Proposal # X9.01-8721
ISRU Chemical Vapor Deposition (CVD) as a low-energy,
high-performance metals extraction and fabrication substitute for
Heavy Industries in support of Manned Exploration.
Galactic Mining Industries, Inc. // sysRand Corporation
Denver, Colorado 80212-2922 719-930-3161
spaceguy2008@aol.com www.space-mining.com www.sysrand.com

 

Phase 1 Proposal

 

Parts:

  1. Table of Contents                                                                                1
  2. Identification and Significance of the Innovation                            1
  3. Technical Objectives                                                                           6
  4. Work Plan                                                                                            7
  5. Related R/R&D                                                                                    9
  6. Key Personnel and Bibliography of Directly Related Work           10
  7. Relationship with Phase 2 or Future R/R&D                                   16
  8. Company Information and Facilities                                                 18
  9. Subcontracts and Consultants                                                            18
  10. Potential Post Applications                                                                 19

11.    Similar Proposals and Awards                                                     --      19

12.    Letter of Commitment from sysRand                                          --     20

13.    Letter of Commitment from Colorado School of Mines            --      21

 

Part 2:  Identification and Significance of the Innovation -

In-Situ Resource Utilization (ISRU) is the key enabler of future space travel and space exploration and colonization. It is essential to use materials indigenous to the Moon to build and support exploration missions, Moon bases and other space infrastructure construction programs. Present-day estimates are that it costs about $50,000 to $100,000 ("Tom Sullivan, pers. comm.")to take a one kilogram mass from the Earth to the surface of the Moon. With such a prohibitive cost, it will be essential to learn to “live off the land” on the Moon. Effective and efficient utilization of in-situ resources on the Moon must be maximized to provide the exploration effort with the infrastructure, propellants, and other material requirements necessary for lunar operations. Cost control for lunar and other space operations can be achieved by the use of in-situ resources.

 

This proposal describes iron reduction technology and Chemical Vapor Deposition (CVD) technology which are together capable of converting lunar soils into things such as oxygen and steel products. Analogous CVD technologies are used by International Nickel (INCO) of Canada to process over 100,000,000 pounds of nickel annually. CVD technology in this respect is not a laboratory curiosity, but is a well developed industrial process with significant levels of success.

 

Lifting mass from the lunar surface to Low-Lunar-Orbit requires approximately 1.6 percent of the energy needed to launch identical mass from Earth to the same LLO. NASA will require in situ materials (indigenous to the Moon) in the manufacture of infrastructure needed for manned lunar, martian and other missions. ISRU-based Chemical Vapor Deposition has the potential to convert lunar regolith - hydrogen reduced feedstocks to finished precision hardware (engines), structural components (pressure vessels, hulls) and tools (wrenches, etc.).  CVD is also very synergistic with other potential ISRU processes such as fiberglass.

 

In situ iron from lunar soils will be extracted by first converting the FeO (ferrous oxide) content to Fe0 (ferrum) iron metal by hydrogen reduction. This iron metal content is then extracted (digested) using gaseous digestion techniques such as carbonyl chemistry. The resultant volatile iron-containing gaseous molecules are used in Chemical Vapor Deposition (CVD) manufacturing techniques. Vapor deposition of steel alloys can produce pressure vessels, structural elements, tools and tooling, fasteners, mirror contours and other products needed to support lunar and martian exploration – with minimal machining. CVD of steel alloys is performed on internal and external surfaces of inflatable contours, slush cast molds, ISRU-fiberglass forms, and other suitable mold/mandrel contour objects.

 

CVD has great potential to be a major enabler of deep space missions and will revolutionize the options available for mission planners to develop extended duration manned and robotic space exploration missions. Significantly larger (and redundant) payload masses originating from LLO or L1 (when compared with provisioning from Earth’s surface) will enable longer duration sustainable missions and larger scope of exploration of Mars and CisLunar Space.

 

CVD of various materials is commonplace in today’s industrial economy. Diamond coatings are produced using relatively high-temperature techniques. The semiconductor foundry industry uses CVD of metals and other materials in the manufacture of devices such as computers, detection equipment, optical devices, etc.. ISRU low-temp CVD of steel to make structural steel components made of steel will significantly simplify extraction and recycling processes and will develop into real competition for the prevailing high-temperature steel processing paradigms employed by terrestrial applications, slashing energy needs and smokestack environmental impacts by obsolescing energy-intensive processes.

ISRU CVD Research Program Objectives

Our space exploration program is dominated and restricted by two realities: gravity and the rocket equation.  Until costs associated with the launch of material and men are lowered significantly, we will have to be clever and innovative if we are to afford extensive space exploration.

The ISRU approach is to launch less materiél into space, and what does get shipped are mostly factories. Factories will be able to provide real advantages by multiplying the amount of product produced from utilization of limited payloads brought from earth. A factory launched from earth that is made up of component modules for example will be able to produce hundreds or thousands of times their initial weights of extracted oxygen for propellants and breathing and extracted iron for making steel products. Success lies with fabricating products outside of Earth’s gravity well. Such a place with resources, energy and practical proximity to Earth is the Moon, which is well-positioned as a literal stepping-stone to Mars, Jupiter and beyond.  It is on and near Luna that we will fashion products from rocks and soil.

Those products include fuel storage containers, pressure vessels, dewars, habitats, structural steel components, rocket engine components, motors, plumbing, valves, etc., which usually have mass and bulk and, when manufactured from indigenous space resources, allow us to avoid lifting them out of Earth’s gravity well. ISRU CVD will allow for fabrication of bulkheads with high-precision docks, hatches and seals with limited high-precision machining.  When mounted on a mandrel the bulkheads form the anchors for double-walled dewars which are wrapped with ISRU FiberGlass composites, plated-up with CVD inside and out, and later the insulating cavity is injected with ISRU Silicon Aerogel.  Applications include pressure vessels, habitats, structural components, fiberglass hybrids, thin-films, ceramics, spacecraft components including thrusters, etc.

 

Near Side                          Far Side

Figure 1.

This image shows results of the Lunar Prospector analysis for iron content in the lunar regolith. Orange is 12% to 16% iron, with yellow near 18% iron concentration. Blue areas represent between 2% and 6% iron. These percentages are estimates and should not be used as exact data. A more detailed mapping of iron is found later in this proposal.

 

ISRU CVD foundry operations will support LEO, MEO and GEO operations, and  ISRU-sourced metals and fuels will make a new CisLunar economy possible, thereby making robust missions to Mars and Jupiter logistically possible.  ISRU CVD steel foundry operations can deliver fuel and oxidizer storage tanks, enabling ISRU oxygen extraction and storage to continue apace.  It is clear that the fusion of ISRU CVD with other ISRU products, such as ISRU FiberGlass, will redefine space transport and exploration infrastructures.

The top-level view of the project is expected to be applied directly to planning for projects such as:

²      Specialized and custom manufacturing of spare and original parts for exploration,

²      Projection of heavy industries based on steel for lunar habitation, transport and industry.

The potential capabilities represented by developing indigenous lunar capabilities in steel foundry capabilities are staggering.  This would appear to be an economically-advantageous way to finesse the rocket equation and be second perhaps to ISRU-LOX as a valuable exploration resource. The project will focus on steel alloys for apples-to-apples comparisons of low-energy ISRU CVD processes to conventional high-energy terrestrial steel foundries which do not appear to be adaptable to space..

Comparative Analysis

As in any credible trade study, it is important to conduct a comparative analysis of conventional iron extraction and steel production methods versus our proposed low-temperature CVD processes.  We are convinced that we will be able to demonstrate energy and logistical features which are very favorable to low-temperature CVD in space. A necessary precursor for most ISRU is hydrogen reduction of lunar soils, a process which extracts oxygen from the minerals. The process temperatures for hydrogen reduction of lunar soils and ores are 700°C to 900°C. Once the iron is in a reduced state, carbonyl (CO) digestion techniques (low temperature CVD) extract the metallic iron content by formation of iron pentacarbonyl. This formation of iron pentacarbonyl, from iron and carbon monoxide, proceeds in the temperature range of 75°C to 100°C. Iron pentacarbonyl is a gas/liquid which is then stored for later use in depositing steel compositions. Iron pentacarbonyl decomposition (CVD) is performed in the temperature range of 175°C to 200°C.

Conventional extractive/conversion steel foundry processes employed in the steel industry here on the Earth are very energy-intensive. Typical steel foundry process temperatures are between 1500°C, and 2000°C. The much higher temperatures used in conventional steel foundry operations give a clear advantage thermodynamically to our low temperature CVD techniques. The steel foundry operations on Earth require truly massive plant, special (and massive) refractory vessels and other heavy types of equipment. Terrestrial iron foundry operations consume very large quantities of energy (electricity). The heavy equipment and large energy requirements make conventional steel foundry operations in space logistically impractical.

