Co3O4纳米颗粒的制备及表征

以脱脂棉为碳源,硝酸钴为前驱物,采用碳辅助法焙烧制备了粒径为50nm Co3O4纳米颗粒。用X射线衍射(XRD)对不同焙烧温度(200~600℃)下样品的物相、晶粒度进行了研究,并结合傅立叶红外光谱(FT-IR)对Co3O4物相演变进行了分析,确定中间产物前躯体是CoCO3;通过扫描电镜(SEM)和透射电镜(TEM)对制备的Co3O4样品的形貌、粒径进行了分析;同时,X射线能谱(EDS)和氮气吸附-脱附曲线测试等表明制备的Co3O4表面存在碳元素和孔结构,具有较大的比表面积,有利于提升其光解水制氢能力。     

Ag掺杂优化g-C3N4结构及提升可见光降解性能的研究

石墨相氮化碳的改性已经成为光催化领域,特别是光催化材料领域的研究热点。本文以硝酸银和尿素为原料制备一系列不同Ag含量的Ag/g-C₃N₄光催化剂,并以罗丹明B水溶液模拟废水,在可见光下考察Ag/g-C₃N₄催化剂的光催化降解性能,最终获取最佳Ag掺杂量。通过XRD、SEM、FTIR、UV-Vis、PL等对光催化剂进行分析,发现Ag的掺杂有助于g-C₃N₄的剥离,改变了g-C₃N₄的电子结构,降低了其带隙能,使其在可见光区的吸收增强,抑制了光生电子-空穴对的复合。研究表明,当Ag掺杂量为2%时,Ag/g-C₃N₄光催化剂的效果最佳,300 min内降解率高达95.8%。     

BiOI/BiOBr0.9I0.1光催化剂的制备及其对2,4-二氯苯氧乙酸的降解性能

农药污染严重危害生态环境和饮用水安全。采用溶剂热法制备一种新型高效的BiOI/BiOBr_0.9I_0.1光催化剂。通过XRD、SEM、XPS、UV-vis DRS、PL、EIS等手段表征其结构、形貌和光学性能等理化性质。制备的BiOI/BiOBr_0.9I_0.1呈团簇状堆积结构,有助于活性位点的增加,固溶体和异质结两种策略的结合拓宽了BiOBr的光响应范围,有效防止光生电子-空穴对在BiOI/BiOBr_0.9I_0.1内部复合并提高产生光生载流子的氧化还原能力。光催化实验结果表明,合成的15wt%BiOI/BiOBr_0.9I_0.1在可见光下对2,4-二氯苯氧乙酸(2,4-D)有最佳的光催化性能,120 min降解2,4-D效率最高可达95%,4次循环实验后降解率仍达到80.9%。结合捕获实验与电子自旋共振(ESR)技术结果可以证实?O₂?和h+是主要的活性物种。制备的BiOBr_0.9I_0.1能有效调节BiOBr能带结构。BiOBr_0.9I_0.1和BiOI构成的异质结符合Z型异质结特点,构建异质结和固溶体两方法之间可在增强BiOBr光催化活性上产生协同作用。      

g-C3N4-Ag/SiO2复合材料光催化降解甲醛的应用

将Ag、薄层石墨相氮化碳（g-C₃N₄）和硅铝胶球（SiO₂）通过液相超声剥离-光化学沉积法-浸渍法合成复合光催化材料。设计甲醛降解密闭实验舱,探究g-C₃N₄、Ag-g-C₃N₄和g-C₃N₄-Ag/SiO₂材料的光催化特性及其对甲醛的降解效果。结果表明,在可见光源条件下,对于g-C₃N₄-Ag/SiO₂材料,降解甲醛的效率最高可达到65.6%。40%的相对湿度可有效提升降解效果。负载30 mg 4%Ag/g-C₃N₄的硅铝胶球循环使用16次时,甲醛降解效率仅下降9.71%。结合材料表征结果表明,通过超声剥离和Ag的引入,提升了材料可见光的吸收强度和吸收范围,并且有效促进了光生电子和空穴的分离,有效提升甲醛分子的降解效率。研究结果表明g-C₃     

