brea Se ——— — / _ Technical Note N-4h6 St ‘PR EFFECTS OF THE DEEP-OCEAN ENVIRONMENT ON MATERTALS =- A PROGRESS REPORT 2a Dp) U. S. NAVAL CIVIL ENGINEERING > california a N 4 “4 NS WS J tfeck (p AUG 1 3 962 EFFECTS OF THE DEEP-OCEAN ENVIRONMENT ON MATERIALS = A PROGRESS REPORT Task Y-FO15-01-001(c) Type C by Kenneth O. Gray OBJECT OF TASK To develop systems and techniques for construction in deep-ocean areas. The task envisages obtaining all necessary data to permit engineers to design, construct, and install required structures and equipment in deep- ocean areas. ABSTRACT A research program to determine what materials are suitable for use in the construction of deep-ocean structures and facilities is delineated. The program, initiated in August 1959, involves (1) the exposure of a wide variety of constructional materials in deep-ocean environments, and (2) the exposure of companion specimens in laboratory-simulated deep-ocean environments. ‘A Submersible Test Unit carrying 1318 specimens of 301 different materials was placed on the ocean floor on 29 March 1962 in 5300 feet of water for an exposure period of 6 months. Five additional units are proposed, one each for 12 and 24 months submersion at 6000 feet and one each for 6, 12, and 24 months submersion at 12,000 feet on the ocean floor. A system of medium sized (9-inch ID) pressure vessels capable of simulating various aspects of the deep-ocean environment, with a pressure range from zero to 20,000 psi, has been fabricated and will be in operation early in FY-63. A large (18-inch ID) pressure vessel with similar capabilities is under procurement and is expected to be in operation in FY-63. CONTENTS page INMUROW WICH SG O66 6 0/6) 66 36 66 66 66 6 0.0 6 000 69 Go dk SCOPE OF DEEP-OCEAN MATERIALS INVESTIGATION ....+-+++e-+-e-e+-e-e-L1 EXPERIMENTAL ENVGRONMENTS . . « . <6 «© 6s 60 © © © © © 2 oe DSS ANehoere havalgtoyam=oheyso Go O06 ao 0 O00 O10 0 00 6 6.01016 4 66 Laboratory-Simulated Environments. . . « « « « « « « «© «© e « « e Shallow-Water Environments . ....«.+.+.-«e-«+-+e¢e-+ © « © @ MATERGPALS LOPE RPE N VES TiGARED. jill ello) lc) le 6) © <2 (eile! ee) (el) EXPHRUMEN TAT METH ODSIs) ter letiter Neliies elle! teil e! veilsofilel leo 6) (elle ver lof oll ollie (fel le) Unstressed Specimen Experiment ...+..o-+«.-+.eeeece#eee e Stressed Specimen Experiment ....e.o+«+ce«ceeee-eecee Syseskwsia eyiehlales 6 G06 6.6 6606060 0006009606 6 0 Cc Evaluation of Specimens after Exposure to Test Environment .. . OCEAN ENVIRONMENT EXPERIMENTS . » « « » « « © © © © © © © © © © @ © © Oo O© Oo @©@ N OW OW Ww WH WT Ww ww Deep=Water Experiments. < cs «6 « © «© « 9 « « © © «© 6 «© © = 1%) Shallow-Water Experiments. . ». + © © « » e « © © e e © © © « » =) Oo LABORATORY-SIMULATED DEEP-OCEAN ENVIRONMENT EXPERIMENTS . - «© « « « = 1S) IPRORGAM aU arireluuecttens ctitel ael),/e tre cus) eh, volte Mikel mente etal Siero hie lel 9) roipellevitte Re i Deep-Ocean Laboratory Equipment. . . -« » « e e © © ¢e © « « © o 9 a Oo DEEP-OCEAN BIBLIOGRAPHY FILE. « - o » « © « © © # © © «@ FUTURE PLANS ° e es e iJ J * e e e e e oe c.) ° e o e ° e € e o nm ° e © eo e 18 Ocean Environment Research Facilities. . - +++ «-+«+e+-ee 18 iaboraLvorywResearchwmacdlatiesme 6. si ciilel lst voiel e) eileleilcl iis lewis Werle, ll OT ivi 0301 0040198 CONTENTS (Cont'd) Ocean Environment Research. Laboratory-Simulated Ocean Environment Research REFERENCES . ° ° © o e ° ° © e ° ° ° C) o © ° e ° a © C) APPENDIX = Specimens on STU Placed 29 March 1962 . . TABLE 1. FIGURES. ° e © ° ° INTRODUCTION Subtask Y-F015-01-00l(c), “Effects of Deep-Ocean Environment on Materials," is part (c) of Task Y-FO15-01-001, “Deep Ocean Studies," assigned to NCEL by the Bureau of Yards and Docks. The object of the basic task is to develop systems and techniques for construction in deep-ocean areas. The purpose of this report is to describe the program for the execution of that part of the task related to the effects of the deep-ocean environment on materials and to summarize the progress made in this program since the issuance of the preceding progress report, TN-380, published 23 March 1960.1 SCOPE OF DEEP-OCEAN MATERIALS INVESTIGATION While no specific structures or equipment are delineated in the scope of the investigation, it is reasonable to assume that they will eventually include the following types, as well as other more exotic types of submerged facilities: Structures on which to mount antisubmarine warfare gear Fuel caches Supply depots Refueling stations Submarine repair facilities Nuclear weapon shelters Utility (water, air, heat, electricity, etc.) systems