Journal
, 82 [10] 2900–905 (1999)
Formation of Ettringite from
Monosubstituted Calcium Sulfoaluminate Hydrate and Gypsum
Department of Materials Science and Engineering, Pennsylvania State University,
The formation of ettringite (3CaOⴢAl2O3ⴢ3CaSO4ⴢ32H2O)
from monosulfate (3CaOⴢAl2O3ⴢCaSO4ⴢ12H2O) and gyp-
sum (CaSO4ⴢ2H2O) was investigated by isothermal calo-
rimetry and X-ray diffraction (XRD) analyses. Hydration
was carried out at constant temperatures from 30° to 80°C
using deionized water and 0.2M, 0.5M, and 1.0M sodium
hydroxide (NaOH) solutions. Ettringite was found to be the
dominant crystalline phase over the entire temperature
range and at all sodium hydroxide concentrations. A so-
dium-substituted monosulfate phase was formed as a hy-
dration product in the 1.0M sodium hydroxide solution
regardless of temperature. XRD and calorimetry demon-
strate that hydration in increasing sodium hydroxide con-
centrations decreases the amount of ettringite formed and
retards the rate of reaction. The apparent activation energy
for the conversion of the monosulfate/gypsum mixture to
ettringite was observed to vary depending on the sodium
hydroxide concentration. Ettringite formation was ob-
served to depend upon the concentration of calcium in so-
lution; thus the formation of calcium hydroxide and so-
dium-substituted monosulfate phase competes with
ettringite formation.
I. Introduction
E TTRINGITE is a hydrated sulfoaluminate compound
(3CaO⭈Al2O3⭈3CaSO4⭈32H2O) and is commonly formed in
concrete during curing. Monosulfate (3CaO⭈Al2O3⭈CaSO4⭈
12H2O) is a related sulfoaluminate compound. In cement no-
menclature ettringite is also referred to as AFt and monosulfate
as AFm. Ettringite formation while the concrete is in a plastic
state contributes to the initial “setting” of concrete. Alterna-
tively, ettringite formation after concrete has “set” into a rigid,
solid mass can be deleterious and can cause the loss of struc-
tural integrity. The reason for this dual character is due to the
solid specific volume increase accorded to ettringite formation.
In the literature, expansion due to ettringite formation is attrib-
uted to its needlelike structure.1 Monosulfate incorporates only
1 mol of sulfate and exhibits a platelike microstructural mor-
phology.2 The formation of monosulfate in hardened concrete
is generally not considered deleterious, because its formation
causes less expansion than does that of ettringite. There is,
however, evidence in the literature which indicates that mono-
sulfate formation also causes expansion.3,4
The formation of ettringite and monosulfate from cement
phases (tricalcium aluminate and gypsum) has been studied
C. M. Jantzen—contributing editor
Manuscript No. 190392. Received February 9, 1998; approved April 24, 1998.
Supported by the National Science Foundation under Grant No. CTS 93-09528 and
by the R. J. Lee Group, Inc.
*Member, American Ceramic Society.
2900
J. Am. Ceram. Soc.
Boyd A. Clark* and Paul W. Brown*
University Park, Pennsylvania 16802
extensively.5–9 The formation of these sulfoaluminates occurs
during normal curing, but can also be caused by interaction
with a variety of environments, including intrusion of solutions
containing high concentrations of sulfate and/or other ionic
species. Thus the interaction of various ionic species and their
effects on ettringite and monosulfate formation have also been
studied extensively.10 Concrete is a hydrated, porous medium
and a certain amount of “free” water is usually present in the
pores. This porosity allows solutions to move through concrete
and this may result in sulfoaluminate compound formation.
There is also evidence in the literature that the interaction of
ionic species (most notably alkali ions) initially present may
cause subsequent sulfoaluminate compound formation.11
The presence of various ionic species can cause a conversion
of monosulfate into other AFm phases. One such phase is a
sodium-substituted AFm phase referred to as the “U-phase.”
