二氧化硅包覆磁性纳米粒子的制备与表征

由多元醇法制得四氧化三铁纳米粒子,利用Stber水解法在其表面生成了一层无定型二氧化硅包覆层。由于四氧化三铁纳米粒子的特殊表面结构,使其在醇水体系中能够保持良好的胶体稳定性,并与硅酸酯有亲和作用,所得Fe3O4/SiO2复合纳米粒子包覆均匀,尺寸可控。     

PS/SiO2复合微球包覆过程的可控研究

采用分散聚合法制备的聚苯乙烯(PS)阳离子微球为模板,以正硅酸乙酯(TEOS)为前驱体,经溶胶-凝胶反应和静电吸附作用,形成结构稳定的PS/SiO2核壳复合微球,并采用SEM、TEM和Zeta电位仪对制备过程中的主要影响因素进行了研究.结果表明,氨水用量增加可以加速包覆过程,并使表面包覆层粗糙;PS表面电荷密度越大,SiO2在PS微球表面吸附效果越好;复合微球壳层厚度则会随着TEOS用量增加而增加.     

Fe-SiO2磁性核壳复合粒制备与表征

采用溶胶凝胶方法制备羰基铁/Si02核壳复合粒子.采用SEM、TEM、XRD、VSM、TG-DSC测试手段对材料形貌、微观结构与性能进行表征.实验结果表明羰基铁粉粒子表面均匀地包覆非晶态SiO2纳米壳层.包覆后的核壳复合粒子仍具有很好的超顺磁性能,适当控制壳层的厚度可以提高超顺磁性能.同时抗氧化性能也明显提高.     

镍体系(NiCl2/PPh3)催化的表面引发反向原子转移自由基聚合制备有机/无机杂化材料

考察了以过氧基团改性的纳米SiO2为引发剂,NiCl2/PPh3为催化体系的甲基丙烯酸甲酯(MMA)的反向原子转移自由基聚合(ATRP).通过纳米SiO2与氯化亚砜反应,得到了表面由氯-硅基团改性的纳米SiO2,然后再将其与叔丁基过氧化氢(TBHP)反应,在纳米二氧化硅表面成功引入过氧基团,得到了过氧基团改性的纳米SiO2粒子.结果表明,通过调控Ni2 和Ni 之间的变价关系,使得整个聚合反应具有活性自由基聚合的特征.通过酯交换反应,即将聚甲基丙烯酸甲酯接枝的纳米SiO2杂化粒子与氢氟酸反应,可将聚合物层从二氧化硅粒子表面成功解离.GPC结果表明,该纳米材料聚合物接枝层的分子量基本可控,分子量与单体转化率呈线性关系,ln([M0]/[M])与反应时间成正比,两者成线性关系.AFM分析表明,聚合后聚合物链均匀接枝到纳米SiO2表面,得到了分散稳定的以二氧化硅粒子为核,聚甲基丙烯酸甲酯为壳的核壳杂化粒子.     

可磁分离光催化剂的制备及其光催化性能研究

通过反胶束法和溶胶-凝胶法制备出了一种类蛋结构的可磁分离光催化剂纳米球ZnO@SiO2@NiFe2O4(ZSN),这种光催化剂显示出了超顺磁性和较好的光催化活性。该光催化剂的X-射线衍射和TEM分析结果表明:NiFe2O4纳米粒子被包裹在二氧化硅内形成磁性硅球SiO2@NiFe2O4(SN)载体,ZnO纳米粒子包覆在SN的表面,形成ZnO光催化壳层。光催化实验表明,在500℃下煅烧3h的ZSN表现出最佳的光催化活性。     

TiO_2-SiO_2复合粒子的制备与表征

采用溶胶-凝胶技术通过水解法在SiO2表面包覆纳米TiO2,制备出TiO2-SiO2复合粒子。借助于傅立叶红外光谱、扫描电镜、透射电镜对其进行了表征,结果表明TiO2成功地包覆在SiO2的表面。通过采用X射线衍射定量分析方法来测量复合粒子中锐钛矿型二氧化钛的质量分数,得出当pH=2、SiO2与TiO2摩尔比10∶90、煅烧温度750℃为最佳制备条件;通过复合粒子和二氧化钛粒子分别对甲基橙溶液进行光催化降解的比较表明,复合粒子光催化效果比较好。     

