Pesce et al.

Herit Sci (2021) 9:72

https://doi.org/10.1186/s40494-021-00546-9

RESEARCH ARTICLE Open Access

Towards a better understanding

of hot‑mixed mortars for the conservation
of historic buildings: the role of water
temperature and steam during lime slaking
Cecilia Pesce1, Martha C. Godina1, Alison Henry2 and Giovanni Pesce1*

Abstract
According to various historic accounts and material evidence, the practice of producing lime mortars by mixing
the quicklime with the sand (i.e. hot-mixing) before first slaking it with water was much more common in the past
centuries than appreciated by most contemporary academics, conservation professionals and craftsmen. However,
in the last 10 years, there has been resurgence in interest in hot-mixing. In such systems, the steam developed during
the mixing is supposed to be crucial in determining the superior characteristics of the mortars, but in-depth investiga-
tions on the role of steam in hot-mixing are very few. This study reports the results of some experimental work inves-
tigating the effects of water temperature and steam used for lime slaking on the characteristics of lime and related
mortars. In these tests, calcic quicklime was slaked in water at 20 and 75 °C, and with steam at 90 °C. Microstructure
and mineralogical characteristics of the hydrates were characterized by scanning electron microscopy (SEM) and X-ray
diffraction (XRD). Mortars produced with these limes were tested for fresh (water retention and flowability) and hard-
ened (compressive and flexural strength) properties. Carbonation was assessed using SEM, XRD and phenolphthalein
tests. Results show that steam-slaked lime is characterised by portlandite crystals with smaller crystallite size and
significantly different microstructure compared to that of water-slaked lime. Results also show that mortars made with
steam-slaked lime have higher water retention and flowability than the mortars produced with water-slaked lime.
Under conditions of comparatively low relative humidity (c 40–50%), carbonation is slower in the steam-slaked lime
mortar due to the lower water content compared to water-slaked lime mortars. Overall, these results confirm anecdo-
tal reports of better workability and water retention and suggest that this production technology, which is only rarely
used nowadays, can produce mortars with improved characteristics, and provide a means by which to match the
performance of some historic mortars, and create compatible materials for conservation and restoration work.
Keywords: Hot-mixed lime mortar, Water retention, Water demand, Mechanical properties, Steam slaking

Introduction used nowadays by a few specialists [1–3]. Such techno-

Recent years have seen a growing interest in a traditional logical process differs from the more common ‘wet’ mix
method of mortar production, generally referred to as in the fact that quicklime is mixed with sand without
‘hot-mixing’, that was widely used in the past but is only being first slaked with water. Although slightly differ-
ent approaches can apply to this production process, the
basic method is essentially the same across the world and
*Correspondence: [email protected] throughout time. What makes this technology ‘different’
1
Department of Architecture and Built Environment, Northumbria
is the fact that the slaking is achieved through the mois-
University, Newcastle upon Tyne NE1 8ST, UK
Full list of author information is available at the end of the article ture of the sand, first, and only subsequently by adding

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Pesce et al. Herit Sci (2021) 9:72 Page 2 of 18

just enough water to bring the mixture to a workable a short paragraph in the book ‘Practical Building Con-
mortar [4, 5]. servation: Mortars Renders and Plaster’ published by
The increasing interest in hot-mixing within the con- English Heritage [9], and a recent book written by Nigel
servation industry is demonstrated by the growing num- Copsey [4]. Even less is available within the scientific lit-
ber of events such as conferences, workshops, training erature: Margalha et al. [10] asserted that the hot-mixing
courses and public demonstrations organised over the method has positive effects on flexural and compres-
past years on this topic (e.g. events organised by the sive strength, cracking susceptibility and capillary water
Building Limes Forum and by the Scottish Lime Centre absorption of mortars. The results of an investigation of
in the UK), that have attracted hundreds of attendees and historic hydraulic mortars prepared by hot-mixing led
much attention from specialists. Furthermore, several by Moropoulou et al. [11] allowed the authors to state
contractors currently offer the use of hot-mixed mortars that this production technology (and the raw materials
in conservation and restoration projects. Within the con- used) imparted high strength to the mortars. In a study
servation industry, hot-mixed mortars find application in by Valek et al. [12], the authors compared properties of
brickwork, rubble masonry, wall cores, and bridge con- hot-mixed mortars with those of mortars prepared with
struction, as well as in finishes such as hot limewashes lime putty and commercial dry hydrate and found that
and sheltercoats [1, 4]. hardened properties of the mortars were comparable
Hot-mixed mortars carry high historic relevance. across the production methods, whereas the hot mix had
According to the work of Schmidt [6], who analysed the higher porosity and higher capillary absorption capacity
database of over 3500 historic mortar samples of the than the ‘cold-mixed’ mortars. However, none of these
Scottish Lime Centre Trust, hot-mixed mortars com- studies has been able to unravel the relationship between
prised over 80% of all mortar samples dating from before the changes induced in the lime by different slaking pro-
the 17th century, more than 60% of samples dating from cesses and the improved characteristics of the mortars,
the 17th to the 19th century. Even in the early 20th cen- a fundamental step in understanding the mechanisms
tury, when the use of lime mortars started to phase out underlying this technology.
in favour of Portland cement mortars, hot-mixed mortars An important aspect that deserve attention for
were far more common than putty-based mortars. Fur- advancing our understanding of the properties of hot-
thermore, more and more peer-reviewed papers focused mixed mortars, is the role that steam plays in hot-mixed
on the analysis of historic mortars suggest the use of this technology, as highlighted in a recent publication by
technology in the past centuries, such as in the case of Copsey [4]. Considering the descriptions available in
the 16th century mortars used in the Amaiur Castel the literature [4] and the practical experiences of some
(Navarre, Spain) [7] and medieval wall painting plasters of the authors, it has been inferred that in the “hot-
in Denmark [8]. mixed” system the slaking process of lime (CaO) is
The advocates of hot-mixed mortars suggest that these likely to take place through two steps: in the first, the
mixes outperform the mortars made with lime putty in water adsorbed on the surface of the sand grains in con-
terms of workability, durability and costs (i.e. are cheaper tact with CaO reacts with the CaO initiating the slak-
to produce). Further claims suggest that hot-mixing ing. Because of the heat produced during this reaction,
improves the bond between lime and aggregate; that the the water adsorbed on the surface of the surrounding
development of steam may create an altered pore struc- sand grains is subsequently converted to steam that dif-
ture that facilitates the carbonation reaction and enhance fuses through the pores in between the sand grains and
the durability of the mortars; that aggregates of a wider promotes the slaking of further unreacted CaO (step 2).
range of dimensions are efficiently held in suspension (i.e. If this is the case, the effects of steam slaking on port-
reduced gravity segregation), easing the application of the landite crystals is an essential aspect of hot-mixed mor-
fresh mix [1, 4]. However, none of these claims has been tars that has never been investigated in detail. Studies
scientifically proved yet, since all these benefits are exclu- that partly investigate this effect have been carried out
sively evaluated on an empirical basis and interpreted by in other research areas such as in the desulphuriza-
unproved technical explanation. tion process of industrial emissions. In such context,
A possible reason for the uncertainty surrounding this vapour hydration of CaO is a process commonly used
technology is the very little technical literature available to produce high-performance ­CO2 sorbents [13, 14].
on it. This includes the Technical Paper 28 published by The vapour hydration reaction mechanism was firstly
Historic Environment Scotland [5], a book chapter writ- investigated in 1964 by Ramachandran [15] and later
ten by Alan Foster in the book: ‘Building Limes in Con- confirmed by Beruto et al. [6], who suggested that a
servation’ [2], a journal article published by the same different path is followed when CaO is slaked by liquid
author in the Journal of Architectural Conservation [1], water then when slaked by steam. In the former case, a
Pesce et al. Herit Sci (2021) 9:72 Page 3 of 18

