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At least 217 records · Page 12

Fabrication and Modification of Nanoporous Silicon Particles

Silicon-based nanoporous particles as biodegradable drug carriers are advantageous in permeation, controlled release, and targeting. The use of biodegradable nanoporous silicon and silicon dioxide, with proper surface treatments, allows sustained drug release within the target site over a period of days, or even weeks, due to selective surface coating. A variety of surface treatment protocols are available for silicon-based particles to be stabilized, functionalized, or modified as required. Coated polyethylene glycol (PEG) chains showed the effective depression of both plasma protein adsorption and cell attachment to the modified surfaces, as well as the advantage of long circulating. Porous silicon particles are micromachined by lithography. Compared to the synthesis route of the nanomaterials, the advantages include: (1) the capability to make different shapes, not only spherical particles but also square, rectangular, or ellipse cross sections, etc.; (2) the capability for very precise dimension control; (3) the capacity for porosity and pore profile control; and (4) allowance of complex surface modification. The particle patterns as small as 60 nm can be fabricated using the state-of-the-art photolithography. The pores in silicon can be fabricated by exposing the silicon in an HF/ethanol solution and then subjecting the pores to an electrical current. The size and shape of the pores inside silicon can be adjusted by the doping of the silicon, electrical current application, the composition of the electrolyte solution, and etching time. The surface of the silicon particles can be modified by many means to provide targeted delivery and on-site permanence for extended release. Multiple active agents can be co-loaded into the particles. Because the surface modification of particles can be done on wafers before the mechanical release, asymmetrical surface modification is feasible. Starting from silicon wafers, a treatment, such as KOH dipping or reactive ion etching (RIE), may be applied to make the surface rough. This helps remove the nucleation layer. A protective layer is then deposited on the wafer. The protective layer, such as silicon nitride film or photoresist film, protects the wafer from electrochemical etching in an HF-based solution. A lithography technique is applied to pattern the particles onto the protective film. The undesired area of the protective film is removed, and the protective film on the back side of the wafer is also removed. Then the pattern is exposed to HF/surfactant solution, and a larger DC electrical current is applied to the wafers for a selected time. This step removes the nucleation layer. Then a DC current is applied to generate the nanopores. Next, a large electrical current is applied to generate a release layer. The particles are mechanically suspended in the solvent and collected by filtration or centrifuge.

Ferrari, Mauro↗

Effects of varying oxygen partial pressure on molten silicon-ceramic substrate interactions

The silicon sessile drop contact angle was measured on hot pressed silicon nitride, silicon nitride coated on hot pressed silicon nitride, silicon carbon coated on graphite, and on Sialon to determine the degree to which silicon wets these substances. The post-sessile drop experiment samples were sectioned and photomicrographs were taken of the silicon-substrate interface to observe the degree of surface dissolution and degradation. Of these materials, silicon did not form a true sessile drop on the SiC on graphite due to infiltration of the silicon through the SiC coating, nor on the Sialon due to the formation of a more-or-less rigid coating on the liquid silicon. The most wetting was obtained on the coated Si3N4 with a value of 42 deg. The oxygen concentrations in a silicon ribbon furnace and in a sessile drop furnace were measured using the protable thoria-yttria solid solution electrolyte oxygen sensor. Oxygen partial pressures of 10 to the minus 7 power atm and 10 to the minus 8 power atm were obtained at the two facilities. These measurements are believed to represent nonequilibrium conditions.

Ownby, D. P.↗

Converting a carbon preform object to a silicon carbide object

A process for converting in depth a carbon or graphite preform object to a silicon carbide object, silicon carbide/silicon object, silicon carbide/carbon-core object, or a silicon carbide/silicon/carbon-core object, by contacting it with silicon liquid and vapor over various lengths of contact time in a reaction chamber. In the process, a stream comprised of a silicon-containing precursor material in gaseous phase below the decomposition temperature of said gas and a coreactant, carrier or diluent gas such as hydrogen is passed through a hole within a high emissivity, thin, insulating septum into the reaction chamber above the melting point of silicon. The thin septum has one face below the decomposition temperature of the gas and an opposite face exposed to the reaction chamber. Thus, the precursor gas is decomposed directly to silicon in the reaction chamber. Any stream of decomposition gas and any unreacted precursor gas from the reaction chamber is removed. A carbon or graphite preform object placed in the reaction chamber is contacted with the silicon. The carbon or graphite preform object is recovered from the reactor chamber after it has been converted to a desired silicon carbide, silicon and carbon composition.

