Characterization of Low Pressure DMA System for the size selection of magnetic nano-particles

For the size selection of magnetic nano particles produced in laser ablation, a low pressure differential mobility analyzer (LPDMA) was constructed. The LPDMA was characterized using the transmission electron microscopy (TEM) image of laser-ablated CoPt nano particles. Using TEM image, the geometrical standard deviation, _g, was measured to be around 1.13. The dependence of the performance of LPDMA on the gas path temperature and the pressure was measured using an electrode which measures the number of the selected particles.The size-selected magnetic nano-particles were deposited on Si substrates, whose magnetizations were measured by SQUID. It was found that nano-particles with a diameter of 20 nm have different temperature dependences from nano-particles with a diameter of 40 nm and the coercivity of 40 nm dia. nano-particles is smaller than that of 20 nm dia. nano-particles. PACS 74.25.Ha; 78.67.Bf; 81.09.-b     

Size classification of Si nanoparticles formed by pulsed laser ablation in helium background gas

We have developed an integrated process system for the formation of nanoparticles by pulsed laser ablation (PLA) in helium background gas, size classification using a differential mobility analyzer (DMA), and deposition on a substrate. The DMA has been improved to operate at pressures of less than 10 Torr. The classification resolution of the low-pressure operating DMA (LP-DMA), transporting properties of nanoparticles under low pressure, have been investigated theoretically in order to evaluate the performance of the size classification for the integrated system. By operating the integrated system at less than 10 Torr, we have measured the size distribution of Si nanoparticles in the gas phase formation field by sweeping the applied voltage to the LP-DMA and counting the charged nanoparticle concentration with an electrometer. Moreover, we successfully deposited the classified Si nanoparticles on a substrate by fixing the voltage. We have verified that the integrated system can be applied to the clean physical vapor deposition process for accurately size-controlled nanoparticles.     

Characterization of nanoparticles of organic carbon (NOC) produced in rich premixed flames by differential mobility analysis

Differential mobility analysis (DMA) is used to measure on-line the size distributions of inception particles in atmospheric pressure premixed ethylene air flames ranging from C/O = 0.61 to 0.69, just at the onset of soot formation. DMA is also used, in combination with electrospray, to measure the size distributions of suspended flame products captured in water samples. The DMA systems used for this work employ detectors sensitive to the full range of molecular clusters/nanoparticles in gas-to-particle conversion processes (as small as about 1 nm) and they have much larger sheath gas flow rates than is typically used to reduce losses and peak broadening by diffusion. The measured size distributions show that the first particles observed in flames have a size of 2 nm, consistent with previous in situ measurements by light scattering and extinction (LSE) and the off-line measurements of material captured in water samples from the same flames. For richer flames, the quantity of the 2 nm particles measured increases, and the width of its size distribution shifts asymmetrically toward larger sizes. A numerical coagulation model assuming size-dependent coagulation efficiency predicts well the experimentally measured size distributions in the flames examined. Similarly, the slightly larger size distributions measured by atomic force microscopy of inception particles deposited on surfaces can also be attributed to the size-dependent coagulation/adhesion efficiency. The results imply that the smaller nanoparticles formed in combustion processes have a longer lifetime than those larger than 6-7 nm and may play an important role in the formation of fine organic carbon particulate in the atmosphere.     

氩气中铝丝电爆炸沉积能量对制备铝纳米粉体特性的影响

研制了基于脉冲电容器放电回路的亚微秒金属丝电爆炸纳米粉体制备实验平台,包括电爆炸过程电流和电压测量系统。利用透射电子显微镜(TEM)观察纳米粉体的形态与结构,并通过电镜统计观察法分析TEM图像得到纳米粉体的粒度大小及其分布。在氩气中电爆炸铝丝制备铝纳米粉体,通过改变电容器充电电压,即初始储能,实验研究沉积能量对铝纳米粉体特性的影响规律。结果表明:铝纳米粉体颗粒形态与结构主要由氩气气压的高低决定,与沉积能量基本无关。增大丝爆过程的沉积能量可显著缩小铝纳米粉体粒度分布范围,减小颗粒平均粒径,并有效地抑制纳米粉体中亚微米颗粒的形成。随着沉积能量E与氩气气压p比值(Ep-1)增大,铝纳米粉体颗粒平均粒径、最大粒径和粒径大于100 nm颗粒所占比例均呈指数函数单调减小。     

