CharacterisationCharacterisationof ooffofold ...cathedral.lnec.pt/publicacoes/c4.pdf · CharacterisationCharacterisationof ooffofold oollddoldmortars mortars ... TG - DTA Binder

CharacterisationCharacterisationCharacterisationCharacterisation ofofofof oldoldoldold mortarsmortarsmortarsmortars

António Estêvão CandeiasWorkshop “Science for Cultural Heritage” Trieste, October 23-28, 2006

City of Évora UNESCO World Heritage Site since 1986

Trieste, 0ctober 23-28, 2006

one or two binders(lime, clay, gypsum, cement)

aggregates(siliceous, dolomitic or calcareous sands)

water

additives(ceramics, pozzolans, fibers, etc.)

and occasionally painted layers

WhatWhatWhatWhat isisisis a a a a mortarmortarmortarmortar ????

A mortar is a composite material made of :

Mortars are classified according to the type of binder used.

• Evaluate their macro- and micro-structural properties

• Can give valuable information about a monuments history,namely the techniques of construction, past interventionsand degradation processes

• The information is essential for the design of newaesthetic and functional compatible mortars.

TheTheTheThe studystudystudystudy ofofofof oldoldoldold mortarsmortarsmortarsmortars

University of Évora

António Candeias (chemist)Pedro Nogueira (geologist)José Mirão (mineralogist)

National Laboratory of Civil Engineering

António Santos Silva (chemist)Rosário Veiga (civil engineer)Patrícia Adriano (chemist, grant student)Ana Christian (civil engineer, PhD student)

Portuguese Institute of Architectural Heritage (IPP AR)Margarida Botto (art historian)Sofia Salema (architect)Deolinda Tavares (conservator, Master student)

Portuguese Institute of Conservation and Restoratio n (IPCR)

Isabel Seruya (physicist)Milene Gil Casal (conservator; PhD student)Isabel Ribeiro (chemist)

Polytechnic Institute of Tomar (IPT)

João Coroado (geologist)

JointJointJointJoint CollaborationCollaborationCollaborationCollaboration Projects POCI/HEC/57915/2004

POCI/HEC/59555/2004

VillaVillaVillaVilla ofofofof S. S. S. S. CucufateCucufateCucufateCucufate

II AC

Tank

Main House wall

RomanRomanRomanRoman PeriodPeriodPeriodPeriod

S. S. S. S. CucufateCucufateCucufateCucufate

II AC

III AC

TrTrTrTróóóóia (Setia (Setia (Setia (Setúúúúbal)bal)bal)bal)Cetareas (salt tanks)

Tumbs



II AC

III AC

TrTrTrTróóóóia (Setia (Setia (Setia (Setúúúúbal)bal)bal)bal)

V-VI AC

MMMMéééértolartolartolartola

River Tower

Cryptoportic



II AC

III AC


V-VI AC


XII

MosqueMosqueMosqueMosque / M/ M/ M/ Méééértolartolartolartola’’’’s s s s mainmainmainmain ChurchChurchChurchChurch

Mihrab

MuslimMuslimMuslimMuslim perperperperííííodododod

MMMMéééértolartolartolartola’’’’s s s s mosquemosquemosquemosque

XII-XVI

ÉÉÉÉvoravoravoravora’’’’s s s s CathedralCathedralCathedralCathedral

ChristianChristianChristianChristian EraEraEraEra


II AC

III AC


V-VI AC


XII

XII-XVI

XIV

Amieira Amieira Amieira Amieira CastleCastleCastleCastle

ChristianChristianChristianChristian EraEraEraEraMMMMéééértolartolartolartola’’’’s s s s mosquemosquemosquemosque

XII-XVI


II AC

III AC


V-VI AC


XII

ÉÉÉÉvoravoravoravora’’’’ssssCathedralCathedralCathedralCathedral

XVI

Viana do Alentejo Viana do Alentejo Viana do Alentejo Viana do Alentejo CastleCastleCastleCastle