Presented here is an overview of the types of iron foundry operations on Earth which have been used or are used today on Earth in the manufacture of steel:

  1. Bottom-Blown Acid Process.  Also known as the Bessemer Conversion this process uses ambient air to provide Oxygen as the reactive/transport agent to remove contaminants from molten iron in a refractory siliceous vessel.  Since nitrogen is the majority constituent of the atmosphere, the efficiency of heating air is slashed by the nitrogen/oxygen ratio (~4:1).
  2. Basic Bessemer Process.  Also known as the Thomas-Gilchrest process uses a basic flux instead of acidic, for the refining and conversion in a basic-lined vessel.
  3. Open Hearth Process.  Also named for its inventor, Karl Wilhelm Siemens, this process employs iron ore to oxidize the carbon and other contaminants in the molten metal.
  4. Oxygen Steel Making.  This process employs gaseous oxygen which provides a substantial improvement in process efficiency over its predecessors by eliminating nitrogen from the loop.
  5. Electric Furnace Steel Making.  This process has two principal versions, Basic Oxygen and Electric Arc, using carbon-graphite electrodes in a controlled atmosphere.  This 1500°C process temperature is typical of these conversion processes although Electric Arc has been optimized to a 400KW / ton electrical consumption.

 

Another problem of all of these conventional iron foundry processes in the lunar context is that rich ores, often approaching 60% iron, are required to make the process work.  The relatively low iron concentrations in regolith are non-functional for these processes, even if all of the other energy and mass problems are solved.

Iron is found in the lunar regolith (soil) in the form of FeO (ferrous oxide). FeO is found in the lunar soils in concentrations as high as 18%. The Maria regions on the near side of the moon show concentrations of FeO in the range of 12% to 18%. The Highlands regions show iron concentrations in the range of 2% to 6%. These levels of iron are well below the 60% purity necessary for conventional iron foundry operations. Our proposed hydrogen reduction – carbonyl digestion processing of lunar regolith is able to extract the iron from these low iron lunar soils. Of course, the Maria regions are preferred over the lower iron concentrations of the Highlands regions of the Moon’s surface.

The oxygen extracted by the hydrogen reduction of FeO results in large quantities of oxygen, useable as breathable air and as propellant oxidizer. A lunar oxygen plant is a great place to locate a carbonyl iron foundry operation on the surface of the Moon. Operations by companies where oxygen is produced on the Moon will be allied with our iron extraction/fabrication facilities to the benefit of both companies.

"It should be obvious from the above discussion that the CVD process needs a feedstock rich in metallic Fe.  It has been assumed that this would be the waste material from one of several oxygen-production processes.  For the Phase 1 portion of this SBIR, we will produce our own feedstock in much the manner that it might be done on the Moon.  Portions of terrestrial ilmenite will be completely reduced to metallic Fe and TiO2 in a hydrogen reduction furnace.  Lunar ilmenite contains only Fe2+ whereas terrestrial ilmenite also contains Fe3+ in addition to the major Fe2+.  However, such readily available starting material is suitable for hydrogen reduction, especially where kinetics are not a concern.  Such an experiment has already been conducted by Taylor et al. (1993) where they used both synthetic FeTiO3 as well as Fe3+ bearing terrestrial ilmenite.  The resultant waste product from this ilmenite reduction will form the feedstock for experimentation with the CVD process."(per Larry Taylor)

 

"If this process provides a suitable feedstock for the CVD process, an experiment will be conducted to form metallic Fe from the lunar soil simulant JSC-1A.  This will not be difficult, although the reduction kinetics are much slower."(per Larry Taylor)

 

Taylor, L.A., E.A. Jerde, D.S. McKay, M.A. Gibson, C.W. Knudsen, and H.

Kanamori, 1993, Production of O2 on the Moon:  A lab-top demonstration of ilmenite reduction with hydrogen.  Lunar & Planetary Science XXIV, Lunar and Planetary Institute, Houston, 1411-1412.

Figure 2.

This map of the Moon was made from the data collected by the Clementine Mission in the mid ‘90s.  Paul Lucey and colleagues at the University of Hawaii are responsible for the algorithms that permitted the raw data from multi-spectral imaging cameras to be transposed into this fully quantitative Fe compositional map of the Moon.  They used the Apollo soil chemistry in their modeling.  Notice that the maria on the near-side of the Moon vary in FeO content from about 12 to 18 wt%, whereas the majority of the far-side terrain, the true lunar highlands, is about 5 wt% FeO.  The yellow-orange at the bottom of the far-side map is the South Pole-Aiken Basin, a massive crater some 2400 km in diameter, which has excavated rocks from beneath the highland crustal cover, resulting in an average of ~10 wt% FeO for this large area. (per Larry Taylor)

Benefits of the Proposed Technology to NASA Missions

The main benefit of carbonyl (CVD) lunar foundry operations is the ability to produce large quantities of oxygen and to multiply the resultant tonnages of useable steel produced when compared to the weight of the equipment and process gases brought from Earth to begin with. The equipment is used over and over again in the operation of the lunar foundry. The process gases are recycled over and over again, allowing great quantities of iron products and oxygen to be produced with the finite and limited quantities of gases brought from the Earth. The equipment brought from Earth will be supplemented and added onto by the production of pressure vessels and other items using lunar derived steel. The way to look at these operations is to see that the steel foundry will replicate and multiply itself many times.

 

Many missions which will require launching significant masses to distant orbits will be two orders of magnitude less expensive and technically simpler to achieve using lunar resources. Lifting manufactured goods from the lunar surface to Lunar-Low-Orbit (LLO) requires approximately 1.6 per cent of the energy needed to launch the same mass from Earth to the same Lunar Orbit. Since ISRU CVD has the potential to convert the iron component of hydrogen reduced lunar regolith to finished hardware and structural components it has the potential to be a major enabler of deep space missions.

The next significant energy savings is realized by the intrinsic efficiencies and relatively ‘cool’ CVD process temperatures. These replace many energy-intensive separation, alloying and ‘working’ processes of conventional metals processing.  No smelting, casting, hot-rolling, extruding, forging and heavy machining is necessary.  Only light machining will be needed for drills, taps, and cleanup of flashing.

Energy-savings in concert with simplified processes will make the implementation of a lunar CVD foundry a reality which, in turn, will make ambitious and robust missions a fact.

The majority of missions originate on Earth. The more mission support provided in space leverages all missions. Missions which are enlarged/provisioned by bootstrapping in lunar orbit with materials and equipment produced on the lunar surface can be much larger and better supplied than missions which get their supplies solely from Earth. In-Situ Resource Utilization enables long duration missions. This will mean larger crews and more equipment and supplies on Mars and in Mars Orbit.  This suggests that a Jupiter Mission can have greatly enhanced numbers of robotic probes to target the gas giant and her complement of moons and other objectives.  Lunar CVD Foundry will allow mission masses which are multiples of those economically achievable from Earth.

ISRU CVD will also be a foundational component of any CisLunar economy and infrastructure, reducing the launch masses required for Lunar settlement.  Some of this capacity will be employed in the manufacture of manufacturing facilities on the Moon and elsewhere.  ISRU CVD will also enhance the value of other indigenous processes, especially the FiberGlass family.

This project is a multi-disciplinary effort incorporating Chemical Engineering, Industrial Manufacturing, ISRU and Systems Architecture expertise.

 

Figure 3.  Nickel CVD Tractor seat mold 24” x 24”

Part 3: Technical Objectives -

In Phase One the project will investigate:

  1. deposition of simple iron and steel alloys resulting in one or more test articles from iron-containing gases. Planning for Phase 2 research will include defining an analysis matrix of experiments to be carried on;
  2. formation of iron pentacarbonyl by digestion of iron powders. Planning for Phase 2 research will include defining an analysis matrix of gaseous extraction (CVD digestion) experiments. Iron will be extracted in Phase 2 from various forms of iron containing materials (iron powder, lunar soil simulants, powdered scrap metal) – note: glassy agglutinates in real lunar regolith, which contain iron may need to be ground or crushed to expose iron oxide and iron metal for the hydrogen reduction and carbonyl digestion steps of the processing;
  3. the ISRU context, including the distribution of minerals in lunar regolith and their utility as feedstock for reaction with hydrogen to release iron metal from the mineral/glass phases;
  4. the process structures necessary for a comprehensive front-to-back industrial CVD production;
  5. the energy requirements for each step of a comprehensive process.

 

The chemical vapor deposition of steel alloys will be briefly examined in Phase 1. Extensive work involving the chemical vapor deposition of nickel from nickel tetracarbonyl has been performed, however less work has been done on iron chemical vapor deposition. Nonetheless, William Jenkin of the company has performed ground-breaking work in the past on the iron deposition process. There are examples in the literature involving the chemical vapor deposition of iron and many other metals from volatile metal containing vapors.

