矿化剂浓度和温度对水热法合成氧化锌晶体形态的影响

采用水热法，通过改变矿化剂浓度和温度合成了具有不同形态的氧化锌晶体。在较低的温度(350℃)，填充度为35％。矿化剂KOH浓度小于2mol／L时，只合成了氧化锌微晶。当矿化剂KOH浓度大于3mol/L时，合成出多种形态氧化锌晶体，大的晶体达到几十到几百微米，小晶体仅几微米。当矿化剂KOH浓度从4mol／L增加到5mol／L时，晶体的大小没有明显改变。在高矿化剂条件下合成的晶体显露完整的晶面结构，主要显露柱面m{1010}、锥面p{1011}、负极面O面{0001}，有时也显露Zn面{0001}。晶体表面出现斑坑，显示出晶体的表面缺陷。在430℃，填充度为35％，矿化剂KOH浓度大于1．5moL／L时。合成了多种形态氧化锌晶体，大晶体有几十到几百微米，小晶体仅几微米。当矿化剂KOH浓度为2mol／L，KBr浓度为lmol/L时，最大晶体的长度达到1mm。矿化剂KOH浓度为4mol/L时，晶体没有增大。粒度较大的氧化锌晶体形状多为六棱锥体，显露柱面m{1010}、锥面p{1011}、负极面O面{0001}。晶体表面光滑，完整性好。质量高于350℃时合成的晶体。     

Influence of MnO_2 Mineralizer on the Crystal Structure,Properties of SiC Kiln Furniture Bonded with Fine Silicon Powder

lINTRODUCTIONSiCkilnfllrniturepossessesgoodhigh-temperaturepropertiesandsmoothness.Itishighlyresistanttowarddeforming,slaggingandthermalshock.Thefurniturecanpracticallyresultinimprovingqualityandproductionofceramicsandiswidelyusedovertheworld.However,SiChassinteringtemperatureofupto2OOO:Ct13landitisdifficulttosinterasproductbyusingcommonkilnfurnace.Toserveashigh-temperaturerefractorykilnfurniture,itmustbemixedwithabonder.Thisworkus-esfinesiliconpowderasabonder,whichisadustproducedfroms…     

Preparation and Structural Defects of Al2-xZrx＋yTi1-yO5 and Al4.54Si1.46O9.73 Multiphase Material

In the study, sludge from the aluminum profile factory and kaolin were used as the raw materials. Through adding ZrO2 mineralizer in different contents, Al2-xZrx+yTi1-yO5 and Al4.54Si1.46O9.73 solid solution multiphase material was prepared to effectively inhibit the decomposition of aluminum titanate solid solution and optimize high temperature property of the multiphase material. With XRD and SEM means, crystalline structure and microstructure of each sample were characterized, and properties of each sample were tested. According to experimental results, the optimal addition amount of ZrO2 mineralizer was determined to be 1.5%. Correspondingly, contents for aluminum titanate solid solution, mullite solid solution and α-Al2O3 were 70.3%, 26.8% and 2.9% respectively, bulk density was 3.20 g/cm3, degree of porosity was 5.57%, water absorption rate was 1.74%, and the once thermal shock rupture strength retention rate was 90.52%.     

水热法可控制备铋铁系化合物材料

本文以Fe(NO₃)₃·9H₂O和Bi(NO₃)₃·5H₂O为反应原料,以NaOH为矿化剂, 利用水热方法制备出几种纯相的铋铁系化合物材料,通过调节NaOH的浓度范围可以很容易的控制铋铁系化合物的物相。在NaOH浓度为0.1~0.4 mol·L^-1区间,可以得到立方相的软铋矿Bi₂₅FeO₄₀,当NaOH浓度提高到0.8~2.0 mol·L^-1区间,可以得到六方钙钛矿结构的BiFeO₃,再提高NaOH浓度至8.0 mol·L^-1以上可以得到正交相的Bi₂Fe₄O₉,在NaOH浓度为12.0 mol·L^-1时可以获得纳米片状Bi₂Fe₄O₉。同时探讨了铋铁系化合物的生长机理。     

无机矿化剂辅助水热合成高长径比的α-Fe2O3多孔纳米线

本文以K₂SO₄为矿化剂,在100 ℃低温水热条件下,制备出大量形貌均一、高分散的直径约40 nm、长度为2~3 μm的α-FeOOH纳米线。该纳米线在300 ℃煅烧2 h后,得到一维形貌保持良好且表面具有多孔结构、长径比可达20的α-Fe₂O₃纳米线。通过XRD、FTIR、TG-DSC、HRTEM、SAED以及N₂物理吸附技术对产物的形貌和结构进行了表征。研究发现,无机盐对一维纳米线形貌的控制至关重要,还详细讨论了K₂SO₄在α-FeOOH纳米线的成核和生长过程中所起的作用。     

