characterization of Ni---W/A12O3-SiO2 aromatics saturation catalysts used in a one-year commercial HDS run

A series of Ni---W/A1₂O₃-SiO₂ catalysts with different A1₂O₃/SiO₂ ratios were prepared and loaded in a commercial HDS unit for a year. The catalytic properties of the freshly sulfided and spent catalysts were investigated by performing structural analyses and model test reactions. The aggregation of the WS₂ slabs in the lateral direction, which was observed by EXAFS and TEM, was a major cause of the catalyst deactivation. The addition of SiO₂ into the catalyst support was found to suppress the structural changes of the catalyst.     

Characterization and tribological investigation of sol-gel Al2O3 and doped Al2O3 films

Thin films of Al₂O₃ and doped Al₂O₃ were prepared on a glass substrate by dip coating process from specially formulated ethanol sols. The morphologies of the unworn and worn surfaces of the films were observed with atomic force microscope (AFM) and scanning electron microscope (SEM). The chemical compositions of the obtained films were characterized by means of X-ray photoelectron spectroscopy (XPS). The tribological properties of obtained thin films sliding against Si₃N₄ ball were evaluated and compared with glass slide on a one-way reciprocating friction tester. XPS results confirm that the target films were obtained successfully. The doped elements distribute in the film evenly and exist in different kinds of forms, such as oxide and silicate. AFM results show that the addition of the doped elements changes the structure of the Al₂O₃ films, i.e., a rougher and smoother surface is obtained. The wear mechanisms of the films are discussed based on SEM observation of the worn surface morphologies. As the results, the doped films exhibit better tribological properties due to the improved toughness. Sever brittle fracture is avoided in the doped films. The wear of glass is characteristic of brittle fracture and severe abrasion. The wear of Al₂O₃ is characteristic of brittle fracture and delamination. And the wear of doped Al₂O₃ is characteristic of micro-fracture, deformation and slight abrasive wear. The introduction of ZnO is recommended to improve the tribological property of Al₂O₃ film.     

Ni/Al_2O_3催化剂的CO_2-TPD表征

Ni/Al_2O_3催化剂是甲烷二氧化碳重整反应制取合成气研究最多、最具应用潜力的一种催化剂。通过对催化剂进行CO_2-TPD研究,考察还原态Ni/Al_2O_3催化剂的CO_2脱附特性。结果表明,浸渍法制备的Ni/Al_2O_3催化剂CO_2脱附曲线呈现双峰,分别在(60~65)℃和(350~380)℃出现高低温两个活性位;高温CO_2吸附量为3.0 cm~3·g~(-1),低温CO_2吸附量为24.0 cm~3·g~(-1)。催化剂的CO_2吸附量与其Ni含量无关。考察选用不同载体的CO_2脱附行为,发现以Al_2O_3为载体的催化剂CO_2吸附量是MgO和SiO_2为载体催化剂的2~4倍,以TiO_2为载体的催化剂几乎不吸附CO_2。     

还原条件对三元载体加氢催化剂加氢脱氮性能的影响

用原位溶胶凝胶法制备了不同TiO：含量的MoP／TiO2-SiO2-Al2O3催化剂,对含喹啉的模型化合物,在连续同定床反应器上进行。THDN活性评价（反应温度为300～400℃,反应压力为3．0MPa）。在不同还原条件下,对催化剂进行加氢脱氮活性评价。结果表明：还原条件对MoP／TiO2-SiO2-Al2O3催化剂加氢活性有较大影响,评价确定的最佳还原条件为：还原气速60mL／min,还原温度为600℃。     

Effect of Al2O3 on mechanical properties of Ti3SiC2/Al2O3 composite

The effect of Al₂O₃ on mechanical properties of Ti₃SiC₂/Al₂O₃ composite fabricated by SPS was studied systematically. The results show that the hardness of the Ti₃SiC₂/Al₂O₃ composite can reach 10.28 GPa, 50% higher than that of pure Ti₃SiC₂. However, slight decrease in the other mechanical properties was observed with Al₂O₃ addition higher than 5–10 vol.%, which is believed to be due to the agglomeration of Al₂O₃ in the composite.     