liquid-state homogeneous dissolution/re-precipitation Materials and methods

process occurs, whereas in the latter case a solid-state Raw materials
topotactic reaction takes place. As a result, Ca(OH)2 The quicklime used in all experiments was Calbux Fine
formed by steam slaking is made up of a fine, poorly 6 (0–6 mm high reactivity quicklime) from Tarmac Bux-
crystalline phase which can rapidly react with ­ C O2 ton Lime and Cement. The aggregate used in mortars
[13, 14]. Our recent preliminary work [17] shows that was a silica sharp sand as defined by the producer (Chas
portlandite formed by CaO vapour hydration exhibits Long & Son Aggregates, Richmond, UK), granulometry
different mineralogical features from portlandite pre- 0–4 mm. The raw materials were characterised in terms
cipitated by CaO in solution. of density and grain size distribution. The skeletal den-
This study aims at investigating the characteristics sity was measured with a Micromeritics AccuPyc II 1340
and properties of lime when subject to slaking under helium pycnometer; the grain size distribution was meas-
conditions similar to those in the hot-mixing tech- ured by dry sieving according to the standard BS ISO
nology—under a heap of moist sand, in a receptacle 11277:2020 [18]. The results are shown in Table 1 and
very rich in steam—by recreating such conditions in Fig. 1.
a simplified system under controlled temperature and
humidity. This is achieved by: (i) slaking Ca-rich quick- Lime slaking
lime in different conditions (steam and water at vari- To investigate the effect of steam-slaking and water slak-
ous temperatures) and analysing the mineralogy and ing at different temperature on the microstructural and
microstructure of the obtained slaked limes, and (ii) mineralogical characteristics of lime, 3 different batches
testing some of the properties of mortars prepared of slaked lime were produced by slaking the same quick-
with the lime produced. It is worth noting that mixing lime in different conditions (Table 2). Lime ‘A’ was pro-
steam-slaked lime with sand does not necessarily pro- duced at room temperature as a ‘control’ slaking process
duce a mortar with the same properties as a hot-mixed and, therefore, to be used as a reference for evaluating
mortar, nor this study was aimed at producing a hot- any differences observed in the other batches of lime as
mixed mortar. However, it is important to stress that, a result of slaking at higher temperature. For producing
although this research focuses on the characteristics of lime ‘A’, the quicklime was mixed with de-carbonated de-
steam-slaked lime rather than of the hot-mix mortars, ionised (DI) water in 1:3 CaO:H2O mass ratio, as indi-
its results can be used to broaden our knowledge of the cated by other authors for the preparation of lime putty
hot-mixed mortars. In fact, the outcome of this inves- [19–23]. The water was poured all at once onto the quick-
tigation provides insights on what is regarded by prac- lime in a metal bucket and, immediately after the initial
titioners and most literature as an essential factor in vigorous bubbling, hand-mixed for at least 10 min. When
determining the advantageous properties of hot-mixed the temperature reached again the environmental condi-
lime mortars: the presence of vapour as one of the main tions, samples of the obtained putty were collected and
phases of the slaking process. Since hot-mixed mortars dried in a desiccator for at least 24 h for characterisation.
are increasingly used in conservation works, where they The remaining content was stored in excess of DI water,
seem to outperform putty-based mortars and a like-for- inside airtight containers until mortar production.
like approach is often sought, it is vital to gain scientific Lime ‘B’ was produced to investigate the effect of the
knowledge on this technology. water temperature on the characteristics of lime. For

Table 1 Grain size distribution and density of the raw materials

CaO Sand
Sieve Retained mass Cumulative retained Skeletal Sieve Retained mass Cumulative retained Skeletal
aperture size proportion % mass proportion % density (g/ aperture size proportion % mass proportion % density (g/
(μm) cm3) (μm) cm3)

63 1.76 1.76 2.88 63 2.96 2.96 2.70

106 3.26 5.02 106 0.29 3.25
212 2.04 7.06 212 11.36 14.61
250 3.38 10.45 250 13.39 28.00
500 88.93 99.38 500 19.37 47.37
1000 22.73 70.10
2000 25.56 95.66
Pesce et al. Herit Sci (2021) 9:72 Page 4 of 18

Fig. 1 Cumulative grain size distribution chart of the raw materials

Table 2 Slaking conditions and mortar preparation Lime ‘C’ was produced to investigate the effect of steam
Sample Lime slaking Mortar preparation
slaking on the characteristics of lime. For producing lime
name ‘C’, the quicklime was crushed and sieved to obtain par-
Slaking T slaking Lime form Binder:aggregate w/b
conditions water (v:v) ratio ticles with ø < 500 µm. The quicklime was then placed in
(°C) (w/w) an oven together with open beakers filled with de-car-
bonated water at 90 °C, so that steam was produced but
A Water 20 Putty 1:3 –
B Water 75 Putty 1:3 –
water did not reach boiling point and so the spilling of
C Steam – Dry hydrate 1:3 0.6
liquid water into the CaO tray was prevented. The quick-
lime was left to slake in the oven for 8 h. Figure 2 shows
the experimental setup and the visible volumetric expan-
sion of the lime that occurred as a result of slaking. At the
producing lime ‘B’, the quicklime and de-carbonated end of the test, samples of lime were collected and dried
DI water were separately heated in an oven until they in a desiccator for at least 24 h prior to characterisation.
reached 75 °C. Subsequently, the quicklime and the The remaining lime was sealed inside airtight containers
water were mixed in a mass ratio 1:3 CaO:H2O, in a until mortar production.
similar way to the lime ‘A’.

