PREPARING NANO-CRYSTALLINE La DOPED WC/Co POWDER BY HIGH ENERGY BALL MILLING

The La doped WC/Co powder was prepared by high energy ball milling. The changes of crystal structure, micrograph and defect of the powder were investigated by means of XRD (X-ray diffraction), SEM (scanning electron microscope) and DTA (differential thermal analysis). The results show that adding trace La element into carbides is effective to minish the grain size of WC/Co powder. The La doped carbides powder with grain size of 30nm can be obtained after 10h ball milling. The XRD peak of Co phase disappeared after 20h ball milling, which indicated solid solution (or secondary solid solution) of Co phase in WC phase. The La doped powder with grain size of 10nm is obtained after 30h ball milling. A peak of heat release at the temperature of 470℃ was emerged in DTA curve within the range of heating temperature, which showed that the crystal structure relaxation of the powder appeared in the process of high energy ball milling. After consolidated the La doped WC/Co alloy by high energy ball milling exhibits ultra-fine grain sizes and better mechanical properties.

Synthesis and Characterization of Storage Energy Materials Prepared from Nano-crystalline Cellulose/Polyethylene Glycol

This paper gives a brief report of the synthesis of a new kind of solid-solid phase change materials （SSPCMs）, nano-crystalline cellulose/polyethylene glycol （NCC/PEG）. These PCMs have very high ability for energy storage, and their enthalpies reach 103.8 J/g. They are composed of two parts, PEG as functional branches for energy storage, and NCC as skeleton. The flexible polymer PEG was grafted onto the surface of rigid powder of NCC by covalent bonds. The results of DSC, FT-IR were briefly introduced, and some comments were also given.

Effect of Gas Sources on the Deposition of Nano-Crystalline Diamond Films Prepared by Microwave Plasma Enhanced Chemical Vapor Deposition

Nano-crystalline diamond （NCD） films were deposited on silicon substrates by a microwave plasma enhanced chemical vapor deposition （MPCVD） reactor in C2H5OH/H2 and CH4/H2/O2 systems, respectively, with a constant ratio of carbon/hydrogen/oxygen. By means of atomic force microscopy （AFM） and X-ray diffraction （XRD）, it was shown that the NCD films deposited in the C2H5OH/H2 system possesses more uniform surface than that deposited in the CH4/H2/O2 system. Results from micro-Raman spectroscopy revealed that the quality of the NCD films was different even though the plasmas in the two systems contain exactly the same proportion of elements. In order to explain this phenomenon, the bond energy of forming OH groups, energy distraction in plasma and the deposition process of NCD films were studied. The experimental results and discussion indicate that for a same ratio of carbon/hydrogen/oxygen, the C2H5OH/H2 plasma was beneficial to deposit high quality NCD films with smaller average grain size and lower surface roughness.

Fabrication of nano-crystalline W-Ni-Fe alloy with Mo and rare earth element additives

Three kinds of nano-crystalline high density alloys(86W-7Ni-3Fe-4Mo, 90W-4Ni-2Fe-4Mo and 90W4Ni-2Fe-3.8Mo-0.2RE) were fabricated by a technique combining lower temperature vacuum sintering with highenergy ball milling mechanical alloying. The crystalline size and microstructures of the specimens sintered at different sintering temperatures were examined by X-ray diffraction(XRD) and scanning electron microscope(SEM). The results show that the optimal sintering temperature of 86W-7Ni-3Fe-4Mo, 90W-4Ni-2Fe-4Mo and 90W-4Ni-2Fe3.8Mo-0.2RE alloys are 1 300 - 1 350 ℃. When they are sintered at 1 300 ℃ for 75 min, the hardness of three kinds of specimens can reach above HRC30, the relative density can reach above 96%,and 90W-4Ni-2Fe-3.8Mo-0.2RE alloy possesses the best integrated properties, its hardness is HRC35 and its relative density is 98%.

Reinforcement of Lignin-Based Phenol-Formaldehyde Adhesive with Nano-Crystalline Cellulose (NCC): Curing Behavior and Bonding Property of Plywood

The curing behavior of lignin-based phenol-formaldehyde (LPF) resin with different contents of nano-crystalline cellulose (NCC) was studied by differential scanning calorimetry (DSC) at different heating rates (5, 10 and 20&degC/min) and the bonding property was evaluated by the wet shear strength and wood failure of two-ply plywood panels after soaking in water (48 hours at room temperature and followed by 1-hour boiling). The test results indicated that the NCC content had little influence on the peak temperature, activation energy and the total heat of reaction of LPF resin at 5 and 10&degC/min. But at 20&degC/min, LPF0.00% (LPF resin without NCC) showed the highest total heat of reaction, while LPF0.25% (LPF resin containing 0.25% NCC content) and LPF0.50% (LPF resin containing 0.50% NCC content) gave the lowest value. The wet shear strength was affected by the NCC content to a certain extent. With regard to the results of one-way analysis of variance, the bonding quality could be improved by NCC and the optimum NCC content ranged from 0.25% to 0.50%. The wood failure was also affected by the NCC content, but the trend with respect to NCC content was not clear.

