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Aug. 21, 1973 3,753,883 Aug. 21, 1973 B GRIGGS 3,753,883 PROCESS FOR PROVIDING A HYDRIDE-FREE AND OXIDE-FREE SURFACE ON ZIRCONIUM AND ZIRCONIUM-ALLOY BODIES Filed June 26, 1972 (&J.70A) ~7£//J. Al3J- OcJ 3,753,883 United States Patent Office Patented Aug. 21, 1973 1 3,753,883 The single figure of the drawing is a graph showing the PROCESS FOR PROVIDING A HYDRIDE-FREE current-potential-time relationship employed^ in carrying AND OXIDE-FREE SURFACE ON ZIRCO- out the present invention in accordance with one em- NIUM AND ZIRCONIUM-ALLOY BODIES bodiment thereof. Bruce Griggs, Richland, Wash., assignor to the United 5 In accordance with this invention, a body consisting States of America as represented by the United States essentially of zirconium and having a zirconium hydride Atomic Energy Commission surface layer is electrolytically anodized in aqueous nitric Filed June 26, 1972, Ser. No. 266,110 Int. CI. C23b J/00,1/02 acid solution to remove the hydride surface, fluoride ion U.S. CI. 204—144.5 7 Claims is added to the solution and electrolytic anodization is 10 continued to render the surface susceptible to chemical etching and chemical etching is performed in situ using ABSTRACT OF THE DISCLOSURE the anodization bath as etchant, or the body may be A zirconium or zirconium-alloy body having a zirco- etched in a separate HN03-HF etching solution. nium hydride surface layer is electrolytically anodized In the anodization operation, nitric acid is suitably in aqueous nitric acid solution to remove the hydride 15 present in 2.0% to 20% by weight of the aqueous solu- surface. Fluoride ions are then added to the solution and tion, preferably about 3% by weight. electrolytic anodization is continued. Chemical etching The cathode of the electrolyte cell may suitably be with HNO3-HF solution thereupon provides a hydride- stainless steel or other conductor resistant to nitric acid, free and oxide-free surface. Chemical etching may be such as graphite. in situ employing the anodization bath as etchant if the 20 The anode current density is governed by the resistance concentration of fluoride ions therein is high or a separate of the oxide film and the applied potential. Many different etchant solution may be employed. anode current densities were tested and found satisfactory. The upper limiting current densities will usually be determined by the geometry of the anode (its current- CONTRACTUAL ORIGIN OF THE INVENTION 25 carrying capacity) and heating effects of the current. Thus The invention described herein was made in the course a high surface area to volume ratio anode will probably of, or under, a contract with the United States Atomic have its current density limited by the ability of the Energy Commission. anode to carry the current. The electrolyte is heated by current passage and thus the total current input can be SPECIFICATION 30 limited by the heat dissipation capability of the electro- The invention relates to a process for providing a lyte system. The potential of the process is adjusted to hydride-free and oxide-free surface on zirconium and maintain the maximum current density suitable for the zirconium-alloy bodies. particular system until the maximum potential (80-100 Zirconium and its alloys tend to react with or absorb volts) is reached. Initially about 5 volts may be employed. hydrogen under certain processing or use conditions.' The 35 The current density is then allowed to decay to a low hydrogen thus absorbed forms a hydrogen-rich phase in value which indicates all the surface hydride has been the metal. This zirconium hydride phase can distribute removed. itself as a surface layer, a uniformly distributed precip- Apparently the anodic removal of the surface hydride is itate, or both, depending on the conditions of its formation 4n accomplished in stages. The first stage appears to be and3 subsequen1 ta treatmentj. a .1.. ThT"1 e presence o_ fr zirconiu_* * m electrochemicaQlaf'trr\r,nOtnir>n1l attacof fn r>V-k of the continuou+J«-»Tt/-»f«f<s annn/di fairl-Poiy densea hydride in zirconium or its alloys usually produces unde- hydride layer. The electrical conductivity of the hydride sirable properties for structural applications. The removal allows current flow at low potentials and one expects the of a zirconium hydride surface layer from a zirconium current density to be fairly constant over the anodic alloy is frequently desirable to avoid its future redis- 45 surface. This stage could be considered dissolution of tribution throughout the metal during subsequent process- the hydride. ing or use conditions. The second stage occurs when zirconium metal is Surface layers of zirconium hydride can be removed by exposed at the surface and begins to anodize or form chemical etching in HN03-HF solutions, abrasive blast a protective oxide layer. The cell potential increases became of tbe techniques, machining or grinding. None of these methods 5q increasing^ resistance to current flow at are selectiv1 J.; e andJ thuil s requir... 