规则镁铝水滑石超分子的组装及其结构分析

以MgCl_2·6H_2O、AlCl_3·6H_2O、Na_2CO_3为原料,采用乙二醇-水热法组装了超分子结构镁铝水滑石,考察了乙二醇-水热法对水滑石晶形、结构、分散性、规整性的影响.样品用XRD、SEM、TEM、IR、TG-DTA、N_2吸附-解吸进行了表征.结果表明,在水热反应体系中加入15(vol)%的乙二醇,于T-180℃反应16h可获得晶形好、板层结构显著、规整性好、分散性好的优质镁铝水滑石,谢乐公式估算粒子粒径为36nm左右.     

Mg(OH)2晶须的制备

以MgCl2为原料,NaOH为沉淀剂,研究了它们的浓度配比、反应温度、晶化温度、晶化时间、晶化方式等因素对形成Mg(OH)2晶须的影响. 结果表明,当n(MgCl2): n(NaOH)=1.20: 1.92、混合温度Tm=86 ℃、晶化温度Tc=100 ℃、晶化时间Time=5.5 h时,可以得到发育不完全的初级Mg(OH)2晶须. 若改用水热法晶化,可得到发育较好的Mg(OH)2晶须. 在此基础上,若在NaOH溶液中加入一定量的有机溶剂OR(NaOH浓度不变)时,即可得到发育更完善的Mg(OH)2晶须. 电子显微镜照片显示,粒子呈晶须形状,粒度分布均匀,分散性好,晶形好,纯度高. 并对晶须生长机理进行了初步分析.     

分级多孔γ-Al2O3空心微球微波水热法制备及其对刚果红的快速吸附

以KAl(SO₄)₂和尿素为前驱体,通过微波水热法于180 ℃反应20 min,经600 ℃焙烧2 h制得分级多孔γ-Al₂O₃空心微球.所制备的样品被用于吸附典型有机染料刚果红(CR)溶液.结果表明,制备的γ-Al₂O₃空心微球直径为0.8-1.0 μm,厚度约为200 nm.此γ-Al₂O₃空心微球具有高的比表面积(243 m²·g^-1)和分级大孔-中孔结构,此结构非常有利于液相过程中的质量传递.微波水热法制备的γ-Al₂O₃空心微球比水热法制备的γ-Al₂O₃和商用的γ-Al₂O₃样品显示出更快和更强的吸附性能.此样品的吸附数据很好地符合假二级速率方程和Langmuir吸附理论模型.从Langmuir吸附理论模型计算得到微波水热法制备的γ-Al₂O₃空心微球的最大吸附量(q_max) 25 ℃时高达515.4 mg·g^-1.由于具有分等级结构、高比表面积、大的孔容和吸附能力,微波水热法制备的γ-Al₂O₃空心微球样品有望成为一种具有很好应用潜力的环境吸附剂.     

双注-水热法制备高分散氢氧化镁纳米片

本工作以氯化镁、氢氧化钠为原料，氯化钠为衬底溶液，探讨了采用双注-水热法制备高分散氢氧化镁纳米片的可行性。结果表明：采用双注方式或提高衬底溶液氯化钠浓度均有利于降低反应体系过饱和度，改善常温产物的结晶性和分散性；对常温合成的氢氧化镁进行水热处理可进一步提高产物的结晶度，形成形貌规则、粒径分布窄、分散良好的氢氧化镁纳米片。     

高分散性片状阻燃型氢氧化镁的制备

以轻烧氧化镁为原料, 通过水化水热法制备高分散性片状氢氧化镁. 考察了不同的水化温度、水化时间、水热时间和分散剂体系对氢氧化镁材料形貌的影响. 采用X射线衍射(XRD)、扫描电子显微镜(SEM)、全自动氮物理吸附仪(ASAP)等对所制得的氢氧化镁颗粒的物相、形貌和比表面积进行了分析. 结果表明, 通过水热反应控制和分散剂的加入, 可以得到高分散性片状的阻燃型氢氧化镁.     

水热法合成单分散ZnS微球

以醋酸锌、硫代乙酰胺为原料, P123表面活性剂为模板, 采用水热法, 成功合成ZnS微球, 并提出其可能的形成机理. 通过XRD, TEM, FT-IR, N₂吸附-脱附表征, 发现该微球由ZnS纳米颗粒组成, ZnS纳米颗粒尺寸为6～7 nm; 微球直径500～600 nm, 具有单分散性, 表面光滑, 大小均匀; 在4000～400 cm^－1波段具有热红外透过性等特点, 有望在光、电、磁等领域发挥其潜在的应用价值.     

