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To date, many investigations have focused on the ceramic fibers, and some methods such as melt/drawing method, slurry method, solution dipping method, CVDmethod, CVR method, sol-gel method, preceramic polymer method, hydrothermal method have been developed for the preparation of the ceramic fibers.

各种制备方法都各有优缺点,各种制备技术因所制备的纤维性能和用途不同而使其依然发挥各自不同的作用,但纵观连续陶瓷纤维制备技术的发展轨迹,可以发现溶胶-凝胶法日益成为研究与开发的主流。

Producted RF and CRF aerogels by process of sol-gel technics, dynamic-exchange, CO2 supercritical drying, and procedural increase in temperature carbonization methods, which have eximious capability and nanometer network structure; Systemic analysis various factors which effect gel course, such as ratio of reactants and the dosage of catalyst, and probed into the better experiments conditions(the concentration of resorcinol and formaldehyde is more than 2% and the value of R/C is between 50 and 300); During gel course , primary investigated the viscosity curve and particle size distribution of sol-solution, and analyzed the reason of catalyst dosage effects particle size of gel, and confirmed that the up-growth of gel follows the theory of " polymerize increase ".The experiment results indicated that ultrasonic with unvarying temperature disposal shortened gel time and optimized quality of gels, and the factors of ultrasonic effect gel reaction velocity were analyzed; Prepared organic aerogels using compounds of resorcin and hydroquinone substitute resorcinol reacts with formaldehyde the first time, and also optimized the proportion of resorcinol and hydroquinone (the proportion of hydroquinone in 10%~40%).

采用溶胶-凝胶工艺结合动态溶剂交换、CO2超临界流体干燥与程序升温碳化方法制备出性能优良、具有纳米网络结构的RF与CRF气凝胶;深入研究了反应物配比催化剂用量等条件对凝胶过程的影响,得到了较佳的RF凝胶制备条件(RF浓度应大于2%,R/C值取50~300);初步研究了凝胶过程中的粘度、粒径变化情况,分析了催化剂用量影响凝胶中粒子尺度的原因,在实验上印证了凝胶生长遵循"聚增长"的理论;通过引入超声波改进了RF气凝胶的制备工艺,缩短了凝胶反应时间,提高了凝胶品质,并探讨了超声波促进RF凝胶反应作用的原因;首次用对苯二酚与间苯二酚复配制备了混合有机气凝胶,优化出复配比(对苯二酚含量为10%~40%)。2。

Compared with other methods, the present solvent thermal method can produce ITO nano-powders with high purity and uniform particle size. The manipulation is very simple and convenient and no calcination process is needed. The reaction temperature can be as low as 190 ℃, which is by far the lowest temperature in ITO nano-powder preparation. The sample also gives a good dispersion property benefited from the unique solvent thermal reaction environment.

结果表明,制备的ITO纳米粉体为立方晶相,粉体的平均颗粒小于100 nm;与已有的ITO纳米粉体制备方法相比,本溶剂热法制备过程无需高温烧结、流程简单,反应过程所需的温度可低至190 ℃,是迄今为止文献报导制备ITO的最低温度,同时所得产物纯度高、粒度均匀、分散性很好。

The experimental results show that the mean particle size of griseofulvin precipitated by RESS is smaller than 1, 0μm, narrow distribution and 95% fine particles is smaller than 1. 0μm. Increase of the pre-expansion pressure, the extraction temperature, the expansion chamber temperature, the spraying distance, the concentration of cosolvent and decrease of the nozzle diameter resulted in decrease of the particle size under the operating condition studied. Enhancement of the pre-expansion temperature resulted in increase of the particles size. The SEM of GF shows that the shape of original is atactic and a wide size distribution, but the microparticles obtained by RESS is reverse. Similar melting points and XRD patterns were observed for the original material and the precipitates obtained by RESS.

实验结果表明,用含夹带剂的RESS法制备的灰黄霉素微粒的平均直径在1μm左右,且分布均匀,95%微粒在1μm以下,仅用CO〓作为超临界流体制备的微粒与上述方法制备的微粒的平均直径和分布相似,只是产量太低,而用机械法制备的微粒平均直径在3μm左右且分布较宽;不同的过程参数对沉析微粒尺寸有不同的影响,预膨胀压力、膨胀室温度、溶解温度以及夹带剂浓度的提高或增大,均可使沉析微粒的直径变小;预膨胀温度提高,所得微粒的直径变大;喷射距离的增加,沉析微粒的直径变小;喷嘴直径越小,由此制得的微粒的直径就越小;根据实验结果还可知道,通过理论计算的马赫盘处微粒的直径可以较好地估计出膨胀室中收集到的微粒的直径。

For double jet method, effects of used solvent, shape of stirrer, adding reactant position, reaction temperature, excessive silver ion concentration in reaction solution and adding rate on the nucleus formation, and growth of silver behenate crystal were systematically studied.

本文分别采用单注沉淀法和双注沉淀法制备了山嵛酸银晶体,通过对两种制备方法的对比及优选,最后确定双注沉淀法更适合制备细粒径的山嵛酸银,通过采用SEM、TEM等对山嵛酸银晶体形貌的表征发现,制备山嵛酸银所使用的溶剂、搅拌方式、加料的位置、反应温度、反应初始液中银离子浓度及加料速度等,均对山嵛酸银的晶体成核与生长有一定的影响。

The method for the production thereof is that as the main ingredient, the cornsilk powder is produced into the cornsilk soft capsule by cornsilk powder preparation, capsulation liquid blending, capsule shell cellophane preparation and soft capsule pill preparation, making effective use of cornsilk.