TEM Imaging of Mass-selected Polymer Molecules

Polyethylene glycol (PEG) molecules with masses below 1300amu are electrosprayed (ES) from solution, mobility-selected at high resolution in a differential mobility analyzer (DMA), collected on a grid and imaged by transmission electron microscopy (ES–DMA–TEM). The DMA resolves individual n-mers, and selects only one out of the many present in the original sample. Ion identity is established from parallel mass spectra (ES-MS). The images reveal spherical particles 1.46nm in diameter, in good agreement with the known ion mass and bulk density. The DMA-selection technique opens new paths for the study of very small particles.     

Well-crystallized zinc oxide quantum dots with narrow size distribution

In this study, pulsed laser ablation, online annealing, and following size classification using a differential mobility analyzer (DMA) were employed to fabricate quantum dots (QDs) of zinc oxide (ZnO). The irregularly shaped ZnO particles were obtained at annealing temperature less than 873 K, which gradually transformed into spherical QDs with increasing the annealing temperature. Finally, ZnO QDs with narrow size distribution having spherical shapes were successfully obtained at temperatures above 1173 K under the DMA classification at a nominal size of 10 nm. TEM observation demonstrated that the ZnO QDs obtained by this process were well-crystallized single crystallites with a wurtzite structure. Further, ZnO QDs with average sizes in the range of 4.8–8.1 nm were successfully fabricated by reducing the specified sizes of DMA. These features of the fabricated ZnO QDs are favorable for investigation of intrinsic quantum size effect in ZnO.     

A new dual-type DMA for measuring nanoparticles emitted from combustion engines

A new dual-type differential mobility analyzer (dual-type DMA) was developed in order to detect transient number concentrations of airborne nanoparticles with diameters centralized at around 10 nm (for nuclei mode particles) and 100 nm (for accumulation mode particles) in automobile exhaust gas. The apparatus divides the gas sample into two parts, and each part is sent through one of two coaxially nested sections for analysis. For the scanning mode measurement, the nanoparticles are charged by ²⁴¹Am and their size distributions are determined by varying the applied voltage over 2 min. The transient mode measurement, on the other hand, fixes the voltages for the two sections at peaks near 10 and 100 nm in order to monitor the transient behavior of the exhaust nanoparticles. The measurement principles and design of the dual-type DMA are detailed and the results for time response experiments are presented using model nanoparticles charged by a corona charger. The transient concentrations of the nuclei mode and the accumulation mode particles from a diesel engine were shown to be detected by this method, when ²⁴¹Am was used for charging the particles.This revised version was published online in August 2005 with a corrected issue number.     