TiO2-SiO2复合粒子的制备与表征

采用溶胶-凝胶技术通过水解法在SiO2表面包覆纳米TiO2,制备出TiO2-SiO2复合粒子.借助于傅立叶红外光谱、扫描电镜、透射电镜对其进行了表征,结果表明TiO2成功地包覆在SiO2的表面.通过采用X射线衍射定量分析方法来测量复合粒子中锐钛矿型二氧化钛的质量分数,得出当pH=2、SiO2与TiO2摩尔比10∶90、煅烧温度750 ℃为最佳制备条件;通过复合粒子和二氧化钛粒子分别对甲基橙溶液进行光催化降解的比较表明,复合粒子光催化效果比较好.     

丁二酸改性磁性复合吸附剂的制备及表征

采用高温溶剂热法制备了Fe_3O_4纳米粒子,通过碱性条件下正硅酸乙酯(TEOS)的水解和缩聚反应实现外层SiO2的包覆,利用丁二酸酐改性核壳结构的Fe_3O_4@SiO_2,制备了一种表面具有羧基的磁性复合吸附剂Fe_3O_4@SiO_2-NH-COOH.通过傅里叶红外光谱(FT-IR)、X-射线衍射仪(XRD)、热重分析(TGA)和X射线光电子能谱仪(XPS)对吸附剂的组成和结构特性进行了研究,结果表明:氨基和羧基成功修饰在Fe_3O_4@SiO_2表面,未改变晶型结构,且材料具有良好的磁特性和磁分离性能.     

盐酸沉淀法制备纳米SiO_2/粉煤灰微珠复合颗粒

以工业级粉煤灰微珠和模数为3.3的水玻璃溶液为原料,采用盐酸沉淀法,利用非均相形核沉积原理,在微米级粉煤灰颗粒表面包覆一层纳米SiO2颗粒.通过扫描电子显微镜、X射线衍射仪、傅里叶转换红外线光谱仪等对包覆产物进行表征,制备得到了具有"核-壳"结构的微珠/SiO2复合结构颗粒,同时SiO2包覆层是以Si-O-Si键的形式结合于微珠表面并不断生长.对这种二级结构复合颗粒进行有机疏水改性,通过"涂敷法"构建超疏水性表面,表面平均接触角为152.4°,达到超疏水性能要求.     

化学镀法合成Fe/Ni纳米复合粉体

目的为实现由直流电弧法所获得的Fe纳米粉体表面活性,合成非晶Ni-P包覆Fe纳米胶囊.方法利用化学镀法对由直流电弧法所获得的Fe纳米粉体表面改性,合成Ni及Ni-P包覆Fe纳米胶囊.结果高分辨电镜（HRTEM）和能量散射谱（EDS）以及XPS光电子能谱研究表明该复合粉体颗粒具有壳核结构,颗粒的尺寸为20~200 nm,核为Fe纳米颗粒,壳为Ni-P合金,其厚度为3~10 nm.同时磁性研究表明该Fe/Ni复合粉体的饱和磁化强度和初始材料Fe粉的饱和磁化强度没有明显差别,分别为141.39 Am2/kg、143.28 Am2/kg;而矫顽力略有增加.结论由于非晶合金壳层的存在,减弱核纳米粒子Fe的氧化程度,提高了Fe纳米粒子的稳定性,利用化学镀法可以实现粉体的表面改性,实现双金属粉体合成.     

Effect of Ni-doping on electrochemical capacitance of MnO2 electrode materials

Mn/Ni composite oxides as active electrode materials for supercapacitors were prepared by solid-state reaction through the reduction of KMnO4 with manganese acetate and nickel acetate at low temperature. The products were characterized by X-ray diffractometry(XRD) and transmission electron microscopy(TEM). The electrochemical characterizations were performed by cyclic voltammetry (CV) and constant current charge-discharge in a three-electrode system. The effects of different potential windows, scan rates, and cycle numbers on the capacitance behavior of Mn0.8Ni0.2Ox composite oxide were also investigated. The results show that the composite oxides are of nano-size and amorphous structure. With increasing the molar ratio of Ni, the specific capacitance goes through a maximum at molar fraction of Ni of 20%. The specific capacitance of Mn0.8Ni0.2Ox composite oxide is 194.5 F/g at constant current discharge of 5 mA.     