Influence of Fe2O3 and V2O5 on Crystalline Structure of Mg-Al Spinel Synthesized by Waste Aluminum Slag

Mg-Al spinel is synthesized by using industrial waste-residue and basic magnesium carbonate in the aluminum factory as the main raw materials. The influence of V2O5 and Fe2O3 mineralizers on the structure, cell parameters and microscopic morphology of synthesized Mg-Al spinel has been discussed. The Mg-Al spinel is characterized by using XRD, SEM and relevant analytical software, such as Philips plus, Rietveld quantification and so on. The experimental results show that certain amounts of V2O5 and Fe2O3 are beneficial to the formation of Mg-Al spinel, and the optimum addition of V2O5 and Fe2O3 is respectively 2wt% and 3wt%. V2O5 has few effects on cell parameters of Mg-Al spinel; but Fe2O3 can form solid solution with Mg-Al spinel in which Mg-Fe spinel can also dissolve to form continuous solid solution. Therefore, with the increase of Fe2O3 content, the cell parameters of Mg-Al approximately present linear increase.     

双矿化剂对合成ZSM-5分子筛酸性和织构特征及其甲醇转化制丙烯催化性能的影响

采用静态水热法在F^--OH^-体系中,以四丙基氢氧化铵为模板剂、偏铝酸钠为铝源、正硅酸乙酯为硅源,合成了纳米SiO₂-ZSM-5分子筛,考察了F^-/Al₂O₃物质的量比对所合成的ZSM-5分子筛织构性质和甲醇转化制丙烯催化性能的影响。结果发现,随着初始溶胶F^-/Al₂O₃物质的量比的增大,产物中SiO₂的含量增大,ZSM-5分子筛的相对结晶度有所降低;同时,分子筛的比表面积和孔容减小、酸强度降低、酸量减少。对于甲醇转化制丙烯,最佳F^-/Al₂O₃物质的量比为12;此时,丙烯选择性高于45%,丙烯/乙烯（P/E）比值大于10。反应机理分析表明,过渡态择形选择性是控制烯烃选择性的重要因素。     

不同矿化剂对水热法合成ZnO晶体形态的影响

研究了在350℃,填充度为35%时,分别以不同浓度的NaOH和KOH为矿化剂,合成具有不同晶体形态的氧化锌晶体。当以KOH为矿化剂,浓度小于2 mol.L-1时,只能合成出微米级晶体,随着矿化剂浓度增加,开始出现大的晶体,最大晶体的长度为50~100μm;如以NaOH作矿化剂,当矿化剂浓度为2 mol.L-1时,即可以合成出个体较大的晶体长度,最大晶体的长度达到100μm。提高矿化剂浓度,有利于合成个体更大的晶体,其长度远远大于以KOH作矿化剂时的晶体长度,最长为200~300μm,证实在350℃,以NaOH作矿化剂比KOH更易获得个体较大的晶体。     

水热法合成Mnx Zn1-xO微晶体

本文采用水热法合成了MnxZn1-xO晶体,水热反应条件为3mol·L-1KOH作为矿化剂,填充度为35;,温度为430℃,在Zn(OH)2中添加一定量的MnO2为前驱物,反应时间为24h.通过X射线能谱仪测量了晶体中的Mn含量,随着前驱物中MnO2含量的增加,晶体中Mn的原子百分比随着增加,Mn最大原子百分比含量超过了2;,晶体的形貌具有纯ZnO晶体的六角柱形特征.显露柱面m{1010}、锥面p{1011}、负极面O面{0001}和正极面{0001}.晶体直径为50～200μm,高度为20～100μm.     

Effects of BaF2 on Preparing Mullite with Sludge from the Aluminum Profile Factory and Pyrophyllite

In this study, sludge from the aluminum profile factory and pyrophyllite were used as major raw materials to prepare mullite. Through determining optimum formula, the optimum calcination temperature and optimum temperature retention time as well as the effects of BaF2 mineralizer on the crystal structure, microstructure and properties of mullite were studied and the optimum BaF2 mineralizer dosage was determined. With XRD and SEM methods, the crystal structure and microstructure of each sample were characterized. With Rietveld Quantification method, crystal phase content in each sample was determined and properties of each sample were tested. Based on the comprehensive analysis result, it was determined that optimum BaF2 dosage was 0.5%, the fairly good calcination temperature was 1550 ℃, and the corresponding mullite solid solution content was 95.8%.