XII-XVI

XIV


XII-XVI


II AC

III AC


V-VI AC


XII

AmieiraAmieiraAmieiraAmieiraCastleCastleCastleCastle


XVI-XVIII

Elvas Elvas Elvas Elvas CathedralCathedralCathedralCathedral


XVIXII-XVI

XIV


XII-XVI


II AC

III AC


V-VI AC


XII



Viana Viana Viana Viana CastleCastleCastleCastle

XVI-XVIII

Elvas Elvas Elvas Elvas cathedralcathedralcathedralcathedral


XVIXII-XVI

XIV


XII-XVI


II AC

III AC


V-VI AC


XII




XVI

OdemiraOdemiraOdemiraOdemiraMercysMercysMercysMercys ChruchChruchChruchChruch

XVI-XVIII

Elvas Elvas Elvas Elvas cathedralcathedralcathedralcathedral


XVIXII-XVI

XIV


XII-XVI


II AC

III AC


V-VI AC


XII




XVI

EstremozEstremozEstremozEstremozCapuchos Capuchos Capuchos Capuchos MonasteryMonasteryMonasteryMonastery

OdemiraOdemiraOdemiraOdemiraMercysMercysMercysMercys ChruchChruchChruchChruch

XVII

CharacterisationCharacterisationCharacterisationCharacterisation MethodologyMethodologyMethodologyMethodology MORTARSMORTARSMORTARSMORTARS

Drying at 40 ºCStereo-zoom microscope

(7.5- 120x)

Sample disaggregation and preparation for characterisat ion

XRD

Mineralogicalcomposition

TG - DTA

Binder compositonand classification

AAS....

Chemicalanalysis

Solublefraction

Insolubleresidue

Soluble saltsBinder composition

Aggregates compositionParticle size distribution

SEM-EDX

Mortar compositionand morphology

Degradation diagnosis

opticalmicroscopy

Nature, colorand morphologyof the aggregates

Watersorption

Cappilarycoefficient

mechanicalresistance

Compressiveresistance

mercuryporosimetry

PorosityPore size distribution

ChemicalChemicalChemicalChemical analysisanalysisanalysisanalysis MORTARSMORTARSMORTARSMORTARS

� � � � Soluble salts (NO 3-, Cl-, SO4

2-)

�� Elemental analysis (Si, Al, Fe, Na, K, Ca, Mg)

Soluble fraction

Biotite Ceramic fragments

Rose and green quartz

Quartz with mica

�� Aggregates composition and morphology

Schist

Quartz (rolled)Insoluble fraction

ÉÉÉÉvora Cathedralvora Cathedralvora Cathedralvora Cathedral MertolaMertolaMertolaMertola CryptoporticCryptoporticCryptoporticCryptoportic

0

5

10

15

20

25

30

35

40

G1 G2 G3 G4 G5 G6 G7 G8

fracções granulométricas

%

SEV1

SEV2

SEV4

SEV6

SEV7

�� Particle size distribution

XXXX----rayrayrayray diffractiondiffractiondiffractiondiffraction MORTARSMORTARSMORTARSMORTARS

Mineralogical compositionof crystalline fases

Mortars binder composition and CO2 content

Combined with chemical analysisallows determination of the:

aggregates / binder ratio

TGA / DTATGA / DTATGA / DTATGA / DTA MORTARSMORTARSMORTARSMORTARS

calciticlime

dolomiticlime

Gypsum

MihrabMihrabMihrabMihrab, , , , MertolaMertolaMertolaMertola

EvoraEvoraEvoraEvora CathedralCathedralCathedralCathedral

EvoraEvoraEvoraEvora CathedralCathedralCathedralCathedral

SEM / EDXSEM / EDXSEM / EDXSEM / EDX MORTARSMORTARSMORTARSMORTARS

Elemental analysis / composition



Aggregates and binder morphology

quartz mica

brucite

paste

paste feldspar



Aggregates and binder morphology

Neoformation / degradation products

halite

gypsum

biological colonization carbon particle

C. A. S. polen

Aggregates nature, color and morphology

Spatial interrelations of mortar components

POLISHED SURFACES

OpticalOpticalOpticalOptical MicroscopyMicroscopyMicroscopyMicroscopy MORTARSMORTARSMORTARSMORTARS

THIN SECTIONS

OpticalOpticalOpticalOptical MicroscopyMicroscopyMicroscopyMicroscopy MORTARSMORTARSMORTARSMORTARS

Aggregates nature, color and morphology

Spatial interrelations of mortar components

aggregate / binder interfacial reactions

ElvasElvasElvasElvas CathedralCathedralCathedralCathedral ÉÉÉÉvora Cathedralvora Cathedralvora Cathedralvora Cathedral

