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Atomic Energy Je^K L'energie Atomique of Canada Umited Ksv Du Canada Li Mite E AECL-7416 ATOMIC ENERGY JE^K L'ENERGIE ATOMIQUE OF CANADA UMITED KSV DU CANADA LI MITE E PROGRESS REPORT CHEMISTRY AND MATERIALS DIVISION 1 April -30 June, 1981 PR-CMa-57 Chalk River Nuclear Laboratories Chalk River, Ontario August 1981 PREVIOUS REPORTS IN THIS SERIES PR-CMa-56 January 1 to March 31, 1981 AECL-7332 PR-CMa-55 October 1 to December 31, 1980 AECL-7242 PR-CHa-54 July 1 to September 30, 1980 AECL-7156 PR-CMa-53 April 1 to June 30, 1980 AECL-7094 PR-CMa-57 ATOMIC ENERGY OF CANADA LIMITED PROGRESS REPORT April 1, 1981 - June 30, 1981 CHEMISTRY AND MATERIALS DIVISION The results and conclusions given here are not classified or restricted in any way; however, some of the information is of a preliminary nature. Readers interested in using the information in their own research are invited to consult with the contributors for further details. Copies of the AECL publications referred to in this report may be obtained by writing to the Scientific Document Distribution Offfee, Chalk River Nuclear Laboratories, Chalk River, Ontario, KOJ 1J0. Chalk River Nuclear Laboratories Chalk River, Ontario 1981 August AECL-7416 PROGRESS REPORT April 1, 1981 - June 30, 1981 CHEMISTRY AND MATERIALS DIVISION Director - T. A. Eastwood Secretary - Ms. A. E. Goodale Contents Page HIGHLIGHTS T.A. Eastwood (i) 1. SOLID STATE SCIENCE BRANCH I.V. Mitchell 1 2. GENERAL CHEMISTRY BRANCH I.H. Crocker 27 3. PHYSICAL CHEMISTRY BRANCH D.R. Smith 53 4. MATERIALS SCIENCE BRANCH B. Cox 71 (i) CHEMISTRY AND MATERIALS DIVISION HIGHLIGHTS T. A. Eastwood Solid State Studies Computer calculations have emphasized the importance of axial symmetry in measurements of ion stopping power by the time-of-flight method. Recent measurements which meet this condition and include other refinements give preliminary results which confirm earlier measurements of stopping powers. These had shown a thickness dependence in the stopping powers of thin films of carbon and gold for neon and argon ions. We believe this dependence may be used to show explicitly the contribution of nuclear inelastic events to total stopping processes. Previously it was shown that the number of ions scattered through 180° from an ion beam impinging on a target with heavy atoms implanted in a lower atomic weight host material or with a surface oxide film was as much as twice that calculated for simple elastic collisions. It has now been shown, for the first time, that enhancement of ion scattering at 180° can also develop strongly even when the scattering occurs in the first two or three atomic layers of a single crystal of gold. Results are consistent with the predictions of a two atom model. In order to familiarize staff with the Scanning Auger Microprobe (SAM) instrument recently installed by the Systems Materials Branch the depth profile of nitrogen atoms implanted in aluminum foil was measured. By alternatively sputtering and analyzing for Al, N and 0 with the SAM both the implanted nitrogen and surface oxide layers were clearly discerned. Energy measurements showed that both the N and 0 atoms are chemically combined with Al. To obtain a depth profile in accord with that expected from the implantation parameters it was apparently necessary to include a more careful treatment of the Auger satellite intensities than is allowed for by the manufacturer's software. To understand the details of heavy ion channeling in crystals and apply the process in solid state research it is necessary to know the rate at which ions are scattered out of the channels (i.e. dechanneled) as they penetrate to greater depths in the crystal. Encouraging agreement has now been obtained between experimental and calculated rates for dechanneling of protons in gold crystals. Taken with earlier results for Si and Ge, crystals which differ considerably from gold in solid state properties, this agreement builds confidence in our description of dechanneling. (11) Radiation Chemistry In the analysis of hypothetical reactor accidents hypoiodous acid, HOI, often plays a key role in predictions of the amount of fission product iodine released to the environment. The properties of HOI are not known very well because it is a very unstable and reactive compound but radiation chemistry techniques are proving to be useful for investigating some of its important properties. Using its optical absorption spectrum for identification and concentration measurements, it has been possible to determine the rate of decomposition of HOI in aqueous solutions. Dithiothreitol is being used as a model compound in studies of the effects of irradiation on biochemically active compounds containing sulphydryl (-SH) groups. Formation of Hg arising from the attack of hydroxyl radicals on the carbon chain of