for under- water habitation Heavy mobile construction equipment Power-generating stations It is apparent that most known significant types of engineering materials may be involved and that eventually they should be evaluated for deep-ocean applications. It is also clear that this is a monumental task which could easily involve the concerted efforts of a large number of engineers and scientists for many years. It is therefore necessary to place limitations on any list of materials to be tested in the first phases of this program. Another reason for limiting the initial materials list is that it is always possible that the proposed experiments may show that the information already available concerning the behavior of materials in shallow marine environments is applicable with only slight modifications to similar materials in a deep-ocean environment. For these reasons the selection of materials for inclusion in the first phases of this program has been limited to a representative sampling of various material types rather than directed toward the systematic coverage of each variety of each type of material. However, through the cooperation of certain industrial research laboratories, a wide variety of small “screening specimens" of various alloys has been included in the specimen load of the first Submersible Test Unit (STU). Although time-dependent changes in engineering properties of materials may occur, chemical deterioration and corrosion are expected to be the major processes of deterioration in the deep-ocean environment. For purposes of this report the term corrosion is defined as "... a gradual chemical or electrochemical attack on a metal by its surroundings, such 2 that the metal is converted into an oxide, salt or some other compound.” These major processes of deterioration will be influenced by the physical environment (high hydrostatic pressure and low temperature) and the biological environment. Since the rate and degree of deterioration are also influenced by specimen configuration and by the mechanical and physical structure of the metals, it will be necessary, in the case of metallic specimens, to include variations in these factors as well as variations in the alloying elements. The first materials to be extensively tested for suitability for use in the deep-ocean environment will be those commonly used in cone= ventional construction and available through normal supply channels. If it is determined that these materials are not satisfactory for deep= ocean structures, then the less commonly used, exotic, and unusual materials will also be studied. When constructing in a medium of relatively high density (compared to air) such as sea water, there is immediately available a unique technique of building virtually weightless structures and thus regulating the dead- load pressure such a structure will exert on the ocean bottom. This technique is based on the use of low-density structural plastics, foamed materials, and/or the incorporation of buoyancy through the use of either voids or spaces filled with a buoyant fluid or other material. For this reason, and also because of their resistance to sea-water corrosion, Plastic materials take on great importance. These include acrylics, polyvinyl chlorides, polypropylene, polyethylene, polyeurthane, teflon, nylon, rubber (both natural and synthetic), glass-fiber laminates, and others. Samples of many of these materials will be included in this program. Ceramic and glass materials are important to provide electrical insulation, view ports, and transparent closures for light sources, cameras, and television; they are also used as structural elements in some electrical lead-through systems. Some of these types of materials will be tested. ho Cables for lowering and raising Loads in deep water, for mooring buoys and ships, for guying structures, and cables for general-purpose work are important to the deep-ocean program and will be tested. Included in this program will be galvanized steel, electrogalvanized steel, aluminized steel, unccated steel, and polyvinyl-chloride-coatea steel cables. Stainless steels and other alloys will be included. Specimens of some electrical. cables will also be included. The suitability of concrete for use in deep-ocean structures will be investigated. Experiments will be set up to evaluate the effect of this environment on its permeability, water absorption, volume change, and durability. The types of reinforcing material for this use will also be investigated. EXPERIMENTAL ENVIRONMENTS If the results of experiments conducted in deep-ocean