液相剥离法制备超薄氧化钛纳米薄片

自石墨烯问世以来,纳米薄片材料以其独特的二维结构和电学性能,被视为未来电子器件的优秀备选材料。其中,二维氧化钛纳米薄片在减薄至纳米厚度时仍具有高介电常数,是一种很好的绝缘材料,但较小的横向尺寸限制了其应用。采用晶体的高温熔融生长法和层状材料的化学液相剥离法相结合,制备了单层和薄层的氧化钛(Ti_(0.87)O_2~(0.52-))纳米薄片,并结合X射线衍射仪(XRD)、扫描电子显微镜(SEM)等材料分析手段对其制备工艺进行了优化。通过降低高温熔融生长过程中的降温速率减少了副产物的生成,从而提高了产物的纯度,并将生成前驱体钛酸盐(KTO)的尺寸由约20μm增大至约200μm。还通过控制化学液相剥离过程中TBAOH溶液的浓度得到了剥离效果更好的氧化钛纳米薄片,并利用能谱仪(EDS)和原子力显微镜(AFM)等分析了氧化钛纳米薄片的形貌和成分。还利用静电吸引将氧化钛纳米薄片拼接成大面积的纳米薄膜,并通过超声处理大大减小了拼接时样品的重叠和空白。     

专利信息

一种陶瓷涂层的制备方法　本发明公开了一种陶瓷涂层的制备方法,涉及化工、环境和材料加工领域,以陶瓷粉末为原料,采用冷喷涂方法制备陶瓷涂层,特别是制备氧化钛光催化涂层。若以氧化钛块体粉末或氧化钛团聚粉末为原料,采用冷喷涂在基体上沉积二氧化钛涂层。按本发明制备的Ti O2涂层,能够在小于600℃的条件下形成涂层,可以将原始粉末的结构与性能较好地移植到涂层中,尤其是在纳米结构涂层制备和高性能光催化涂层制备方面具有突出地优越性。该方法工艺简单、生产成本低廉、可控性好、对基体影响小。本发明的实施将可以制备结构与性能更加优…     

锂离子电池中高容量Si-Cu/C复合负极材料的制备与性能研究

采用高能球磨方法制备了用作锂离子电池负极材料的Si—Cu／C复合材料。X射线衍射和扫描电子显微镜结果表明，复合材料中Si和Cu5Si是共存的，活性硅颗粒均匀地分散在石墨和惰性的铜硅合金基体中。电化学测试在电流密度0．2mA·cm^-2，电压范围0—1．4V条件下进行，其结果表明高分散Si—Cu／C复合材料首次可逆容量为524mAh·g^-1，远高于目前普遍使用的中间相碳微球；循环寿命也远优于同粒度的硅单体，经过30次循环后容量仍保持531mAh·g^-1。其高比容量和良好的循环性能表明：高分散Si—Cu／C复合材料有望替代碳成为锂离子电池负极材料。     

ZrH_2/W/B_4C/Al复合材料的制备与性能研究

采用粉末冶金法制备了Zr H2/W/B4C/Al复合材料,研究了屏蔽组元的分散均匀性、材料的力学性能和快中子慢化性能。通过扫描电子显微镜(SEM)和X射线无损检测分析方法检测了材料的微观分散性和宏观分散性,检测结果表明,采用本文所述的制备工艺实现了屏蔽组元在铝基体中的均匀分散。分析了热等静压后材料的相结构和微观组织结构,分析认为在Zr H2/W/B4C/Al复合材料的热等静压过程中,Al和Zr H2两相之间在高温条件下容易发生物相反应,生成Zr Al3相,而采用合适的热等静压工艺可以避免这种有害反应的发生。研究结果表明,当热等静压温度为540℃时,材料内部没有发生物相反应,材料的致密度和力学性能良好。采用DT中子源,测试了14. 88 Me V快中子穿过测试样品的中子能谱和无样品时的源中子能谱。测试结果表明,快中子经80 mm厚的样品屏蔽后,中子能量有了显著降低,材料对快中子具有良好的慢化效果。     