Such a sodium-substituted AFm phase (4CaO⭈0.9Al2 O3 ⭈
1.1SO3⭈0.5Na2O⭈16H2O) has been observed when C3A hydra-
tion was carried out in high concentrations of sodium and
sulfate.12 Recent studies indicate that the U-phase also forms in
ordinary portland cement and its formation results in expan-
sion, implying a deleterious effect in hardened concrete.4,13
Although much work has been done to study the formation
of ettringite from C3A followed by its conversion to monosul-
fate, we are unaware of any studies which have considered the
conversion of monosulfte to ettringite. Therefore, the mecha-
nism and kinetics of ettringite formation from monosulfate are
investigated in the present study. Deionized water and various
concentrations of sodium hydroxide solutions were used to
hydrate a monosulfate/gypsum mixture. Isothermal calorimetry
and X-ray diffraction (XRD) were used to characterize the rates
of hydration and the crystalline phases formed. Analysis of the
results obtained by these methods provides insight into the
kinetics of the hydration processes involved and the stability of
the various phases formed.
II. Methods and Materials
(1) Monosulfate Synthesis
The precursor monosulfate powder was prepared by mixing
a slurry of tricalcium aluminate and gypsum under an inert gas
(nitrogen) using a modification of the method outlined by Tay-
lor14 (CaCl2 or soda lime were not used for drying). The slurry
was filtered and dried, again under nitrogen, and then mixed
with gypsum powder at a molar ratio of 1:2.5.
(2) Experimental Procedure
Isothermal calorimetry was performed using the experimen-
tal setup described by TenHuisen et al.15 Approximately 1.00
g of the monosulfate/gypsum mixture and 3.0 mL of solution
were used for each sample run. Solutions used were deionized
water, and 0.2M, 0.5M, and 1.0M NaOH. The solid sample and
a syringe containing the solution were allowed to reach equi-
librium at each experimental temperature before injection.
Sample runs were carried out at 30°, 40°, 50°, 60°, 70°, and
80°C.
October 1999 Formation of Ettringite from Monosubstituted Calcium Sulfoaluminate Hydrate and Gypsum 2901

As the solution was inoculated onto the solid sample, heat

output was measured by thermopiles, which completely en-
closed the sample cup. Data points were collected at 0.1 s
intervals. When further heat output could not be observed, the
solids present were removed from the calorimeter, washed with
acetone, and allowed to air dry before XRD characterization.
These solids were hand ground in an agate mortar and pestle
to a fineness of approximately 325 mesh (45 ␮m diameter
particulate).
A Scintag 3100 system powder diffraction unit was used to
examine the powders. All samples were scanned at 2°/min
between 5° and 55° 2␪, using CuK␣ radiation. Analysis of the
XRD data is complicated in that the ettringite pattern has dif-
fraction X-ray peaks which overlap the primary diffraction
peaks for monosulfate, calcium hydroxide, and the U-phase.
This problem was overcome by examining the ratio of the
primary (monosulfate, calcium hydroxide, or U-phase) peak
and primary ettringite peak intensities and then determining
where the ratio varies. Quantitative analysis of the hydration
products was performed by determining the heights of the pri-
mary diffraction peaks for each crystalline phase. The primary
diffraction peak for each hydrated phase is listed in Table I.

III. Results
Figures 1(a) and (b) show the rates of reaction and heat
output for reaction between monosulfate and gypsum hydrated
in deionized water between 30° and 80°C. In general, the rate
of hydration is observed to increase with increasing tempera-
ture in any given solution. The hydration reactions are, at all
temperatures, characterized by a single major peak. The dura-
tion of the peak is less than 1 h for every hydration tempera-
ture. The total heat evolved (Fig. 1(b)) reaches a maximum
value of approximately 140 kJ/(mol of Al2O3) at 70° and 80°C
and is indicative of complete hydration when ettringite is the
final product. The kinetics of reaction are apparent in Fig. 1(b)
and indicate only small differences with hydration temperature.
