Self-Levelling Flooring Compounds

Based on

Ternary Binder Systems

CIMSA Dry-Mix Mortar Seminar

Istanbul, 21 September 2017
Prof. Dr. Johann Plank
Technische Universität München
Chair for Construction Chemistry
Content ……
….. Dry-Mix Mortar Products

….. Principle Properties of CAC

….. SLUs - Properties & Composition

….. Admixtures for SLUs

….. Raw Materials and Formulations

….. Ageing of SLUs

….. Conclusion
 Modern Building Technology

Phaeno Center, Wolfsburg

Residence of German
Chancellor, Berlin

© Prof. Plank 2017

 The Origin of Dry-Mix Mortar Technology

• rebuilding German cities

after World War II

• shortage of workers for con-

struction in the 1960s/1970s

• dry-mix mortar allows to

build faster and in
Nuremberg, May 1945 better quality

© Prof. Plank 2017

 The Origin of Dry-Mix Mortar
- traditional building: manual mixing on construction site
- no quality control
- many workers required

Traditional job-site mortar mixing

Early mortar mixing machine from
Kalkwerk Mathis, Merdingen (early 1970s)

In the 1970s, beginning of dry-mix mortar industry

© Prof. Plank 2017
 Thin-Bed Tile Adhesives
• Thin-bed technology invented by Sponagel in Switzerland in 1930s

• First dry-mix CTA introduced in 1959 by ARDEX and

Polychemie GmbH (PCI) Augsburg

Laying tiles by conventional Laying tiles by modern thin-

„buttering“ method bed mortar technology

Thin-bed mortar allows to save approx. 35 % of material

© Prof. Plank 2017
 Wall Renders and Plasters

Exterior and interior wall

plasters / renders

© Prof. Plank 2017

 CTAs and Joint Fillers (Grouts)

Tile grout Flooring using CTA

© Prof. Plank 2017
 External Insulation and Finishing
System (EIFS)

Adhesives and mortars for EIFS

© Prof. Plank 2017

 EIFs Systems

- difficult to place
- expensive
- problem of waste
- fire hazard

2017
© Prof. Plank 2012
 Fire at Grenfell Tower, London
• Fire on 14 June 2017
• at least 80 people were killed
• polystyrene boards behind Al sheets caught fire

© Prof. Plank 2017

 Fire Hazard of Conventional EIFS

Shanghai, 2011
Istanbul, July 2012
2017
© Prof. Plank 2012
 Inorganic Insulation Materials

Aerogel granulate

Glass wool

Mineral wool

Application of aerogel render

© Prof. Plank 2017
 Self-Levelling Underlayments (SLUs)

• Perfect self-spreading and self-healing property

• Excellent smooth surface
© Prof. Plank 2017
 Self-Levelling Underlayments (SLUs)

SLU based on a
ternary binder system

Demonstration of
self-levelling and self-healing
property of a SLU

© Prof. Plank 2017

SLU Formulation Based on Ternary Binder
Grey alumina cement (~ 40 % Al2O3) for high early strength

Portland Cement (CEM I 42,5 R) 18,50 wt.-%

Calcium Alumina Cement (~ 40% Al2O3) 11,50 wt.-%
CaSO4 (synthetic anhydrite) 6,50 wt.-%
Quartz sand (0,1 to 0,315 mm) 41,00 wt.-%
Limestone powder (10 to 20 µm) 19,40 wt.-%
Casein or PCE (Superplasticizer) 0,40 wt.-%
Vinylacetate-Copolymer (Redispersible Powder) 2,00 wt.-%
NaK-tartrate (Retarder) 0,40 wt.-%
Li2CO3 (Accelerator) 0,10 wt.-%
Cellulose ether (Water Retention Agent) 0,05 wt.-%
Polyglycol (Defoamer) 0,15 wt.-%

Mixing Water (for 100 wt.-% powder blend) 20,00 wt.-%

 Dry-Mix Mortar Industry

© Prof. Plank 2017

Content ……
….. Dry-Mix Mortar Products

….. Principle Properties of CAC

….. SLUs - Properties & Composition

….. Admixtures for SLUs

….. Raw materials and formulations

….. Ageing of SLUs

….. Conclusion
 Definition and Origin of CAC
Cements with at least 35 % of Al2O3

Main hydraulic phases: CA, C12A7 and less reactive CA2

1840 J.L. Vicat realized the sulfate resistance of CAC

1908 Industrial development of Aluminate Cement is

associated with the work of J. Bied (British Pat. 8193)

