Forming, Welding & Heat Treatment of SS Equipment & Components for Nuclear Recycle Plants

Santosh H Takale, Ramakant and D. S. Rana Nuclear Recycle Group, Bhabha Atomic Research Centre, Trombay, Mumbai-400 085.

Key Words: Stainless steel, NAG, corrosion, IGC, forming, Knuckle, SF, expansion bellows, solution annealing, GTAW, QA/QC.

Abstract Back-end Fuel Cycle Plants play a vital role in Nuclear Power Programme as these enable recovery & recycle of useful materials from the discharged spent fuel from nuclear reactors. The recovery process entails handling of high concentration of nitric acid solutions coupled with high levels of radioactivity. Austenitic stainless steel (SS) generally withstands these aggressive process conditions. Apart from material selection, all manufacturing steps inclusive of forming, heat treatment, joining, cleaning & contamination checks play very important role in lifetime integrity & functioning of process equipment. Years of experience in the use of such equipment has shown that unattended microscopic defects as well as locked up stresses at the stage of manufacturing lead to much detrimental effect and at times failures in the operational stage. To ensure lifetime integrity of the process systems comprising equipment, piping and assemblies a well defined & established manufacturing set up dedicated to such special production is required. The paper shares the experiences on various aspects pertaining to fabrication of austenitic stainless steel equipment with emphasis on forming and heat treatment. 1. Introduction: Nuclear Recycle Group (NRG) of Bhabha Atomic Research Centre (BARC) functionally consist of design, engineering, construction and operation of reprocessing & waste management plants. Separation of fertile materials from spent fuel is done by chemical processing, which results in generation of high level liquid radioactive wastes. The separation process is carried out within RCC shielded cells having wall & roof thickness ranging from 900 mm to 1500 mm. The main process medium is nitric acid with various levels of concentration, containing a host of isotopes some of which are highly corrosive in nature. Presence of radioactivity makes equipment and systems inaccessible for in-service maintenance. Hence, lifetime integrity of fabricated equipment is a prerequisite. The special equipment viz. dissolver assembly, extraction columns, thermo-syphon evaporators, conditioners, denitrators, annular vessels, condensers, scrubbers, etc. employed in reprocessing of spent fuel and waste management demand utmost attention & due care at manufacturing stage mainly during forming (cold working), heat treatment & welding. Each of the above equipment and vessels is designed for different process conditions ranging from normal temperature to boiling condition operations & 0.1 M to 12 M of HNO3 concentrations. Hence it is essential to control cold working on formed components & various parameters in welding technique, apart from maintaining the surfaces contamination free. The detail of various aspects with respect to forming, joining and heat treatment of SS equipment & components is elaborated in succeeding paragraphs.

2. Forming: The Austenitic stainless steel being very ductile can be easily made to flow in desired size and shapes. Most of components for equipment fabrication are manufactured by cold working process to have smoother surface contours and for minimum weld joints. Process vessels & equipment are constructed from Shells, Dished ends, Expansion bellows, Nozzle pipe bends, Cooling/Heating/Sparger coils & Pull outs, which are all formed components. The pull-out provides smother geometry for nozzles and eases the complete draining of the equipment. It makes joint accessible for radiography and better result interpretation. The degree of cold work depends to great extent on the method of forming, which in turn have significant impact on corrosion resistance of the material. 2.1 Effect of cold work: The cold working of SS material results in increase in susceptibility to sensitization between temperature range of 450 to 800 0C [6]. Further, the susceptibility to sensitization of austenitic stainless steels increases with increasing cold work [4]. Cold work levels up to 1520% increase retained energy in the material and as a result the energy required to nucleate carbide at grain boundary decreases, [1]. The cold working also affects the susceptibility to Low temperature sensitization (LTS). Also machining and cold working results in martensite formation due to plastic deformation within grains. It is evident from the studies that the corrosion resistance of SS is impaired because of cold working hence care has been taken to keep degree of cold work to minimum level. The dished ends geometries are maintained to knuckle radius (KR) of 10 % of ID whereas the conventional torispherical dished ends have KR of 6 % [9]. Higher KR gives added advantage of reduced thinning at knuckle region. Various processes adopted for forming of dishes are die punch technique (for small diameter up to 350 mm), spinning (up to 2000 mm), point pressing for higher diameters. The care has been taken to maintain strict tolerance on die, punches & rollers used as well surface finish to obtained better product quality in terms of dimensions, surface finish & uniformity in thickness. Similarly, sharp bends in pipe components are avoided. The radius given to pipe bends is always more than 5D (D is nominal diameter of pipe). The techniques of material forming are carefully selected to minimize the cold working. e. g. Coils (cooling/heating/sparging) are always manufactured on coiling machine consisting of three rollers, which produces coils with better dimension control, meets tolerances and minimizes induced stress. The acceptable values of ovality after bending of the pipe components are kept less than the codal values. The hardness values obtained after cold working are restricted to 200 BHN. Solution annealing heat treatment is given to the components exceeding the hardness value of 200 BHN [9]. The details are as mentioned in heat treatment section ahead. 3. Welding: The equipment used in nuclear recycle plants are of fully welded construction to provide high reliability and also due to inaccessibility for any repair and maintenance once put into use. Austenitic stainless steels have excellent weldability and can adapt to various available welding process viz. GTAW, SMAW, SAW, FCW, EBM, LBM etc. The high thermal expansion and low thermal conductivity of stainless steel demands controlled heat input along with special jigs and fixtures during welding process. GTAW ensures minimum defects in welding due to its inherent features such as absence of flux/slag, inert gas shielding, non consumable electrode, etc. The manual GTAW adds to quality by providing easy arc maneuvering, welder controlled feed rate etc. Manual GTAW over automatic welding

