Development Study of Cartridge/Crucible Tube Materials

The limitations of traditional alloys and the desire for improved performance for components is driving the increased utilization of refractory metals in tile space industry. From advanced propulsion systems to high temperature furnace components for microgravity processing, refractory metals are being used for their high melting temperatures and inherent chemical stability. Techniques have been developed to produce near net shape refractory metal components utilizing vacuum plasma spraying. Material utilization is very high, and laborious machining can be avoided. As-spray formed components have been tested and found to perform adequately. However, increased mechanical and thermal properties are needed. To improve these properties, post processing thermal treatments such as hydrogen sintering and vacuum annealing have been performed. Components formed from alloys of tungsten, rhenium, tantalum, niobium, and molybdenum are discussed and a metallurgical analyses detailing the results are presented. A qualitative comparison of mechanical properties is also included

Progress in Fabrication of Rocket Combustion Chambers by VPS

Several documents in a collection describe aspects of the development of advanced materials and fabrication processes intended to enable the manufacture of advanced rocket combustion chambers and nozzles at relatively low cost. One concept discussed in most of the documents is the fabrication of combustion-chamber liners by vacuum plasma spraying (VPS) of an alloy of 88Cu/8Cr/4Nb (numbers indicate atomic percentages) -- a concept that was reported in "Improved Alloy for Fabrication of Combustion Chambers by VPS" (MFS-26546). Another concept is the deposition of graded-composition wall and liner structures by VPS in order to make liners integral parts of wall structures and to make oxidation- and thermal-protection layers integral parts of liners: The VPS process is started at 100 percent of a first alloy, then the proportion of a second alloy is increased gradually from zero as deposition continues, ending at 100 percent of the second alloy. Yet another concept discussed in one of the documents is the VPS of oxidation-protection coats in the forms of nickel-and-chromium-containing refractory alloys on VPS-deposited 88Cu/8Cr/4Nb liners

High-Temperature Crystal-Growth Cartridge Tubes Made by VPS

Cartridge tubes for use in a crystal growth furnace at temperatures as high as 1,600 deg. C have been fabricated by vacuum plasma spraying (VPS). These cartridges consist mainly of an alloy of 60 weight percent molybdenum with 40 weight percent rhenium, made from molybdenum powder coated with rhenium. This alloy was selected because of its high melting temperature (approximately equal.2,550 C) and because of its excellent ductility at room temperature. These cartridges are intended to supplant tungsten/nickel-alloy cartridges, which cannot be used at temperatures above approximately equal 1,300 C

High-Pressure Lightweight Thrusters

Returning samples of Martian soil and rock to Earth is of great interest to scientists. There were numerous studies to evaluate Mars Sample Return (MSR) mission architectures, technology needs, development plans, and requirements. The largest propulsion risk element of the MSR mission is the Mars Ascent Vehicle (MAV). Along with the baseline solid-propellant vehicle, liquid propellants have been considered. Similar requirements apply to other lander ascent engines and reaction control systems. The performance of current state-ofthe- art liquid propellant engines can be significantly improved by increasing both combustion temperature and pressure. Pump-fed propulsion is suggested for a single-stage bipropellant MAV. Achieving a 90-percent stage propellant fraction is thought to be possible on a 100-kg scale, including sufficient thrust for lifting off Mars. To increase the performance of storable bipropellant rocket engines, a high-pressure, lightweight combustion chamber was designed. Iridium liner electrodeposition was investigated on complex-shaped thrust chamber mandrels. Dense, uniform iridium liners were produced on chamber and cylindrical mandrels. Carbon/carbon composite (C/C) structures were braided over iridium-lined mandrels and densified by chemical vapor infiltration. Niobium deposition was evaluated for forming a metallic attachment flange on the carbon/ carbon structure. The new thrust chamber was designed to exceed state-of-the-art performance, and was manufactured with an 83-percent weight savings. High-performance C/Cs possess a unique set of properties that make them desirable materials for high-temperature structures used in rocket propulsion components, hypersonic vehicles, and aircraft brakes. In particular, more attention is focused on 3D braided C/Cs due to their mesh-work structure. Research on the properties of C/Cs has shown that the strength of composites is strongly affected by the fiber-matrix interfacial bonding, and that weakening interface realizes pseudo-plastic behavior with significant increase in the tensile strength. The investigation of high-temperature strength of C/Cs under high-rate heating (critical for thrust chambers) shows that tensile and compression strength increases from 70 MPa at room temperature to 110 MPa at 1,773 K, and up to 125 MPa at 2,473 K. Despite these unique properties, the use of C/Cs is limited by its high oxidation rate at elevated temperatures. Lining carbon/carbon chambers with a thin layer of iridium or iridium and rhenium is an innovative way to use proven refractory metals and provide the oxidation barrier necessary to enable the use of carbon/ carbon composites. Due to the lower density of C/Cs as compared to SiC/SiC composites, an iridium liner can be added to the C/C structure and still be below the overall thruster weight. Weight calculations show that C/C, C/C with 50 microns of Ir, and C/C with 100 microns of Ir are of less weight than alternative materials for the same construction