1918 Ciment Fondu first CAC marketed by Lafarge Company Alumina cement based concrete used
in WW I for heavy guns

After World War II, aluminate cement was developed as binder for refractory castables

In the 1950‘s, development of complex mortars containing combinations of aluminate

cement, Portland cement and Ca- Sulfates for the building industry (dry mortars)

© Prof. Plank 2017

Chemical Composition of Aluminate Cements

Portland Cement

Aluminate Cement
 Main Phases in CAC
• Monocalcium aluminate CA
• Grossite CA2
• Mayenite C12A7
• Gehlenite C2AS
• Belite C2S
• Ferrite C4AF CA CA2

C12A7 C2AS
© Prof. Plank 2017
 Chemical Composition of Aluminate Cements

Oxide Aluminate Cement Portland Cement

Al2O3 36% to 80% 4% to 8%

CaO 20% to 42% 60% to 70%
SiO2 0,2% to 8% 18% to 24%
Fe2O3 0,2% to 20% 1% to 5%
TiO2 < 2%
MgO < 1% < 3%
Na2O < 0,3% < 1%
K2O < 0,1% < 1%

© Prof. Plank 2017

 Type

(dark)
Fondu
(grey)
(white)
Secar 71

Secar 51

15
CA CA

Mayenite
CA CA CA

20
CA2

CA
CA CA

CA CA CA
CA2

CA

2-Theta - Scale
CA

CA2

30
CA CA CA

Gehlenite Gehlenite

Perowskite
Perowskite
Ca3Fe2TiO8
Brownmillerite
CA2

CA CA CA
XRD Diagrams of Aluminate Cement

40
 Manufacture of Aluminate Cements
Raw Materials: Limestone and Bauxite
In many cases, red mud from the Bayer process is used as raw material

Standard grade Aluminate Cement Grades of higher Aluminate Cement

Up to 50% Al2O3 60% to 80% Al2O3
Up to 20% Fe2O3 Very low Fe2O3
Several per cent TiO2 Very low SiO2
Silica content must be fairly low

Usually made by melting in Usually made by sintering in

furnaces at 1600 °C rotary kilns at 1450 °C
 Advantages of CAC vs. OPC
Unique properties of CAC:
Rapid hardening with setting time similar to Portland Cement

High Resistance to sulfate attack and acids

Ability to withstand repeated heating to high temperatures

Ability to hydrate and perform at low temperatures (e.g. 2 °C)

Resistance to abrasion

Adjustable properties in mixtures with Portland Cement and

calcium sulfates

© Prof. Plank 2017

 CAC Develops Higher Early Strength Than OPC

Alumina Cements harden more rapidly than Portland Cements;

within one or two days they reach their specified strength

Strength development of CAC and OPC Heat flow of CAC and OPC

30

25
CAC 40 % Al2O3
Fondu
80

Wärmefluß [mW/g]
20 PZCEM
42,5I 42,5
Mielke Classic
R Milke Classic
compressive strength

70
60
15
50
MPa

40 10
30
20 5
CAC
10
OPC
0 0
3h 6h 1 day 7 days 28 days 0 10 20 30 40
Zeit [Stunden]

CAC is used to accelerate strength development of OPC

© Prof. Plank 2017

 Shrinkage Behavior of Calcium Aluminate Cement

Addition od CAC to OPC compensates the shrinkage of OPC

through ettringite formation

CAC/OPC

OPC/CAC

OPC

Shrinkage as a function of alumina cement content in binder:

A = OPC; B = OPC-rich blend; C = CAC-rich blend

© Prof. Plank 2017

 Applications of Aluminate Cements

Sewage pipes Tile grouts

Rotary Kiln, Cement Plant

Refractory
Corrosive
environments Dry-mix mortars

© Prof. Plank 2017

 Benefits from Aluminate Cements

Self-levelling underlayment Tile adhesive

Rapid Shrinkage
Hardening Compensation

Quick Chemical
Drying Resistance
Cementitious tile grout
© Prof. Plank 2017
 Tile grouts: CAC vs. OPC
Cleaning machine

dissolved OPC grout CAC grout

Tile grouts based on CAC are much more durable

© Prof. Plank 2017

Content ……
….. Dry-Mix Mortar Products

….. Principle Properties of CAC

….. SLUs - Properties & Composition

….. Admixtures for SLUs

….. Raw Materials and Formulations

….. Ageing of SLUs

….. Conclusion
 Self-Levelling Underlayments (SLUs)