Fig. 2 Set up of the steam-slaking experiment. a Quicklime particles before the slaking. b Lime particles at the end of the slaking process
Pesce et al. Herit Sci (2021) 9:72 Page 5 of 18

Mortar preparation and curing conditions mortars (flexural and compression tests) were measured
The slaked limes obtained as described in Sect. “Lime to investigate the effect of the slaking process on their
slaking” were used to produce mortars as described in characteristics.
Table 2. Each batch of lime was mixed with silica sand
using a binder-to-aggregate (b:a) ratio of 1:3 v/v. All Scanning electron microscopy
mortar mixtures were mechanically combined with a The microstructural characteristics of the quicklime,
laboratory mixing equipment (a planetary mixer similar slaked lime and mortar samples were investigated using a
to the mixer specified in EN 196-1 [24] for 15 min. In Tescan Mira 3 SEM in high-vacuum mode and gun volt-
the case of water-slaked limes (A and B), the lime putty age of 10 kV. Quicklime samples were fixed on a metal
was mixed with sand without adding further water. In stub with carbon tape and sputtered with a 5 nm thick
the case of steam-slaked lime, which was in the form layer of platinum to make the analysed surface conduc-
of a powder, firstly the hydrated lime was combined tive. The samples of slaked lime were dried in a vacuum
with sand in the mixer, and subsequently DI water was oven for 6 h and then fixed on a metal stub with carbon
added gradually to the mix until reaching a w/b ratio of tape and platinum coated. For the mortar samples, a
0.6 w/w to obtain a workable consistency. freshly cut sub-sample was removed from the core of 3
The moulding of the mortars was carried out manu- cylinders of each age (described in Sect. “Mortar prepa-
ally by compacting the mortar using a metal rod. The ration and curing conditions”). The fragments were then
samples were cast in two layers, tamping firmly the mounted on a metal stub with carbon tape and platinum
mortar surface in a uniform manner with ~ 25 strokes coated. Since sample preparation took place at low RH
each layer. Two different types of mould were used for (~ 30%), it is possible to assume that during this time, no
testing: significant carbonation occurred.

1. Plastic cylinders of 30 mm diameter × 50 mm height X‑Ray diffraction

for microstructural and mineralogical characterisa- The mineralogical characteristics of the quicklime,
tion and phenolphthalein test. Twenty-four samples slaked lime and mortar samples were investigated using a
were produced for each batch of lime in order to Rigaku SmartLab X-ray diffractometer (Cu-Kα radiation,
obtain 3 replicas at each pre-set age of: 15, 16, 17, 20, parallel beam geometry, 2 − θ range 10–90°, step 0.05°,
21, 28, 35, 42 days of curing. The time points were scan speed 1.5°/min, 40 kV, 50 mA). Phase identification,
selected in order to allow the samples to be safely quantitative phase analysis and crystallite size evalua-
demoulded, and to closely monitor the evolution tion were carried out using the Rigaku SmartLab Studio
of the samples at early ages (within one week from II software. The crystallite size was calculated using the
demoulding) and at mid-term on a weekly frequency, Hall’s method implemented in the same software [25].
in addition to the standard curing times usually Prior to XRD analysis, quicklime and slaked lime sam-
selected in studies of hydraulic binders. ples were ground with an agate pestle and mortar, sieved
2. Prismatic specimens of 40 × 40 × 160 mm for flex- to < 63 µm, and mixed with 10% w/w zincite used as
ural and compression tests. All specimens were cured internal standard for quantification of possible amor-
inside the mould for 14 days in laboratory conditions phous phases.
(~ 20 °C, 50% relative humidity [RH]) after which For each pre-set mortar age, one of the 3 cylindrical
they were demoulded. Four replicas were produced samples was chisel-cut to obtain a central 2 cm thick slice,
per batch of lime and testing was carried out after which was then crushed using a hammer until particle
28 days of curing. size was < 5 mm. From the crushed material, a sub-sam-
ple was selected using the coning and quartering method.
The sample obtained was then finely crushed with an
agate pestle and mortar to a < 106 µm granulometry.
Characterisation methods
The microstructural and mineralogical characteristics of Phenolphthalein test
the quicklime and slaked limes were investigated using To provide visual evidence of the carbonation front, the
scanning electron microscopy (SEM) and X-ray diffrac- phenolphthalein test was carried out on all the cylindri-
tion (XRD) analyses. Chemical, microstructural and min- cal samples at each age, according to the British Standard
eralogical characteristics of mortars were investigated BS EN 14630 [26]. The phenolphthalein was sprayed onto
using phenolphthalein, SEM and XRD. the surface of two longitudinal halves of the cylinders,
Fresh-state properties (water retention and obtained by splitting them with a chisel. The stained sur-
water demand) and hardened-state properties of faces were photographed immediately after spraying.
Pesce et al. Herit Sci (2021) 9:72 Page 6 of 18

Water retention with water-slaked lime (batch A and B), mixtures were
The water retention of fresh mortars was investigated produced without adding any water, whereas to evalu-
using the method detailed in the British Standard BS ate the consistency of the mortar produced with steam
EN 459-2:2010 [27], previously used by other research- slaked lime (type C), various amounts of water were
ers [28], and the testing equipment provided by Novanna added until the mortar samples achieved a similar
Measurement Instrument (product code 1.0246). In these spread to those containing lime putty. This also allowed
tests, freshly-mixed mortars with known water fraction evaluating water quota to add to the mixtures produced
are put in contact with a filter plate, simulating the action using steam-slaked lime in order to reach an appropri-
of an absorptive substrate. To calculate the water reten- ate workability as required for water retention test. To
tion of the fresh mortars, 3 samples of each batch of lime obtain a statistically significant value of the spread in
were tested in order to acquire statistically meaningful mortars produced with lime putties, 3 tests were car-
data. ried out for each mix.
According to BS EN 459-2:2010, the water fraction
(W1) of the mortars is calculated as in Eq. (1) where m21
is the total mass of water in fresh mortar (g) and m22 is Mechanical tests
the mass of dry mortar (g). Hardened-state properties of the same mortars pre-
m21 pared for the water demand test (previously described in
W1 = . (1) Sect. “Water demand”) were measured after 28 days of
m21 + m22
curing. Flexural and compression tests were carried out
The water content of the tested samples of mortar (W2) using an INSTRON 3382 Floor Model Universal Testing
was defined as in Eq. (2): System with loading cell of 100 kN capability, and load
accuracy of 0.5% of the indicated load, as described in the
W2 = m23 × W1 , (2) British Standard BS EN 196-1:2016 [24].
where m23 is the mass of the tested sample of mortar (g). Flexural tests were carried out on the prismatic sam-
The mass of water absorbed by the filter plate (W3) was ples described in Sect. “Characterisation methods”.
defined as in Eq. (3): Table 3 reports the geometrical characteristics of the
samples tested. Flexural strength was evaluated using the
W3 = m20 − m17 , (3) three-point loading method. Load rate was 0.2 mm/min,
and the distance between the two supports was 100 mm.
where m20 is the mass of the soaked filter plate (g), and
Flexural strength (Rf, in megapascals) was calculated
m17 is the mass of the dry filter plate (g). The relative loss
according to Eq. (6) where Ff is the load applied to the
of water from the mortar (W4) was defined as in Eq. (4).
middle of the prismatic sample at fracture in newtons; b
W3 is the width of the tests sample in millimetres; h is the
W4 = × 100. (4) thickness of the tested sample, in millimetres; l is the dis-
W2
tance between the supports, in millimetres.
The water retention capacity (WR) of a freshly-mixed
mortar was calculated as a percentage according to
Eq. (5). Table 3 Width (b), thickness (h) and cross-sectional area of the
prismatic samples tested for flexural strength at 28 days
WR = 100 − W4 . (5)
Mortar sample b (mm) h (mm) Area ­(mm2)

