溶胶－凝胶法制备莫来石晶须

用正硅酸乙酯、硝酸铝为原料，采用溶胶－凝胶工艺制备了Ａｌ＿２Ｏ＿３－ＳｉＯ＿２干凝胶，通过高温热处理制得了直径为０．５～２．５μｍ，长径比为５～４０的莫来石晶须。采用ＸＲＤ，ＳＥＭ，ＴＥＭ和ＳＡＤＰ等手段研究了莫来石晶须的晶相组成、形貌与生长方向，发现莫来石晶须是沿其ｃ轴方向生长的。用４ｍｏｌ／ＬＮＨ＿３·Ｈ＿２Ｏ催化的Ａｌ＿２Ｏ＿３－ＳｉＯ＿２溶胶的凝胶化时间越短，经高温热处理后莫来石晶须含量越高。     

溶胶—凝胶法制备莫来石晶须

用正硅酸乙酯，硝酸铝为原料，采用溶胶－凝胶工艺制备了Ａｌ２Ｏ３－ＳｉＯ２干凝胶，通过高温热处理制得了直径为０．５－２．５μｍ，长径比为５－４０的莫来石晶须。采用ＸＲＤ，ＳＥＭ，ＴＥＭ和ＳＡＤＰ等手段研究了莫来石晶须的晶相组成，形貌与生长方向，发现莫来石晶须是沿其ｃ轴方向生长的。     

Al2O3/TC4合金钎焊接头中TiB晶须对接头组织结构及力学性能的影响

分别采用CuTi、CuTi+B和CuTi+TiB2钎料,在钎焊温度为930℃,保温时间为10min条件下,钎焊连接Al2O3和TC4合金。通过扫描电子显微镜、透射电子显微镜和压剪试验等方法,研究了接头中生成的TiB晶须对接头组织结构及力学性能的影响。结果表明:B或TiB2粉的添加均可在钎焊接头中原位自生TiB晶须。当钎料中添加B粉时,接头中原位自生的TiB晶须比添加TiB2时的尺寸小。原位自生的TiB晶须可将Al2O3/TC4合金钎焊接头界面分为5个区域,各区分布满足延性–刚性–延性结构,此结构有助于减小降低接头残余应力,提高接头抗剪强度。采用CuTi+TiB2钎料时,Al2O3/TC4合金钎焊接头的抗剪强度最大为143 MPa,比用CuTi钎料时所获接头强度提高了239%。     

磷石膏制备硫酸钙晶须的初步研究

以磷石膏为原料,直接采用水热法制备硫酸钙晶须,为磷石膏制备硫酸钙晶须的工业化生产提供重要理论依据。实验考察反应温度、料浆初始pH、反应时间、料浆浓度及磷石膏粒度对生成硫酸钙晶须的影响,用扫描电镜观察硫酸钙晶须的形貌,并通过偏光显微镜和图像分析软件分析不同反应条件下制备的硫酸钙晶须的直径和长度。结果表明:反应温度为130~140℃,料浆初始pH为4.0,反应时间为4 h,料浆质量分数为5%,原料粒度为50~75μm是生成硫酸钙晶须的最佳反应条件,在此条件下可制备出平均直径为2μm,长径比为42的硫酸钙晶须产品。     

用天然石膏制备硫酸钙晶须的研究

以天然石膏为原料,采用水热法制备硫酸钙晶须。以电镜作为分析硫酸钙晶须直径的手段,得出硫酸钙晶须的最优化工艺条件为:反应温度为130℃、料浆初始pH为10.0、料浆质量分数为5%、原料粒度小于122μm、反应时间为1.5 h。在此条件下,制备出了平均直径为1.32μm、长径比为76~90的硫酸钙晶须产品。中试试验结果显示,以天然石膏为原料制备硫酸钙晶须的长径比和直径与以纯石膏为原料制备的硫酸钙晶须相当。得出的结论对硫酸钙晶须的工业化生产具有重要的指导意义。     

不同酸对胶凝过程及莫来石晶须形成的影响

以工业纯铝溶胶和硅溶胶为原料,采用溶胶-凝胶工艺制备了莫来石晶须。研究了不同酸对胶凝过程及莫来石晶须形成的影响。结果说明,采用柠檬酸调节溶胶的pH值可以缩短胶凝时间,制备出形貌规则、长径比大的莫来石晶须。     