Mechanical properties of Al2O3/ZrO2 composites

In the present study, both t-phase zirconia and m-phase zirconia particles are incorporated into an alumina matrix. Dense Al₂O₃/(t-ZrO₂+m-ZrO₂) composites were prepared by sintering pressurelessly at 1600 °C. The microstructure of the composites are characterized, the elastic modulus, strength and toughness determined. Because the ZrO₂ inclusions are close to each other in the Al₂O₃ matrix, the yttrium ion originally in t-ZrO₂ particles can diffuse to nearby m-ZrO₂ particles during sintering, and the m-phase zirconia is thus stabilized after sintering. The strength of the Al₂O₃/(t-ZrO₂+m-ZrO₂) composites after surface grinding can reach values as high as 940 MPa, which is roughly three times that of Al₂O₃ alone. The strengthening effect is contributed by microstructural refinement together with the surface compressive stresses induced by grinding. The toughness of alumina is also enhanced by adding both t-phase and m-phase zirconia, which can reach values as high as two times that of Al₂O₃ alone. The toughening effect is attributed mainly to the zirconia t–m phase transformation.     

Preparation and characterization of nano-sized CoMo/Al2O3 catalyst for hydrodesulfurization

CoMo on Al₂O₃ catalyst prepared by spray pyrolysis method was found in the form of spheres of 0.5–1.2 μm, which consisted of tiny primary particles of ca. 10–20 nm diameter. The materials shows comparable activity to those of commercial catalysts in HDS of straight run gas oil, in particular, refractory 4,6-dimethyldibenzothiophene (4,6-DMDBT). Weaker interactions between CoMo and Al₂O₃ are suggested by temperature-programmed reduction (TPR), Raman spectroscopy, to give more active species than those over the impregnated catalysts. This accounts for its comparable activity in spite of its smaller surface area.     

Phase diagram of the Al2O3–ZrO2–Nd2O3 system

The phase diagram of the Al₂O₃–ZrO₂–Nd₂O₃ system was constructed in the temperature range 1250–2800 °C. The liquidus surface of the phase diagram reflects the preferentially eutectic interaction in the system. Two new ternary and one new binary eutectics were found. The minimum melting temperature is 1675 °C and it corresponds to the ternary eutectic Nd₂O₃·11Al₂O₃ + F-ZrO₂ + NdAlO₃. The solidus surface projection and the schematic of the alloy crystallization path confirm the preferentially congruent character of phase interaction in the ternary system. The polythermal sections present the complete phase diagram of the Al₂O₃–ZrO₂–Nd₂O₃ system. No ternary compounds or regions of remarkable solid solution were found in the components or binaries in this ternary system.     

TiO2-SiO2 and V2O5/TiO2-SiO2 catalyst: Physico-chemical characteristics and catalytic behavior in selective catalytic reduction of NO by NH3

TiO₂-SiO₂ with various compositions prepared by the coprecipitation method and vanadia loaded on TiO₂-SiO₂ were investigated with respect to their physico-chemical characteristics and catalytic behavior in SCR of NO by NH₃ and in the undesired oxidation of SO₂ to SO₃, using BET, XRD, XPS, NH₃-TPD, acidity measurement by the titration method and activity test. TiO₂-SiO₂, compared with pure TiO₂, exhibits a remarkably stronger acidity, a higher BET surface area, a lower crystallinity of anatase titania and results in allowing a good thermal stability and a higher vanadia dispersion on the support up to high loadings of 15 wt% V₂O₅. The SCR activity and N₂ selectivity are found to be more excellent over vanadia loaded on TiO₂-SiO₂ with 10–20 mol% of SiO₂ than over that on pure TiO₂, and this is considered to be associated with highly dispersed vanadia on the supports and large amounts of NH₃ adsorbed on the catalysts. With increasing SiO₂ content, the remarkable activity decrease in the oxidation of SO₂ to SO₃, favorable for industrial SCR catalysts, was also observed, strongly depending on the existence of vanadium species of the oxidation state close to V⁴⁺ on TiO₂-SiO₂, while V⁵⁺ exists on TiO₂, according to XPS. It is concluded that vanadia loaded on Ti-rich TiO₂-SiO₂ with low SiO₂ content is suitable as SCR catalysts for sulfur-containing exhaust gases due to showing not only the excellent de-NO_x activity but also the low SO₂ oxidation performance.