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At least 19 records

One-step synthesis of dithiocarbamates from metal powders

Neutral metal dithiocarbamate complexes (M(NR2CS2)X) are well-known precursors to metal sulfides, a class of materials with numerous technological applications. We are involved in a research effort to prepare new precursors to metal sulfides using simple, reproducible synthetic procedures. We describe the results of our synthetic and characterization studies for M = Fe, Co, Ni, Cu. and In. For example, treatment of metallic indium with tetramethylthiuram disulfide (tmtd) in 4-methylpyridine (4-Mepy) at 25 deg C produces a new homoleptic indium (III) dithiocarbamate, In(N(CH3)2CS2)3(I), in yields of over 60 percent. The indium (III) dithiocarbamate was characterized by X-ray crystallography; (I) exists in the solid state as discrete distorted-octahedral molecules. Compound (I) crystallizes in the P1bar (No. 2) space group with lattice parameters: a = 9.282(1) A, b = 10.081(1) A, c = 12.502 A, alpha = 73.91(1) deg, beta = 70.21(1) deg, gamma = 85.8(1)deg, and Z = 2. X-ray diffraction and mass spectral data were used to characterize the products of the analogous reactions with Fe, Co, Ni, and Cu. We discuss both use of dithiocarbamates as precursors and our approach to their preparation.

Hepp, Aloysius F.

Plated Metal Powders for Electrode Pastes

Metal grains to be sintered precoated with frit metal. Coated metal powders used to make ink-like electrode pastes for printing and sintering electrode-fabrication process. Grains of base metal coated with lowmelting-point--, lead or tin-- by electroless deposition.

Bickler, D. B.

Container Prevents Oxidation Of Metal Powder

Sealed high-vacuum container holds metal powder required free of contamination by oxygen from point of manufacture to point of use at vacuum-plasma-spraying machine. Container protects powder from air during filling, storage, and loading of spraying machine. Eliminates unnecessary handling and transfer of powder from one container to another. Stainless-steel container sits on powder feeder of vacuum-plasma-spraying machine.

Woodford, William H.

Comparison of gamma-gamma Phase Coarsening Responses of Three Powder Metal Disk Superalloys

The phase microstructures of several powder metal (PM) disk superalloys were quantitatively evaluated. Contents, chemistries, and lattice parameters of gamma and gamma strengthening phase were determined for conventionally heat treated Alloy 10, LSHR, and ME3 superalloys, after electrolytic phase extractions. Several of long term heat treatments were then performed, to allow quantification of the precipitation, content, and size distribution of gamma at a long time interval to approximate equilibrium conditions. Additional coarsening heat treatments were performed at multiple temperatures and shorter time intervals, to allow quantification of the precipitation, contents and size distributions of gamma at conditions diverging from equilibrium. Modest differences in gamma and gamma lattice parameters and their mismatch were observed among the alloys, which varied with heat treatment. Yet, gamma coarsening rates were very similar for all three alloys in the heat treatment conditions examined. Alloy 10 had higher gamma dissolution and formation temperatures than LSHR and ME3, but a lower lattice mismatch, which was slightly positive for all three alloys at room temperature. The gamma precipitates of Alloy 10 appeared to remain coherent at higher temperatures than for LSHR and ME3. Higher coarsening rates were observed for gamma precipitates residing along grain boundaries than for those within grains in all three alloys, during slow-moderate quenching from supersolvus solution heat treatments, and during aging at temperatures of 843 C and higher.

Superalloys

Metal powder reactions in ball milling

On milling chromium powder in three metal chlorides and either chromium or nickel powders in ten organic liquids representative of nine different functional groups, the powders always reacted with the liquids and became contaminated with elements from them. The milled powders had specific surface areas ranging from 0.14 to 37 sq m/g, and the total contamination with elements from the milling liquid ranged from 0.01 to 56 wt%. In most milling runs, compounds resulting from substitution, addition, or elimination reactions formed in or from the milling liquid, and in most runs with organic liquids H2, CH4, and CO2 were generated.

Arias, A.

