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Proc.

International Conf on Surface Techniques (INSURE-2001), Chennai, India

NON-DESTRUCTIVE TESTING METHODS FOR INVESTIGATION


OF SURFACES OF MATERIALS

T. Jayakumar, B.P.C. Rao and S. Thirunavukkarasu


Division for PIE and NDT Development
Indira Gandhi Centre for Atomic Research
Kalpakkam – 603 102, Tamil Nadu
Phone: 04114 40208, Fax: 04114 40356, e-mail: tjk@igcar.ernet.in

ABSTRACT

Surface modification or coating of engineering materials is routinely followed in


automobile, power, aerospace and other industries to enhance resistance to corrosion, wear,
and fatigue and to improve high temperature properties. NDT techniques are being
increasingly applied for characterisation of surfaces of materials. This paper discusses details
of various conventional and advanced NDT techniques for characterisation of material
surfaces with due emphasis to capability, applicability and limitations.

1. INTRODUCTION

The surface characteristics of a component are very important. Many engineering


components in automobile, power, and aerospace industries are required to possess wear or
corrosion resistant surface properties as well as tough and shock-resistant bulk properties.
Since, it is the surface/sub-surface region where fatigue cracks originate, as a remedial
measure, good surface finish, high hardness with adequate toughness and residual
compressive stresses are ensured on surface of engineering components. For this purpose,
surface treatment processes such as shot peening, case carburising and nitriding and induction
hardening are usually given. Some times, surfaces are cladded or bonded with hard layers and
also are modified or coated for better appearance.

In general, surfaces with desired quality and characteristics are obtained through
thermal, mechanical, chemical and electrochemical processes. During these processes, the
pre-service quality of surfaces is ensured by assessing the technological properties such as
tensile strength, hardness, surface roughness, and residual stresses and for the absence of
detrimental defects [1]. For this purpose, destructive and non-destructive testing (NDT)
methods are required. Destructive methods are always sampling methods and provide a
statistical certainty only. In addition, they are time-consuming and difficult to integrate into
production lines. On the other hand, there is a high demand for NDT methods for application
at industrial scale, especially for large and expensive components, especially due to high
speed of testing and reusability of component after testing [2]. NDT techniques are also
applied on operating components for detection as well as characterisation of degradation in
surface characteristics [3]. NDT techniques can be classified into surface and volumetric
techniques, depending on the interrogation volume and the information content. For
investigation of surfaces, surface techniques such as liquid penetrant, magnetic particle, eddy
current, and thermography are preferred to radiography and ultrasonic techniques, which are
volumetric techniques. Ultrasonic surface waves are employed for characterisation of
surfaces. Each technique has certain capabilities and limitations. For example, techniques like
liquid penetrant require removal of paint, dirt etc. from the surfaces, on the other hand,
magnetic particle and eddy current techniques do not require. Thus, great care is required
while selecting an NDT technique.

Recently advanced NDT techniques such as laser scattering, magnetic Barkhausen


noise, X-ray diffraction, pulse thermography, atomic force microscopy, and scanning acoustic
microscopy are also being used for investigation of material surfaces. Like in the case of
conventional NDT techniques, selection of advanced techniques is also very important and is
dependent on three important aspects viz. capability, applicability, and limitation of the
techniques. In some situations, it may be necessary to employ more than one technique. This
paper discusses details of various conventional and advanced NDT techniques for
characterisation of surfaces of materials. Due emphasis will be given to the recent NDT
techniques applied for ensuring manufacturing quality and evaluation of in-service
degradation of surface characteristics. In an effort to guide readers to choose appropriate NDT
technique for a specific application, the three important aspects mentioned above are critically
assessed in this paper.

