Nanocrystalline CaO as adsorbent to remove COD from paper mill effluent

Porous nanocrystalline CaO has been prepared by the solution combustion process using calcium nitrate as oxidizer and glycine as a fuel. As prepared calcium oxide has been characterized using powder X-Ray Diffraction (XRD), BET surface area, and Scanning Electron Microscopy (SEM). The powder XRD pattern confirms the crystallinity and phase purity of the powder. The particle size of the powder obtained from Scherrer's formula lies in the range of 37-53 nm. The particles are loosely agglomerated and spherical in shape as observed by SEM. The specific surface area of the powder is 18.5 m2/g and the average pore diameter obtained from N2-desorption isotherm is approximately 5.2 nm. Batch shaking process was performed using CaO as adsorbent with effluent collected from pulp and paper mill to remove chemical oxygen demand (COD). The COD removal capacity of the CaO is approximately 93%.     

纳米WC粉末的制备研究

本文主要讲述了用低温碳化的方法制备平均晶粒度为20～30nm,颗粒尺寸小于100 nm的纳米碳化钨粉末.并利用成分分析和DSC,SEM,XRD以及BET检测手段,对纳米级WC粉末进行了分析研究.通过对有机炭、活性炭和工业炭的对比研究发现,有机炭为较理想炭源,能在较低的温度下碳化,制备出合格的纳米碳化钨粉末.同时发现碳化的颗粒度与炭源有着紧密的关系,在钨粉原料相同的情况下,炭源的颗粒度越细,其制备出的碳化钨的颗粒也越细.而且在试验中研究发现,炭源对于碳化温度有明显的影响,在本试验所采取的三种不同炭源中,通过DSC和XRD的研究分析表明,碳化温度由低到高依次为有机炭＜活性炭＜工业炭.     

Large scale synthesis and characterization of Ni nanoparticles by solution reduction method

Ni nanoparticles were mass synthesized by solution reduction process successfully. The influence of the parameters on the particle size of Ni nanoparticles were studied and the referential process parameters were obtained. The morphology and structure of the synthesized Ni nanoparticles were characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), Brunauer-Emmett-Teller (BET) surface area analysis and infrared spectroscopy (IR). The results show that Ni nanoparticles are of high purity and are covered by hydroxyethyl carboxymethyl cellulose (HECMC) layer and the mean size being about 31 nm. The magnetic measurement revealed that Ni nanoparticles are ferromagnetic.     

Optimisation of high energy ball milling parameters to synthesize oxide dispersion strengthened Alloy 617 powder and its characterization

In the present work, ultra-fine powder of oxide dispersion strengthened Alloy 617 was synthesized by high energy ball milling. Milling parameters such as rpm and milling time were varied in the range of 500–2000 and 5–360 min, respectively. Energy applied to the powder in the milling process (Energy per unit mass per hit, E_c) was estimated using the collision model. Effect of milling parameters on the microstructure of powder and refinement of oxides was investigated using X-ray Diffraction (XRD), Scanning electron Microscopy (SEM), conventional Transmission Electron Microscopy (TEM) and High resolution Transmission Electron Microscopy (HRTEM). Desired convoluted lamellar structure with average particle size ∼33 μm was observed during milling at 1000 rpm (E_c ∼ 0.4 kJ/g.hit) for 6 h. TEM analysis of the powder showed the presence of fine oxide dispersoids in the size range 4–16 nm. HRTEM analysis substantiated the presence of fine dispersoids of size ∼4 nm and showed the presence of deformation twins in the matrix. The fine dispersoids in a nanocrystalline matrix is expected to provide superior creep strength to the material at high temperatures.     

Nanostructure in a Ti alloy processed using a cryomilling technique

A nanocrystalline Ti alloy with a uniform distribution of grains was synthesized using cryogenic mechanical milling. The effects of cryomilling parameters, such as milling time and ball to powder ratio (BPR), on the particle size, grain size, chemistry, and structure of cryomilled Ti powders were investigated using X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). The experimental results show that nanocrystalline Ti powders with a grain size of about 20 nm can be prepared using the cryomilling technique. Compared to SPEX milling at room temperature, cryomilling led to lower contamination levels of oxygen, nitrogen, and iron in the cryomilled Ti powder. The average particle size initially increased from the original 55 μm to a maximum value of 125 μm after 2 h of milling, and then decreased to 44 μm after 8 h of milling. Both the average particle size and the grain size decreased as the BPR increased.     

