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At least 19 records

The first products made in space - Monodisperse latex particles

Monodisperse latex particles developed by seeded emulsion polymerization on various Space Shuttle flights are analyzed. The flight hardware was composed of a monodisperse latex reactor and a support electronics package, and the particles were examined by optical microscopy and TEM. Data on the particle size distributions, larger and smaller off-size particles, and conversion-time curves for the particles are examined and compared to ground-based results. It is observed that the ground-based polymerizations have more coagulum than the flight polymerizations; the flight latex particles have narrower size distributions than the ground particles; and the number of off-size larger particles in the flight particles is smaller than in the ground data.

Vanderhoff, J. W.↗

Producing Large-Particle Monodisperse Latexes

Chemical process produces latex particles of relatively large, uniform size for use as size standards for instrument calibration. Process, based on seeding of mixture by very small latex particles, yields particles measuring 2 to 30 micrometer or more in average size. Produces monodisperse latexes in which deviation from average size is less than 2 percent. Particles used directly, without tedious separation procedures for removing off-size particles.

Vanderhoff, J. W.↗

Process for preparation of large-particle-size monodisperse latexes

Monodisperse latexes having a particle size in the range of 2 to 40 microns are prepared by seeded emulsion polymerization in microgravity. A reaction mixture containing smaller monodisperse latex seed particles, predetermined amounts of monomer, emulsifier, initiator, inhibitor and water is placed in a microgravity environment, and polymerization is initiated by heating. The reaction is allowed to continue until the seed particles grow to a predetermined size, and the resulting enlarged particles are then recovered. A plurality of particle-growing steps can be used to reach larger sizes within the stated range, with enlarge particles from the previous steps being used as seed particles for the succeeding steps. Microgravity enables preparation of particles in the stated size range by avoiding gravity related problems of creaming and settling, and flocculation induced by mechanical shear that have precluded their preparation in a normal gravity environment.

Vanderhoff, J. W.↗

Preparation of large-particle-size monodisperse polystyrene latexes in microgravity

Three large-particle-size monodisperse latexes (3.44, 4.08, and 4.98 micron diameter) were prepared in an automated four-reactor apparatus on the third orbital mission of the 'Columbia' begun on March 22. Comparison with ground-based controls showed that the 4.98 micron-size flight sample was the more uniform; the uniformity at the other two sizes was about the same. The rates of polymerization in microgravity and on earth were the same within experimental error, demonstrating that radical-initiated vinyl addition polymerizations are unaffected by the weightless environment.

Vanderhoff, J. W.↗

High purity silica reflecting heat shield development

A reflecting heat shield composed of fused silica in which the scattering results from the refractive index mismatch between silica particles and the voids introduced during the fabrication process is developed. Major considerations and conclusions of the development are: the best material to use is Type A, which is capable of ultra-high-purity and which does not show the 0.243 micrometer absorption band; the reflection efficiency of fused silica is decreased at higher temperatures due to the bathochromic shift of the ultraviolet cut-off; for a given silica material, over the wavelength region and particle sizes tested, the monodisperse particle size configurations produce higher reflectances than continuous particle size configurations; and the smaller monodisperse particle size configurations give higher reflectance than the larger ones. A reflecting silica configuration that is an efficient reflector of shock layer radiation at high ablation temperatures is achieved by tailoring the matrix for optimum scattering and using an ultra-high-purity material.