Specimens hydrated at 30° through 60°C evolve less total heat
than those at 70° and 80°C, evolving approximately 115 kJ/
(mol of Al2O3). Fig. 1. (a) Rates of heat evolved when monosulfate and gypsum are
Figures 2(a) and (b) also show rates of reaction and heat hydrated in deionized water. (b) Total heats evolved when monosulfate
output curves for specimens hydrated in 0.2M NaOH solutions and gypsum are hydrated in deionized water.
between 30° and 80°C. The rate curves (Fig. 2(a)) are again
characterized by single peaks which reach maxima before 1 h
for hydration temperatures greater than 50°C and at approxi- kJ/(mol of Al2O3) for samples hydrated between 30° and 60°C,
mately 2.5 h for hydration at 30° and 40°C. The reaction rates while 140 and 150 kJ/mol are evolved for samples hydrated at
are observed to increase as the temperature is increased. The 80° and 70°C, respectively.
total heat evolved reaches a maximum value of approximately Reaction rate curves for monosulfate and gypsum hydrated
120 kJ/(mol of Al2O3) for hydration at 80°C; these values are in 1.0M NaOH are very similar to those hydrated in 0.5M
approximately 110, 95, and 85 kJ/(mol of Al2O3) for hydration NaOH, shown in Fig. 4(a). The rate curves all show distinct
at 70°, 50°, and 60°, and 40° and 30°C, respectively. endothermic reactions, except for the sample hydrated at 80°C.
The rate curves shown in Fig. 3(a) for specimens hydrated in As with hydration in 0.5M NaOH solution, the rate curves are
0.5M NaOH are more complex than those observed for the very diffuse without apparent, distinct hydration peaks. The
deionized water and 0.2M solutions. There is still a single total heat evolved, shown in Fig. 4(b), reaches a maximum of
major peak observed for each specimen, but the peaks are not approximately 100 kJ/(mol of Al2O3) when hydration is carried
as distinct as those observed in less concentrated solutions. A out at 70°C.
distinct endothermic reaction is observed in specimens hy- Samples hydrated in deionized water generated approxi-
drated at 30°, 40°, and 50°C. The results of integrating the rate mately the same amounts of heat between 30° and 60°C, while
curves in Fig. 3(a) are shown in Fig. 3(b). The reaction rates more heat was liberated from samples hydrated at 70° and
are, as in the 0.2M solution, observed to increase with increas- 80°C. Because all of the experiments in deionized water were
ing temperature. The total heat evolved is approximately 80 carried out using approximately 1 g of mixed precursor, these

Table I. Primary Diffraction Peak Listing

Hydrated Angular Position hkl Crystal JCPDS
phase position 2␪ d-spacing indices structure Ref.
Monosulfate 9.93 8.90 003 Hexagonal 18–275
Ettringite 9.08 9.72 100 Hexagonal 41–1451
Calcium hydroxide 34.08 2.63 101 Hexagonal 4–733
U-Phase 17.67 5.01 006 Hexagonal 44–272
Gypsum 11.58 7.63 020 Monoclinic 33–311
2902 Journal of the American Ceramic Society—Clark and Brown
Fig. 2. (a) Rates of heat evolved when monosulfate and gypsum are
hydrated in 0.2M NaOH. (b) Total heats evolved when monosulfate
and gypsum are hydrated in 0.2M NaOH.
results indicate the extent of hydration to be affected by a
change in ettringite morphology and/or an unidentified change
in the hydration reaction.
The total heat evolved varies as a function of temperature for
hydration in a given sodium hydroxide concentration; in gen-
eral the introduction of higher sodium hydroxide concentra-
tions causes the rate of the reaction to be retarded and the total
heat evolved to be reduced.
