Optimizing the Electroforming Process to Enhance the Thickness Uniformity of Full Shell X-Ray Optics
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Electroform/plasma-spray laminates have shown promise as lightweight, strong, low-thermal-expansion components for xray optics. The basic idea is to exploit both (1) the well-established art of fabrication of optical components by replication and (2) plasma spraying as a means of reinforcing a thin replica optic with one or more backing layer(s) having tailorable thermomechanical properties. In x-ray optics as in other applications, replication reduces the time and cost of fabrication because grinding and polishing can be limited to a few thick masters, from which many lightweight replicas can thereafter be made. The first step in the fabrication of a component of the type in question is to make a replica optic by electroforming a thin layer of nickel on a master. Through proper control of the electroforming process conditions, it is possible to minimize residual stress and, hence, to minimize distortion in the replica. Next, a powder comprising ceramic particles coated with a metal compatible with the electroformed nickel is plasma-sprayed onto the backside of the nickel replica. Then through several repetitions and variations of the preceding steps or perhaps a small compressive stress, alternating layers of electroformed nickel and plasma-sprayed metal-coated ceramic powder are deposited. The thicknesses of the layers and the composition of the metal-coated ceramic powder are chosen to optimize the strength, areal mass density, and toughness of the finished component. An important benefit of using both electroforming and plasma spraying is the possibility of balancing stresses to a minimum level, which could be zero or perhaps a small net compressive stress designed to enhance the function of the component in its intended application.
The contracted activities for the procurement of 'Investigate Zero-Stress Replicated Optics' to support the AXAF-S x-ray spectrometer mirrors has been completed. To date four large Wolter I grazing incidence x-ray optical shells have been electroformed from nickel. The mirrors were fabricated utilizing each of two nickel alloy plated aluminum substrates twice. A wide variety of testing has been completed by NASA MSFC and UAH. This testing includes heat treatment control tests, subscale plating and fixture testing, alloy control of the electroless nickel, adhesion and release testing of the gold to electroless nickel, electroforming instrumentation and software and fabrication of subscale models. The full scale shells are one millimeter thick nickel electrodeposited over a thin gold layer which in turn has the optical surface on the inside. The optical surface is the replicate of the surface prepared on the substrate. Appendix I briefly outlines the fabrication process. Major objectives which were shared by UAH and MSFC include the design of facilities, equipment and tooling and procurement of materials and equipment. Process development followed with the fabrication of small scale pilot units. Procurement commenced immediately and equipment and materials were ordered to implement the fabrication of first surface full scale substrates (mandrels) and the second surface electroformed optical components. All principal objectives have been achieved. Inspection of the mirrors in visible and x-ray modes validates that the required performance and the quality can be achieved by an electroforming replication process. A very distinct progressive improvement has been achieved with each of the four mirrors produced. The final mirror exceeded the original goals and set an improved standard for flight hardware. The future goal of a 30 arc second resolution at 8 KEV x-ray appears to be achievable by this process when proper cleanliness and process control is utilized.
Because of their wave nature, thermal and cold neutrons can be reflected from smooth surfaces at grazing incidence angles, be reflected by multilayer coatings or be refracted at boundaries of different materials. The optical properties of materials are characterized by their refractive indices which are slightly less than unity for most elements and their isotopes in the case of cold and thermal neutrons as well as for x-rays. The motivation for the optics use for neutrons as well as for x-rays is to increase the signal rate and, by virtue of the optic's angular resolution, to improve the signal-to-noise level by reducing the background so the efficiency of the existing neutron sources use can be significantly enhanced. Both refractive and reflective optical techniques developed for x-ray applications can be applied to focus neutron beams. Typically neutron sources have lower brilliance compared to conventional x-ray sources so in order to increase the beam throughput the neutron optics has to be capable of capturing large solid angles. Because of this, the replicated optics techniques developed for x-ray astronomy applications would be a perfect match for neutron applications, so the electroformed nickel optics under development at the Marshall Space Flight Center (MSFC) can be applied to focus neutron beams. In this technique, nickel mirror shells are electroformed onto a figured and superpolished nickel-plated aluminum cylindrical mandrel from which they are later released by differential thermal contraction. Cylindrical mirrors with different diameters, but the same focal length, can be nested together to increase the system throughput. The throughput can be increased further with the use of the multilayer coatings deposited on the reflectivr surface of the mirror shells. While the electroformed nickel replication technique needs to be adopted for neutron focusing, the technology to coat the inside of cylindrical mirrors with neutron multilayers has to be developed. The availability of these technologies would bring new capabilities to neutron instrumentation and, hence, lead to new scientific breakthroughs. We have established a program to adopt the electroformed nickel replication optics technique for neutron applications and to develop the neutron multilayer replication technology.