In this Phase 1 research program we will digest iron powder using the carbonyl process in order to demonstrate the process of metals digestion as expeditiously as possible, with minimal risk to schedule. In this initial iron powder digestion we must use hydrogen reduction to convert oxides on the surface of the iron powder to iron metal, whereas in the hydrogen reduction of lunar soil simulants the hydrogen reduction process must convert the FeO content to metallic iron. In Phase 2 we will actually use the reactor developed for digestion of iron powder to research the reduction/extraction of iron from more complex iron feedstocks such as lunar soil simulants and finely divided scrap steel.

The investigation, systems architecture and definition of the ISRU context for CVD implementation will be conducted in order to provide validation of CVD as a low-energy process flow in an exploration setting.  The key components of the validation process are 1) a mapping of the distribution of minerals in lunar regolith using the current data sets made available by Clementine and Lunar Prospector Orbiters, 2) an enumeration of the utility of lunar minerals as feedstock for various processing which will produce oxygen and leave an iron metal rich byproduct destined for carbonyl iron extraction 3) an enumeration of potential, and high-value CVD products, 4) identification of other industrial processes, such as fiberglass which are enhanced (or enabled) by the availability of lunar-based CVD, 5) identification of the missions which are substantially enabled by lunar-based CVD.

Further systems architecture will yield the process structures necessary for a comprehensive front-to-back definition of industrial CVD production.  This ‘drill down’ of the processes, the flow of product components and integration with other exploration systems will provide the roadmap for the next stage of development (Phase 2).  This task stream will also indicate the opportunities for automation and the specification of custom manufacturing from terrestrial design centers to lunar-based CVD plants.

The necessary energy requirements for each step of a comprehensive front-to-back process will be characterized to include efficiencies, types and locations of energy inputs, and regenerative recovery opportunities (if any). Comparison with conventional steel foundry operations will clearly show the CVD energy requirements to be significantly less than conventional steel manufacturing requirements. Reduced energy consumption in the CVD foundry operations will result in significant savings over conventional steel foundry operations.

Part 4:  Work Plan -

The systems architects will develop and define a Work Breakdown Structure which will provide some guidance to the researchers in anticipating their laboratory needs and order of research and development.

Research Components

Deposition

The company has purchased a kilogram of iron pentacarbonyl to use in initial chemical vapor deposition of iron coatings. The control of carbon content and oxygen content in the resultant iron coatings will be addressed to a limited extent in the Phase 1 research, while the deposition of controllable steel alloys will be done in the Phase 2 research. CVD of iron/steel is done with these gases in varying concentrations - carbon monoxide, water, ammonia, nitrogen monoxide, trifluorophosphine, and hydrogen. It is believed that some of the more complex iron-bearing volatile species may yield more controllable steel alloys (for example, iron carbonyl/nitrosyl). The research into the formation of iron-bearing volatile species from lunar simulants will set the groundwork for design of actual lunar ore and soil processing equipment. Deposition of iron/steel is done in the temperature range of 175°C to 200°C. To prevent unwanted deposition of coatings it is necessary to maintain surface temperatures of less than 125°C in the areas where deposition is not desired.

Digestion

The detailed work plan involves the use of special stainless steel apparatus for the containment of the appropriate process gas mixtures. Iron powder will have a thin iron oxide corrosion surface layer which must be converted back to metallic iron by hydrogen reduction, prior to the process of carbonyl digestion. In the case of reduction of iron in lunar regolith simulants it is possible to collect and measure the resultant water vapor to determine the amount of iron converted in the stimulant. The various gases to be used in the iron digestion itself include; carbon monoxide, nitrogen monoxide, trifluorophosphine, hydrogen, nitrogen and noble gases (He, Ne, Ar).  An experiment series will be conducted using these gases individually, and as mixtures. Carbonyl extraction (digestion) of iron occurs with temperatures of 75°-100°C and carbon monoxide pressures of 200 to 3000 psi. Recent work by Butler, Debelak and Roth (Vanderbilt Univ., Nashville, TN)

have shown that ilmenite reduction was accelerated in the presence of catalysts. The catalysts mentioned are KCL (100% to 170% increased rates) and K2CO3 (164% to 276% increased rates). The temperature of reaction is greater than 8070C. This 807oC temperature is probably the best temperature for hydrogen reduction.

Measurements of resultant gaseous molecules will be done by measuring the infrared spectrum, densities, melting point/boiling point and other measurable characteristics of the resultant iron-bearing gases.

Development Components

Lunar In-Situ Resource Inventory

Lunar regolith minerals and their distributions have been compiled and published. This information will be examined in order to identify the most promising regions capable of sustained steel production.  Recent distribution data from the Clementine and Lunar Prospector Orbiters are used to determine iron concentrations over the surface of the moon. There are oxygen-producing processes that can use highland regolith (i.e., ~5% FeO) and result in useable oxygen and iron metal containing waste. Taylor & Carrier (1992) compiled and reviewed 20 different processes for the production of oxygen on the moon. They examined the feedstocks, masses, number of steps and relative potential for success in the lunar logistical situation.

 

Figure 4.  Top-Level ISRU Flow Diagram

The ore concentrations will probably not be the sole determinant for mission planning although the numbers may tip the scale when competing landing and development sites are down-selected. The lunar mares areas are preferred in the current work.

Process Inventory

1.        Hydrogen reduction of iron oxide to produce iron metal.

2.        Carbonyl reaction with iron metal to produce iron pentacarbonyl.

3.        Iron pentacarbonyl decomposition reaction producing a metallic coating of iron/steel.

The company, Galactic Mining Industries, Inc., has assembled a team of individuals which have extensive expertise in the required subject matter areas. Bill Jenkin has 17 U.S. Patents and 45 years experience in developing nickel CVD technology for industry. We have compiled a bibliography of over 50 U.S. Patents which deal with the subject of CVD of metals. The PI, Richard Westfall has extensive chemistry/physics research experience. Larry Taylor is the company’s Moon Geophysicist with over 350 publications involving lunar characterization and mission planning. Larry provides the company with the expertise to select locations on the Moon with useable iron concentrations. Larry also has expertise with the specifics of lunar mineral composition/availability. With the compilation of background information and the hands on experience of the chemistry team, we feel confident we can develop state-of-the-art processes capable of manufacturing steel products on the Moon using material feedstocks of materials found on the Moon. The two principal research matrices are the hydrogen reduction/preparation of the iron feedstock materials and the conditions and chemistry of steel coating CVD processes. Optimization of these technologies will be completed in Phase 2. Phase 1 will begin with modest work product goals. Bill Jenkin has already produced a limited number of iron coatings in work for John Lewis of the University of Arizona.

Lunar soils and pyroclastic deposits which have undergone the hydrogen reduction and carbonyl iron extraction can undergo further processing to extract the metals left behind. The metals of interest which are left behind after hydrogen reduction/carbonyl extraction processing include oxides of: aluminum, silicon, titanium and others. We propose taking this waste stream and dissolving it in molten salt baths (FLINAK, 4540C mp, for example) where through electrodeposition these other metals can be extracted for other industrial uses. The aluminum can be converted into aluminum alkyls (tri-isobutyl aluminum, for example). The aluminum alkyl is useable as a CVD gas in aluminum CVD deposition. The silicon can be used to make photovoltaic devices. The titanium can be used to make spacecraft components and structural components. The topic of new uses for the lunar regolith will be looked at in Phase 2 to provide direction for future research.

Steel Compositions are Controlled

Steel deposited by CVD can be modified by varying the amount of carbon included in the lattice, by impurities and by post deposition anneal cycles. Management of the process gas composition during steel deposition can be used to vary the carbon content of deposited films. Additional gases added to the gas stream during the digestion step can result in iron bearing gaseous products which have a mixture of ligands. Instead of iron pentacarbonyl, it is possible to form iron carbonyl-nitrosyl complexes. These gases show promise for making exceptionally low carbon steel coatings. Impurities such as boron can be added to dramatically improve mechanical properties of deposited coatings. In the case of nickel CVD coatings it is possible to increase the yield strength of deposited films to near 200,000 psi. The report at the end of phase 2 will provide details of areas of research which can result in unique and valuable coating technologies.

Industrial Issues

The industrial issues are largely logistical in nature and it is essential to develop familiarity with issues such as process gas compatibilities, storage for feedstock queueing, process gas reuseabilities and interactions, along with product type differentiation.  Energy requirements have to be quantified.