综合利用稻壳制备木糖、电容炭与硅酸钙晶须

利用酸水解稻壳中的半纤维素制备木糖, 并将糖渣经过炭化后分离出碳和硅, 碳采用稀碱溶液活化改性制备电容炭, 硅采用水热法合成了硅酸钙晶须, 从而使稻壳所有组分得到充分利用. 采用循环伏安(CV)和恒流充放电(GCD)研究了电容炭的电化学性能. 通过X射线衍射(XRD)和扫描电子显微镜(SEM)对所得硅酸钙晶须的结构和形貌进行了表征. 实验结果表明, 稻壳酸水解的最优条件为硫酸浓度7%(质量分数)、 固液比(g/mL)为1:8、 反应时间为2.0 h, 在该条件下, 一次水解、 二次水解和三次水解的木糖收率(Y₁/Y₂/Y₃)和浓度(质量分数, C₁/C₂/C₃)都能达到最大值, Y₁=98.5%, C₁=3.6%; Y₂=85.4%, C₂=6.3%; Y₃=76.6%, C₃=9.0%. 采用15 mL 8%(质量分数) NaOH稀碱溶液活化改性制得的电容炭(AC/15)比电容值为77.32 F/g, 而且具有较好的倍率性和循环稳定性; 硅酸钙晶须为扫帚状针钠钙石晶须.     

Nd-Fe-MoO42-氰桥混配聚合物修饰铂电极的丙三醇电催化氧化

利用软模板结合电沉积法制备了一种有序化氰桥混配聚合物修饰铂电极（Nd-Fe-MoO₄^2-/Pt）,用循环伏安法研究了在该化学修饰铂电极的丙三醇电催化氧化,并重点讨论了支持电解质的H⁺和SO₄^2-浓度、丙三醇浓度、扫速等因素对丙三醇电催化氧化活性的影响. 结果表明,在弱酸性硫酸钠支持电解质中,适当量SO₄^2-的存在有助于提高Nd-Fe-MoO₄^2-/Pt电极的丙三醇电催化氧化电流;-0.2 ~ 0.3 V电位区间内,其丙三醇氧化峰电流1与循环伏安曲线扫描速率的平方根之间呈现良好的线性关系,体现了扩散控制的反应特性;Nd-Fe-MoO₄^2-/Pt电极的丙三醇电催化氧化电流密度值约为裸铂电极的4倍,而丙三醇电催化氧化反应的表观活化能相对较小,修饰电极的电催化氧化呈现了明显的协同效应,其电催化氧化活性高、电流响应快、催化稳定性好.     

铁掺杂铈基复合氧化物CO催化还原NO的性能研究

采用浸渍法、水热法和微波加热法制备铁掺杂的铈基复合氧化物催化剂,研究温度、铈铁摩尔比、制备方法对铈基复合氧化物的催化还原性能的影响,并且使用BET, NO-TPD, H₂-TPR, XRD, Raman等对催化剂进行表征分析。结果表明：随着温度的升高,NO转化率是一个先不断增加后趋于稳定的过程;无论是浸渍法、水热法还是微波加热法,最佳铈铁摩尔比均为10∶2; 3种制备方法的催化活性顺序：微波加热法>水热法>浸渍法。微波加热法制备的铈基复合氧化物催化剂在500℃的脱硝率为76%,脱硝率在700℃达到99%。通过XRD和Raman表征说明Fe³⁺取代Ce⁹⁴⁺进入到CeO₂晶格中,改变CeO₂的萤石结构,增加氧空位,造成晶格畸变。     

Ce1-xGdxO2-x/2的溶胶-凝胶法合成及其性质

利用溶胶-凝胶法合成了Ce₁-xGdxO_2-x/2(x=0.1～0.6)系列固体电解质,系统地研究了其结构、热膨胀系数和导电性.XRD结果表明,160℃即完全形成立方萤石结构.由于溶胶-凝胶法合成的物质粒度均匀,颗粒小,故在较低温度(1300℃)时即可形成高致密样品,此温度明显低于传统的高温固相法烧结温度(1600～1650℃).高温X射线衍射测得Ce_0.8Gd_0.2O_1.9的热膨胀系数为8.125×10^-6K₁.阻抗谱表明,溶胶-凝胶法合成可减少或消除固体电解质的晶界电阻,600℃时Ce_0.8Gd_0.2O_1.9的电导率为5.26×10^-3S/cm,活化能E_a=0.82eV.     

Study of In Situ Formation of Magnesium Hydroxide Whisker via Basic Magnesium Chloride Whisker Regulated by Organic Parcels at Low Temperature

In this work, we demonstrate an in situ phase conversion from basic magnesium chloride（BMC） into magnesium hydroxide whisker by using polar organic solvent at low temperature. The morphology and phase composition of magnesium hydroxide whiskers prepared at different reaction temperature, alkali concentration and organic solvent were analyzed by X-ray diffraction（XRD） and scanning electronic microscope（SEM）. It was found that when one of the organic solvents such as absolute ethyl alcohol, butanol, polyethylene glycol（PEG-400）, acetone, et al. was selected as the template, the precursor BMC can transform into whisker-like magnesium hydroxide through precipitate transformation in low temperature and non-hydrothermal system. It can be reasonably explained that the regulation of Mg^2＋ solubility by those organic solvents and the sustained release of Mg^2＋ dissolution by organic adsorption played a significant role in the formation of magnesium hydroxide whisker via BMC whisker as the precursor.     