Lime type A-1 39.62 39.81 1577.27

Water demand Lime type A-2 39.08 38.25 1494.81
The water demand of fresh mortars was evaluated Lime type A-3 39.25 38.2 1499.35
through the consistency of the mix, measured by flow Lime type A-4 39.24 39.4 1546.06
table test as in BS EN 459-2:2010 [27] and BS EN Lime type B-1 38.35 39.19 1502.94
12350-5:2019 [29]. This apparatus determines the con- Lime type B-2 39.19 39.44 1545.65
sistency of the fresh mortars by measuring their spread Lime type B-3 38.42 39.47 1516.44
on a horizontal flat plate which is subjected to jolting. Lime type B-4 38.44 39.24 1508.39
Results are reported as the average obtained by meas- Lime type C-1 39.11 38.84 1519.03
uring the minimum and maximum dimension of the Lime type C-2 37.46 37.01 1386.40
mortar spread and are reported to the nearest 10 mm. Lime type C-3 39.46 39.37 1553.54
To evaluate the consistency of the mortar produced Lime type C-4 39.42 39.02 1538.17
Pesce et al. Herit Sci (2021) 9:72 Page 7 of 18

1.5 × Ff × l hexagonal {00.1} faces, with habits varying from platelets,

Rf = 2
. (6) short prism and rod-like. Such crystals are embedded in a
b×h
matrix of smaller (10–100 nm) crystals showing a granular
Compressive test was carried out on the broken halves of habit with less regular crystal facets. Pores have diameters
the prismatic samples used in the flexural test. Compres- of various sizes ranging from few nm to 0.5 µm.
sive strength was evaluated using the same load rate of The microstructure of the putty slaked with water at
0.2 mm/min and calculated using Eq. (7) where Rc is the 75 °C (batch B) (Fig. 3c) has pores of various size and shape
compressive strength, in megapascals; Fc is the maximum (ranging from few nm to 0.5 nm, similar to the control
load at fracture, in newtons; b is the width of the tests sam- putty). Portlandite crystals in batch B have less regular fac-
ple in millimetres; h is the thickness of the test sample in ets than those observed in the control putty. Few µm-sized
millimetres. crystals can be observed, while most crystals are nm-sized
and of irregular shape.
Fc
Rc = . (7) The microstructure of the steam-slaked lime (batch C)
b×h (Fig. 3d) shows interconnected particles similar to the
Compressive and flexural strength values reported in quicklime and with a similar heterogeneous pore network
paragraph Sect. “Flexural and compressive tests” are the (pore diameter 0.1–0.5 µm). Although the crystal facets
mean values of the measurements on the four replicas of appear mostly irregular, hexagonal thin platelets can be
each lime mortar sample. Error bars represent confidence recognised in some of these nm-sized particles. The surface
intervals at 90% and were calculated with the following for- of several particles is characterised by nm-sized cracks.
mula [30]: The diffractograms of the CaO and hydrated lime A, B
and C are shown in Fig. 4. The results of phase identifica-
s
±tn−1 √ , (8) tion and quantification performed by XRD-Rietveld anal-
n ysis are reported in Table 4. In the quicklime, CaO is the
where tn−1 is the Student’s t-score reflecting a confidence dominant phase, but minor quantities of portlandite are
level of 90% (= 1.96) at n−1 (= 3) degrees of freedom, s identified as well. Traces of calcite were found in all lime
is the sample standard deviation, and n is the sample size samples, likely due to reaction with moisture and atmos-
(= 4). pheric ­CO2 during sample preparation. In all slaked limes,
portlandite is the dominant phase but some differences can
Results and discussion be observed across the three batches of lime.
Microstructural and mineralogical characteristics of limes In the Batch A (lime slaked in water at 20 °C) no trace
Figure 3 shows SEM images of the quicklime and the three of original quicklime was found, suggesting that the CaO
batches of lime analysed. The quicklime (Fig. 3a) is char- has fully reacted with water. Conversely, in Batch B (the
acterised by a regular microstructure of interconnected putty slaked at 75 °C) a small trace (3%) of CaO was iden-
particles with heterogeneous sub-rounded pores of about tified. This could be due to various reasons: the slaking in
0.1 µm in diameter. The observed morphology is typical hot water results in a more violent reaction than with water
of calcined carbonate minerals [31, 32]. The pore diam- at room temperature [36], and the subsequent rapid evapo-
eter observed by SEM is included in the range of values ration of water may have had an effect on some hot spots
measured in literature for other calcined limestones [33], in the core of quicklime particles that remain unreacted.
although it should be noted that there are several factors Another possible explanation is that the rapid evapora-
that can contribute to the microstructure of the calcined tion of water increased the actual CaO:H2O ratio, resulting
material, including the morphology of the parent material in the development of hot-spots with high temperatures
and the calcination conditions [31, 33–35]. (e.g. > 200 °C) that may have dehydrated some of the lime
The microstructure of the control putty (batch A) slaked that had initially hydrated [36]. In Batch C (lime slaked with
at 20 °C (Fig. 3b) displays partially agglomerated crys- steam) most of the quicklime has been hydrated (80% port-
tals of a wide variety of habits and size. Most portlandite landite), but the remaining 20% was unreacted CaO. This
crystals have size up to 1.5 µm and display well-developed was probably due to the limited diffusion of steam within
the pores of the pulverised quicklime.

(See figure on next page.)

Fig. 3 SEM images of parent quicklime and of portlandite crystals in limes slaked with the different methods. a CaO crystals in quicklime. b Lime
slaked in 1:3 lime:water ratio at 20 °C. c Lime slaked in 1:3 lime:water ratio at 75 °C. d Steam-slaked lime. The left and right columns show a low and
high magnification, respectively. Insets in b and d show details of individual crystals
Pesce et al. Herit Sci (2021) 9:72 Page 8 of 18
Pesce et al. Herit Sci (2021) 9:72 Page 9 of 18

Fig. 4 Diffractograms of the quicklime (yellow plot), of lime A (green plot), lime B (blue plot) and lime C (orange plot). The phases are shown with
the following keys: P = portlandite; C = calcite; Z = zincite; Q = calcium oxide

Table 4 Quantitative phase analysis of the lime samples

Sample CaO (%) Portlandite (%) Calcite (%)