The growth of Y2SiO5:Ce thin films with pulsed laser deposition

Y₂SiO₅:Ce phosphor thin films were grown onto Si(100) substrates with pulsed laser deposition (PLD) using a 248-nm KrF excimer laser. Process parameters were varied during the growth process and the effect on the surface morphology and cathodoluminescence (CL) was analysed. The process parameters that were changed included the following: gas pressure (vacuum (5×10⁻⁶ Torr), 1×1⁻² Torr and 1 Torr O₂), different gas species (O₂, Ar and N₂ at a pressure of 455 mTorr), laser fluence (1.6±0.1 J cm⁻² and 3.0±0.3 J cm⁻²) and substrate temperature (400 and 600°C). The surface morphology was investigated with atomic force microscopy (AFM). The morphology of the thin films ablated in vacuum and 10 mTorr ambient O₂ showed more or less the same trend. An increase in the pressure to 1 Torr O₂, however, showed a definite increase in deposited particle sizes. Ablation in N₂ gas resulted in small particles of 20 nm in diameter and ablation in O₂ gas produced bigger particles of 20, 30 and 40 nm as well as an agglomeration of these particles into bigger size clusters of 80 to 100 nm. Ablation in Ar gas led to particle sizes of 30 nm and the particles were much more spherically defined and evenly distributed on the surface. The higher fluence deposition led to bigger particle and grain sizes as well as thicker layers with respect to the lower fluence. The particle sizes of the higher fluence vary mainly between 130 and 140 nm and the lower fluence sizes vary between 50 and 60 nm. The higher fluence particles consist of smaller particles ranging from 5 to 30 nm as measured with AFM. The surface structure of the thin film ablated at 400°C substrate temperature is less compact (lesser agglomeration of particles than at 600°C). The increase in substrate temperature definitely resulted in a rougher surface layer. CL was measured to investigate the effect of the surface morphology on the luminescent intensities. The increased O₂ ambient (1 Torr) resulted in a higher CL intensity compared to the thin films ablated in vacuum. The thin film ablated in Ar gas showed a much higher CL intensity than the other thin films. Ablation at a high fluence resulted in a higher CL intensity. The higher substrate temperature resulted in better CL intensities. The more spherically shaped particles and rougher surface led to increase CL intensities.     

Coating thickness measurements on gas-borne nanoparticles by combined mobility and aerodynamic spectrometry

An on-line method is described and validated to measure the thickness of coatings on gas-borne nanoparticles. The method is essentially a tandem technique which measures the aerodynamic diameter of a particle twice—before and after coating—by a single-stage low-pressure impactor (SS-LPI) for the same mobility equivalent diameter preselected via differential mobility analyzer (DMA). A shell thickness is then derived from the change in effective particle density determined by the SS-LPI. The method requires a difference in mass density between carrier particle and coating material. Its theoretical sensitivity is shown to range between about 0.1 and 1 nm, depending on the density ratio. One advantage of this approach is that both DMA and SS-LPI are situated in series but downstream of the coating step, so as not to interfere with the coating process. The method was validated against transmission electron microscopy (TEM) measurements, using spherical silica–titania particles coated with conformal shells of molybdenum and bismuth oxide by chemical vapor deposition (CVD). For such spherical particles, the agreement with TEM was excellent. The technique was able to provide layer thicknesses for sub-nanometer layers barely or not resolved by TEM. The paper also discusses the impact of ‘non-ideal’ phenomena such as the formation of doublet particles by coagulation, the effect of multiply charged particles, or the onset of homogeneous decomposition of the coating precursor. With supporting experimental data, it is shown that such phenomena can be interpreted reliably from certain features of the impactor penetration curve. The on-line method can thus be used for fast screening of process parameters and reliable process monitoring for gas-phase synthesis of composite nanopowders.     

A sampler designed for nanoparticles and respirable particles with direct analysis feature

A sampler has been designed to collect particles in the nanometer and respirable sizes directly onto a membrane filter and transmission electron microscopy (TEM) grid. The novel design aspects of this sampler include the selection of the diameter of the inlet probe, geometry of the sampler, and the resulting air flow to the sampler. Together, they control the cutoff diameter, which was determined experimentally to be a mass median aerodynamic diameter (MMAD) of 3.8 μm. The maximum aerodynamic diameter entering the sampler is designed to be approximately 8 μm. Nanometer-sized particles are collected on both the filter and grid through diffusion, as confirmed by testing with aluminum oxide engineered nanoparticles collected on the filter which measured a count median diameter (CMD) of 500 nm and a geometric standard deviation (GSD) of 1.97. The primary particles and small agglomerates collected on the grid have a CMD of 100 nm and GSD of 2.3. This diffusion sampler collected close to, if not 100%, of the particles entering the sampler. The sampler is easily wearable for personal exposure and environmental sampling, operates at 0.3 L/min, and can collect particles in various settings at indoor and outdoor environments. Particles are analyzed directly by transmission electron microscope on the grid and by scanning electron microscope on the filter to assess the exposure through particle counts and elemental composition analysis.     

