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 Mechanical Properties of New Dental Pulp Capping Materials
Capt Matthew J. Nielsen

ABSTRACT

The mechanical properties of new pulp capping materials may affect their

resistance to fracture under load either during placement of a final restorative material

or while supporting an overlying restoration over time. Objective: The purpose of this

study was to evaluate the flexural strength/modulus and compressive strength of two

new pulp capping materials (TheraCal LC, Bisco; Biodentine, Septodont) compared to

mineral trioxide aggregate (ProRoot MTA, Dentsply), and calcium hydroxide (Dycal,

Dentsply) over time. Method: Ten specimens per group were formed as per

manufacturers’ directions in a 2x2x25mm split mold for flexural strength/modulus testing

and in a 6mm long x 4mm diameter split mold for compressive strength testing.

Specimens were stored in darkness at 37°C and 98% humidity in a lab oven. After 15

minutes, 3 hours, and 24 hours, specimens were tested to failure in a universal testing

machine (Instron). Flexural modulus was determined from the slope of the linear region

of the load-deflection curve. A mean and standard deviation was determined per group.

Data were analyzed with multiple ANOVA/Tukey’s test (alpha=0.007). Result: A

significant difference was found between groups based on material or time (p<0.007).

Conclusion: MTA did not set at 15 minutes. At all time periods, TheraCal LC had the

greatest flexural and compressive strength. After 3 and 24 hours, Biodentine had the

greatest flexural modulus. Discussion: TheraCal LC had greater early strength to

potentially resist fracture during immediate placement of a final restorative material.

1
However, Biodentine was the least flexible after three hours for potentially greater

support of an overlying restoration under function over time.

INTRODUCTION

A dental pulp can become exposed in two distict ways during a preparation for a

restoration. A mechanical pulp exposure occurs when a rotating bur inadvertently

comes in contact with the dental pulp. A carious pulp exposure occurs when the pulp is

exposed with the removal of carious tooth structure. A direct pulp cap is a procedure in

which a medicament is placed directly over the exposed dental pulp, with the specific

aim of maintaining pulp vitality and health (Camp and Fuks, 2006; Hilton, 2009; Hilton

2013; Mente et al., 2010). At times, the provider might decide to leave residual affected

dentin to avoid a pulp exposure. It is common to place a pulp capping material over the

affected dentin. This type of pulp cap is known as an indirect pulp cap (Al-Zayer et

al.,2003). Ideally, the pulp capping material will promote pulpal healing and formation of

tertiary dentin while providing protection from further insult by bacteria or mechanical

forces (Thompson et al., 2008; Graham et al., 2006). Several pulp capping materials

are currently available for use in direct and indirect pulp capping situations that meet

these two criteria. Another desirable property for this type of material would be ease of

use by the practitioner. Calcium hydroxide and Mineral Trioxide Aggregate (MTA) have

been used for pulp capping and have a successful clinical history (Hilton, 2009).

According to the manufacturers, newer products like Biodentine (Septodont, Lancaster,

PA) and TheraCal (Bisco, Schaumburg, IL) have much more desirable handling

characteristics, however the research is limited.

2
 Calcium hydroxide is considered the “gold standard” in direct pulp capping

materials and has been used in dentistry since 1921 (Hilton, 2009). Calcium hydroxide

has antibacterial properties and promotes the formation of new tertiary dentin (Stuart et

at., 1991; Ribeiro et al., 2006). The antibacterial effects of calcium hydroxide has been

attributed to a high pH - approximately 12.5-12.8 (Mohammadi and Dummer, 2011).

Calcium hydroxide has been shown to free Bone Morphogenic Proteins (BMPs) and

Transforming Growth Factor-Beta One (TGF-β1) from surrounding dentin. It is believed

that these growth factors promote the formation of new dentin in the adjacent pulp

chamber (Graham et al., 2006). Two undesirable properties of calcium hydroxide are its

high water solubility and poor seal formation due to a lack of inherent adhesive qualities

(Hilton, 2009). It also has low compressive strength, potentially providing an inadequate

foundation under restorative materials (Mohammadi and Dummer, 2011).

