CROSS-LINKING OF CHITOSAN WITH GLUTARALDEHYDE IN THE PRESENCE OF CITRIC ACID——A NEW GELLING SYSTEM

The procedure for preparing a new type of uniform and porous chitosan gel from citric acid medium is described. Its swelling behavior in different media was compared with those of the gels prepared by other methods. The ultrastructure of the xerogel prepared from citric acid was characterized using electron microscopy (SEM).

Citric Gel Synthesis and Luminescent Properties of Ce^(3+)-Activated SrGa_2O_4 Phosphor

Ce^3＋-activated SrGa2O4 phosphor was synthesized by a method of citric gel,wherein citric acid served as a chelate agent,and the as-synthesized powder was calcined in a slightly reduced ambient.The crystallization characteristics of the sample varied with the calcining temperature.Compared with the phosphor prepared by the solid-state reaction,the phosphor synthesized by citric gel was calcined at a relatively lower temperature.Consequently,the volatilization of Ga2O3 during high-temperature calcining process was avoided.The typical double-peak emission of Ce^3＋ originated from 2D（5d）→4F5/2（4f）,and 2D（5d）→4F7/2（4f）was observed,and the intrinsic emission of SrGa2O4 host was much restricted.The emission intensity varied with the calcining temperature because the different crystallinity and the optimal concentration of Ce-dopant was determined at 3%.

The Mechanism of Sol-Gel Synthesis of Normal Spinel LiMn_2O_4 with Chelation of Citric Acid

The sol-gel process of citric acid chelating with metal cations for the synthesis of normal spinel LiMn 2O 4 and the reaction mechanism were investigated by means of XRD,IR,TG-DTA, and SEM.The results show that at the beginning lithium citrate and chelate compound of citric acid with manganese ions formed,and then with heating the esterification and condensation reactions occured between them and glycol.The products obtained are polymers in which metal cations are distributed homogeneously on atomic scale that ensure high reactivity to cations of Li + and Mn 2+.Firing the gel prepared by this process,the lattice diffusions of solid reactant ions caused by non-homogeneity of reactants are eliminated and avoided.At 400℃ phase-pure LiMn 2O 4 with nanometer scale crystallization having precise stoichiometry and perfect crystallization can be obtained.The model of chelate coordinate of double-molecule between citric acid and Mn 2+ in the gel network is proposed.It is important for explaining the dispersion state of Mn 2+ and the formation process of gel by this model.

Influence of citric acid content on magnetic properties of BaFe12O19 powder prepared by sol-gel auto-combustion method

BaFe12O19 powders with nanocrystaUine sizes were produced by sol-gel auto-combustion method. The precursors were prepared under the molar ratios of citric acid to the metal nitrate of 0.5, 1.0 and 1.5. Appropriate ethylene diamine （C2H8N2） was added in order to adjust pH of 7. The ions distribution of citric acid at different pH explains the effect of citric acid in the starting solution. The XRD patterns of the as-burnt powders and annealing powders show different phases for different citric acid content. In addition, the lattice constants （a, c） derived from X-ray diffraction pattern were changed from 0.58881 nm to 0.58997 nm and 2.32057 nm to 2.32296 nm respectively. The data from VSM indicated that the powder with high citric acid content took on good magnetic properties. Pure single BaFe12O19 of the specific maximum magnetization M（1 T）≈ 49.73 Am^2/kg, the specific remanent magnetization Mr ≈ 30.77 Am^2/kg and the coercive force He≈ 467 kA/m was produced when the molar ratios of citric acid to the metal nitrate was 1.5.

sol-gel法制备Ba_(3.99)Sm_(9.34)Ti_(18)O_(54)微波介质陶瓷

以柠檬酸为络合剂,通过sol-gel法制备了Ba3.99Sm9.34Ti18O54陶瓷前驱体;经1100℃预烧2h压片成型后,再在1300℃保温3h,即得到了烧结致密的陶瓷样品。与传统固相法相比,其烧结温度降低了50℃,且陶瓷晶粒细小,晶粒分布均匀,具有更加优良的微波介电性能:εr=79.56,Q·f=9636GHz(4.71GHz),τf=–1.23×10–6/℃。

溶胶-凝胶法合成钛酸锌锂负极材料

以溶胶-凝胶法制备锂离子电池Li_(2)ZnTi_(3)O_(8)(LZTO)负极材料,考察退火温度和退火时间对LZTO电化学性能的影响,得到了最佳工艺条件:退火温度为700℃,退火时间为3 h。在最佳工艺条件下制备的LZTO中添加络合剂柠檬酸进行了改性。结果表明,当金属离子与柠檬酸的物质的量比为2.00∶1.50时,制备的样品LZTO-2/1.50颗粒小、分散均匀,表现出良好的电化学性能;当电流密度为0.5 A/g时,恒流充放电300次后放电比容量为203.6 mA·h/g。

