硅溶胶分散氧化铝浆料的免脱气注凝成型工艺

基于气泡的稳定性理论,发展了一种免脱气注凝成型技术制备莫来石陶瓷素坯。利用pH约为9.5的硅溶胶对氧化铝颗粒的分散作用,制备了固相体积分数为50%,浆料粘度为953 mPa.s的符合莫来石计量组成的硅溶胶分散氧化铝浆料。采用NH4Cl作为电解质,直接利用硅溶胶凝胶化实现浆料的原位凝固成型。研究发现:由于在浆料中不引入任何表面活性物质,浆料脱气处理时间对成型素坯气孔率影响不大,浆料无须经过脱气处理,即可成型得到抗折强度达4.83 MPa、显微结构致密均匀的莫来石素坯。     

钛酸铝陶瓷凝胶注模成型工艺的研究

通过凝胶注模工艺成型了钛酸铝坯体。研究了分散剂和固相含量对钛酸铝浆料流变性的影响,并探讨了单体和交联剂用量对钛酸铝坯体性能的影响规律。结果表明,聚甲基丙烯酸铵(PMAA-NH4)比柠檬酸铵(TAC)的分散效果更佳。加入0.5vol%的PMAA-NH4可制备出固相体积含量达52vol%的低粘度钛酸铝浆料。单体丙烯酰胺(AM)加入量应控制在1.0wt%￣1.5wt%,交联剂N,N'-亚甲基双丙烯酰胺(MBAM)的最佳用量为0.1 5wt%。凝胶注模成型的钛酸铝烧成试样晶粒细小,其强度相比于干压成型或注浆成型的试样提高了一倍。     

用凝胶法制备片状莫来石粉及其应用

用拟薄水铝石和非晶态ＳｉＯ_２微粉为原料，用溶胶－凝胶工艺制取了莫来石凝胶。通过干燥、煅烧，制得片状结晶莫来石粉．初步研究了凝胶法莫来石粉在钛酸铝陶瓷和烧结刚玉砖中的应用。实验结果表明，片状莫来石起了促进烧结、降低烧成温度的作用，并使钛酸铝－莫来石复相陶瓷和刚玉砖的强度得到显著提高．     

莫来石-钛酸铝窑具的制备与性能研究

采用原位合成技术合成莫来石一钛酸铝复相材料(ATM),并以复相材料和烧结莫来石(M60)为主要原料制备莫来石一钛酸铝窑具,借助于XRD、SEM和热态模拟试验等手段研究了烧成温度、复相材料添加量对莫来石-钛酸铝高温窑具性能和显微结构的影响.结果表明:合成的莫来石-钛酸铝复相材料适于制备高温窑具;在1 600℃烧成的窑具试样具有较高的高温抗折强度和良好的抗热震性;合成复相材料的添加量为45%时可获得综合性能好的窑具材料;热态模拟试验表明研制的莫来石-钛酸铝高温窑具适合在低于1 400℃,承重小于8 kg的条件下使用.     

凝胶法片状莫来石粉的制备及应用

采用拟薄水铝石和非晶态超细SiO_2微粉为原料。以溶胶-凝胶工艺制取莫来石凝胶,通过干燥、煅烧研制得片状结晶莫来石粉。初步研究了凝胶法莫来石粉在钛酸铝陶瓷和烧结刚玉砖中的应用。实验结果表明:凝胶粉起到了促进烧结、降低烧成温度的作用,并使钛酸铝——莫来石复相陶瓷和刚玉砖的强度得到了显著提高。     

莫来石凝胶粉──钛酸铝复相陶瓷的研究

初步研究了莫来石凝胶粉──钛酸铝复相陶瓷的室温与高温强度及抗热震性。结果表明，此复相陶瓷具有较高的室温及高温强度以及良好的抗热震性，室温强度的提高主要是由于莫来石抑制钛酸铝晶粒的生长并阻碍裂纹的扩展。高温强度的提高是由于裂纹弥合的结果。     

