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Microscopy: advances in scientific research and education (A. Mndez-Vilas, Ed.


Applying microscopic techniques for the investigation of the behaviour of

building materials
M. Stefanidou1, L. Papadopoulou2, E. Pavlidou3 and I. Papayianni1

Laboratory of Building Materials, Civil Engineering Department, Aristotle University of Thessaloniki 54124, University
campus, Greece
School of Geology, Aristotle University of Thessaloniki 54124, University campus, Greece
Department of Physics, Aristotle University of Thessaloniki 54124, University campus, Greece
The main challenge in construction field is to build functional, economical and durable structures. In order to accomplish
this, an essential precondition is the thorough understanding of the properties of the materials used focusing on their
microstructure. For this reason, classical microscopic techniques, like stereoscope, optical microscope and SEM remain
the irreplaceable tools for the direct observation and study of the materials. By proper combination of microscopic
techniques a deeper penetration into the structure at different scales, precious data as defects of the materials can become
evident giving answers to their macroscopic behavior and allowing interpretations for improvements. The aim of this
article is to show, after a review of the potential and limits of the microscopic tools, how these may be used to extract
concrete remarks about the examined materials.
Keywords: building materials; stereoscope; optical microscope; SEM; AFM

1. Introduction
The term microscopy is referring to the techniques through which the materials can be viewed at an appropriate scale
for examination. The image is formed by direct imaging for the optical or light microscopy and electronic processing of
the wave nature for electron microscopy. Nowadays, the research fields incorporating microscopes were multiplied and
these techniques have evolved rapidly, providing valuable and in many cases unique information. Microscopy could be
considered as one non-destructive method of analysis, since a very small sample is required. The sample size and its
representativeness, the disturbance of the sample during preparation stages as well as the necessary experience required
for gaining and evaluating the results are still some significant drawbacks on the use of these techniques.
Building materials despite their homogeneous macroscopic appearance present a rather heterogeneous structure.
Moreover, they contain a net of pores and cracks by which their mechanical strength and durability are strongly
influenced. A direct view of the pores and cracks in the material is only possible through microscopes which are the
basic tools when designing modifications for upgrading the properties of a material. The influence of supplementary
additions such as fibers, binary or ternary binding systems, different aggregates, admixtures, consolidates or surface
treatments can be efficiently recorded. The monitoring of innovative products can be made by powerful microscopes in
order to record any defects, understand their behavior or find the cause and extent of any failure. Microscopic analysis
is always used for the study of materials when they do not perform as expected causing problems to the construction.
The establishment of regulations in applying microscopic techniques for the examination of building materials
contributes to the validation of microscopic analysis in particular in the multi-phase materials [1] [2] [3]. As Sarkar
stated a micro-structural investigation is the only way to identify defects in concrete and is therefore an essential part
of any investigation [4]. Many researchers recognize microscopic techniques as a basic tool for characterizing a
material [5] [6] [7] [8] [9].

2. Review of basic microscopes

Stereoscope: This is the first step in order to study of a 3-D bulk material, even large in size, without any processing of
the sample and gain the first information about its structure. Actually, the ability to magnify the image up to x100 is an
easy and inexpensive way to distinguish the phases of the material and get an idea about its texture, pathology stage,
cohesion between inclusions (such as fibers) and binder, the existence of secondary minerals (salts, re-crystallization
phases) or distinguish multiple layers for example in the cases of mortars (substrates or renders) [10]. The type of
stereoscope used in this study was a Leica Wild M10.
Optical microscope: Optical microscopic methods are widely applied in material characterization since they allow the
observation of the internal structure of a material. Microstructure features such as grains and grain sizes, precipitates,
inclusions, pores and pore sizes, alteration products, textures, shapes and morphology of crystals or aggregates,
cracking and interfacial reactions, twin boundaries can be recognized and quantified. Also, crystallization sequence,
observe frozen-in reactions, note weathering or alteration, identification of phases and characterize the structure of a
material can be determined. For the recognition of minerals and mineral phases, a polarized optical microscope, also
called a petrographic microscope, is considered to be the basic tool. Two main types of polarizing optical microscopes