2. NON-DESTRUCTIVE TESTING METHODS

2.1 Ultrasonic Methods

Ultrasonic methods use sound waves having frequencies usually in the MHz range. A
sound wave travelling through a material will lose energy when it encounters a defect.
Ultrasonic waves can penetrate into materials, thus it is possible to study the microstructure of
materials, detect small defects, study adhesive interfaces, and also to gain information about
elastic properties. The two basic ultrasonic techniques are through transmission and pulse
echo. The widely used wave modes in NDT are the longitudinal waves and the shear waves.
These waves are used for determination of thickness of materials as well as coatings in
addition to evaluation of materials with respect to defects, microstructures and residual
stresses. Ultrasonic methods are also used for evaluation of debonds and delaminations in a
variety of materials. For characterisation of surface defects, surface Rayleigh waves and lamb
waves are used. It is possible to use surface waves to evaluate the bond quality. Ultrasonic
back scattering technique is used to characterise the surface layers in the case of case
hardened components. For estimation of grain size in the surface regions, surface wave modes
have been employed using parameters such as amplitude of back-scattered leaky Rayleigh
wave and amplitude of Rayleigh surface wave.

Ultrasonic methods have been applied to measure hardening depth which is defined as
the distance from the surface where the hardness drops below a specified value. For
hardening depth more than 3 mm, ultrasonic immersion technique is employed and the time
of flight between surface echo and rising part of the back-scattering signal is used for
determination of hardening depth, with the knowledge of ultrasonic velocity and the angle of
propagation of ultrasonic waves in the material. Making use of the developments in
electronics and lasers, a few ultrasonic imaging methods have been developed in the recent
times. Two such microscopy methods which use ultrasonic waves of frequencies from
approx. 10 MHz - 2 GHz namely, Scanning Acoustic Microscopy (SAM) and Scanning Laser
Acoustic Microscopy (SLAM) are discussed here.

In SAM, a focussed ultrasonic beam is used for imaging, analogous to optical


microscope. The wave generated by the ultrasonic transducer is focussed by the acoustic lens
and then partly reflected at the object. The amplitude and/or phase of the waves returning to
the transducer are measured. If the distance between the lens and the object is kept in the
focus, and the amplitude of the returning sound wave is recorded as a function of the object
surface co-ordinates, an acoustic image of the object surface is obtained. The contrast in the
acoustic images is determined by the elastic properties of the material, i.e. by the variations in
the acoustic impedance. SAM can be used to evaluate corrosion attack and to characterise
machined ceramic surfaces. Ceramic materials are usually brittle despite their impressive
material strength due to the lack of plastic deformation. For improved surface properties,
ceramic materials are coated or deposited, e.g. carbide, carbonitride, diamond tipped tools etc.
SAM can be used to assess micro-crack damage in ceramics. SAM can detect defects smaller
than 100 microns, which are missed by conventional non-destructive techniques.

The operating principle of a Scanning Laser Acoustic Microscope (SLAM) is outlined


in Fig.1. A sample is insonified at an angle with respect to the surface of the sample. The
ultrasound causes a dynamic ripple of the opposite surface in a homogenous sample, off
which a laser beam is reflected and guided on a photodiode. The ripples cause the laser beam
to be partially diffracted and frequency-shifted, which is demodulated by knife-edge
detection. The amplitude of the AC component in the photodiode is proportional to the
amplitude of the ripples. The ultrasonic wave is scattered and reflected by pores, inclusions,
cracks and debonding, which in turn become visible as a modulation of the otherwise
homogenous surface ripple. By scanning the laser beam over the sample, these modulations
are displayed on a computer. The resolution in such images is given by the wavelength  of
the ultrasound and is typically 50 m. By measuring both the amplitude and the phase of this
holographic acoustic field, one can reconstruct the defect geometry. SLAM methods are
increasingly used for detection of very fine defects in ceramics used in electronic applications
such as microcircuit packages and substrates.