莫来石凝胶粉—钛酸铝复相陶瓷的研究

初步研究了莫来石凝胶粉－钛酸铝复相陶瓷的室温与高温强度及抗热震性。结果表明，此复相陶瓷具有较高的室温及高温强度以及良好的抗热震性，室温强度的提高主要是由于莫来石抑制钛酸铝晶粒的生长并阻碍裂纹的扩展，高温强度的提高是由于裂纹弥合的结果。     

水解反应诱导凝固成型制备莫来石陶瓷坯体

根据pH值对硅溶胶分散氧化铝浆料稳定性的影响及机理,用一种免脱气水解反应诱导原位凝固成型技术制备了莫来石陶瓷坯体.在pH值为2.0左右,制备得到A12O3固相体积分数为55%、粘度小于1.0 Pa·s符合莫来石化学计量组成的硅溶胶分散氧化铝浆料,利用尿素的自水解反应,将浆料的pH值从2.0调节到5.0,实现浆料的原位凝固成型,浆料无须脱气处理,可成型得到抗折强度为5.H MPa、显微结构致密均匀的莫来石素坯.     

莫来石-钛酸铝高温窑具的研制

在合成莫来石/钛酸铝复相原料的基础上,借助于XRD、SEM和热态模拟试验等手段研究了烧成温度、复相原料添加量对莫来石-钛酸铝高温窑具性能的影响.研究结果表明:合成的莫来石/钛酸铝复相原料适于制备高温窑具;在1600 ℃烧成的窑具试样具有较高的高温抗折强度和良好的抗热震性;复相合成原料添加量为45%时可获得综合性能较好的窑具材料;热态模拟试验表明研制的莫来石-钛酸铝高温窑具适于作为硬磁材料烧成窑具.     

注凝成型制备莫来石–钛酸铝复相陶瓷(英文)

引入10%(摩尔分数,相对于A12O3,下同)MgO和15%SiO2双组分添加剂合成了钛酸铝粉体.采用不同质量比的钛酸铝粉体和工业莫来石,用干压和注凝成型工艺制备了莫来石-钛酸铝(mullite-aluminium titanate,MAT)复相陶瓷.用X射线衍射分析了双组分添加剂对钛酸铝相组成和热稳定性的影响.通过扫描电镜表征了MAT复相陶瓷的微结构.研究了钛酸铝含量对采用于压、注凝2种成型工艺制备的MAT复相陶瓷的弯曲强度和平均热膨胀系数(室温～1 000℃)的影响.结果表明:MgO和SiO2双组分添加剂促进了钛酸铝的形成,增强了钛酸铝的热稳定性.通过注凝成型制备的MAT复相陶瓷比于压成型制备的MAT复相陶瓷具有史均匀的结构和更高的机械性能.当铸酸铝含量为lO%(质量分数,下同),运用注凝成型工艺 制备的MAT复相陶瓷的弯曲强度最大,达110.05 Mpa.     

Gel-casting of fused silica based core packing for investment casting using silica sol as a binder

A novel approach for the fabrication of core packing via silica sol gel-casting is described. Concentrated slurry dispersed in silica sol with high solid loading but low viscosity is successfully prepared at about pH 10.2. In situ consolidation of the slurry is realized through adjustment of NH₄Cl concentration to control the gelation time of the slurry. High compaction and uniform green body is obtained by gel-casting technology without de-airing process. The results from flexural strength tests show that wet gel bodies with 0.5 wt.% calcium aluminate obtained by silica sol gel-casting have exceptionally high strength, which are responsible for the integrity of core packing during autoclaving.     

Dispersion properties of alumina powders in silica sol

The dispersion of alumina powders in silica sol has been investigated by zeta potential, sedimentation, and rheological measurements. Zeta potential of alumina in silica sol changes significantly in comparison with that of alumina in deionized water. This is caused by the absorption of silica colloidal particles with negative charge on the surface of alumina particles. Sol-dispersed alumina slurry shows a minimum in sedimentation volume and viscosity around pH 10. The viscosity depends strongly on the silica sol concentration and reaches a minimum in 10–15 wt.% silica sols. It is proposed that the dispersion and stabilization of alumina particles in silica sol are attributed to the electrostatic and steric effects of the colloidal particles absorption. Effects of pH, solids content and silica sol concentration on the rheological behavior of sol-dispersed alumina slurries are discussed in detail.     