喷雾法制备活塞环用MP43喷镀合金钼粉

分析了喷雾法制备活塞环用MP43喷镀合金钼粉的生产过程。过程中选择含三氧化二硼的氧化硅纳米胶为粘接相，混合金属粉体（钼、镍、铬）与粘接相组成的粉浆为分散体，经离心式雾化器分散并热空气干燥以及焙烧和烧结等热处理过程而生产合金喷镀钼粉。分析结果表明，选择混合金属粉体为制粒材料符合经济性原则；选择含三氧化二硼的氧化硅纳米胶为粘接相符合晶界细化原则。选择喷雾干燥制粒和热处理相结合的过程，能够生产出流动性和粒度分布满足等离子喷镀工艺要求的喷镀合金钼粉产品。     

金属离子在环境净化材料中的应用研究

本文以天然硅藻土、微晶白云母、钛酸丁酯、硝酸银等为原料,通过溶胶-凝胶法法制备了硅藻土、微晶白云母矿物负载金属离子掺杂n-TiO_2环境净化材料。对所制备材料进行了抗菌和光催化实验,并利用X射线粉晶衍射、扫描电镜等进行了表征,结果表明,硅藻土能与掺杂的银、铜、锌、钇等金属离子和TiO_2粉体形成Si-O-Ti(M)键的牢固结合,有利于粉体的分散,提高其抗菌和光催化活性,金属离子掺杂n-TiO_2/硅藻土复合材料在暗场下也有很好的抗菌作用;金属离子的掺入可显著提高材料的抗菌与光催化性能;金属离子掺杂n-TiO_2/硅藻土复合材料易于加工和利用,在环境净化材料领域具有很好的应用前景。     

由钛铁矿制备SCR催化剂载体TiO_2的优化试验

以钛铁矿为原料,通过硫酸法固相酸解制取二氧化钛(TiO2)具有较高的酸解率。在钛液水解过程中,添加适量乙二胺四乙酸可促进钛铁分离。超声波的机械作用和空化效应有助于进一步除去微量的杂质离子。采用X射线荧光能谱分析、BET比表面积与孔隙度分析、及扫描电子显微镜分析研究了EDTA及超声波对TiO2颗粒的优化作用,并制备以不同TiO2为载体的SCR催化剂进行脱硝活性测试。结果表明:EDTA在钛液水解阶段可以起到很好的除铁效果,从而缩短工艺流程,提高TiO2纯度。超声波在提高除杂效果的同时可降低TiO2的粒度,优化其分散性能,进而使SCR催化剂具备更优的脱硝催化活性。     

添加氧化钛对钇铝石榴石纤维形貌的影响

以金属铝粉、氯化铝、冰醋酸、氧化钇为原料,通过溶胶—凝胶法制备了钇铝石榴石纤维(YAG)。通过在溶胶中引入氧化钛,研究其对YAG纤维形貌的影响。结果表明,氧化钛可促进YAG晶粒生长,含氧化钛的纤维在1 400℃烧结6h后,晶粒尺寸达0.5～1.0μm。     

纳米颗粒市场的前景看好

美国商业通讯有限公司的高级工业分析师MindyRittner博士在纽约召开的 2 0 0 2年纳米颗粒会议上发表的统计报告表明 :2 0 0 1年全球纳米颗粒材料的市场规模为 5 5 6亿美元 ,预计到 2 0 0 5年全球纳米颗粒材料的市场规模将增加到 9 0 0亿美元 ,年增长率约为 12 5 % ,在 2 0 0 5年纳米颗粒市场的份额中电子、磁性材料、光电子等领域占 74 2 % ;生物、制药、化妆品等行业占 16 % ;在能源、崔化剂和结构材料等领域占 9 8%。应用最多的纳米颗粒是纳米氧化硅、纳米氧化铝、纳米氧化钛等化合物纳米粉末及一些纳米金属颗粒 ,预计 2 0 0 5年全球…     