In situ observation of UF5 nanoparticle growth in a low-pressure mixed-flow reactor

5 nanoparticles equipped with an in situ size-monitoring system, a LPDMA (low-pressure differential mobility analyzer), was developed to experimentally investigate the nanoparticle growth mechanism. The concentration of photoproduced UF₅ molecules was controlled by changing three factors: (I) the concentration of the feed UF₆ gas, (II) the laser pulse energy of the irradiation, and (III) the repetition rate of the laser pulses. The dependence of the volumetric average diameter of the photoproduced particles on the UF₅ nascent concentration in all three cases was found to be very similar. The result strongly suggests that the reactor functions as a mixed-flow reactor under a complete mixing condition. The particle size measured by the LPDMA was found to be in the range of 6 to 11 nm, and it was approximately proportional to the power 0.3 of the initial concentration of photoproduced UF₅ molecules. Received: 11 May 1998/Accepted: 15 September 1998     

Effect of temperature on growth and structure of carbon nanotubes by chemical vapor deposition

The effect of temperature on growth and structure of carbon nanotubes (NTs) using chemical vapor deposition (CVD) has been investigated. Iron embedded silica was used to grow NTs in large quantity at various temperatures from 600 to 1050 °C with gas pressure fixed at 0.6 and 760 Torr, respectively. The growth and structure of the NTs are strongly affected by the temperature. At low gas pressure, the NTs are completely hollow at low temperature and bamboo-like structure at high temperature. While at high gas pressure, all the NTs are bamboo-like structure regardless of temperature. The diameter of NTs increases significantly with temperature. At low gas pressure the diameter gets bigger by mainly increasing the number of graphene layers of the wall of NTs, whereas at high gas pressure the diameter gets bigger by increasing both the number of graphene layers of the wall and the inner diameter of the NTs. This result indicates that the growth temperature is crucial in synthesizing NTs with different structures. The findings here are important for realizing controlled growth of NTs for their applications in different fields. Received: 20 November 2001 / Accepted: 21 November 2001 / Published online: 4 March 2002     

Procedure for Predicting a Minimum Volume or Mass of Sample to Provide a Given Size Parameter Precision

Previous work to predict the minimum count or mass of particles to achieve a given repeatability of a size parameter has focussed on relatively narrow size distributions. Work by Masuda and Gotoh [1], based upon the log‐normal distribution by number, produce a prediction of the number of particles to be counted to achieve a defined accuracy of median volume mean MVD and mass median diameter MMD. The published paper limited the geometric standard deviations (s_g) to a maximum of 1.6. This equates to a size distribution covering just less than 1 decade of size. Modern laser diffraction units have optical arrangements enabling a range of particle sizes between 0.05 microns to 2000 microns to be determined. With the laser diffraction unit in mind the predictions of Masuda and Gotoh were extended to higher values of (s_g) where limitations were seen. An alternative prediction was then explored whose results compare very favourably with practical measurements of a characterised certified reference material CRM.     

铁、钴、镍金属超微粒的制备与磁性

用气体蒸发法制备粒径在100—800?之间的铁、钴、镍金属超微粒。超微粒的生长机制与气压相关,在低气压下(P<3Torr)为成核生长;在高气压下(P>3Torr)为凝聚生长。电子显微镜观察到铁的非晶态超微粒。X射线衍射表明:铁、镍超微粒的晶格结构与相应的块物质相同,但钴超微粒有所不同,粒度为200—300?的钴为fcc结构。室温下,铁、钴、镍超微粒最高矫顽力分别为1000,1500和450Oe,对应的平均粒度为210,200和320?,其数值与理论计算的单畴颗粒尺寸大致相同。其饱和磁化强度随粒度的减小而单 关键词：     

Lasers based on electrodynamically dispersed media

We demonstrate the possibility of creating a suspension of active-media particles in a discharge tube by using an electrodynamic dispersing system. An electric discharge in an electrodynamically dispersed system of 30-μm Cu particles was studied. The velocity of Cu (30 μm), Al (30 μm), and W (6-μm flakes) particles was measured at atmospheric pressure using a laser Doppler velocimeter. The velocities were found to be in the 0.1−5-m/s range. The electric field strength required to levitate Cu, Al, and W particles was studied as a function of buffer gas (air) pressure in the range from 2 × 10⁻² Torr to 1 atm. It is shown that powders can be suspended with the help of electrodynamic dispersing system at air pressure below 0.1 Torr or above 100 Torr.     