2 e a detailei,.»t1d t knowledg1 4 e ofC thttteQ Zircalo7lt*r>r\ 1 ATyT surfaceo »•»•»-£<-> nn . DurinT\n ntn g thiI s„ seconnnnMM dJ stagen^n , "L.hydridJ e» the amount and distribution of the zirconium hydride to is still being removed. However, spalling or sloughing of be removed. Hot vacuum extraction can only be employed the hydride, oxide and/or metal is noted, apparently due for hydrogen removal if the part be sufficiently heated in to undercutting of the surface along hydride precipitates. a high vacuum. 5g The third stage occurs when the potential rapidly An object of this invention is to provide a process for increases to a high value, above 80 volts. This is an indi- the selective removal of dense zirconium hydride layers cation that the current paths on the Zircaloy-2 sample from zirconium and its alloys, and the obtaining of a have been effectively blocked by the anodic film formed hydride-free and oxide-free surface. on the surface. The hydride case will have essentially Another object is to provide an efficient and econom- 60 teen removed by this time. ical process for the removal of surface hydride layers The electrolyte may be at any temperature between 20" present on nuclear reactor process tubes made of zirco- and 40° C., the upper limit being specified because slight nium or zirconium alloys consisting essentially of zirco- pitting of the zirconium body has been observed at elec- nium, such as Zircaloy-2 (an alloy of zirconium with trolyte temperatures above 40° C. 1.5% by weight Sn, 0.15% Fe, 0.10% Cr and 0.0-0.05% 65 Subsequent to the nitric acid anodizing, fluoride ions Ni). (HF, NH4F, NH4-HF, etc.) are added to the solution and 5 3,754,138 4 electrolytic anodization is continued to render the anod- The specimen was removed from the anodizing treat- ically formed oxide layer susceptible to chemical etching. ment and immersed for about 7 minutes in standard The amount of fluoride added affects the subsequent HNO3-HF etch solution at room temperature which anodizing process. Small amounts of fluorides such as caused all the visible oxide layer to flake off and the part 0.04% will require a high (50-100 v.) anodizing voltage g to etch normally. Continued chemical etching to remove to make the oxide film subject to removal in a standard about 1 mil of metal produced a normal etched surface zirconium etch solution (approximately 33% HN03, appearance. This combined process will also remove any 1.6% HF and 65% H20 by weight). Alternatively, a layer of detached platelets of zirconium hydride that larger amount of fluoride (<~1%) will require a lower escape removal in the plain nitric acid anodizing treat- anodizing voltage (5 to 20 v.) and can also act as the io ment. etch solution by reducing the potential after decomposing For some applications, in situ etching is very desirable, the oxide layer. Any of these processes can be conducted particularly since the sensitivity of zirconium and zir- by changing the composition of the solution in one liquid conium alloys to the rate of flow of a standard etching system or moving the body being treated from one liquid solution is very high. For such applications a fluoride system to another having the desired composition. For 15 concentration on the order of \% may be employed and some applications one method is better and for other the initial voltage is reduced to 5 to 20 volts. Maximum applications the other method would be better. and minimum fluoride concentrations have not been es- Removal of the hydride layer by electrical anodiza- tablished; however, it is clear that somewhat larger and tion in nitric acid is shown in the following. smaller concentrations would be acceptable. The process, as applied to one particular specimen, con- 20 According to a specific example of this embodiment of sisted of making a 20-inch section of 1.8 inch-diameter the invention, a Zircaloy tube was electrolytically anodized Zircaloy-2 tubing the anode of an electrolytic cell. The while flowing 3% nitric acid through the tube as described cathode of the cell was a central piece of Vi -inch-diameter above. After the potential reached 100 volts the current stainless steel tubing which also carried the 3% nitric was shut off and 1.2 weight percent ammonium bifluoride acid solution which was pumped into the Zircaloy tube 25 (NH4F-HF) was added to the anodizing solution. A po- section from a recirculation reservoir containing 24 liters tential of 5 volts was applied and maintained until the of the acid solution. The Zircaloy tube section had an current density reached 100 ma./cm.2 at which time internal surface layer of zirconium hydride approximately the voltage was backed off to hold the current steady.
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