2.2 Eddy Current Methods

Eddy current testing (ECT) method uses the principle of electromagnetic induction to
test electrically conducting components for detection and characterisation of defects [2]. An
alternating magnetic field generated by an excitation coil induces eddy currents in the coating
or substrate. According to Lenz's rule, the magnetic field of the eddy current reduces the
exciting field which can be measured as impedance change of the excitation and, if present, of
a separate receiving coil. Due to ‘skin effect’, ECT methods can readily detect surface defects
and usually high frequencies are employed for detection of very fine defects. In general, the
amplitude and phase angle of ECT signals are used for evaluation of size of defects. Besides
detection of defects, ECT methods are widely used for determination of hardness, corrosion,
grain size, and thickness of the coatings, especially non-conductive on metals. In case of
conductive coatings, the conductivity ratio between the coating to the substrate must be
sufficiently high. The thickness of non-magnetic coatings on ferromagnetic substrates can
also be measured by magnetic adhesive force method [refer to ISO 2178 standard]. Brief
details of this method are discussed in section on magnetic methods.

2.2.1 Eddy Current Imaging

Imaging techniques have the potential for automating the measurement process and
providing estimates of defect sizes from the image data. Eddy current imaging is a recently
emerging trend. An imaging system has been built at the authors’ laboratory to generate eddy
current images of defects. This involves scanning the material surface in a raster, measuring
the impedance change point by point and displaying the impedance data in grey level or
colour images. Eddy current images of welds, notches, corrosion pits and cracks have been
studied. In order to quickly detect and automatically evaluate surface defects, an intelligent
imaging scheme has been developed. This scheme has been successfully applied to austenitic
stainless steel welds for detection and evaluation of defects in the presence of microstructural
variations, -ferrite, surface roughness and edge effect (Fig.2). Application of this scheme to
SS plates and welds has resulted in a high probability of detection and ten-fold reduction in
the imaging time, besides ensuring accurate three-dimensional reconstruction of defects.

2.2.2 Pulsed Eddy Current Testing

For accurate characterisation of hidden corrosion in multi-layered aircraft structures, a


new method called pulsed eddy current (PEC) testing is being applied [5]. In contrast to
conventional eddy current methods, pulsed eddy current (PEC) excites the probe's driving coil
with a repetitive broadband pulse, such as a square wave. The resulting transient current
through the coil induces transient eddy currents in the test piece, associated with highly
attenuated magnetic pulses propagating through the material. At each probe location, a series
of voltage-time data pairs are produced as the induced field decays, analogous to ultrasonic
inspection data. Since a broad frequency spectrum is produced in one pulse, the reflected
signal contains depth information of the material. Physically, the pulse is broadened and
delayed as it travels deeper into the highly dispersive material. Therefore, flaws or other
anomalies close to the surface will affect the eddy current response earlier in time than deep
flaws. The modes of presentation of PEC data are analogous to ultrasonic methods in the
form of A-, B- and C-scans and allow detailed characterisation of defects [4].

2.3 Thermographic Methods

Thermography refers to the mapping of the temperature profiles on the surface of an


object. The method is non-contact dry, safe, fast and displays results of inspection in a
convenient visual format, which make it attractive for inspection of operating components
and plants. Pulse thermography is a new technique and this allows a faster and reliable NDE
of large areas of coated surfaces with good resolution [7]. This technique employs a heat
source that produces a well-defined heat impulse. This impulse can be single or continuously
modulated. The impulse is directed towards the examined surface and reflected signal is
collected by infrared camera and subsequently processed in a computer. Differences in
coating thickness, coating and adhesion defects, microstructural changes, an aggregation of
pores as well as oxide or metallic inclusions cause a significant change in the signal intensity
and are therefore detected. Pulse thermography can detect defects as small as 20 to 100 m in
thermal spray coatings. Other advantage of this technique is its applicability for early
detection of growing defects.

