磁控溅射非晶CNx薄膜的热稳定性研究

为了研究非晶CNx薄膜的热稳定性,采用射频磁控溅射方法沉积了非晶CNx薄膜样品,并在真空中退火至900℃,利用FTIR,Raman和XPS谱探讨了高温退火对CNx薄膜化学成分及键合结构的影响.研究表明:CNx薄膜样品中N原子分别与sp、sp2和sp3杂化状态的C原子相结合,退火处理极大地影响了CN键合结构的稳定性;当退火温度低于600℃时,膜内N含量的损失较少,CNx薄膜的热稳定性较好,退火温度超过600℃时,将导致CNx膜中大多数C、N间的键合分离,造成N大量损失,膜的热稳定性下降;退火可促使膜内sp3型键向sp2型键转变,在膜中形成大量的sp2型C键,导致CNx膜的石墨化.     

Ni-S二元化合物的杂化微波合成及性能表征

采用可控温、通气氛的杂化微波加热技术,成功合成了Ni3S2、ε-NiS、δ-NiS和NiS2四种化合物.采用XRD和SEM对样品的物相和形貌进行了表征,结果表明此方法容易合成单相的Ni3S2,通过改变烧结条件可获得主相分别为ε-NiS和δ-NiS的样品,合成单相NiS2则比较困难.电磁测量和低温XRD衍射的结果表明,随着温度上升,δ-NiS在260K附近发生顺磁-反铁磁(金属-非金属)转变,同时晶体点阵参数a、c分别减小0.38％和1.4％,在相变温区表现负热膨胀性.Ni3S2单相样品显示顺磁金属性质.     

SnS_2纳米薄膜的制备及结构和光学特性

采用真空热蒸发法,在玻璃衬底上制备纳米SnS2薄膜。研究不同Sn和S配比及不同热处理条件对薄膜性能的影响。实验给出采用Sn∶S=1∶1.5摩尔比混合粉末制备的薄膜,经T=430℃,t=40min氮气保护热处理可获得性能良好的SnS2纳米多晶薄膜。薄膜呈n型、表面结构较致密,平均晶粒尺寸为77nm,直接光学带隙约为2.02eV。     

Sn2S3薄膜制备及结构与光学特性

采用真空热蒸发法在玻璃衬底上制备Sn2S3薄膜.研究不同Sn和s配比及热处理条件对薄膜的结构及光学特性的影响.结果显示:采用Sn:S为1:1.2(at%)混合粉末制备出的薄膜,在T=430℃,t=40min氮气保护热处理后,可得到结构良好的n型Sn2S3纳米多晶薄膜.薄膜表面致密较平整,颗粒分布均匀,平均晶粒尺寸为60.37m.Sn2S3薄膜的直接光学带隙约为2.0eV.     

Bi2WO6的水热合成及其光催化性能研究

水热法合成了Bi2WO6粉体,并采用XRD、FESEM及UV-Vis分光光度计对样品进行表征,研究了不同合成条件对产物形貌和催化性能的影响.UV-Vis漫反射谱表明产物在紫外和可见光区域均有吸收.样品的光催化性能通过降解RhB溶液来评价.结果表明:180℃,pH=2下合成24h获得的Bi2WO6紫外光催化性能最好,反应速率常数为0.03688/min.还讨论了不同pH值对合成样品催化性能的影响.催化剂的稳定性实验通过180℃,pH=2下合成24h获得的Bi2WO6多次催化实验来评估,结果表明4次循环实验后,样品的催化性能未有明显地衰减.在可见光下照射150min,催化剂对染料的降解率达到38%.     

氮离子注入法合成CNx膜的化学键表征

采用N离子注入金刚石膜和热解石墨方法合成了CNx膜,用Raman光谱和XPS谱对合成薄膜中C、N的化学键合状态进行了研究.通过与Raman光谱的比较,我们对合成样品XPS谱中N1s的化学键合状态作出如下归属:≈400.0 eV属于sp2 C-N键;≈398.5 eV则属于sp3 C-N键.结果显示:碳原子、氮原子间的化学键合状态,明显地依赖于衬底材料及注入N离子的能量.     