Congdon, W.↗

The first products made in space: Monodisperse latex particles

The preparation of large particle size 3 to 30 micrometer monodisperse latexes in space confirmed that original rationale unequivocally. The flight polymerizations formed negligible amounts of coagulum as compared to increasing amounts for the ground-based polymerizations. The number of offsize large particles in the flight latexes was smaller than in the ground-based latexes. The particle size distribution broadened and more larger offsize particles were formed when the polymerizations of the partially converted STS-4 latexes were completed on Earth. Polymerization in space also showed other unanticipated advantages. The flight latexes had narrower particle size distributions than the ground-based latexes. The particles of the flight latexes were more perfect spheres than those of the ground-based latexes. The superior uniformity of the flight latexes was confirmed by the National Bureau of Standards acceptance of the 10 micrometer STS-6 latex and the 30 micrometer STS-11 latexes as Standard Reference Materials, the first products made in space for sale on Earth. The polymerization rates in space were the same as those on Earth within experimental error. Further development of the ground-based polymerization recipes gave monodisperse particles as large as 100 micrometer with tolerable levels of coagulum, but their uniformity was significantly poorer than the flight latexes. Careful control of the polymerization parameters gave uniform nonspherical particles: symmetrical and asymmetrical doublets, ellipsoids, egg-shaped, ice cream cone-shaped, and popcorn-shaped particles.

Vanderhoff, J. W.↗

Feasibility study: Monodisperse polymer particles containing laser-excitable dyes

The objective was to determine the feasibility of the preparation of monodisperse spherical poly(methyl methacrylate) and polystyrene particles that contain laser-excitable dyes in the size range 0.1 microns to 1 cm. Poly(methyl methacrylate) and polystyrene were chosen because of their excellent optical properties. The sphericity was required for uniformity of spectral output of re-irradiated light from the dye-containing particles. The monodispersity was required to give each particle the same optical properties when exposed to laser light.

Vanderhoff, John W.↗

Preparation of large-particle-size monodisperse latexes in space: The STS-3, STS-4, and STS-7 mission results

Large-particle-size monodisperse latexes were prepared on four STS missions of the space shuttles Columbia and Challenger using flight hardware comprising four automated 100 cm(3) polymerization reactors. Seven polymerizations carried out on the March 1982 STS-3 mission of the Columbia, and the April 1983 STS-6 and June 1983 STS-7 missions of the Challenger, gave monodisperse latexes of 5 to 18 micron diameter with narrower particle size distributions than the corresponding ground-based control polymerizations. The rates of polymerization in microgravity were the same as on Earth. The results of these experiments are reviewed, and the prospects of the development of a space production process are discussed.

Vanderhoff, J. W.↗

Production of large-particle-size monodisperse latexes

The research program achieved two objectives: (1) it has refined and extended the experimental techniques for preparing monodisperse latexes in quantity on the ground up to a particle diameter of 10 microns; and (2) it has demonstrated that a microgravity environment can be used to grow monodisperse latexes to larger sizes, where the limitations in size have yet to be defined. The experimental development of the monodisperse latex reactor (MLR) and the seeded emulsion polymerizations carried out in the laboratory prototype of the flight hardware, as a function of the operational parameters is discussed. The emphasis is directed towards the measurement, interpretation, and modeling of the kinetics of seeded emulsion polymerization and successive seeded emulsion polymerization. The recipe development of seeded emulsion polymerization as a function of particle size is discussed. The equilibrium swelling of latex particles with monomers was investigated both theoretically and experimentally. Extensive studies are reported on both the type and concentration of initiators, surfactants, and inhibitors, which eventually led to the development of the flight recipes. The experimental results of the flight experiments are discussed, as well as the experimental development of inhibition of seeded emulsion polymerization in terms of time of inhibition and the effect of inhibitors on the kinetics of polymerization.

Vanderhoff, J. W.↗

Preparation of large-particle-size monodisperse latexes in space

Results are reported of latex sphere polymerization experiments performed on two flights of the Columbia and three flights of the Challenger. The trials were carried out because polymerization of the spheres in space avoids coagulation, nucleation of a new crop of particles, and excessive stirring requirements, and allows growth of spheres larger than 4 microns diam. The Monodisperse Latex Reactor (MLR) held four stirred 100 cc sealed stainless steel cylindrical containers. The mixtures were monitored for the conversion times, volume decreases as spheres formed and the mixture temperature. The spheres were grown from 0.19 micron seeds. Details of the flight preparation efforts are outlined. In flights which did not experience mechanical malfunctions spheres 3-30 microns diam were grown that had noticeably lower size variations than did the ground-based control particles. The 10 micron diam spheres grown on STS-6 were accepted as standard reference material by the NBS and became the first products made in space to be commercially sold on earth; the 30 micron spheres also became NBS standards. The experiments confirmed all projected benefits of producing the spheres in space, as well as provided the opportunity to grow more larger offsize spheres by finishing the growths on earth.

