Flexible Superconducting Interconnects Realized by Electrodeposition of Rhenium on an Aerosol Jet Printed Seed Layer
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Manzi, Jacob Richard [Sandia National Laboratories↗
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Advanced Materials and Fabrication Techniques for the Orion Attitude Control Motor
Rhenium, with its high melting temperature, excellent elevated temperature properties, and lack of a ductile-to-brittle transition temperature (DBTT), is ideally suited for the hot gas components of the ACM (Attitude Control Motor), and other high-temperature applications. However, the high cost of rhenium makes fabricating these components using conventional fabrication techniques prohibitive. Therefore, near-net-shape forming techniques were investigated for producing cost-effective rhenium and rhenium alloy components for the ACM and other propulsion applications. During this investigation, electrochemical forming (EL-Form ) techniques were evaluated for producing the hot gas components. The investigation focused on demonstrating that EL-Form processing techniques could be used to produce the ACM flow distributor. Once the EL-Form processing techniques were established, a representative rhenium flow distributor was fabricated, and samples were harvested for material properties testing at both room and elevated temperatures. As a lower cost and lighter weight alternative to an all-rhenium component, rhenium- coated graphite and carbon-carbon were also evaluated. The rhenium-coated components were thermal-cycle tested to verify that they could withstand the expected thermal loads during service. High-temperature electroforming is based on electrochemical deposition of compact layers of metals onto a mandrel of the desired shape. Mandrels used for electro-deposition of near-net shaped parts are generally fabricated from high-density graphite. The graphite mandrel is easily machined and does not react with the molten electrolyte. For near-net shape components, the inner surface of the electroformed part replicates the polished graphite mandrel. During processing, the mandrel itself becomes the cathode, and scrap or refined refractory metal is the anode. Refractory metal atoms from the anode material are ionized in the molten electrolytic solution, and are deposited onto the cathodic mandrel by electrochemical reduction. Rotation of the mandrel ensures uniform distribution of refractory material. The EL-Form process allows for manufacturing in an inert atmosphere with deposition rates from 0.0004 to 0.002 in./h (10.2 to 50.8 m/h). Thicknesses typically range from microns to greater than 0.5 in. (13 mm). The refractory component produced is fabricated, dependably, to within one micron of the desired tolerances with no shrinkage or distortion as in other refractory metal manufacture techniques. The electroforming process has been used to produce solid, nonporous deposits of rhenium, iridium, niobium, tungsten, and their alloys.
Gorti, Sridhar↗
Electrodeposition of Tungsten using Hydrotropic Agents
The current work sought to electrodeposit tungsten from water-based solutions. The work’s initial hypothesis was that methoxide reducing agents could be used to generate urea anions that could enable tungsten electrodeposition. Unfortunately, this hypothesis was found to be incorrect. However, the work led to the understanding that chemical reducing agents not only enable the electrodeposition of refractory metals like rhenium from water-based solutions, but that the key to plating tungsten in the future involves chemical reduction followed by stabilization with proper ligands. The work resulted in a manuscript under review at Inorganic Chemistry Communications on the discovered of L-histidine as a suitable reducing agent from rhenium electrodeposition. Rhenium-tungsten alloys with 4% tungsten were deposited. A technical advance was filed for the rhenium chemistry and parts were delivered to an internal Sandia customer that used the chemistry.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Technology status of a liquid fluorine-hydrazine rocket engine for a planetary spacecraft propulsion system
This paper discusses the current status of a fluorine-hydrazine rocket engine development program. Incorporation of a thin rhenium inner liner successfully eliminated corrosion of the carbon/carbon composite thrust chamber wall experienced during a previous test program. The results of hot-fire tests utilizing reworked and new injectors which provide increased fuel film cooling showed that thrust chamber head-end temperatures could be maintained at an acceptable level. As expected, the accompanying specific impulse performance loss requires optimizing the amount of film cooling to minimize the loss. The efforts to refine the rhenium liner vapor deposition process culminated in a carbon/carbon composite thrust chamber total test duration of 1008 seconds. Tasks presently in process include: (1) fabrication of two carbon/carbon composite thrust chambers incorporating 60:1 expansion ratio nozzles; (2) injector tests to optimize performance and cooling; (3) additional refinements to the rhenium lining process; and (4) fabrication and test of a freestanding rhenium thrust chamber.
