溶剂热法合成硫化镉微晶工艺研究

以氯化镉为前驱体,硫化钠、硫代乙酰胺、硫脲等为硫源,乙二醇、乙醇等为溶剂,通过溶剂热法制备硫化镉微晶.设计L9(34)正交试验,探讨了反应温度、反应时间等对硫化镉微晶大小和形貌的影响.所得产物经离心、洗涤、干燥后,用纳米粒度仪分别测定各产物的平均粒径,同时用扫描电子显微镜测定部分产物的大小和形貌,并用极差分析法找寻最佳合成工艺.结果表明:以硫代乙酰胺为硫源,乙二醇为溶剂,反应温度为100℃,反应时间为10 h,可得到直径为0.5～0.7μm的片状硫化镉晶体.该方法工艺简单,反应条件温和,制备的硫化镉晶体大小分布均匀,形貌单一.     

溶剂热法合成纳米材料的研究进展

本文介绍了溶剂热法的特点,综述了溶剂热法在非氧化物纳米材料如Ⅲ-Ⅴ族半导体、金刚石、碳化物、氮化物、金属硫属化合物及一维纳米材料制备中的研究进展,并对溶剂热法合成纳米材料的发展方向进行了展望。     

溶剂热法可控合成纳米氯化亚铜

以氯化铜为铜源,甲醇、乙醇、异丙醇等为溶剂和还原剂,采用溶剂热法制备纳米氯化亚铜,探讨了温度、时间、还原剂等条件对所得氯化亚铜的形貌、粒径大小、物相组成的影响。结果表明,以乙醇、异丙醇为溶剂,在120~180℃反应24~48 h,Cu Cl纳米颗粒可在2~50 nm范围内有效调控。     

溶剂对溶剂热法合成钴纳米花微晶的影响

在水/乙醇混合溶剂中采用溶剂热法合成了六方密堆积晶型(hcp)、形貌新颖的钴纳米花微晶。研究发现溶剂对产物形貌、晶型以及结晶度、收率有显著的影响。在所研究的溶剂中,只有在水/乙醇溶剂可以得到钴纳米花微晶。在较慢的反应速率下倾向于形成较低结晶度、hcp和面心立方(fcc)混晶钴,而提高反应速率有助于形成高结晶度、纯hcp相晶体钴。     

溶剂热法合成LuAG纳米粉体的晶粒生长研究

采用溶剂热法合成了镥铝石榴石(LuAG)纳米粉体,研究了晶化温度和晶化时间对晶粒成核和生长的影响规律。XRD的结果发现晶化时间相同时,晶化温度只有高于某一临界温度时才有晶粒析出,而且随着晶化温度的升高,LuAG纳米粉体的晶粒结构趋于完整;晶化温度相同时,晶化时间也只有长于某一临界时间时才有晶粒析出,而且随着晶化时间的延长,晶粒结构趋于完整。TEM的结果表明实验条件下得到的LuAG纳米粉体为球形,说明晶粒生长沿各个方向的生长速率是相同的。这一溶剂热反应过程支持了晶粒生长的成核/晶化机理。     

溶剂热法合成氧化锌纳米棒

采用PEG辅助溶剂热合成了ZnO纳米棒,通过SEM、EDS和XRD等手段对产物进行了表征。结果显示,合成的ZnO纳米棒直径在20 nm左右,长大约150,且长度和直径分布均匀。研究了PEG的添加量对形成ZnO纳米棒的影响,并且探讨了PEG促进纳米棒生长的机理。     

溶剂热法制备FeS2

研究了用乙二醇（C2H6O2）为溶剂,硫脲（NH2CSNH2）做硫源溶剂热法制备FeS2的反应机理.当反应温度达到300℃后,产物中存在黄铁矿（FeS2）,理论分析表明：这些FeS2是磁黄铁矿（FeS）被硫脲分解出的硫化氢（H2S）氧化后形成的.溶液中的碱性环境令FeS不能完全转化成FeS2.另外,由于乙二醇把部分2价Fe离子氧化成Fe^3＋,实验所获得的最终是FeS,Fe3S4与FeS2的混合物.     