2.4 Laser Methods

Laser based methods are finding increasing applications in specialised areas because
of the high sensitivity achievable and also because of the non-contact nature of
measurements. Some of these techniques include laser scattering for surface roughness
characterisation & for fatigue damage assessment, and laser holographic interferometry for
detection of defects in surface modified layers/coatings and for detection of cracks/ debonds
in composite specimens. These techniques are employed as part of qualification procedure
and also for assessment of in-service degradation of surfaces [8]. One most widely used
method is the laser scattering method. This is applied for the evaluation of surface roughness,
fatigue damage, defects in surface modified coatings/layers and for the detection of crack/
debonding in composites. In this method, a laser beam from a He-Ne laser is allowed to fall
on a specimen whose surface characteristic is to be evaluated. The scattered radiation falls on
a translucent screen held at a distance of 600 mm from the specimen. The screen is placed
perpendicular to the specular directions of the beam. A charge coupled device (CCD) camera,
interfaced to a computer through an image acquisition card, is placed in line with the specular
direction behind the screen. The laser scattering parameters such as peak height and full width
at half maximum are used for the evaluation of surface characteristics. The laser scattering
parameters have been used for on-line monitoring of corrosion specifically intergranular
corrosion and also for assessing the surface quality of artificial heart valves. Laser scattering
method has also been applied to study the periodic wall thickness variations in nuclear fuel
cladding tubes, indigenously manufactured at Nuclear Fuel Complex, Hyderabad. Typical
projected interferometry patterns of a good surface and a region with periodic thickness
variations is shown in Fig.3. Thickness variations of the order of 25 microns have been
characterised using the laser scattering method. This method has also been used in quality
control of soft surface components, and in finding the surface roughness of thin wires. This
method, being non-contact, has potential for high temperature applications.

2.5 Atomic Force Microscopy

The methods to evaluate the roughness at the surface of solids based on either
mechanical contacting or optical non-contacting sensors are applicable for coatings and
layers, too. Atomic Force Microscope (AFM) is the latest development in this area. The
working principle of an AFM is as follows. A cantilever, which is extremely sensitive to
weak forces, is fixed at one end and the other end has a sharp tip, which gently touches the
surface of a sample. When the surface is sampled, because of the ultra-small repulsive forces
existing between the tip atoms and the surface atoms of the sample, the cantilever will move
up and down in the direction vertical to the surface of the sample. The topographic images are
obtained by recording the deflections of the cantilever corresponding to the contours of the
interaction force between tip and surface atoms of the sample. AFM is applied to measure
surface roughness in small areas (<100 µm) with contact as well as without contact.

2.6 X-ray Methods

X-ray methods find various applications in material science. A few important X-ray
methods and their applications are covered in this section.

2.6.1 X-ray Fluorescence Method

In the case of X-ray fluorescence method (refer to ISO 3497 standard), the specimens
are exposed to X-rays. X-rays cause the atoms to emit fluorescence radiation with
characteristic line spectra of the elements of the substrate and all the layers of the coating. The
intensity of fluorescence radiation, among other things, depends on density and thickness of
layers. Provided the density is known, the thickness and composition of up to three layers of a
multi-layer coating can be measured simultaneously without restrictions regarding the
material type. The thickness range and measurement accuracy depend on the material
combination. The method has found a wide range of applications, such as metal finishing,
microelectronics and data storage [9].

2.6.2 Beta Back-scattering Method

The intensity of electrons back-scattered from an element under exposure to an


electron beam depends on the atomic number. In case of coating-substrate systems, the
effective intensity, which is a measure for the coating thickness, ranges between two limits
that correspond to the intensities of coating and substrate. In the beta backscatter gauge (refer
to ISO 3543 standard), this dependency is used. Coating and substrate can be both metallic
and non-metallic. Due to the measuring principle, only mono-layers can be studied and their
atomic number must sufficiently differ from the one of substrate (more than 20 %). The
measuring range depends on coating-substrate material combination and hence a suitable beta
source has to be selected to meet the specific application [9].