Levin, Harry↗

A New Process for Fabricating Random Silicon Nanotips

An improved process for the fabrication of random arrays of silicon nanotips has been demonstrated to be feasible. Relative to other such processes, this process offers advantages of low cost and simplicity. Moreover, this process can readily be combined with other processes used to fabricate integrated circuits and other monolithic silicon structures. Arrays of silicon nanotips are subjects of research and development efforts directed toward utilizing them as field emitters in flat-panel displays, vacuum microelectronics, and microwave devices. Other silicon-nanotip-fabrication processes developed thus far predominantly include lithography, etching, and/or elaborate deposition steps followed by oxide sharpening steps and are both process intensive as well as expensive. In addition to being cheaper and simpler, the present process can efficiently produce silicon nanotips that range in height from a few microns to several tens of microns and are distributed over large areas. The process mentioned here can be summarized as consisting of (1) the growth of micro-etch masks on a silicon substrate, followed by (2) etching away of the masks, along with some of the substrate, to make an array of sharp tips. In the first step of the process, a cleaned silicon substrate is subjected to reactive ion etching (RIE) in a certain mixture of oxygen and carbon tetrafluoride under radio-frequency excitation. This process step results in the growth of fluorine based compounds in the form of stumps randomly distributed on the substrate. These stumps are known in the art as polymer RIE grass. The dimensions of these stumps are of the order of hundreds of nanometers, the exact values depending on process time and gas composition. The areal density of the stumps decreases with increasing process time as they grow and merge with neighboring stumps. These stumps constitute the micro-etch masks for the next step of the process. In the second step of the process, the substrate covered with the microetch masks is subjected to deep reactive ion etching (DRIE) process, which consists of cycles of reactive ion etching alternating with passivation (the Bosch process). The gas used in the etching substeps is sulfur hexafluoride (SF6); the gas used in the passivation substeps is octafluorocyclobutane (C4F8). The portions of the substrate directly under the RIE grass stubs are etched more slowly than are the portions between the stubs. Hence, what remains at the end of the process, after the stubs and parts of the substrate have been etched away, are silicon spikes where the stubs were (see figure). In a variation of the process, one starts with a silicon or silicon-on-insulator substrate with the intent to etch through the full thickness of the substrate. That is to say, one chooses the thickness so that the DRIE step releases individual nanotips. Such individual silicon nanotips may have utility as microscopic probes in biomedical applications.

Manohara, Harish↗

Fluidized bed silicon deposition from silane

A process and apparatus for thermally decomposing silicon containing gas for deposition on fluidized nucleating silicon seed particles is disclosed. Silicon seed particles are produced in a secondary fluidized reactor by thermal decomposition of a silicon containing gas. The thermally produced silicon seed particles are then introduced into a primary fluidized bed reactor to form a fluidized bed. Silicon containing gas is introduced into the primary reactor where it is thermally decomposed and deposited on the fluidized silicon seed particles. Silicon seed particles having the desired amount of thermally decomposed silicon product thereon are removed from the primary fluidized reactor as ultra pure silicon product. An apparatus for carrying out this process is also disclosed.

Hsu, George C.↗

Fluidized bed silicon deposition from silane

A process and apparatus for thermally decomposing silicon containing gas for deposition on fluidized nucleating silicon seed particles is disclosed. Silicon seed particles are produced in a secondary fluidized reactor by thermal decomposition of a silicon containing gas. The thermally produced silicon seed particles are then introduced into a primary fluidized bed reactor to form a fludized bed. Silicon containing gas is introduced into the primary reactor where it is thermally decomposed and deposited on the fluidized silicon seed particles. Silicon seed particles having the desired amount of thermally decomposed silicon product thereon are removed from the primary fluidized reactor as ultra pure silicon product. An apparatus for carrying out this process is also disclosed.

Hsu, George↗

Friction and wear behavior of single-crystal silicon carbide in contact with titanium

Sliding friction experiments were conducted with single crystal silicon carbide in sliding contact with titanium. Results indicate that the friction coefficient is greater in vacuum than in argon and that this is due to the greater adhesion or adhesive transfer in vacuum. Thin films of silicon carbide transferred to titanium also adhered to silicon carbide both in argon at atmospheric pressure and in high vacuum. Cohesive bonds fractured on both the silicon carbide and titanium surfaces. The wear debris of silicon carbide created by fracture plowed the silicon carbide surface in a plastic manner. The friction characteristics of titanium in contact with silicon carbide were sensitive to the surface roughness of silicon carbide, and the friction coefficients were higher for a rough surface of silicon carbide than for a smooth one. The difference in friction results was due to plastic deformation (plowing of titanium).