Appel, M. A.↗
Advanced liquid rockets
A program to substitute iridium coated rhenium for silicide coated niobium in thrust chamber fabrications is reviewed. The life limiting phenomena in each of these material systems is also reviewed. Coating cracking and spalling is not a problem with iridium-coated rhenium as in silicide-coated niobium. Use of the new material system enables an 800 K increase in thruster operating temperature from around 1700 K for niobium to 2500 K for rhenium. Specific impulse iridium-coated rhenium rockets is nominally 20 seconds higher than comparable niobium rockets in the 22 N class and nominally 10 seconds higher in the 440 N class.
Schneider, Steven J.↗
Space Storable Rocket Technology program (SSRT). Option 1 program
The Space Storable Rocket Technology (SSRT) Option 1 Program was initiated in October 1991 after completion of the Basic Program. The program was restructured in mid-July 1992 to incorporate a Rhenium Technology Task and reduce the scope of the LO2-N2H4 engine development. The program was also extended to late February 1993 to allow for the Rhenium Technology Task completion. The Option 1 Program was devoted to evaluation of two new injector elements, evaluation of two different methods of thermal protection of the injector, evaluation of high temperature material properties of rhenium and evaluation of methods of joining the rhenium thrust chamber to the columbium injector and nozzle extension. In addition, critical experiments were conducted (Funded by Option 2) to evaluate mechanisms to understand the effects of GO2 injection into the chamber, helium injection into the main LO2, effect of the splash plate and effect of decreasing the aspect ratio of the 120-slot (-13a) element. The performance and thermal models were used to further correlate the test results with analyses. The results of the work accomplished are summarized.
Chazen, Melvin L.↗
Use of a Tantalum Liner to Reduce Bore Erosion and Increase Muzzle Velocity in Two-Stage Light Gas Guns
Muzzle velocities and gun erosion predicted by earlier numerical simulations of two stage light gas guns with steel gun tubes were in good agreement with experimental values. In a subsequent study, simulations of high performance shots were repeated with rhenium (Re) gun tubes. Large increases in muzzle velocity (2 - 4 km/sec) were predicted for Re tubes. In addition, the hydrogen-produced gun tube erosion was, in general, predicted to be zero with Re tubes. Tantalum (Ta) has some mechanical properties superior to those of Re. Tantalum has a lower modulus of elasticity than Re for better force transmission from the refractory metal liner to an underlying thick wall steel tube. Tantalum also has greater ductility than Re for better survivability during severe stress/strain cycles. Also, tantalum has been used as a coating or liner in military powder guns with encouraging results. Tantalum has, however, somewhat inferior thermal properties to those of rhenium, with a lower melting point and lower density and thermal conductivity. The present study was undertaken to see to what degree the muzzle velocity gains of rhenium gun tubes (over steel tubes) could be achieved with tantalum gun tubes. Nine high performance shots were modeled with a new version of our CFD gun code for steel, rhenium and tantalum gun tubes. For all except the highest velocity shot, the results with Ta tubes were nearly identical with those for Re tubes. Even for the highest velocity shot, the muzzle velocity gain over a steel tube using Ta was 82% of the gain obtained using Re. Thus, the somewhat inferior thermal properties of Ta (when compared to those of Re) translate into only very slightly poorer overall muzzle velocity performance. When this fact is combined with the superior mechanical properties of Ta and the encouraging performance of Ta liners/coatings in military powder guns, tantalum is to be preferred over Re as a liner/coating material for two stage light gas guns to increase muzzle velocity and reduce bore erosion.
Launchers↗
Performance of prototype thermionic converters.