Effects of cellulose whiskers on properties of soy protein thermoplastics

Environmentally-friendly SPI/cellulose whisker composites were successfully prepared using a colloidal suspension of cellulose whiskers, to reinforce soy protein isolate (SPI) plastics. The cellulose whiskers, having an average length of 1.2 microm and diameter of 90 nm, respectively, were prepared from cotton linter pulp by hydrolyzing with sulfuric acid aqueous solution. The effects of the whisker content on the morphology and properties of the glycerol-plasticized SPI composites were investigated by scanning electron microscopy, dynamic mechanical thermal analysis, differential scanning calorimetry, ultraviolet-visible spectroscopy, water-resistivity testing and tensile testing. The results indicated that, with the addition of 0 to 30 wt.-% of cellulose whiskers, strong interactions occurred both between the whiskers and between the filler and the SPI matrix, reinforcing the composites and preserving their biodegradability. Both the tensile strength and Young's modulus of the SPI/cellulose whisker composites increased from 5.8 to 8.1 MPa and from 44.7 to 133.2 MPa, respectively, at a relative humidity of 43%, following an increase of the whisker content from 0 to 30 wt.-%. Furthermore, the incorporation of the cellulose whiskers into the SPI matrix led to an improvement in the water resistance for the SPI-based composites.     

氧化镁两步法制备阻燃型氢氧化镁

以氯化镁焙烧生成的氧化镁为原料,采用两步法即先水化后水热的方法制备出六方片状氢氧化镁。考察了水化时间、水热时间和温度及水热添加剂氢氧化钠浓度对氢氧化镁材料形貌的影响。研究表明,水化时间超过3h,氧化镁水化率基本不变,水热温度越高对晶体形貌改善越大,水热时间的延长可促进晶体粒径及厚度的增加,但是对晶体的宽厚比改变不大。水热添加剂氢氧化钠浓度的增加可明显地提高晶体结晶度,减小晶体微观内应变,提高粉体分散性。     

晶须概念的泛化与学术影响

最初只称单晶短纤维为晶须,稍后结晶较好的多晶纤维也被称为"晶须",现在无定形纤维也归进了晶须专著,通过对晶须概念泛化过程的反思,希能澄清学术著作中10多年来相沿的一个模糊认知。     

半水硫酸钙晶须的水化机理及稳定性调节

通过探讨半水硫酸钙晶须(HCSW)贮存过程在空气中形貌和晶形的变化,研究了半水硫酸钙晶须的水化机理,分析了不同处理方法对其稳定性的调节。研究发现,HCSW的水化是由晶须表面的-OH基团和Ca^2+活性位点以及HCSW存在的内部通道引起的,煅烧和二元醇改性均可提高硫酸钙晶须的耐水性。结果表明,煅烧后,半水硫酸钙晶须转化为无水可溶硫酸钙晶须和无水死烧硫酸钙晶须,易于水化的内部通道消失,耐水性增强;水热合成过程二元醇的加入,可利于醇羟基吸附在HCSW的(200)、(020)和(220)表面,阻止H2O分子中羟基在晶须表面的吸附,进而提高晶须的耐水性,当添加剂为三乙二醇(TEG)且浓度为18.8 mmol·L^-1时,HSCW在空气中耐水稳定性不小于7 d。     

基于纳米氢氧化镁稳定的Pickering乳液悬浮聚合制备盔甲结构聚苯乙烯@氢氧化镁复合微球

以苯乙烯为单体、 偶氮二异丁腈(AIBN)为引发剂、 片状纳米氢氧化镁(MH)为Pickering稳定剂, 采用悬浮聚合法制备盔甲结构的聚苯烯@氢氧化镁(PS@MH)复合微球. 采用扫描电子显微镜(SEM)、 能谱分析(EDS)、 傅里叶变换红外光谱(FTIR)、 X射线衍射(XRD)、 热失重分析(TGA)和微型燃烧量热分析(MCC)等对PS@MH复合微球进行表征, 确认了其形貌和结构: 纳米氢氧化镁紧密包覆在聚苯乙烯微球表面, 形成了以纳米氢氧化镁为外层、 聚苯乙烯为内球的盔甲结构复合微球; 同时证明了具有盔甲结构的PS@MH复合微球能降低热释放速率, 抑制聚合物的降解. 该方法操作简单, 成本低廉, 制得的盔甲结构PS@MH复合微球粒径尺寸小、 分布窄, 球形度较高.     