Ultrasonic characterization of microstructure in powder metal alloy

The ultrasonic wave propagation characteristics were measured for IN-100, a powder metallurgy alloy used for aircraft engine components. This material was as a model system for testing the feasibility of characterizing the microstructure of a variety of inhomogeneous media including powder metals, ceramics, castings and components. The data were obtained for a frequency range from about 2 to 20 MHz and were statistically averaged over numerous volume elements of the samples. Micrographical examination provided size and number distributions for grain and pore structure. The results showed that the predominant source for the ultrasonic attenuation and backscatter was a dense (approx. 100/cubic mm) distribution of small micropores (approx. 10 micron radius). Two samples with different micropore densities were studied in detail to test the feasibility of calculating from observed microstructural parameters the frequency dependence of the microstructural backscatter in the regime for which the wavelength is much larger than the size of the individual scattering centers. Excellent agreement was found between predicted and observed values so as to demonstrate the feasibility of solving the forward problem. The results suggest a way towards the nondestructive detection and characterization of anomalous distributions of micropores when conventional ultrasonic imaging is difficult. The findings are potentially significant toward the application of the early detection of porosity during the materials fabrication process and after manufacturing of potential sites for stress induced void coalescence leading to crack initiation and subsequent failure.

Tittmann, B. R.

Metallic Powder Core Tubular Wire Development for Additive Manufacturing

NASA Langley Research Center (LaRC) in Hampton, VA, and the Center for Welding, Joining, and Coating Research (CWJCR) in the Department of Metallurgical and Materials Engineering at the Colorado School of Mines (CSM) in Golden, CO, have collaborated for nearly fifteen years to develop metallic powder core tubular wire (PCTW) feedstock for additive manufacturing (AM) using electron beam deposition. The motivation for this development was to offset dealloying observed during deposition of titanium and aluminum alloy solid wire feedstock in the LaRC electron beam freeform fabrication (EBF3) system and to explore novel alloy compositions by tailoring the powder fill. EBF3 is a fusion-based AM process that is performed under vacuum and is consequently prone to vaporization loss of low vapor pressure alloying elements. Research spanning four graduate student research projects succeeded in developing the basic methodology to fabricate PCTW, the mass balance equations used to define the powder fill, microstructure control through particulate inoculation, and the feasibility of producing metal matrix composite materials.

powder core tubular wire (PCTW)

Surface fatigue and failure characteristics of hot forged powder metal AISI 4620, AISI 4640, and machined AISI 4340 steel spur gears

Spur gear surface fatigue endurance tests were conducted to investigate hot forged powder metal AISI 4620 and 4640 steel for use as a gear material, to determine endurance characteristics and to compare the results with machined AISI 4340 and 9310 steel gear materials. The as-forged and unground SISI 4620 gear exhibited a 10 percent fatigue life that was approximately one-fourth of that for AISI 9310 and less than one-half that for the AISI 4340 gears. The forged and finish ground AISI 4620 gears exhibited a 10 percent life, approximately 70 percent that of AISI 9310 and slightly better than that of AISI 4340. The AISI 4640 hot forged gears had less fracture toughness and slightly less fatigue life than the AISI 4620 test gears.

Townsend, D. P.

Surface fatigue and failure characteristics of hot-forged powder metal AISI 4620, AISI 4640, and machined AISI 4340 steel spur gears

Spur gear surface fatigue endurance tests were conducted to investigate hot forged powder metal AISI 4620 and 4640 steel for use as a gear material, to determine endurance characteristics and to compare the results with machined AISI 4340 and 9310 steel gear materials. The as-forged and unground AISI 4620 gear exhibited a 10 percent fatigue life that was approximately one-fourth of that for AISI 9310 and less than one-half that for the AISI 4340 gears. The forged and finish ground AISI 4620 gears exhibited a 10 percent life, approximately 70 percent that of AISI 9310 and slightly better than that of AISI 4340. The AISI 4640 hot forged gears had less fracture toughness and slightly less fatigue life than the AISI 4620 test gears.

Townsend, Dennis P.