等离子熔覆铁基非晶纳米晶复合涂层及其性能

利用等离子熔覆技术在A3钢表面制备了一层与基体呈冶金结合的、性能良好的非晶纳米晶复合涂层.涂层有非晶相和纳米相组成,根据衍射峰的半高宽,计算出铁基涂层中平均晶粒尺寸为22～24nm.对涂层进行XRD、SEM、EDS、TEM和DSC分析,并利用显微硬度计和电化学工作站研究涂层的硬度和耐蚀性能,研究表明所制备的铁基涂层具有良好的性能.     

爆轰裂解可膨胀石墨制备石墨微粉

在不改变石墨原始结构与成分的基础上,利用冲击波对可膨胀石墨进行爆轰,收集爆轰灰,进行X射线衍射、SEM的测量分析以及BET法测定比表面积。结果表明,可膨胀石墨经过爆轰后,得到了颗粒大小为1μm～10μm的石墨粉,比表面积由8.096m^2/g增大至47.48m^2/g,并且孔隙变得更为均匀,常规研磨设备是无法达到这种效果的。为石墨的细化提供了一种更为简便快捷而又节省能源的方法。     

不同乳化剂作用下三聚氰胺-甲醛@正十八烷微胶囊相变复合材料微观形貌和热性能

采用原位聚合法,通过改变非离子/阴离子乳化剂组合制备了一系列以正十八烷(OD)为芯材、三聚氰胺(M)-甲醛树脂(F)为壁材的微胶囊相变储能材料,并借助FTIR、SEM、DSC和激光粒度分析仪等手段系统研究了乳化剂复配对M-F@OD微胶囊相变材料微观形貌和相变潜热的影响。结果表明,不同乳化剂组合及掺量对M-F@OD微胶囊相变材料的形貌和性能产生显著影响,当采用非离子和阴离子复合乳化剂时,M-F@OD微胶囊相变材料团聚现象得到明显改善,粒径分布更加均匀,颗粒尺寸进一步细化,粒径大小范围为0.1~1μm,储热能力明显提高,相变潜热达到70.86J/g。     

利用聚合物的性质制备X型分子筛

以聚合物甲基纤维素作空间位阻剂合成了X型分子筛.对合成的样品进行了XRD、BET与SEM等表征.结果表明,随甲基纤维素加入量的增加,合成样品的BET、孔体积与颗粒尺寸减小,而且BET与孔体积减小幅度增大,外比表面先增大后减小,但加入甲基纤维素量过多会导致合成样品的相对结晶度下降.与常规水热法相比,加入了空间位阻剂甲基纤维素成功地限制了颗粒的生长,合成样品的相对结晶度与外比表面增大,BET、孔体积与颗粒尺寸都减小,而且15g凝胶加2.5g甲基纤维素合成的样品最好,其相对结晶度为110%,外比表面为24.3cm2/g,BET为600.9cm2/g,孔体积为0.255cm3/g,平均颗粒尺寸为1.5μm,是常规水热法合成样品平均粒径的1/4.     

Comparison of sol-gel and co-precipitation methodson the structural properties and phase transformation ofγ andα-Al2O3 nanoparticles

The nanostructured c and a alumina powders were synthesized by sol-gel and co-precipitation methods,and properties of the powders were studied by XRD, SEM,TEM, BET and FTIR. The results showed that both c and a phases were formed in the lower temperature in precipitation method compared to sol-gel. The size of spherical aalumina synthesized by sol-gel was 10–15 nm, whereas the sample prepared by co-precipitation yielded nearly spherical and hexagon a-powder with particle size of 10–50 nm.At 750 ℃ the resulting powder prepared by co-precipitation  exhibited larger surface area (206.2 m2/g) compared to sol-gel (30.72 m2/g), hence it is recommended for catalytic and sensing applications.     

海绵状NiFe2O4团簇的合成与表征

以乙醇-水为混合溶剂,六亚甲基四胺(HMTA)与聚乙烯吡咯烷酮(PVP)为添加剂,通过溶剂热法合成海绵状的镍铁氧体(NiFe2O4)团簇,并对其进行了XRD、VSM、SEM、TEM、BET与ICP表征。结果表明,在反应体系中同时引入PVP与HMTA时,合成的海绵状NiFe2O4团簇具有尖晶石晶体结构,晶粒均匀细小,比饱和磁化强度为57.30emu/g,比表面积与孔容分别为91.57m2/g、0.26cm3/g。     

胶体碳微球的活化及其亚甲基蓝液相吸附性能的研究

以葡萄糖为前驱体,采用液相碳化法,制备颗粒约为100～200nm胶体碳微球.采用KOH作活化剂对胶体碳微球进行活化处理.考察了碱炭比、活化温度和保温时间等工艺因素对孔径和比表面积的影响.通过XRD、SEM等分析手段对胶体碳微球活化前后的表面形貌、孔径分布、显微结构进行分析.经热处理和活化后,胶体碳微球的BET比表面积从26.6m2/g增加到1383.4m2/g.相同实验条件下,在亚甲基蓝液相吸附试验中,经活化处理后的样品所表现出的吸附量是商业活性炭Calgon-F300的两倍.     