Quicklime 94.3 3.4 2.3

Water 20 °C 0 94.5 5.5
Water 75 °C 3.3 95.2 1.5
Steam slaked 19.2 79.1 1.8

Results of the crystallite size analysis for the various

types of lime, calculated from the XRD data are shown
in Fig. 5. The graph shows that the steam-slaked lime
has significantly smaller crystallites (180 Å) than the
water-slaked limes (~ 400–900 Å). The putty slaked in
liquid water at room temperature shows crystallite size
Fig. 5 Portlandite crystallite size calculated from XRD data in the
of 394 Å, whereas the putty slaked at 75 °C shows a big- control lime (a), in the water-slaked lime at 75 °C (b), and in the
ger crystallite size (900 Å) but also a remarkably higher steam-slaked lime (c)
standard deviation, suggesting that either the crystallites
have a wide size distribution or have a high aspect ratio
(e.g. plates or needles). Although the SEM micrographs
formed in the latter samples display a morphology that
cannot be used as a direct comparison for the crystallite
is commonly encountered in freshly-slaked lime putties
size calculated with XRD (as the lime particles observed
[23], whereas the steam-slaked lime reveals a distinct
by SEM can be aggregates of several crystallites), they
microstructure that resembles that of the CaO. Such
can be used for drawing some considerations. In the
remarkable difference can be ascribed to the different
putty slaked at 75 °C (Fig. 3c) the particles are rather
conditions in which portlandite crystals are formed
granular and do not show a remarkable high aspect
upon reaction with water.
ratio with respect to control lime, which instead display
Previous studies have shown that well-crystallised
crystals with elongated and plate-like shapes (Fig. 3b).
Ca(OH)2 forms upon reaction between CaO and liq-
Arguably, it is possible to discard the high aspect ratio
uid water due to the portlandite crystallisation path,
hypothesis in favour of the wide crystallite distribution
via precipitation from a supersaturated solution, and to
hypothesis, which however should be further verified and
the subsequent growth enhanced by the rapid diffusion
investigated.
of ionic species in a liquid medium [15, 16]. However,
Overall, the SEM images suggest that the microstruc-
the different microstructure of the steam-slaked lime
ture of the steam-slaked lime is significantly different
suggests that hydration took place following a different
from that of water-slaked lime. Portlandite crystals
Pesce et al. Herit Sci (2021) 9:72 Page 10 of 18

reaction path at a gas–solid interface. Without the where r is the pore radius (m), γ is the surface tension of
presence of a liquid phase, diffusion of ionic species— water (0.0608 J/m2 at 90 °C), Vm is the molar volume of
which allows CaO and ­H2O to react—is very slow and water (1.8·10−5 mol/m3), R is the gas constant 8.134 J/
does not account for the extensive portlandite forma- (mol K), T is the temperature (363°K), and P/P0 is the
tion measured by XRD. The reaction path proposed by relative vapor pressure of water. Since during the steam-
Beruto et al. [16] involves the diffusion of gaseous H ­ 2O slaking experiment, the reservoir of water had to be peri-
molecules into the CaO phase through the {111} planes odically refilled, we can assume that inside the slaking
of CaO made of O− 2 , which convert upon adsorption chamber, water vapour never reached equilibrium with
of water into {001} planes of Ca(OH)2. However, the its liquid phase and hence the humidity was far from
distance between {111} planes of CaO is only 2.780 Å saturation. Even assuming a high RH%, e.g. 90%, it is
whereas the distance between {001} planes of Ca(OH)2 possible to calculate that capillary condensation in such
is 4.910 Å and this results in a high anisotropic expan- conditions occurs in pores with diameter < 15 nm, which
sion in the direction normal to the {001} planes. Such is almost 2 orders of magnitude lower than the pores
mechanism is supported by our SEM images, which observed in the SEM images. Thus, the hypothesis that
show extensive cracks formation (width in the mag- the majority of CaO during steam-slaking was slaked in
nitude order of 10 nm) on the surface of the newly liquid water by capillary condensation can only apply to
formed portlandite (Fig. 3d, right column) likely gener- a limited pore volume and, consequently, it is possible
ated by the stress caused by the volumetric expansion to assume that most of the hydration during our steam-
during the conversion from CaO to Ca(OH)2. slaking experiments occurred in the absence of a liquid
Furthermore, the XRD analysis showed that the steam- phase.
slaked lime has crystallites of remarkably smaller size than
those formed upon water-slaking. This can be explained Water retention
by considering the mechanism underlying the hydration Results of the water retention (WR) tests are reported
of CaO by water in vapour phase proposed by Molinder in Table 5. The results obtained for the water retention
et al. [37]. According to this study, during early hydra- of mortar based on lime A (water-slaked at 20 °C) are
tion Ca(OH)2 nucleates on the {111} planes of CaO, with in good agreement with WR values reported by other
Ca(OH)2 {001} planes parallel to the CaO {111} planes. authors for lime mortars [39, 40] and references therein.
However, the Ca-Ca bond length in the CaO {111} plane Water retention of the mortar based on lime ‘B’ (water-
(3.401 Å) is different from the one in the Ca(OH)2 {001} slaked at 75 °C) is closer to the WR of the mortar based
plane (3.589 Å) and such lattice mismatch induces a sig- on the steam-slaked lime (type ‘C’) suggesting a possible
nificant internal stress in the Ca(OH)2 lattice, which results influence of the slaking temperature on the capability of
in failure of the crystal structure and eventually in a small the mortars to retain water during mixing. The results
crystallite size. also show that the mortar containing steam-slaked lime
During vapour hydration, the growth of Ca(OH)2 prefer- is capable to retain more water than mortars produced
entially occurs in the direction parallel to the {001} planes, using water-slaked lime.
as a result of (i) easier diffusion of Ca and O ions from the WR values of mortars based on lime ‘B’ and ‘C’ are
CaO-core to the Ca(OH)2 surface layer and (ii) easier con- remarkably high and this is likely related to the micro-
tact with ­H2O molecules [14, 37]. The preferential growth structural characteristics of these types of lime, that
of portlandite along the {001} planes results in crystals
with a high aspect ratio (thin platelet shape), as supported
by our SEM observations (Fig. 3), which show that in our Table 5 Results of water retention tests
steam-slaked lime, portlandite mainly exhibits a thin plate-
Lime Type Replica n Water fraction WR %
let habit, whereas in the other limes (A and B), crystals W2 (g)
have thicker, well-developed platelets, short prism, rod-like
or granular habits. A (20 °C) 1 55.7 87.5 ± 1.2
It may be argued that during steam slaking, hydration 2 55.9
occurs through contact of CaO with liquid water formed by 3 54.1
capillary condensation. The minimum radius of the pores B (75 °C) 1 51.3 92.6 ± 1.4
in which water can condense can be calculated using the 2 55.8
Kelvin equation [38]: 3 54.9
C (steam-slaked) 1 41.3 96.2 ± 0.8
2γ Vm 2 52.3
r= ,
RT ln(P0 /P) 3 55.4
Pesce et al. Herit Sci (2021) 9:72 Page 11 of 18

are, in turn, consequence of the slaking conditions.

