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1.
采用简单沉积-沉淀法合成了Bi2WO6@Bi2MoO6-xF2x(BWO/BMO6-xF2x)异质结,借助XRD、XPS、TEM、SEM、EDS、UV-Vis-DRS、PC和EIS等测试技术对其组成、形貌、光吸收特性和光电化学性能等进行系统表征,并以模型污染物罗丹明B(RhB)的光催化降解作为探针反应来评价Bi2WO6@Bi2MoO6-xF2x异质结的光催化活性增强机制。形貌分析表明,所得Bi2MoO6微球由大量厚度为20~50 nm的纳米片组成;FE-SEM和HR-TEM分析表明,尺寸约为10 nm的Bi2WO6量子点均匀沉积在Bi2MoO6-xF2x微球表面,形成新颖的Bi2WO6@Bi2MoO6-xF2x异质结;与纯Bi2MoO6或者Bi2WO6相比,1∶1Bi2WO6@Bi2MoO6-xF2x异质结表现出更好的光催化活性和光电流性质,其对RhB光催化降解的表观速率常数分别为纯BMO和BWO的6.4和11.6倍。PC和EIS图谱分析表明,Bi2WO6量子点表面沉积显著提高Bi2MoO6-xF2x光生电子/空穴的分离效率和迁移速率;活性物种捕获实验证明了·O2-和h+是主要的活性物种。根据实验结果,探讨了F-掺杂和Bi2WO6量子点之间的协同效应对Bi2MoO6的光催化活性的影响机制。  相似文献   

2.
The equilibrium solubilities of the ternary system YCl3-CdCl2-H2O, the quaternary system YCl3-CdCl2-HCl(~8.8%)-H2O were determined at 25 ℃ and the phase diagrams were constructed. The results show that the ternary system was complicated with six equilibrim solid phases CdCl2·2.5H2O, CdCl2·H2O, 8CdCl2·YCl3·15H2O (8∶1 type), 4CdCl2·YCl3·13H2O(4∶1 type), 5CdCl2·2YCl3·26H2O (5∶2 type) and YCl3·6H2O. The quaternary system was also complicated with four equilibrim solid phase CdCl2·H2O, 4CdCl2·YCl3·13H2O (4∶1 type), 5CdCl2·2YCl3·26H2O(5∶2 type) and YCl3·6H2O. Among the three new compounds 8CdCl2·YCl3·15H2O, 4CdCl2·YCl3·13H2O and 5CdCl2·2YCl3·26H2O, 8CdCl2·YCl3·15H2O was a kind of metastable compound only in ternary system, and it was changed into 4CdCl2·YCl3·13H2O with time. Both 4∶1 type and 5∶2 type existed in ternary and quaternary system, but they were also congruently soluble compounds in quaternary system. They have been prepared from the system and have been characterized by XRD, TC-DTG and DSC.  相似文献   

3.
纳米Mn-Zn铁氧体的制备和研究   总被引:10,自引:0,他引:10  
Nanosize manganese zinc ferrites were fabricated by hydrothermal precipitation route using Fe2(SO4)3, ZnSO4·7H2O, MnSO4·H2O as material, then some calcinated at 500 ℃ and studied by XRD, TEM, IR and VSM. The results showed that the products were spinel crystal structure and uniformly sized nanoparticles (15~25 nm) with little aggregation. The analysis of IR showed that the superficial water can be eliminated, but that was embedded in crystal lattice can not be removed by calcinating. The effect Zn content x on the lattice (a) of nanosize Mn1-xZnxFe2O4 was also discussed. The lattice of nanosize Mn1-xZnxFe2O4 decreases with x increasing; and its value deviated the standard lattice (a0) of normal size manganese zinc ferrites. A lot of water was absorbed during the hydrothermal process owing to the large surface of nanosize particles. The change of magnetic properties of MnxZn1-xFe2O4 with x increasing was studied: nanosize MnxZn1-xFe2O4 particles synthesized by us exhibited peculiar magnetic properties curve with Zn content (x) increasing, Superparamagnetic behaviors of the synthesized ZnFe2O4 samples were confirmed by magnetic characterization, which can be explained by the difference between the distribution of the metal ions (Mn2+, Zn2+ and Fe3+) among the tetrahedral (A) and the octahedral (B) sites of nanosize ferrite and that of bulk ferrite.  相似文献   