纳米ZnO·Bi_2O_3·La_2O_3复合粉体的Sol-Gel法制备工艺与表征

纳米ZnO作为应用前景意义很大的半导体材料,有较高的研究价值,为此以Zn(AC)2.2H2O、La2O3、Bi(NO3)3.5H2O为主要原料,柠檬酸为络合剂,利用溶胶-凝胶法制备了纳米ZnO.Bi2O3.La2O3复合粉体.通过实验研究制备纳米ZnO.Bi2O3.La2O3复合粉体的最佳工艺条件,并利用x-射线衍射(XRD)、透射电镜(TEM)、比表面积测定对制备的复合粉体性能进行表征.结果表明,在最佳工艺条件下,干凝胶在600℃条件下煅烧2 h,得到了粒径分布约为54 nm、比表面积为120.77 m2/g的纳米ZnO.Bi2O3.La2O3复合粉体,说明溶胶-凝胶法制备纳米ZnO有较好的结果.

Sol-gel synthesis and photoluminescence characterization of La_2Ti_2O_7:Eu^(3+) nanocrystals

Eu3＋ doped La2Ti2O7 nanocrystals with pure monoclinic phase and size of about 100 nm were prepared by a citric acid （CA） assisted sol-gel method. Techniques of thermo-gravimetric （TG） and differential scanning calorimetry （DSC）, X-ray diffraction （XRD）, as well as transmission electron microscopy （TEM） were employed to characterize the as-synthesized nanoparticles. Furthermore, photoluminescence （PL） performances of the Eu3＋ doped La2Ti2O7 nanocrystals were evaluated with focus on the effects of calcination temperature and Eu3＋ doping concentration on the photoluminescence properties.

Preparation and optical characteristics of ZnO films by chelating sol-gel method

The effect of different annealing temperatures on the structure, morphology,and optical properties of ZnO thin films prepared by the chelating sol-gel method was investigated.Zinc-oxide thin films were coated on quartz glass substrates by dip coating. Zinc nitrate, absoluteethanol, and citric acid were used as precursor, solvent, and chelating agent, respectively. Theresults show that ZnO films derived from zinc-citrate have lower crystallization temperature (below400℃), and that the crystal structure is wurtzite. The films, treated over 500℃, consist ofnano-particles and show to be porous at 600℃. The particle size of the film increases with theincrease of the annealing temperature. The largest particle size is 60 nm at 600℃. The opticaltransmittances related to the annealing temperatures become 90% higher in the visible range. Thefilm shows a starting absorption at 380 nm, and the optical band-gap of the thin film (fired at500℃) is 3.25 eV and close to the intrinsic band-gap of ZnO (3.2 eV).

SYNTHESIS OF MESOPOROUS POLY(STYRENE-co-MALEIC ANHYDRIDE)/SILICA HYBRID MATERIALS VIA A NONSURFACTANT-TEMPLATED SOL-GEL PROCESS

Mesoporous poly(styrene-co-maleic anhydride)/silica hybrid materials have been prepared. The synthesis was achieved by the HCl-catalyzed sol-gel reactions of tetraethyl orthosilicate (TEOS) and styrene-maleic anhydride copolymer in the presence of 3-aminopropyl triethoxysilane (APTES) as a coupling agent and citric acid as a nonsurfactant template or pore-forming agent, followed by ethanol extraction. Characterization results from nitrogen sorption isotherms and powder X-ray diffraction indicate that polymer-modified mesoporous materials with large specific surface areas (e.g. 900 m(2)/g) and pore volumes (e.g. 0.6 cm(3)/g) could be prepared. As the citric acid concentration is increased, the specific surface areas, pore volumes and pore diameters of the hybrid materials increase.

Preparation and Characterization of Pb(Zr_(0.52)Ti_ (0.48))O_3 Ultrafine Powders by a Sol-gel Combined with Combustion Process

A simple and rapid process for synthesizing lead zirconate titanate,Pb（Zr0.52Ti0.48）O3（PZT）,ferroclectric powders was developed.This process,combining the sol-gel and combustion process.offers several advantages over conventional methods.including rapid solution synthesis,use of commercially available materials lower synthesis temperature and ease of obtaining ultrafine powders.The precursor solution for synthesizing powders was prepared from lead nitrate.zireonium nitrate.titanium oxynitrate,citric acid and deionized water.The precarsor was investigated by DSC-TG,and the PZT powders were investigated by powder-XRD,IR spectra and TEM.XRD analysis shous that the powders possess a single phase perovskite type structure,no pyrochlore phase exists.and TEM image shows that the grain size of the powders is about 40nm.