页岩提钒中和渣制备硫酸钙晶须填料的研究

以页岩提钒中和渣为原料,采用水热法制备硫酸钙晶须,并进行稳定-改性处理,最终制备用于填充塑料的硫酸钙晶须填料。研究了反应温度、反应时间、料浆浓度及助晶剂用量对硫酸钙晶须长径比的影响以及改性剂用量、初始料浆浓度、改性温度及改性时间对硫酸钙晶须改性效果的影响。结果表明,在反应温度为130℃、反应时间为6 h、料浆质量分数为3%、助晶剂六水氯化镁用量为10%的条件下,制备出的硫酸钙晶须长径比达90,但晶须在空气中易水化变粗,长径比降至20以下。在硬脂酸用量为4%、初始料浆质量分数为8%、改性温度为90℃、改性时间为20 min的条件下,制备的硫酸钙晶须填料活性指数达0.72,吸油值为0.278 8 g/g,制得的硫酸钙晶须填料呈棒状或纤维状,表面光滑,结晶度较好,长径比稳定在40~50。结合XRD、SEM、FT-IR分析可知,硬脂酸能有效抑制晶须水化过程,保持晶须晶型及形貌稳定,硬脂酸通过与晶须表面发生化学键链接封闭其亲水活性点而抑制晶须水化。     

专利技术

四氟化硅生产方法，超干燥碳酸钙，一种两亲型纳米二氧化硅的制备方法，一种提高二氧化硅气凝胶热稳定性的方法，超细氧化锌及氧化锌晶须的制备方法     

莫来石晶须的特性及应用

通过溶胶─凝胶工艺制备了莫来石前驱体,加入适当矿化剂经高温煅烧合成了高纯、单相莫来石晶须。XRD及SEM分析结果显示:晶须直径为50～100nm,长度为3～8μm,晶须尺寸均匀性好,表面光洁,直晶率高。运用所制备的晶须制备了多孔基板试样,并与普通粒子堆积法烧成样品显微结构与性能进行比较,进而分析了低维晶须材料与普通粒子的堆积成孔方式的异同。在此基础上,对莫来石晶须在其它方面的应用进行了展望。     

SiC晶须表面涂覆Al2O3的溶胶—凝胶工艺及机理

用异丙醇铝为先驱体通过溶胶-凝胶工艺成功地在SiC晶须表面涂覆了5—30nm的Al_2O_2涂层。认为SiC表面与Al(OC_2H_7)_2(OH)形成配位键并构成胶团是形成涂层的重要机制。研究了溶胶浓度、晶须预处理,晶须直径和反复涂层对涂层效果的影响。     

莫来石晶须的制备

采用化学法制备Ａｌ２Ｏ３－ＳｉＯ２粉料,在氟化物气相存在条件下经过高温合成制得均匀且长径比大的莫来石晶须。研究结果表明,莫来石晶须形成与生长机理为气－固反应机制;铝硅氟化物气相、Ａｌ２Ｏ３－ＳｉＯ２粉料细度、烧成温度及保温时间是制备莫来石晶须的重要工艺条件。     

Synthesis of Mullite Whiskers and Their Application in Composites

Mullite whiskers were synthesized by a vapor-solid reaction. Mullite composition xerogels were fired at 900° to 1600°C with AlF₃ in an airtight container. An average whisker increased in length from 7 μm at 1100°C to 10 μm at 1600°C, whereas an average whisker decreased in aspect ratio from 25 to 10 with increased firing temperature. The whiskers elongated to the c -axis and the side planes were the {110}. A clear lattice image corresponding to (110) lattice spacing up to the edges of the whiskers was observed with high-resolution electron microscopy, and no droplet was observed on the tips of the whiskers. The chemical composition of the whiskers synthesized below 1100°C showed an apparent Al₂O₃-rich composition of about 72 mol%. Composites reinforced by 15 vol% of mullite whiskers in the matrix of 75 vol% mullite/25 vol% Y-TZP enhanced the fracture toughness compared with those materials without mullite whiskers.     

The preparation of mullite foamed ceramics reinforced by in-situ SiC whiskers and their reinforcement mechanism

A SiC whisker-bonded mullite foamed ceramic was prepared by using white clay, industrial alumina and silicon powder as raw materials without solid carbon sources. The XRD, SEM, EDS, and Factsage® software were used to investigate the effect of sintering temperature on the phase composition, microstructure, compressive strength, and Young's modulus of foamed ceramics. Additionally, the synthesis reaction of in-situ SiC whiskers and the effect of their formation on the properties of ceramics were studied. The results showed that the in-situ SiC whiskers with dendrite shapes were formed after firing above 1300 °C at the expense of Si/SiO vapors as well as CO vapor, though there were no solid carbon sources in raw materials, which provided a new idea for the synthesis of SiC whiskers. The formation of SiC whiskers was helpful for improving the compressive strength and Young's modulus of mullite foamed ceramics remarkably. Furthermore, the reinforcement mechanism has been investigated systematically.     