processes was also preferred due to presence of complex internal geometry of the equipment. The quality of the welding is affected by the base material & filler wire used. The corrosion rate of material is restricted to 12 mpy when a sample having all the structures i.e. weld pool, heat affected zone (HAZ) & parent metal is tested in accordance with ASTM A 262 Pr. ‘C’ [7]. This has been achieved by modifying the composition of Austenitic Stainless Steel and maintaining the metallurgical cleanliness i.e. Inclusion-rating (A+B+C+D) < 4.5 [8]. The purity of argon gas for welding is also found to have great impact on the weld joint quality. Therefore, only high purity argon gas (>99.995%) for shielding as well as for back purging was used during all the welding operations [9]. Care was taken to envelope all surface expose to weld heat during and after welding to avoid any heat tint or oxidation. HF units were used for arc initiation and to minimize the inclusion due to non consumable electrode. Only qualified welders were permitted to do welding including temporary and attachment welds. Weld procedures were qualified not only to meet ASME Section IX criteria but also to meet the requirements of corrosion, controlled content of delta-ferrite etc [9]. To the extent possible all the welds were full penetration joints, back chipped & rewelded. Inside weld joints were finished smooth with the parent metal and outside contours of the welds were made smooth. This way it was ensured that no crevices are left during fabrication, which otherwise is highly detrimental during the use of the equipment because of corrosive environment inside the equipment. Reinforcement on welds was not allowed to exceed 10% of the material thickness. Consideration has been given to fact that stresses present due to cooling from high temperatures during welding in constrained geometries cause deformation in materials. Skip-welding, back-step welding, specially designed fixtures etc. were used to avoid distortion and to control residual stress. The precise control over welding parameters (Voltage & Current) was also maintained. Generally the current and voltage used on lower side to minimize the heat affected zone and to reduce the extent of possible sensitization of the material. Reduction in residual stresses introduced during forming, welding etc. was one of the critical requirements of fabrication, as this may result in stress related corrosion during use. Solution heat treatment was resorted to wherever it was found necessary. Wherever the formed components were of joined type, the representative sample coupons with same heats of the material were tested for corrosion tests stipulated as above. Ferrite number or delta ferrite content was measured at random places on welds by contact type ferrite gauge of certified calibration. The value of ferrite content in the weld both for the welding procedure qualification as well as production welds should not be less than 4 FN and shall not exceed 8 FN [9].