4.
SrAl12O19:Mn4+是一种用于高显色性白光发光二极管的候选红色荧光材料。本论文研究了Mg2+、Zn2+和Ge4+离子的掺杂效应以及Ga3+、Ca2+和Ba2+离子的取代效应对SrAl12O19:Mn4+荧光材料性能的影响。样品通过高温固相反应制备,焙烧温度在1 250~1 500 ℃之间。利用X射线衍射技术表征了材料的相纯度,用荧光激发光谱和发射光谱表征了材料的荧光性能。研究结果指出,与未进行Mg2+或Zn2+掺杂的样品相比,Mg2+或Zn2+离子对Al3+格位的掺杂可以使材料的发光强度提高~60%,其原因被认为是掺杂促进了激活剂Mn4+离子进入晶格,其过程可以表示为:MO+MnO2⇔MAl''+MAl·+3OO×(M=Mg,Zn),电子顺磁共振谱支持这一结果。Ge4+离子的掺杂使材料的发光性能明显下降。Ga3+离子可以取代Al3+离子形成全范围的固溶体,其中少量Ga3+离子的掺杂可以使材料的荧光发射强度提高~13%,而掺杂量进一步提高使材料的荧光性能下降。Ca2+和Ba2+对Sr2+的取代仅形成有限范围的固溶体。Ca2+的取代使材料的发光性能提高;而 Ba2+的取代使材料的发光强度下降。  相似文献   

5.
周诗晖  王喆  张占辉 《无机化学学报》2023,39(12):2311-2316
采用高温固相法制备了2个系列的荧光粉样品:Ba2-xZnGe2O7xBi3+(系列Ⅰ)和Ba1.994-yKyZnGe2O7:0.006Bi3+(系列Ⅱ)。X射线衍射(XRD)测试结果表明,少量Bi3+、K+的掺杂不会明显改变材料的物相结构。样品的荧光光谱测试结果表明,虽然2个系列样品的发光光谱都随组成成分变化有少量变化,但发光颜色基本上均为黄绿色。在358 nm的激发下,荧光粉的发射光谱呈现一个峰值在500 nm的宽发射带,归属于3P11S0能级跃迁。在500 nm监测下,荧光粉的最强激发峰位于358 nm,归属于1S03P1能级跃迁,此外还有一个位于320 nm的肩峰归属于O2--Bi3+电荷转移带。系列Ⅰ样品的光谱数据结果指出,Bi3+的最佳掺杂量x为0.006。在该基质中,Bi3+掺杂取代Ba2+属于不等价取代,会在晶格中产生Ba2+空位或间隙O2-,对材料的发光强度产生负面影响。对此,采用K+与Bi3+协同掺杂起到电荷补偿的作用,填补Ba2+空位或捕获间隙O2-缺陷。空位被填补或间隙被捕获均减少了晶格畸变,从而使发光强度明显提高。系列Ⅱ样品的光谱数据表明,完全电荷补偿的荧光粉样品相比于没有掺K+的样品,其发光强度提高了约2.5倍。  相似文献   

6.
利用类石墨氮化碳(g-C3N4)和亚稳相钙钛氧化物(CaTi2O5)固相法制备C3N4/CaTi2O5复合材料。利用X射线衍射(XRD)、金相显微镜、扫描电子显微镜(SEM)及附带能谱分析仪(EDS)和N2吸附-脱附对样品的显微结构和比表面积进行检测分析,并用紫外-可见吸收光度计(UV-Vis)测试了样品的光吸收性能,研究C3N4与CaTi2O5物质的量之比(nC3N4/nCaTi2O5)对C3N4/CaTi2O5复合样品的物相结构和微观形貌的影响,同时考察C3N4/CaTi2O5复合样品在可见光照射下光催化降解罗丹明染料效果。实验结果表明:相比纯C3N4和CaTi2O5样品,C3N4/CaTi2O5复合样品在可见光下具有较高的光催化性能,随着nC3N4/nCaTi2O5增加,样品的光催化降解率随之增加而后降低,当nC3N4/nCaTi2O5=1:1时,样品的光催化降解率达到最大值99.5%,并且循环重复利用5次后,样品的光催化剂降解率仍几乎保持不变。复合样品光催化性能提高主要归因于复合能级结构有效地抑制了电子和空穴复合所致。  相似文献   

