Characterization of Large Particles in Fumed Silica Based CMP Slurry

2010 ◽  
Vol 1249 ◽  
Author(s):  
W. Scott Rader ◽  
Timothy Holt ◽  
Kazusei Tamai

AbstractLarge particles in fumed silica dispersions were characterized by sedimentation, light scattering techniques, Transmission Electron Microscopy (TEM), and lacunarity. Applying centrifugation to fumed silica dispersions generated differences in sedimentation rates of large particles. The sedimentation rates of the large particles were affected by morphological differences and the particles remaining in the supernatant displayed buoyant behavior. The large particle morphology varied from branch like aggregates containing large primary particles to particles comprised of highly coalesced, tightly packed small primary particles. The results indicate the presence of different types of large particles in fumed silica dispersions to which conventional large particle characterization is unable to distinguish.

Author(s):  
O. L. Shaffer ◽  
M.S. El-Aasser ◽  
C. L. Zhao ◽  
M. A. Winnik ◽  
R. R. Shivers

Transmission electron microscopy is an important approach to the characterization of the morphology of multiphase latices. Various sample preparation techniques have been applied to multiphase latices such as OsO4, RuO4 and CsOH stains to distinguish the polymer phases or domains. Radiation damage by an electron beam of latices imbedded in ice has also been used as a technique to study particle morphology. Further studies have been developed in the use of freeze-fracture and the effect of differential radiation damage at liquid nitrogen temperatures of the latex particles embedded in ice and not embedded.Two different series of two-stage latices were prepared with (1) a poly(methyl methacrylate) (PMMA) seed and poly(styrene) (PS) second stage; (2) a PS seed and PMMA second stage. Both series have varying amounts of second-stage monomer which was added to the seed latex semicontinuously. A drop of diluted latex was placed on a 200-mesh Formvar-carbon coated copper grid.


2009 ◽  
Vol 81 (8) ◽  
pp. 1489-1498 ◽  
Author(s):  
Amreesh Chandra ◽  
Alexander J. Roberts ◽  
Eric Lam How Yee ◽  
Robert C. T. Slade

Nanostructured materials are extensively investigated for application in energy storage and power generation devices. This paper deals with the synthesis and characterization of nanomaterials based on oxides of vanadium and with their application as electrode materials for energy storage systems viz. supercapacitors. These nano-oxides have been synthesized using a hydrothermal route in the presence of templates: 1-hexadecylamine, Tweens and Brij types. Using templates during synthesis enables tailoring of the particle morphology and physical characteristics of synthesized powders. Broad X-ray diffraction peaks show the formation of nanoparticles, confirmed using scanning electron microscopy (SEM) and transmission electron microscopy (TEM) investigations. SEM studies show that a large range of nanostructures such as needles, fibers, particles, etc. can be synthesized. These particles have varying surface areas and electrical conductivity. Enhancement of surface area as much as seven times relative to surface areas of starting parent materials has been observed. These properties make such materials ideal candidates for application as electrode materials in supercapacitors. Assembly and characterization of supercapacitors based on electrodes containing these active nano-oxides are discussed. Specific capacitance of >100 F g–1 has been observed. The specific capacitance decreases with cycling: causes of this phenomenon are presented.


2012 ◽  
Vol 5 (4) ◽  
pp. 4905-4925 ◽  
Author(s):  
M. Gysel ◽  
M. Laborde ◽  
J. C. Corbin ◽  
A. A. Mensah ◽  
A. Keller ◽  
...  

Abstract. The single particle soot photometer (SP2) uses laser-induced incandescence (LII) for the measurement of atmospheric black carbon (BC) particles. The BC mass concentration is obtained by combining quantitative detection of BC mass in single particles with a counting efficiency of 100% above its lower detection limit (LDL). It is commonly accepted that a particle must contain at least several tenths of femtograms BC in order to be detected by the SP2. Here we show the unexpected result that BC particles from a PALAS spark discharge soot generator remain undetected by the SP2, even if their BC mass, as independently determined with an aerosol particle mass analyser (APM), is clearly above the typical LDL of the SP2. Comparison of counting efficiency and effective density data of PALAS soot with flame generated soot (combustion aerosol standard burner, CAST), fullerene soot and carbon black particles (Cabot Regal 400R) reveals that particle morphology can affect the SP2's LDL. PALAS soot particles are fractal-like agglomerates of very small primary particles with a low fractal dimension, resulting in a very low effective density. Such loosely-packed particles behave like "the sum of individual primary particles" in the SP2's laser. Accordingly, the PALAS soot particles remain undetected as the SP2's laser intensity is insufficient to heat the primary particles to vaporisation because of their small size (primary particle diameter ~5–10 nm). It is not surprising that particle morphology can have an effect on the SP2's LDL, however, such a dramatic effect as reported here for PALAS soot was not expected. In conclusion, the SP2's LDL at a certain laser power depends on total BC mass per particle for compact particles with sufficiently high effective density. However, for fractal-like agglomerates of very small primary particles and low fractal dimension, the BC mass per primary particle determines the limit of detection, independent of the total particle mass. Consequently, care has to be taken when using the SP2 in applications dealing with loosely-packed particles that have very small primary particles as building blocks.