Architect a Production Facility

For maximum versatility in product types it is important to architect a production facility based on rapid prototyping methods so that terrestrial design centers can transmit design files and remotely set up a production run.  Each line of a plant will be designed to handle a certain scale of component, that is a finite range of sizes, where some lines build parts up to the size of an electric motor rotor, others up to a rocket nozzle, and yet others up to a large I-Beam.  Each front-to-back process will produce identical parts in a custom mass-production format until the line is reprogrammed to build something else.  Figure 4 is a starting point for development of a fully-fledged architecture.

Integrate CVD into other Manufacturing Processes

The feasibility of integrating steel CVD with ISRU-derived fiberglass will be investigated in order to manufacture high-quality composite products.  A plate-up of fiberglass forms with CVD to produce metal matrix composites will enable the manufacture of a wide variety of products on a broad scale of sizes. In future work aluminum metal matrix composites could be an important product line.

CVD cladding applied to glass fibers will be a precursory stage for another manufacturing process: combustion synthesis. This is accomplished by the chemical fusing of dissimilar metals as a replacement for epoxy, an organic product which will likely not be available on the Moon due to the scarcity of Carbon and Nitrogen.

Part 5:  Related R/R&D -

Galactic Mining Industries, Inc. has extensive in-house experience with the chemical vapor deposition of coatings of Nickel, Iron, Aluminum, and other metals. William C. Jenkin is specifically responsible for over 45 years of development of chemical vapor deposition of metals. In 1990, William Jenkin worked for Dr. John Lewis of the University of Arizona to develop techniques for the chemical vapor deposition of iron from iron pentacarbonyl.

The history of this work is outlined by the mass of papers and patents enumerated elsewhere in this document.

Figure 5. Nickel CVD of a Complex                      Figure 6. Experimental Apparatus – Iron Digestion on

                 Shape                                                                      the left – Deposition Test Chamber on right 

Part 6:  Key Personnel and Bibliography of Directly Related Work –

Richard M. Westfall – President and Research Director of Galactic Mining Industries, Inc. – Project Principal Investigator                                   

Mr. Westfall has worked for the government and private industry. He founded Galactic Mining Industries, Inc. in 1989. Galactic Mining Industries, Inc. has operated as a think tank for the last 15 years and is dedicated to developing the technical and legal foundations of space colonization. The focus of Galactic Mining Industries, Inc. has been the development of technology to use space reaources and to develop the legal basis for mining claims and property ownership in space. With the president’s focus on return to the moon, Mr. Westfall has decided to apply the Carbonyl chemistry which his company has prepared to the extraction of Iron from Lunar ores and soils for the in situ resource utilization of Lunar materials on the moon.

Mr. Westfall has extensive experience in scientific research. He is currently a Professional Research Associate (PRA) at the Physics Department of the University of Colorado Boulder. Mr. Westfall is employed by Dr. Allen Hermann of the Superconductivity Laboratory in the Physics Department. He has been employed for eleven years at the University of Colorado. Employment at the University of Colorado Physics Department has involved work as a chemist/physicist in the areas of photovoltaics, metal-hydride batteries, and laboratory support. While working for the University of Colorado Physics Department he for a time worked at the Lockheed Martin Plant southwest of Denver on photovoltaic research. The work performed at Lockheed Martin included vacuum system maintenance and upgrade, x-ray diffraction, surface roughness measurements using the Atomic Force Microscope (AFM) in the Keck Lab of JILA at the University of Colorado in Boulder and other tasks. Atomic Force Microscopy resulted in a more complete understanding of such measurements in the characterization of the flatness/roughness of photovoltaic device substrates.

Mr. Westfall began his scientific career at the National Oceanic and Atmospheric Administration (NOAA) in Boulder Colorado while still a University of Colorado Student. Work at NOAA involved the observation of atmospheric phenomena, and computer modeling of the atmosphere.

Mr. Westfall began work on photovoltaics in 1977 as a CU student on the Denver campus, with follow up research under Dean Bob Rogers of the graduate school on the Boulder campus. The material focused on at this time was Cadmium Telluride as a p-type semiconductor/absorber.

Mr. Westfall worked at the Solar Energy Research Institute (SERI) in Lakewood Colorado in 1979 and 1980. SERI is now the National Renewable Energy Lab  (NREL). While at SERI Mr. Westfall worked in the Photovoltaics Research Branch, under Dr. Sigurd Wagner. Duties there included vacuum system operations, thin-film coatings of II-VI compounds Cadmium Telluride (CdTe) and Cadmium Sulfide (CdS), device measurements and materials characterization. Hall and Van der Pauw measurements were performed to characterize carrier properties of films.

Mr. Westfall started a company by the name of C.E.L. Systems Corporation to continue this photovoltaic research. While working as C.E.L. Systems Corporation, Mr. Westfall received 3 U.S. Patents, 4,632,736, 4,826,579, and 5,215,631. These patents disclose electrolytic techniques for the production of crystalline materials for use in electronic devices.

Photovoltaic research at the University of Colorado under Dr. Allen Hermann involved the semiconductor Copper Indium Gallium Selenide (CuInGaSe2).

Battery research performed at CU Boulder successfully produced Nickel Metal Hydride Rechargeable Batteries. This work entailed Alloy-Metallurgy, Electrochemistry, Electrode Construction, Hermetic Packaging, Furnace Construction and other tasks.

Process chemistry work was performed for a company in Schertz, Texas (near San Antonio) by the name of Texas Medical Instruments. Work was performed under a U.S. Army contract for the White Sands Missile Range.  Indium Gallium Arsenide (InxGa1-xAs) and Mercury Cadmium Telluride (HgxCd1-xTe) were the materials used in the manufacture of linear photoresistive infrared detector arrays for night vision systems on military vehicles. Work included materials characterization, photoresists, device delineation, contact application, semiconductor modeling, and other tasks.

Most recently, in work for his company Galactic Mining Industries, Inc. Mr. Westfall has been involved in detailed literature studies involving the chemical vapor deposition techniques which will be useful in the colonization of space using in situ resources. Mr. Westfall asked William C. Jenkin to be involved, and Mr. Jenkin joined the team over ten years ago. This work on chemical vapor deposition carried on by Mr. Westfall and Mr. Jenkin has laid the theoretical foundation for the processing of Lunar materials and the production of steel on the moon.

Subject Matter Expert, Chemistry -William C. Jenkin - Galactic Mining Industries, Inc.

William Jenkin has over 45 years experience in developing Chemical Vapor Deposition techniques for industry. As of 1959, only a laboratory technology to perform Nickel CVD had been developed, at Commonwealth Engineering Company of Ohio.  At this time Jenkin was hired to direct technology development and help find applications.  An outstanding discovery during this period was that adding Carbon Monoxide to the deposition gases in the amount of 10% of the Nickel Carbonyl enormously increased uniformity of deposits.  Union Carbide Corporation sponsored the program until 1965, when it backed out because commercial applications had not been found.  From 1965 to 1968, W. C. Jenkin Company set up a lab and secured research contracts and continued technology development.

In 1968, Jenkin convinced AKRON STANDARD MOLD, Company (of Akron, Ohio) to set up a division of the company to make Nickel shell molds for various industrial polymer molding operations, including automobile tire molds.  Jenkin was the division manager.  This was the first jump to an industrial technology.  By 1971, experimentation led to an important development of technology where a mandrel (made of epoxy bonded with a mix of coarse & fine Aluminum powders) was heated on the back side by jetted hot heat exchange fluid while Carbonyl vapors were directed to the important “shaped” side and decomposed and formed a Nickel metal deposit thereon.  Another division of the company incorporated the 1/8” thick Nickel shells typically made into structures for the molding of plastics.

By 1972, several shells up to 6 ft long and weighing up to 100 lbs had been made.  Sales were slow because it was a new product, but also due to the recession of 1972.  This company, as well as the division, were unprofitable so the division was sold to the PRESSURE CHEMICAL COMPANY of Pittsburgh, Pa., in 1972.  It operated at the same location in Akron until 1975.  The purchaser was a chemical manufacturer and also made the Nickel Carbonyl that was being used. 

The PRESSURE CHEMICAL COMPANY continued to sponsor manufacture of Nickel shell molds and sold them to several firms.  Production was moved to New Kensington in 1975 and continued.  The sponsor (Pressure Chemical Co.) in early 1976 had a catastrophic fire at their main plant in the heart of Pittsburgh, and due to financial problems sold the CVD operation to FORMATIVE PRODUCTS of Detroit, a company that manufactured molds for polymer molding.  The operation remained in New Kensington.  Jenkin continued as manager and reported to a man named Steigerwald.  At the end of 1967 production was going smoothly.  The division set up to make their own Nickel Carbonyl in 1977.  In the fall of 1977, Jenkin departed by mutual agreement, and his assistant took over management.