模板法合成g-C3N4基复合材料及其光催化性能的研究进展

石墨相氮化碳(g-C₃N₄)作为一种新型非金属高聚物半导体,具有易于合成、无毒无害、耐酸碱腐蚀、环境亲和性好等性质。独特的层状结构赋予了其较高的比表面积,适中的禁带宽度给予了其较好的光催化性能,使得其在光催化领域受到了广泛的关注。然而,纯相g-C₃N₄存在着比表面积小、活性位点不足、载流子复合过快和氧化还原能力偏弱等缺点,制约了其光催化领域的有效应用。研究表明,使用模板诱导工艺对g-C₃N₄进行结构调控可以有效解决上述问题。综述了目前常用于制备石墨相氮化碳的模板法(即硬模板法、软模板法和生物模板法),扩展讨论了多相复合工艺的进展情况,并归纳总结了g-C₃N₄基材料在光催化降解、CO₂转化和制氢等方面的应用情况。     

Co3O4/碳复合超级电容器材料的研究进展

Co₃O₄作为超级电容器材料,因具有理论比容量高、价格成本低、无毒环保、储量丰富等优点而备受关注,但制备出电化学性能优异的Co₃O₄超级电容器材料仍是个巨大的挑战。通过与导电性突出的碳材料复合,增加了电子/离子的传输速度,提高了Co₃O₄超级电容器材料电化学性能。综述了Co₃O₄/碳复合超级电容器材料的合成方法,归纳了各个方法的优缺点,分析了影响Co₃O₄/碳复合超级电容器电化学性能的因素,最后,指出了Co₃O₄/碳复合超级电极材料所面临的问题和发展前景。     

硅藻土/g-C3N4/氧化石墨烯复合材料的制备及其光催化性能研究

采用半封闭一步热解方法,以三聚氰胺为前驱物制备g-C₃N₄,然后以圆筒状硅藻土(DE)为载体,合成DE/g-C₃N₄复合材料。并选取天然鳞片石墨为基本原料,运用Hummers法合成了氧化石墨烯(GO),在一定量的DE/g-C₃N₄粉末中加入不同质量分数的GO,得到DE/g-C₃N₄/GO三元复合光催化材料。通过SEM、BET、EDS、XRD、FT-IR对样品的晶体结构、形貌等进行表征,研究复合材料对罗丹明B溶液的光催化降解性能。结果表明,当GO的烯掺量为5%时,DE/g-C₃N₄/GO在可见光下,120min时,对RhB的降解率为93.74%,分别比DE/g-C₃N₄和g-C₃N₄提高了15.05%和31.03%。     

g-C3N4/BiOCl复合光催化剂作为2D/2D异质结用于光催化降解染料性能研究

为扩大BiOCl的太阳光吸收范围,获得更高效的光催化剂,本文通过水热法制备了石墨相氮化碳(g-C₃N₄)/BiOCl (2D/2D)复合光催化剂并对其进行详细表征。结构与形貌表征结果显示BiOCl纳米片沉积在层状g-C₃N₄表面,形成了2D/2D面-面复合结构;光电化学性质分析表明形成的异质结构能有效扩展光吸收频率范围,促进光生载流子分离和迁移,从而有利于光催化性能的提高。以500 W氙灯模拟太阳光源,光催化降解罗丹明B(RhB)的结果表明g-C₃N₄/BiOCl异质结的光催化降解活性远高于单纯的g-C₃N₄和BiOCl。其中9wt%g-C₃N₄/BiOCl表现出了最优越的光催化活性,在180 min内对RhB的降解率为94%,其表观速率常数K_app值为g-C₃N₄和BiOCl的5.7和3.6倍。同时对g-C₃N₄/BiOCl异质结的光催化机制展开研究,结合复合催化剂电子结构和自由基捕获实验提出了在染料敏化作用下RhB的光催化降解机制。      