Analyses of the XRD patterns shown in Figs. 5, 6, 7, and 8
indicate that ettringite, gypsum (CaSO4⭈2H2O), calcium hy-
droxide (Ca(OH)2), and a sodium calcium aluminum sulfate
hydrate phase (3CaO⭈Al2O3⭈CaSO4⭈0.5Na2SO4⭈15H2O, desig-
nated “U-phase”) are the crystalline phases observed. The
amounts of these phases vary with hydration temperature and
hydration solution. No residual monosulfate was observed in
any of the samples.
In general, in each sodium hydroxide concentration, the
amount of ettringite is observed (by XRD) to increase with
increasing temperature. However, the extent to which increased
ettringite formation is observed decreases as the concentration
of sodium hydroxide is increased. Ettringite and gypsum are
the only crystalline phases observed, over the entire tempera-
ture range, in samples hydrated in deionized water, and 0.2M
and 0.5M sodium hydroxide solutions. Ettringite, the U-phase,
and calcium hydroxide are observed, over the entire tempera-
ture range, in samples hydrated in 1.0M sodium hydroxide. The
primary U-phase XRD peak is also observed to increase with
temperature and substantially at 80°C, in the 1.0M solution.
Vol. 82, No. 10
Fig. 3. (a) Rates of heat evolved when monosulfate and gypsum are
hydrated in 0.5M NaOH. (b) Total heats evolved when monosulfate
and gypsum are hydrated in 0.5M NaOH.
The primary calcium hydroxide peak also increases with tem-
perature above 40°C, in the 1.0M solution. Small XRD peaks
observed in samples hydrated at 50°, 60°, and 70°C are also
attributable to calcium hydroxide, but their intensities are only
slightly above those observed in samples hydrated in 0.2M
sodium hydroxide.
Again, in general, the amount of gypsum detected by XRD
decreases as the sodium hydroxide solution concentration in-
creases. Gypsum detected in the XRD patterns is due to an
excess of gypsum present in the precursor mix. As the sodium
hydroxide concentration and temperature increase, more of
gypsum is observed to go into solution. In the 0.2M solution
gypsum is observed to substantially decrease in samples hy-
drated between 60° and 80°C (indicating a reaction occurring
at approximately 50°C). In the 0.5M solution gypsum is ob-
served in samples hydrated at 40° and 50°C, but is not present
in samples hydrated between 60° and 80°C (again indicating a
reaction is occurring at 40° to 50°C). Small amounts of gypsum
are observed in the sample hydrated in 1.0M sodium hydroxide,
and at 30°C, none of the other samples hydrated in 1.0M so-
lution show any indication of gypsum.
The conditions under which gypsum was not completely
consumed or where Ca(OH)2 precipitated were calculated us-
ing the aqueous geochemical code PhreeqC.16 These calcula-
tions were carried out as a function of temperature (30°, 50°, or
70°C) and NaOH concentration (H2O, 0.2M NaOH, and 1.0M
NaOH). Table II summarizes the output from the calculation
reporting the pH, the saturation indices for calcium hydroxide
October 1999 Formation of Ettringite from Monosubstituted Calcium Sulfoaluminate Hydrate and Gypsum
Fig. 4. (a) Rates of heat evolved when monosulfate and gypsum are
hydrated in 1.0M NaOH. (b) Total heats evolved when monosulfate
and gypsum are hydrated in 1.0M NaOH.
Fig. 5. XRD patterns obtained when monosulfate and gypsum are
hydrated in deionized water at various temperatures.
(CH) and gypsum (a value of zero indicates saturation), and the
moles of solid (gypsum or CH). These calculated results are
consistent with the XRD analyses.
IV. Discussion
The first observation to be discerned from a review of the
data concerns the amount of gypsum dissolved into each solu-
2903
Fig. 6. XRD patterns obtained when monosulfate and gypsum are
hydrated in 0.2M NaOH at various temperatures.
Fig. 7. XRD patterns obtained when monosulfate and gypsum are
hydrated in 0.5M NaOH at various temperatures.