The SEM analyses (Fig. 3), in fact, show that lime A is
constituted by µm-sized, well-crystallised portland-
ite, whereas in lime B and C portlandite crystals seem
of sub-micrometer granular shape and nm-sized thin
platelets, respectively. These morphologies are likely
to produce a higher specific surface area than the big-
ger crystals in lime A. The specific surface area of the
binder is known to be positively correlated with the
water retention of a mortar [28, 41]. Moreover, the
morphologies of limes B and C (particularly the latter),
are also likely to be related to a higher colloidal stabil-
ity [42] and in these systems water is more homogene-
ously distributed, allowing a higher water retention. In
particular, small and plate-like Ca(OH)2 particles (like
the ones found in our steam-slaked lime samples) are
Fig. 6 Plot of flowability vs w/l ratio of mortars based on
reported to have higher capacity of absorbing water steam-slaked lime (blue plots and trend line) and on putties
than bigger, prism-shaped crystals and are thus able to water-slaked at 20 °C (green plot) and 75 °C (orange plot)
increase the overall water retention of a mortar [42].

Water demand
The water demand of the mortars was assessed by
measuring their flowability and putting it in relation
with the water/lime ratio (w/l). The w/l of putties A
and B was determined gravimetrically by oven-drying
(Table 6). Note that during mortar preparation no extra
water was added to the mixture other than that already
contained in the lime putties. Differently from the mor-
tars produced using putties, a water quota was added
to the mortar made of steam-slaked lime (i.e. a powder)
and sand in order to obtain an appropriate workability.
Figure 6 shows the flowability vs w/l plot of mortars Fig. 7 Bending stress at maximum load at 28 days for the mortars
based on lime putty (types A and B) and of steam- produced with water-slaked lime at 20 °C (A) and 75 °C (B) and with
slaked lime (type C) mortar, prepared by adding vari- steam-slaked lime (C)
ous quotes of water. The figure shows that the mortar
made with steam-slaked lime needs a w/l = 0.75–0.77
to obtain a spread similar to the mortar produced with
Flexural and compressive tests
lime slaked at 20 °C of w/l = 1.4; and a w/l = 0.56–0.63
Figures 7 and 8 report the results of the flexural and com-
to reach a spread similar to the mortar produced with
pressive test at maximum load after 28 days of curing, for
lime slaked at 75 °C (w/l = 1.3). Hence, these results
the mortars produced with lime type ’A’, ‘B’ and ‘C’.
suggest that to produce mortars based on steam-slaked
Results show that mortars produced with steam-slaked
lime that have a spread similar to a “traditional” putty-
lime (‘C’) have a significantly higher flexural strength
based mortar, only about half the amount of water is
than mortars produced with water-slaked lime at 75˚C in
required.
flexure. Mortar C shows also a higher mean value in flex-
ural strength with respect to mortar A (made with lime
slaked in water at 20 °C) however, the large error bar for
Table 6 Calculated w/l values in putty-based mortars, obtained mortar C that partially overlaps that of mortar A reduces
by oven-drying
the significance of these results (Fig. 7). In compression,
Lime used Before drying (g) After drying (g) w/l instead, steam-slaked lime mortars have a strength very
similar to the mortars produced with the other types of
Type A 36.2 15 1.4
lime (Fig. 8).
Type B 52.5 22.9 1.3
Pesce et al. Herit Sci (2021) 9:72 Page 12 of 18

originated during mixing of the mortar. It is possible that

the use of a putty (hydrated lime particles already dis-
persed in water) allows for a more homogeneous combi-
nation with sand during mortar mixing, unlike the use of
the steam-slaked lime powder.

Microstructural evolution and carbonation study

during mortar hardening
Figures 9, 10 and 11 show the microstructural evolu-
tion at 21, 28 and 42 days of mortars produced with lime
slaked at 20 °C and 75 °C and steam-slaked, respectively.
The images show that, after 21 days of curing, the mor-
Fig. 8 Compression stress at maximum load at 28 days for the tar produced with lime A (at 20 °C) is characterised by
mortars produced with water-slaked lime at 20 °C (A) and 75 °C (B) a large number of hexagonal portlandite crystals. At
and with steam-slaked lime (C) 28 days, the number of visible portlandite crystals starts
to reduce and some calcite crystals started to appear in
the same mortar. At 42 days, portlandite crystals are no
Remarkably, the confidence intervals for the measure- longer visible and the microstructure appears more com-
ments of the steam-slaked lime mortars are much larger pact. Conversely, in the mortars made with lime B (slaked
than the other two tested mortars, both in flexure and in at 75 °C) and with steam-slaked lime, portlandite crystals
compression. A possible explanation that accounts for are visible throughout the whole curing period, and no
the higher confidence interval of the steam-slaked lime significant reduction in porosity can be observed.
mortar measurements is a higher heterogeneity of these Figure 12 shows the results of the phenolphthalein tests
mortars, as it has been observed for uniaxial compres- for the three types of mortar tested, at 15, 20, 28 and
sion tests performed on natural rocks, where a higher 35 days of curing. The pink colour suggests a pH > 8–9
level of heterogeneity was related to a higher coefficient and, therefore, the presence of portlandite, whereas the
of variation [43]. Such a heterogeneity could have been

Fig. 9 Microstructural evolution of mortar produced with lime A (slaked 20 °C) at 21, 28 and 42 days of curing

Fig. 10 Microstructural evolution of mortar produced with lime B (slaked 75 °C) at 21, 28 and 42 days of curing
Pesce et al. Herit Sci (2021) 9:72 Page 13 of 18

Fig. 11 Microstructural evolution of mortar produced with lime C (steam slaked) at 21, 28 and 42 days curing

Fig. 12 Comparison between mortars prepared with different types of lime: carbonation front as shown by phenolphthalein sprayed on broken
surfaces of carbonated mortar samples

absence of significant pink staining suggests a limited lime mortar, with the only difference that at 28 days
presence of portlandite, which is assumed to be corre- the stained area is slightly thicker. The steam-slaked
lated to the conversion of portlandite to calcite through lime mortar shows different results instead. At 28 days,
the carbonation reaction. The results show that in the significant staining is still observed in the core of the
20 °C water-slaked lime mortar cured for 20 days, the specimens, and only at 35 days the fracture shows no sig-
staining front is drastically reduced involving only a nificant staining.
few mm along the core of the cylinder; at 28 days, no It is worth noting that, as indicated in the BS EN
pink staining is observed on the fractured surface. A 14630:2006 [26], the colour change to pink in our samples
similar result is obtained with the 75 °C water-slaked was recorded within 30 s from spraying the surface. After
Pesce et al. Herit Sci (2021) 9:72 Page 14 of 18