dithiothreitol has been observed and indicates that oxidation can occur at two sites in this model compound. Isotope Separation (a) Laser Photochemistry Studies of the multiphoton decomposition (MPD) processes show that MPD is more easily achieved in 2,2,2-trifluoroethanol (THE) than in methanol at comparable pressures and HF laser fluences. This is in accord with earlier observations of multiphoton absorption and is attributed to the greater density of vibrational energy levels available for laser excitation in TFE. Significant progress was made during the first year of a research contract at McMaster University. The objective of the work is to devise and characterize an organo-zirconium molecule suitable for research on laser-induced zirconium isotope separation. A molecule is required with adequate volatility for gas phase photolysis at room temperature or lower and which absorbs COg laser radiation in a Zr-ligand vibrational mode. A number of candidate molecules have received preliminary consideration. Analytical Chemistry A method for the preparation of oxygen gas samples for the determination of oxygen isotope ratios in light and heavy water has been successfully tested. To avoid isotope fractionation during the preparation, essentially all the oxygen in the sample has to be converted to oxygen gas. Gaseous oxygen yields in the range of 93% to 100% were achieved by reacting water with bromine trifluoride and purifying the resultant gas mixture. The procedure was tested on a sample of heavy water standard that was 99.96% DgO. It was found that 0-18 was enriched by a factor of 2 to 3 relative to its abundance in natural water. (iii) Studies on the application of high-performance liquid chromatography and trace enrichment to the determination and speciation of metals in ground waters, within and external to a waste-management site at CRNL, have been completed and the work has been prepared for publication. The results show that this approach can be used to monitor the variations in metal concentrations in ground waters in the pg.aiL"! to ng*mL~l range with reproducibilities of 2 to 10%. Total metal-ion concentrations were determined after exposure of the samples to Y-irradiation and a comparison with neutron-activation results for Co showed excellent agreement. The results obtained after equilibration of the samples with nitric acid or citrate suggested that this approach should be useful for monitoring the speciation of several trace elements in ground waters; however, a more extensive study is required to fully assess the usefulness of this approach. Materials Science Sputtered coatings of ferritic stainless steel on the surface of Zircaloy fuel cladding result in large reductions in the oxidation rate in high-temperature, high-pressure steam. In high-temperature water the coating has little or no effect on the oxidation rate. If the protective capacity of the coating in steam persists after long exposures in high temperature water then the coatings could be valuable for minimizing the oxidation rate of Zircaloy cladding during small-break loss-of-coolant situations (e.g. Three Mile Island) where extensive high temperature oxidation of the cladding occurred. A theoretically based design equation for irradiation growth has been derived which predicts the growth rate and flux exponent of the growth component of the irradiation induced dimensional changes in Pickering Unit-1 pressure tubes. Bauschinger effect studies on annealed thin-walled Zircaloy-2 tubing have shown that <1% compressive pre-strain is sufficient to reduce the 0.2% yield stress by a factor of two. Thus, even very small amounts of compressive deformation must be avoided if the tensile yield strength of calandria tubes is to be preserved. - 1 - SOLID STATE SCIENCE BRANCH (Edited by L.M. Howe and J.A. Davies) 1.1 STAFF 1.2 ION PENETRATION 4 1.2.1 Stopping Powers for 7Li Ions 4 1.2.2 Stopping Powers of Oxide Films 5 1.2.3 Effect of Geometry on Average Flight Distances in 6 Time-Of-Flight (TOF) Spectrometer 1.2.4 Time-Of-Flight Measurements 6 1.3 SURFACE PHENOMENA 7 1.3.1 Studies of the (110) Surface of Monocrystalline Pt 7 1.3.2 Preparation of a (111) Pt Single Crystal 8 1.3.3 An Investigation of the Enhanced Rutherford 8 Backsc«ttering Yield at 180° from Aligned Au Crystals 1.4 RADIATION DAMAGE 9 1.4.1 Collision Cascades in Ge 9 1.4.2 The Depth and Angular Dependence of the Mid-Channel 10 Flux of 4He Ions in Al Crystals 1.4.3 Channeling Measurements of Interstitial Trapping by Ag 12 Atoms in an Al-0.05 at% Ag Crystal 1.5 ION BEAM MODIFICATION OF MATERIALS 14 1.5.1 Ion Beam Modification of Metals 14 1.5.2 Determination of Composition" vs. Depth Profiles of 15 N?+ implanted in Al, Using the Scanning Auger Microprobe (SAM) - 2 - 1.6 INTERDISCIPLINARY RESEARCH 18 1.6.1 A Study of the Rutherford
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