© Prof. Plank 2017

 Three Principle Types of SLUs
Component CAC -rich w/CSA cement OPC - rich

CAC 40 27 % 48 % 56 %
OPC 54 % - 30 %

β - HH - 17 % 14 %

α - HH 19 % - -

CSA - 35 % -

Superplasticizer 0.38 – 0.78 %

Set Control agents 1–2%
Na3-citrate × × ×
Tartaric acid × × ×
Li2CO3 × × ×
Na2CO3 × - -
Ca(OH)2 × - -
Water-to-Binder 0.59 0.76 0.92

© Prof. Plank 2017

 CAC – Rich SLU Formulation
Component Function Mass %
CAC 40 % Al2O3 Aluminate Cement 18.00
CEM I 52,5 N Portland Cement 3.60
CaSO4 ∙ 0.5 H2O HH - Binder 6.30
CaCO3 powder Filler 24.35
Sand Filler 45.34
Tartaric acid Retarder for OPC 0.06
Li2CO3 Accelerator for CAC 0.03
RDP Latex Powder Provides adhesion 2.00

Polyglycol Defoamer 0.10

Methyl cellulose Water retention 0.10
PCE powder Superplasticizer 0.12
Total 100.00
Water 23.00
Water/Cement Ratio 1.06
Water/Binder Ratio 0.82

© Prof. Plank 2017

 OPC – Rich SLU Formulation
Grey alumina cement (~ 40 % Al2O3)

Portland Cement (CEM I 42,5 R) 18,50 wt.-%

Calcium Alumina Cement (~ 40% Al2O3) 11,50 wt.-%
CaSO4 (synthetic anhydrite) 6,50 wt.-%
Quartz sand (0,1 to 0,315 mm) 41,00 wt.-%
Limestone powder (10 to 20 µm) 19,40 wt.-%
Casein or PCE (Superplasticizer) 0,40 wt.-%
Vinylacetate Copolymer (Redispersible Powder) 2,00 wt.-%
NaK tartrate (Retarder) 0,40 wt.-%
Li2CO3 (Accelerator) 0,10 wt.-%
Cellulose ether (Water Retention Agent) 0,05 wt.-%
Polyglycol (Defoamer) 0,15 wt.-%

Mixing Water (for 100 wt.-% Powder blend) 20,00 wt.-%

 Setting Time of Mixtures CAC/OPC

• blends of CAC and OPC often show

extremely fast setting

no workability OPC-
CAC-
rich
rich

• only CAC/OPC 20:80 or 85:15 work

• retarders for OPC required to prevent

rapid setting

© Prof. Plank 2017

Combinations of Alumina Cement and Portland Cement

Mixtures of OPC and CAC are used to accelerate setting/strength

development of cement
Such mixtures show lower compressive strength than pure OPC or CAC

80
28d Pure CAC
70

Compressive Strength [MPa]

60 7d

Compressive strength 50 Pure 1d

40 OPC
of OPC and CAC 6h
30
combinations 3h
20

10

0
0 20 40 60 80 100

Alumina Cement %

© Prof. Plank 2017

Combination of Alumina Cement and Portland Cement

Combinations of CAC and Portland cement are very sensitive

to variations in OPC composition

350 50
45
300 Portland Cement A
Portland Cement A 40
Portland Cement B

compressive strength
Portland Cement B
250 35 Portland Cement C
Initial Set [min]

Portland Cement C
30
200

150
B C 25 B
20

100
A 15
10
50
5
0 0
0% 5% 10% 15% 20% 25% 30% 35% 40% 45% 0% 5% 10% 15% 20% 25% 30% 35% 40% 45%

Alumina Cement added Alumina Cement added

Influence of OPC type on setting time Influence of OPC type

on 1 day compressive strength

© Prof. Plank 2017

Rapid Hardening Owed to Ettringite Formation

Ettringite

Ettringite crystals formed in the matrix of a ternary binder

© Prof. Plank 2017

 Rapid Drying of SLU
„Chemical“ drying owed to huge water consumption for ettringite formation