4. Heat Treatment: The heat treatment of Austenitic stainless steel has two fold intentions - getting alloying elements back to the solid solution in their free form & to nullify the effect of cold working and stresses induced. The process of formation of chromium depletion zones is called sensitization. In the temperature range 500-800 0C, the chromium and carbon of the austenitic stainless steel react favorably with each other to form chromium carbides (Cr23C6) at the grain boundaries. Thus a narrow chromium depleted zone is produced adjacent to grain boundaries [2, 3]. The above mentioned temperature range is often encountered during welding in which the material remains for considerably longer durations. Sensitization increases the susceptibility to intergranular corrosion and this will occur when the steel is heated to temperatures in the

above range. The cold working also increases susceptibility of ASS to above phenomenon as well as for low temperature sensitization (LTS). Sensitization occurs in stainless steels containing carbon levels as low as 0.02 wt%. The probability of IGSCC occurrence increases rapidly with carbon concentrations above this level up to 0.055% and there after maintains an approximate steady rate [5]. The welding of stainless steel welded components produces a narrow band of chromium carbide in an area close to the weld, which has been heated into the sensitization range and the cracks occur primarily in this area. To overcome some of the above detrimental effects, heat treatment process is employed. However, the process should be such that it does not itself induce ill effects. The following procedure is found to provide acceptable results. 4.1 Typical furnace Specifications: Furnace type Furnace size Furnace insulation Mode of fire Max. operating temp. Min. thermocouples : : : : : : Gas-fired Furnace (Electrical type are preferred) Depending on Job size. [Typ : 5000mm (L) X 5000mm (W) X 2000mm (H)] 250mm ceramic fiber on walls and roof of furnace. High velocity oil fired burners (HSD) 1150 oC 6 nos. per charge (Calibrated by approved agency).

4.2 Heat treatment Specifications: Loading Temperature Rate of Heating Soaking Temperature Soaking Time Special Requirement : : : : : 150 oC – 200 oC 150 oC/hr. above 300 oC 1050 oC + 10 oC minimum 30 minutes (1 hr. per inch of section thickness) After soaking, the dished ends & formed components is immediately quenched in water within 60 - 90 seconds. Automated quenching mechanism is preferred.

4.3 Furnace calibration & Setup:     All thermocouples are of Nickel- Chromium/ Nickel-Aluminum of ‘K’ type. The calibrated M.I. thermocouple are held against dummy plate of same thickness with the help of T/c nuts placed on dished ends & formed component. Minimum 6 thermocouples per charge installed on the dishes. All dished ends & formed components are placed on appropriate SS fixture and kept minimum 300 mm above the refractory bricks. The fixture is supported in such a way that after completing the soaking period the job can be immediately quenched in water tank [Approx volume 200 times job volume] within 90 seconds (max.). After quenching temperature of job need to be below 200o C. The water tank capacity should be adequate around 45 Cu. meter (min.) with additional arrangement for cooling and circulation. Placement arrangement for dished ends to be as per approved sketch. Potentiometric self-compensating, type ‘K’ duly calibrated recorder, traceable to national standards. Certificate confirming the same to be handed over to QA personnel. Documents consist of Approved procedure, Heat treatment specification, Calibration certificate of temperature recorder and thermocouple, recorded Time-Temperature chart duly signed by concern authority, HSD Test Certificate & chloride level test certificate for water. The sulphur content in oil not to exceed 0.5% wt [9].