MoS2/g-C3N4 S型异质结的构建及光催化性能研究

制备高效稳定的光催化剂对于光催化技术的发展至关重要。本研究采用超声辅助沉积加低温煅烧的方法制备了2H相MoS₂/g-C₃N₄ S型异质结光催化剂(MGCD),并综合考察了材料的相结构、微观形貌、光吸收性能、X射线光电子能谱、电化学交流阻抗和光电流等对光催化性能的影响。结果表明:经过超声辅助沉积-煅烧处理,MoS₂微米球发生破碎分散结合在g-C₃N₄纳米片层表面上并形成异质结。可见光下5%MGCD(添加5%MoS₂)对罗丹明B(RhB)在20 min时的降解率达到了99%,且样品重复使用5次后对Rh B的降解率仍能达到95.2%,表现出良好的光催化性能及稳定性。从内建电场形成的角度进一步分析表明,异质结中MoS₂与g-C₃N₄间耦合形成的内建电场引起的能带弯曲可以有效引导载流子的定向迁移,并促进光生载流子的分离,从而提高了光催化反应效率。异质结光催化剂的自由基捕获实验表明...     

SnS2-Ag/g-C3N4三相复合材料的合成及其光催化性能

为解决单相光催化材料结构和性能上的缺陷,通过二次煅烧法获得二维石墨相氮化碳g-C₃N₄,通过光沉积法获得Ag/g-C₃N₄,选择SnS₂与Ag/g-C₃N₄通过简单的超声和蒸发溶剂的方法制备了三相复合材料SnS₂-Ag/g-C₃N₄,成功构建了n-n型异质结,并对材料的微观形貌、相结构、光响应能力和孔隙结构等进行了详尽表征。结果表明：材料依然保留了片层状结构并构建了浪花状形貌,各相结晶度较高且界面构建良好,形成了类似三明治结构的2D-0D-2D形貌,复合材料较单相材料具有更高的比表面积和更强的可见光响应性能。当SnS₂的含量为10wt%时,所合成SnS₂-Ag/g-C₃N₄复合材料对罗丹明B的光催化降解效率达到最高的95.6%,降解速率最快且为g-C₃N     

Fabrication of Co3O4 cubic nanoframes: Facet-preferential chemical etching of Fe ions to Co3O4 nanocubes

The novel Co₃O₄ cubic nanoframes, sized in ca. 30 nm, were firstly fabricated via a facile solvothermal route. Based on the transmission electron microscopy and the powder X-ray diffraction analyses of the time-dependent products, a mechanism of facet-preferential chemical etching of Fe³⁺ ions to the pre-synthesized Co₃O₄ nanocubes is proposed for the formation of Co₃O₄ cubic nanoframes. This synthetic strategy can probably be extended to fabricate nanoframes of some other binary metal oxides, by designing similar chemical etching process.     

Synthesis of Co3O4 nanoparticles via the CTAB-assisted method

Cobalt oxide (Co₃O₄) nanoparticles were successfully synthesized by the cetyltrimethylammonium bromide (CTAB)-assisted method at normal pressure for the first time. The structure and morphology of the as-prepared Co₃O₄ nanoparticles were characterized by powder X-ray diffracton (XRD), infrared spectroscopy (IR), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and N₂-sorption analysis. XRD studies indicated that the as-prepared product was well-crystallized cubic phase of Co₃O₄ with a cell constant of α = 8.0722 Å. The EM images showed that the obtained Co₃O₄ sample consisted of dispersive quasi-spherical particles with the size ranged from 15 to 25 nm.     