that time, a diffused pink colouration slowly appeared on

the whole fractured surface, suggesting that in all mortar
samples after 35 days of curing only partial carbonation
occurred [26].
By comparing the phenolphthalein results with the
SEM observations, it can be observed that the analyses
are in good agreement in showing that steam-slaked
lime mortars are characterised by a slower carbonation
rate than 20 °C water-slaked lime mortars. On the other
hand, no clear distinction in carbonation rate could be
observed with SEM analysis between the 75 °C water-
slaked lime mortars and the steam-slaked lime mortars,
whereas the phenolphthalein tests clearly show that the Fig. 14 Calcite:portlandite ratio of different mortar samples at
steam-slaked lime mortars carbonate significantly slower various ages (up to 42 days), exposed to laboratory conditions (20 °C,
than the 75 °C water-slaked lime mortars. 40–50% RH)
Results of the XRD analysis used to investigate the car-
bonation in mortars are reported in Fig. 13, where dif-
fractograms of the mortar samples after 42 days of curing carbonation progress. The steam-slaked lime mortar
are shown, and in Fig. 14, where the calcite:portlandite is the least carbonated and shows the highest flexural
(C/P) ratios of the mortar samples are plotted against strength, although with high variation. However, the C/P
the curing time, from 21 to 42 days. The results are in ratio plot in Fig. 14 shows that at 28 days the carbonation
good agreement with the phenolphthalein tests and SEM progress is still at a very early stage, with a curve that is
observations and confirm that the mortar produced still steeply rising, and suggesting that most of the binder
with steam-slaked lime has the lowest carbonation rate. is still unconverted Ca(OH)2. This is likely the reason why
Calcite:portlandite ratios measured in the mortars made the results of the mechanical tests are close to each other
limes slaked at 20 and 75 °C show the highest values, across the tested mortars.
suggesting a high carbonation rate within these samples Since the carbonation reaction is a process that pro-
compared to the mortar made with steam-slaked lime. ceeds from the surface towards the core of the material,
By comparing the results of the carbonation tests a weak correlation between specific surface area and
at 28 days with the mechanical tests, it is possible to carbonation rate has been reported [44]. Hence, con-
observe to that the flexural strength seems to reflect the sidering the microstructural observations in the lime

Fig. 13 Diffractograms of mortar samples at 42 days of curing. Keys: P = portlandite; Qz = quartz; C = calcite; A = anorthite; D = dolomite
Pesce et al. Herit Sci (2021) 9:72 Page 15 of 18

samples tested in this research (see Sect. “Microstruc- than in the water-slaked lime (both at 20 and 75 °C). In
tural and mineralogical characteristics of limes”), it is a recent study of historic hot-mixed lime plasters [8], it
expected that the carbonation of the mortars tested in was found through SEM observations of thin sections
this research would follow this order (from the highest that in hot-mixed plasters the portlandite crystals are sig-
carbonation rate to the lowest): steam-slaked > water- nificantly smaller than those of putty-based plasters. This
slaked at 75 °C > water-slaked at 20 °C. Nevertheless, the supports the hypothesis that steam slaking plays a major
data collected suggest a different behaviour. To explain role in determining the characteristics of the binder in
such a behaviour, it is important to take into account the hot-mixed mortars.
limited RH during curing (see paragraph in Sect. “Mor- The smaller portlandite crystal size formed upon
tar preparation and curing conditions”) that promoted steam-slaking is also likely to be responsible for the
water evaporation, and the effect of the water content higher water retention and lower water demand meas-
of our mortars on the carbonation rate. It was assessed ured in our steam-slaked lime mortars with respect to
that water content was the highest in the mortars based putty-based lime mortars, as a consequence of a higher
on water-slaked lime and the lowest was in the steam- colloidal stability of the formers [42]. This finding can
slaked-lime mortar (see parameter ­W2 in Table 5). It has also be related to the superior quality of hot-mixed mor-
been extensively shown that carbonation can only take tars in terms of workability and water retention [4], likely
place within an optimal range of RH% included between imparted by the presence of smaller portlandite crystals
40 and 80 [45]. In such humidity conditions, a molecu- in the binder with respect to putty-based mortars, as a
lar-scale layer of water forms on the surface of lime par- consequence of the steam-slaking occurring during the
ticles, allowing for the dissolution of Ca(OH)2 and ­CO2 hot-mixing process.
and subsequent precipitation of ­CaCO3, but the mortar Furthermore, the same modified mineralogical char-
pores are not fully saturated with water and the diffusion acteristics of steam-slaked lime are also likely to allow to
of ­CO2 inside the pore network is guaranteed [45–49]. produce a mortar highly rich in binder, as in hot-mixed
Therefore, it is possible to suggest that in the water- mortars. The exceptionally high b/a ratio typical of hot-
slaked lime mortars, the higher water content facili- mixed mortars is regarded as beneficial in terms of both,
tated the formation of a water layer where dissolution of workability and ‘stickiness’ of the mix in its fresh state,
Ca(OH)2 and ­CO2 could occur, fostering in this manner and enhanced durability in its hardened state [3, 4, 8, 50].
the carbonation reaction. Carbonation was slowed down Our mechanical tests showed similar strength of the
in the steam-slaked mortar because of the lower water steam-slaked lime mortars and the water-slaked lime
content that limited the formation of the water molecular mortars, nonetheless the carbonation progress of the for-
layer on the surface of Ca(OH)2 necessary for the dissolu- mer was less advanced than the latters at time of testing.
tion of the involved species. This suggests that steam-slaked lime mortars potentially
Overall, this suggest that in the same environmental outperform water-slaked lime mortars. Long-term tests
conditions, the water content was the main driving force should be carried out to elucidate the strength develop-
in governing the carbonation reaction, rather than the ment of the mortars and whether steam-slaked lime mor-
microstructural characteristics of portlandite crystals. tar perform better than water-slaked lime mortars when
fully carbonated.
Implications for hot‑mixed mortars technology Remarkably, a systematic higher variability was
The reason why the performance of hot-mixed mortars is recorded in the steam-slaked mortar samples suggest-
superior to lime putty mortars is not yet well understood. ing a higher structural heterogeneity. It can be argued
It is also true that, as stressed by Henry [3] and Midt- that such heterogeneity is originated by the presence of
gaard et al. [8], hot-mixed mortars should not be con- lumps in the steam-slaked lime mortars. Indeed, lime
sidered as a panacea for any conservation work, instead lumps are frequently found in historic hot-mixed mor-
their use should be assessed according to the required tars as a consequence of late hydration and poor mixing
application and further studies are needed to make hot- of the binder with the aggregate [4, 8, 45, 51–53]. Never-
mixing a more established practice. theless, lime lumps, usually clearly visible either by naked
The results of our study allow to clarify some of the eye or with the aid of optical microscopy, could not be
characteristics that make hot-mixed mortars attractive observed in our steam-slaked lime mortars. This leads to
to practitioners and conservators, related to the slaking two considerations: (i) the procedure of the steam-slaked
conditions of lime and the role of steam in the hot-mix- lime mortar preparation seems to result in a poorer mix-
ing process. ing than putty mortars, such to lead to a structural het-
Both our SEM and XRD investigations on steam-slaked erogeneity but not enough to lead to the formation of
lime suggest the formation of smaller portlandite crystals visible pure lime lumps, as in hot-mixed mortars; (ii) the
Pesce et al. Herit Sci (2021) 9:72 Page 16 of 18