羧甲基壳聚糖/Ce^3＋掺杂TiO2复合抗菌材料的研究

采用溶胶-凝胶法制备稀土（Ce^3＋）掺杂纳米TiO2（纳米Ce/TiO2）,借助XRD、BET、SEM对Ce/TiO2进行表征。结果表明纳米Ce/TiO2晶型为锐钛矿,平均晶粒大小为19.95nm,比表面积为43.302m^2/g。采用超声波催化法合成了羧甲基壳聚糖（CMC）,并与Ce/TiO2复配制得羧甲基壳聚糖/Ce3＋掺杂纳米TiO2复合材料（CMC/Ce/TiO2）,借助FT-IR对CMC及CMC/Ce/TiO2复合材料进行了结构表征。初步研究了纳米Ce/TiO2、普通纳米TiO2、CMC/Ce/TiO2、CMC的抗菌性能,结果显示纳米Ce/TiO2对大肠杆菌和金黄色葡萄球菌的抗菌率分别为55%和53%,普通纳米TiO2对两种菌的抗菌率分别为50%和45%,Ce^3＋的掺杂可提高纳米TiO2的抗菌性能;CMC/Ce/TiO2对大肠杆菌和金黄色葡萄球菌的抗菌率分别达到99%和95%,CMC对两种菌的抗菌率分别为90%和80%,Ce/TiO2的复合可显著提高CMC的抗菌性能。     

Optimization of Amorphous Silica Nanoparticles Synthesis from Rice Straw Ash Using Design of Experiments Technique

In this study, a chemical method of dissolution-precipitation was applied to produce amorphous silica nanoparticles from rice straw ash (RSA; the waste material of rice cultivation. The morphology, particle size, structure, and area of specific surface of synthesized amorphous silica nanoparticles were evaluated using transmission electron microscopy (TEM), x-ray diffraction analysis (XRD), and BET method to measure the specific surface area of materials. In addition, chemical composition of RSA used and the synthesized silica nanoparticles was studied by x-ray fluorescence (XRF) spectroscopy. The atomic concentration of synthesized silica was determined by x-ray photoelectron spectroscopy (XPS). The effects of sodium hydroxide concentration, precipitation reaction temperature, and precipitation reaction duration on the area of specific surface were determined through design of experiments (DOE) technique. Results depicted that silica nanoparticles with particle size of 10–15 nm were successfully synthesized. Average area of specific surface and purity were 327 m2/gr and 99.5%, respectively. The interactive influence of temperature and duration had the highest effect on the average area of specific surface.     

纳米FePO4的合成及其正极材料LiFePO4/C的电化学性能研究

以Fe3+为铁源,采用控制结晶技术合成了纳米FePO4.xH2O,将FePO4.xH2O于500℃热处理4 h后得到纳米FePO4前驱体,然后通过碳热还原在不同温度下煅烧合成橄榄石结构的纳米LiFePO4/C样品.采用差热/热重、X射线衍射、扫描电镜、比表面测试、电化学性能测试等分析测试方法对纳米FePO4.xH2O、FePO4前驱体及不同煅烧温度下制得的纳米LiFePO4/C样品进行表征.研究结果表明,700℃烧结10 h合成LiFePO4/C样品的粒径在40~100 nm左右,比表面积为79.8 m2/g;700℃煅烧合成样品在电压2.5~4.2 V,倍率为0.1C、1C、5C、10C、15C时的放电比容量分别达到156.5、134.9、105.8、90.3和80.9 mAh/g,具有较好的倍率性能;样品还表现出较好的容量保持率.     