This division of FORMATIVE PRODUCTS continued under several changes of managers until 1991, all this time making many 1/8” thick Nickel shells, one as long as 14 ft.  In 1991, the then manager, Kenneth Mackenzie, carelessly toxically exposed himself to Nickel Carbonyl vapors and spent 2 months in the hospital.  The medical treatment available enabled him to recover completely, but the company shut down for two months and lost their customers.  The division had also been on the verge of being bought by a Japanese firm, who then backed off.

In 1992, the operation was liquidated, assisted by Jenkin.  Remember, however, that Nickel shells were made in production from 1971 through 1992. 

Meantime, about 1994, a Nickel shell CVD operation was set up in Toronto, Canada, by Mirotech, Ltd.  Jenkin supplied technology consulting services to this group.  They operated until about 2000, when the owner-manager sold out.  They made small shells (20” or smaller) for tooling use, plus experimental shells for other uses.

In 1965, INCO Ltd., of Canada set up a Nickel shell CVD manufacturing operation in Sudbury, Ontario.  Nickel Carbonyl was already being made on a production scale of hundreds of million pounds per year here, thus the refining plant supplied the Nickel Carbonyl.  Jenkin provided limited consulting services as they used mainly the technology developed by the Toronto firm, Mirotech Ltd.

About 1994, a Japanese owned firm, FET Engineering, Inc., set up a Nickel shell CVD manufacturing operation in Fallon, Nevada.  They obtained technology and consulting services from Kenneth Mackenzie, who had been shop foreman for my and all operations in Akron and New Kensington from 1969 through 1992.  The operation continued for several years under the name New American TEC.

In 1999, the Fallon, Nevada operation developed serious technical problems and Mackenzie was sick and not available.  Jenkin was called and asked to render services and correct their problems, but Jenkin had a consulting contract with INCO Ltd., that barred him from working for them.  The last Jenkin heard, the company never recovered.  The problems must have been solvable, however, because Nickel shells were produced in Akron and New Kensington from 1971 through 1992. 

In 2003, a company, Weber Tool and Technology of Midland, Ontario, Canada, set up a Nickel shell CVD operation.  They obtained the technology by hiring INCO Ltd employees from the INCO Sudbury, Ontario, Canada operation.  Weber had been buying the Nickel shells that INCO made and finished the processing and mounting in structures for production molding of plastics.  So they took over the CVD.

Other applications of Nickel CVD that made it to production are coating of Carbon fiber “tow” with Nickel, plus at the same facility, the making of Nickel foam for batteries (by coating polyurethane foam).  This technology developed by Jenkin is currently being done in Clydach, Wales, U.K.   Another firm, Powdermet, Inc., in Pacoima, California, is currently coating powders with CVD Nickel.

There is continuing activity in developing industrial uses of Nickel CVD technology by Metal Matrix Composites, Inc., a firm in Midway, Utah.  They are currently perfecting technology to make fine solid Nickel fibers (dubbed “nanofibers”) directly from Nickel Carbonyl.  Their work is supported by research contracts with the U.S. Air Force.  The fibers made are exceptional in their ability to increase the electrostatic conductivity of epoxy type polymers, which the Air Force says is widely important in military equipment.  The base technology here was developed by Jenkin and is covered by his US Patent 5,130,204.  This firm is also perfecting technology to Nickel coat Carbon nanofibers under an Air Force research contract, for which they foresee a huge market.

 

United States Patents -

U.S. Patent 455,227, June 30, 1891, Ludwig Mond, Process of Making Compounds of Nickel and Carbon Monoxide

U.S. Patent 480,405, August 9, 1892, Clemens Jones, Process of Treating Ores Containing Hydrated Sesquioxide of Iron

U.S. Patent 760,852, May 24, 1904, J. Dewar, Manufacture of Nickel Carbonyl

U.S. Patent 1,783,744, December 2, 1930, Alwin Mittasch, Manufacture of Iron Carbonyl

U.S. Patent 1,802,155, April 21, 1921, Martin Muller-Cunradi, Stable Iron Carbonyl Composition

U.S. Patent 1,816,122, July 28,1931, Alwin Mittasch, Manufacture of Iron Carbonyl

U.S. Patent 1,816,476, July 28, 1931, C.G. Fink, Manufacture of Double Walled Receptacles

U.S. Patent 1,836,732, December 15, 1931, L. Schlecht, Production of Finely Divided Metals

U.S. Patent 1,868,044, July 19, 1932, Leopold Brandt of Dortmund-Horde, Germany, Assignor to Vereineigte Stahlwerke Aktiengesellschaft, of Dusseldorf, Germany, Method of Producing IronCarbonyl

U.S. Patent 1,909,762, May 16, 1933, Christopher Maurice Walter Grier, Method for the Production of Nickel Carbonyl

U.S. Patent 2,004,534, June 11, 1935, Carl Miller, Separation of Metals

U.S. Patent 2,070,079, February 9, 1937, Charles Frederick Reed Harrison, Manufacture of Nickel Carbonyl

U.S. Patent 2,086,881, July 13, 1937, Leo Schlecht, Production of Nickel and Iron Carbonyls

U.S. Patent 2,105,037, January 11, 1938, Charles Frederick Reed Harrison, Manufacture of Nickel Carbonyl

U.S. Patent 2,167,112, July 25, 1939, C.F.R. Harrison, Preparation of Nickel Carbonyl

U.S. Patent 2,212,459, August 20, 1940, K.M. Simpson, Recovery of Nickel from Nickel Containing Iron Ores

U.S. Patent 2,245,503, June 10, 1941, Leo Schlecht, Manufacture of Nickel Carbonyl

U.S. Patent 2,254,158, August 26, 1941, K.M. Simpson, Process of Recovering Nickel

U.S. Patent 2,344,138, March 14, 1944, F.E. Drummond, Coating Method

U.S. Patent 2,378,053, June 12, 1945, Albert Edward Wallis, Production of Iron Carbonyl

U.S. Patent 2,395,999, March 5, 1946, J.V. Fill, Method for the Manufacture of Metal Carbonyls

U.S. Patent 2,548,727, April 10, 1951, John F. Kincaid, Preparation of Nickel Carbonyl

U.S. Patent 2,590,078, March 25, 1952, Arthur Maeder, Process for the Manufacture of the Carbonyls of Nickel

U.S. Patent 2,599,978, June 10, 1952, O.F. Davis, Process of Plating Carrier Particles with a Catalytic Metal

U.S. Patent 2,602,033, July 1, 1952, J.J. Lander, Carbonyl Process

U.S. Patent 2,612,440, September 30, 1952, G.O. Altmann, Production of Metal Carbonyl Powders of Small Size

U.S. Patent 2,619,433, November 25, 1952, O.F. Davis, Method of Gas Plating

U.S. Patent 2,631,948, March 17, 1953, H.G. Belitz, Method and Apparatus for Gas Plating

U.S. Patent 2,650,564, September 1, 1953, A.O. Fink, Dynamic Pyrolytic Plating Apparatus

U.S. Patent 2,653,879, September 29, 1953, Albert O. Fink, Bonding of Metal Carbonyl Deposits

U.S. Patent 2,656,283, October 20, 1953, A.O. Fink, Method of Plating Wire

U.S. Patent 2,656,284, October 20, 1953, H.A. Toulmin, Jr., Method of Plating Rolled Sheet Metal

U.S. Patent 2,657,457, November 3, 1953, H.A. Toulmin, Jr., Continuous Metal Production and Continuous Gas Plating

U.S. Patent 2,749,255, June 5, 1956, H.R. Nack, Method of Producing Metallized Glass Fiber Rovings

U.S. Patent 2,791,515, May 7, 1957, H.R. Nack, Metal Coated Glass Fiber and Method of its Formation

U.S. Patent 2,757,077, July 31, 1956, R. Lewis, Method for Recovering Metallic Values from Ores Containing Iron and Nickel

U.S. Patent 2,824,828, February 25, 1958, H.J. Homer, Colored Glass Fibers and Method of Producing the same

U.S. Patent 3,070,469, December 25, 1962, William C. Jenkin, Method of Encapsulation of Lithium Borohydride, Class 149-5, Commonwealth Engineering Company

U.S. Patent 3,086,881, April 23, 1963, William C. Jenkin, Method for Securing Adhesion of Gas Plating, Class 117-50, Union Carbide

U.S. Patent 3,158,499, November 24, 1964, William C. Jenkin,  Method of Depositing Metal Coatings in holes, tubes, crack, fissures & the like , Class 117-107.2, Union Carbide

U.S. Patent 3,160,517, December 8, 1964, William C. Jenkin Method of depositing metals & metallic compounds through-out the pores of porous body, Class 117-93.3, Union Carbide

U.S. Patent 3,167,831, February 2, 1965, William C. Jenkin, Gas Plated Metal Shell Molds & Patterns, Class 22-136, Union Carbide