单晶型LiNi0.8Co0.1Mn0.1O2正极材料的制备及性能对比

基于高镍三元正极材料容量和成本等方面的优异性,通过熔盐法结合高温固相法进行梯度煅烧,成功制备出了具有大尺寸单晶颗粒状的高镍LiNi_0.8Co_0.1Mn_0.1O₂材料,并与传统固相反应煅烧制备的材料进行比对,通过XRD衍射分析其结构特征,反映阳离子混排程度。依托扫描电子显微镜和透射电子显微镜,表征其表面形貌和晶体特征,研究表明:在经过循环伏安测试后,在高倍率测试条件下,循环稳定性和容量保有量的优势明显,契合锂离子电池近些年在快速发展过程中所面临的安全稳定的条件。这种采用熔盐法制备的NCM-811材料为制备微米级单晶型的正极材料提供了新的思路。      

磁性TiO2空心球的制备及其光催化性能

分别制备Fe3O4和ZnFe2O4粉体并以它们作为磁芯,葡萄糖为模板剂,氟钛酸铵为钛源,通过水热法制备出Fe3O4/C/TiO2和ZnFe2O4/C/TiO2前驱体,煅烧后获得磁性Fe3O4/TiO2和ZnFe2O4/TiO2空心球。采用扫描电子显微镜、X射线衍射仪、X射线光电子能谱仪分析了产物的形貌、结构和化学组成,用振动样品磁强计测试了样品的磁化强度。结果表明,以Fe3O4为磁芯得到的Fe3O4/TiO2空心球的比饱和磁化强度是ZnFe2O4为磁芯得到的ZnFe2O4/TiO2空心球的20倍。以亚甲基蓝溶液为降解模型,考察了磁芯Fe3O4添加量对Fe3O4/TiO2空心球在紫外光下的催化降解能力。结果显示,Fe3O4的添加量对Fe3O4/TiO2空心球的光降解性能影响较小,且Fe3O4/TiO2空心球的紫外光降解能力均比纯TiO2空心球略低,但Fe3O4/TiO2空心球具有在外加磁场下易于回收的优势,具有潜在的应用前景。     

Preparation of Y-H3PW12O40/TiO2 and La-H3PW12O40/TiO2 by hydrothermal method and its photocatalytic activity for dinitrotoluene decomposition

A series of mesoporous materials （H3PW12O40/TiO2, Y-H3PW12O40/TiO2 and La-H3PW12O40/TiO2） were prepared by a modified sol-gel-hydrothermal route, which realized the load and modification of H3PW12O40 at the same time. The prepared samples were characterized by X-ray diffraction （XRD）, Fourier transform infrared spectroscopy （FT-IR）, nitrogen adsorption-desorption analysis, ultraviolet-visible absorption spectrum （UV-Vis） and scanning electron microscopy （SEM）. The XRD and FT-IR results displayed that the catalysts had uniform anatase phase and the primary Keggin structure of H3PW12O40 remain intact. Nitrogen ad-sorption-desorption analysis suggested that suitable doping of rare earth elements could increase the specific surface area from 177.9 m2/g （H3PW12O40/TiO2） to 229.5 （1 wt.%Y-H3PW12O40/TiO2） or 236.1 m2/g （1 wt.%La-H3PW12O40/TiO2）. Results of UV-Vis spectra showed that the band of the 1 wt.%Y-H3PW12O40/TiO2 and 1 wt.%La-H3PW12O40/TiO2 have an obvious redshift compared with the H3PW12O40/TiO2. Additionally, the composites were used as heterogeneous photocatalysts to the degradation of dinitrotoluene （DNT）. It is the first time that polyoxometalate （POM） is applied in the degradation of explosive wastewater.     

Structure and Properties of TiO2-CeO2 Films Deposited on Soda-Lime Silicate Glass Substrates by R.F.Magnetron Sputtering

TiO2-CeO2 films were deposited on soda-lime glass substrates at different ratio of O2 to Ar (0.10, 0.15,0.20) by R. F. magnetron sputtering. The structure, surface composition, UV-visible spectrum of the films were measured by scanning electron microscopy, X-ray diffraction, X-ray photoelectron spectroscopy and spectrometer. The results show that the films are amorphous, and the relative molar ratio of Ce to Ti is higher than that of the target at lower ratio of O2 to Ar. Only tetravalent Ti 4 and Ce 4 ions are present in the films, and the obtained TiO2 -CeO2 films appear good uniformity and high density. The films deposited on the glass can shield ultraviolet light without significant absorption of visible light.     