溶剂热法合成肉桂酸酯

文章首次利用溶剂热合成技术高效合成了肉桂酸酯。以肉桂酸与甲醇、乙醇反应为例,考察了在对甲苯磺酸催化下溶剂热合成的反应温度、反应时间、醇酸摩尔比及催化剂用量对反应的影响。经过实验,确定了溶剂热法合成肉桂酸酯的最佳反应条件。     

水热-溶剂热法合成铌酸钾粉体的研究

以分析纯Nb2O5,KOH为原料,通过添加无水乙醇利用水热-溶剂热法合成了结晶度高、晶粒发育完整的KNbO3粉体。借助X射线衍射仪、扫描电子显微镜以及透射电镜对所得粉体进行了表征,研究了合成时间对产物晶相、粒径大小以及形貌的影响。实验结果表明:采用水热-溶剂热法,在矿化剂浓度为6mol/L的条件下反应3h得到了纯正交相结构的KNbO3粉体,反应时间对产物形貌影响较大,随着反应时间的延长KNbO3由棒状晶体转化为规则的六边形晶体。     

低温溶剂热法合成单分散氧化钛纳米棒

以Ti（OC4H8）4为无机前驱体、正辛酸为溶剂,在80-100℃一步合成了单分散的锐钛矿TiO2纳米棒状粉末。用X射线衍射、高分辨透射电子显微镜观察对样品进行了表征。结果表明：纳米棒状粉末具有窄的尺寸分布,直径为3～4nm,长度为10～20nm,长度方向为锐钛矿相C轴。此外,初步探讨了纳米棒的形成机理。     

聚吡咯/硫化镉的制备及其光学性能研究

将聚吡咯和纳米粒子结合起来制备的复合材料兼具了导电高分子材料、无机半导体材料的优势,与此同时这种的复合材料还具有显著的三阶非线性光学性质。本文拟采用界面氧化聚合法制备聚吡咯膜,通过实验发现反应的最佳溶剂为三氯甲烷,最佳的氧化剂为过硫酸铵。当聚吡咯于过硫酸铵反应浓度均为0.15 mol/L左右时可以生成表面平整、厚度适中、力学性能较好的聚吡咯膜。通过将上述方法制备的聚吡咯膜先浸泡在醋酸镉溶液中吸附Cd2+,最后与硫代乙酰胺处理得到PPy/CdS复合材料。本实验采用了探针式表面轮廓仪分析、扫描电镜(SEM)、傅立叶红外光谱(FTIR)、X-射线衍射(XRD)、Z-扫描测试法、热重(TG)分析等对产物进行表征。结果表明,聚吡咯/硫化镉纳米复合材料上纳米粒子的分布状况及粒子大小与掺比浓度有关,浓度越低分布越密、粒子直径越小,当聚吡咯、硫化镉的掺杂比达到1:0.001时粒子直径可达20 nm左右。此外,复合了硫化镉纳米粒子后聚吡咯的热稳定性提高了33.3%。由Z-扫描结果显示PPy/CdS具有很强的三阶非线性特性。     

Surfactant-free synthesis of homogeneous nano-grade cadmium sulfide grafted reduced graphene oxide composite as a high-activity photocatalyst in visible light

Zero-dimensional cadmium sulfide (CdS) nanoparticles with small size (∼50 nm) were grafted on the two-dimensional reduced graphene oxide (RGO) nanosheet via a facile hydrothermal method without any surfactant to synthesize CdS@RGO nanocomposites in this paper. The structural analysis confirms the strong attachment and interaction between CdS and RGO in CdS@RGO photocatalyst, which leads to a higher photocatalytic efficiency (95.3%) with superior anti-corrosion stability (almost no change of efficiency over three repeated experiments) to that of pure CdS in visible light. The unique hybrid nanostructure of CdS@RGO can effectively prevent the self-corrosion of CdS and facilitate the separation of electron-hole pairs. Consequently, these outstanding photocatalytic performances of CdS@RGO endow it with a promising prospect for the degradation of organic pollutants and this work can be extended to other graphene-based inorganic semiconductor composites.     

Synthesis of cadmium sulfide nanosheets for smart photocatalytic and sensing applications

Herein, we report the synthesis, characterizations, photocatalytic and sensing applications of ultra-wide cadmium sulfide (CdS) nanosheets. The CdS nanosheets were prepared by a simple solution process at low-temperature using cetyltrimethyl ammonium bromide (CTAB) as a stabilizing agent. The synthesized CdS nanosheets were characterized by several techniques which confirmed large-scale growth, well-crystallinity and hexagonal crystal phase of the prepared nanosheets. The synthesized nanosheets were used as effective photocatalyst for the photocatalytic degradation of harmful toxic dye, i.e. methyl orange. The photocatalytic activities were evaluated by measuring the photodegradation rate of MO in presence of CdS nanosheets under UV light irradiation. Interestingly, over 90% degradation of MO dye was achieved in 75 min using 0.15 g of photocatalyst, i.e. CdS nanosheets. Further, the synthesized nanosheets were used as efficient scaffold to fabricate highly sensitive, selective and reproducible fluorescent sensor for the detection of Picric Acid (PA). The observed detection of limit for the fabricated sensor was ~2.46 μM. Moreover, the interfering studies confirmed that the developed sensor possesses very good selectivity towards PA as it detect selectively even in the presence of several other coexisting aromatic compounds such as phenol, benzaldehyde, benzoic acid and aniline.     