Performance of thermionic converters, discussing voltage output, interelectrode spacing, rhenium- rhenium and rhenium-molybdenum electrode systems
ENERGY CONVERSION EFFICIENCY↗
Linear Free Energy Relationships Associated with Hydride Transfer From [(6,6'-R 2 -bpy)Re(CO) 3 H]: A Cautionary Tale in Identifying Hydrogen Bonding Effects in the Secondary Coordination Sphere
Here, six rhenium hydride complexes, [(6,6'-R 2 -bpy)Re(CO) 3 H] (bpy = 2,2'-bipyridine, R = OEt, OMe, NHMe, Me, F, Br), were synthesized. These complexes insert CO 2 to form rhenium formate complexes of the type [(6,6'-R 2 -bpy)Re(CO) 3 {OC(O)H}]. All the rhenium formate species were characterized using X-ray crystallography, which revealed that the bpy ligand is not coplanar with the metal coordination plane containing the two nitrogen donors of the bpy ligand but tilted. A solid-state structure of [(6,6'-Me 2 -bpy)Re(CO) 3 H] determined using MicroED also featured a tilted bpy ligand. The kinetics of CO 2 insertion into complexes of the type [(6,6'-R 2 -bpy)Re(CO) 3 H] were measured experimentally and the thermodynamic hydricities of [(6,6'-R 2 -bpy)Re(CO) 3 H] species were determined using theoretical calculations. A Brønsted plot constructed using the experimentally determined rate constants for CO 2 insertion and the calculated thermodynamic hydricities for [(6,6'-R 2 -bpy)Re(CO) 3 H] revealed a linear free energy relationship (LFER) between thermodynamic and kinetic hydricity. This LFER is different to the previously determined relationship for CO 2 insertion into complexes of the type [(4,4'-R 2 -bpy)Re(CO) 3 H]. At a given thermodynamic hydricity, CO 2 insertion is faster for complexes containing a 6,6'-substituted bpy ligand. This is likely in part due to the tilting observed for systems with 6,6'-substituted bpy ligands. Notably, the 6,6'-(NHMe) 2 -bpy ligand could in principle stabilize the transition state for CO 2 insertion via hydrogen bonding. This work shows that if only the rate of CO 2 insertion into [(6,6'-(NHMe) 2 -bpy)Re(CO) 3 H] is compared to [(4,4'-R 2 -bpy)Re(CO) 3 H] systems, the increase in rate could be easily attributed to hydrogen bonding, but in fact all 6,6'-substituted systems lead to faster than expected rates.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Thermal shock and erosion resistant tantalum carbide ceramic material
Ceramic tantalum carbide artifacts with high thermal shock and mechanical erosion resistance are provided by incorporating tungsten-rhenium and carbon particles in a tantalum carbide matrix. The mix is sintered by hot pressing to form the ceramic article which has a high fracture strength relative to its elastic modulus and thus has an improved thermal shock and mechanical erosion resistance. The tantalum carbide is preferable less than minus 100 mesh, the carbon particles are preferable less than minus 100 mesh, and the tungsten-rhenium particles are preferable elongate, having a length to thickness ratio of at least 2/1. Tungsten-rhenium wire pieces are suitable as well as graphite particles.
Honeycutt, L., III↗
Compatibility experiments of facilities, materials, and propellants for electrothermal thrusters
Experiments were performed to determine the compatibility of materials and propellants for electro-thermal thrusters. Candidate propellants for resistojet propulsion include carbon dioxide, methane, hydrogen, ammonia, and hydrazine. The materials being examined are grain stabilized platinum for resistojets for Space station and rhenium for high performance resistojets for satellites. Heater mass loss and deterioration of materials were evaluated. A coiled tube of platinum, with yttria dispersed throughout the base material to inhibit grain growth, was tested in carbon dioxide at 1300 C for 2000 hr. Post-test examination indicated the platinum-yttria heater would last over 100 000 hr with less than 10 percent mass loss. Short-term compatibility tests were conducted to test the integrity of the platinum-yttria in hydrogen, methane, carbon dioxide/methane mixtures and ammonia environments. In each of these 100 hr tests, the platinum-yttria mass change indicated a minimum coil life of 100 000 hr. Facility related effects were investigated in materials tests using rhenium heated to high tempertures. Vacuum facility water reduction was monitored using a mass spectrometer. In vacuum environments obtained using only diffusion pumping and those obtained with the assistance of cryogenic equipment there were mass gains in the rhenium heaters. These mass gains were the result of the high amount of oxygen and water contained in the gas. Propellant purity and preferred test facility environments are discussed.