2.6.3 X-ray Diffraction

In some of the cases (fatigue, stress corrosion cracking etc.), it is the surface residual
stress condition, which determines the life of the components. The most reliable method to
measure residual stresses is the X-ray diffraction (XRD). The technique measures the inter-
planar spacing of the lattice with the help of Bragg’s diffraction condition (2d sin = n). If
there is any strain in the grains, the diffraction peak gets shifted from the strain free peak
position. Using the shift in the peak position, the strain or stress can be calculated. This
diffraction takes place from a thin surface layer (approximately 20 - 40 m) and hence gives
strain information only from the top most surfaces. PC-based systems are now available for
reliable and rapid measurement of stresses. Adequacy of post weld heat treatment for
relieving residual stresses in autogenous butt weld joints of 2,25 Cr-1Mo steel tubes has been
assessed using XRD technique in the authors’ laboratory. XRD based residual stress
measurement method has been developed for assessing the extent of fatigue damage and also
the quality of rejuvenation process in landing gears of aircrafts [10]. The applicability of the
XRD technique is, however, restricted to crystalline materials.

2.7 Magnetic Methods

Magnetic methods are potential methods for evaluation of surface manifestations such
as microstructural degradation, residual stresses, surface roughness and defect detection in
surface coatings of magnetic substrates.

2.7.1 Magnetic Adhesive Force Method

Magnetic adhesive force method uses the distance dependency of the magnetic
attractive force between a ferromagnetic substrate and a permanent magnet touching the
surface of coating, which must be made from a non-magnetic material. If the thickness is less
than 15 µm, an absolute accuracy of about  1.5 µm can be achieved [9].

2.7.2 Magnetically Inductive Method

Another popular method is the magnetically inductive method (refer ISO 2178
standard) which is based on measuring the magnetic flux that passes through a non-
ferromagnetic coating into a ferromagnetic substrate. Under these circumstances, the
magnetic flux depends on coating thickness and can be applied for measuring the thickness of
monolayers and multi-layers. For multi-layer coatings, however, the total thickness can only
be evaluated [9].

2.7.3 Magnetic Barkhausen Emission Method

Magnetic flux perturbations and acoustic emissions are generated when an induced
magnetic field is swept in a hysteresis loop in ferromagnetic materials. This is referred to as
Magnetic Barkhausen Emissions (MBE). MBE signals are produced as a result of sudden
irreversible motion of magnetic domain walls as they break away from pinning sites. Hence,
the MBE depends on the interaction of domain walls with pinning sites. The MBE is detected
using coils kept on the surface or sometimes encircling the sample. Surface characteristics
such as hardness, residual stress and fatigue damage have been shown to influence
Barkhausen activity and MBE technique is routinely used for evaluation of these
characteristics both on production-line and in operating components [11]. High resolution
MBE scanning systems that can be used for studying magnetic uniformity and stress
concentrations near defects have also been developed. The MBE techniques provide surface
information from the top layers of 100 to 300 m thickness.

3. SUMMARY

NDT techniques are being increasingly applied for detection as well as


characterisation of surfaces of materials. The widely used NDT techniques for
characterisation of surfaces are discussed in this paper. The range of surface thickness and the
measurement accuracy (refer Table 1) as well as the capability, applicability, and limitation of
each technique is different (refer Table 2). This calls for a careful selection of appropriate
technique for a specific industrial need or application. With advent of portable, efficient and
low-cost of electronic components, more developments are taking place as regard to
designing and developing smart instruments and sensors to characterise material surfaces.
Techniques which have been catering to the laboratory needs, e.g. acoustic microscopy are
being used in industrial applications and NDT methods are being accepted more and more in
the industry for achieving high quality levels, profitability and reputation. The role of NDT
for characterisation of materials surfaces is expected to grow further in the near future.

4. ACKNOWLEDGEMENTS

The authors wish to thank Dr. Baldev Raj, Director, Materials, Chemical and
Reprocessing Groups, Indira Gandhi Centre for Atomic Research, Kalpakkam for his
encouragement. The authors also thank a large number of their colleagues from the Division
for PIE & NDT Development, IGCAR, for many useful contributions and discussions.