稀土上转光剂(Y3Al5O12∶Er^3+)复合TiO2光催化剂的制备及其催化性能的研究

采用溶胶-凝胶法、高温煅烧法和超声分散法制备了Y3Al5O12∶Er^3+/TiO2复合光催化剂,并对制备的样品进行了XRD和SEM表征。利用次甲基蓝水溶液模拟有机污染水,对比了单一TiO2,上转光剂Y3Al5O12∶Er^3+以及Y3Al5O12∶Er^3+/TiO2复合光催化剂的催化活性。同时讨论了煅烧温度、煅烧时间、光照射时间、光照强度以及光催化剂用量等因素对光催化剂性能的影响。结果表明,煅烧温度为550℃、煅烧时间为90 min,照射时间为150 min,光照强度为1.0 mW/cm2和催化剂的量为1.00 g/L时,Y3Al5O12∶Er^3+/TiO2复合光催化剂降解次甲基蓝表现出了最佳的催化效果。     

A common mechanism for the interaction of nitric oxide with the oxidized binuclear centre and oxygen intermediates of cytochrome c oxidase

The reactions of nitric oxide (NO) with fully oxidized cytochrome c oxidase (O) and the intermediates P and F have been investigated by optical spectroscopy, using both static and kinetic methods. The reaction of NO with O leads to a rapid (approximately 100 s-1) electron ejection from the binuclear center to cytochrome a and CuA. The reaction with the intermediates P and F leads to the depletion of these species in slower reactions, yielding the fully oxidized enzyme. The fastest optical change, however, takes place within the dead time of the stopped-flow apparatus (approximately 1 ms), and corresponds to the formation of the F intermediate (580 nm) upon reaction of NO with a species that we postulate is at the peroxide oxidation level. This species can be formulated as either Fe5+ = O CuB2+ or Fe4+ = O CuB3+, and it is spectrally distinct from the P intermediate (607 nm). All of these reactions have been rationalized through a mechanism in which NO reacts with CuB2+, generating the nitrosonium species CuB1+ NO+, which upon hydration yields nitrous acid and CuB1+. This is followed by redox equilibration of CuB with Fea/CuA or Fea3 (in which Fea and Fea3 are the iron centers of cytochromes a and a3, respectively). In agreement with this hypothesis, our results indicate that nitrite is rapidly formed within the binuclear center following the addition of NO to the three species tested (O, P, and F). This work suggests that nitrosylation at CuB2+ instead of at Fea32+ is a key event in the fast inhibition of cytochrome c oxidase by NO.     

Effect of Tb2O3 additive on structure of anatase and photocatalytic activity of TiO2/(O'+β')-Sialon multi-phase ceramics

Effect of rare earth oxide Tb2O3 additive on transformation behavior and grain growth of anatase and photocatalytic activity for TiO2/(O'+β')-Sialon multi-phase ceramic was investigated and the mechanism was discussed. X-ray diffractometer (XRD) was employed for the analysis of phase composition, grain size and lattice parameters of anatase. Photocatalyfic activity of the composites was investigated through its photocatalytic degradation to methylene blue (MB) solution. The results showed that Tb2O3 significantly inhibited the transfor-marion process, which displayed an appreciably intensified effect with increasing Tb203 content. It could be attributed to the coaction of the active and passive influence mechanisms. For Tb3+ entering TiO2 lattice, replacing Ti4+ accelerated the transformation, whereas the lattice distortion caused by it was unfavorable for the process. On the other hand, the redox reaction between Tb3+ and TiO2 as well as the Tb2O3 deposited on the surface of TiO2 inhibited the transformation. The addition of Tb2O3 effectively restrained the grain growth of TiO2 and the effect became significant with the increase of its content. With the increase of Tb2O3 addition, the photocatalytic activity of the catalysts in-creased and then dropped after reaching the maximum at about 2%. The action mechanism of Tb2O3 could be attributed to its optical proper-ties and its effect on phase transformation, grain growth and crystal structure of TiO2.     