environments differ materially from what would be expected of similar materials exposed in shallow-water environments ( judged on the basis of data published in the literature), it will then be necessary to conduct similar experiments using identical specimens in shallew water to insure that the anomalous results were in fact due to the environmental differences and not due to some variable in the particular specimens used or to the experimental technique. In the event that such shallow- water exposure seems desirable, Port Hueneme Harbor will probably be used. Various pressurized and unpressurized laboratory-simulated deep- ocean environments will also be used to isolate and study the contribution of individual factors to the deterioration of materials exposed in the deep ocean. Deep-Water Enviromments The environments with which this task is primarily concerned are those of the water near the ocean bottom (at depths beyond normal 3 engineering construction practices; i.e., depths in excess of 2000 £t)) the water-bottom interface, the sediments adjacent to the water-bottom interface, and to a somewhat lesser extent, the intervening water mass between the ocean bottom and the surface. This study concentrates on these environments because the effects of the near-surface (shallow-water) environment on materials have been and are under intensive study by many other agencies. Also it is believed that the greater part of most deep-ocean structures of interest to BuDocks will be on the ocean bottom or in its immediate vicinity. The intervening water mass between the bottom and surface will be considered primarily as an environment for mooring cables and small suspended structures such as underwater buoys and arrays. In order to appreciate the potential effects of the deep-sea en= vironment and the necesssity for evaluating materials while exposed to it, the following example of physical data describing the actual en- AERTS as measured at the bottom in the Romanche Deep of the Atlantic Ocean, is presented: Depth = 25,000 feet Ambient pressure = 11,000 psi Temperature - 1.459 ¢ Salinity - 34.75 o/oo Oxygen - 5.1 m1/L BH = ier, Currents = probably on the order of O.1 knot or less While these are the conditions which prevail at this depth, it must be remembered that anything being placed on the bottom must pass through the upper portions of the sea where strong currents, wave action, sunlight, relatively high oxygen content, and a very active biological environment prevail. In addition to these factors, the object being lowered would go through a pressure gradient ranging from atmospheric pressure at the surface to many thousands of psi hydrostatic pressure at the bottom. Factors contributing to changes in and/or the deterioration of materials exposed to the deep-ocean environment are summarized as follows: Low ambient temperature Biological environment High hydrostatic pressure Stress Chemical environment Electrochemical effects of immersion in an electrolyte Water movement These factors, separately or in combination, may operate to pro- duce one or a combination of the following effects which may change certain properties of the materials exposed to this environment: Creep Mechanical failure Physical deterioration Chemical deterioration Biological deterioration Electrochemical deterioration Volume change Water absorption Laboratory-Simulated Environments One of the early objectives of this task has been the investigation of means of reproducing the deep-sea environment in the laboratory under controlled conditions. Toward this end the literature has been studied to determine the state of the art in this field. Visits have been made to various government, university, and industrial laboratories throughout the country to examine high-pressure research facilities and to determine what work has been done on this problem. As an outgrowth of these searches, which disclosed a lack of the desired facilities, various high-pressure laboratory vessels and facilities have been designed and are being fabricated. NCEL's high-pressure laboratory, which will be described in detail later in this report, will, when fully developed, be used to reproduce the following aspects of the deep-ocean environment ; Hydrostatic pressure to 20,000 psi Temperature down to O°C Sea-water chemistry as found in situ at great depth Shallow-Water Environments In order to study the differences in deterioration processes and rates of deterioration in deep and in shallow water and to determine if observed differences are in fact due to the environmental differences and not differences