Whalen, M. V.↗
Compatibility experiments of facilities, materials, and propellants for electrothermal thrusters
Experiments were performed to determine the compatibility of materials and propellants for electro-thermal thrusters. Candidate propellants for resistojet propulsion include carbon dioxide, methane, hydrogen, ammonia, and hydrazine. The materials being examined are grain stabilized platinum for resistojets for space station and rhenium for high performance resistojets for satellites. Heater mass loss and deterioration of materials were evaluated. A coiled tube of platinum, with yttria dispersed throughout the base material to inhibit grain growth, was tested in carbon dioxide at 1300 C for 2000 hr. Post-test examination indicated the platinum-yttria heater would last over 100,000 hr with less than 10 percent mass loss. Short-term compatibility tests were conducted to test the integrity of the platinum-yttria in hydrogen, methane, carbon dioxide/methane mixtures and ammonia environments. In each of these 100 hr tests, the platinum-yttria mass change indicated a minimum coil life of 100,000 hr. Facility related effects were investigated in materials tests using rhenium heated to high temperatures. Vacuum facility water reduction was monitored using a mass spectrometer. In vacuum environments obtained using only diffusion pumping and those obtained with the assistance of cryogenic equipment there were mass gains in the rhenium heaters. These mass gains were the result of the high amount of oxygen and water contained in the gas. Propellant purity and preferred test facility environments are discussed.
Whalen, M. V.↗
High-temperature gaseous oxygen/hydrogen thrusters for space station
Efforts to determine the critical technologies necessary for the development of a high-temperature GO2/GH2 thruster are reviewed, for space station applications. Two types of thrust chambers are evaluated: one operable at high temperature and the other incorporating regenerative cooling. The high temperature chamber made of rhenium requires minimum cooling of the chamber wall, however, an oxidation barrier should be incorporated to prevent the rhenium thruster from readily oxidizing. The use of rhenium brought about a lower cost, lower weight, and simplicity of fabrication. The igniter-injector, the chamber, the test facility, and the test program are discussed. It is found that an obtained flow split of 58/42 increased the thruster performance from 3893 N-s/Kg to 4030 N-s/Kg for the same chamber pressure and overall mixture ratio. An increase in performance is also observed when the core mixture ratio is lowered. The thruster was tested for 1.9 hrs with no well degradation.
Dowdy, M. W.↗
High Pressure Earth Storable Rocket Technology Program: Basic Program
The HIPES Program was conducted for NASA-LeRC by TRW. The Basic Program consisted of system studies, design of testbed engine, fabrication and testing of engine. Studies of both pressure-fed and pump-fed systems were investigated for N2O4 and both MMH and N2H4 fuels with the result that N2H4 provides the maximum payload for all satellites over MMH. The higher pressure engine offers improved performance with smaller envelope and associated weight savings. Pump-fed systems offer maximum payload for large and medium weight satellites while pressure-fed systems offer maximum payload for small light weight satellites. The major benefits of HIPES are high performance within a confined length maximizing payload for lightsats which are length (volume) constrained. Three types of thrust chambers were evaluated -- Copper heatsink at 400, 500 and 600 psia chamber pressures for performance/thermal; water cooled to determine heat absorbed to predict rhenium engine operation; and rhenium to validate the concept. The HIPES engine demonstrated very high performance at 50 lbf thrust (epsilon = 150) and Pc = 500 psia with both fuels: Isp = 337 sec using N2O4-N2H4 and ISP = 327.5 sec using N2O4-MMH indicating combustion efficiencies greater than 98%. A powder metallurgy rhenium engine demonstrated operation with high performance at Pc = 500 psia which indicated the viability of the concept.