MTA was first used as a retrograde filling material in the early 1990’s and has

since been used in many situations where its biocompatible properties are

advantageous (Okiji and Yoshiba, 2009). MTA is a type I Portland cement with bismuth

oxide added in a 4:1 ratio (Camilleri, 2008). MTA forms reaction products in the

presence of water with the primary product being calcium hydroxide (Camilleri, 2008;

Hilton, 2009). MTA has the ability to induce new dentin formation and stimulate more

reparative dentin than calcium hydroxide (Witherspoon, 2008). MTA also has the ability

to provide a seal to tooth structure, allowing it to better protect the pulp from further

bacterial insult (Ferk Luketic et al., 2008). However, MTA also has some significant

3
disadvantages - it is water soluble, has a setting time of 2 to 3 hours (Islam et al., 2006),

and has a cost approximately 24 times that of calcium hydroxide (Hilton, 2009).

Biodentine is a tricalcium silicate material (Ca 3SiO5). Tricalcium silicate is one of

the components of MTA. It releases calcium hydroxide like MTA, but has a much faster

setting time (approximately 10 minutes). Biodentine is described as a dentin substitute

with the ability to be used as a provisional restoration for up to 6 months (Raskin et al.,

2012). The provisional restoration can be prepared and left in place as a base, sealing

off the direct or indirect pulp exposure (Koubi et al., 2013). The manufacturer suggests

waiting 48 hours before preparing and placing a permanent restoration. Biodentine has

a potential advantage over MTA due to its shorter setting time while reportedly providing

an ability to induce biomineralization (Zanini et al., 2012; Laurent et al., 2012). Also, the

cost of Biodentine is just less than 1/3 of MTA.

TheraCal LC is a new product with very little published information. It is a new

light-curable resin formulation which contains mineral oxides and is marketed for direct

and indirect pulp capping. It is composed of a mineral material (type III Portland

cement), a radiopaque component (barium sulphate), a hydrophilic thickening agent

(fumed silica) and resin (Bis-GMA and PEGDMA) (Suh et al., 2008). According to

Gandolfi and others (2012), TheraCal LC releases more calcium hydroxide and has a

lower solubility than either ProRoot MTA (Dentsply, Milford, DE), or Dycal (Dentsply).

Because it can be light cured up to a depth of 1.7mm, there is no waiting for it to

polymerize prior to placement of the permanent restoration (Gandolfi et al., 2012).

Presumably this will make it a more convenient pulp capping material because it will

have immediate strength for placement of a final restoration.

4
 The flexural and compressive strength of pulp capping materials is an important

property when considering the forces that are applied during the placement and function

of a restorative material. Studies describing the compressive strength of MTA have

been published and found that its properties are time dependent. (Islam et al., 2006;

Camilleri, 2010). The manufacturer has shown the compressive strength of Biodentine

to be greater than that of MTA and flexural strength that is less than composite.

Because of their recent introduction into the market, the physical properties of

Biodentine and TheraCal have been studied by the manufacturers but not

independently. There are no studies simultaneously comparing the strength properties

of all four of these pulp capping materials. The purpose of this study was to compare

the mechanical properties of two new pulp capping materials with other commonly used

pulp capping materials. The null hypothesis tested was that there would be no

significant difference in compressive strength, flexural strength, or flexural modulus

based on 1) material or 2) time.

METHODS AND MATERIALS

This study involved the testing of TheraCal LC (Bisco), Biodentine (Septodont),

ProRoot MTA (Dentsply), and Dycal (Dentsply). Specimens from each the four different

types of pulp capping materials were evaluated using compressive strength and flexural

strength/modulus testing after 15 minutes, 3 hours, and 24 hours.

Compressive Strength

5
 To prepare each specimen, an aluminum mold (Sabri, Downers Grove, IL), 6mm

long and 4mm in diameter was placed on a plastic-strip-covered glass slide. Dycal and

ProRoot MTA were mixed according to the manufacturer’s directions and then

spatulated into the mold. Biodentine was triturated, placed into the mold with an

amalgam carrier, and condensed with amalgam condensers according to the

manufacturer’s instructions. TheraCal LC was injected from the syringe using an

applicator tip provided by the manufacturer. The top surface of the mold was covered

with a second plastic strip and glass slide to ensure that the end of the specimen was

flat and parallel to the opposite surface of the mold. For Dycal, ProRoot MTA, and

Biodentine, the material was allowed to chemically set. For TheraCal LC, six, 1mm

increments were exposed to a visible-light polymerization unit (Bluephase G2, Ivoclar

Vivadent, Amherst, NY) for 20 seconds. The specimens were then removed from the

mold and the longitudinal ends were polymerized for 20 seconds each. The adequacy

of the irradiant output from the light was evaluated using a radiometer (Bluephase

Meter, Ivoclar Vivadent) and considered acceptable when greater than 1000mW/cm2.