in specimens or experimental technique, it may be necessary to expose duplicate specimens of certain of the materials under study in both environments for similar periods of time. Because of its proximity, Port Hueneme Harbor has, for some years, been used as a site for corrosion and protective coating studies by NCEL. The harbor waters are relatively unpolluted and are monitored weekly for pH, salinity, and solid content. Specimens exposed in this environment would be prepared from the same lots of material used in the deep-water tests. The essential difference in the exposure conditions, other than the environment, would be the spacing of specimen plates. Due to the high fouling rate in the harbor, it would be necessary to provide more separation between adjacent specimen plates than is believed necessary for deep-ocean exposure. MATERIALS TO BE INVESTIGATED Since this is a continuing program it is not feasible to provide a complete list of all the materials to be tested. The Appendix contains a list of all the materials contained in the specimen load of the first Submersible Test Unit placed in FY-62. Selections of materials to be included in the tests have been based on gleanings from the literature and from the records of meetings held by various naval activities and scientific groups. The major producers of metals, as well as nonmetals, have been requested to supply their recommendations. In most instances the producers have provided advice, and in some cases have supplied samples of production materials for test. The Naval Air Material Center at Philadelphia, Pennsylvania, the U. S. Naval Engineering Experiment Station at Annapolis, Maryland, the U. S. Naval Underwater Ordnance Station at Newport, Rhode Island, the Naval Ordnance Test Station at China Lake, California, the Navy Electronics Laboratory at San Diego, California, and some industrial laboratories, as well as NCEL, have contributed specimens for inclusion in this program. EXPERIMENTAL METHODS Unstressed Specimen Experiment Unstressed materials will be utilized as the primary type of specimens to be exposed in the experimental environments. Where it is feasible (generally a matter of having a sufficient quantity of the test material), rigid sheet materials have been cut to 6 inches by 12 inches in size and mounted in racks. The purpose of utilizing specimens cf this size is to reduce the possibility of edge effects obscuring the effects of the environment on normal flat surfaces. Sixteen such plates are shown in Figure 1 in a exposure rack designed for specimen exposure above the water-bottom interface. Similar racks are used for exposure of specimens in the environment of the sediments below the water-bottom interface. As may be noted in Figure 1, each 6-inch by 12-inch specimen is in contact with nothing except porcelain insulators and each set of four specimens is separated from adjacent dissimilar materials by a vinyl separator plate. In this illustration, four replicate sets, each containing four plates of a single material, are shown. The arrangement of the four specimens is such that the two outside specimen plates of each set are separated from the adjacent vinyl plate by about 1/2 inch and from the closest of the inside pair of specimen plates by about 1 inch. The inside pair of specimen plates are separated one from another by about 3/4 of an inch. This arrangement is designed to test the effects of the spacing of the plates (from each other and from adjacnet materials) on the rate and on the degree as well as type of deterioration of the plates. In each set of four replicate specimens, one plate has a l-inch by leinch square "patch" of the same material bolted to it (as shown in Figure 1) by a nylon bolt. The purpose of this procedure is to investigate the susceptibility of the material to crevice corrosion. Specimen identification code numbers are applied to all rigid 6- inch by 12-inch specimens by a combination of two edge notches and two 1/8-inch holes which are drilled through the specimen at specific "grid points." When the quantity of material available is insufficient for the fabrication of 6=-inch by 12-inch plates, a specimen size of l-inch by 6-inches is used. These specimen strips are fastened to 2 1/2-inch- thick polyethylene strip by means of 1/4-inch-diameter nylon machine screws. The specimens are spaced about 1/8 inch from the polyethylene strips by means of an acrylic washer. By using this method, both rigid and nonrigid materials are mounted for exposure. Figure 2 shows two sets of the l-inch by G-inch racks installed on the Submersible