development of lime lumps in hot-mixed mortars is likely determining the carbonation rate over other fac-
a consequence of the reduced effects of the physical mix- tors, such as the portlandite crystals morphology.
ing action, rather than by a difference in the microstruc- The higher water content of the mortars made with
tural characteristics of the binder as a direct consequence water-slaked lime favours the carbonation whereas
of the steam-slaking process. the same process is hindered in the mortar made
with steam-slaked lime because of the lower water
Conclusions content.
In this study, the slaking conditions of lime found accord- • Overall, steam-slaked lime is characterised by
ing to the traditional technique of hot-mixing were re- microstructural properties that allow to produce
created in a simpler system, i.e. by steam-slaking lime mortars with higher water retention and that
in an oven at controlled temperature, in order to isolate require less water to reach an appropriate consist-
the effect of steam, regarded as a crucial factor in the ency than putty-based mortars. These are possibly
improved properties of hot-mixed mortars, and inves- among the reasons why craftsmen, both nowadays
tigate it as a single variable. The characteristics of lime and in the past, preferred hot-mixed mortars over
slaked in steam were compared with those of lime slaked putty-based mortars. Thus, during conservation
in water at two different temperatures (20 and 75 °C), works the production technology of lime mor-
and the properties of the related mortars were also inves- tars should thoroughly be taken into account and
tigated. Both limes and mortars were characterised at a should guide the decision-making process, espe-
microstructural level and their carbonation rates were cially where historic accounts and scientific evi-
assessed, in an attempt to provide new scientific knowl- dence suggest that hot-mixed mortars were origi-
edge on the properties of lime mortars made by the hot- nally employed.
mixing process, and to explain the reasons why these
mortars are regarded by many practitioners as superior Further research should investigate the effects of
compared to mortars made with putty. The following steam-slaking lime on the performance and carbona-
conclusions can be drawn from this study: tion rate of mortars over a long period of time, as well
as the porosity development in steam-slaked lime mor-
• Portlandite crystals formed by steam-slaking are dif- tars which is likely one of the major factors affecting
ferent from those formed by water-slaking. In par- carbonation rate.
ticular, the formers are characterised by a smaller
crystallite size, irregular shape and are grouped in Abbreviations
assemblies with a micromorphology that resem- γ: Surface tension; b: Width of mechanical tests sample; b:a: Binder to aggre-
gate ratio; C/P: Calcite:portlandite ratio; DI: Deionised; Fc: Maximum load;
bles that of the unslaked CaO. These differences are Ff: Load applied to the middle of the prismatic sample at fracture; h: Height
likely due to the different reaction path of the hydra- of mechanical tests sample; l: Distance between the flexural test apparatus
tion process when it occurs at a solid/gas interface supports; m17: Mass of the dry filter plate; m20: Mass of the soaked filter plate;
m21: Total mass of water in fresh mortar; m22: Mass of dry mortar; m23: Mass of
compared to solid/liquid interface. The differences mortar sample; P/P0: Relative vapour pressure; r: Pore radius; R: Gas constant;
between portlandite formed by slaking in room tem- Rc: Compressive strength; Rf: Flexural strength; RH: Relative humidity; SEM:
perature water and portlandite formed after slaking Scanning electron microscope/microscopy; T: Temperature; Vm: Molar volume;
w/l: Water:lime ratio; W1: Water fraction; W2: Water content of mortar; W3: Mass
in hot water are not as significant as those between of water absorbed by the filter plate; W4: Loss of water from the mortar; WR:
water- and steam-slaked lime. Water-slaked lime has Water retention capacity; X21: Water fraction in the putty; X22: Dry mortar frac-
mostly big, rod-like crystals while steam-slaked lime tion; XRD: X-ray diffraction.
has mostly smaller granular particles. Acknowledgements
• Water retention of mortars showed the following We acknowledge Tarmac Buxton Lime for providing the quicklime.
trend: steam-slaked lime mortar >  > water-slaked at
Authors’ contributions
75 °C lime mortar > water-slaked at 20 °C lime mor- Conceptualisation: AH, GP and CP. Design of the work: GP and CP. Data acquisi-
tar. Such trend is likely the result of the morphologi- tion: MCG and CP. Data analysis and interpretation: CP, MCG and GP. Writing—
cal characteristics of portlandite crystals, as the finer- original draft: CP and GLP. All authors read and approved the final manuscript.
sized crystals observed in the first two limes can Funding
impart higher colloidal stability and capacity of water This research was funded by Historic England through the project: “Investiga-
to evenly distribute within the body of the mortar. tion of the effect of steam slaking on the characteristics of Portlandite crystals
in hot-mixed mortars”, agreed with Northumbria University on December
• Carbonation rate of the mortars follows the 2019. Alison Henry of Historic England contributed to the design of the study
trend (from the lowest to the highest): steam- and in reviewing the manuscript.
slaked <  < water-slaked at 75 °C < water-slaked at
20 °C. Water content plays an important role in
Pesce et al. Herit Sci (2021) 9:72 Page 17 of 18

Availability of data and materials 20. Rodriguez-Navarro C, Ruiz-Agudo E, Ortega-Huertas M, Hansen E. Nano-
All data generated or analysed during this study are included in this published structure and irreversible colloidal behavior of Ca(OH)2: implications in
article. cultural heritage conservation. Langmuir. 2005;21(24):10948–57.
21. Rodriguez-Navarro C, Ruiz-Agudo E, Burgos-Cara A, Elert K, Hansen EF.
Crystallization and colloidal stabilization of Ca(OH)2 in the presence of
Declarations nopal juice (Opuntia ficus indica): implications in architectural heritage
conservation. Langmuir. 2017;33(41):10936–50.
Competing interests 22. Rosell JR, Haurie L, Navarro A, Cantalapiedra IR. Influence of the traditional
The authors declare that they have no competing interests. slaking process on the lime putty characteristics. Constr Build Mater
[Internet]. 2014;55:423–30. https://​doi.​org/​10.​1016/j.​conbu​ildmat.​2014.​
Author details 01.​007.
1
Department of Architecture and Built Environment, Northumbria University, 23. Navrátilová E, Tihlaříková E, Neděla V, Rovnaníková P, Pavlík J. Effect of the
Newcastle upon Tyne NE1 8ST, UK. 2 Historic England, The Engine House, Fire preparation of lime putties on their properties. Sci Rep. 2017;7(1):1–9.
Fly Avenue, Swindon SN2 2EH, UK. 24. British Standards Institution. BS EN 196-1:2016 methods of testing
cement. 2016.
Received: 12 February 2021 Accepted: 6 June 2021 25. Hall WH. X-ray line broadening in metals [3]. Proc Phys Soc A.
1949;62(11):741–3.
26. British Standards Institution. Products and systems for the protection and
repair of concrete structures—test methods—determination of carbona-
tion depth in hardened concrete by the phenolphthalein method. BS EN
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