Synthesis and characterization of Co3O4 hollow spheres

Co₃O₄ hollow spheres were hydrothermally prepared at 130 °C for 16 h in the presence of Poly-vinylpyrrolidone (PVP). The as-prepared products were characterized by powder X-ray diffraction (XRD), field-emission scanning electron microscope (FE-SEM), transmission electron microscopy (TEM), infrared spectrum (IR), X-ray photoelectron spectrum (XPS), and optical absorption spectrum. PVP surfactant plays important roles in the formation of Co₃O₄ hollow spheres. These Co₃O₄ hollow spheres have average diameters of ca. 350 nm, and the wall thickness around the shell is about 42 nm. The possible formation mechanism of hollow Co₃O₄ spherical structures has simply been proposed.     

MoS2/g-C3N4复合催化剂的制备及CdSe量子点敏化产氢性能研究

太阳能光催化分解水制氢被认为是从根本上解决能源与环境问题较为理想的途径之一。在以尿素为原料制得石墨相氮化碳(g-C_3N_4)的基础之上,采用简单的低温溶液反应法将二硫化钼(MoS_2)与石墨相氮化碳(g-C_3N_4)复合得到复合催化剂MoS_2/g-C_3N_4,并利用透射电子显微镜(TEM)、X射线衍射(XRD)、紫外-可见漫反射(DRS)、傅里叶变换红外光谱(FT-IR)和荧光光谱等对该复合光催化剂的组成、形貌和光物理性能进行了表征;进而以CdSe量子点为光敏剂,三乙醇胺(TEOA)为牺牲剂,构建了不含贵金属的三组分光催化产氢体系,并对体系pH值、CdSe量子点浓度等对产氢性能的影响进行了研究。结果表明:将MoS_2纳米颗粒负载到g-C_3N_4上可使g-C_3N_4的光催化产氢性能得到显著提高。当MoS_2负载量为7%(质量比)时,在最佳的条件下(pH=9.0,CdSe量子点的体积为25mL),最大产氢速率达到了141.74μmol·h-1,6h的产氢总量达到了212.61μmol。最后,结合荧光猝灭实验,推测了该体系的产氢机理。     

B掺杂g-C3N4的一步合成及可见光下降解RhB和TC研究

为研究非金属离子掺杂对g-C₃N₄光催化性能的影响,以三聚氰胺和硼酸为前驱体,采用一步煅烧法制备了B掺杂g-C₃N₄光催化剂。罗丹明B(RhB)的可见光降解实验表明,当三聚氰胺和硼酸的添加比例(质量比)为10∶0.05(0.05BCN)时显示出最好的光催化性能,表现为光照RhB 30 min降解率高达100%,远高于纯g-C₃N₄(38%)。同时,四环素(TC)降解9 min达到100%,降解速率为纯g-C₃N₄的2.09倍。基于结构表征和光学性能测量,高光催化性能可归因于B原子掺杂替代引起的带隙调制。B掺杂不仅减小了带隙且可能在带隙中引入杂质态能级,这些都能导致可见光吸收的增强和光生载流子复合的抑制,从而大大提高了光催化性能。本工作提供了一种原子级水平获取非金属元素修饰g-C₃N₄纳米片的方法,该材料可作为一种在可见光下具有良好稳定性的RhB降解光催化剂。     

Synthesis and characterization of Co3O4/RuO2 composite nanofibers fabricated by an electrospinning method

Co₃O₄-RuO₂ composite nanofibers (NFs) were synthesized by an electrospinning method and were calcinated at 400°C for 1 hr in air. Scanning electron microscopy and high-resolution transmission electron microscopy (HRTEM) examinations show that all the synthesized NFs have uniform surface morphology and their diameters are in the range of ~ 30-~70 nm. X-ray diffraction (XRD) results show that crystalline Co₃O₄ phase and RuO₂ phase coexist in the composite NF matrix which is confirmed by X-ray photoemission spectroscopy. In addition, the HRTEM energy-dispersive X-ray spectroscopy mapping results show that the Co₃O₄ and RuO₂ phases are uniformly distributed across the NF matrix.     