Fig. 8. XRD patterns obtained when monosulfate and gypsum are
hydrated in 1.0M NaOH at various temperatures.
tion. Increasing the sodium hydroxide concentration increases
the extent of gypsum dissolution via the double decomposition
reaction:
CaSO4⭈2H2O(s) + NaOH(aq) ⳱ Ca(OH)2(s) + Na2SO4(aq)
Thus sodium hydroxide promotes gypsum dissolution and the
formation of calcium hydroxide. Our studies have shown the
2904 Journal of the American Ceramic Society—Clark and Brown Vol. 82, No. 10

Table II. PhreeqC Output Summary

Saturation index Amount in solid (mol)
Solution Temp (°C) pH CH† Gypsum Gypsum CH†
DI H2O 30 7.0 −10.7 0.0 0.064 0.000
50 6.8 −9.8 0.0 0.064 0.000
70 6.6 −9.0 0.0 0.065 0.000
0.2M NaOH 30 12.6 0.0 0.0 0.006 0.061
50 11.9 0.0 0.0 0.000 0.069
70 11.4 0.0 −0.1 0.000 0.072
1.0M NaOH 30 13.7 0.0 −2.4 0.000 0.080
50 13.1 0.0 −2.7 0.000 0.080
70 12.6 0.0 −2.9 0.000 0.080
†
Calcium hydroxide.

dissolution of gypsum in 1.0M sodium hydroxide to be endo-

thermic. The dissolution of gypsum influences both the to-
tal heat evolved and the rate of the reaction. This is why the
total heat output is observed to decrease with increasing
sodium hydroxide concentrations and why samples hydrated
in 1.0M NaOH solution undergo a reaction which is initially
endothermic.
The XRD and calorimetry data indicate the monosulfate/
gypsum mixture converts to ettringite at all temperatures in
deionized water or in solutions with low concentrations of
sodium hydroxide. This conversion indicates ettringite is the
stable phase over this temperature range. The similarity of the
hydration rates of all samples in deionized water, regardless of
temperature, is consistent with prior work indicating a diffu-
sion-controlled process.17
While the hydration rates of all samples in deionized water
are similar, the total heats evolved are slightly different. These
differences may be due to morphological and/or crystallinity
differences in the final products. Similar small discrepancies
between the total heats of samples hydrated in NaOH solutions Fig. 9. Plot showing apparent activation energy for monosulfate hy-
are also observed. The maximum total heat occurs at 70° or dration to ettringite at various NaOH concentrations.
80°C, evolving 20 to 80 kJ/(mol of Al2O3) more than at lower
temperatures.
The presence of sodium hydroxide retards the monosulfate/
gypsum to ettringite conversion and lowers the total heat out- each of the hydration solutions. The plot shows that the reac-
put. For samples hydrated in sodium hydroxide solutions, the tion rates are in general nonlinear over the entire temperature
hydration rates show a dependence on temperature and sodium range; at higher temperatures (70° and 80°C) the reaction rates
hydroxide concentration. This suggests that the hydration pro- decrease significantly in deionized water, and in 0.2M NaOH
cess is not solely diffusionally controlled, but may also be and 0.5M NaOH solutions. The plot also shows that sodium
controlled by an interfacial process. hydroxide significantly decreases the rate of reaction, although
Small U-phase diffraction peaks are observed in the XRD the apparent activation energy, the slope of the linear region
patterns for the samples hydrated in 0.5M NaOH. The calorim- along each curve, increases with low concentrations of sodium
etry data also provides indications (reduced heat output, irregu- hydroxide. To determine the apparent activation energy, the
larly shaped rate curves) of a second reaction taking place. slope was taken of each curve from 30° to 60°C in Fig. 7; the
When monosulfate is hydrated in 1.0M sodium hydroxide, both apparent activation energies vary as shown in Table III.