Miyoshi, K.↗

Surface chemistry and friction behavior of the silicon carbide (0001) surface at temperatures to 1500 deg C

X-ray photoelectron and Auger electron spectroscopy analyses and friction studies were conducted with a silicon carbide (0001) surface in contact with iron at various temperatures to 1200 or 1500 C in a vacuum of 10 to the minus 8th power Pa. The results indicate that there is a significant temperature influence on both the surface chemistry and friction properties of silicon carbide. The principal contaminant of adsorbed amorphous carbon on the silicon carbide surface in the as received state is removed by simply heating to 400 C. Above 400 C, graphite and carbide type carbine are the primary species on the silicon carbide surface, in addition to silicon. The coefficients of friction of polycrystalline iron sliding against a single crystal silicon carbide (0001) surface were high at temperatures to 800 C. Similar coefficients of friction were obtained at room temperature after the silicon carbide was preheated at various temperatures up 800 C. When the friction experiments were conducted above 800 C or when the specimens were preheated to above 800 C, the coefficients of friction were dramatically lower. At 800 C the silicon and carbide type carbon are at a maximum intensity in the XPS spectra. With increasing temperature above 800 C, the concentration of the graphite increases rapidly on the surface, whereas those of the carbide type carbon and silicon decrease rapidly.

Miyoshi, K.↗

Silicon material technology status

Silicon has been the basic element for the electronic and photovoltaic industries. The use of silicon as the primary element for terrestrial photovoltaic solar arrays is projected to continue. The reasons for this projection are related to the maturity of silicon technology, the ready availability of extremely pure silicon, the performance of silicon solar cells, and the considerable present investment in technology and manufacturing facilities. The technologies for producing semiconductor grade silicon and, to a lesser extent, refined metallurgical grade silicon are considered. It is pointed out that nearly all of the semiconductor grade silicon is produced by processes based on the Siemens deposition reactor, a technology developed 26 years ago. The state-of-the-art for producing silicon by this process is discussed. It is expected that efforts to reduce polysilicon process costs will continue.

Lutwack, R.↗

Behavior of Particle Depots in Molten Silicon During Float-Zone Growth in Strong Static Magnetic Fields

In the photovoltaics industry, the largest market share is represented by solar cells made from multicrystalline silicon, which is grown by directional solidification. During the growth process, the silicon melt is in contact with the silicon nitride coated crucible walls and the furnace atmosphere which contains carbon monoxide. The dissolution of the crucible coating, the carbon bearing gas, and the carbon already present in the feedstock, lead to the precipitation of silicon carbide, and silicon nitride, at later stages of the growth process. The precipitation of Si3N4 and SiC particles of up to several hundred micrometers in diameter leads to severe problems during the wire sawing process for wafering the ingots. Furthermore the growth of the silicon grains can be negatively influenced by the presence of particles, which act as nucleation sources and lead to a grit structure of small grains and are sources for dislocations. If doped with Nitrogen from the dissolved crucible coating, SiC is a semi conductive material, and can act as a shunt, short circuiting parts of the solar cell. For these reasons, the incorporation of such particles needs to be avoided. In this contribution we performed model experiments in which the transport of intentionally added SiC particles and their interaction with the solid-liquid interface during float zone growth of silicon in strong steady magnetic fields was investigated. SiC particles of 7μm and 60μm size are placed in single crystal silicon [100] and [111] rods of 8mm diameter. This is achieved by drilling a hole of 2mm diameter, filling in the particles and closing the hole by melting the surface of the rod until a film of silicon covers the hole. The samples are processed under a vacuum of 1x10(exp -5) mbar or better, to prevent gas inclusions. An oxide layer to suppress Marangoni convection is applied by wet oxidation. Experiments without and with static magnetic field are carried out to investigate the influence of melt convection on the distribution of particles and their incorporation into the crystal. The field strengths applied by a superconducting magnet are 1T, 3T, 4.5T, and 5T. The increase in field strength dampens the melt flow, and so this study provides comparative data to the crystal growth experiment to be carried out onboard the sounding rocket mission TEXUS 51, where purely diffusive growth condition will be achieved under microgravity conditions.