Chazen, M. L.↗
Rhenium/Oxygen Interactions at Elevated Temperatures
The oxidation of pure rhenium is examined from 600-1400 C in oxygen/argon mixtures. Linear weight loss kinetics are observed. Gas pressures, flow rates, and temperatures are methodically varied to determine the rate controlling steps. The reaction at 600 and 800 C appears to be controlled by a chemical reaction step at the surface; whereas the higher temperature reactions appear to be controlled by gas phase diffusion of oxygen to the rhenium surface. Attack of the rhenium appears to be along grain boundaries and crystallographic planes.
Jacobson, Nathan↗
A Study of Tungsten-Technetium Alloys
Technetium is a sister element to rhenium and has many properties that are similar to rhenium. It is predicted that technetium will have about the same effects on tungsten as rhenium in regard to increase in workability, lowered ductile to brittle transition temperature, and improved ductility. The objectives of the current work are to recover technetium from fission product wastes at Hanford Atomic Products Operation and reduce to purified metal; prepare W-Tc alloys containing up to 50 atomic% Tc; fabricate the alloy ingots to sheet stock, assessing the effect of technetium on workability; and perform metallurgical and mechanical properties evaluation of the fabricated alloys. Previous reports have described the separation and purification of 800 g of technetium metal powder, melting of technetium and W-Tc alloys, and some initial observation of the alloy material.
Maltz, J. W.↗
A Study of Tungsten-Technetium Alloys
Technetium is a sister element to rhenium and has many properties that are similar to rhenium. It is predicted that technetium will have about the same effects on tungsten as rhenium in regard to increase in workability, lowered ductile to brittle transition temperature, and improved ductility. The objectives of the current work are to recover technetium from fission product wastes at Hanford Atomic Products Operation and reduce to purified metal; prepare W-Tc alloys containing up to 50 atomic% Tc; fabricate the alloy ingots to sheet stock, assessing the effect of technetium on workability; and perform metallurgical and mechanical properties evaluation of the fabricated alloys. Previous reports have described the separation and purification of 800 g of technetium metal powder, melting of technetium and W-Tc alloys, and some initial observation of the alloy material.
Maltz, J. W.↗
High-Performance Bipropellant Engine
TRW, under contract to the NASA Lewis Research Center, has successfully completed over 10 000 sec of testing of a rhenium thrust chamber manufactured via a new-generation powder metallurgy. High performance was achieved for two different propellants, N2O4- N2H4 and N2O4 -MMH. TRW conducted 44 tests with N2O4-N2H4, accumulating 5230 sec of operating time with maximum burn times of 600 sec and a specific impulse Isp of 333 sec. Seventeen tests were conducted with N2O4-MMH for an additional 4789 sec and a maximum Isp of 324 sec, with a maximum firing duration of 700 sec. Together, the 61 tests totalled 10 019 sec of operating time, with the chamber remaining in excellent condition. Of these tests, 11 lasted 600 to 700 sec. The performance of radiation-cooled rocket engines is limited by their operating temperature. For the past two to three decades, the majority of radiation-cooled rockets were composed of a high-temperature niobium alloy (C103) with a disilicide oxide coating (R512) for oxidation resistance. The R512 coating practically limits the operating temperature to 1370 C. For the Earth-storable bipropellants commonly used in satellite and spacecraft propulsion systems, a significant amount of fuel film cooling is needed. The large film-cooling requirement extracts a large penalty in performance from incomplete mixing and combustion. A material system with a higher temperature capability has been matured to the point where engines are being readied for flight, particularly the 100-lb-thrust class engine. This system has powder rhenium (Re) as a substrate material with an iridium (Ir) oxidation-resistant coating. Again, the operating temperature is limited by the coating; however, Ir is capable of long-life operation at 2200 C. For Earth-storable bipropellants, this allows for the virtual elimination of fuel film cooling (some film cooling is used for thermal control of the head end). This has resulted in significant increases in specific impulse performance (15 to 20 sec). To determine the merits of a powder rhenium thrust chamber, Lewis On-Board Propulsion Branch directed TRW (under the Space Storable Rocket Technology Program and the High Pressure Earth Storable Rocket Technology Program) to design, fabricate, and test an engineering model to serve as a technology demonstrator.
Biaglow, James A.↗