U.S. Patent 3,176,356, April 6, 1965, William C. Jenkin, Method & Apparatus for Obtaining the Release of Gas Plated Deposits from Substrate Surfaces, Class 22-57.3, Union Carbide

U.S. Patent 3,196,003, July 20, 1965, William C. Jenkin, Process for Making Metal Strips & Sheets from Waste Metal, Class 75-62, Union Carbide

U.S. Patent 3,213,827, October 26, 1965, William C. Jenkin, Apparatus for Gas Plating Bulk Material to Metallize the Same, Class 118-49.5, Union Carbide

U.S. Patent 3,219,482, November 23, 1965, William C. Jenkin, Method of Gas Plating Adherent Coatings on Silicon, Class 117-213, Union Carbide

U.S. Patent 3,355,318, November 28, 1967, William C. Jenkin, Gas Plating Metal Deposits Comprising Boron, 117-107.2, Union Carbide

U.S. Patent 3,466,229, September 9, 1969, William C. Jenkin, Metallizing Plastics by Gas Plating (John R. Whitacre & W.C. Jenkin), Class 204-30, Union Carbide

U.S. Patent 3,554,880, January 12, 1971, William C. Jenkin, Process for Electroplating Polyoxymethylene Resins, Class 204-30, Dupont

U.S. Patent 3,619,288, November 9, 1971, Erhard Sirtl, Process for Precipitating a High Melting Metal-Contact Layer at Low Temperatures

U.S. Patent 4,187,200, February 5, 1980, William C. Jenkin, Method of Making a Supported Catalyst

U.S. Patent 4,606,941, August 19, 1986, William C. Jenkin, Deposition Metallizing Bulk Material by Chemical Vapor

U.S. Patent 4,632,736, December 30, 1986, Richard M. Westfall, Electrolytic Preparation of Tin

U.S. Patent 4,826,579, May 2, 1989, Richard M. Westfall, Electrolytic Preparation of Tin and Other Metals

U.S. Patent 4,938,999, July 3, 1990, William C. Jenkin, Process for Coating a Metal Substrate by Chemical Vapor Deposition using a Metal Carbonyl

U.S. Patent 5,008,160, April 16, 1991, William C. Jenkin, Method of Securing Adherent Coatings by CVD from Metal Carbonyls, and Articles Thus Obtained

U.S. Patent 5,130,204, July 14, 1992, William C. Jenkin, Randomly Dispersed Metal Fiber Mat

U.S. Patent 5,215,631, June 1, 1993, Richard M. Westfall, Electrolytic Preparation of Tin, other Metals, Alloys and Compounds

Published Articles and Non-Published Notes -

Forms of Iron Deposited by the Thermal Decomposition of Iron Pentacarbonyl in the Gas Phase, D. Beischer, Z. Electrochemie, 45, 310-13(1939)

Iron and Nickel by Carbonyl Treatment, R.M. Lewis, Journal of Metals, June 1958, 419-424

Twenty-Five Years Progress in Nickel Refining, The Industrial Chemist, December, 1959, 583-588

The Kinetics of Nickel Carbonyl Formation, W.M. Goldberger, I&EC Process Design and Development, 1962, 202-2090

Direct Synthesis of Trifluorophosphine Complexes of Cobalt as well as of Nickel and it’s Homologs, Thomas Kruck, Chem. Ber. 101, 138-142, (1968)

Phosphorus-Fluorine Compounds, Part XIV, Direct Synthesis of Tetrakis(fluorophosphine) Complexes of Zerovalent Nickel, John Nixon, J. Chem. Soc. (A), 1969, 1089-1091

Shortened Route to Pure Nickel, International Nickel Co., Chemical Engineering, November 24, 1975, 54-55

Letter from Dr. John Lewis, The University of Arizona, to William C. Jenkin, December 14, 1989, involving research on Iron CVD

Kinetic Study of the Chemical Vapor Deposition of Iron Films Using Iron Pentacarbonyl, Francisco Zaera, Langmuir, 1991, 7, 1188-1191

Analysis of Various Carbonyl Systems, F.A. Houle, J. Phys. Chem., 96, 10425 (1992)

Dissociation Dynamics of Core Excited Iron Carbonyl Nitrosyl, M. Simon – Lure, Univ. Paris-sud, Orsay, France; Serial Title: AIP Conference Proceedings, Issue: 258, 1992, pp. 323-31

Magnetic Properties of Vapor-Deposited Iron-Noble-Metal Multilayers, B.X. Liu, (Dept. of Mater. Sci. & Eng., Tsinghua Univ., Beijing, China); Physical Review B (Condensed Matter), v. 48, n. 14, 1 Oct. 1993, pp. 10276-83

JSC-1: A New Lunar Soil Simulant, David S. McKay, Engineering, Construction, and Operations in Space IV, American Society of Civil Engineers, pp. 857-866, 1994

Pattern Generation Below 0.1 micron by Localized Chemical Vapor Deposition with the Scanning Tunneling Microscope, A. de Lozanne, (Dept. of Phys., Texas Univ., Austin, TX, USA) Japanese Journal of Applied Physics, Part 1 (Regular Papers & Short Notes), v. 33, n. 12B, Dec. 1994, pp. 7090-3

Initial Stages of Fe Chemical Vapor Deposition onto Si(100), D.P. Adams, Physical Review Letters, Volume 74, Number 25, 19 June 1995, 5088-5091

Three-Dimensional Laser Chemical Vapor Deposition of Nickel-Iron Alloys, J.L. Maxwell, (Center for Integrated Electronics & Electronics Manufacture, Rensselaer Polytech. Inst., Troy, NY, USA); Advanced Laser Processing of Materials – Fundamentals and Applications. Symposium, 1996, pp. 601-606. Conference: Advanced Laser Processing of Materials – Fundamentals and Applications, 27-30 Nov. 1995, Boston, MA, USA. Publisher: Mater. Res. Soc., Pittsburgh, PA, USA

Atmospheric Laser Chemical Vapour Deposition of Iron-Carbon Composites, P.C. Chen, (Dept. of Chem., Spelman Coll., Atlanta, GA, USA;); Journal of Materials Science Letters, v. 14, n. 18, 15 Sept. 1995, pp. 1289-91

Infrared and Ultraviolet Laser-Assisted Deposition from Iron Pentacarbonyl, R. Alesandrescu, (Laser Dept., Inst. of Atomic Phys., Bucharest, Romania); Optical Engineering, v. 35, n. 5, May 1996, pp. 1377-82

Real-Time Volumetric Growth Rate Measurements and Feedback Control of Three-Dimensional Laser Chemical Vapor Deposition, J.L. Maxwell, (Lab. For Micromanufacturing, Louisiana Tech. Univ., Ruston, USA;); Applied Physics A (Materials Science Processing), v. A67, n. 3, Sept. 1998, pp. 323-9

Iron-Iron Oxide Composite Thin Films Prepared by Chemical Vapor Deposition from Iron Pentacarbonyl, T. Maruyama (Dept. of Chem. Eng., Kyoto Univ., Japan); Shinyashiki, Y. Source: Thin Solid Films, v. 333, n 1-2, 23 Nov. 1998, pp. 203-206

Preparation of Iron Nanoparticles by Chemical Vapor Condensation, C.J. Choi, (Korea Inst. of Machinery & Metals 66, Changwon, South Korea;); Materials Letters, v. 56, n. 3, Oct. 2002, pp. 289-94

Microstructure and Orientation of Iron Crystals by Thermal Chemical Vapor Deposition with Imposition of Magnetic Field, N. Yoshikawa, (Dept. of Metall., Tohoku Univ., Sendai, Japan;); Journal of Materials Research, v. 17, n. 11, Nov. 2002, pp. 2865-2874

 

Subject Matter Expert, Lunar Geochemist:  Dr. Lawrence A. Taylor

Distinguished Professor of Earth & Planetary Sciences

Director, Planetary Geosciences Institute        http://web.utk.edu/~pgi

University of         Tennessee                                             Telephone:  (865) 974-6013

Knoxville, TN 37996                                                            FAX: (865) 974-6022 e-mail:  lataylor@utk.edu

Expertise:  material scientist/geologist:  Lunar regolith & soil science and soil characterization; chemical, physical, & geotechnical properties of Lunar regolith; Lunar dust abatement; microwave heating of Lunar soil and Lunar simulants;  Oxygen-production processes; development of proper Lunar simulant; design and development of process for Lunar and martian regolith heating for the production of Oxygen; trafficability on Lunar surface: Lunar ‘ground truth’, etc.