Metallic Powder Core Tubular Wire (PCTW) Development for Additive Manufacturing

NASA Langley Research Center (LaRC) in Hampton, VA, and the Center for Welding, Joining, and Coating Research (CWJCR) in the Department of Metallurgical and Materials Engineering at the Colorado School of Mines (CSM) in Golden, CO, have collaborated for nearly fifteen years to develop metallic powder core tubular wire (PCTW) feedstock for additive manufacturing (AM) using electron beam deposition. The motivation for this development was to offset dealloying observed during deposition of titanium and aluminum alloy solid wire feedstock in the LaRC electron beam freeform fabrication (EBF3) system and to explore novel alloy compositions by tailoring the powder fill. EBF3 is a fusion-based AM process that is performed under vacuum and is consequently prone to vaporization loss of low vapor pressure alloying elements. Research spanning four graduate student research projects succeeded in developing the basic methodology to fabricate PCTW, the mass balance equations used to define the powder fill, microstructure control through particulate inoculation, and the feasibility of producing metal matrix composite materials. Metallic PCTW is comprised of a thin foil sheath wrapped around a powder blend. Fabrication of PCTW at CSM was accomplished using a tubular wire mill system to first bend a flat strip into a u-shaped cross section, deposit a powder fill, create a lap joint to seal the wire, and draw to final diameter. Powder management systems were developed to ensure uniform mixing of powder constituents and identify feed rates for optimum fill ratios. Processing parameters were successfully developed for titanium and aluminum alloy sheaths to account for material work hardening during drawing. Mass balance equations were developed to account for compositional contributions of the sheath and powder fill. PCTW composition can be adjusted through selection of the sheath or powder materials. PCTWs were successfully developed to offset Al loss in deposits of Ti-6-4 and Mg loss in Al 6061, resulting in deposits that were within the composition limits for each material. Ti-6-4 deposits were fabricated using PCTW comprised of commercially pure (CP) titanium sheath and a fill of pre-alloyed Ti-6-4 powder with additions of elemental Al and V powders. Additions of both elements were required to account for the CP Ti from the sheath, and Al was further enhanced to offset documented losses in EBF3 deposits. For Al 6061 deposits, composition was modulated through the choice of sheath material. The PCTW was made using an Al 5052 sheath to supplement Mg content and a fill composition of pre-alloyed 6061 powder with additions of Si and Cu.The slower solidification rate of the EBF3 process compared with laser powder bed fusion processes can lead to coarse-grained microstructures and mechanical property anisotropy. EBF3deposits of Ti-6-4 exhibited large epitaxially grown β grains, which result in degraded mechanical properties in the deposition direction. Microstructure refinement was achieved through a combination of electron beam modulation and the use of a PCTW designed for Ti-6-4 deposits and modified by the addition of powder made from Fe and B. Resulting deposits exhibited reductions in β grain size, α phase colony intercept length and lath width, and an increased volume fraction of β phase. The mechanism of microstructure refinement was related to precipitation of boride particles. Hardness testing confirmed that mechanical property anisotropy was reduced and an overall increase in hardness was achieved.Metal matrix composite (MMC) materials offer strength and stiffness benefits over unreinforced materials. Two methods were investigated using PCTW technology for producing Al 6061 basedMMC materials; the direct addition of SiC reinforcing particles and the in-situ generation of reinforcements through reaction synthesis of precursor powders. Al 6061 based MMCs reinforced with SiC exhibited particle clustering and formation of aluminum carbides during deposition. The application of a Ni coating to the SiC particles prior to incorporation into the powder fill eliminated aluminum carbide formation and aided particle distribution during deposition. Modulation of beam focus and power further reduced aluminum carbide formation and aided particle distribution. In reaction synthesis, precursor additions undergo an exothermic reaction during deposition to form new ceramic products, generally of finer scale than the initial precursor components. The product phases provide reinforcement in the MMC and act as nucleation sites during solidification, resulting in grain refinement, improved mechanical properties, and reduced susceptibility to solidification cracking. Higher tensile strength and stiffness were demonstrated in Al 6061 based MMCs with 2 vol% reinforcement. These combined research efforts demonstrate the potential of PCTW technology for customizing of alloy composition and achieving microstructure control. A manufacturing process for titanium- and aluminum-based PCTWs was developed based on iterative design, theoretical calculations, and empirical data. PCTW technology successfully mitigated Al loss from Ti-6-4 and Mg loss in Al 6061, resulted in grain refinement in Ti-6-4, and demonstrated fabrication of Al based MMCs

Marcia S Domack