Microscopy: advances in scientific research and education (A. Mndez-Vilas, Ed.)


can be used in material characterization: transmitted light and reflected light [11] [12]. A transmitted light polarizing
microscope is used for the observation of transparent minerals while a reflected or incident light microscope is used for
the observation of metallic and opaque minerals. Examination under the polarizing microscope can be made with
parallel or crossed Nichols. In parallel Nichols only the polarizer is used and optical properties as color, relief, shape,
form and cleavage of a crystal can be investigated. In crossed Nichols an analyzer is placed into the light path at right
angle to the polarizer and optical properties such as interference colors and distinction can be examined. Examining a
thin section (2D, small size material) with transmitted light permits further understanding of the size and the percent of
voids and solid particles. The advantages of optical microscopy are the direct imaging and straightforward information.
Certain features are better visualized at low magnification, for example directional deformation and twin boundaries,
while porosity and phase fractions can be better quantified. The combination of both stereoscope and optical
microscope with image analysis systems gives a privilege to quantify the gained information. The disadvantage of this
method is the low resolution. Practically, a common optical microscope can distinguish objects that range from 1 to
100m in size, at a magnification of about 1500X, due to the light diffraction limit. Another drawback can be sample
preparation since thin sections are required from all samples studied under the polarizing microscope. In the present
study polarized microscope was Leica laborlux 12 pol s, assisted by image analysis system Qwin using a digital camera
(ProgRes c5).
Scanning electron microscopy (SEM): It has been extensively used for the material characterization, especially in
combination with energy dispersive X-ray microanalysis (SEM/EDS) [13]. The SEM technique requires electrically
conductive specimens. Insulating specimens need to be covered by a thin (110 nm) conducting surface layer, usually
applied by sputtering with gold in an argon atmosphere, or with carbon coating in vacuum. The sample size can be
maximum 10 cm in diameter and 50 mm in height, but there is a restriction in the specimens movement, so the area of
interest should be about 2.5 cm in diameter around the center of the goniometer stage. Restrictions also apply regarding
the maximum height, tilt and rotation, depending on the specific stage. This particular microscope is very effective in
morphology investigation, as easily produced micrographs provide topographical information together with the
qualitative and quantitative analysis, evaluating the characteristics of the materials. Micrographs of powder samples
may show weather the grains have irregular angular shape, if particle agglomerations composed of spherical aggregates,
or smoother surfaces and their size can be measured. The point, either area microanalysis, shows the spectra of the
elements composing the sample, with results presented in wt% and at%. SEM micrographs, highlights the diversity of
microstructures, as the combination of aggregate with the binder in the case of concrete, or the bond characteristic of
various fibrous materials, steel, fiberglass, and carbon-fiber in the reinforced cement. Micrographs of fiber surface,
shows weather the fibers are covered densely implying the good bond with cement matrix. If the bond is loose, a space
appears between fibers and in many cases they are pulled out forming a smooth surface. This characteristic indicates
aging, which causes a possible de-bonding by the decrease of the compressive strength as the years go by. Because of
long exposure, lime mortars develop failure in the mode of cracks, crumbling and erosion. By measuring, the area of
voids from micrographs taken from historical buildings, qualitative and quantitative results of the damaged area and the
materials used can be estimated. To study the ageing of various materials as they degrade with time, it is important to
analyze the microstructure changes supplemented with measurement of the area of damages in the form of micro-voids.
The micrographs reveal loose microstructures in damaged materials and uniform and dense microstructures in protected
and durable materials. The high vacuum SEM observations require specific preparation methods such as removing of
water and coating by sputtering of samples. Thus, the images in those cases represent a frozen state. The environmental
scanning electron microscope (ESEM) is a direct descendant of the conventional SEM, but also permits wet and
insulating samples to be imaged without prior specimen preparation the ESEM. For example it allows the observation
of samples with different content of water phase [14] [15]. The SEM used for this study is a JSM 840 A, assisted by
Atomic Force Microscopy (AFM): The conventional use of AFM is the study of surface topography both visualize
and quantify it. This information has been investigated in relation to other properties such as elastic properties,
hydration degree and binder determination [16]. These possibilities as well as their combination with other techniques
constituted AFM a popular tool in studying composite materials. This technique is advantageous in relation to other
imaging techniques as a reliable 3D image of the sample surface at very high resolution is achieved and it doesnt
require any sample preparation or coating. Its main limitation is the tip convolution which affects tiny dimensions. The
AFM used for this study is NT-MDT, Negra.

