Non-destructive and optical thickness measurements of steam grown oxide on contacting surfaces of power plant

E.M. Piedra1, M.J. Lodeiro2, A.T. Fry2

1

Fraunhofer IWM, Freiburg, Germany 2National Physical Laboratory, Teddington, Middlesex, UK tony.fry@npl.co.uk

Introduction
The growth of iron oxide scale (magnetite) on the inside and outside of boiler tube surfaces is a significant limiting factor that affects tube life due to its thermal insulation effect which in turn impacts on corrosion rate, spallation and metal wastage. Measurement of these oxide layers is crucial to plant asset management. Ultrasonic thickness gauging techniques have commonly been used to measure the oxide scale thickness for many years. Commercial 20 MHz longitudinal wave ultrasonic transducers can measure down to a minimum oxide thickness of approximately 250 m. By using normal incidence shear wave transducers that limit can be reduced to 125 m. However, with increasing use of higher alloyed materials a lower detection limit is needed to monitor the oxide formation and growth. The methodology used for this work demonstrates that oxide layers as thin as 65 m could be measured ultrasonically.

Experimental
Specimen design
Specimens were manufactured using a pin in collar design. This ensured close mating surfaces between the two alloys, IN738 and P92. They were then exposed to a flowing steam environment at atmospheric pressure at 650C for a set duration. The feed water used was deionized and deaerated to a level of dissolved oxygen of ~15 ppb.

Section of a pin and collar specimen with an indication of the measurement locations for (a) light microscopy and (b) ultrasonic NDE.

Oxide scale in the interface of an IN738 pin in a P92 collar exposed for 500 and 1000 hours at 650C in flowing steam.

After the steam exposure, and to facilitate the ultrasonic measurements, each specimen was machined flat over a small region of the external collar surface to remove the external oxide scale and enable good acoustic contact with the transducer. A water-based gel couplant was used on the contacting face of the transducer to improve the acoustic coupling between the transducer and the specimen. Ultrasonic waveforms were captured at three locations on each sample, covering roughly top, middle and lower regions of the pin and collar contact length. The ultrasonic measurements were made with a signal gain of around 45 dB to accommodate the small signals received due to the tightly curved internal surfaces of both the pin and collar (~6 mm diameter pin compared with a transducer contact diameter of 5 mm).

Results
Ultrasonic and optical oxide thickness measurements are presented together for comparison. The filled points are the individually measured total oxide thicknesses, considering both spinel and magnetite layers, determined by optical microscopy. The unfilled points represent the mean value of the total oxide thickness. The crosses indicate the ultrasonic thickness averages from each region. For the 500 h specimen, the ultrasonic measurements were slightly lower but within the range of the optical results for the first two regions. For the third area, the ultrasonic thickness values perfectly matched the optical measurements.

Utrasonic equipment
Pulser unit variable pulse amplitude (100 900 V) adjustable pulse energy levels impedance outputs and damping resistances  excitation pulses can be produced at pulse repetition (PRF) ranging from 100 Hz to 1600 Hz Integrated receiver unit adjustable gain from 13 to 76 dB low and high pass filters for the received signal bandwidth of the system is 50 MHz High-speed digitiser maximum real-time capture rate of 100 MHz  can be increased to 2.5 GHz using random interleaved sampling for regularly repeated signals

For these tests, a 30 MHz longitudinal wave contact transducer, with a 5 mm diameter removable polystyrene delay line, was used to measure the oxide thicknesses. The pulse excitation used was approximately 300 V negative spike amplitude, with a 12.5 MHz high pass filter and a 50 MHz low pass filter on the received signal. The digitisation rate was maintained at 1 GHz throughout. The system was operated in pulse echo mode with the same transducer acting as both transmitter and receiver. Averaging was performed on multiple consecutive signals to minimise noise and the effect of sporadic signals (usually averaged over 100 complete waveforms).

Ultrasound and optical thickness measurements for an IN738 pin in a P92 collar exposed to flowing steam at 650C for 500 hours.

Ultrasound and optical thickness measurements for an IN738 pin in a P92 collar exposed to flowing steam at 650C for 1000 hours.

The results obtained from 1000 h steam exposure are represented in a similar way. In this case a discontinuity between the inward growing Fe-Cr spinel and outward growing magnetite layer was found. The presence of this gap resulted in only the spinel thickness being measured ultrasonically. The ultrasonic results showed good agreement with the measured spinel oxide thickness in all three regions, corresponding to approximately half of the total oxide thickness, maintaining the conventional 1:1 ratio of spinel to magnetite thickness.

Similar results for this material combination were obtained after 3000 h exposure. In this sample there was unconstrained growth of the oxide at the top of the specimen, leading to higher internal porosity of the magnetite and indistinct ultrasonic signals from which quantitative measurements could not be made. For the other two regions there was good agreement between both techniques, as with the previous specimens.

Ultrasound and optical thickness measurements for an IN738 pin in a P92 collar exposed to flowing steam at 650C for 3000 hours. Ultrasonic gauging equipment and typical response from a pin and collar specimen.

Conclusions
Ultrasonic inspection is typically used in industry for inspection of both remnant metal thickness and bore oxide scale thickness, but the limited resolution may be a concern with the increased use of austenitic and superalloy materials. It has been demonstrated that improved resolution in the thickness measurement of oxide scales by ultrasonic methods can be obtained with accurate measurements becoming possible down to an oxide thicknesses of ~65 m. Previous practical limits of around 100 to 250 m have been quoted in the literature depending on the nature of the transducer being used for the measurement.

It has also been shown that: Ultrasound velocity calibration

Specimens of steam oxidised Grade 92 material were produced to enable the calibration of the oxide ultrasound velocity. These were flat coupons with dimensions of approximately 15x15x3 mm, ultrasonic measurements were compared with optical measurements, providing a calibration value for the oxide velocity of 5472 ms-1 (typically ~6000 ms-1 is quoted for oxide scales).  The ultrasonic technique is susceptible to microstructural and morphological features in the oxide. This is a characteristic of the measurement method and cannot be overcome. Use of a larger diameter transducer to improve the spatial averaging or to measure in several places in a localised area and use an average thickness value would help  Ultrasonic measurements of oxide thickness agreed very well with optical measurements where there was no integral discontinuity in the oxide scale. In these instances, the measurement correlated with the thickness of the Fe-Cr spinel layer since fracture of the interface between this layer and the magnetite layer was often seen to occur  The speed of the ultrasound wave has been measured and calibrated for steam grown oxides on a 9%Cr martensitic alloy, giving a value of 5472 ms-1, a figure somewhat lower than that usually quoted
US transit time through the oxide layer and the measured thickness.

 Considering the tight radius and difficult geometries used in this work the use of ultrasonic transducers to make higher resolution measurements of the oxide thickness has been demonstrated and should be easier to apply to large scale items such as pipe work and tubing in plant

Acknowledgements
The authors are grateful to Jim Banks and David Laing, and would like to acknowledge funding from the Department of Business Innovation and Science for the work reported in this document.

www.npl.co.uk

Queens Printer and Controller of HMSO, 2013. 10607/0913