Jauss, T.↗

Improved toughness of silicon carbide

Impact energy absorbing layers (EALs) comprised of partially densified silicon carbide were formed in situ on fully sinterable silicon carbide substrates. After final sintering, duplex silicon carbide structures resulted which were comprised of a fully sintered, high density silicon carbide substrate or core, overlayed with an EAL of partially sintered silicon carbide integrally bonded to its core member. Thermal cycling tests proved such structures to be moderately resistant to oxidation and highly resistant to thermal shock stresses. The strength of the developed structures in some cases exceeded but essentially it remained the same as the fully sintered silicon carbide without the EAL. Ballistic impact tests indicated that substantial improvements in the toughness of sintered silicon carbide were achieved by the use of the partially densified silicon carbide EALs.

Palm, J. A.↗

New technologies for solar energy silicon - Cost analysis of dichlorosilane process

A reduction in the cost of silicon for solar cells is an important objective in a project concerned with the reduction of the cost of electricity produced with solar cells. The cost goal for the silicon material is about $14 per kg (1980 dollars). The process which is currently employed to produce semiconductor grade silicon from trichlorosilane is not suited for meeting this cost goal. Other processes for producing silicon are, therefore, being investigated. A description is presented of results obtained for the DCS process which involves the production of dichlorosilane as a silicon source material for solar energy silicon. Major benefits of dichlorosilane as a silicon source material include faster reaction rates for chemical vapor deposition of silicon. The DCS process involves the reaction 2SiHCl3 yields reversibly SiH2Cl2 + SiCl4. The results of a cost analysis indicate a total product cost without profit of $1.29/kg of SiH2Cl2.

Yaws, C. L.↗

Silicon production in a fluidized bed reactor

Part of the development effort of the JPL in-house technology involved in the Flat-Plate Solar Array (FSA) Project was the investigation of a low-cost process to produce semiconductor-grade silicon for terrestrial photovoltaic cell applications. The process selected was based on pyrolysis of silane in a fluidized-bed reactor (FBR). Following initial investigations involving 1- and 2-in. diameter reactors, a 6-in. diameter, engineering-scale FBR was constructed to establish reactor performance, mechanism of silicon deposition, product morphology, and product purity. The overall mass balance for all experiments indicates that more than 90% of the total silicon fed into the reactor is deposited on silicon seed particles and the remaining 10% becomes elutriated fines. Silicon production rates were demonstrated of 1.5 kg/h at 30% silane concentration and 3.5 kg/h at 80% silane concentration. The mechanism of silicon deposition is described by a six-path process: heterogeneous deposition, homogeneous decomposition, coalescence, coagulation, scavenging, and heterogeneous growth on fines. The bulk of the growth silicon layer appears to be made up of small diameter particles. This product morphology lends support to the concept of the scavenging of homogeneously nucleated silicon.

Rohatgi, N. K.↗

Hydrogen-silicon carbide interactions

A study of the thermochemistry and kinetics of hydrogen environmental attack of silicon carbide was conducted for temperatures in the range from 1100 C to 1400 C. Thermodynamic maps based on the parameters of pressure and oxygen/moisture content were constructed. With increasing moisture levels, four distinct regions of attack were identified. Each region is defined by the thermodynamically stable solid phases. The theoretically stable solid phases of Region 1 are silicon carbide and silicon. Experimental evidence is provided to support this thermodynamic prediction. Silicon carbide is the single stable solid phase in Region 2. Active attack of the silicon carbide in this region occurs by the formation of gases of SiO, CO, CH4, SiH4, and SiH. Analysis of the kinetics of reaction for Region 2 at 1300 C show the attack of the silicon carbide to be controlled by gas phase diffusion of H2O to the sample. Silicon carbide and silica are the stable phases common to Regions 3 and 4. These two regions are characterized by the passive oxidation of silicon carbide and formation of a protective silica layer.