3. Detection of deterioration
Most building materials are porous and susceptible to deterioration. This process is usually slow and results from the
effect of environmental conditions on materials. Different mechanisms can intriguer deterioration and their combination
with the materials used can naturally lead to a certain macroscopic pattern. Microscopic techniques can assist on the
study of the whole spectrum of deterioration and find the predominant mechanism [17] [18]. Starting from the
macroscopic image and going deeper up to the crystal unit means that a researcher can see all the path of the procedure.
The cause, the type and the depth of deterioration is possible to be determined by microstructure investigation [19].



Microscopy: advances in scientific research and education (A. Mndez-Vilas, Ed.)


Determining the cause of deterioration is important in order to understand mistakes during designing or applying the
materials and by this way it is important to improve the materials properties and also it is crucial in order to organize
the appropriate repair procedure. For the heterogeneous materials such as concrete and mortars with features ranging
from nano to centimeters, microscopy can give information concerning the size, the distribution and the topology in
detail [20] [21]. Figure 1 demonstrates the presence of salts as recorded under different microscopes for mortars where
salts are in abundance and degradation phenomena were macroscopically observed.

Fig. 1 Mortar from the Medieval walls in Rhodes a)under stereoscope (x8) where pore within crystallized salts is observed,
b)under polarized microscope (x150) the presence of angular crystal salts are shown and c)under SEM the morphology and
composition of salts can be recorded.

Figure 2 indicates the presence of salts (ettringite) in concrete sample causing a strength reduction as recorded from
25MPa to a healthy sample to 10.5MPa in the sample with salt presence.

Fig. 2


Weight %
















Ettringite fibres inside a concrete structure and the analysis of the fibres by EDS.

Basic minerals in the composition of building materials are often altered causing further degradation problems. For
example orthoclase and plagioclase are two minerals of the feldspar group. They both have a hardness of 6, on the
Mohs scale. Under chemical weathering, orthoclase is altered to kaolinite, a clay mineral, with a hardness of 2-2.5,
while plagioclase is often hydrothermally altered to sericite, a fine-grained mica, with an equal hardness (Figures 3 and
4). As a result, the decrease of mechanical resistance is inevitable. Furthermore, kaolinite can be dissolved from the
material causing secondary porosity formations.



Microscopy: advances in scientific research and education (A. Mndez-Vilas, Ed.)


Fig. 3

Alteration of orthoclase to kaolin (parallel Nichols)

Fig. 4

Alteration of plagioclase to sericite (parallel Nichols left and crossed on the right

4. Characterization of porosity and crack pattern

Porosity is a basic characteristic of materials influencing most of their properties such as mechanical strength,
deformation, resistance to weathering, insulating properties. There are many, widely applied, indirect techniques for
porosity measurement. The major advantage that the microscopic techniques offer is that pore structure has an image
and as the observation is direct, the exact size and position of the pore can be identified. In this way pores and cracks
occurring inside the matrix or in the transition zones can be distinguished. Microscopic techniques are the only methods
that can relate porosity with pathology [22] [23]. Additionally, a wide range of pore sizes can be characterized. Cracks
in the materials microstructure pre-exist or are formed during the service life of materials. Their topography recorded by
microscopy of different magnification capacity, allows concluding about the main mechanism responsible for them [24]
[25]. For example, cracks in the cement matrix of concrete may be related to sulfate attack and ettringite or thaumasite
is easily detected from the characteristic crystals. Similarly, cracks originated from aggregate grains may be attributed
to alkali-aggregate reaction and the products of this reaction can also be microscopically identified. Cracks in limebased mortars are mainly localized in the transition zone around aggregates and they are often filled with re-crystallized
calcite which contributes to the increase in density and strength of mortars (Figures 5, 6).

