非水解溶胶-凝胶法制备TiO2光催化薄膜

以TiCl4为前驱体,无水乙醇为氧供体,聚乙二醇(polyethylene glycol,PEG)为成膜控制剂,通过非水解溶胶-凝胶法制备了TiO2光催化薄膜.应用X射线衍射和热重-差式扫描量热研究了TiO2凝胶在热处理过程中的物相变化.采用场发射扫描电镜和光照甲基橙的降解实验研究了TiCl4浓度和镀膜次数对TiO2薄膜显微结构和光催化活性的影响.结果表明:非水解溶胶-凝胶法制备的TiO2薄膜开始出现金红石相的温度为750 ℃,高于传统水解溶胶-凝胶法制备的薄膜.TiCl4浓度和PEG用量是影响薄膜结构和光催化性能的关键因素.当TiCl4浓度为0.83 mol/L,PEG与TiCl4摩尔比为0.1时,所制备的薄膜是一种晶粒细小且孔隙及孔径分布均匀的多孔膜,这有利于提高薄膜的比表面积,薄膜具有最佳的光催化性能.     

焙烧温度对Pd-Pt/TiO_2-SiO_2-Al_2O_3加氢脱芳影响

采用改进的溶胶-凝胶法以不同物质的量配比的Ti、Si、Al制备成TiO2-SiO2-Al2O3复合载体,在不同温度下焙烧并对其进行BET、XRD表征。BET结果表明,随焙烧温度的升高,TiO2-SiO2-Al2O3复合载体的比表面积减小,孔体积和平均孔径逐渐增加。XRD结果表明,复合载体中TiO2以锐钛矿晶型存在,SiO2和Al2O3在TiO2上高度分散;锐钛矿特征峰随钛含量增大逐渐增强。考察焙烧温度对Pd-Pt/TiO2-SiO2-Al2O3催化剂的加氢脱芳性能影响。     

聚乙二醇对合成多孔SiO2块体结构和性能的影响

以正硅酸乙酯、聚乙二醇、乙醇和氨水为主要原料,采用溶胶-凝胶法制备了固定化酶用的块状多孔SiO2。研究了引入不同聚乙二醇对多孔材料的结构、孔径分布和水热稳定性的影响。结果表明：随着聚乙二醇含量的增加和聚乙二醇相对分子量降低,胶凝时间缩短。随聚乙二醇引入量增加,材料的比表面积、孔容和平均孔径值均增加。当添加的聚乙二醇的质量分数为30％时,各值达到极大。添加不同含量聚乙二醇所得的多孔块材在80℃热水中浸泡72h后气孔率变化均不超过8％,质量损失率小于6％,热水浸泡前后材料的孔径分布曲线形状基本不变,所得多孔材料的水热稳定性能好。     

常压干燥溶胶-凝胶法制备的TiO_2气凝胶织构和结构研究

以廉价的四氯化钛为前驱体,环氧丙烷为促凝剂,甲酰胺为干燥控制化学添加剂,有机配体丙酸为水解降速剂,采用正交实验设计以常压干燥-溶胶-凝胶法制备TiO2气凝胶,并用BET和XRD对样品的织构和结构进行表征。结果表明,以n(四氯化钛)∶n(去离子水)∶n(甲酰胺)∶n(丙酸)∶n(环氧丙烷)=1∶14∶2∶0.5∶10制备的TiO2气凝胶,比表面积为632.87 m2·g-1,平均孔径7.87 nm,孔容1.24 cm3·g-1;当平均孔径小、孔容大时比表面积较高,反之,比表面积很低;随着焙烧温度升高,晶化度增强,但仍未出现金红石相衍射峰,表明具有较好的热稳定性。TiO2气凝胶孔容较大时,锐钛矿相结晶度差,反之,结晶度好;孔容居中的TiO2气凝胶出现游离的无定型SiO2,而较低的丙酸含量有利于提高焙烧后样品的晶化度。     