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5. Cleanliness: The parts & assemblies after solution annealing need thorough cleaning for removal of hard scales formed during heat treatment process. Earlier experience from the failure analysis of some of the equipment reveled that the contamination at any stage in fabrication stage affects reliability & its performance under use. Hence proper cleaning of all the surfaces is very important. The raw materials were thoroughly cleaned before use in order to remove traces of paint, oil, grease, dust or any other contamination. Cleaning of prepared weld edges and completed weldments was also done on immediate basis. Wire brushes used were of stainless steel and reserved specifically for SS jobs to avoid contamination of the weld surfaces by carbon steel material. All scales, dents, burrs, weld spatter, oxide, oil and other foreign materials were also completely removed from inside and outside of the vessel. The Chloride & Iron contamination checks were carried out on a continuous basis. Scales and Oxide films occurring during the welding & solution heat treatment are subjected to pickling subsequent to mechanical cleaning in order to attain a metallic bright surface which is finally passivated to attain evenly corrosion resistant oxide layer on all areas. The materials are also be subject to pickling treatment before commencement of heat treatment operations. All external and internal irregularities like tacks, dents and other effects if any and also scale formation due to solution annealing are removed mechanically. Any blemishes on the parent material were rectified and inspected by DP test. Oil, dirt, welding spatters and any other foreign matters adhering to the surface are cleaned by DM water and when required also by grinding, brushing etc. The grinding wheels employed were silicon based and were reserved for the SS jobs only. Chemical composition of pickling solution is 20 % HNO3 (70 % Concentration) with upto 2 % HF (if required) and remaining DM Water. Pickling time depends on the condition of pickling solution and the extent of thickness of scale. However, minimum 30 minutes are required at normal temperatures. During pickling, the residual slags and all black spots are cleaned by scrubbing the surfaces and the welds thoroughly with a nylon brush. Finally, all traces of acid are removed by DM water rinsing. Passivation solution consists of 15-20 % HNO3 (70 % concentration) and remainder DM water. Passivation solution is applied for 20 to 30 minutes at a temperature of 40-500 C. No brushing is done during the passivation. After passivation, all traces of acid are removed thoroughly by DM water (chloride less than 25 ppm) [9]. Finally, the surfaces are completely dried. 6. Contamination Check: Diameter of 5 sq. inch circular area of the surface to be checked is scoured with 10 % HNO3 solution laden swab. The free liquid is reabsorbed by swab and dropped into glass test tube containing 5 ml. of DM. water. Few drops of AgNO3 are then added to the solution. Evaluation of the surface contamination is done by comparing the turbidity of the spot check test solution with control sample solution. If turbidity of the spot is more than the control solution then the surface is deemed contaminated and in this case the test area should be cleaned again and re-checked to ensure effective removal of chloride contamination [9]. The check for iron-contamination consists of dropping 10 ml. of CuSO4 solution on a clean surgical swab and scouring a 5” Dia. circular area of the surface to be tested. The surface is then observed for change in colour of CuSO4 solution. If the colour of the swab changes to golden brown, the surface may be deemed contaminated with Iron and in this case the


affected area should be cleaned and re-checked to ensure effective removal of Iron contamination followed by passivation [9]. 7. Quality Assurance: The final result is determined through quality surveillance and control followed during forming, heat treatment & welding operations. Procedurally the detailed quality assurance plan was established & approved before the start of activity. Requisite inspection & tests were pre-qualified on mock-up trial pieces so as to achieve satisfactory results on production job. Apart from other non-destructive examinations visual inspection was given significant importance. Acceptance criteria specified for other NDE’s were more stringent than the codal requirement [9]. These modifications are based on hands on experience for more than 300 equipment fabrication.

8. Conclusion: It is clear that considering the use of equipment in radioactive & highly corrosive environment, special attention is required in forming, welding & heat treatment steps. Orientation of fabricator towards specific requirements is very much desired. Equally important is extensive mock-up trials to evolve right methodology to be adopted in forming, heat treatment & welding operations. 9. References: 1. 2. 3. 4. 5. A. H. Advani, L. E. Murr, D. G. Atteridge and R. Chelakara. Metallurgical Transactions 22A, December 1991, p. 2917. C. L. Briant, R. A. Mulford and E. L. Hall (1982), ”Sensitization of Austenitic Stainless Steels, I. Controlled Purity Alloys”., Corrosion, vol.38 No. 9 September 1982, p. 468 F. B. Pickering, `Physical metallurgy of stainless steel developments’, Int. Met. Rev., 21, pp 227-268, 1976. H.D. Solomon, Corrosion Vol. 41 No. 9 September 1985, p. 512. R. M. Horn and G. M. Gordon, F. P. Ford and R. L. Cowan “Experience and assessment of stress corrosion cracking in L-grade stainless steel BWR internals ”, Nuclear Engineering and Design, Vol. 174 (1997), p. 313 Mars G. Fontana, Book on Corrosion Engineering, Ed. 3 page 74. Standard Practices for detecting Susceptibility to Intergranular Attack in Austenitic Stainless Steels, ASTM A 262-02a Standard Test Methods for Determining the Inclusion Content of Steel, ASTM E 45-97 (re-approved 2002). Technical specifications for equipment fabrication, [TSE-05/P3A/183766/TECH SPECS, (R1)]

6. 7. 8. 9.

Regards. Santosh Takale,
Scientific Officer, BARC Ph - 0-9967584554.
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