添加剂对酸性硅溶胶及料浆胶凝与流变行为的影响

以酸性硅溶胶及其结合料浆为研究对象,通过对比胶凝时间、黏度、触变环面积、剪切应力等流变参数,研究了聚丙烯酰胺、氢氧化镁、柠檬酸三铵等对酸性硅溶胶及结合料浆流变行为、凝聚过程的作用规律。结果表明:氢氧化镁电离出Mg²⁺促进了酸性硅溶胶的缩合反应,对酸性硅溶胶胶凝过程的影响较为显著;氢氧化镁添加量的增加,增大了胶凝速度,酸性硅溶胶的稳定性下降。聚丙烯酰胺作为阴离子表面活性剂,通过空间位阻效应,缔合溶胶中的氢键,在溶胶中形成三维网络结构,同时聚丙烯酰胺水解吸附在溶胶胶团颗粒表面,加快了SiO₂粒子的絮凝,提高了酸性硅溶胶及其结合料浆的黏度。控制柠檬酸三铵的含量低于10 mg/mL,有助于降低硅溶胶结合料浆的黏度,提高体系的稳定性。     

In situ preparation of inorganic nanoparticles in amino-functionalized porous cellulose particles

Amino-functionalized cellulose particles with a porous structure were prepared by a solvent-releasing method with 1-butyl-3-methylimdazolium chloride ([Bmim]Cl) followed by an amination reaction, and were incorporated with silica. The amino groups provided the base catalyst for the formation of silica on the porous structure during the in situ sol–gel reaction of tetraethyl orthosilicate. After the reaction, no free silica remained in the reaction medium. The microscopic morphologies (specific surface area, pore diameter, and pore volume) of the composite particles were affected by the silica content in the composites, which was controllable by the sol–gel reaction time. When silver nanoparticles were introduced to the pores of the cellulose particles by reduction of AgNO₃ with amino groups, the composite exhibited catalytic ability and recyclability.     

微滴乳液聚合制备PDMS/SiO2纳米复合材料

采用超声分散的方法,以少量八甲基环四硅氧烷(D₄)对硅溶胶粒子进行表面接枝改性。然后在改性硅溶胶存在下,以十二烷基苯磺酸(DBSA)为乳化剂兼催化剂进行D₄的微滴乳液聚合,得到聚硅氧烷(PDMS)/二氧化硅(SiO₂)纳米复合乳液。采用FTIR、TGA、纳米粒度仪、TEM和拉力机分别对样品进行了表征。结果表明:采用超声分散的方法,能够有效地实现硅溶胶粒子的表面改性。通过微滴乳液聚合得到的复合乳胶粒是聚合物包覆二氧化硅粒子的核壳结构形态。SiO₂的引入提高了有机硅复合膜力学性能,增强了热稳定性。     

用于TS-1催化剂回收的陶瓷膜污染机理

Ceramic ultrafiltration membranes were used to separate titanium silicalite-1(TS-1) catalysts from the slurry of catalytic ammoximation of cyclohexanone to oxime.Silica was shown to have a great effect on membrane fouling in the alkaline environment of this system.In the ammoximation system,there are three main silica sources,which are residual silica on the catalyst particles surface during preparation,silica dissolved from TS-1 catalyst particles by ammonia solvent,and silica sol added into the reaction slurry to inhibit the dissolution erosion of the TS-1 catalyst.The silica dissolved by ammonia has been proved to influence membrane fouling most among the three silica sources.This was because the amount of silica dissolved by ammonia was the largest,and the polymerization of silica monomers at high concentration caused colloid particles formation,which led to a dense cake layer depositing on the membrane surface.Meanwhile,the size reduction of catalyst particles caused by alkaline dissolution also increased specific resistances of cake layers.     