The specimens were stored in darkness at 37°C and 98% humidity in a lab oven (Model

20GC, Quincy Labs, Chicago, IL). After 15 minutes, 3 hours, and 24 hours, ten

specimens from every material and time interval were tested by placement on the

platens of a universal testing machine (Model 5943, Instron, Canton, MA) with exception

of the 15 minute ProRoot MTA sample which did not set in 15 minutes. The specimens

were loaded to failure in compression at a crosshead speed of 1.0mm/min. The

4F
compressive strength was determined from the equation 
=
CS
d 2 where F is the

perpendicular loading force and d is the diameter (4mm) of the cylindrical rod.

6
Measurements were made using an electronic digital caliper (GA182, Grobet Vigor,

Carlstadt, NJ). The mean and standard deviation were calculated for each of the four

pulp capping materials.

Flexural Strength / Modulus

To prepare each specimen, an aluminum mold (2mm x 2mm x 25mm) (Sabri)

was placed on a plastic strip covered glass slide as before. Thirty rectangular

specimens per each of the four pulp capping materials were made by inserting the

materials into the mold (n=10) as described before. The top surface of the mold was

covered with a second plastic strip. For Dycal, ProRoot MTA, and Biodentine, the

material was allowed to set. For TheraCal LC, one side of the specimen was exposed

to the light-polymerization unit for 20 seconds each in five separate overlapping

increments. Next, the mold was turned, and the opposite side of the specimen was

exposed to the light in a similar manner. Then, the specimens were removed from the

mold and stored as before. After 15 minutes, 3 hours, and 24 hours, ten specimens

from every material and time interval were placed on a three-point bending test device,

which was constructed with a 20mm span length between the supporting rods. The

central load was applied with a head diameter of 2mm using the universal testing

machine at a crosshead speed of 0.25mm/min. The flexural strength was calculated

3Fl
using the equation
 FS
=
2bd 2 where F is the loading force at the fracture point, l is the

length of the support span (20mm), b is the width, and d is the depth of the specimens.

Measurements were made using an electronic digital caliper as before. The mean and

standard deviation was calculated for each of the four pulp capping materials. Flexural

7
modulus was determined from the slope of the linear region of the load-deflection curve

using the analytical software (Instron).

A two-way ANOVA followed by Tukey’s post-hoc pairwise comparison test was

used to determine if significant differences existed between the groups per property

based on pulp capping material (4 levels) and time (3 levels) at the 0.05 level of

significance.

RESULTS

Using the two-way ANOVA, significant differences were found between groups

based on material (p<0.001) and time (p<0.001) per test type, however, there were

significant interactions (p<0.01). The data was further analyzed with multiple one-way

ANOVAs and Tukey’s post hoc tests per property to evaluate the effect of material or

time. A Bonferroni correction was applied because multiple groups were compared

simultaneously (alpha = 0.007). MTA did not set at 15 minutes. A significant difference

was found between groups based on material or time (p<0.007). TheraCal LC had

significantly higher flexural strength and compressive strength compared to the other

pulp capping materials tested in all time periods. TheraCal LC had a significantly higher

flexural modulus at 15 minutes, but Biodentine had significantly higher flexural modulus

at 3 and 24 hours. Dycal, MTA, and Biodentine had a significant increase in properties

over time. With TheraCal LC, there was no significant difference in properties over

time. See table below.

8
 Flexural Strength MPa (st dev)
Time
Material 15 mins 3 hrs 24 hrs
Dycal 2.7 (0.5) Bb 4.9 (1.3) Ab 6.3 (1.7) Ac
MTA Did not set 1.1 (0.6) Bb 4.8 (3.5) Ac
Biodentine 0.6 (0.5) Bb 9.4 (5.0) Ab 13.4 (5.2) Ab
TheraCal LC 31.1 (9.2) Aa 41.2 (10.1) Aa 33.3 (6.5) Aa
Groups with the same upper case letter per row or lower case letter per column are
not significantly different (p>0.007).

Flexural Modulus GPa (st dev)

Time
Material 15 mins 3 hrs 24 hrs
Dycal 0.7 (0.3) Cb 2.2 (0.4) Bb 3.5 (1.1) Ab
MTA Did not set 1.7 (1.4) Bb 6.6 (3.3) Ab
Biodentine 0.6 (0.8) Cb 9.3 (4.1) Ba 24.1 (5.5) Aa
TheraCal LC 1.9 (0.7) Aa 1.8 (0.6) Ab 2.0 (0.6) Ab
Groups with the same upper case letter per row or lower case letter per column are
not significantly different (p>0.007).