A novel approach for the formation of Mg(OH)2/MgO nanowhiskers on magnesium: Rapid anodization in chloride containing solutions

In the present work we report on the electrochemical formation towards layers of multiscale MgO nanowhiskers by a two step approach. First, metallic magnesium was anodized under “high-voltage”-conditions in chloride containing ethanol/water mixtures. This results within seconds in the formation of dense areas of magnesium hydroxide nanowhiskers on the surface. The individual as-grown whiskers have a needle tip shape, and a length depending on the growth time of up to 20 μm. The whiskers can be transformed to MgO by a thermal annealing process. To gain more insight into this very rapid growth process, the paper describes the influences of the key parameters of the anodization (pH, ion-concentration, electrolyte composition) and the effect of the thermal treatment on the morphology. All steps were characterized using SEM, EDX, XRD and XPS measurements.     

Surface treatment of magnesium oxysulfate whiskers through plasma polymerization

The surface of magnesium oxysulfate (MOS) whiskers was treated through plasma polymerization to increase the compatibility between the MOS whiskers and a polymer matrix. Different plasma parameters were chosen to determine the most hydrophobic coating. The surface structure of the plasma-treated MOS whiskers was examined. The MOS whiskers retained their crystal structure after plasma treatment, as shown by X-ray powder diffraction (XRD) analyses. X-ray photoelectron spectroscopy (XPS) and Fourier transform infrared (FT-IR) spectroscopy analyses revealed that a polymer sheath was formed on the surface of the MOS whiskers, and interfacial chemical bonds were generated between the polymer sheath and the MOS whiskers. The thin-layer polymer sheath was uniform around the entire surface of the MOS whiskers and exhibited a typical amorphous structure, as determined by transmission electron microscopy (TEM) combined with selected area electron diffraction (SAED) analyses. The possible reaction mechanism on the surface of the MOS whiskers under plasma treatment was then proposed. Finally, the effect of surface treatment was evaluated by scanning electron microscopy (SEM), measurement of the contact angle and contact angle hysteresis, and torque rheometer. Results showed that plasma treatment could markedly increase the hydrophobicity of the MOS whiskers' surface, effectively reducing the agglomeration and improving the dispersibility of the MOS whiskers in the matrix, which results in the improved compatibility between the MOS whiskers and the polyvinyl matrix, as well as the processability of the composites.     

Polymer-assisted growth of molybdenum oxide whiskers via a sonochemical process

Whiskers of molybdenum oxides with high aspect ratios were synthesized from peroxomolybdate precursor solutions in the presence of small amounts of poly(ethylene glycol) (PEG) via a sonochemical process at temperatures of 25-70 degrees C. Irradiation with ultrasound reduces the time needed for the growth of micrometer-sized whiskers from weeks to a few hours. The simplicity of the sonochemical approach also compares favorably to a hydrothermal/solvothermal process. The morphology, crystal structure, and other characteristics of the whiskers were characterized by scanning electron microscopy, transmission electron microscopy, selective area electron diffraction, energy-dispersive X-ray spectroscopy, wide-angle X-ray diffraction, Raman spectroscopy, thermogravimetric analysis, differential scanning calorimetry, and the Brunauer-Emmett-Teller method. The surface area of the calcified molybdenum oxide whiskers (55.4 m2/g) was found to be much higher than those of molybdenum oxide nanofibers (35 m2/g) or nanorods (13.4 m2/g) The growth rate of various crystal faces could be postulated to be controlled by the binding of peroxomolybdate ions to pseudo-crown ether cavities formed by PEG. The reduction of molybdenum oxide to produce mixed-valent oxides and their growth could also be controlled by the reducing ability of PEG. The aspect ratio of the molybdenum oxide whiskers increased with decreasing concentration in the initial peroxomolybdate precursor solution. Whether the precursor solution species was H2Mo2O3(O2)4(H2O)2, H2MoO2(O2)2, or MoO2(OH)(OOH), the peroxide group in all the species disproportionates to give the final product MoO3 by a catalytic process. On the basis of experimental evidence of the dual role of glycols, a mechanism for the growth of the molybdenum oxide whiskers is proposed.     

氧化镁两步法制备阻燃型氢氧化镁

以氯化镁焙烧生成的氧化镁为原料,采用两步法即先水化后水热的方法制备出六方片状氢氧化镁。考察了水化时间、水热时间和温度及水热添加剂氢氧化钠浓度对氢氧化镁材料形貌的影响。研究表明,水化时间超过3 h,氧化镁水化率基本不变,水热温度越高对晶体形貌改善越大,水热时间的延长可促进晶体粒径及厚度的增加,但是对晶体的宽厚比改变不大。水热添加剂氢氧化钠浓度的增加可明显地提高晶体结晶度,减小晶体微观内应变,提高粉体分散性。