Plasma spray nozzle with low overspray and collimated flow

An improved nozzle for reducing overspray in high temperature supersonic plasma spray devices comprises a body defining an internal passageway having an upstream end and a downstream end through which a selected plasma gas is directed. The nozzle passageway has a generally converging/diverging Laval shape with its upstream end converging to a throat section and its downstream end diverging from the throat section. The upstream end of the passageway is configured to accommodate a high current cathode for producing an electrical arc in the passageway to heat and ionize the gas flow to plasma form as it moves along the passageway. The downstream end of the nozzle is uniquely configured through the methodology of this invention to have a contoured bell-shape that diverges from the throat to the exit of the nozzle. Coating material in powder form is injected into the plasma flow in the region of the bell-shaped downstream end of the nozzle and the powder particles become entrained in the flow. The unique bell shape of the nozzle downstream end produces a plasma spray that is ideally expanded at the nozzle exit and thus virtually free of shock phenomena, and that is highly collimated so as to exhibit significantly reduced fanning and diffusion between the nozzle and the target. The overall result is a significant reduction in the amount of material escaping from the plasma stream in the form of overspray and a corresponding improvement in the cost of the coating operation and in the quality and integrity of the coating itself

Improved Mo-Re VPS Alloys for High-Temperature Uses

Dispersion-strengthened molybdenum- rhenium alloys for vacuum plasma spraying (VPS) fabrication of high-temperature-resistant components are undergoing development. In comparison with otherwise equivalent non-dispersion-strengthened Mo-Re alloys, these alloys have improved high-temperature properties. Examples of VPS-fabricated high-temperature-resistant components for which these alloys are expected to be suitable include parts of aircraft and spacecraft engines, furnaces, and nuclear power plants; wear coatings; sputtering targets; x-ray targets; heat pipes in which liquid metals are used as working fluids; and heat exchangers in general. These alloys could also be useful as coating materials in some biomedical applications. The alloys consist of 60 weight percent Mo with 40 weight percent Re made from (1) blends of elemental Mo and Re powders or (2) Re-coated Mo particles that have been subjected to a proprietary powder-alloying-and-spheroidization process. For most of the dispersion- strengthening experiments performed thus far in this development effort, 0.4 volume percent of transition-metal ceramic dispersoids were mixed into the feedstock powders. For one experiment, the proportion of dispersoid was 1 volume percent. In each case, the dispersoid consisted of either ZrN particles having sizes <45 m, ZrO2 particles having sizes of about 1 m, HfO2 particles having sizes <45 m, or HfN particles having sizes <1 m. These materials were chosen for evaluation on the basis of previously published thermodynamic stability data. For comparison, Mo-Re feedstock powders without dispersoids were also prepared