7.
钙钛矿型LaxSr1-xNi1-yCoyO3光电催化活性研究   总被引:1,自引:0,他引:1  
用甘氨酸-硝酸盐燃烧合成法, 制备LaxSr1-xNi1-yCoyO3复合氧化物的陶瓷粉末, 对钙钛矿氧化物进行了XRD结构分析. 在通氧或不通氧下测试氧还原和氧析出的循环伏安曲线. 结果表明: 该氧电极具有双功能催化特性, 但不完全可逆. 利用汞灯作为激发光源, 进行几种水溶性染料和五种混合染料光解实验, 利用紫外-可见、红外以及人工神经网络光度法研究LaxSr1-xNi1-yCoyO3的催化性能. 结果表明: LaxSr1-xNi1-yCoyO3 (x=0.7, 0.9, 1; y=0.3, 0.75)复合氧化物都具有较强光催化特性; LaxSr1-xNi1-yCoyO3的光催化活性高于LaxSr1-xNiO3, 这与B位离子(Ni2—, Co2-)的电子构型有关; Co2+的加入可使LaxSr1-xNiO3的光催化活性有所提高.  相似文献   

8.
CO2在纳米SiO2/TiO2悬浮体系中的光催化还原   总被引:6,自引:0,他引:6  
用水热法合成了氧化硅改性的具有高比表面积、高催化活性的锐钛型二氧化钛, 并在其悬浮体系中将CO2光催化还原合成甲醇. 采用XRD, TEM, 物理吸附, UV-Vis吸收光谱和FTIR等表征手段对催化剂结构特征进行了研究. 结果表明: 添加氧化硅后, 氧化硅和二氧化钛之间形成Si—O—Ti键, 抑制了TiO2晶粒生长, 提高了锐钛型TiO2的比表面积, 且随着含硅量的增加, SiO2/TiO2的UV吸收逐步蓝移, 禁带宽度增加. 还原反应结果表明: SiO2/TiO2具有光催化还原活性, 且随着含硅量的增加先增加后减小, 当SiO2质量分数为3.5%时, SiO2/TiO2复合催化剂反应活性最强, 5 h内甲醇产量可达到21.0 mg/L, 并有少量甲醛生成.  相似文献   

9.
以4种Keggin型多酸作为原料(分别为H3PW12O40·36H2O(简写为PW12a)、H3PMo12O40·34H2O(简写为PMo12a)、H4SiW12O40·35H2O(简写为SiW12a)和H4GeW12O40·40H2O(简写为GeW12a)),采用表面活性剂智能化控制的软化学法制备了相应的4种Keggin型多酸纳米材料,分别为Ag3PW12O40·36H2O(简写为PW12b)、Ag3PMo12O40·34H2O(简写为PMo12b)、Ag4SiW12O40·35H2O(简写为SiW12b)和Ag4GeW12O40·40H2O(简写为GeW12b)。采用IR、UV-Vis、XRD和SEM表征多酸的结构和纳米粒子的形貌。在室内黑暗条件下,100mg样品可在5min内把20mg·L-1的100mL亚甲基蓝(MB)染料溶液脱色,使其变为接近无色,吸附效率最高可达96.3%,吸附效率大小为PMo12b >PW12b >GeW12b >SiW12b。相同条件下,100mg样品使20mg·L-1的100mL罗丹明B(RhB)染料溶液30min内脱色完全,脱色效率最高可达96.1%,吸附效率大小为PW12b >PMo12b >SiW12b >GeW12b。说明该4种多酸纳米材料具有较高的吸附有机染料性能。  相似文献   