超声辅助TiO2包覆尖晶石LiMn2O4及电化学性能研究

采用超声辅助溶液法在尖晶石LiMn2O4表面包覆TiO2.通过X射线衍射、扫描电子显微镜、恒电流充放电、交流阻抗技术分析合成材料的结构、形貌及电化学性能.结果表明:TiO2包覆LiMn2O4与LiMn2O4具有相似的X射线衍射结果,衍射峰尖锐,样品颗粒大小均匀,无明显团聚.室温下0.2C充放电时,表面包覆1％TiO2的LiMn2O4首次放电比容量为123.51 mAh·g-1,略低于未包覆LiMn2O4的124.02 mAh·g-1,但在2C和4C高倍率时,表面包覆1％TiO2的LiMn2O4比容量分别为105.54和80.73 mAh·g-1,远高于未包覆的79.76和66.37 mAh·g -1.室温及55℃下以0.2C倍率循环50后,表面包覆1％ TiO2的LiMn2O4容量保持率分别为91.69％和87.36％,远高于未包覆LiMn2O4的86.58％和78.02％.室温下以1C倍率循环100次后,表面包覆1％ TiO2的容量保持率比未包覆LiMn2O4高出3.75％.表面包覆TiO2后LiMn2O4的循环性能得到了大大的提高,尤其是高温循环性能.     

Effects of SrO/Li2O/La2O3/Ta2O5/TiO2-coating on electrochemical performance of LiCoO2

Commercial cathode material (LiCoO2) was modified by coating with a thin layer of SrO/Li2O/La2O3/Ta2O5/TiO2 for improving its performance in lithium ion battery. The morphology and structure of the modified cathode material were characterized by scanning elec-tron microscopy (SEM) and X-ray diffraction (XRD). The performance including cycling stability, diffusion coefficient under different volt-age, C-rate discharge of the batteries with this modified cathode material was examined. The results showed that the battery with the coated cathode material could discharge at a large current density, and it possessed a stable cycle performance in the range from 3.0 V to 4.2 V. It was explained that the rate of Li ion diffusion increased in the batteries using SrO/Li2O/La2O3/Ta2O5/TiO2-coated LiCoO2 as the cathode and the coated layer could act as a fast ion conductor (Sr0.5La0.05Li0.35Ti0.5Ta0.5O3) and as a protecting shell to prevent LiCoO2 particles from be-ing attacked by the acidic electrolyte.     

CuO-TiO_2对多孔氧化铝陶瓷支撑体性能的影响

以α-Al2O3为骨料,羧甲基纤维素(CMC)为造孔剂和粘结剂,丙三醇为润滑剂和增塑剂,CuO-TiO_2为烧结助剂,采用挤压成形和固态粒子烧结法制备管式多孔氧化铝陶瓷支撑体。通过X线衍射(XRD)、扫描电镜(SEM)、抗折强度测试等,研究CuO-TiO_2对氧化铝陶瓷支撑体的晶相组成与微观形貌、孔隙率、抗折强度、耐酸/碱腐蚀等性能的影响。结果表明:TiO_2与Al2O3固相反应生成Al2TiO5,并生成大量正离子空位而提高扩散系数,促进氧化铝陶瓷的致密化,同时CuO的液相润湿作用使TiO_2的固溶温度降低,生成液相低共熔物CuAl2O4,进而实现低温烧结。当TiO_2与CuO的添加量(质量分数)分别为3%和1.5%、烧结温度为1200℃时,获得孔隙率为33%、抗折强度104.4MPa、酸/碱腐蚀后的质量损失率为0.02%/0.09%的性能优异的管式多孔氧化铝陶瓷支撑体。     

Effects of La2O3/Li2O/TiO2- Coating on Electrochemical Performance of LiCoO2 Cathode

Conventional cathode material （LiCoO2） was modified by coating with a thin layer of La2O3/Li2O/TiO2 for improving its performance for lithium ion battery. The morphology and structure of the modified cathode material was characterized by SEM, XRD, and Auger electron spectroscopy. The performance of the cells with the modified cathode material was examined, including the cycling stability, the diffusion coefficient under different voltages, and the C-rate discharge. The results showed that the cell composed of the coated cathode material discharged at a large current density, and possesses a stable cycle performance in the range from 3.0 to 4.4 V. It was explained that the rate of Li ion diffusion increased in the cell while using La2O3/Li2O/TiO2-coated LiCoO2 as the cathode and the coating layer may act as a faster ion conductor （La2O3/Li2O/TiO2）.