Fig. 5

Pore size distribution in mortar using stereoscopic observation and image analysis system



Microscopy: advances in scientific research and education (A. Mndez-Vilas, Ed.)


Fig. 6

Re-crystallization of calcite in the contact zone of binder-aggregate filling the crack

5. Detection of interfaces
In composite materials many interfaces exist which are considered as the weak phases of the materials and special care
is given to reinforce them. Good compaction, proper additives are often used to avoid weak zones and increase long
time service life of materials [26] [27]. The microscopic investigation of the interfaces provides information about the
techniques used for building with these materials. Indicatively it can be mentioned that in high quality old mortars taken
from monuments, the interfaces between brick-mortars or bedding mortar-renders or even mortar-mortar are quite
compact (Figures 7,8,9). In many cases the microscopic examination showed chemical reaction products between the
bonding materials (Figure 9). In the case of a roller compacted concrete pavement the cold joint due to premature
setting and inadequate compaction of concrete implies for a low performance pavement.

Fig. 7

Interface zones under stereoscope x8 a) stone-mortar b)mortar render c)brick-mortar

Fig. 8


Interface zones under polarized microscope x150 a)brick-mortar b)mortar-render and c)two mortar layers


Microscopy: advances in scientific research and education (A. Mndez-Vilas, Ed.)


Fig. 9

SEM micrograph of contact zone of 30m thickness between brick fragment and binder

6. Study of surface characteristics

Building materials are exposed to environment and the quality of their surface used as the skin of a structure is of great
importance for their long service life. Density, roughness porosity, permeability, hydrophobicity are some of them.
Since the science of films has been impressively developed the use of AFM in testing surface characteristics has been
extended [28] [29]. Recording the effectiveness of a hydrophobic treatment on stone (marble) surfaces using nanomodified coatings, AFM measurements indicate different succeeded roughness justifying different behavior (Fig 10).

Fig. 10
one (a)

AFM images demonstrating the acute nano-roughness accomplished in nano-modified coating (b) in relation to untreated

7. Conclusions
Microscopes are valuable tools to the researchers in order to detect the damages, identify phases and develop improved
materials used in the construction field. The ability of penetrating and having a direct observation of the structure in the
scale of micro or nano allows the detection of the inherent defects as well as ageing or deterioration effects which
determine the behavior of the material. The study of building materials has benefited greatly from the microscopy. The
evolution and specialization of building materials in order to cover different construction needs was in a significant
extent based on them.


ASTM C856 - 13 Standard Practice for Petrographic Examination of Hardened Concrete

ASTM C1324 Examination and Analysis of Hardened Masonry Mortar
ASTM C1721 - 09 Standard Guide for Petrographic Examination of Dimension Stone
Sarkar S. H. The importance of microstructure in evaluating concrete Advances in concrete technology ed. V.M. Malhotra,
CANMET Ottawa, Canada, MSL 94-1, 1994 123-202



Microscopy: advances in scientific research and education (A. Mndez-Vilas, Ed.)