Exploitation of nano alumina for the chromatographic separation of clinical grade 188Re from 188W: a renaissance of the 188W/188Re generator technology

The (188)W/(188)Re generator using an acidic alumina column for chromatographic separation of (188)Re has remained the most popular procedure world over. The capacity of bulk alumina for taking up tungstate ions is limited (～50 mg W/g) necessitating the use of very high specific activity (188)W (185-370 GBq/g), which can be produced only in very few high flux reactors available in the world. In this context, the use of high-capacity sorbents would not only mitigate the requirement of high specific activity (188)W but also facilitate easy access to (188)Re. A solid state mechanochemical approach to synthesize nanocrystalline γ-Al(2)O(3) possessing very high W-sorption capacity (500 mg W/g) was developed. The structural and other investigations of the material were carried out using X-ray diffraction (XRD), transmission electron microscopy (TEM), Brunauer Emmett Teller (BET) surface area analysis, thermogravimetric-differential thermal analysis (TG-DTA), and dynamic light scattering (DLS) techniques. The synthesized material had an average crystallite size of ～5 nm and surface area of 252 ± 10 m(2)/g. Sorption characteristics such as distribution ratios (K(d)), capacity, breakthrough profile, and elution behavior were investigated to ensure quantitative uptake of (188)W and selective elution of (188)Re. A 11.1 GBq (300 mCi) (188)W/(188)Re generator was developed using nanocrystalline γ-Al(2)O(3), and its performance was evaluated for a period of 6 months. The overall yield of (188)Re was >80%, with >99.999% radionuclidic purity and >99% radiochemical purity. The eluted (188)Re possessed appreciably high radioactive concentration and was compatible for the preparation of (188)Re labeled radiopharmaceuticals.     

An eco friendly and solvent free method for the synthesis of Zinc oxide nano particles using glycerol as organic dispersant

Zinc oxide nano particles can be synthesized using a simple solvent free, economic and eco friendly combustion method. The structural characterization of synthesized nano particles are carried out using XRD and SEM. The optical characterization was carried out using UV and Photoluminescence spectrofluorimeter. The XRD result shows that the nano particles are of hexagonal shape and the average crystal size of the Zinc oxide nano particle is in the range of 70 nm. The SEM analysis shows that the shape of the nano particles is of nano rods. The quality and purity of the Zinc oxide nano particles are confirmed using XRD and EDAX spectral analysis.     

Aging and wear resistant characterization of al-5Mg-X(Si, Cu, Ti)/SiCp composites produced by pressureless infiltration method

The effects of SiC particle size and alloy elements such as Si, Cu and Ti on the response to aging treatment and wear resistance in Al-5Mg-X(Si,Cu,Ti)/SiCp composites fabricated by pressureless infiltration method have been investigated by hardness tester, scanning electron microscope (SEM), X-ray diffractometer (XRD), differential scanning calorimetry (DSC) and wear tester. The Al-5Mg-0.3Si-0.1Cu-0.1Ti/SiC_P composites had better wear resistance property among Al-5Mg-X(Si,Cu)/SiC_P composites. The wear resistance property of all the composites was enhanced after aging at 170°C for 8 hrs due to precipitates of '(Mg₂Si) phase. The wear resistance property of the composite as-fabricated with 50 m size of SiC particle is superior to that of the composite as-fabricated with 100 m SiC size of particle. In Al-5%Mg alloy aged at 170°C for 8 hrs, the frictional seizure appeared more than abrading speed of 1.90 m/s, but in Al-5Mg-(Si,Cu,Ti)/SiC_P composites aged at 170°C for 8 hrs, the frictional seizure was not found at abrading speed ranging from 0.5 m/s to 4.3 m/s.     

A simple route to synthesis and characterization of CoAl2O4 nanocrystalline via combustion method using egg white (ovalbumine) as a new fuel

Single phase of CoAl₂O₄ nanocrystalline spinel has been synthesized first time successively by combustion method using extracted egg white (ovalbumine) as new fuel. The prepared samples were characterized using XRD, TGA, DSC, TEM, BET, IR, UV-Vis and CIE L*a*b* colorimetric method. The average particle sizes were in the range 10.45-26.58 nm and fine agglomerates in a way that specific surface area up to 188.55 m² g⁻¹ could be obtained.     

新型复合钙钛矿Ba(SbⅢ,SbⅤ)O3的水热合成和表征

采用水热晶化法制备了Ｂａ（Ｓｂ^Ⅲ,Ｓｂ^Ⅴ）Ｏ_３新型钙钛矿型氧化物,并通过ＸＲＤ、 ＩＲ、ＳＥＭ和ＩＣＰ等方法对产物物相、形貌和组成等进行了表征．结果表明,产物为立方钙钛矿结构,晶胞参数为α＝０．４１５ｎｍ,粒度为１～２μｍ具有一定团聚的多晶粉末．产物中锑为三价和五价两种价态．水热条件对合成影响的研究结果表明, Ｂａ（Ｓｂ^Ⅲ,ｓｂ^Ⅴ）Ｏ_３合成的适宜碱度和ｎ_{Ｓｂ（Ⅴ)}／ｎ_{Ｓｂ（Ⅲ）}分别为 ８～１０Ｍｏｌ／Ｌ ＫＯＨ和 ０～１