Microstructure and corrosive property of Ni-P/nano-CeO<Subscript>2</Subscript> coating electrolessly prepared in acidic condition

Electroless Ni-P/nano-CeO₂ composite coating was prepared in acidic condition, and its microstructure and corrosive property were compared with its CeO₂-free counterpart. Scanning electronic microscopy (SEM), transmission electronic microscopy (TEM) and differential scanning calorimeter (DSC) were used to examine surface morphology and microstructure of the coating. Aqueous corrosion was done in 3%NaCl+5%H₂SO₄ solution and high temperature oxidation was done at 750 °C in air. The results showed that Ni-P coating had partial amorphous structure mixed with nano-crystals, while the Ni-P/CeO₂ coating had perfect amorphous structure. At high temperature, Ni3P precipitation and Ni crystallization took place in both coatings at different temperatures. Aqueous corrosion property and high temperature oxidation property of the composite coating were remarkably improved due to the coating’s microstructure change and the rare earth doping effect. During the co-deposition process, some Ce ⁿ⁺(n=3, 4) ions may be adsorbed to metal/solution interface and hinder nickel deposition. Ni-P/CeO₂ coating’s perfect amorphous structure results from the hindered crystal- typed deposition of nickel and the promoted deposition of phosphorous.     

无机/有机掺杂CdTe/PMMA的合成

采用乳液聚合的方法合成了CdTe/SiO_2/PMMA复合粒子.为了改善微乳体系中CdTe量子点与MMA的相容性,发生聚合物反应前在水/油微乳液体系中采用TEOS的水解合成了二氧化硅修饰的CdTe/SiO_2纳米粒子.扫描电镜显示CdTe/SiO_2/PMMA复合粒子的直径比CdTe/SiO_2纳米粒子的直径略大,为1μm左右.并采用扫描电镜(SEM)、傅氏转换红外线光谱分析仪(FT-IR)、热重分析仪(TGA)和荧光光谱仪对产物进行了表征.结果表明CdTe表面的SiO_2粒子在复合材料中起着物理交联点和化学交联点作用,所合成材料不易产生相分离现象.     

Structural characteristics of spherical Ni(OH)_2 and its charge/discharge process mechanism

1　INTRODUCTIONSince Ni MH batteries came to the market in1990, the improvement of the performances oncathode active materials of nickel hydroxides havebeen mainly based on empirical optimization[1 6].Nowadays, more sophisticated methods are appliedto correlate the chemical composition processes microstructure electrochemical performance of thematerials. In the last two decades, a lot of investi gations have been done concerning electrochemicalmechanisms for Ni MH bat…     

磷掺杂碳纳米管负载镍催化剂的小分子电氧化性能研究

镍基催化剂作为碱性溶液中高催化活性和稳定的非贵金属催化剂,广泛用于小分子电催化氧化领域研究。以磷掺杂碳纳米管为载体,将负载镍/氧化镍核壳的纳米粒子用于甲醇小分子的电氧化,获得了良好的稳定性及催化活性。在仅有3%的低负载量时,在氧化峰电位,其质量活性为6 800 mA/mg,未掺杂碳纳米管载体上负载的纳米粒子活性仅为2 070 mA/mg。而且,与CNTs相比,PCNTs为载体时甲醇电氧化的起始电位及氧化电位均有一定程度的负移。该高催化性能归因于镍/氧化镍核壳纳米粒子的小粒径,以及磷掺杂碳纳米管载体与金属之间的相互作用。     

Preparation and Characterization of Monodisperse Nickel Nanoparticles by Polyol Process

