Figure 2 Doughlike cementitious paste (Sample No.

4) for extrusion

Extrudability of Cement-Based Materials

A penetration resistance test was used to assess the extrudability
of cementitious materials.

Y. Chen, L. J. Struble and G. H. Paulino

Dept. of Civil and Environmental Engineering, University of Illinois at Urbana-Champaign,
Urbana, Ill.

xtrusion is a process in which a stiff paste is forced to pass through a rigid

E die with high shear, which produces a fluid behavior. A ram extruder is
used in this process (Fig. 1). Extrusion has been successfully applied in pro-
duction of various cement-based products, e.g., pressure pipe,1 plate2 and
fiberboard.3 Extrusion can be used to manufacture complicated shapes,4
and it can improve the performance properties of products, such as toughness, tensile
strength and flexural strength.5,6

Extrusion of cementitious pastes requires controlling the rheology to obtain good-quality

products. Peled et al.7 have measured the applied pressure on pastes during extrusion to
compare the effect of fiber types and fly-ash addition on rheological properties. Srinivasan
et al.8 and Shen9 have applied the physically based paste-flow model developed by
Benbow and his colleagues10,11 to characterize the rheology of cementitious paste.

Li and his colleagues12,13 have studied the rheological behavior of cementitious paste
based on a nonlinear viscoelastic constitutive relationship. These techniques are time
consuming and probably more useful in academic settings. Benbow and Bridgewater14
have provided a rapid approach to measure the yield value of pastes that contain low-
viscosity liquids.

©The American Ceramic Society American Ceramic Society Bulletin www.ceramicbulletin.org June 2006 9101
 None of the methods mentioned deals with the problem of opera-
Piston tional time for extrusion. The cementitious paste begins to hydrate
upon contact with water and thereafter stiffens gradually and progres-
sively. Thus, time is a critical issue during extrusion of cement-based
materials. Paste preparation for extrusion may involve mixing, feedrod
Barrel stacking and deairing. Longer time is needed during slow-speed extru-
sion. Therefore, it often is necessary to know the allowable operational
Paste time for extrusion of cementitious pastes.

We provide a method to measure the extrusion time window using

penetration resistance (PR). PR is used to measure the setting time of
concrete in the ASTM Standard C 403.15 PR has been related to the rhe-
ological parameters of a cementitious paste.16 The penetration test has
Die been used to determine the extrudability of cementitious pastes short-
ly after mixing with water.

Materials and Test Methods

Figure 1 Schematic diagram of ram extruder
A Type I portland cement (Essroc Cement Corp.) was used. Methyl hydrox-
yethyl cellulose (MHEC; Culminal® 40,000 PF, Hercules Inc.) was used to
produce extrudable pastes.The dosage of MHEC was 1% by mass, based
on cement for all pastes. Specific paste proportions were selected (Table 1). Below a water to
cement ratio (w/c) of 0.17, the paste was dry and could not be consolidated in the container for
measuring PR. Actually, the paste with w/c = 0.16 was too dry to be extruded using the extrusion
system. At w/c > 0.29, the paste was too wet to retain its shape after extrusion.

For each paste, cement and MHEC were dry mixed for 3 min using a planetary mixer (Model N-
50, Hobart Corp.) at low speed. Water then was added, and the mixture was further mixed at
low speed until a doughlike paste was formed (Fig. 2).

The PR test was performed at room temperature following the procedure of Standard C 403.15
The paste was consolidated into a rectangular container. A series of needles then was used to
penetrate the paste. A smaller needle was used as the PR increased. A vertical force was applied
downward by a screw-driven testing machine (Model 4500, Instron Corp.) with a load cell of 1
kN at a rate of 2.5 mm/s until the needle penetrated the paste to a depth of 25 mm. The maxi-
mum force at each penetration was recorded against hydration time. Each data point was the
average of four penetrations. The coefficient of variation was generally <10%. The PR was calcu-
lated by dividing the average force by the bearing area of the needle.

Test Results
The PR was plotted against hydration time (t) for various pastes (Fig. 3). Data were fitted to
power-law expressions determined by regression analysis for each paste (Table 2). The correla-
tion coefficient values (R2) of the power-law expressions were >0.94. Such high correlations
indicated good fits.

An upper limit for PR corresponding to our current extrusion setup (Model 323-40T, Loomis
Products Co.) was ~2000 kPa; above this limit, the paste was too dry to be extruded. The lower
limit of PR was 10 kPa; below this limit, the paste was too wet to retain its shape after extru-
sion for rod extrudates. A paste shortly after mixing with water in this experiment was extrud-
able in the range 10–2000 kPa.