Preparation and electrochemical performance of Li_2Mn_(0.5)Fe_(0.5)SiO_4 cathode material with sol-gel method for lithium ion batteries

Li2Fe0.5Mn0.5SiO4 material was synthesized by a citric acid-assisted sol-gel method. The influence of the stoichiometric ratio value of n(citric acid) to n(Fe2+-Mn2+) on the electrochemical properties of Li2Fe0.5Mn0.5SiO4 was studied. The final sample was identified as Li2Fe0.5Mn0.5SiO4 with a Pmn21 monoclinic structure by X-ray diffraction analysis. The crystal phases components and crystal phase structure of the Li2Fe0.5Mn0.4SiO4 material were improved as the increase of the stoichiometric ratio value of n(citric acid) to n(Fe2+-Mn2+). Field-emission scanning electron microscopy verified that the Li2Fe0.5Mn0.5SiO4 particles are agglomerates of Li2Fe0.5Mn0.5SiO4 primary particles with a geometric mean diameter of 220 nm. The Li2Fe0.5Mn0.5SiO4 sample was used as an electrode material for rechargeable lithium ion batteries, and the electrochemical measurements were carried out at room temperature. The Li2Fe0.5Mn0.5SiO4 electrode delivered a first discharge capacity of 230.1 mAh/g at the current density of 10 mA/g in first cycle and about 162 mAh/g after 20 cycles at the current density of 20 mA/g.

磁条中的铁氧体材料制备工艺和磁性能研究

以硝酸钡、硝酸铁与柠檬酸为原料,依据溶胶-凝胶法设计铁氧体材料制备工艺,制备铁氧体材料。通过振动样品磁强计,分析在不同煅烧温度和原料比例条件下所制备铁氧体材料的磁导率;利用扫描电子显微镜,分析材料的微观形貌;利用阻抗分析仪,分析材料的磁导率;采用霍尔效应测试仪,研究铁氧体材料磁性能。实验结果表明,煅烧温度由750℃升至1 150℃时,材料晶粒生长越充分,实部、虚部磁导率以及磁化强度均先上升后下降;煅烧温度为950℃时,实部、虚部磁导率以及磁化强度均最高,在280 H/m、98 H/m与81.99 A□m2/kg左右;煅烧温度与材料收缩率呈正比。综合分析磁导率、收缩率与磁化强度得出,最优煅烧温度为850℃至1 050℃,此时材料磁性能最优;提升硝酸铁添加量,可提升材料的磁导率,即提升材料磁性能,最佳硝酸钡与硝酸铁比例是1∶9;提升柠檬酸添加量,可优化材料磁性能,最佳柠檬酸比例是1.2。

柠檬酸-凝胶法合成ZnGa_2O_4∶Mn^(2+)/Eu^(3+)及其发光性能的研究

采用柠檬酸 凝胶法合成了纯的ZnGa2 O4粉末以及ZnGa2 O4∶Mn2 + /Eu3 + 粉末 ,利用X射线衍射(XRD)、热重及差热分析 (TG DTA)、发光光谱等测试手段对ZnGa2 O4和ZnGa2 O4∶Mn2 + /Eu3 + 的结晶过程、发光性质进行了研究。XRD结果表明 ,柠檬酸 凝胶法合成的样品在 5 0 0℃时已开始结晶 ,在 70 0℃时可得到纯相的ZnGa2 O4多晶粉末 ,这比传统固相法的烧结温度低 5 0 0℃。发光光谱测试表明ZnGa2 O4∶Mn2 + 在4 5 0nm和 5 0 6nm处出现两个发射带 ,前者属于ZnGa2 O4基质的发射 ,后者属于Mn2 + 的4T1→6A1的跃迁发射。ZnGa2 O4∶Eu3 + 则呈现Eu3 + 的特征红光发射 ,最强峰位于 6 13nm ,属于Eu3 + 的5D0 →7F2 超灵敏跃迁。通过光谱分析进一步证实了ZnGa2 O4∶Mn2 + /Eu3 + 的发光机理是基质敏化 。

溶胶-凝胶法制备纳米氧化镁

以六水硝酸镁为前驱体,采用柠檬酸溶胶-凝胶法合成了不同粒径(10-100nm)和结晶度的纳米MgO粉末。研究了柠檬酸的作用机理、不同的工艺条件(水、无水乙醇、柠檬酸的加入量)对溶胶-凝胶稳定性的影响以及焙烧温度对粉末晶体粒径、结晶度的影响。结果表明:未引入柠檬酸时,凝胶的稳定性较差,氧化镁产物粒径较大且团聚较严重。引入柠檬酸后,并当水:六水硝酸镁:柠檬酸:乙醇=100:9:9:2:1(摩尔比)时可形成稳定的凝胶体系。焙烧温度对制得的MgO粉末的化学成分和晶体形貌基本无影响,但对粉末结晶度和粒径有显著的影响。500℃焙烧制得的纳米氧化镁粉末粒径为10nm左右,结晶度低,粒子间有一定的团聚;600℃的粉末粒径为30-60nm,结晶度有所提高,粒子的分散性较好;900℃的粉末粒径为50-100nm,结晶度更高,晶相更完整。