EDUCATION

1958 – 1963            B.S. 1961; M.S. 1963; Indiana University, Bloomington, IN

1965 – 1968            Ph.D. 1968; Lehigh University, Bethlehem, PA; Geol. Sci./Materials Sciences

PROFESSIONAL EXPERIENCE

Dr. Taylor is a petrologist/geochemist who practices materials science on geologic materials.  He is a long-time “lunatic”, having worked on Lunar samples since the first return of materials during the Apollo 11 Mission.   He and his research group continue these studies ever enthusiastically today.  His early background in the mining industry and his initial education in economic geology and materials sciences have greatly aided his applications of Lunar science for the study of the In-Situ Resource Utilization (ISRU) of the Moon and Mars.  About 25% of his science and  and engineering publications have been concerned with the ISRU of Lunar materials.

1977 – present        Professor of Earth & Planetary Sci. - Univ. of Tennessee at Knoxville

1981 – 1982              Discipline Scientist & Program Manager, Planetary Materials Program,

                                  Solar System Explor. Div., NASA Headquarters, Washington, D.C.

1993 – present   Director, Planetary Geosciences Institute, Univ. of Tennessee at Knoxville

2004 – present   Univ. of Tennessee Distinguished Professor

AFFILIATIONS & AWARDS: 

Too many NASA Committees; UT Chancellor's Research Scholar, 1981-82: UT, Excellence In Research Award, ‘92-93; Award From French Government: Recognition Of Space Endeavors - 1993,  Dijon, France.;  Editor, Int’l Geology Review, 1995 – present; Indiana University Alumnus of the Year 1997-1998;  UT, Chancellor’s Research Scholar: 1998-1999; UT, Distinguished Professor, 2004.

SELECTED RELEVANT PUBLICATIONS (from >350 refereed publications)

Taylor, L.A., 1990, Hydrogen, Helium, and other solar-wind components in Lunar soil:  Abundances and predictions.  Proc. Space 90, Amer. Soc. Civil Engr., 68-77.

Taylor, L.A., and D.-H. Taylor, 1997, Considerations for a return to the Moon and Lunar Base site selection workshops.  Jour. Aerosp. Engr. 10, 68-79.

Pieters, C.M., Taylor, L.A., Noble, S.K., Keller, L.P., Hapke, B., Morris, R.V., Allen, C.C., McKay, D.S., and Wentworth, S., 2000, Space Weathering on Airless Bodies: Resolving a Mystery with Lunar Samples, Meteor. Planet. Sci. 35, 1101-1107

Taylor, L.A., Pieters, C.M., Keller, L.P., Morris, R.V.,  McKay, D.S., 2001, Lunar mare soils: Space weathering and the major effects of surface-correlated nanophase Fe. Jour. Geophys. Lett. 106, 27,985-27,999.

Taylor, L.A., McSween, H.Y., et al., 2002,  Martian meteortie Dhofar 019:  A new Shergottite, Meteor. Planet. Sci. 37, 1107-1128.

Anand, M., Taylor, L.A., Nazarov, M.A., Shu, J., Mao, H.-K., and Hemley, R.J., 2004, Space weathering on airless planetary bodies: Clues from the Lunar mineral hapkeite.  Proc. Nat. Acad. Sci., 101: 6847-6851.

Taylor, L.A., H.H. Schmitt, W.D. Carrier III, and M. Nakagawa, 2005, The Lunar dust problem: From liability to asset, AIAA, Proc. 1st Space Exploration Conf., Orlando, CD ROM.

Taylor, L.A., and T.T. Meeks, 2005, Microwave sintering of Lunar soil:  Properties, theory, and practice.  Jour. Aerosp. Engr. 18, 188-196.


Subject Matter Expert, Systems Architecture & Integration:  Gary ‘ROD’ Rodriguez

A nuts and bolts technologist from 'way back, Rod designs and develops products with electronics or intelligence content for the industrial world.  Raised to be a generalist and an artist in a long line of artists he is comfortable working in the oil patch, avionics, mining, systems, industrial automation and the like.  His customers have mass-produced his designs in oil well controllers installed on five continents, avionics flying in commercial and military fleets worldwide as well as the President's Helicopter Fleet, specialized test equipment and numerous other products. These devices are often, although not exclusively, embedded controllers operating in hazardous environments.

His life's passion is lost and ancient technologies.  His efforts in this arena include cross-disciplinary application of "out-of-context" technology, and discovery of math imbedded in archaic structures.  He holds a Bachelor's degree in Math and Computer Science, having grown up with computers since the sixties.  He is a VietNam-era veteran and a sometimes-current private pilot.

Applications Papers

The Development and Realization of a Silicon-60-Based Economy in CisLunar Space.  G.J. Rodriguez, Space Resources Roundtable II (2000),  #7031.

SILICON: The Foundations of a CisLunar Economy.  G.J. Rodriguez, sysRAND Corporation, W.A. Good, ESTS Inc., AIAA 2001-4662.

A World of Silicon, G.J. Rodriguez, sysRAND Corporation, W.A. Good, ESTS Inc., (publication pending).

Power Architectures for Lunar Resource Development, G.J. Rodriguez, Space Resources Roundtable V (2003).  (Google with search key "Power Architectures Lunar").

Power Lander for Support of Lunar Exploration and Development, C.R. Joyner, G.J. Rodriguez, SRR VI (2004), #6032.

Lunar and Martian Fiberglass as a Versatile Family of ISRU Value-Added Products, G.J. Rodriguez, SRR VI (2004), #6034.

Part 7:  Relationship with Phase 2 or Future R/R&D -

Work performed in Phase 1 of this program will be expanded in Phase 2 to perfect the extraction of Iron from Lunar simulants. Chemical Vapor Deposition of steel alloys and the precursor Hydrogen Reduction process will be central to the Phase 2 activity. Special emphasis will be paid to the levels of Carbon and Oxygen inclusion in the deposited coatings. Such coatings will be produced with less than 1% Carbon and only trace levels of Oxygen are acceptable. Inclusion of trace chemicals such as Boron are expected to increase the strength of these steel alloys in a similar fashion to properties achievable with Nickel CVD. Deliverables for Phase 2 include a complete how-to manual for lunar production of steel, along with samples of deposited steel coatings and small experimental pressure vessels made using this technology. Terrestrial markets for products made with this technology will also be defined in order to establish sales here on Earth for the company’s products.

Phase 2 research will include:

  1. Hydrogen reduction of iron powders, lunar soil simulants, ilmenite and finely divided scrap metal. Grinding may be necessary to improve the efficiency of hydrogen reduction. Real lunar soils contain glassy agglutinates which must be ground in order to expose iron oxide for the reduction step. Once reduced, the iron content must be exposed to carbon monoxide for the extraction/digestion process. Electrolysis of water is to be examined. The hydrogen produced by electrolysis is used in further reduction of more lunar soils. The oxygen is used for breathing and for propellant oxidizer.
  2. Carbonyl extraction (CVD digestion) of iron from hydrogen reduced samples of; iron powders, lunar soil simulants, ilmenite and finely divided scrap metal.
  3. Assembling a gas handling manifold system capable of delivering appropriate CVD gas mixtures by the selective mixing, sorting, separating and re-using of the individual constituent gas components.
  4. Deposition and alloying processes and methodologies will be examined, tested and documented.
  5. Industrial processes such as storage strategies for metal-laden gas/liquid feedstocks will be examined in detail and documented.
  6. Discovery of available derivative processes, practical flowrates, subsystem definition and interactions will be done toward a systems integration overview standpoint.
  7. Effort will be expended toward the adapting and integrating of low-energy CVD into ISRU activities such as infrastructure design and construction. FiberGlass materials and low-temperature CVD technologies to make composite materials will be applied to fulfill various infrastructure requirements and specifications.
  8. We will map diverse families of products foundational to various missions and efforts.
  9. CisLunar Infrastructures will be designed with ISRU CVD technology implications taken into account.
  10. Shipyards to support a robust exploration effort will be influenced by ISRU CVD technology.
  11. Fabrication of second-generation lunar facilities will be influenced by ISRU CVD technology.
  12. Systems Architecture, definition of a pilot plant with capacity, flows and feedstock needs, and partitioning into functional subsystems will be modeled.

 

 

Hydrogen reduction of various iron containing feedstocks will proceed until the production of water ceases. The water is collected in a cryo-trap or dessicant. The amount of water is then determined and the amount of oxygen extracted from the sample is calculated. Grinding of the sample may be necessary to increase the surface area of feedstock materials in order to maximize the amount of extractable oxygen and to maximize the available iron for conversion to the carbonyl (or other volatile iron-bearing species). 