Synthesis of sphere-like Co3O4 nanocrystals via a simple polyol route

A simple polyol method was developed to synthesize uniform sphere-like Co₃O₄ nanocrystals in ethylene glycol. Powder X-ray diffraction (XRD) and electron diffraction (ED) showed that the as-prepared sample was indexed as the cubic spinel structure. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) indicated that the Co₃O₄ nanocrystals were spherical with the crystallite size in the range of 90-110 nm. Infrared spectra and Raman spectra confirmed the formation of the Co₃O₄ nanocrystals. The magnetic properties of the Co₃O₄ nanocrystals were measured by using a superconducting quantum interference device (SQUID) magnetometer, which showed that the as-prepared sample exhibited a tiny hysteresis loop with the magnetization value of 2.4 emu/g and the coercivity of 110 Oe.     

Molten salt synthesis of single-crystal Co3O4 nanorods

The synthesis of the single-crystal Co₃O₄ nanorods by molten salt approach was reported for the first time. The products were characterized by Transmission electron microscopy (TEM), X-ray diffraction (XRD), High-resolution transmission electron microscopy (HRTEM) and Selected-area electron diffraction (SAED). TEM results indicate that these nanorods have diameters of about 150 nm and lengths of about 2 μm. According to the analysis of the SAED and HRTEM results, we drew the conclusion that these nanorods grew along an unusual [− 1,− 1,15] direction by Ostwald ripening mechanism.     

基于Pd/Fe3O4/rGO纳米复合材料的H2O2无酶传感器

环境监测、食品工业、临床、制药等领域对过氧化氢(H_2O_2)的快速、准确检测有极大的需求,而电化学检测方法由于灵敏度高、响应快、检测限低等特点被认为是最理想的H_2O_2检测方法.本文利用电化学沉积的方法将Pd纳米颗粒沉积到四氧化三铁/石墨烯(Fe_3O_4/rGO)纳米复合材料修饰的玻碳电极表面,形成基于新型磁性纳米复合材料的H_2O_2无酶传感器;并采用循环伏安和计时安培电流等方法对修饰电极的电化学性能进行了表征.结果表明:制备的Pd/Fe_3O_4/r GO/GCE对H_2O_2的催化还原显示出较好的电催化活性,Pd纳米颗粒和Fe_3O_4/rGO在催化H_2O_2还原的过程中表现出了良好的协同作用.测定H_2O_2的线性范围为0.05~1 m M和1~2.6 m M两段,最低检测限达到3.918μM(S/N=3).并且该传感器具有较高的灵敏度和较好的重现性和抗干扰性,具有一定的实际应用价值.     

Crystallinity, magnetic and electrochemical studies of PVDF/Co3O4 polymer electrolyte

Organic-inorganic nanocomposites are gaining importance in the recent times as polymer electrolyte membranes. In the present work, composites were prepared by combining nano sized Co₃O₄ and poly(vinyledene fluoride) (PVDF), using spin coating technique. The surface of the PVDF/Co₃O₄ system characterized through field emission scanning electron microscopy (FESEM) revealed a porous structure of the films. The nanoparticles tend to aggregate on the surface and inside the pores, leading to a decrease in the porosity with an increase in Co₃O₄ content. Co₃O₄ nanoparticles prohibit crystallization of the polymer. Differential scanning calorimetry (DSC) studies revealed a decrease in crystallinity of PVDF/Co₃O₄ system with an increase in the oxide content. Magnetic property studies of the composite films revealed that with an increase in Co₃O₄ content, the saturation magnetization values of the nanocomposites increased linearly, showing successful incorporation of the nanoparticles in the polymer matrix. Further, ionic conductivity of the composite films was evaluated from electrochemical impedance spectroscopy. Addition of Co₃O₄ nanoparticles enhanced the conductivity of PVDF/Co₃O₄ system.