TiO_2纳米多孔薄膜结构与光电化学性能相关性的研究

采用二步电压氧化法制备了两组孔径及孔密度不同的TiO_2纳米多孔薄膜,利用电化学测试方法对制备出的TiO_2纳米多孔薄膜的开路电位-时间曲线、交流阻抗谱图以及计时电流曲线进行了测试,研究了多孔薄膜材料的孔径及孔密度对材料光电化学性能以及比表面积的影响。结果表明,制备出的具有不同孔径和孔密度的试片在光照情况下的电化学反应电阻均明显下降,相关电化学反应更容易发生;增大薄膜材料的比表面积有利于提高其光电性能,性能最佳的薄膜材料的孔径为103 nm,孔密度为10×10~8个/cm~2。     

添加剂对γ-Al2O3陶瓷膜微孔结构的影响

以化学纯异丙醇铝为原料,采用溶胶凝胶法制备了γ-Al2O3陶瓷膜。研究了曲拉通(C34H62O11)、N,N-二甲基甲酰胺、硝酸镧等添加剂对γ-Al2O3陶瓷膜的微孔结构的影响,利用比表面积分析对陶瓷膜的性能进行了表征。结果表明：在γ-Al2O3陶瓷膜制备过程中,添加有机添加剂后,所制备的陶瓷膜的孔径、比表面积均变大。陶瓷膜经过高温热处理后,孔径急剧增大。在陶瓷膜的制备过程中引入硝酸镧,可以有效地抑制孔径的增大。化学添加剂可以起到改变陶瓷膜孔形状的作用。     

TiO_2溶胶改性PVDF超滤膜的制备与性能研究

利用溶胶-凝胶法制备二氧化钛(TiO2)溶胶并添加到铸膜液中,应用非溶剂致相法制备聚偏氟乙烯(PVDF)成品膜。系统研究了溶胶态TiO2、无机态Ti O2以及无机态TiO2/分散剂体系对TiO2/PVDF杂化膜的表面形貌、热稳定性、纯水接触角的影响。结果表明,溶胶态TiO2在铸膜液中分散良好,制取所得成品膜具有优良的综合性能,溶胶态TiO2的加入使得膜的接触角明显降低,孔隙率和平均孔径增大。     

超声场对钛溶胶及其材料微结构的影响

采用超声溶胶-凝胶法,以钛酸四丁酯为前驱体,乙酰丙酮为螯合剂,硝酸为催化剂,利用超声空化效应制备颗粒粒径小且分布窄的TiO_2溶胶,考察了超声时间和超声功率对TiO_2溶胶及材料的微结构性质的影响。采用流变仪、粒径分析仪、X射线衍射(XRD)、低温N_2吸附-脱附等手段对溶胶及材料进行了系统表征。结果表明,随着超声时间和超声功率的增大,溶胶粒径逐渐变小,而对溶胶的粘度影响不大,溶胶稳定性较好;且随着超声时间和超声功率的增大,制备的TiO_2材料的孔容和比表面积逐渐增加,晶粒尺寸逐渐减小,TiO_2材料主要为锐钛矿相,因此将超声溶胶-凝胶法应用于制备小孔径二氧化钛超滤膜具有良好的应用前景。     

石墨球模板溶胶-凝胶法制备TiO2团聚空心球

以石墨球为模板,采用溶胶-凝胶法制备TiO2团聚空心球,在400～600℃煅烧制备的材料中生成锐钛矿相TiO2,在750℃煅烧则以金红石相TiO2为主.包围在石墨球外围的TiO2凝胶在煅烧过程中生成晶体,同时形成球形空心结构.适当温度的煅烧可以完全去除石墨球模板,并在材料中生成Ti—O—Ti键.当煅烧温度从400℃升高到750℃时,材料的比表面积从7.6 m2·g-1降低到4.0 m2·g-1,而平均孔径和总孔容出现较大的增加.煅烧温度低于600℃样品的光催化活性随温度升高而快速增强.     