制备方法是以玉米花丝粉为主料;经玉米花丝粉制备、囊化液调配、囊壳胶膜制备、软胶囊丸制备的过程制得玉米花丝软胶囊。

Composition of suspension will chang from titanium monoxide to titanium dioxide during standstill procedure. Experimental results show that the proposed method can successfully prepare the anatase phase of titanium dioxide .In the photocatalysis experiment, the prepared titanium dioxide nanofluid absorbs the Ultraviolet when light wavelength was 360 to 380 nm. Adsorption experimental results show that the efficiency of absorbing methylene blue using TiO2 is higher than that for TiO2 (Degussa P-25) or ZnO. Depigmentation of methylene blue experimental using TiO2 can depigmentize methylene blue reach 100% in 60 min.

悬浮液所含之奈米颗粒在静置过程中,成份方面会由似一氧化钛转变为二氧化钛;在结晶组成方面,所制备之二氧化钛颗粒之结晶组成为锐钛矿结构;在光催化方面,所制备之奈米二氧化钛悬浮液在光波长360nm~380nm时产生吸收紫外光现象,在吸附实验中本制程所制备的二氧化钛颗粒的吸附效果优於商用的二氧化钛及氧化锌,在亚甲基蓝的脱色实验中本制程所制备的二氧化钛颗粒能在60分钟内达到脱色率100%。

The chapter two was focused on the samarium diiodide promoted organic reactions and their applications in organic synthesis, firstly, a new synthesis of highly substituted cyclopentadienes from a,β-alkynone promoted by samarium diiodide was investigated and the highly substituted cyclopentadienes were prepared in moderate to good yields under mild conditions. Secondly, the Michael addition and Michael-aldol tandem reaction of diorganyl diselenides or diorganyl disulfides with α,β-alkynones mediated by samarium diiodide were studied and a series of alkenylsulfides and alkenylselenides were prepared in good yields. Then the highly regioselecfive nucleophilic addition of the allylsamarium bromide to α,β-alkynones were explored. We found that the allylsamarium bromide reacts with α,β-alkynones to afford regiospecificly 1. 2-nucleophilic addition products in good yields under mild condition. At last we studied the coupling reaction of aryl halides promoted by NiCl〓/PPh〓/Sm〓.

第二章 研究了二碘化钐、金属钐促进的有机反应:1、二碘化钐促进下α,β-炔基酮的偶联环化反应,提供了一种制备多取代环戊二烯的新方法;2、二碘化钐促进下的二硫醚、二硒醚与α,β-炔基酮的Michael加成反应,为高产率地制备多取代的烯基硫或烯基硒化合物提供了方便可靠的新方法;3、二碘化钐促进下的二硫醚、二硒醚与α,β-炔基酮和醛、酮的Michael—aldol串联反应,提供了一种一锅法高产率地制备多取代的含硫的烯丙基醇或含硒的烯丙基醇类化合物的方便可靠的原子经济性的新方法;4、烯丙基溴化钐与α,β-炔基酮的高度区域选择性的1,2-亲核加成反应;5、NiCl〓/PPh〓/Sm〓促进的卤代芳烃的偶联反应-一种从各种卤代芳烃制备联苯类化合物的有效方法。

The characters of powder are connected with the inside structure and synthesize-technics of materials. In this paper, we want to search a optimize technics of materials synthesizing, and prepare a kind of nanosize powder which shape like ball and have good dispersed character. At the same time, we want to obtain a bridge structure of Zn-O-Tb through dopping of Tb, which can achieve efficient energy transfer from ZnO hosts to excited states of dopants, The doped powder can eradiate blazing green light because of efficient emission buildup from dopants and ZnO hosts, and the powder can emission a pure light. And we want to research the structure in doped ZnO for the further research of low-tension fluorescence of ZnO.

粉体的这些特性无不与其内部结构特征和制备工艺有关,基于这些,本文的实验目的是希望能寻找一种合适的制备方法和优化工艺,制备分散性好的球形纳米颗粒,希望改善其表面形貌,同时,通过铽掺杂,希望得到一种Zn-O-Tb桥联结构,实现氧化锌基体向铽发光中心的能量传递,希望铽中心特征发射和氧化锌绿光发射能有效叠加增强,改善粉体的单色性,制备出好的复合粉体,分析清楚其结构,从而为后续低压荧光特性研究作准备。

Ni-P-mCMC/mCS bipolar membrane was prepared from carboxymethyl cellulose modified with phosphorylated agent as a cation exchange layer and chitosan modified with glutaraldehyde as an anion exchange layer. The electrolysis cell was constituted by Ni-P-mCMC/mCS BPM as a septum for electrogenerating furfural alcohol and furoic acid.

以磷酸化试剂改性羧甲基纤维素钠制备了阳膜层,以戊二醛改性壳聚糖制备了阴膜层溶胶,将阴膜层溶胶流延于阳膜层上,制备了P-mCMC/mCS双极膜,而后以化学镀方法在阳膜层表面镀镍,制备了Ni-P-mCMC/mCS双极膜,并应用于成对电合成糠醇、糠酸。

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