Test Unit. Short pieces of wire, cable, and rodlike specimens are held in plastic mounting clips fastened to 1/2-inech-thick polyethylene strips by means of 1/4-inch-diameter nylon machine screws. The polyethylene strips are held in their racks by means of mild-steel bolts. Stressed Specimen Experiment Exposure to the experimental environment under stressed conditions is accomplished in either of two ways according to the type of material. Cables exposed in a stressed condition are placed in tension jigs patterned after similar devices developed by the American Steel & Wire Company. Figure 3 shows a jig containing two specimens of cable under tension. In use, the cable is threaded through the jig end=plates and tensioning screw; mild-steel end stops are swaged in place and the tension screw is then adjusted using a cable tension indicator (see Figure 4) in order to stress the wire to 20 percent of its ultimate strength. All metal-to-metal contact between the cable specimens and the tension jig is eliminated by means of fiber-reinforced plastic washers and Plastic sleeves. Four cable-tensioning jigs containing specimens of eight different materials are included in the test program for the first deep-sea tests. The cable materials are as follows: Bright plow steel Bright Monitor Galvanized plow steel Electrogalvanized plow steel Type 316 stainless steel PVC over Amgal USS Tenelon Aluminized steel Two specimens are mounted in each of the four jigs. The jigs are located on the STU so that each cable specimen crosses the water and sea-floor interface and is partially embedded in the sea floor. Stress-corrosion testing of appropriate metallic materials may be conducted by utilizing the method illustrated in Figure 5 and described by Phelps. In this method, the specimen, which is prepared in the form of a strip 1 inch wide and 0.050 inch thick, is placed in flexure in a rigid jig. The jig holds the ends 7.000 + 0.001 inches apart. The tensile stress induced in the outer fibers of the mounted specimen is a function of the length of the specimen; the length is calculated for a desired stress level. In order to assure that there are no bimetallic electrical currents between the metal specimen under test and the metallic jig, an insulating film is placed between the jig and the specimen. To prevent complete loss of a broken or displaced specimen, a hole is drilled through each end of each specimen and a thin plastic cord is used to tie it to the jig. Specimen Handling The following procedure for treating the specimens which were mounted on the first Submersible Test Unit (see Ocean Environment Experiments) is planned for all deep-ocean exposure tests. Following the degreasing, the metallic specimens were handled with clean cotton gloves and immediately placed in sealed canisters which contained silica-gel desiccant. All materials, both metallic and nonmetallic, were then taken to a workroom where the humidity was maintained at approximately 20 percent relative humidity. The specimens 8 were then weighed and placed in the racks in which they were to be exposed to the deep=ocean environment. The individual racks were then wrapped in polyethylene and transferred to the assembly room where they were attached to the STU, which is shown in Figures 6 & 7 with the complete specimen load. The assembly room consisted of a large plastic=- covered, humidity-controlled chamber (see Figure 8) which was erected in a warehouse=type building. The humidity in this chamber was con- trolled at approximately 35 percent relative humidity. When the STU was removed from the assembly room for transporation to the ship and the sea-installation site, it was wrapped in a polyethylene cover with desiccant included. The cover and desiccant were removed about an hour before the actual placement of the STU in the water. Evaluation of Specimens After Exposure to Test Environment Immediately after removal of specimens from the ocean environment they will be photographed with color film and then examined by a biologist who will collect, for identification, specimens of any organisms which may be attached. For a discussion of the biological aspects of materials deterioration see NCEL Technical Report R-182, The Effects of Marine Organisms on Engineering Materials for Deep Ocean Use. Following the collection of biological specimens, the STU and its contents will be washed off with fresh water, and the test racks and jigs will be removed and dried and cleaned so as to permit examination of the surfaces of the specimens. Pitting depth, edge deterioration, and loss of plate thickness