Vanderhoff, J. W.↗

Measuring Monodisperse Small Particles En Masse

New optical method enables determination of sizes of approximately-micron-sized particles. Arrays of particles act as diffraction gratings. Simple and inexpensive apparatus replaces high-magnification microscopes in measurements of diameters of small polystyrene latex spheres. Device being used to determine monodispersity and diameters of polystyrene latex microspheres used as seeding material for laser-velocimetry flow measurements in NASA's wind tunnels. Characterization of particle sizes important in wide range of fields, including manufacture of plastics and ceramics, biochemistry, and medicine.

Bruce, Robert A.↗

Preparation of large-particle-size monodisperse latexes in space - Polymerization kinetics and process development

Monodisperse polystyrene latexes are prepared by seeded emulsion polymerization; however, sizes larger than 2 microns are difficult to prepare because of the creaming and settling of the particles and their sensitivity to mechanical shear. Preparation in space would obviate the creaming and settling, and allow agitation just sufficient for good heat transfer and mixing. Three polymerizations yielding 3-5 micron size particles were carried out successfully on the third flight of the 'Columbia' launched Mar. 22, 1982; however, four polymerizations yielding sizes up to 10 microns on the fourth flight launched June 27, 1982 were incomplete owing to apparatus malfunction. The results of these polymerizations and the prospects of developing a preparative space process are reviewed.

Vanderhoff, J. W.↗

Structure of particle-laden jets - Measurements and predictions

Measurements of mean and fluctuating velocities of both phases as well as particle mass fluxes were completed in turbulent, particle-laden jets containing monodisperse particles with well-defined initial and boundary conditions. The new measurements were used to evaluate a stochastic separated flow model of the process which treated effects of interphase slip and turbulent dispersion using random-walk computations for particle motion. The continuous phase was treated using a modified k-epsilon model allowing for direct contributions of interphase transport to both mean and turbulence properties. The model performed reasonably well over the new data base, with all empirical parameters fixed from earlier work. In contrast, simplified models ignoring either interphase slip or turbulent dispersion yielded poor agreement with the measurements.

Shuen, J.-S.↗

Production of Large-Particle-Size Monodisperse Latexes in Microgravity

A latex is a suspension of very tiny (micrometer-size) plastic spheres in water, stabilized by emulsifiers. The growth of billions of these tiny plastic spheres to sizes larger than can be grown on Earth is attempted while keeping all of them exactly the same size and perfectly spherical. Thus far on several of the Monodisperse Latex Reactor (MLR) flights, the latex spheres have been returned to Earth with standard deviations of better than 1.4%. In microgravity the absence of buoyancy effects has allowed growth of the balls up to 30 micrometers in diameter thus far. The MLR has now flown 5 times on the Shuttle. The MLR has now produced the first commercial space product; that is the first commercial material ever manufactured in space and marketed on Earth. Once it is demonstrated that these large-size-monodisperse latexes can be routinely produced in quantity and quality, they can be marketed for many types of scientific applications. They can be used in biomedical research for such things as drug carriers and tracers in the body, human and animal blood flow studies, membrane and pore-sizing in the body, and medical diagnostic tests.

Vanderhoff, J. W.↗

Feasibility study: Monodisperse polymer particles containing laser-excitable dyes