In Standard C 403,15 the initial setting time of concrete is the time when PR = 3.5 MPa. The
upper limit set in this study was >>3.5 MPa, which indicated the initial setting of the pastes was
not reached when doing extrusion.

©The American Ceramic Society American Ceramic Society Bulletin www.ceramicbulletin.org June 2006 9102
 Using these results, the time window in which the paste is extrudable can readily be deter-
mined. The extrusion time window of the w/c = 0.18 paste is 0–561 min from the regression
expression (Table 2). The higher the w/c, the wider is the time window. However, in general, the
regression expressions are applicable only in their tested ranges. Beyond these tested ranges,
the cement may hydrate in a different manner, such that PR vs t curves may be different.

Not every paste in this study was tested until the PR limit was reached. Pastes with w/c >0.20
were not tested, because other time windows were wide.

The PR at any hydration time can be predicted from regression. However, the PR at time zero
cannot be estimated using these regression models. There is no practical significance, because
extrusion cannot begin immediately after water is added to cementitious powders. For a simple
single extrusion, the time for paste preparation after water addition is generally ≥10 min. The
time for three-layer feedrod coextrusion generally is ≥40 min using one mixer.

If we plot the PR against w/c at a given hydration time, some other useful information can be
obtained (Fig. 4). PRs at 20, 40 and 80 min hydration times have been presented as a function
of w/c. The PR of the tested pastes at any hydration time within the tested time range can be
predicted by regression (Fig. 3). Therefore, the PR value for any w/c at a given hydration time can
be obtained using regression (Fig. 4).

At 40 min hydration, the regression expression for PR vs w/c is PR = 1.18
10–5(w/c)–10.513. For
w/c = 0.21, PR = 157.5 kPa, which is in the extrudable range. The plots have been extended to
w/c = 0.16 and w/c = 0.31 (although not accurate, because w/c = 0.16 and w/c = 0.31 are out of
the tested range) to show that even the paste with w/c = 0.16 is too stiff to be extruded at 20
min hydration and that the paste with w/c = 0.31 is too wet to be extruded, even after 80 min
hydration.

The limits of PR are deter-

mined by the extrusion sys-
tem. The upper and lower lim-
its of the resistance value
depend on the cross section of
the die. The die shape deter-
mines the extrudability of a
paste. An extrudable paste in a
circular die might be unex-
trudable in a honeycomb die.
The upper limit of the PR value
PR (kPa)

also strongly depends on the

maximum pressure the extrud-
er can apply. If the extruder
can apply higher pressure, the
upper limit of the resistance
value is greater. However, as
cement hydration continues,
the paste becomes stiffer.
Although the paste may still
be extrudable, the mechanical
properties of the paste may be
adversely affected. The extrud-
ability may be determined by t (min)
trial and error for the specific Figure 3 Penetration resistance (PR) vs hydration time (t) for various pastes.
extruder and die.

©The American Ceramic Society American Ceramic Society Bulletin www.ceramicbulletin.org June 2006 9103
 The PR values may be related to rheological param- Table 1 Paste Proportions
eters, for example, yield stress. Benbow and
Bridgewater14 measured the penetration depth using Sample No. Cement (g) MHEC (g) Water (g) w/c
a cone, and they experimentally related the cone 1 100 1 17 0.17
penetration to the yield value in the paste flow 2 100 1 18 0.18
model developed by Benbow and his colleagues. 10,11 3 100 1 20 0.20
16 4 100 1 22 0.22
Struble et al. have reported that the PR values agree 5 100 1 25 0.25
well with the storage moduli of various cement 6 100 1 29 0.29
pastes. It is expected that a relationship can be
derived between the penetration resistance and yield
stress at any hydration time. ■ Table 2 Power-Law Expressions
Correlation coefficient
Sample No. w/c Regression expressions values (R2)
Acknowledgments
This material is based upon work supported by NSF under 1 0.17 PR = 367.71t 0.401 0.98
Award No. 0333576. Any opinions, findings, and conclusions 2 0.18 PR = 104.02t 0.467 0.97
or recommendations expressed in this publication are 3 0.20 PR = 60.85t 0.406 0.99
those of the authors and do not necessarily reflect the 4 0.22 PR = 40.47t 0.359 1.00
views of NSF. The authors also gratefully thank the Hercules 5 0.25 PR = 10.00t 0.179 0.94
Cooperated for providing the MHEC.
6 0.29 PR = 4.84t 0.267 0.96

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©The American Ceramic Society American Ceramic Society Bulletin www.ceramicbulletin.org June 2006 9104
PR (kPa)

w/c

Figure 4 PR vs w/c for various hydration times. Correlation coefficients for the three times (20, 40 and
80 min) are R2 = 0.97.