3 CaAl2O4 + 3 CaSO4 ∙ 0.5 H2O [Ca3Al(OH)6•12H2O]2•(SO4)3•2H2O

ettringite

Structure of ettringite, showing

plenty of water molecules Ettringite crystals

© Prof. Plank 2017

 Shrinkage Behavior of SLUs

Shrinkage compensation through addition of alumina cement

Reason for reduced shrinkage: expansion because of ettringite formation

CAC-rich

OPC-rich

OPC

© Prof. Plank 2017

 Shrinkage of OPC
OPC develops high shrinkage

After addition of superplasticizers shrinkage becomes even much higher

ettringite formation in ternary binder compensates shrinkage from OPC

Anhydrite (CaSO4)
floor screed

Shrinkage-reduced
cement screed
OPC - based screed

OPC - based screed

with superplasticizer

© Prof. Plank 2017

 Shrinkage of Hardened Cement

Chemical shrinkage Drying shrinkage

Only pores between 10 and 100 nm

cause shrinkage
© Prof. Plank 2017
 Shrinkage Problem of Floor Screeds

Dry Shrinkage
- Severe at high w/c ratio (e.g. 0.70)

Chemical Shrinkage
- Severe at low w/c ratio (e.g. 0.40)

Drying shrinkage
Chemical shrinkage
© Prof. Plank 2017
 Experimental Determination of Chemical and
Drying Shrinkage

© Prof. Plank 2017

Content ……
….. Dry-Mix Mortar Products

….. Principle Properties of CAC

….. SLUs - Properties & Composition

….. Admixtures for SLUs

….. Raw Materials and Formulations

….. Ageing of SLUs

….. Conclusion
 SLU Formulation Based on Ternary Binder

Portland cement (CEM I 42,5 R) 18,50 mass-%

Grey alumina cement (ca. 40 % Al2O3) 11,50 mass-%
Calcium sulfate (anhydrous, synthetic anhydrite) 6,50 mass-%
Silica sand (0,1 - 0,315 mm) 41,00 mass-%
Limestone powder (calciumcarbonate, 10 - 20 µm) 19,40 mass-%
Superplasticizer casein or PCE 0,40 mass-%
Latex polymer (redispersible powder based on vinylacetate) 2,00 mass-%
Retarder (K/Na tartrate / trisodium citrate) 0,40 mass-%
Accelerator (lithium carbonate) 0,10 mass-%
Stabilizer (cellulose ether, low-viscosity type) 0,05 mass-%
Defoamer (powder) 0,15 mass-%
Sum of powder components Total 100,00 mass-%
Water (for 100,00 mass-% powder): 20,00 mass-%

© Prof. Plank 2017

 Casein Superplasticizer

- casein content in bovine milk 2,5 - 3%

- heterogeneous mixture of partly

glycosylated phosphoproteins

- manufactured by acid precipitation

from milk at pH 4,6 / 20 °C

Four major casein fractions:

 -casein ~ 50%  κ-casein ~ 10%

 β-casein 35- 40%  γ-casein < 5%

© Prof. Plank 2017

 Casein Superplasticizer in SLU

Superplasticizers: Casein
Melamine Formaldehyde Sulfite (MFS) Polycondensate
Polycarboxylate (PCE)

© Prof. Plank 2017

 Casein Forms Micelles
Casein micelle according to WALSTRA (1999)

Sub-micelles :
hydrophobic core, consisting
of 20-25 -/b- caseins and
calcium phosphate

Micelle :
Electrostatic and steric stabilization
through formation of an outer ``hairy
layer´´, containing hydrophilic
saccharide residues from the k-
© Prof. Plank 2017 caseins
 -Casein

Tertiary structure of αS1-casein

~ 50,8 % in bovine casein

O
-
- 199 amino acids with 8 phosphate groups O
+
H3N H
- phosphate groups esterified with serine CH2

- net anionic charge: –24 (at pH 6,7) O

-
O P O

- above 2 mmol/L Ca2+ charge neutralization  O-

precipitation Phosphoserine
 b- Casein

Tertiary structure of β1-casein

~ 36,3 % in bovine casein

209 amino acids and 5 phosphate groups

net anionic charge –13 (at pH 6,7)

Formation of Ca precipitate depends on temperature

© Prof. Plank 2017

 k- Casein
Tertiary structure of κ1-casein

~ 12,9 % in bovine casein

- 169 amino acids, up to 5

trisaccharide groups

- only one phosphate group

- net anionic charge –11 (at pH 6,7)