聚乙二醇对合成多孔二氧化硅块体结构和性能的影响

以正硅酸乙酯、聚乙二醇、乙醇和氨水为主要原料，采用溶胶-凝胶法制备了固化酶用的块状多孔二氧化硅。研究，引入同不聚乙二醇对多孔材料的结构、孔径分布和水热稳定性的影响。结果表明：随着聚乙二醇含量的增加和聚乙二醇相对分子量降低，胶凝时间缩短。随着聚乙二醇引入量增加，材料的比表面积、孔容和平均孔径均增加。     

Effect of additive structure and size on SiO2 formation in polymer‐derived SiOC ceramics

Silicon oxycarbide (SiOC) ceramics with highly adjustable properties and microstructures have many promising applications in batteries, catalysis, gas separation, and supercapacitors. In this study, additive structures on the nucleation and growth of SiO₂ within SiOC ceramics are investigated by adding cyclic tetramethyl‐tetravinylcyclotetrasiloxane (TMTVS) or caged octavinyl‐polyhedral oligomeric silsesquioxane (POSS) to a base polysiloxane (PSO) precursor. The effects of the 2 additives on the polymer‐to‐ceramic transformation and the phase formation within the SiOC are discussed. POSS encourages SiO₂ nucleation and leads to more SiO₂ formation with significantly increased ceramic yield, which subsequently leads to higher specific surface of 1557 m²/g with a larger pore size of ～1.8 nm for the porous SiOC. High TMTVS content decreases both the specific surface area and pore volume of the resulting porous SiOCs. This study demonstrates a new approach of using Si‐rich additive POSS to increase the SiOC yield while maintaining or even increasing the specific surface area.     

Effect of Viscosity on Preparation of Foamed Silica Ceramics by a Rapid Gelation Foaming Method

An environmentally benign preparation method for silica foam (the rapid gelation foaming method) was developed by combining sol-gel reactions and mechanical foaming without using organic polymers or monomers, in order to generate less CO₂ and harmful gases from the decomposition of organic compounds contained in the raw material. The viscosity of the silica sol during foaming affects the porous properties of the silica foam, i.e. the porosity and average pore size decrease with increasing viscosity. The pore structure of the silica foams depend on the viscosity of silica sol, two types of pore structure being formed. An open-pore structure is obtained by foaming low-viscosity sols, while a closed-pore structure is obtained by foaming high-viscosity sols. Since the viscosity of the silica sol affects the stability and foaming ability of the foam, the porous properties of the product can be controlled by controlling the viscosity of the silica during foaming.     

A novel method for the preparation of porous zirconia ceramics with multimodal pore size distribution

This work presents a new route of processing porous ceramic materials by vacuum induction melting of metallic ternary alloys from the system Ni–Zr–Y. Following internal oxidation results in an interpenetrating network of nickel and oxide phase consisting of yttria and zirconia. After dissolution of the metallic nickel matrix the oxide phase remains as a stable porous ceramic material with a multimodal pore size distribution. The porosity, pore size distribution and specific surface area can be controlled by alloy composition, solidification conditions and oxidation parameters.     

多孔硅酮建筑密封胶的制备与机理研究

研究了多孔功能材料、表面改性剂种类和用量等对密封胶性能的影响。使用扫描电镜（SEM）、X射线衍射（XRD）、氮气吸附-脱附等温测试（BET）和脱附孔径测试（BJH）等对多孔功能材料的形貌、物相、比表面积、孔体积和孔径进行了表征。结果表明,多孔材料比表面积和孔体积均增大,平均孔径减小,有利于拉伸模量的提高。     

Effects of compression on the textural properties of porous solids

This work deals with the analysis of the effects of compression in the textural properties, the crystallinity and the packing density of porous solids. It has been found that compression produces the decrease of both, the pore volume and the interparticle voids of porous solids. The reduction of the pore volume depends on the mechanical strength of the material. Activated carbons and inorganic porous oxides with a high mechanical strength, show a relatively low reduction of their pore volume, while porous solids in which the pore walls are constituted by organic frameworks, like MOF-5, have a lower mechanical strength and thus, their porous texture is largely affected by compression. In general terms, an increasing compressive pressure produces the removal of pores in the following sequence: mesopores, broad micropores and narrow micropores. Thus, compression of porous materials could be considered as a procedure to tailor the pore volume and the pore size distribution of porous solids. The results obtained in this work allow affirming that, in the preparation of adsorbent materials, together with the development of a high specific pore volume or a specific surface area, the behaviour upon compactatation must, undoubtedly, be taken into account.     