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

Nano powders, components and coatings by plasma technique

Ultra fine and nanometer powders and a method of producing same are provided, preferably refractory metal and ceramic nanopowders. When certain precursors are injected into the plasma flame in a reactor chamber, the materials are heated, melted and vaporized and the chemical reaction is induced in the vapor phase. The vapor phase is quenched rapidly to solid phase to yield the ultra pure, ultra fine and nano product. With this technique, powders have been made 20 nanometers in size in a system capable of a bulk production rate of more than 10 lbs/hr. The process is particularly applicable to tungsten, molybdenum, rhenium, tungsten carbide, molybdenum carbide and other related materials

Better VPS Fabrication of Crucibles and Furnace Cartridges

An experimental investigation has shown that by (1) vacuum plasma spraying (VPS) of suitable refractory metal alloys on graphite mandrels, and then (2) heat-treating the VPS alloy deposits under suitable conditions, it is possible to fabricate improved crucibles and furnace cartridges that could be used at maximum temperatures between 1,400 and 1,600 C and that could withstand chemical attack by the materials to be heated in the crucibles and cartridges. Taken by itself, the basic concept of fabricating furnace cartridges by VPS of refractory materials onto graphite mandrels is not new; taken by itself, the basic concept of heat treatment of VPS deposits for use as other than furnace cartridges is also not new; however, prior to this investigation, experimental crucibles and furnace cartridges fabricated by VPS had not been heat treated and had been found to be relatively weak and brittle. Accordingly, the investigation was directed toward determining whether certain combinations of (1) refractory alloy compositions, (2) VPS parameters, and (3) heat-treatment parameters could result in VPS-fabricated components with increased ductility

Improved Blackbody Temperature Sensors for a Vacuum Furnace

Some improvements have been made in the design and fabrication of blackbody sensors (BBSs) used to measure the temperature of a heater core in a vacuum furnace. Each BBS consists of a ring of thermally conductive, high-melting-temperature material with two tantalum-sheathed thermocouples attached at diametrically opposite points. The name "blackbody sensor" reflects the basic principle of operation. Heat is transferred between the ring and the furnace heater core primarily by blackbody radiation, heat is conducted through the ring to the thermocouples, and the temperature of the ring (and, hence, the temperature of the heater core) is measured by use of the thermocouples. Two main requirements have guided the development of these BBSs: (1) The rings should have as high an emissivity as possible in order to maximize the heat-transfer rate and thereby maximize temperature-monitoring performance and (2) the thermocouples must be joined to the rings in such a way as to ensure long-term, reliable intimate thermal contact. The problem of fabricating a BBS to satisfy these requirements is complicated by an application-specific prohibition against overheating and thereby damaging nearby instrumentation leads through the use of conventional furnace brazing or any other technique that involves heating the entire BBS and its surroundings. The problem is further complicated by another application-specific prohibition against damaging the thin tantalum thermocouple sheaths through the use of conventional welding to join the thermocouples to the ring. The first BBS rings were made of graphite. The tantalum-sheathed thermocouples were attached to the graphite rings by use of high-temperature graphite cements. The ring/thermocouple bonds thus formed were found to be weak and unreliable, and so graphite rings and graphite cements were abandoned. Now, each BBS ring is made from one of two materials: either tantalum or a molybdenum/titanium/zirconium alloy. The tantalum-sheathed thermocouples are bonded to the ring by laser brazing. The primary advantage of laser brazing over furnace brazing is that in laser brazing, it is possible to form a brazed connection locally, without heating nearby parts to the flow temperature of the brazing material. Hence, it is possible to comply with the prohibition against overheating nearby instrumentation leads. Also, in laser brazing, unlike in furnace brazing, it is possible to exert control over the thermal energy to such a high degree that it becomes possible to braze the thermocouples to the ring without burning through the thin tantalum sheaths on the thermocouples. The brazing material used in the laser brazing process is a titanium-boron paste. This brazing material can withstand use at temperatures up to about 1,400 C. In thermal-cycling tests performed thus far, no debonding between the rings and thermocouples has been observed. Emissivity coatings about 0.001 in. (.0.025 mm) thick applied to the interior surfaces of the rings have been found to improve the performance of the BBS sensors by raising the apparent emissivities of the rings. In thermal-cycling tests, the coatings were found to adhere well to the rings