- charge derives from glutamine and

asparagine and saccharides
sialinic acid
- soluble in presence of calcium
© Prof. Plank 2017
 Dispersing Effect of Casein Protein
Fractions
Spread of SLU in mini slump test :

α-casein

© Prof. Plank 2017

 Problems Associated with Casein
• Unstable quality
• Decomposes in alkaline cement strong smell of ammonia !
• Enhances proliferation of mould “sick house syndrom“

Replacement by PCEs

Mould

© Prof. Plank 2017

 PCEs in SLUs
• Excellent dispersing performance…….

but……

• poor compatibility with retarders (tartrate, citrate)

• no self-healing property

160 Casein (0,4%) w ith:

140 Tartrat (0,4%)

slump flow [mm]

120 Citrat (0,4%)

100 PCE (0,4%) w ith:

a fs
fs

80 Tartrat (0,4%)
PCE: poor fluidity with citrate
60 Citrat (0,4%)
0 10 20 30 40 50 60

time after water addition [min]

This PCE is not compatible with citrate

© Prof. Plank 2017
 Adsorption of Casein with/without Retarder

100 80 80 80
Adsorptionsrate [%]

90
80
70
50
60
50
40
30
20
10
0
Casein mit Tartrat Casein mit Citrat

© Prof. Plank 2017

 Adsorption of PCE with / without Retarder

100
90
67
80 67
Adsorption [%]

70
48
60
50
40
30
7
20
10
0
PC mit Tartrat PC mit Citrat

© Prof. Plank 2017

 Optimized PCE For Ternary SLU

Optimized PCE has high anionic charge density

100
82 82
90
80
Adsorption [%]

70 56
60 47
50
40
30
20
10
0
PC 2 mit Tartrat PC 2 mit Citrat

© Prof. Plank 2017

 Rapidly Dissolving PCE Powder
Modified PCEs which hydrate and adsorb immediately (e.g. Melflux® 5581)

PCE Molecule

Cementitious flowing floor screed

© Prof. Plank 2017

Self-Healing Property of PCE-Based SLU
• requires a second admixture: „viscosity - modifying agent“ (VMA)
• e.g. copolymer of AMPS/NNDMA („Starvis“, BASF)
• combination of PCE and VMA provides comparable properties than from
casein

AMPS/NNDMA copolymer
© Prof. Plank 2017
 Tartrate and Citrate Retarders
• generally, tartrate works better as retarder than citrate and is more
compatible with superplasticizers
• however, tartrate is more expeasive
• tartrate has to be the NaK salt of natural tartaric acid („Seignette salt“,
L(+) type), not of the D(-) type or the racemic mixture !

L(+) tartaric acid

citric acid
© Prof. Plank 2017
Content ……
….. Dry-Mix Mortar Products

….. Principle Properties of CAC

….. SLUs - Properties & Composition

….. Admixtures for SLUs

….. Raw Materials and Formulations

….. Conclusion
 CAC - Rich PCE-Based SLU
CAC 40 % Al2O3 20.0 Mass %
CEM I 52.5 R 4.0 Mass %
α - hemihydrate 7.0 Mass %
Durcal 15 (limestone) 19.0 Mass %
Durcal 130 (limestone) 9.0 Mass %
Sand (0 - 0.315 mm) 37.8 Mass %
Li2CO3 0.1 Mass %
Citric acid, Na salt 0.02 Mass %
PCE (Melflux, BASF) 0.25 Mass %
VMA (Starvis, BASF) 0.05 Mass %
MHEC Dow 0.05 Mass %
RDP (Vinnapas, Wacker) 2.00 Mass %
Defoamer (Agitan, Münzing) 0.10 Mass %
Water 24.00 Mass %

© Prof. Plank 2017

 CAC - Rich PCE-Based SLU
CAC 40 % Al2O3 60.00 Mass %
CEM I 32.5 R (Heidelberg) 39.00 Mass %
Anhydrite (Solvay, Hannover) 36.00 Mass %
Quartz sand (H33, 0.1 - 0.315 mm) 83.70 Mass %
CaCO3 powder (Omyacarb 20 - BG) 72.70 Mass %
Calciumhydroxide 4.50 Mass %
PCE (Melflux PP 100 F, BASF) 2.70 Mass %
RDP (Vinnapas RE 523 Z, Wacker) 4.50 Mass %
Tartaric acid (L(+), Merck) 0.90 Mass %
Li2CO3 (< 40 µ, Chemetall) 0.90 Mass %
MHEC (Walocel MT 400, Dow) 0.09 Mass %
Defoamer (Agitan P 800, Münzing) 0.60 Mass %