Compressive Strength MPa (st dev)

Time
Material 15 mins 3 hrs 24 hrs
Dycal 7.7 (2.1) Bb 16.3 (5.0) Abc 20.4 (5.8) Abc
MTA Did not set 0.5 (0.2) Bc 5.9 (2.2) Ac
Biodentine 1.3 (0.5) Bb 33.9 (13.1) Ab 40.1 (10.1) Ab
TheraCal LC 87.7 (18.8) Aa 95.8 (20.9) Aa 102.8 (26.9) Aa
Groups with the same upper case letter per row or lower case letter per column are
not significantly different (p>0.007).

DISCUSSION

The null hypothesis was rejected. Significant differences were found between

the different materials in all time periods. In this study, the materials were tested at 15

minutes, 3 hours, and 24 hours. A 15 minute time period was chosen to evaluate the

ability of these materials to be placed as a direct or indirect pulp cap during a restorative

procedure and then immediately have a permanent restorative material placed over it.

The 3 hour time period was selected because it is near the minimal time MTA requires

9
to set according several studies (Torabinejad et al., 1995, Islam et al., 2006). The 24

hour time period was chosen to represent a setting time that is near the maximum for all

of the materials.

The physical properties that would enable the materials to be used as a base or

liner under a permanent restoration were evaluated. The ideal pulp capping material

would have a flexural modulus (17.5 GPa) and compressive strength (300 MPa) similar

to dentin (Plotino et al., 2007; Craig and Peyton, 1958), or the permanent restoration

that would be placed over it and set quickly enough that the final restoration could be

placed immediately.

At the 15 minute interval, TheraCal LC had a compressive strength that was

more than 10x that of Dycal and Biodentine, MTA did not set. At 3 hours, the

compressive strength of TheraCal LC was nearly 3x that of Biodentine, and 6x that of

Dycal and over 100x that of MTA. At 24 hours the compressive strength of TheraCal

LC was 2.5x that of Biodentine, 5x that of Dycal, and 17x that of MTA.

Ca(OH)2 has been considered the gold standard of pulp capping materials

(Baume and Holz, 1981). Unlike MTA-based materials, Ca(OH)2 induces tertiary dentin

through a process that leads to an area of necrosis between the Ca(OH)2 and the newly

formed reparative dentin (Sangwan et al., 2013). Dycal is an example of a popular

product that contains Ca(OH)2. It is a self-cure formulation that has the disadvantage of

being very soluble (Prosser et al., 1982). It is possible to place a restorative material

immediately over Dycal, but there may be residual voids after it the material resorbs, (de

Lourdes et al., 2006) leaving an undesirable foundation for the restoration.

10
 MTA is marketed for multiple applications including pulp capping, pulpotomy,

apical barrier formation in teeth with open apices, repair of root perforations, and root

canal filling (Parirokh and Torabinejad, 2010). MTA has been shown clinically to induce

the formation of tertiary dentin (Tziafas et al., 2002). Compared to Ca(OH)2, MTA

induces a dentin bridge that forms faster and is more complete with greater structural

integrity (Faraco and Holland, 2001). MTA causes less inflammation, hyperemia, and

necrosis than Ca(OH)2, indicating its greater biocompatibility (Aeinehchi et al., 2003).

The setting time and the potential occurrence of tooth discoloration (Felman and

Parashos, 2013) along with its handling characteristics are less than ideal.

Biodentine is advertised to be used as a pulp capping material that is placed as a

liner, or in bulk, and then subsequently reduced in volume. The manufacturer reports

the working time of Biodentine is 6 minutes with a final setting time of 10-12 minutes

(Septodont, 2009). In this study, after setting for 15 minutes, Biodentine achieved only

3.8% of its 3 hour compressive strength (33.9 MPa) and 6.5% of its 3 hour flexural

strength (9.3 GPa). According to the manufacturer, a composite restoration can be

placed over Biodentine after setting for 12 minutes (Septodont, 2009). The setting

reaction continues for two weeks after the initial set (Pradelle-Plasse et al., 2009). The

findings in this study bring into question the ability of Biodentine to support an

immediate restoration. When mixing Biodentine, a triturator is used for 30 seconds until

a consistency similar to that of zinc-phosphate cement is achieved

(www.septodont.com). The consistency of Biodentine is highly dependent on the

amount of liquid accelerator added to the powder component and amount of trituration.