A baseline configuration for a three section folding array, with retraction capability, was developed which would utilize electroformed aluminum hollowcore substrates and beryllium frames. The three section array was not fabricated because of difficulties with impurities in the aluminum electroforming bath. A procedure was developed for etching the copper mandrel from virtually any size of aluminum hollowcore panel in approximately one hour. Procedures were developed for analyzing the content of peroxide, water, total aluminum, and lithium-aluminum-hydride in an aluminum electroforming solution.
The capabilities and limitations of nondestructive evaluation methods were studied to detect and locate bond deficiencies in regeneratively cooled thrust chambers for rocket engines. Flat test panels and a cylinder were produced to simulate regeneratively cooled thrust chamber walls. Planned defects with various bond integrities were produced in the panels to evaluate the sensitivity, accuracy, and limitations of nondestructive methods to define and locate bond anomalies. Holography, acoustic emission, and ultrasonic scan were found to yield sufficient data to discern bond quality when used in combination and in selected sequences. Bonding techniques included electroforming and brazing. Materials of construction included electroformed nickel bonded to Nickel 200 and OFHC copper, electroformed copper bonded to OFHC copper, and 300 series stainless steel brazed to OFHC copper. Variations in outer wall strength, wall thickness, and defect size were evaluated for nondestructive test response.
Micromachining-and-electroforming process makes rigid metal meshes with cells ranging in size from 0.002 in. to 0.05 in. square. Series of steps involving cutting, grinding, vapor deposition, and electroforming creates self-supporting, electrically thick mesh. Width of holes typically 1.2 times cutoff wavelength of dominant waveguide mode in hole. To obtain sharp frequency-cutoff characteristic, thickness of mesh made greater than one-half of guide wavelength of mode in hole. Meshes used as high-pass filters (dichroic plates) for submillimeter electromagnetic waves. Process not limited to square silicon wafers. Round wafers also used, with slightly more complication in grinding periphery. Grid in any pattern produced in electroforming mandrel. Any platable metal or alloy used for mesh.
Nickel alloys are favored for electroforming precision components. Nickel phosphorous and nickel cobalt phosphorous are studied in this work. A completely new and innovative electrolytic process eliminates the fumes present in electroless processes and is suitable for electroforming nickel phosphorous and nickel cobalt phosphorous alloys to any desirable thickness, using soluble anodes, without stripping of tanks. Solutions show excellent performance for extended throughput. Properties include, cleaner low temperature operation (40 - 45 C), high Faradaic efficiency, low stress, Rockwell C 52 - 54 hardness and as much as 2000 N per square millimeter tensile strength. Performance is compared to nickel and nickel cobalt electroforming.
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.
This contribution explores an alternate route to forming pinhole-based poly-Si/dielectric/c-Si passivating contacts. The method utilizes controlled dielectric breakdown or electroforming to produce nanoscale pinholes in a thick (non-tunnelling) dielectric which, when annealed, allows dopant atoms to pass from doped poly-Si through the pinholes and into the c-Si wafer, forming conductive pathways. We show that the pinholes lose passivation after electroforming but can be repassivated with a forming gas anneal. N-type contacts show contact resistivities of ~20 mOhm-cm2, but p-type contacts are ~100 mOhm-cm2. Devices show a distinct kink in the J-V curve indicative of a barrier to transport. The method can be expanded to optimized dielectric passivation stacks (not just thin, single layers) and can be formed in parallel over the faces of the wafer in selected areas (pinholes only under the grid lines).
A regeneratively cooled thrust chamber has been designed and fabricated, consisting of an inner TD nickel liner which was spin formed, welded, and machined and an outer shell of electroformed nickel. Coolant channels were produced in the outer surface of the inner liner by the electric discharge machining process before electroforming the shell. Accessory manifolds and piping were attached by welding. Manufacturing processes employed are described.
Pertinent mechanical and physical properties of six high conductivity metals were determined. The metals included Amzirc, NARloy Z, oxygen free pure copper, electroformed copper, fine silver, and electroformed nickel. Selection of these materials was based on their possible use in high performance reusable rocket nozzles. The typical room temperature properties determined for each material included tensile ultimate strength, tensile yield strength, elongation, reduction of area, modulus of elasticity, Poisson's ratio, density, specific heat, thermal conductivity, and coefficient of thermal expansion. Typical static tensile stress-strain curves, cyclic stress-strain curves, and low-cycle fatigue life curves are shown. Properties versus temperature are presented in graphical form for temperatures from 27.6K (-410 F) to 810.9K (1000 F).
The replication of grazing incidence optics is reviewed. Electroform and epoxy replication are described and compared. It is concluded that for light weight and deep nesting, replication has a distinct advantage over direct production. The resolution of optics produced in this manner is however, limited to about 10 arc seconds; a typical value is 40 arc seconds. Epoxy replicated pieces tend to have better optical figures than electroformed optics, but the latter can be made thinner to make more deeply nested systems.