介孔Zr（HPO4）2的合成及表征

以十六烷基三甲基溴化铵(CTAB)为模板剂,采用溶胶-凝胶法配合水热晶化合成了具有短程有序介孔结构的层状化合物Zr(HPO4)2。通过XRD、N2吸附、HRTEM等技术对样品的物相、孔结构和形貌进行了表征,结果表明,按n(CTAB)∶n(Zr)=0.8引入CTAB作为模板剂所合成的前驱体在120℃水热晶化48h,可以得到比表面积为66.9m2/g、孔容为0.11cm3/g、平均孔径为8.1nm的单相Zr(HPO4)2结晶化合物。     

AgSbTe_2热电化合物的超声化学法合成

采用超声化学法结合还原热处理合成了单相的AgSbTe2粉体,并结合放电等离子烧结(SPS)制备了相应的块体.系统研究了不同前驱体制备条件、热处理温度、时间和起始化学计量比对相组成的影响,并对烧结块体的热电性能进行了初步研究.结果表明:超声化学法合成的前驱体在500℃、2h还原热处理后可以得到近单相的AgSbTe2,且通过调节起始原料的摩尔比可以得到单相的AgSbTe2.所得粉体颗粒平均粒径约为10μm,表面均匀分布着20~50nm的纳米颗粒.性能测试表明单相样品的无量纲热电优值ZT值在570K最大可达1.14.     

水热法制备Cu_2S及其热电性能研究

采用水热法制备Cu_2S粉末,研究了合成温度、表面活性剂添加量对Cu_2S粉末形貌的影响以及表面活性剂对Cu_2S热电性能的影响。采用XRD、SEM和TEM表征Cu_2S粉末材料的相组成和微观形貌,之后采用放电等离子烧结技术(SPS)制备了Cu_2S块体热电材料,采用激光闪光法和塞贝克系数/电阻测量系统测试了块体材料的热电性能。实验结果表明,水热法成功合成了由纳米晶组成的尺寸为亚微米的Cu_2S粉末,其中180℃合成的Cu_2S粉末的平均粒径比160℃合成的小;添加适量的表面活性剂十二烷基苯磺酸钠可以有效地降低Cu_2S粉末的晶粒尺寸,而适量地添加乙二醇促进层片状Cu_2S粉末的生成;3种样品的塞贝克系数都为正,说明Cu_2S为p型热电材料;180℃添加0.5g十二烷基苯磺酸钠制备的Cu_2S粉末的平均晶粒尺寸最小,该样品的热电性能最好,873K时其热电优值达到0.69。     

共聚物聚苯硫醚-聚苯硫醚酮的合成及表征

在聚苯硫醚(PPS)的合成体系中加入不同比例的第三单体4,4二氯二苯甲酮(DCBP)从而合成了共聚物PP/SK.主要通过加入不同量的DCBP来考察产品的熔点及分子量的变化.合成工艺条件:前期反应的最高温度为T1=190℃～230℃,反应时间为t1=3h～5h;后期的反应温度最高为T2=250℃～270℃,反应时间为t2=2h～4h.n(Na2S·9H2O):n(对二氯苯/4,4二氯二苯甲酮)=1.1mol:1mol,m(N甲基吡咯烷酮):n(Na2S·9H2O)=282g:0.1mol,m(催化剂):n(Na2S·9H2O) =2g:0.1mol.根据上述加料及反应条件合成了线性的高分子量的共聚物PPS/SK,其重均分子量接近55000g/mol,产品的平均收率达到91.32％.通过一步循环回收工艺就实现了溶剂和催化剂的循环.用红外、元素分析、X-RD及热分析对产品进行了表征.     

燃烧法合成超细SrAl_2O_4:Eu~(2+),Dy~(3+)长余辉发光材料

利用氧化还原反应燃烧过程合成SrAl2O4:Eu2+,Dy3+长余辉发光材料,采用荧光光谱、X射线衍射、扫描电镜、余辉测试等多种测试手段研究产物的性质,并从多方面与高温固相法合进行对比。结果表明:燃烧法合成的产物为单斜晶系的SrAl2O4,结晶干净完整,晶粒尺寸在0.3～1μm之间;光谱分析显示燃烧法合成材料发射波长为514 nm。相比高温固相法,燃烧法在工艺上具有低温、快速、节能的优点,所得产物易于粉碎,晶粒大大减小。     

Effect of Oxygen Admittance Temperature on the Growth of ZnO Microcrystals by Thermal Evaporation Technique

Hexagonally well-faceted microcrystals of ZnO have been grown by thermal evaporation of Zn powder in oxygen ambient at 700 C under atmospheric pressure. It has been observed that the properties (size and quality) of ZnO microcrystals have a strong dependence on the reactor temperature at which the oxygen gas is admitted into the growth zone. The microcrystals grown with oxygen admittance at 450 C have a length of 1 μm and a diameter of 0.75 μm while that grown with oxygen admittance at 600 C have a length of 1.5-2 μm and a diameter of 1 μm. Room temperature photoluminescence spectra show a ultraviolet (UV) emission peak at 385 nm with a green band emission at around 500 nm. The UV-to-green band emission ratio for the microcrystals grown with oxygen admittance at 450 C is observed to be 1.25 and the ratio decreases to 0.45 for the sample grown with oxygen admittance at 600 C.     