Preparation of Nano-crystalline Tungsten Carbide Thin Film by Magnetron Sputtering and Their Electrocatalytic Property for PNP Reduction

Nano-crystalline tungsten carbide thin films were deposited on Ni substrates by magnetron sputtering using WC as target material. The crystal structure and morphology of the thin films were characterized by X-ray diffraction （XRD） and scanning electron microscopy （SEM） Electrochemical investigations showed that the electrode of the thin film exhibited higher electrocatalytic activity in the reaction of p-nitrophenol （PNP） reduction. FT-IR analysis indicated that p-aminophenol （PAP） was synthesized after two step reduction of PNP on nano-crystalline tungsten carbide thin film electrode.

Size Effects of Nano-crystalline Cellulose

Natural cellulose with the crystal form of cellulose Ⅰ, when treated with condensed lye (e.g. 18%NaOH), can change into new crystal form of cellulose Ⅱ. But the nano-crystalline cellulose (NCC) can do it when only treated with dilute lye (e.g. 1%NaOH) at room temperature and even can dissolve into slightly concentrated lye (e.g. 4%NaOH).

Dynamic modeling of preloaded size-dependent nano-crystalline nano-structures

The vibration behavior of size-dependent nano-crystalline nano-beams is investigated based on nonlocal, couple stress and surface elasticity theories. A nano- crystalline nano-beam is composed of three phases which are nano-grains, nano-voids, and interface. Nano-voids or porosities inside the material have a stiffness-softening impact on the nano-beam. A Eringen＇s nonlocal elasticity theory is applied in the analysis of nano-crystalline nano-beams for the first time. Residual surface stresses which are usually neglected in modeling nano-crystalline nano-beams are incorporated into nonlocal elasticity to better understand the physics of the problem. Also, a modified couple stress theory is used to capture rigid rotations of grains. Applying a differential transform method （DTM） satisfying various boundary conditions, the governing equations obtained from the Hamilton＇s principle are solved. Reliability of the proposed approach is verified by comparing the obtained results with those provided in the literature. The effects of the nonlocal parameter, surface effect, couple stress, grain size, porosities, and interface thickness on the vibration characteristics of nano-crystalline nano-beams are explored.

PREPARATION OF NANO-CRYSTALLINE Fe-Cu THIN FILMS AND THEIR MAGNETIC PROPERTIES

Fe-Cu thin films of 0.2 mum in thickness with different Cu contents wereprepared by using r.f. magnetron sputtering onto glass substrate. The effect of sputteringparameters, including Ar gas pressure and input rf power, on the structure and magnetic propertieswas investigated. It was found that when the power is lower than 70W, the structure of the filmsremained single bcc-Fe phase with Cu solubility of up to 50at. percent. TEM observations for thebcc-Fe phase showed that the grain size was in the nanometer range of less than 20nm. The coercivityof Fe- Cu films was largely affected by not only Ar gas pressure but also rf power, and reachedabout 2.5Oe in the pressure of 0.67-6.67Pa and in the power of less than 100W. In addition,saturation magnetization, with Cu content less than 60at. percent, was about proportional to thecontent of bcc-Fe. When Cu content was at 60at. percent, however, saturation magnetization was muchsmaller than its calculation value.

Ellipsometric analysis and optical absorption characterization of nano-crystalline diamond film

A nano-crystalline diamond (NCD) film with a smooth surface was successfully deposited on silicon by a hot filament chemical vapor deposition (HFCVD) method. Scanning electron microscopy (SEM), atomic force microscopy (AFM), RAMAN scattering spectra, as well as spectroscopic ellipsometry were employed to characterize the as-grown film. By fitting the spectroscopic ellipsometric data in the energy range of 0.75?1.50 eV with a three-layer model, Si|diamond+non-diamond|diamond+ non-diamond+void|air, the optical constants are obtained. The refractive index of the NCD film varies little from 2.361 to 2.366 and the extinction coefficient is of the order of 10?2. According to the optical transmittance and absorption coefficient in the wavelength range from 200 to 1 100 nm, the optical gap of the film is estimated to be 4.3 eV by a direct optical transition mechanics.