Carbonyl extraction of metallic iron from the hydrogen reduced feedstock produces iron carbonyl volatile gas/liquid. This gas/liquid is collected for use in the deposition of iron/steel compositions. Both of the well known lunar simulants are to be employed: JSC-1 is a lunar simulant which is low in titanium, while MLS-1 is a lunar simulant with high titanium content. Once the iron is reduced with hydrogen gas, extraction of iron will be performed by the use of various gases which can act as ligands, attaching to the metallic iron atoms. Suitable ligands include carbon monoxide (CO), nitrogen monoxide (NO) and trifluorophosphine (PF3). Examples of volatile gaseous iron-bearing molecules include – Fe(CO)5 iron pentacarbonyl, Fe(NO)2(CO)2 iron nitrosyl carbonyl, Fe(PF3)5 iron penta-trifluorophosphine, and other combinations of  ligands.

Extensive development of processes for the chemical vapor deposition of steel alloys will be performed in Phase 2 research. Significant work has been done involving the chemical vapor deposition of nickel from nickel tetracarbonyl.

The remaining process components of mixing, sorting, separating and re-using process gases, definition of second-order industrial processes such as storage strategies for metal-laden gas feedstocks, available derivative processes, practical flowrates, subsystem definition and interactions are all of a type which will be precursors to design and development of  a pilot plant.

In Phase 2 the detailed work plan involves the use of the same special stainless steel apparatus for the containment of lunar simulant powdered materials and reduction process. Hydrogen will be introduced into the special apparatus of the company and through control of conditions such as temperature (700-900°C)  and hydrogen pressure, the iron portion of the lunar simulants will be reduced to the metallic state of Iron (Fe0).

Reduction of Iron will be detectable through the formation of water vapor in the exhaust gas stream from the extraction apparatus. The water vapor can be measured by either condensation in cold traps, or the measurement of weight increase of desiccant materials through which the exhaust gases are expelled.

Figure 5.  Nickel CVD Pontiac Fascia Mold

Part 8:  Company Information and Facilities -

Galactic Mining Industries, Inc. was first established in 1989 by Richard Westfall. Mr. Westfall has over the years continued to promote the idea of using ExtraTerrestrial resources in space exploration and colonization efforts. The company has had many individuals involved with the development of the plans and technologies to be used in these efforts. The company has established a relationship with individuals at the Colorado School of Mines (CSM) in Golden Colorado. The company has a consulting relationship with CSM. Through this consulting relationship we will use the laboratory facilities and capabilities of the Colorado School of Mines to fulfill the work defined in this Phase 1 proposal. Equipment will be provided by the company for the hydrogen reduction of lunar simulants, formation of iron carbonyl and other volatile compounds of iron, and for the Chemical Vapor Deposition of steel alloys. The Colorado School of Mines will provide consulting and other support to this effort. The Colorado School of Mines team members are discussed in Part 9 of this proposal.

Part 9:  Subcontracts and Consultants -

The Colorado School of Mines in Golden, Colorado will act as the 1/3 participation consultant to the company in this effort. Laboratory space and supporting capabilities will be provided by CSM during the 6 month duration of this research. Two groups at CSM will participate, the Metallurgy Dept. and the Center for Commercial Applications of Combustion in Space.

Dr. John J. Moore of the Metallurgy Dept. will act as a consultant in the planning and execution of research carried on in this effort. Dr. John J. Moore is the Head of the Metallurgical and Materials Engineering Department and Director of the Materials Science Program at the Colorado School of Mines. He is also the Director of the Advanced Coatings and Surface Engineering Laboratory. Dr. Moore has a BSc from the University of Surrey and a PhD., D. Eng. From the University of Birmingham in England.

Dr. Michael Duke of the Center for Commercial Applications of Combustion in Space (CCACS) will also serve in a consulting role in this effort. Dr. Duke, CCACS Research Professor and Director of CCACS, has extensive experience in the use of extraTerrestrial resources and hosts the annual Space Resources Roundtable at CSM. Dr. Duke has been involved with research on the use of Lunar resources for over 3 decades.

Bradley Blair of CCACS will serve in a consulting role in this effort.  Mr. Blair has worked on economic models for ExtraTerrestrial resource utilization and has extensive experience and contacts in space commercialization.

sysRAND Corporation is a Colorado ‘S’ Corporation since 1989, and majority-owned by Gary Rodriguez, cited in a previous section.  The company is SBA-certified as an 8(a) Minority-owned and Small Disadvantaged Business (SDB), and self-certified as a VietNam-Era Veteran-Owned Firm.  sysRAND is a Product Development company in ruggedized commercial / industrial arenas, including custom intelligent controls, military and commercial avionics and space commercialization and development. sysRAND’s customers have included Rockwell Collins, Raytheon, Time Products, Simtek, Unidot and others.  sysRAND Corporation has repeatedly demonstrated the ability to manage avionics, industrial controls and other R&D efforts, including one of the few truly modular parallel computer systems ever featured in the commercial market.  The company has earned ‘top vendor’ rating with one aerospace prime and has taken many projects from the whiteboard or ‘back of the envelope’ through design and into manufacturing.  Gary Rodriguez has submitted numerous papers on a variety of ISRU topics, introducing numerous original applications and process concepts to the field.  The company maintains facilities in Parker, Colorado and near the ‘Tech Center’ in Englewood, Colorado.

Part 10:  Commercial Applications Potential -

Low-temperature CVD is a low-energy process which is adaptable to dual-use, in the form of small-scale Terrestrial industrial plants. Commercial applications for these extractive and steel producing technologies include both Terrestrial and CisLunar markets. CVD Nickel production by INCO of Canada is greater than 100,000,000 pounds annually. Whether steel production using CVD will ever reach these levels of industrial application on Earth will be the subject of company trade and market studies.

CVD does not make use of conventional hot processes, resulting in small physical and environmental footprints and a miniscule power budget. Simple steel buildings serve as containment shells and inexpensive COTS ionic fire detectors provide additional safety features. CVD Digestion can be effectively used to recycle metals and those toxic materials typical of the electronics industry such as batteries.  The low-energy requirements, ability to recycle low-grade scrap, and small footprint of CVD production will encourage adoption throughout the world as a truly environmentally-friendly industry with moderate and manageable risks.

In space, the slow rate of deposition of steel coatings is offset by the economic advantage of CisLunar steel production at the top of the gravity well. The applicability of CVD technologies on Earth may be selective, since conventional steel production with the large stamping and sheet metal fabrication techniques are much more economical than CVD steel production. In contrast, CVD versatility makes it an outstanding candidate for CUSTOM MASS PRODUCTION – where small to large production runs are choreographed by proven CAD-to-product automation. CVD will excel whenever the product’s added value is relatively high, since CVD eliminates complex machining, hot rolling and other energy-intensive production steps required to manufacture high-tech parts from raw metals.

CVD industrial pallets can become an U.S. export to both the industrial and emerging third world. An actual market study for a turn-key CVD plant has yet to be conducted, although the potential in sales of such a modular plant is likely to be in terms of hundreds of millions to a few billions of dollars in annual sales. This would rapidly replace the large smokestack facilities seen worldwide and bring metal technologies to local markets in the third-world, which represents a ground-up injection of resources and wealth into the economies of nations and private organizations on Earth and throughout the solar system.

Part 11:  Similar Proposals and Awards –

Galactic Mining Industries, Inc. has previously submitted a similar topic as a NASA SBIR proposal in 2004. The company does not intend to submit this proposal to any other organization during the proposal review and acceptance period.

Galactic Mining Industries, Inc. has never received research monies for this work in the past.

sysRAND Corporation has previously submitted a 2005 NIAC proposal which sought to define industrial and systems architectures for integrating CVD and Silicon Fiberglass processes towards a Lunar infrastructure capable of supporting Shipyards in Lunar Orbit.  The proposal failed to include the advances in Lunar Exploration made in the last twenty years which support the extensive presence of Iron and other metals in the Lunar regolith.

sysRAND has never received research monies for this work.

 

 

 

 

sysRAND Corporation                              8(a)   SDB   VO

 

Space Applications and Commercialization
Avionics and Industrial Controls

 

 

1 September 2005

 

Richard Westfall

President

Galactic Mining, Inc.

4838 Stuart Street

Denver, CO  80212-2922

 

Dear Sirs,

 

This letter serves as a commitment that I will be available at the times required and for the purposes and extent of effort described in Galactic Mining's SBIR Phase I proposal: X9.01-8721

 

SBIR 2005-I: ISRU Chemical Vapor Deposition (CVD) as a low-energy,

high-performance metals extraction and fabrication substitute for Heavy Industries in support of Manned Exploration,

 

a technical proposal which concerns the proof-of-concept of Iron Vapor Digestion and Deposition and the realization and maturation of industrial processes for space applications.

 

We enthusiastically anticipate participating in this project, and thank you for providing this opportunity for us to apply our demonstrated capabilities to the nation’s space effort.

 

 

Sincerely,

Gary J. Rodriguez

President, Systems Architect

 

 

 

15306 Foxglove Ct  Parker  CO 80134  Voice 303.840.0797 Fax 303.840.0796  rod@sysrand.com

 


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