and weight will be recorded. Other tests to determine changes in properties such as durometer, hardness, moisture content, resistivity, tensile strength, chemical composition, and elasticity will be conducted as appropriate for the individual materials. OCEAN ENVIRONMENT EXPERIMENTS Deep-Water Experiments Submersible Test Unit (STU). The STU (Figures 6 & 7) is designed for placing specimens and/or instruments on or near the ocean bottom, exposing its load to the effects of the deep-ocean environment for extended periods of time, and recovering its load at the end of the exposure period. The STU is a towerlike structure 14 feet high with a 30-inch by 30-inch cross section supported on a 13-fcot by 13-foot square base to assure stability on soft or sloping bottoms. The structural members are fabricated from A-7 structural steel and are protected with a vinyl paint. This particular paint was selected to inhibit corrosion of the structure and at the same time not to inhibit fouling activity. It was felt that the introduction of 2 fouling inhibitor would interfere with the effects of the experimental environment (including the resident organisms) on the various specimens under test. The tower portion of the STU is provided with adjustable shelves, each consisting of a steel grating fastened to an angle-iron framework. The weight of the loaded STU is approximately 7000 pounds in air and 6000 pounds in sea water. Program. The STU provides a means for exposing a large number of specimens of various materials to the effects of the deep-ocean environ- ment. The initial program, as presently envisioned, is divided into two phases. In the Phase I program three STU's are to be placed at a depth of 6000 feet for periods of 6, 12, and 24 months respectively. In Phase II, three STU's are to be placed at a depth of 12,000 feet for periods of 6, 12, and 24 months respectively. The extent of this program beyond Phases I and II will depend entirely on the results obtained from these first experiments. The first STU of Phase I has been fabricated and was emplaced in 5300 feet of water on 29 March 1962 for a 6-month exposure. Emplacement of the next STU is planned for late in FY-63. Operational Testing. Tests at sea in 1200 and 6000 feet of water, which involved the Placement of the STU with a 1600-pound simulated specimen load on the bottom, were conducted with the YFU-48 during November and December 1961. These tests revealed the following facts: 1. The YFU-4k3, a 116-fcot converted LCU, is adequate for the STU placement operation at the 6000-foot-depth site in favorable weather. e2. The standard Navy UQN-1E depth sounder is not adequate for tracking the STU during placement in 6000 feet of water using the standard recording equipment. 3. The two devices designed and constructed at NCEL to sense any departure of the STU's attitude from a normal vertical position during lowering and placement on the bottom worked satisfactorily. 10 4. 08: e YVVNWWW FF FUUMU AH IJ--3 oO e e ee © e@ «6 WE CPR) SRLS WS NO ce CN 100 FW Note: a, Overlapping casts b. Samples bubbled when drawn, doubtful values 27 i si) neg, = x b i "41UP) 4SO] S/qissswqns eu4 ul JUsWUOIIAUa UDEd0-daap ayy Oo} suaWoeds pIBI4 YouI-Z| Aq -g passesysun yo ainsodxa ayy Joy yODY “| eunBiy Figure 2. Arrangement of 1- by 6-inch specimen racks in the Submersible Test Unit. ’ ( i ne aM eo Winey Figure 3. Cable tensioning jig for the exposure of wire rope and cable specimens to the deep-ocean environment while under load. Figure 4. Cable specimen in a tensioning jig being loaded to a predetermined stress level. Pte erase: Figure 5. Stress corrosion jig with a specimen. Figure 6. 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Tensile stress corrosion jig disassembled to show component parts. isin | te puis ne ay iy 4 Ha SNDL Code 23A 398 39D 39E E16 F177 Fal FLO FAL F42 F48 DISTRIBUTION LIST Chief, Bureau of Yards and Docks (Code 70) Naval Forces Commanders (Taiwan Only) Construction Battalions Mobile Construction Battalions Amphibious Construction Battalions Construction Battalion Base Units Chief of Naval Research = Only Chief of Naval Operations (op-07, op-04) Bureaus Colleges Laboratory ONR (Washington, D. C. only) Research Office ONR (Pasadena, only) Training Device Center Station = CNO (Boston; Key West; San Juan; Long Beach; San Diego; Treasure Island; and Rodman, C. Z. only) Communication Station (San Juan; San Francisco; Pearl Harbor; Adak, Alaska; and Guam only) Administration Command and Unit CNO (Saipan only) Communication Facility (Pt. 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