Fabrication of nano-crystalline W-Ni-Fe pre-alloyed powders by mechanical alloying technique

Nano-crystalline pre-alloyed powders of W-Ni-Fe were fabricated by high energy ball milling mechanical alloying (MA) technique. The change of appearances and the crystallite sizes of powders before and after high energy ball milling were investigated by XRD, TOPAS P software, SEM and EDS. The results show that the nano-crystalline pre-alloyed powders can be fabricated by 5 h high energy ball milling. During the MA process, the diffusion of W, Ni and Fe happens in the process of repeated welding and fracturing. As a result, nano-crystalline supersaturated solid solutions are formed. The crystallite sizes won't be refined after 10 h ball milling. The crystallite sizes of different compositions are almost the same under the same MA condition. Due to the toughening mechanism of rare earth element, the powders of 90W-4Ni-2Fe-3.8Mo-0.2RE alloy are seriously agglomerated after ball milling compared with the other alloys. It can be concluded that the optimal sintering temperature of 90W-4Ni-2Fe-3.8Mo-0.2RE pre-alloyed powders after 15 h mechanical alloying is 1 300-1 350 ℃.

Preparation of Nano-Crystalline Diamond Films on Poly-Crystalline Diamond Thick Films by Microwave Plasma Enhanced Chemical Vapor Deposition

Nano-crystalline diamond （NCD） films were prepared on poly-crystalline diamond （PCD） thick flims by the microwave plasma enhanced chemical vapor deposition （MPCVD） method. Free standing PCD thick film （50 mm in diameter） with a thickness of 413 μm was deposited in CHn/H2 plasma. It was then abraded for 2 hours and finally cut into pieces in a size of 10×10 mm^2 by pulse laser. NCD fihns were deposited on the thick film substrates by introducing a micro-crystalline diamond （MCD） interlayer. Results showed that a higher carbon concentration （5%） and a lower substrate temperature （650℃） were feasible to obtain a highly smooth interlayer, and the appropriate addition of oxygen （2%） into the gas mixture was conducive to obtaining a smooth nano-crystalline diamond film with a tiny grain size.

Surface Effect of Silica Nano-Particles with Different Size on Thermotropic Liquid Crystalline Polyester Composites

Interface properties of nano-silica/thermotropic liquid crystalline polyesters (TLCP) composites were investigated by X-ray diffraction analysis and differential scanning calorimetory. The crystallinity of TLCP in the composites drastically decreased with an increase of nano-silica content, depending on the surface area of the silica particles. Little size effects (40 - 400 nm) in the particles and strong interaction between silica surface and the C=O moieties of TLCP were observed by IR analysis. The glass transition temperature of TLCP (。C higher than that in bulk.

Hexagonal Nano-Crystalline BCN Films Grown on Si (100) Substrate Studied by X-Ray Absorption Spectroscopy

Hexagonal nano-crystalline boron carbonitride (h-BCN) films grown on Si (100) substrate have been precisely investigated. The films were synthesized by radio frequency plasma enhanced chemical vapor deposition using tris-dimethylamino borane as a single-source molecular precursor. The deposition was performed by setting RF power at 400 - 800 W. The reaction pressure was at 2.6 Pa and the substrate temperature was recorded at 700°C - 800°C. Formation of the nano-crystalline h-BCN compound has been confirmed by X-ray diffraction analysis. The diffraction peaks at 26.3° together with a small unknown peak at 29.2° were elucidated due to the formation of an h-BCN structure. The films composed of B, C, and N atoms with different B-N, B-C, C-N chemical bonds in forming the sp2-BCN atomic configuration studied by X-ray photoelectron spectroscopy. Orientation and local structures of the h-BCN hybrid were studied by near-edge X-ray absorption fine structure (NEXAFS) measurements. The dominant presence of p* and s* resonance peaks of the sp2-hybrid orbitals in the B K-edge NEXAFS spectra revealed the formation of the sp2-BCN configuration around B atoms like-BN3 in h-BN. The orientation was suggested on the basis of the polarization dependence of B K-edge and N K-edge of the NEXAFS spectra.

Growth of Nano Crystalline Diamond on Silicon Substrate Using Different Etching Gases by HFCVD

We investigate the effects of etching gases on the synthesis of nano crystalline diamonds grown on silicon substrate at the substrate temperature of 550℃ and the reaction pressure of 4 kPa by hot filament chemical vapor deposition method, in which CH4 and H2 act as a source and diluting gases, respectively. N2, H2, and NH3 were used as the etching gases, respectively. Results show that the optimum conditions can be obtained only for the case of H2 gas. The crystal morphology and crystallinity of the samples have been examined by scanning electron microscopy and X-ray diffraction, respectively.