柠檬酸-凝胶燃烧法制备钇铝石榴石(Y_3Al_5O_(12))纳米粉体的研究

透明YAG多晶陶瓷具有优良的光学、力学与化学性能,逐渐成为新一代固体激光基质材料。分散均匀、团聚轻的纳米粉体有利于制备出高度透明的激光陶瓷。以Y2O3、Al(NO3)3·9H2O和柠檬酸为原料,采用柠檬酸凝胶燃烧法制备出黑色粉体,经1100℃烧结出尺寸小于50nm的YAG粉体。采用TG-DTA、XRD、FT-IR和TEM测试手段对YAG纳米粉体进行表征,采用谢莱公式计算出不同烧结温度下的晶粒尺寸。研究结果表明:YAG的析晶温度范围为850～900℃,烧结过程中出现赝YAG相物质,1050℃转变成纯YAG相,随着热处理温度的升高,晶粒呈线性增长,纳米粉体的TEM尺寸和采用谢莱公式计算的结果相一致。     

PVP溶胶-凝胶法制备锂稳定Na-β-Al2O3纳米粉体

作为钠硫电池陶瓷电解质的核心材料, Na-β-Al₂O₃粉体对钠硫电池的性能影响很大。实验以聚乙烯吡咯烷酮(PVP)为络合剂, 合成了纳米Na-β-Al₂O₃粉体。结果表明, 以PVP络合的前驱体形成Na-β-Al₂O₃相的温度低至900?℃, 相比于传统固相合成法及其他化学合成法有显著的降低, 可有效抑制传统制备Na-β-Al₂O₃粉体方法中由于高温而导致Na₂O组份的挥发, 从而避免Na-β-Al₂O₃性能的下降。X射线衍射、扫描电镜和透射电镜对粉体的分析表明, 所获得的粉体为纯相的Na-β-Al₂O₃, 粉体粒径60~70 nm, 分散性好。高分散性的纳米粉体有助于制备高致密度的Na-β-Al₂O₃陶瓷。这种粉体制备烧结的Na-β-Al₂O₃陶瓷的电导率在350℃可达0.22 S/cm。     

液相共沉淀法制备钆镓石榴石(Gd3Ga5O12,GGG)多晶原料

采用液相共沉淀法制备了钆镓石榴石（GGG）的多晶原料，给出了液相合成GGG多晶粒的工艺步骤及其条件，就组分Gd2O3和Ga2O3的配比，滴定氧化物溶解的混合溶液使其沉淀的PH值，共沉淀后烧结温度以及烧结时间等影响GGG多晶粒合成的重要因素进行了讨论，通过和固相合成GGG多晶粒的条件比较可知，液相合成GGG多晶原料的工艺具有合成的GGG多晶料均匀充分，合成温度低与烧结时间短等优点。     

Synthesis and characterization of high purity hydroxyapatite nanorods by hydrothermal technique

High purity hydroxyapatite (HAp) nanorods were synthesized by hydrothermal technique using Ca(NO3)2 x 4H2O and (NH4)2HPO4 as starting materials in a hydrothermal reactor at 150-200 degrees C for 12-24 h with pH6 and pH9.5, respectively. The prepared HAp nanorods were characterized by XRD, FTIR, and TEM techniques. The XRD results confirmed the formation of pure phase of HAp at pH9.5. With increasing temperature and time, the crystallinity of the HAp was increased, showing the hexagonal structure of HAp with the lattice parameter a in a range of 1.144-1.148 nm and c of 0.723-0.724 nm. The crystalline sizes of the powders were found to be 44-85 nm as evaluated by the XRD line broadening technique. The chemical compositions of the HAp nanorods were characterized by FTIR spectroscopies. The peaks of the phosphate carbonate and hydroxyl vibration modes were observed in the FTIR spectra for all the samples. The morphology of the HAp was nanorods of diameter less than 100 nm, as revealed by TEM. Increasing the temperature and time resulted in the transition from polycrystalline to single crystalline phase of the HAp, as clearly confirmed by the analysis of TEM diffraction patterns.     