The optical properties associated with small particles, which include aerosols, hydrosols and solid microspheres have an impact on several areas of science and engineering. Since the advent of high-speed computers and lasers, the interaction of light with matter in the form of small particles with a discontinuous optical boundary relative to the surroundings has been much better understood. Various nonlinear optical effects have been observed involving interaction of a laser beam with both solid microspheres and liquid microdroplets. These include observation of second and third harmonic generation, four wave mixing, optical visibility, two photon absorption, observation of stimulated emission and lasing, and Stimulated Raman Scattering. Many of these effects are observed with laser intensities which are orders of magnitude less than that required by threshold condition for interactions in macroscopic bulk medium. The primary reason for this is twofold. The front surface of the microsphere acts as a thick lens to enhance the internal intensity of the input laser radiation, and the spherical shape of the droplet acts as an optical cavity to provide feedback at specific wavelengths corresponding to the whispering gallery modes or the morphology dependent resonances (MDR's). The most interesting and significant recent finding in this field is undoubtedly the existence of resonance peaks in linear and nonlinear optical spectra. Such resonance peaks are only dependent on the particle morphology, which means the size, shape and refractive index of the particle. Because of the simultaneous presence of these resonances, they have been referred to by many names, including structural resonances, whispering modes or whispering gallery modes, creeping waves, circumferential waves, surfaces modes, and virtual modes. All of these names refer to the same phenomena, i.e. morphology dependent resonances (MDR's) which has already been described and predicted precisely by electromagnetic theory and Loentz-Mie theory since 1908. MDR's can become important when the particle size (radius a) approaches and exceeds the wavelength of the electromagnetic wave (lambda) and the refractive index of the particle is greater than that of the surrounding medium. Such resonances are easiest to observe from a single particle with high symmetry, such as a sphere, spheroid, or cylinder. MDR's correspond to solutions of the characteristic equations of the electromagnetic fields in the presence of a sphere.

Venkateswarlu, Putcha↗

Seeded Growth of Colloidal Silica Particles

The method of seeded growth was studied for producing mondisperse colloidal silica particles. It was shown that particle size as well as weight percent solids could be controlled by using this method. The particles were characterized by transmission electron microscopy (TEM) and quasielastic light scattering (QELS). The particles were found to have a bimodal size distribution when examined by TEM. The particle size as determined by QELS was found to be roughly 10-20% larger than the particle size as determined by TEM. Furthermore, the polydispersity (standard deviation/mean particle size) as determined by QELS was found to be significantly lower than the polydispersity as determined by TEM. This underscores the importance of using TEM as a characterization technique for determining particle monodispersity. It was also noted that there was an increase in particle roughness as the weight percent of the silica particles increased and a new nucleation of particles was observed as the weight percent approached 13%. A recipe for producing monodisperse silica particles in the 150 nm size range is presented.

Wurm, David B.↗

Generation of monodisperse droplets by spontaneous condensation of flow in nozzles

Submicron size monodisperse particles are of interest in many industrial and scientific applications. These include the manufacture of ceramic parts using fine ceramic particles, the production of thin films by deposition of ionized clusters, monodisperse seed particles for laser anemometry, and the study of size dependence of cluster chemical and physical properties. An inexpensive and relatively easy way to generate such particles is by utilizing the phenomenon of spontaneous condensation. The phenomenon occurs when the vapor or a mixture of a vapor and a noncondensing gas is expanded at a high expansion rate. The saturation line is crossed with the supercooled vapor behaving like a gas, until all of a sudden at the so called Wilson point, condensation occurs, resulting in a large number of relatively monodisperse droplets. The droplet size is a function of the expansion rate, inlet conditions, mass fraction of vapor, gas properties, etc. Spontaneous condensation of steam and water vapor and air mixture in a one dimensional nozzle was modeled and the resulting equations solved numerically. The droplet size distribution at the exit of various one dimensional nozzles and the flow characteristics such as pressure ratio, mean droplet radius, vapor and droplet temperatures, nucleation flux, supercooling, wetness, etc., along the axial distance were obtained. The numerical results compared very well with the available experimental data. The effect of inlet conditions, nozzle expansion rates, and vapor mass fractions on droplet mean radius, droplet size distribution, and pressure ratio were examined.

Lai, Der-Shaiun↗

Method accurately measures mean particle diameters of monodisperse polystyrene latexes

Photomicrographic method determines mean particle diameters of monodisperse polystyrene latexes. Many diameters are measured simultaneously by measuring row lengths of particles in a triangular array at a glass-oil interface. The method provides size standards for electronic particle counters and prevents distortions, softening, and flattening.

Kubitschek, H. E.↗