Microstructures and mechanical properties of nanocrystalline NiTi intermetallics formed by mechanosynthesis

The formulation of nanocrystallinc NiTi shape memory alloys has potential effects in mechanical stimulation and medical im- plantology. The present work elucidates the effect of milling time on the product＇s structural characteristics, chemical composition, and mi- crohardness for NiTi synthesized by mechanical alloying for different milling durations. Increasing the milling duration led to the formation of a nanocrystalline NiTi intermetallic at a higher level. The formation of nanocrystalline materials was directed through cold fusion, fractur- ing, and the development of a steady state, which were influenced by the accumulation of strain energy. In the morphological study, uninter- rupted cold diffusion and fracturing were visualized using transmission electron microscopy. Particle size analysis revealed that the mean particle size was reduced to -93 μm after 20 h of milling. The mechanical strength was enhanced by the formation of a nanocrystalline in- termetallic phase at longer milling time, which was confirmed by the results of Vickers hardness analyses.

Sin-QuEChERS Nano净化柱结合气相色谱-串联质谱法快速筛查石斛中84种农药残留

利用Sin-QuEChERS Nano净化柱结合气相色谱-串联质谱(GC-MS/MS)分析,建立了石斛基质中84种不同极性农药残留的快速筛查方法。比较了采用不同的提取溶剂(1%乙酸乙腈、丙酮)和不同的提取方式(加水浸泡和不加水浸泡)下目标物的提取效率。利用金钗石斛样品系统比较了Sin-QuEChERS Nano法与经典的基质固相分散法(dSPE)、固相萃取法(SPE)、QuEChERS法的净化效果及提取回收率,以及净化效果较好的Sin-QuEChERS Nano法与dSPE法基质效应的差异。目标物经DB-1701MS石英毛细管色谱柱(30 m×0.25 mm×0.25μm)程序升温分离,GC-MS/MS多反应监测(MRM)模式检测,基质匹配溶液外标法定量。通过GC-MS/MS检测方法对金钗石斛和铁皮石斛中的84种代表性农药进行了方法学验证。结果表明:各目标物在不同范围内呈良好的线性相关,相关系数(r^(2))均>0.990,方法的检出限(LOD,S/N=3)为1.5~5.8μg/kg,方法的定量限(LOQ,S/N=10)为5.0~15.0μg/kg。在两个水平下,目标农药的加标回收率为68.7%~116.2%,相对标准偏差(RSD,n=6)均低于15%。与其他经典的前处理方法相比,Sin-QuEChERS Nano法在净化效果方面表现更好,该法不仅可以有效去除色素、有机酸、碱性干扰物等物质,还可以节省样品制备时间,避免溶剂转移造成的损失,无需进一步涡旋或离心,是一种简单而有效的提取物纯化程序。该方法灵敏、快速、简便、可靠,有效地提高了石斛中农药快速筛查时的检测效率,具有较强的实际应用价值。此外,所开发的方法可以进一步扩展目标农药的类型,并可以用于检测其他更多食品及中药材中的农药残留。

Simple-QuEChERS Nano结合GC-MS/MS同时检测全血中的97种农药

建立了Simple-QuEChERS Nano结合气相色谱-串联质谱(GC-MS/MS)同时检测血液中97种农药的方法,并对基质条件、提取溶剂以及净化材料进行了优化。0.5 mL血液样品经3倍水稀释混匀,使用2.0 mL乙酸乙酯提取后振荡、离心,过Simple-QuEChERS Nano净化柱及0.22μm有机微孔滤膜后,采用多反应监测模式(MRM)进行分析。结果显示,97种农药在一定质量浓度范围内线性关系良好(r2≥0.9873),除丙烯菊酯(检出限和定量下限分别为11.03、36.76 ng/mL)外,其余农药的检出限为0.06~4.27 ng/mL,定量下限为0.18~14.24 ng/mL。采用空白全血进行加标回收实验,97种农药在100、200、400 ng/mL 3个加标水平下的回收率为32.2%~120%,日内精密度为1.9%~11%,日间精密度为3.6%~13%。该方法由传统QuEChERS方法改进,绿色环保、操作简单、快速高效,可用于血液中多种农药的同时检测,用于实际案件血液样品中农药的筛查与定性定量检验,获得了良好的结果。

NANO碳净化-超高效液相色谱-串联质谱法测定东北黑土壤中多农残含量

本文使用NANO碳净化柱对土壤中的31种农药进行净化,并且通过超高效液相色谱-串联质谱法(UPLC-MS/MS)进行测定。土壤样品经过NANO碳净化柱,净化效果良好。31种农药的检出限为0.001~0.01mg/kg,定量限为0.003~0.033mg/kg,添加回收率在70%~120%之间,相对标准偏差(RSD)在0%~10%之间。结果表明,该方法简单、快捷、灵敏度高,线性范围、回收率和精密度均适合土壤中的31种农药残留检测,在土壤农药残留筛查中具有较好的应用前景。