Investigation of Eu-doped mesoporous titania phosphor with enhanced luminescence

A novel mesoporous TiO2 phosphor doped with Eu was synthesized through a facile hydrothermal synthesis method using cetyltrimethylammonium bromide as structure template reagent. The samples were characterized by X-ray diffraction, N2 adsorption-desorption, scanning electron microscope, high-resolution transmission electron microscopy, ultraviolet visible diffuse reflectance, X-ray photoelectron spectroscopy, and three dimensional Photoluminescence. The X-ray diffraction results demonstrated that the products were anatase type with polycrystalline. N2 adsorption-desorption analysis showed that the samples were of high ordered double mesoporous structures. Eu-doped mesoporous TiO2 indicated the typical fluorescent spectra of Eu3+ ion occurred: the excited-states at 5L6 (394 nm), 5D2 (465 nm) and 5D1 (535 nm); the main emission peaks at 592 and 617 nm, corresponding with the transitions 5D0 --> 7F1 and 5D0 --> 7F2, respectively. Meanwhile, the phenomena of Eu(3+)-doped mesoporous TiO2 phosphor with efficient nonradiative energy transfer from the mesoporous TiO2 host to the activator Eu3+ ions was observed and possible emission mechanism was proposed. High dispersion of Eu in mesoporous TiO2 matrix was responsible for enhanced luminescence.     

水热合成纳米硅酸锆工艺因素分析

通过正交实验并借助于ＸＲＤ 和ＴＥＭ 等手段,研究了前驱物配比、反应温度、反应时间、升温速率等工艺因素对水热合成纳米ＺｒＳｉＯ４ 的影响。结果表明：前驱物配比、反应温度、反应时间及升温速率是影响纳米ＺｒＳｉＯ４ 粉体合成的主要因素,同时,当前驱物ｍ（Ｚｒ）∶ｍ（Ｓｉ）＝ １－２∶１－０ ,反应温度为３３５ ℃,反应时间为４ｈ,升温速率为１－６ ℃／ｍｉｎ 时,可制得晶粒规整、分散性好、粒度在１００ｎｍ 以下的ＺｒＳｉＯ４ 粉体。     

Chemical vapor deposition-based growth of aligned ZnO nanowires on polycrystalline Zn<Subscript>2</Subscript>GeO<Subscript>4</Subscript>:Mn substrates

ZnO nanowires have been grown on polycrystalline Zn₂GeO₄:Mn substrates for the first time using a chemical vapor deposition method. Both Zn and ZnO sources were used to supply Zn vapor in the growth process of ZnO nanowires. The Zn₂GeO₄:Mn substrates were prepared using solid-state ceramic synthesis methods, and average grain sizes of ~1 μm were achieved. The nanowires of diameters in the range of 100–200 nm and length of ~30 μm were observed. In addition to nanowires, other morphologies of ZnO nanostructures, such as ZnO tetrapods, were observed when Zn powder was used as the source for the CVD growth. The results reveal that polycrystalline substrates are also promising as novel alternative substrates for growth of ZnO nanostructures. The as-synthesized ZnO nanowire/Zn₂GeO₄:Mn composites are being developed for future electroluminescent devices.     

水热法制备CoFe2O4纳米颗粒及其穆斯堡尔谱与磁性能研究

用水热法在不同温度下制备结晶性较好、颗粒均一的CoFe2O4纳米颗粒,无需进一步煅烧。利用X射线衍射仪(XRD)、场发射扫描电镜(SEM)、穆斯堡尔谱仪和综合物性测量系统(PPMS)对不同温度下合成的样品进行表征。结果表明,随着合成温度的升高,CoFe2O4纳米颗粒的结晶性增强,粒径逐渐增大,样品的饱和磁化强度逐渐增强。当合成温度为500℃时,CoFe2O4纳米颗粒的饱和磁化强度达到64.1A.m2/kg,与块体的CoFe2O4(72A.m2/kg)接近。穆斯堡尔谱分析表明,当晶粒粒径超过了超顺磁性的临界尺寸,样品的超顺磁性消失,随着合成温度的升高,B位上Fe3+离子的比例增高,磁性能增强。