11
 When considering their ability to have a final restoration placed immediately over

them, the ability of TheraCal LC to be light cured gives it a significant advantage when

compared to the other pulp-capping. TheraCal LC exhibits a command cure similar to

other light-cured resin-based materials, and achieves a high initial strength, allowing the

practitioner to reduce treatment time. TheraCal LC comes in a multi-use syringe that

enables the practitioner to place the material with relative precision and ease due to its

thixotropic properties. The manufacturer markets the material to be used for direct and

indirect pulp capping or as a protective liner under composites, amalgams, cements,

and other base materials (www.bisco.com). Research has shown that TheraCal LC can

be polymerized to a depth of 1.7mm (Gandolfi et al., 2012) however, the manufacturer

recommends that layers of the material should not exceed 1mm in depth

(www.bisco.com). Specimens used for testing compressive strength in this study were

6mm thick. While fabricating these specimens, uniform 1mm increments were light

cured to prevent layers of uncured material. Due to the minimal depth of cure of

TheraCal LC, it may be more indicated as a liner, and not as an interim restoration, as

in the case of Biodentine.

Based on the mechanical properties, the results of this study demonstrate that

Biodentine and TheraCal LC are ideally suited for their intended use. Both are

marketed for treating pulp exposures, but are used differently. Biodentine is used as a

substitute for dentin, therefore it is important that it has a flexural modulus greater than

or equal to dentin. The flexural modulus of dentin is 17.5 ± 3.8 GPa (Plotino et al.,

2007) and in this study that of Biodentine was found to be 24.1 GPa. Of the materials

tested, Biodentine had the highest flexural modulus at 3 and 24 hours making it the

12
least flexible and potentially providing greater support of an overlying restoration.

Studies suggest that it provides a good marginal seal with a faster setting time

compared to MTA (Bachoo et al., 2013, Septodont, 2009). Biodentine could be placed

in teeth with reversible pulpitis as a sedative restoration. If the pulp becomes

asymptomatic, Biodentine could be prepared with a handpiece, reducing its size, and

allowing a permanent restoration to be placed. TheraCal LC had the greatest early

strength, making it the most resistant to fracture during the immediate placement of a

final restorative material. TheraCal LC is placed in a small increment of less than 1mm

thick over a pulp exposure similar to the placement technique for Dycal.

The ability of the pulp capping materials to induce the formation of tertiary dentin

is a critical characteristic when performing a direct or indirect pulp-cap. A large clinical

trial by Hilton and others showed that MTA had a higher success rate compared to

Ca(OH)2 when used as a direct pulp cap (Hilton et al., 2013) as have other studies

(Aeinehchi et al., 2003; Chacko and Kurikose, 2006; Min et al., 2008; Nair et al., 2008).

Studies comparing the effectiveness of pulp capping materials in clinical situations

involving a carious pulp exposure are lacking in the literature (Mente et al., 2010). The

lack of clinical research is especially true for Biodentine and TheraCal LC. An in vivo

study by Nowicka and others showed that there was no difference between MTA and

Biodentine in inducing dentinal bridging over intentional pulp exposures (Nowicka et al.,

2013). That study had relatively limited number of teeth and only included teeth with

intentional mechanical exposures. TheraCal LC has been shown to induce apatite

formation in an in vitro study (Gandolfi et al., 2011), but significantly limited information

is available on the ability of TheraCal LC to induce tertiary dentin. A study by Lodiene

13
and others found that exposure to diluted extracts of cured polyethlene glycol

dimethacrylate resin as found in TheraCal LC caused a post-exposure time-dependent

increase in cell death (Lodiene et al,. 2013). At the same time, however, Portland

cement has been shown to be biocompatible (Abdullah et al., 2002). Although the

results of this study found that TheraCal LC and Biodentine demonstrated good

mechanical properties, more clinical studies are necessary, especially in direct pulp

capping of carious exposures, before these new pulp capping materials can be

recommended for clinical use.

CONCLUSION

At all time periods, TheraCal LC had the greatest flexural and compressive

strength. After 3 and 24 hours, Biodentine had the greatest flexural modulus. MTA did

not set at 15 minutes.

DISCLOSURE

The views expressed in this study are those of the authors and do not reflect the

official policy of the United States Air Force, the Department of Defense, or the United

States Government. The authors do not have any financial interest in the companies

whose materials are discussed in this article.

ACKNOWLEDGMENTS

We would like to acknowledge Mr. Dan Sellers for his assistance in the collection

of the compressive strength data.

14
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