纳米硫化镉粉体制备技术的研究进展

纳米硫化镉在太阳能转化、非线性光学、光电子化学电池和光催化等方面具有广泛的应用，因此其研究成为纳米材料科学和凝聚态物理学领域的重要问题。按照反应物的状态，将纳米硫化镉的制备方法分为固相法、液相法和气相法，进而分为室温固态化学反应法、微乳液法、沉淀法、水热法、前驱体法以及气相沉积法等不同的制备方法。详细介绍了各种制备方法，分析了它们的优点和缺点。此外，还对纳米硫化镉制备的发展方向提出了建议。     

Synthesis of cadmium sulfide spongy balls with nanoconduits for effective light harvesting

Thin films of cadmium sulfide (CdS) consisting of spongy balls with nanoconduits have been chemically synthesized at 70 °C from an aqueous alkaline bath onto soda lime glass and fluorine-doped tin oxide (FTO)-coated glass substrates. The synthesized spongy balls of CdS were characterized using X-ray diffraction (XRD), UV–vis spectroscopy, scanning electron microscopy (SEM), Fourier transform Raman spectroscopy (FT-Raman) and X-ray photoelectron spectroscopy (XPS). The XRD pattern revealed the formation of CdS particles with a cubic crystal structure. SEM micrographs show that the spongy ball-like morphology is composed of nanoconduits. Such spongy balls with nanoconduits that contain numerous nanowalls are a facile way to trap light. The light absorption path length of a photon increases in the nanoconduits and thus can participate in multiple scattering and absorption. This is beneficial for effective light harvesting and improvement in the power conversion efficiency of solar cells.     

溶剂热法制备硒化铅亚微米八面体

在聚乙烯吡咯烷酮K30(PVP)存在下,采用溶剂热法成功地合成出立方相硒化铅(PbSe)纳米晶。分别用扫描电子显微镜(SEM)和X射线衍射仪(XRD)对样品的形貌和晶体结构进行了表征分析。SEM结果表明样品为大量的尺寸均一的八面体形状的纳米晶,经XRD分析证明,八面体状的纳米晶是立方相PbSe。进一步考察了反应时间对样品形貌的影响,并分析了PbSe亚微米八面体的生长机制。     

Phase-controlled solvothermal synthesis and morphology evolution of nickel sulfide and its pseudocapacitance performance

Phase-controlled solvothermal synthesis has been proposed for the synthesis of nickel sulfide of single phase including α-NiS, Ni₃S₄ and NiS₂ by tuning the reaction time and the addition of surfactant. The phase evolution of nickel sulfide proceeds with the increase of sulfur stoichiometry with longer reaction time in the presence of surfactant. With the addition of hexadecyl-trimethyl-ammonium bromide (CTAB), a higher sulfur stoichiometry NiS₂ phase with hollow sphere geometry was synthesized at 9 h, a much shorter time due to the enrichment of S²⁻ on CTAB micelle surface, followed by the transformation to single phase Ni₃S₄ finally due to dissipation of enriched sulfur to the bulk solution. The application of these three single phase materials in supercapacitors was investigated. The α-NiS electrode material outperformed the Ni₃S₄ and NiS₂ electrodes, exhibiting a much higher specific capacitance of 800 F g⁻¹ at 0.5 A g⁻¹, attributable to the small particle size, high electrical conductivity and the unique hexagonal crystal structure.     

四方相钛酸钡纳米晶的制备及其表征

以Ti(OC4 H9) 4、H2 O2 和Ba(OH) 2 ·8H2 O为原料 ,在 180℃下溶剂热处理 2 4h ,制备了四方相钛酸钡纳米晶 ,XRD数据计算其格子常数a =3 .9899,c=4.0 3 2 5 ,c/a =1.0 10 7。并对该法四方相钛酸钡的形成机理进行了浅析     

水溶液中均匀硫化镉微球的制备及其在结构色中的应用

均匀的硫化镉（CdS）微球具有较高的折射率,由其组成的光子晶体颜色亮丽,具有低角度依存性,近年来在结构生色领域被广泛应用。但是,目前较为成熟的合成均匀硫化镉微球的方法存在有机溶剂的大量使用和高温能耗大等问题。因此,设计了一种在水溶液中合成均匀硫化镉微球的绿色合成方法,通过受控注射的方式辅助进料,解决了金属盐前驱体在水中水解速度过快导致微球生长不平衡的问题。同时,受控注射的方式可以更有利于控制体系中二价镉的浓度,成功地合成出180~410 nm的均匀硫化镉微球。进一步通过水平诱导组装的方式构筑了以不同粒径的硫化镉微球为基元的三维光子晶体结构。这种光子晶体薄膜展示出亮丽、低角度依存的结构色,更利于结构色在颜色显示等领域的应用。