Water demand: ~ 20 mL for 100 g dry blend

© Prof. Plank 2017

 CAC - Rich Melamine-Based SLU
CAC 40 % Al2O3 200.00 Mass %
CEM I 32.5 R (Heidelberg) 100.00 Mass %
Anhydrite (Solvay) 125.00 Mass %
Sand (H33, Quarzwerke Köln) 300.00 Mass %
CaCO3 powder (Omyacarb 20 - BG) 240.00 Mass %
MFS (Melment F 10, BASF) 6.00 Mass %
RDP (Vinnapas RE 523 Z, Wacker) 25.00 Mass %
Tartaric acid (L(+), Merck) 1.00 Mass %
MHEC (Tylose H 300P, SE Tylose) 1.00 Mass %
Li2CO3 (< 40 µ, Chemetall) 0.80 Mass %
SRA (1,6 - Hexanediol, BASF) 5.00 Mass %
Defoamer (Agitan P 800, Münzing) 2.00 Mass %

Water demand: 22 mL for 100 g dry blend

Open time: ~ 20 min
Walk-on time: ~ 2.5 hours (shore D ≥ 50)
© Prof. Plank 2017
 OPC - Rich Melamine-Based SLU
CEM I 32.5 R (Heidelberg) 300.00 Mass %
CAC 40 % Al2O3 70.00 Mass %
Anhydrite (Solvay, Hannover) 50.00 Mass %
Quartz sand (H33, Quarzwerke Köln) 379.20 Mass %
CaCO3 powder (Omyacarb 20 - BG) 165.00 Mass %
MFS (Melment F 10, BASF) 6.00 Mass %
RDP (Vinnapas RE 523Z, Wacker) 20.00 Mass %
Tartaric acid (L(+), Merck) 1.70 Mass %
Li2CO3 (< 40 µ, Chemetall) 0.60 Mass %
MHEC (Walocel MT 400, Dow) 1.00 Mass %
SRA (1,6 - hexanediol, BASF) 5.00 Mass %
Defoamer (Agitan P 800, Münzing) 1.50 Mass %

Water demand: 22 mL for 100 g dry blend

Open time: ~ 35 min
Walk-on time: ~ 7 hours (shore D ≥ 50)
© Prof. Plank 2017
 OPC - Rich Casein-Based SLU
CEM I 32.5 R (Heidelberg) 54.00 Mass %
CAC 40 % Al2O3 36.00 Mass %
Anhydrite (Solvay, Hannover) 21.00 Mass %
Quartz sand (H33, 0.1 - 0.315mm) 120.00 Mass %
CaCO3 powder (Omyacarb 20 BG) 61.95 Mass %
Casein (Ardex) 1.20 Mass %
RDP (Vinnapas RE 523Z, Wacker) 4.50 Mass %
Na3 - citrate (Merck) 0.60 Mass %
Li2CO3 (< 40 µ, Chemetall) 0.30 Mass %
MHEC (Tylose H 300P, SETylose) 0.15 Mass %
Defoamer (Agitan P 800, Münzing) 0.30 Mass %

Water demand: ~ 20 mL for 100 g dry blend

© Prof. Plank 2017

Content ……
….. Dry-Mix Mortar Products

….. Principle Properties of CAC

….. SLUs - Properties & Composition

….. Admixtures for SLUs

….. Raw Materials and Formulations

….. Ageing of SLUs

….. Conclusion
 SLU Formulation Tested

SLU prehydrated for 1 or 3 days at 35 °C @ 90 % RH

© Prof. Plank 2017

 Rapid Moisture Uptake by SLU
fresh SLU
SEM images

SLU SLU
aged 1 day aged 3 days

Ettringite crystals
Ettringite crystals

© Prof. Plank 2017

 Impact of Moisture on Flow Behaviour of SLU
System PCE - Tartrate • fresh SLU – good flowability
w/b = 0.25

w/binder ratio

fresh SLU is relatively tolerant

towards increased water contents • aged SLU – no flowability
at w/b = 0.25

Time (min)

Ageing affects SLU stronger than

variation of w/b ratio in fresh SLU

© Prof. Plank 2017

Impact of Moisture Uptake on Flow Behavior of SLU

System PCE - Tartrate

Time (min)