气体中蒸发法制备InSb纳米颗粒

用气体中蒸发的方法在蓝宝石基片上制备了纳米InSb颗粒膜．通过透射电镜分析显示，该方法可以制得多晶的InSb纳米颗粒，且颗粒均匀地分布在蓝宝石基片表面上；用X射线能谱仪分析样品得到两种元素的百分比接近1：1．实验结果表明，通过改变设备的工作条件，可以得到具有不同颗粒尺寸的InSb纳米颗粒．     

Numerical Study on Characteristics of Argon Radio-Frequency Glow Discharge with Varying gas Pressure

A one-dimensional fluid simulation on argon rf glow discharge with varying linearly gas pressure from 1 Torr to 100 Tort is performed. The model based on mass conservation equations for electron and ion under diffusion and mobility approximation, and the electron energy conservation equation is solved numerically by finite volume method. The numerical results show that a uniform plasma with high density can be obtained from rf glow discharge with varying gas pressure, and the density of plasma becomes higher as the gas pressure varies from 1 Tort to 100 Tort. It is also shown that in the range of the gas pressure from 1 Tort to 100 Tort with the slower rate of varying gas pressure, higher density of plasma can be obtained.     

Structure of unsupported bismuth nanoparticles

We present new results of electron diffraction experiments on unsupported nanometer-sized bismuth clusters. The high intensity cluster beam, necessary for electron diffraction, is provided by an inert-gas aggregation source. The cluster beam contains particles with average cluster sizes between 4.5 and 10 nm. When using Helium as a carrier gas we are able to observe a transition from crystalline clusters to a new structure, which we identify with that of amorphous or liquid clusters. Received 28 November 2000     

Effect of metal oxide and oxygen on the growth of single-walled carbon nanotubes by electric arc discharge

The effect of oxygen on the growth of single-walled carbon nanotubes was studied with Ni–Co alloy powder as catalyst under helium atmosphere of 500 Torr by electric arc discharge. The oxygen included in nickel or (and) cobalt oxides was added in catalyst. The content of oxygen in atmosphere was controlled by changing vacuum degree inside furnace before inputting buffer gas. The examinations of TEM and Raman scattering showed that oxygen in metal oxide as catalyst promotes the nucleation of SWCNT by taking effect on the metal catalyst particles. However, O₂ in atmosphere has the role of oxidizing amorphous particles along with nanotubes. When its molar proportion is higher than 0.22 ppm (Parts per million), the carbon nanotubes produced are oxidized and their purity decreases. The diameter of single-walled carbon nanotube obtained under different condition has a narrow distribution around 1.28 nm.     

Electrical conduction mechanism in Fe<Subscript>70</Subscript>Pd<Subscript>30</Subscript> catalyzed multi-walled carbon nanotubes

Carbon nanotubes (CNTs) are synthesized by the catalytic decomposition of acetylene using low pressure chemical vapour deposition method (LPCVD) at 800 °C and at a chamber pressure of 10 Torr over a supported catalyst film of Fe₇₀Pd₃₀. Morphology of these CNTs is studied using Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM) and High Resolution Transmission Electron Microscopy (HRTEM). From HRTEM image of these multi-walled carbon nanotubes (MWNTs), it is clear that these MWNTs do not possess a co-axial cylindrical structure, but are composed of imperfect and broken graphite cylinders of different sizes. The average diameter and length of the nanotubes varies between 20–70 nm and 5–60 μm respectively. Electrical transport measurements of these MWNTs are studied over a temperature range of 298–4.2 K. The results have been interpreted in terms of variable-range hopping (VRH) over the entire temperature range of 298–4.2 K. Three-dimensional variable-range hopping (VRH) is suggested for the temperature range (298–125 K), while two-dimensional VRH is observed for the temperature range (125–4.2 K).