10.
以共沉淀法与煅烧法联用,成功制备了一系列ZnAl2O4:xMn样品。通过扫描电镜和X射线粉末衍射测试研究了样品的形貌和物相特征,结果表明尖晶石结构的ZnAl2O4中[AlO6]的八面体位可以有效被Mn4+替代。通过荧光激发和发射光谱研究了样品的发光性能,发现Mn4+在ZnAl2O4体系中掺杂可以显示出明亮的红色发光(发射峰值位于680 nm处)。比较不同Mn4+浓度(Mn与Al的物质的量之比)掺杂样品的发光强度时发现,Mn4+最佳掺杂浓度为0.06%。通过德克斯特公式分析了发光强度与浓度关系,探究浓度猝灭机制,结果表明最邻近离子之间能量传递造成Mn4+浓度猝灭的发生。为了提高Mn4+的发光强度,选择了7种金属离子(Li+、Na+、K+、Ca2+、Sr2+、Sn2+和Ga3+)与Mn4+共掺杂进入ZnAl2O4基质中,其中效果较突出的为Li+和Ga3+,其共掺杂使Mn4+发光强度分别增强0.6倍和1倍。  相似文献   

11.
采用多壁碳纳米管(MWNT)改性聚N,N-二甲基苯胺(PDMA)膜,制备了新型复合膜修饰玻碳电极,并用SEM、电化学方法对修饰电极进行表征。 结果表明,无论MWNT是以掺杂还是先滴涂MWNT再聚合DMA多层修饰方式,均会改变PDMA膜的形貌和电化学性能。 复合膜修饰电极比单一PDMA膜修饰电极大幅度提高了比表面积和电活化面积,同时使PDMA和MWNT更好地协同发挥其优良的电化学特性。 实验结果表明,层层修饰制备的聚N,N-二甲基苯胺/多壁碳纳米管复合膜修饰电极对香草醛的电化学响应远大于基体电极和其它方法制备的修饰电极,电催化作用显著提高,其过电位降低了148 mV,氧化峰电流约增加了6倍;其电极反应是吸附控制的不可逆氧化过程,转移电子数n为2,质子数m为1,传递系数α为0.4062,吸附量为Γ=3.527×10-9 mol/cm2;检出下限为8.0×10-7 mol/L,样品平均回收率为99.87%。  相似文献   

12.
研究了掺杂多壁碳纳米管(MWNT)改性聚溴甲酚绿膜(PBG),以不同修饰方法制备了4种修饰电极,用扫描电镜、交流阻抗及循环伏安法等对电极进行表征。结果表明:4种修饰电极的电活化面积均得到明显提高,其中以层层修饰制备的聚溴甲酚绿膜/多壁碳纳米管复合膜(PBG/MWNT/GC)电极最能发挥MWNT和PBG的电活性。将电极用于8-羟基喹啉(8-HQ)电化学行为的研究,结果表明:4种修饰电极的伏安响应明显提高,且8-HQ在PBG/MWNT/GC上的氧化峰电位负移最多,峰电流最大,约为裸玻碳电极的4.5倍,电催化作用显著增强。8-HQ在PBG/MWNT/GC上电极反应的电子转移数和质子数均为1,是吸附控制的不可逆电氧化过程,氧化峰电流Ip与浓度c在4.0×10-6~3.5×10-4mol/L范围内呈良好的线性关系,r=-0.997 2,检出限(S/N=3)为1.96×10-8mol/L。PBG/MWNT/GC修饰电极可实现8-HQ的快捷、简便测定。  相似文献   

13.
用壳聚糖对多壁碳纳米管进行修饰,构建了一种用于固定血红蛋白的新型复合材料,并研究了血红蛋白在该碳纳米管上的电化学性质及其对过氧化氢的电催化活性.扫描电镜结果表明,壳聚糖修饰的多壁碳纳米管呈单一的纳米管状,并能均匀分散在玻碳电极表面.紫外光谱分析表明血红蛋白在该复合膜内能很好地保持其原有的二级结构.将该材料固定在玻碳电极上后,血红蛋白能成功地实现其直接电化学.根据峰电位差随着扫描的变化,计算得到血红蛋白在壳聚糖修饰的碳纳米管膜上的电荷转移系数为0.57,表观电子转移速率常数为7.02 s-1.同时,该电极对过氧化氢显示出良好的催化性能,电流响应信号与H2O2浓度在1.0×10-6 ~1.5×10-3 mol/L间呈线性关系,检出限为5.0×10-7 mol/L.修饰电极显示了良好的稳定性.  相似文献   