Sometimes … origin of the aggregates

y = 0,777x

R2 = 0,999

y = 0,454x

R2 = 0,997

y = 0,380x

R2 = 0,9761

0

1

2

3

4

5

6

7

0 5 10 15 20 25 30 35 40

Tempo (min 1/2)

Águ

a ab

sorv

ida

(kg/

m2 )

SEV 1 SEV2 SEV 4

Cappilary coeficients

WaterWaterWaterWater sorptionsorptionsorptionsorption MORTARSMORTARSMORTARSMORTARS

geotextileimpregnated with water

1 cm

CompressionCompressionCompressionCompression resistanceresistanceresistanceresistance MORTARSMORTARSMORTARSMORTARS

Mechanical resistance is correlated with the chemical composition of the mortars

0,00E+00

2,00E-02

4,00E-02

6,00E-02

8,00E-02

1,00E-01

1,20E-01

1,40E-01

0,001 0,01 0,1 1 10

Raio de poro (micrómetros)

dV/d

logr

(cc

/g)

SEV1

SEV2

SEV3-INT

SEV3-IM

SEV3-EXT

SEV4

SEV6

SEV7

SEV8-INT

SEV8-EXT

pore size distribution

MercuryMercuryMercuryMercury porosimetryporosimetryporosimetryporosimetry andandandand nitrogennitrogennitrogennitrogen adsorptionadsorptionadsorptionadsorption MORTARSMORTARSMORTARSMORTARS

Mural Mural Mural Mural paintingspaintingspaintingspaintings / / / / paintedpaintedpaintedpainted layerslayerslayerslayers

CharacterisationCharacterisationCharacterisationCharacterisation MethodologyMethodologyMethodologyMethodology PaintedPaintedPaintedPainted layerslayerslayerslayers

Sample preparation for characterisation

µµµµ−−−−XRD

MineralogicalComposition

Pigment identification

In-situ XRF

Elemental analysisBinder and pigment

identification

SEM-EDX

Elemental analysisPigment morphology

opticalmicroscopy

Layered structureColor, texture

Pigment particle size

µµµµ−−−−chemicalanalysis


S. AntS. AntS. AntS. Antóóóónio dos capuchos nio dos capuchos nio dos capuchos nio dos capuchos MonasteryMonasteryMonasteryMonastery ( XVII ( XVII ( XVII ( XVII centurycenturycenturycentury))))

220x

OpticalOpticalOpticalOptical microscopymicroscopymicroscopymicroscopy PaintedPaintedPaintedPainted layerslayerslayerslayers

Layered structureColorTexturePigment particle size

MicrochemicalMicrochemicalMicrochemicalMicrochemical analysisanalysisanalysisanalysis PaintedPaintedPaintedPainted layerslayerslayerslayers

White lead


Freixo de Espada a Cinta Freixo de Espada a Cinta Freixo de Espada a Cinta Freixo de Espada a Cinta ChurchChurchChurchChurch

220x

Micro Micro Micro Micro XXXX----rayrayrayray diffractiondiffractiondiffractiondiffraction PaintedPaintedPaintedPainted layerslayerslayerslayers

Mineralogical compositionPigment identification

ochre

S. AntS. AntS. AntS. Antóóóónio dos capuchos nio dos capuchos nio dos capuchos nio dos capuchos MonasteryMonasteryMonasteryMonastery ( XVII ( XVII ( XVII ( XVII centurycenturycenturycentury))))

Freixo de Espada a Cinta Freixo de Espada a Cinta Freixo de Espada a Cinta Freixo de Espada a Cinta ChurchChurchChurchChurch

RedRedRedRed layerlayerlayerlayer WhiteWhiteWhiteWhite layerlayerlayerlayer GreyGreyGreyGrey layerlayerlayerlayer

SEM/EDXSEM/EDXSEM/EDXSEM/EDX PaintedPaintedPaintedPainted layerslayerslayerslayers

vermillion White lead Gypsum

Elemental analysis

Pigment morphology

final considerations

Binder

Aggregates

Additives

Mortars composition (binder/aggregates ratio)

State of conservation / degradation products

Physical properties

Insight on technical knowledge

MethodologyMethodologyMethodologyMethodology givesgivesgivesgives informationinformationinformationinformation aboutaboutaboutabout::::

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CharacterisationCharacterisationof ooffofold ...cathedral.lnec.pt/publicacoes/c4.pdf · CharacterisationCharacterisationof ooffofold oollddoldmortars mortars ... TG - DTA Binder