超细层状材料A_2La_2Ti_3O_(10)(A=Na,K)的低温合成及表征

s: Ultrafine A2La2Ti3O10 (A=K, Na) powders with laminar structure were successfully synthesized by citric acid sol-gel method using ANO3(A=K, Na)?La(NO3)3?Ti(OBu)4 and citric acid as starting precursors. The crystalline phase of A2La2Ti3O10 can be obtained by thermal decomposition of citrate complex precursors at a relatively low temperature of 800 ℃ (600 ℃ for A=Na), about 300 ℃(500 ℃ for A=Na) lower than that of conventional solid state reaction process. The properties of the citrate precursors and the calcined powders were characterized by Infrared spectroscopy (IR), X-ray diffraction (XRD), transmission electron microscopy (TEM), thermal-gravimetric-differential thermal analysis (TG-DTA), inductively coupled plasma (ICP) and Brunauer-Emmett-Teller (BET) techniques. Results show that the average size of A2La2Ti3O10 powders obtained by citric acid sol-gel route was reduced to 200 nm×250 nm and the specific surface area was up to 19 m2·g-1. At the same time, the product was with more regular morphological characteristics. The synthesis process and the formation of A2La2Ti3O10 were also discussed. The obtained A2La2Ti3O10 was found to be transformed from A2La2Ti3O9.5 during the formation process.

柠檬酸溶胶-凝胶法制备钡铁氧体

应用solgel技术制备纳米钡铁氧体,研究了3种不同的solgel制备工艺对钡铁氧体生成过程的影响。研究结果表明,影响solgel制备的因素有:温度、pH值和柠檬酸用量、助剂、杂质的处理及溶胶回流的选择;钡铁氧体晶体的平均粒径、结晶形状,分布,团聚程度都影响其磁性质。3种实验方法均可制得高纯度BaFe12O19(简称BaM)磁性材料。在3种方法中,工艺Ⅲ的综合性能最好,在900℃得到钡铁氧体平均粒径为155nm,其比饱和磁化强度Ms=58.78Am2/kg,矫顽力Hc=407.9kA/m。

YAG∶Ce荧光粉的柠檬酸-凝胶法合成与表征

采用柠檬酸-凝胶法合成技术制备YAG∶Ce荧光粉,研究了Ce3+掺杂量、煅烧温度对荧光粉的光谱强度的影响。结果表明:当Ce3+掺杂量x≤0.07时,光谱强度随x增大而增强;当x>0.07时,光谱强度随x增大而减弱。随着煅烧温度的提高,粉体的结晶度不断提高,YAG∶Ce荧光粉的光谱相对强度逐渐增强。光谱的峰形和峰值不受温度和x的影响,主激发峰位于469nm,发射峰位于529nm。

两种络合剂对Ce-Sn-O复合氧化物结构与性能的影响

分别以柠檬酸、葡萄糖为络合剂,用溶胶-凝胶法制备了CeO_2和掺杂少量Sn的Ce-Sn-O复合氧化物,利用XRD、TPR、FT-IR、比表面法、TEM等方法表征了四种催化剂的物理化学性质,同时以甲烷催化燃烧反应为探针对其进行了活性评价.结果表明,以葡萄糖为络合剂合成的掺杂锡后的样品其甲烷完全转化温度较低,比表面积较大,通过透射电子显微镜观察,平均晶粒大小为14nm左右,且分散性良好,而相比之下柠檬酸为络合剂合成的样品出现明显的团聚现象.

溶胶-凝胶法制备Bi_2WO_6微纳米材料及其光催化性能

为了开发可见光响应型光催化剂,以柠檬酸为络合剂,采用溶胶-凝胶法制备前驱体,通过煅烧得到了Bi2WO6微纳米材料。采用X-射线衍射(XRD)、场发射扫描电镜(FESEM)、紫外-可见光漫反射谱(UV-vis DRS)等技术对其进行表征,考察了制备条件对样品晶相结构的影响。结果表明,在煅烧温度450℃、煅烧时间3 h、柠檬酸与Bi3+的物质的量比为3∶1、前驱液的pH=1、分散剂为PEG-4000的条件下制备的Bi2WO6样品为斜方晶系Bi2WO6结构,由粒径为50 nm左右的小薄片堆积而成。所得的Bi2WO6样品具有优良的光催化性能,在可见光照射(200 W点钨灯)及H2O2助剂的存在下,对10 mg/L罗丹明B溶液的光降解率可达82.0%。研究结果可为高效Bi2WO6光催化材料的制备提供新的思路。