14.
《Electroanalysis》2006,18(21):2085-2091
A nanocomposite electrochemical sensing film is assembled on choline (Ch) modified glassy carbon electrode (GCE), which contains multiwalled carbon nanotubes (MWNTs), Nafion cation exchanger, and myoglobin (Mb) or hemoglobin (Hb). The MWNTs provide a 3D porous and conductive network for the enzyme immobilization and Nafion acts as polymeric binder to give cast thin films. Both MWNTs and Nafion provide negative functionalities to bind to the positively charged redox proteins and to attach at the positively charged Ch modified layer, and drive the formation of homogeneous and stable nanocomposite film, the MWNT‐Nafion‐Mb. The nanocomposite film was characterized by field emission scanning electron microscope (FE‐SEM). The Mb in the nanocomposite film showed a pair of well‐defined and nearly reversible cyclic voltammetric peaks at about ?0.32 V vs. SCE at pH 7.0 solution for the heme Fe(III)/Fe(II) redox couple. The immobilized heme proteins can display the features of peroxidase in electrocatalytic reductions of oxygen, hydrogen peroxide, nitric oxide, trichloroacetic acid (TCA), and bromate.  相似文献   

15.
A new method to modify electrodes with carbon nanotubes (CNT) was developed. Multiwalled carbon nanotubes (MWNT) were adsorbed on the electrospun nylon‐6 nanofibrous membranes (Ny‐6‐NFM) and used as a coating to modify conventional glassy carbon electrodes. The modified electrode was designed for the amperometric detection of sulfhydryl compounds with the potential held at +0.3 V vs. Ag/AgCl. The modified electrode showed a linear response for cysteine up to 0.4 mM (R2=0.997), with a sensitivity of 5.1 µA/mM and a detection limit of 15 µM. Other sulfhydryl compounds showed similar results. After use, the Ny‐6‐NFM was easily peeled off, leaving the bare electrode surface back to its original electrochemical behaviour. This is the first attempt to use a disposable membrane functionalized with MWNT for electroanalytical purposes.  相似文献   

16.
《Analytical letters》2012,45(9):1785-1799
Abstract

Multiwalled carbon nanotubes (MWNTs) were treated with a mixture of concentrated sulfuric and nitric acid to introduce carboxylic acid groups to the nanotubes. Conducting polymer film was prepared by electrochemical polymerization of neutral red (NR). By using a layer‐by‐layer method, homogeneous and stable MWNTs and poly (neutral red) (PNR) multilayer films were alternately assembled on glassy carbon (GC) electrodes. With the introduction of PNR, the MWNTs/PNR multilayer film system showed synergy between the MWNTs and PNR, with a significant improvement of redox activity due to the excellent electron‐transfer ability of carbon nanotubes (CNTs) and PNR. The electropolymerization is advantageous, providing both prolonged long‐term stability and improved catalytic activity of the resulting modified electrodes. The MWNTs/PNR multilayer film modified glassy carbon electrode allows low potential detection of hydrogen peroxide with high sensitivity and fast response time. As compared to MWNTs and PNR‐modified GC electrodes, the magnitude of the amperometric response of the MWNTs/PNR composite‐modified GC electrode is more than three‐fold greater than that of the MWNTs modified GC electrode, and nine‐fold greater than that of the PNR‐modified GC electrode. With the immobilization of glucose oxidase onto the electrode surface using glutaric dialdehyde, a biosensor that responds sensitively to glucose has been constructed. In pH 6.98 phosphate buffer, nearly interference‐free determination of glucose has been realized at ?0.2 V vs. SCE with a linear range from 50 µM to 10 mM and response time <10s. The detection limit was 10 µM glucose (S/N=3).  相似文献   