纳米二氧化硅的制备及其超声分散行为研究

采用原位表面修饰技术制备了纳米二氧化硅粉体,并以此为原料,采用超声解团聚法制备有机溶剂硅溶胶。探讨了有机溶剂类型、二氧化硅浓度、超声时间对目标有机体系溶胶稳定性的影响,研究了超声时间与溶胶体系黏度的关系,表征了不同超声时间下溶胶的聚集体状态和粒度,阐述了超声解团聚法制备二氧化硅有机溶胶的机理。实验结果表明：乙二醇单甲醚为最佳有机分散介质,最佳分散质量分数为4%;二氧化硅粉体以50~100 nm聚集体分散在有机溶剂中,体系的黏度随着超声时间的延长而变小。     

骨料浸渍硅溶胶对矾土基耐火材料性能的影响

为了改善矾土基耐火材料的力学性能和抗热震性能,分别以SiO2含量(w)为15%和30%的硅溶胶对3~1 mm的矾土熟料粗颗粒进行浸渍处理,再与≤1 mm的矾土熟料颗粒、≤0.074 mm的矾土熟料细粉、α-Al2O3微粉、≤0.074 mm的红柱石细粉、≤0.074 mm的广西白泥、纸浆废液等经配料、成型、干燥、烧成(1400、1450和1500℃保温3 h),制得矾土基耐火材料,同时制备了使用未浸渍3~1 mm矾土熟料的空白试样。结果表明:1)随着烧成温度的升高,试样的常温抗折强度和常温耐压强度呈先升高后降低的变化趋势,其最佳烧成温度为1450℃。2)随着浸渍用硅溶胶浓度的提高,试样的烧后线变化增大,体积密度、常温抗折强度和常温耐压强度降低,高温抗折强度、荷重软化温度和抗热震性能提高,这是由骨料表面硅溶胶层中的SiO2与骨料及周围基质中的Al2O3反应生成了莫来石所致。3)当浸渍用硅溶胶中SiO2含量(w)为15%时,材料的综合性能最优。     

Rheological behavior of hydrophilic silica dispersion in polyethylene glycol

The rheological properties of hydrophilic fumed silica dispersed in polyethylene glycol (PEG) were investigated. The dispersion was prepared by dispersing the fumed silica in PEG with various concentrations. The reversible sol–gel transition was observed over 5 wt % of silica concentration as a function of temperature. The gelation temperature was found to depend on the applied shear stress and silica concentration, and the high shear stress was found to lead to the decrease of sol–gel transition temperature of the dispersion with the same silica concentration. As the silica concentration increases, the sol–gel transition shifts to the lower temperature. © 2006 Wiley Periodicals, Inc. J Apple Polly Sci 103: 2481–2486, 2007     

Isoprene rubber filled with silica generated in situ

We modified synthetic isoprene rubber by means of the in situ generation of silica particles through the sol–gel process starting from tetraethoxysilane (TEOS) as an inorganic oxide precursor. Different reaction conditions were investigated with variations in the initial TEOS content, the reaction time of the sol–gel process, and the presence of a coupling/surfactant agent (octyltriethoxysilane). Organic–inorganic hybrid materials with a silica content up to 70 phr were obtained with the complete conversion of TEOS to silica for a long enough sol–gel reaction time. A very homogeneous dispersion of silica particles was observed in all cases together with a very good adhesion between the filler and matrix. The size of the in situ generated silica was controlled by the appropriate addition of octyltriethoxysilane. Swelling and extraction tests and dynamic mechanical analysis indicated that the vulcanization process of isoprene rubber was perturbed by the sol–gel process; this led to a slight decrease in the crosslinking degree. However, a significant reinforcing effect due to the presence of silica particles was observed for all of the investigated samples. © 2010 Wiley Periodicals, Inc. J Appl Polym Sci, 2011