1995 ◽  
Vol 73 (11) ◽  
pp. 1747-1756 ◽  
Author(s):  
Anthony J. Paine ◽  
Richard R. Shivers

The interior particle morphology of dispersion-polymerized polystyrene particles was investigated by freeze fracture TEM (FFTEM) in order to compare the morphology of particles formed under two extreme mechanistic conditions: (a) particle growth by scavenging of dead polymer chains formed in solution (which gives rise to large particles of 5–10 μm) and (b) particle growth by oligomeric radical capture and polymerization inside the particle (giving rise to small particles of 1 μm or less). Although not generally recognized in the literature, ascribing mechanistic significance to an observed morphology requires a demonstration that the morphology is of the non-equilibrium type, i.e., the morphology depends upon how the particle was formed. An equilibrium morphology, by definition, must be independent of the particle formation route, and therefore carries no mechanistic information. In this case, large PS particles of 6.5 μm were found to have a nodular morphology that was unchanged on heating well above Tg, indicating an equilibrium structure (the nodularity of amorphous polymers is briefly rationalized by comparison with literature results over the past 20 years). On the other hand, small PS particles of 1.3 μm had a pronounced radial structure that could be converted into the nodular morphology by the same heat treatment, or by dissolving and precipitating from a suitable solvent combination. This means that the small particles have a non-equilibrium morphology, from which we may attempt to draw mechanistic inferences consistent with the suspected growth mechanism. Keywords: dispersion-polymerized polystyrene, non-equilibrium polystyrene particle morphology, freeze fracture transmission electron microscopy.


2012 ◽  
Vol 5 (12) ◽  
pp. 3099-3107 ◽  
Author(s):  
M. Gysel ◽  
M. Laborde ◽  
A. A. Mensah ◽  
J. C. Corbin ◽  
A. Keller ◽  
...  

Abstract. The single particle soot photometer (SP2) uses laser-induced incandescence (LII) for the measurement of atmospheric black carbon (BC) particles. The BC mass concentration is obtained by combining quantitative detection of BC mass in single particles with a counting efficiency of 100% above its lower detection limit. It is commonly accepted that a particle must contain at least several tenths of a femtogram BC in order to be detected by the SP2. Here we show the result that most BC particles from a PALAS spark discharge soot generator remain undetected by the SP2, even if their BC mass, as independently determined with an aerosol particle mass analyser (APM), is clearly above the typical lower detection limit of the SP2. Comparison of counting efficiency and effective density data of PALAS soot with flame generated soot (combustion aerosol standard burner, CAST), fullerene soot and carbon black particles (Cabot Regal 400R) reveals that particle morphology can affect the SP2's lower detection limit. PALAS soot particles are fractal-like agglomerates of very small primary particles with a low fractal dimension, resulting in a very low effective density. Such loosely packed particles behave like "the sum of individual primary particles" in the SP2's laser. Accordingly, most PALAS soot particles remain undetected as the SP2's laser intensity is insufficient to heat the primary particles to their vaporisation temperature because of their small size (Dpp ≈ 5–10 nm). Previous knowledge from pulsed laser-induced incandescence indicated that particle morphology might have an effect on the SP2's lower detection limit, however, an increase of the lower detection limit by a factor of ∼5–10, as reported here for PALAS soot, was not expected. In conclusion, the SP2's lower detection limit at a certain laser power depends primarily on the total BC mass per particle for compact particles with sufficiently high effective density. By contrast, the BC mass per primary particle mainly determines whether fractal-like particles with low fractal dimension and very small primary particles are detectable, while their total BC mass has only a minor influence. This effect shifts the lower detection limit to much higher BC mass, or makes them completely undetectable. Consequently, care has to be taken when using the SP2 in applications dealing with loosely packed particles that have very small primary particles as building blocks.