Middendorf B., Hughes J. J., Callebaut K., Baronio G. and Papayianni I. Investigative methods for the characterization of
historic mortars- Part 1: Mineralogical characterization. Materials and Structures, 38, 2005, RILEM Technical Committees,
Scrivener K.L. Microscopy methods in cement and concrete science Cement Research and Development 1997, p.92-112
Lindqvist J. E., Sandstrom M. Quantitative analysis of historical mortars using optical microscopy. Materials and Structures,
vol.23 Number 10, 2000 RILEM Technical
Elsen J. Microscopy of historic mortars a review. Cement and Concrete Research 36, 2006, 1416-1424
Charola A.E. Salts in the Deterioration of porous media: An overview JAIC 39, 2000, 327-343
Papayianni I., Stefanidou M. Microstructural analysis of Old Mortars of Byzantine Period International Conference
STREMAH, Bologna, Italy, Editor C.A. Brebbia, 2001, pp. 45-52
Davidson M.W and Abramowitz M. Optical microscopy. ed. John Wiley & Sons, Published Online: 15 JAN 2002, DOI:
Yang Leng. Introduction to Microscopic and Spectroscopic Methods Materials Characterization ed. John Wiley & Sons, 2008,
Pavlidou E., in Conservation science for the cultural heritage, Springer, 2013, Ch 3.2.
Donald A.M. The use of environmental scanning electron microscopy for imaging wet and insulating materials Nature
Materials 2, 2003, p.511 - 516
Garca Santosa A., J.Ma. Rincnb, M. Romerob, R. Taleroc Characterization of a polypropylene fibered cement composite
using ESEM, FESEM and mechanical testing Construction and Building Materials, 19,2005, 5, 396403
Peleda A., J. Castro, W.J. Weiss Atomic force and lateral force microscopy (AFM and LFM) examinations of cement and
cement hydration products Cement & Concrete Composites 36 (2013) 4855
Sarkar S.L., S. Chandra, M. Rodhe Microstructural investigation of natural deterioration of building materials in Gothenburg,
Sweden Materials and Structures 1992, vol. 25 p.p 429-435
Riccardi M, Lezzerini M, Caro F, Franzini M, Messoga B (2007) Microtextural and microchemical studies of hydraulic ancient
mortars: Two analytical approaches to understand pre-industrial technology processes. Journal of Cultural Heritage 8: p.350360
Grattan-Bellew P.E. Microstructural investigation of deteriorated Portland cement concretes Construction and Building
Materials 1996, Vol.10, No1, 3-16
Larbi J.A. Microscopy applied to the diagnosis of the deterioration of brick masonry Construction and Building Materials 18
(2004) 299307
Larbi JA., Visser JHM Diagnosis of chemical attack of concrete structures: the role of microscopy Proc. 7th Euroseminar on
Microscopy applied to Building Materials Delft The Netherlands 1999, 55-65
Fitzner B. Porosity analysis- A method for the characterization of building stones in different weathering stages Engineering
Geology of Ancient Works Monuments and Historical Sites, 1990, p.2031-2037
Stefanidou M. Methods for measuring porosity of lime-based mortars Construction and Building Materials 24, 2010, 25722578
Robinson G.C. 1984 The relationship between pore structure and durability of brick Ceramic Bulletin vol.63 No2 295-300
Daniel Q. et.al. Microstructure and transport properties of porous building materials Materials and Structures Vol.31 Issue
209 June 1998 pp.317-324
Lawrence S.J., Cao H.T. 1987 Microstructure of the Interface between brick and Mortar Proc. 8th International Brick/Block
masonry conference Dublin Ed. J.W. DeCourcy vol.1 194-204
Barnes B.D. Diamond S. Dolch W.L. Micromorphology of the interfacial zone around aggregates in Portland cement mortar
The American Ceramic Society 62 1979, 21-24
Manoudis P.N., A. Tsakalof, I. Karapanagiotis, I. Zuburtikudis, C. Panayiotou Fabrication of super-hydrophobic surfaces for
enhanced stone protection Surface & Coatings Technology 203, 2009, 13221328
Zielecka M., Bujnowska E., Silicone-containing polymer matrices as protective coatings: Properties and applications Progress
in Organic Coatings, Volume 55, Issue 2, 2006, p. 160167