沸石补强硅酮建筑密封胶的应用研究

详述了用沸石和焙烧沸石作为补强剂用于制备硅酮建筑密封胶的工艺过程,分析了粉体用量对密封胶热稳定性、拉伸强度、断裂伸长率、干燥时间的影响;用扫描电镜（SEM）、X射线衍射（XRD）、氮气吸附—脱附等温测试（BET）和脱附孔径测试（BJH）方法对沸石和焙烧沸石的微观形貌、物相、比表面积、孔容和孔径进行了表征;研究结果表明它们是一种具有多孔结构的铝硅酸盐矿物,主要成分KNa2Ca2(Si29Al7)O72和K(Si3Al)O8,孔径分别为10nm和14nm,孔体积0.4655cc/g和0.5871cc/g,比表面积153.6m2/g和191.4m2/g,孔径分布宽、孔体积和比表面积大有利于补强,焙烧沸石的补强性优于沸石,揭示了它们的补强作用是硅烷偶联剂表面改性、孔道效应和锚固效应共同作用的结果。     

Sol-gel derived silica membranes with tailored microporous structures

The template effect of amphiphilic systems on the porous structure of silica gel layers has been studied. Membranes with a tailor-made microporosity and pore diameters of between 1 and 2 nm were obtained from these gels. Two different preparation methods have been used and their influence on the sol-to-gel transition of silicon alkoxide sols has been investigated. The first method entails the incorporation of non-ionic surfactants which modify the porous structure of gels. In this case, specific surface area, pore size and porous volume can be varied in the final material as a function of chain length and concentration of the surfactant. In the second method, self-assembled systems made of cationic surfactants develop during the gelation process and lead to an ordered gel structure. After elimination of the organic mesophase by heating, the membrane material exhibits an ordered microporosity with pore size directly related to the size of the surfactant molecules.     

Hierarchical porous ceramics with multiple open pores from boehmite gel emulsions

Ceramic foam materials with highly porous microstructure are playing vital role in increasing areas, especially for those with requirements for open channels and superior specific surface area. In this work, a simple and versatile approach to prepare ceramic foams with open pores has been proposed, that is gelation of boehmite nanoparticle-assembled emulsions. Notably, hierarchical porous microstructure with open channels and uniform pore structure has been built. High specific surface area up to389.4 m²/g is attainable, making it excellent adsorption material when combining the merit of hierarchical pore structure. Furthermore, lattice-shaped ceramics are prepared via direct ink writing gelled emulsion, displaying the potential of forming lightweight material with complex shape and designable macrostructure. The three-dimensional (3D) printed foams exhibit multiple open pores, which cover length scale from mm scale, to μm scale and nm scale, making them promising materials in several fields like adsorption and gas filtrations, etc.     

氧化铝多孔支撑体的制备工艺

叙述了用挤出成型法制备无机膜支撑体的工艺,研究了原料粒径、成孔剂用量和烧结温度对所制得多孔氧化铝支撑体性能的影响。研究结果表明,用粒径小于10μm的-αA l2O3粉体,以7%碳粉为成孔剂,烧结温度为1300℃,可以成功制得孔径分布较窄、平均孔径为2.1μm、孔隙率为48.9%的多通道无机膜支撑体。     

磷酸活化法制备半纤维素基颗粒活性炭

以半纤维素的主要模型物木聚糖为原料,在不添加其他粘结剂的条件下,采用磷酸活化法制备半纤维素基颗粒活性炭。讨论了浸渍比和炭活化工艺对活性炭吸附性能和孔隙结构的影响。研究结果表明:浸渍比的增加,有利于颗粒活性炭的比表面积、亚甲基蓝吸附值、强度、总孔容积和中孔容积的提高。随着炭活化温度的升高,颗粒活性炭的碘吸附值、亚甲基蓝吸附值、比表面积、总孔容积和微孔容积呈下降的趋势,强度呈上升趋势。N₂吸附-脱附等温线和孔径分析表明,颗粒活性炭具有发达的微孔结构,炭活化温度的升高不利于孔隙结构的发达。