Eckel, Andrew J.↗

Hydrogen-silicon carbide interactions

A study of the thermochemistry and kinetics of hydrogen environmental attack of silicon carbide was conducted for temperatures in the range from 1100 C to 1400 C. Thermodynamics maps based on the parameters of pressure and oxygen/moisture content were constructed. With increasing moisture levels, four distinct regions of attack were identified. Each region is defined by the thermodynamically stable solid phases. The theoretically stable solid phases of region 1 are silicon carbide and silicon. Experimental evidence is provided to support this thermodynamic prediction. Silicone carbide is the single stable solid phase in region 2. Active attack of the silicon carbide in this region occurs by the formation of gases of SiO, CO, CH4, SiH4 and SiH. Analyses of the kinetics of reaction for region 2 at 1300 C show the attack of the silicon carbide to be controlled by gas phase diffusion of H2O to the sample. Silicon carbide and silica are the stable phases common to regions 3 and 4. These two regions are characterized by the passive oxidation of silicon carbide and formation of a protective silica layer.

Eckel, Andrew J.↗

Resistance of Silicon Nitride Turbine Components to Erosion and Hot Corrosion/oxidation Attack

Silicon nitride turbine components are under intensive development by AlliedSignal to enable a new generation of higher power density auxiliary power systems. In order to be viable in the intended applications, silicon nitride turbine airfoils must be designed for survival in aggressive oxidizing combustion gas environments. Erosive and corrosive damage to ceramic airfoils from ingested sand and sea salt must be avoided. Recent engine test experience demonstrated that NT154 silicon nitride turbine vanes have exceptional resistance to sand erosion, relative to superalloys used in production engines. Similarly, NT154 silicon nitride has excellent resistance to oxidation in the temperature range of interest - up to 1400 C. Hot corrosion attack of superalloy gas turbine components is well documented. While hot corrosion from ingested sea salt will attack silicon nitride substantially less than the superalloys being replaced in initial engine applications, this degradation has the potential to limit component lives in advanced engine applications. Hot corrosion adversely affects the strength of silicon nitride in the 850 to 1300 C range. Since unacceptable reductions in strength must be rapidly identified and avoided, AlliedSignal and the NASA Lewis Research Center have pioneered the development of an environmental life prediction model for silicon nitride turbine components. Strength retention in flexure specimens following 1 to 3300 hour exposures to high temperature oxidation and hot corrosion has been measured and used to calibrate the life prediction model. Predicted component life is dependent upon engine design (stress, temperature, pressure, fuel/air ratio, gas velocity, and inlet air filtration), mission usage (fuel sulfur content, location (salt in air), and times at duty cycle power points), and material parameters. Preliminary analyses indicate that the hot corrosion resistance of NT154 silicon nitride is adequate for AlliedSignal's initial engine applications. Protective coatings and/or inlet air filtration may be required to achieve required ceramic component lives in more aggressive environments.

Strangmen, Thomas E.↗

Low Cost Fabrication of Silicon Carbide Based Ceramics and Fiber Reinforced Composites

A low cost processing technique called reaction forming for the fabrication of near-net and complex shaped components of silicon carbide based ceramics and composites is presented. This process consists of the production of a microporous carbon preform and subsequent infiltration with liquid silicon or silicon-refractory metal alloys. The microporous preforms are made by the pyrolysis of a polymerized resin mixture with very good control of pore volume and pore size thereby yielding materials with tailorable microstructure and composition. Mechanical properties (elastic modulus, flexural strength, and fracture toughness) of reaction-formed silicon carbide ceramics are presented. This processing approach is suitable for various kinds of reinforcements such as whiskers, particulates, fibers (tows, weaves, and filaments), and 3-D architectures. This approach has also been used to fabricate continuous silicon carbide fiber reinforced ceramic composites (CFCC's) with silicon carbide based matrices. Strong and tough composites with tailorable matrix microstructure and composition have been obtained. Microstructure and thermomechanical properties of a silicon carbide (SCS-6) fiber reinforced reaction-formed silicon carbide matrix composites are discussed.

Singh, M.↗

Bond Sensitivity to Silicone Contamination

Currently during fabrication of the Space Shuttle booster rocket motors, the use of silicone and silicone-containing products is prohibited in most applications. Many shop aids and other materials containing silicone have the potential, if they make contact with a bond surface, to transfer some of the silicone to the substrates being bonded. Such transfer could result in a reduction of the bond strength or even failure of the subsequent bonds. This concern is driving the need to understand the effect of silicones and the concentration needed to affect a given bond-line strength. Additionally, as silicone detection methods used for materials acceptance improve what may have gone unnoticed earlier is now being detected. Thus, realistic silicone limits for process materials (below which bond performance is satisfactory) are needed rather than having an absolute no silicone permitted policy.

Caldwell, G. A.↗