Polymer-protected monodisperse nickel nanoparticles were synthesized by a modified polyol reduction method in the presence of poly（N-vinyl-2-Pyrrolidone）.These nanoparticles were characterized by transmission electron microscopy（TEM）,X-ray diffraction（XRD）,selected area electron diffraction（SAED）,as well as vibrating sample magnetometer（VSM）.The experimental results show that the addition of PVP and the concentration of NaOh have strong influences on the size.agglomeration and uniformity of nanoparticles.In the presence of PVP and NaoH with low concentration.smonodisperse nickel nanoparticles with average diameters about 42 nm were obtained and characterized to the pure nickel crystalline with foc structure.Secondary structures such as clusters.loops.and strings resulted from magnetic interactions between particles were observed.The chemical interaction between the PVP and nickel nanoparticles was found by FTIR.The saturation magnetization（Ms）.remanent magnetization（Mr）and coercivity（Hc）of these nickel nanoparticles are lower than those of bulk nickel.     

Preparation and upconversion luminescence properties of LaF3∶[KG-*2]Yb3+,Er3+／SiO2 nanocomposites with core／shell structure

LaF3:Yb3 +,Er3 + nanoparticles were successfully synthesized using solvothermal treatment,and LaF3:Yb3 +,Er3 +/SiO2 core/shell nanoparticles were also prepared with reverse microemulsion technique.The...     

Effect of Overcharge on Electrochemical Performance of Sealed-Type Nickel/Metal Hydride Batteries

The effects of overcharge on electrochemical performance of AA size sealed-type nickel/metal hydride（Ni/MH） batteries and its degradation mechanism were investigated. The results indicated that the relationship between the effects of different overcharge currents on the increasing velocity of inner pressure and the degradation velocity of cycle life and discharge voltage remains in almost direct proportion. After overcharge cycles, the positive electrode materials remain the original structure, but there occur some breaks because of the irreversible expand of crystal lattice. And the negative electrode alloy particles have inconspicuous pulverization, but are covered with lots of corrosive products and its main component is rare earth hydroxide or oxide. These are all the main reasons leading to the degradation behavior of the discharge capacity and cycle life of Ni/MH batteries.     

急冷法制得的Ni-P非晶态合金的腐蚀试验

用急冷法制得 Ｎｉ１９ Ｐ 合金薄带,由 Ｘ射线衍射测试证实制得的是非晶态结构,由失重法及电化学测试评价其耐蚀性,并且与３１６ 不锈钢,纯 Ｎｉ 作对比。结果表明,制得的 Ｎｉ１９ Ｐ 非晶态合金在１ ｍ ｏｌ／ Ｌ Ｈ Ｃｌ 中的耐蚀性比３１６ 不锈钢及纯 Ｎｉ 要好,并且热处理温度对此非晶态合金的耐蚀性也有影响,略低的加热温度及淬火温度有利于较好的耐蚀性     

碳纳米纤维／镍管复合材料的制备

采用化学镀法在化学纤维布表面覆盖均匀镍层,通过热处理去除基体后获得中空镍纤维管;将其置于化学气相沉积装置中,通过调整合适的氢气和甲烷流量比及气压条件制备了以中空微米镍纤维管为主体结构、碳纳米纤维（CNF）以及金属管体结构为存储介质的碳纳米纤维／镍管复合纤维材料．运用扫描电子显微镜（SEM）分析中空镍纤维及复合纤维管表面形貌,x射线衍射（XRD）对复合纤维管晶相组成进行表征．结果表明,利用模版法制备出的中空镍纤维管孔径在10μm左右,管壁厚约0．5μm;化学气相沉积制备过程中,当微波功率500W,氢气和甲烷流量比100：6,气压4．0kPa,沉积时间5min时,复合纤维管外壁和端口内壁均匀沉积长径比较大且直径均匀分布的碳纳米纤维,碳纤维直径约50nm;复合纤维成分为碳纳米纤维、镍和三镍化磷合金相,其中碳纳米纤维表现为石墨相．表面覆盖有碳纳米纤维的镍管复合材料,增加了材料自身的吸附存储和导电性能,可应用于多相催化、电容存储和电极材料等领域．