17.
《Electroanalysis》2006,18(16):1564-1571
The work details the electrocatalysis of oxygen reduction reaction (ORR) in 0.5 M H2SO4 medium on a modified electrode containing a film of polyaniline (PANI) grafted multi‐wall carbon nanotube (MWNT) over the surface of glassy carbon electrode. We have fabricated a novel modified electrode in which conducting polymer is present as connected unit to MWNT. The GC/PANI‐g‐MWNT modified electrode (ME) is fabricated by electrochemical polymerization of a mixture of amine functionalized MWNT and aniline with GC as working electrode. Cyclic voltammetry and amperometry are used to demonstrate the electrocatalytic activity of the GC/PANI‐g‐MWNT‐ME. The GC/PANI‐g‐MWNT‐ME exhibits remarkable electrocatalytic activity for ORR. A more positive onset potential and higher catalytic current for ORR are striking features of GC/PANI‐g‐MWNT‐ME. Rapid and high sensitivity of GC/PANI‐g‐MWNT‐ME to ORR are evident from the higher rate constant (7.92×102 M?1 s?1) value for the reduction process. Double potential chronoamperometry and rotating disk and rotating ring‐disk electrode (RRDE) experiments are employed to investigate the kinetic parameters of ORR at this electrode. Results from RDE and RRDE voltammetry demonstrate the involvement of two electron transfer in oxygen reduction to form hydrogen peroxide in acidic media.  相似文献   

18.
WANG Yuane  PAN Dawei  LI Xinmin  QIN Wei 《中国化学》2009,27(12):2385-2391
A bismuth/multi‐walled carbon nanotube (Bi/MWNT) composite modified electrode for determination of cobalt by differential pulse adsorptive cathodic stripping voltammetry is described. The electrode is fabricated by potentiostatic pre‐plating bismuth film on an MWNT modified glassy carbon (GC) electrode. The Bi/MWNT composite modified electrode exhibits enhanced sensitivity for cobalt detection as compared with the bare GC, MWNT modified and bismuth film electrodes. Numerous key experimental parameters have been examined for optimum analytical performance of the proposed electrode. With an adsorptive accumulation of the Co(II)‐dimethylglyoxime complex at ?0.8 V for 200 s, the reduction peak current is proportional to the concentration of cobalt in the range of 4.0×10?10?1.0×10?7 mol/L with a lower detection limit of 8.1×10?11 mol/L. The proposed method has been applied successfully to cobalt determination in seawater and lake water samples.  相似文献   

19.
将多壁碳纳米管(MWNT)分散在疏水性表面活性剂双十六烷基磷酸(DHP)溶液中形成稳定、均相的分散液,然后制备多壁碳纳米管-DHP复合膜修饰玻碳电极(MWNT-DHP/GCE).应用方波伏安法研究了沙丁胺醇在修饰电极上的电化学行为,结果表明,碳纳米管复合膜修饰电极对沙丁胺醇的氧化有良好的电催化活性,其氧化反应为一电子一质子过程,氧化电位比裸玻碳电极负移40 mV,峰电流增加了4.5倍.在最佳测试条件下,氧化峰电流与沙丁胺醇浓度在8.3×10-7~3.3×10-6mol/L范围内呈良好线性关系,开路富集2min,检出限达1.8×10-7mol/L.该修饰电极具有良好的重现性、稳定性.  相似文献   

20.
Electrochemical behavior of myoglobin (Myb) incorporated on multi-walled carbon nanotubes (MWNTs) modified GC electrode is investigated by electrochemical impedance spectroscopy (EIS) and cyclic voltammetry (CV). The results indicate that Myb can be strongly adsorbed on the surface of the MWNT-modified electrode to form an approximate monolayer film. MWNTs can greatly promote the redox of horse heart Myb, on which a pair of well-defined and nearly reversible CV peaks for Myb Fe(III)/Fe(II) redox couple were obtained in pH 7.0 buffers. The formal potential of Myb on MWNT modified electrode shifts linearly with pH with a slope of −56.4 mV/pH, showing that the electron transfer is accompanied by single proton transportation. The high efficiency of the Myb/MWNT modified electrode towards the catalytic electro-reduction of nitric oxide has been observed. Potential application of Myb/MWNT modified electrode as biosensors to monitor NO is proposed.  相似文献   

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