Using Si/SiC solid waste to design urchin-like mullite whiskers for oil-water separation

Using recyclable industrial waste Si/SiC and Al₂(SO₄)₃ as starting materials, urchin-like mullite whiskers were successfully synthesized via the molten salt method. The characterizations were focused on the phase transformations and morphology evolution of mullite whiskers. The circular oxidation-dissolution-precipitation mechanism was proposed for the growth of urchin-like mullite whiskers. Then, the pressing-sintering process was used for fabricating porous whisker-structured mullite ceramics for oil-water separation applications. Physical properties of porous ceramic, including bulk density, apparent porosity, mechanical and thermal shock resistance were measured. It was found that excessive reaction temperature could decompose the mullite, and a suitable temperature for pure urchin-like mullite whiskers was found to be 900°C. To achieve oil-water separation, bionic surface grafting technology was used for coating a hydrophobic and lipophilic material (octadecylamine, ODA) on mullite ceramic. Oil adsorption capacities of the ceramic/ODA for various oils, that is, .27 and .24 g/g for cooking and motor oil, respectively, were successfully achieved.     

氟化铝对红柱石莫来石化的影响

本文主要研究了氟化铝的加入对红柱石矿物转化为莫来石的温度,转化程度以及生成相莫来石的形态的影响.结果表明,加入6wt％氟化铝可以使红柱石矿物在1300℃完全莫来石化;同时氟化铝的加入可以促进莫来石晶体各向异性生长,得到直径为0.5～2.0 μm,长径比为20～40的莫来石晶须,可以用于制备自增韧的莫来石陶瓷或莫来石晶须增强的复合材料.     

Microstructural evolution and densification behavior of porous kaolin-based mullite ceramic added with MoO3

Microstructural evolution and densification behavior of porous kaolin-based mullite ceramic added with MoO₃ were investigated. The results indicated that MoO₃ addition not only lowered the secondary mullitization temperature to below 950?°C, but also facilitated effectively the anisotropic growth of mullite grains. Fine mullite whiskers grew and interlocked with one another in the pre-existing pore regions, in-situ forming a stiff 3D skeleton structure of mullite whiskers, which arrested further densification of the sample. On the other hand, due to the great capillary attraction of small pores, the liquid phase tended to spread over small grains, which favored the growth from small mullite grains into whiskers at the expense of the liquid phase. Consequently, competitive mechanisms of sintering and crystal growth of mullite functioned, which further limited the sample densification. As a result, the total linear shrinkage of the sample added with MoO₃ after firing at 1400?°C was only ??2.75%, and its porosity was retained at as high as 67%.     

Lightweight and thermal insulation mullite fibers/whiskers hierarchical framework materials: Low-temperature in-situ growth method and mechanism

Mullite fibers/whiskers hierarchical structure materials (MFWs) were prepared via the three-stage method, i.e. seeds breeding, precursors introducing and whiskers growth. The mechanism of low-temperature in-situ synthesis of mullite whiskers during gas-phase reaction process has been discussed in detail. The seeds bred on mullite fibers (MFs) are the growth points and can effectively reduce the subsequent growth temperature of mullite whiskers (MWs). The precursors composed of aluminum source, silicon source and catalyst provided raw materials for whiskers growth. Under the heat treatment temperature of 800 °C, mullite seed grains were guided to in-situ transform into MWs. Moreover, MFWs fabricated via low-temperature in-situ growth mechanism on the MFs present low density (0.103–0.147 g/cm³) and ultralow thermal conductivity (0.0426–0.0514 W·m^?1·K^?1). Due to the lower whiskers growth temperature in this work than the ones in the most recent literatures, the three-stage method can be regarded as a viable strategy for low-temperature in-situ growth whiskers.     

Preparation of self-reinforcement of porous mullite ceramics through in situ synthesis of mullite whisker in flyash body

Self-reinforced porous mullite ceramics were fabricated by a starch consolidation method with flyash, different aluminium sources (Al(OH)₃ and Al₂O₃) and the additive AlF₃ as raw materials. The reinforcement mechanism of needle-like mullite whiskers through in situ synthesis in ceramic body was investigated. The bulk density, apparent porosity and bending strength of the samples were tested. Phase compositions and microstructures of the sintered samples were measured by XRD and SEM, respectively. It showed that AlF₃ as additive was helpful to the formation of mullite whiskers at a low temperature. As the aluminium sources, Al(OH)₃ was more suitable for the preparation of mullite whiskers than Al₂O₃. The in situ synthesized mullite whiskers formed an interlocking structure, which enhanced the mechanical strength of the porous mullite ceramics. Porous mullite ceramics with bending strength of about 100 MPa and apparent porosity of about 55% were made at 1550 °C.     

原位合成莫来石晶须及其微观结构的研究

本文通过以高岭土、工业氢氧化铝为原料,添加适量AlF3和V2O5,在高温下原位合成了莫来石晶须,采用扫描电镜（SEM）研究了合成的莫来石晶须的微观形貌,探讨了莫来石晶须的生长机理,并讨论了影响莫来石晶须生长的相关因素.在综合考虑影响莫来石晶须生长的相关因素后,制备出晶须多、长径比大、分布均匀的莫来石晶须样品.