Workability of aged SLU with tartrate significantly lower

© Prof. Plank 2017
 1 Day Ageing – Comparison Tartrate / Citrate

System PCE – Tartrate / Citrate (w/b = 0.25)

Tartrate Citrate

After only 1 day of exposure to moist air, SLU containing

tartrate or citrate was no longer fluid;
but tartrate system behaved better than citrate system
© Prof. Plank 2017
 Flow Behavior of SLU with Citrate
System PCE – Citrate dosages 0.44/ 0.44 M.-%

In the aged SLU, the retarding effect of citrate becomes stronger,

leading to longer open times but poor fluidity
© Prof. Plank 2017
 Compressive Strengths: Fresh vs. Aged SLU
1 day compressive strength

Compressive strength (N/mm )

2
Lower compressive 80
70
strength because of 60
- 40 %
50
higher water demand 40 SLU: citrate + PCE
30
and air voids 20
10
0
fresh
fresh aged 1 d
prehydrated
SEM

fresh SLU aged SLU

Compressive Strengths: Fresh vs. Aged SLU

Comparison of different admixture combinations

citrate + PCE citrate + casein tartrate + casein

Compressive strength (N/mm )

Compressive strength (N/mm )

Compressive strength (N/mm )

2

2
80 80
80
70 70
70 - 40 % 60 60
60
50 50 50
40 40 - 40 % 40
30 30
30
20
- 50 %
20 20
10 10 10
0 0 0
fresh
fresh aged 1 d
prehydrated fresh
fresh prehydrated
aged 1 d fresh
fresh aged 1 d
prehydrated

1 day compressive strengths

© Prof. Plank 2017

 Water Demand and Appearance of SLU
SLU with citrate and PCE, aged 1 day

w/b ratio adjusted to

18 cm flow

Prism prepared from fresh SLU (w/b = 0.25)

Aged SLU
contains
air voids
Prism prepared from aged SLU (w/b = 0.27)

© Prof. Plank 2017

Compressive Strengths: Fresh vs. Aged SLU
SLU aged 1 day contains unreacted binders (CAC, anhydrite)

CAC

CaSO4

CAC

fresh aged 1 cm

SLU: citrate + PCE

© Prof. Plank 2017
 Appearance of Aged SLU

Gypsum

© Prof. Plank 2017

 Packaging Requirements For SLUs

• bags must have a plastic inlet which functions as a water vapor barrier

• some SLU producers use bags with Al foil inside, similar as in some food
products

Al foil

© Prof. Plank 2017

Content ……
….. Dry-Mix Mortar Products

….. Principle Properties of CAC

….. SLUs - Properties & Composition

….. Admixtures for SLUs

….. Raw Materials and Formulations

….. Ageing of SLUs

….. Conclusion
 Summary - Part I
• SLUs are high - performance dry mixes

• SLUs provide a perfect smooth substrate for tiles, carpets, parquet,

vinyl floors etc.

• SLUs are easy to place and spread

• SLUs develop strength rapidly, owed to CAC

• Especially CAC - rich formulations can be walked on within 2 - 3 hours

• Rapid and massive ettringite formation provides „chemical“ drying and

shrinkage compensation

© Prof. Plank 2017

 Summary - Part II

• SLUs require high quality packaging (bags) and fresh cements

• SLUs require proper on-site mixing device

Western Europe: batch mixing in bin Scandinavia: mixing by machine

© Prof. Plank 2017

 Why CAC - Based SLU ?
• SLUs can be formulated as well based on α-hemi hydrate ….
but ……….
• CaSO4 - based SLUs show longer walk-on times and slower strength development
• CaSO4 - based SLUs develop a glass-like skin of CaCO3/superplasticizer on the
surface which prevents proper adbesion of the next layer (tiles, carpet…)
• Glassy layer has to be removed by using a milling machine
costly additional step!
• Gypsum is not water - resistant!

Removing glassy skin of

gypsum-based SLU
Milling machine
SLUs – Perfect Products For Modern Building

© Prof. Plank 2017

 Chair For Construction Chemistry at
TU München

© Prof. Plank 2017

International PCE Conference 2017

2nd International Conference

on Polycarboxylate Superplasticizers
(PCE 2017)

September 27 - 28, 2017

Munich, Germany

www.pce-conference.org

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