calcium hydroxide and the U-phase form; these results are in The apparent activation energies reflect the various phase
agreement with recent studies by Li, Bescop, and Moranville- changes produced during hydration of the monosulfate/gypsum
Regourd.18 U-phase formation, in 1.0M sodium hydroxide, is mixture: the dissolution of gypsum and formation of ettringite,
consistent with the double decomposition reaction calcium hydroxide, and U-phase. In deionized water only et-
tringite is produced and residual gypsum remains. In 0.2M and
CaSO4⭈2H2O(s) + NaOH(aq) ⳱ Ca(OH)2(s) + Na2SO4(aq) 0.5M NaOH solutions ettringite is produced, but the apparent
As gypsum dissolves in NaOH solution, both the calcium and activation energy increase indicates the effect of these solutions
sulfate ion concentrations increase and calcium hydroxide pre- on ettringite formation. The slight decrease in the activation
cipitates. The formation of calcium hydroxide therefore com- energy between the 0.2M and 0.5M solutions indicates the
petes with ettringite formation. Thus the amount of calcium
hydroxide formed limits ettringite formation and allows for the
formation of other phases. The U-phase is formed due to the
depletion of calcium from solution due to the common ion Table III. Apparent Activation Energies
effect. Thus calcium is replaced in the AFm structure by so- Apparent
dium or more accurately the calcium sulfate in the structure is activation energy Hydration phases
Hydration solution (kJ/(mol of Al2O3)) observed by XRD
replaced by sodium sulfate.
To establish whether the hydration reactions fit an Arrhenius Deionized water 12.7 AFt
model (k ⳱ exp−(Ea /RT ) ), the apparent activation energy for 0.2M NaOH 68.0 AFt
each hydration reaction was calculated. Figure 9 plots the loga- 0.5M NaOH 56.5 AFt, little CH
1.0M NaOH 25.2 AFt, CH, U-phase
rithm of the reaction rate versus the inverse temperature for
October 1999 Formation of Ettringite from Monosubstituted Calcium Sulfoaluminate Hydrate and Gypsum
formation of calcium hydroxide. Ettringite, calcium hydroxide,
and U-phase are all produced in the 1.0M NaOH solution; the
apparent activation energy is lower due to the formation of the
two additional phases.
Examination of the heat evolution curves and the Arrhenius
plot suggests the rate-controlling mechanism for each reaction.
For samples hydrated in deionized water hydration reaction
rates show little change with temperature, indicating a diffu-
sion-controlled process. For samples hydrated in 0.2M and
0.5M NaOH solutions the rates show substantial changes with
temperature, indicating an interfacially controlled process. For
samples hydrated in 1.0M NaOH solution the reaction rates are
again greatly influenced by temperature, but the analysis is
complicated by calcium hydroxide and U-phase formation.
The reaction kinetics can also be evaluated from the above
data. Between 20° and 70°C samples hydrated in deionized
water and 1.0M NaOH are consistent with an Arrhenius model;
this indicates a first-order reaction. For samples hydrated in
0.2M and 0.5M NaOH the Arrhenius plot (Fig. 9) is nonlinear,
indicating the reactions are now dependent on more than one
parameter due to competing reactions of ettringite and U-phase
formation.
V. Conclusions
The results presented indicate that ettringite is the stable
phase, in the reactions examined, over a wide temperature
range. Complete hydration produces 140 kJ/(mol of Al2O3) of
heat output when ettringite is the only crystalline product. Hy-
dration of the monosulfate/gypsum mixture in increasingly
concentrated sodium hydroxide solutions was observed to re-
tard ettringite formation. Competitive reactions of U-phase and
calcium hydroxide formation occur as the sodium concentra-
tion is increased, decreasing the total heat output and the total
amount of ettringite produced. The consequences of these ob-
servations could be the formation of U-phase, which can be
expansive, in a portland cement or the delayed formation of
ettringite, both of which could lead to crack formation in a
hardened concrete structure.
2905
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