Clay Minerals ◽  
1993 ◽  
Vol 28 (4) ◽  
pp. 539-553 ◽  
Author(s):  
P. De Souza Santos

AbstractThe use of transmission electron microscopy in association with other methods is described for the characterization of Brazilian industrial clays, especially kaolinitic-halloysitic clays. Examples are presented from: (a) tubular 7 Å-halloysites and the characterization of mixtures with ordered and disordered kaolinites in residual china clays; (b) tubular kaolinitic clay from Piedade, São Paulo; (c) platey 10 Å-halloysite from Poģos de Caldas, Minas Gerais; (d) rolled forms similar to 10 Å-tubular halloysite formed by repeated K Ac intercalation in well ordered kaolinite; (e) use of particle shape and size of kaolinite crystals in the São Simão, São Paulo ball clays as orientation for good sanitaryware ball clays; (f) characterization of gibbsite crystals in high alumina gibbsite/kaolinite clays; (g) antigorite as a clay mineral; (h) electron optical studies of thermal phase transformations involving tubular kaolinite, halloysites, antigorite, chrysotile, talc and pyrophyllite mono crystals.


2012 ◽  
Vol 15 (2) ◽  
pp. 27-34
Author(s):  
Nguyet Thi Thuy Dao ◽  
Duong Phuc Nguyen ◽  
Hien Duc Than

This paper presents the synthesis and characterization of Y3Fe5O12, Gd3Fe5O12 and Dy3Fe5O12 nanoparticles by sol-gel method using initial salts solution of Y(NO3)3, Gd(NO3)3, Dy(NO3)3, Fe(NO3). The lattice constant, crystallite size and particle morphology of these ferrite garnet nanoparticles were studied by using X-ray diffraction and transmission electron microscopy (TEM). The results showed that the garnet samples prepared by this method were formed at 800oC, which is lower than the sintering temperature for ceramic bulk samples (1400oC). The particle size is in the range 25- 40 nm as observed via TEM image and the average particle size was found to be 37nm using Debye- Scherrer formula.


Author(s):  
J. R. Reffner

Transmission Electron Microscopy (TEM) is a powerful tool for investigating the structure of latex particles. However, examining low Tg (glass transision, Tg < room temperature) latex particles requires special techniques due to the significant deformation which occurs if the particles are dispersed onto a substrate at room temperature. Here a freeze drying (FD) technique is presented which permits individual emulsion particles, including stained particles, to be examined in a manner that minimizes deformation by maintaining the particles at temperatures below Tg.Typically, particle morphology is determined from images of individual latex particles dispersed onto a supporting ultra-thin substrate or from images of ultra-microtomed sections of films cast from the latex. Examining particles dispersed onto a substrate is often advantageous, allowing direct determination of particle shape and characterization of the morphology prior to the film formation process. Although low Tg materials can be examined using this technique, information about the size, shape and morphology of phase separated domains can be obscured by the deformation which occurs when the particles are examined at room temperature.


1995 ◽  
Vol 400 ◽  
Author(s):  
Timothy M. Owens ◽  
Pratim Biswas

AbstractA detailed characterization was performed of the particles produced under various Pb:Si molar feed ratios in a flow reactor at a maximum temperature of 1000 °C. The silica particles formed in the high temperature region coagulated and only partially coalesced to form large agglomerate structures of high specific surface area. For a lead only feed, the resulting particles were hydrocerussite with small but detectable amounts of massicot. As the silica precursor was inlet in excess amounts (Pb:Si ≤ 1:12), the crystalline lead compounds disappeared and amorphous lead-silica complexes predominated. The particle morphology also changed from cylindrical, polygonal and spherical shapes to large agglomerate structures composed of several size modes of primary particles. At Pb:Si molar feed ratios of 1:12 and 1:29, the particles making up the chain-like agglomerate structure were primarily spherical with larger lead silicate spherical particles (≈ 0.5 μm) attached to the agglomerate. The lead was found to be distributed throughout the large agglomerate structures.


Author(s):  
R. E. Herfert

Studies of the nature of a surface, either metallic or nonmetallic, in the past, have been limited to the instrumentation available for these measurements. In the past, optical microscopy, replica transmission electron microscopy, electron or X-ray diffraction and optical or X-ray spectroscopy have provided the means of surface characterization. Actually, some of these techniques are not purely surface; the depth of penetration may be a few thousands of an inch. Within the last five years, instrumentation has been made available which now makes it practical for use to study the outer few 100A of layers and characterize it completely from a chemical, physical, and crystallographic standpoint. The scanning electron microscope (SEM) provides a means of viewing the surface of a material in situ to magnifications as high as 250,000X.


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