We are engaged in a program to develop focussing hard X-ray telescopes in a double conical or Wolter 1 geometry that function up to 100 keV by employing small graze angles and multilayer coatings. Directly polished substrates are not an option because they are too thick to be nested efficiently. The only alternative is to fabricate the very thin substrates by replication. Our objective is the production of integral cylindrical substrates because they should result in better angular resolution than segmented foil geometries. In addition, integral cylinders would be more resistant to possible stress from deep multilayer coatings than segmented ones. Both electroforming of nickel (method of SkX, JET-X, and XMM) and epoxy replication are under consideration. Both processes can utilize the same types of mandrels and separation agents- While electroforming can produce substrates that are thin, the high density of the nickel may result in high weight optics for some missions. For convenience, experimentation with replication and coating is being carried out initially on flats. Our replication studies include trials with gold and carbon separation agents. This paper reports on our efforts with epoxy replicated optics.
We have developed the electroformed-nickel replication process to enable us to fabricate light-weight hard-x-ray region. Two projects currently utilizing this technology are the production of over 250 r from 5 to 10 cm, for our HERO balloon payload, and 15- and 23-cm-diameter shells for a prototype module. The challenge for the former is to fabricate, mount, align and fly a large number of high-r constraints of a modest budget. For the latter, the challenge is to maintain high angular resolution shell thicknesses (100 micron) which make the shells extremely sensitive to electroforming stresses process does not degrade the ultra-smooth surface finish (approx. 3 A required for eventual multilayer c on these two programs.
We are investigating differential deposition as a way of correcting small figure errors inside full-shell grazing-incidence x-ray optics. The optics in our study are fabricated using the electroformed-nickel-replication technique, and the figure errors arise from fabrication errors in the mandrel, from which the shells are replicated, as well as errors induced during the electroforming process. Combined, these give sub-micron-scale figure deviations which limit the angular resolution of the optics to approx. 10 arcsec. Sub-micron figure errors can be corrected by selectively depositing (physical vapor deposition) material inside the shell. The requirements for this filler material are that it must not degrade the ultra-smooth surface finish necessary for efficient x-ray reflection (approx. 5 A rms), and must not be highly stressed. In addition, a technique must be found to produce well controlled and defined beams within highly constrained geometries, as some of our mirror shells are less than 3 cm in diameter.
A method has been developed for fabricating gratings on flat substrates, and then reproducing the groove pattern on a curved (concave or convex) substrate and a corresponding grating device. First, surface relief diffraction grating grooves are formed on flat substrates. For example, they may be fabricated using photolithography and reactive ion etching, maskless lithography, holography, or mechanical ruling. Then, an imprint of the grating is made on a deformable substrate, such as plastic, polymer, or other materials using thermoforming, hot or cold embossing, or other methods. Interim stamps using electroforming, or other methods, may be produced for the imprinting process or if the same polarity of the grating image is required. The imprinted, deformable substrate is then attached to a curved, rigid substrate using epoxy or other suitable adhesives. The imprinted surface is facing away from the curved rigid substrate. As an alternative fabrication method, after grating is imprinted on the deformable substrate as described above, the grating may be coated with thin conformal conductive layer (for example, using vacuum deposition of gold). Then the membrane may be mounted over an opening in a pressured vessel in a manner of a membrane on a drum, grating side out. The pressure inside of the vessel may be changed with respect to the ambient pressure to produce concave or convex membrane surface. The shape of the opening may control the type of the surface curvature (for example, a circular opening would create spherical surface, oval opening would create toroidal surface, etc.). After that, well-known electroforming methods may be used to create a replica of the grating on the concave or convex membrane. For example, the pressure vessel assembly may be submerged into an electro-forming solution and negative electric potential applied to the metal coated membrane using an insulated wire. Positive electric potential may be then applied to a nickel or other metal plate submerged into the same solution. Metal ions would transfer from the plate through the solution into the membrane, producing high fidelity metal replica of the grating on the membrane. In one variation, an adhesive may be deposited on the deformable substrate, and then cured without touching the rigid, curved substrate. Edges of the deformable substrate may be attached to the rigid substrate to ensure uniform deformation of the deformable substrate. The assembly may be performed in vacuum, and then taken out to atmospheric pressure conditions to ensure that no air is trapped between the deformable and rigid substrates. Alternatively, a rigid surface with complementary curvature to the rigid substrate may be used to ensure uniform adhesion of the deformable substrate to the rigid substrate. Liquid may be applied to the surface of the deformable substrate to uniformly distribute pressure across its surface during the curing or hardening of the adhesive, or the film may be pressed into the surface using a deformable object or surface. After the attachment is complete, the grooves may be coated with reflective or dielectric layers to improve diffraction efficiency.