REFERENCES

1. W.N.Reynolds, NDE of Protective and Thermal Barrier Coatings: A Current Survey,


NDT International, Vol. 20, 1987, pp. 153-156.
2. Baldev Raj, T. Jayakumar and B.P.C.Rao, Non-destructive Testing and Evaluation for
Structural Integrity, SADHANA, Vol. 20, 1995, pp. 5-38.
3. A. Clough, NDE Applications to Materials Processing, eds. O. Buck and A.M. Wolf,
ASM, 1987, p. 3.
4. A. Briggs and W. Arnold, Advances in Acoustic Microscopy, Vol. 2, Plenum Press, New
York, 1996.
5. B.A.Lepine, B.P. Wallace, D.S.Forsyth and A. Wyglinshi, Pulsed Eddy Current Method,
NDT.Net, January 1999, Vol. 4, No.1.
6. B.P.C. Rao, Baldev Raj, T. Jayakumar and P.Kalyanasundaram, An Intelligent Imaging
Scheme for Automated Eddy Current Testing, J Non Destr. Test. & Eval., Elsevier, UK,
2000 (in press).
7. A. Florin, New and reliable method for non-destructive and non-contact testing of thermal
spray coatings, Insight Vol. 42, No 9, September 2000, pp. 606-607.
8. C. Babu Rao, Studies on laser scattering to characterise surfaces, Ph.D Thesis, Submitted
to Madras University, 2000.
9. H.A.Crostack, NDT of Coatings, Surface Modified Layers and Adhesives, Encyclopedia
of Materials Science and Technology, Mechanical Testing and NDT, Elsevier Publ., UK,
2000 (in press).
10. T. Jayakumar, Sanjay K.Rai, V.Moorthy, S.Vaidyanathan and Baldev Raj, Experiences on
Fatigue Damage Assessment using NDT Techniques, in Materials Ageing and Life
Management, Proc. Int. Symposium (ISOMALM – 2000), October 2000, Kalpakkam, eds.
Baldev Raj, K.Bhanu Sankara Rao, T.Jayakumar and R.K.Dayal, pp. 538-546.
11. S. Vaidyanathan, V. Moorty, T. Jayakumar and Baldev Raj, Estimation of Carburisation
Depth in Service Exposed Ferritic Steel using Magnetic Barkhausen Noise Measurements,
Materials Evaluation, 56, 1998, pp. 449-452.

Table 1: Measuring range and accuracy


of NDT methods to measure thickness.

NDT Method Range of Measuring


Thickness Accuracy
[µm] [%]

Eddy current 2  103 0.5  10


Magnetic 5  104  10
adhesive force
Magnetically 5  104  10
inductive
X-ray 0.1  200 1  10
fluorescence
Beta back- 0.2  800 1  10
scatter
Thermal waves 1..103 1 .. 5
Ultrasonic
pulse-echo > 100  10
Ultrasonic
back-scatter > 500 100
Acoustic > 10 2
microscopy
Atomic force <100  10
microscopy Fig.1 Operating principle of scanning laser
Laser scattering <100  10
acoustic microscopy.
Table 2: Summary of capability, applicability, and limitation of various NDT techniques for
detection and characterisation of defects in materials.

NDT Materials Defect Detection Defect Characterisation


Technique Applicable Surface Internal Length Depth Location Orientation
Visual/ Penetrant All √ X √ X * X
Laser/ Optical All √ X √ X * X
Magnetic Ferritic √ * √ * * *
Ultrasonic All * √ √ √ √ √
Eddy Current Conducting √ * √ √ √ *
X-Radiography All * √ √ * * *
Thermography All √ * √ X * X

√ - possible X - not possible * - feasibility exists

Fig. 2 Raw eddy current image (left) of a defect in a stainless steel weld with defect masked
by the weld variations and image of the same region (right) after application of the intelligent
imaging scheme.

(a) Smooth profile (b) Distorted profile

Fig.3 Projected laser interference fringes for smooth and distorted regions in stainless steel
cladding tubes.

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