©

Operative Dentistry, 2008, 33-4, 408-412

Depth of Cure of
Dental Resin Composites:
ISO 4049 Depth and
Microhardness of Types
of Materials and Shades

BK Moore • JA Platt • G Borges

T-MG Chu • I Katsilieri

Clinical Relevance
Achieving a high degree of cure throughout a 2 mm thickness of light-activated resin compos-
ite did not occur for many types and shades of resin composite. Clinicians should check the
depth of cure by using the scraping method.

SUMMARY Unfortunately, the dentist has no means of mon-

The optimal degree of curing throughout the itoring the cure of the resin surfaces not direct-
bulk of a visible light-activated dental resin com- ly exposed to the curing light. Techniques, such
posite is acknowledged to be important to the as the layered buildup of restorations in 2 mm
clinical success of a resin composite restoration. increments with longer activation times than 20
seconds, have been suggested. This study inves-
*B Keith Moore, PhD, professor and director of Graduate Dental tigated the depth of cure (DOC) of a commercial
Materials, Dental Materials Division, Department of resin composite in three types: flowable, hybrid
Restorative Dentistry, Indiana University School of Dentistry, and packable and in three shades: B1, A3 and D3
Indianapolis IN, USA
after 20 second activation with a quartz halogen
Jeffrey A Platt, DDS, MS, associate professor and director of light (620 mW/cm2). Depth of cure was measured
Division of Dental Materials, Department of Restorative
by scraping the uncured material and by using a
Dentistry, Indiana University School of Dentistry, Indianapolis
IN, USA Knoop Hardness profile, starting from the sur-
face exposed to the light. Using a minimum
Gilberto Borges, DDS, PhD, visiting research scholar, Dental
Knoop Hardness ratio of 0.8 bottom/top only, the
Materials Laboratory, Indiana University School of Dentistry,
Indianapolis IN, USA flowable in shade B1 achieved a 2 mm DOC.
Using the less restrictive scraping test, only the
Tien-Min Gabriel Chu, DDS, PhD, assistant professor of
Biomedical Engineering, Purdue School of Engineering,
B1 shade of flowable and hybrid significantly
IUPUI, Indianapolis IN, USA exceeded a 2 mm DOC. Knoop Hardness at the
DOC obtained by scraping ranged from 55%-70%
Iphigenia Katsilieri, DDS, MS, graduate student, Dental
Materials, Indiana University School of Dentistry, Indianapolis of the top surface hardness.
IN, USA These data suggest that a 2 mm buildup layer-
*Reprint request: 1121 W Michigan St, Indianapolis IN 46202, USA; ing technique may not result in adequate curing
e-mail: kmoore@iupui.edu of the bottom layer for such a wide range of
DOI: 10.2341/07-104 materials and that manufacturers need to pro-
Moore & Others: Depth of Cure of Resin Composites 409

vide quantitative information about Table 1: Resin Composites*

DOC at specific activation times and
Aeliteflo Aelite Aelite
light intensities for their entire BISCO All Purpose LS Posterior
range of resin materials and shades Body BISCO
so that the dentist can devise a BISCO
placement technique that will TYPE Flowable Hybrid Packable
ensure adequate cure of the bulk of a SHADES B1, A3, D3 B1, A3, D3 B1, A3, D3
restoration. Ethoxylated Bisphenol A
Dimethacrylate X X X
INTRODUCTION TEGDMA X X
The degree of cure of visible light activat- Glass filler X X X
ed dental resins was recognized as impor- Amorphous silica X X
tant to the clinical success of these mate- *Compositions taken from manufacturer’s Material Safety Data Sheets
rials soon after these materials were BISCO (Schaumburg, IL, USA)
introduced.1-4 While the relative degree of
cure of the external surface of a restora-
tion can usually be evaluated with simple tech- Table 2: Light Output Transmitted Through 1.3 mm Discs of Different
niques, the cure of the inner layers of resin is not Materials (mW/cm2)
similarly accessible to evaluation, and it was recog- Resin Composites
nized early on that, unlike chemically activated Flowable Hybrid Packable
resins, an adequate cure of the entire visible light B1 50 20 12
activated restoration cannot be assumed, based on A3 12 6 4
external surface properties.5 It has been shown that D3 10 8 6
inadequate polymerization would result in a reduc-
tion in physical properties.6 Furthermore, compo-
nents, such as residual monomer washed-out from the mm thickness of material is cured,15 but little quantita-
polymerized resin, may irritate soft tissue and predis- tive advice is typically available to guide the practition-
pose plaque accumulation, jeopardizing clinical success er in adjusting placement technique.
of the restoration.7 This study investigated the depth of cure of three dif-
The depth of cure of a visible-light activated resin has ferent shades (opacities) of a resin composite available
been the subject of considerable laboratory research.3,8-10 in three different types that vary in viscosity and filler
Even after more than 25 years of clinical use, there are levels. Both the ISO scraping technique and a hardness
still controversies about the depth of cure of a visible- profile (Knoop) from the top to the bottom of the speci-
light activated resin. A number of different techniques
8 men were used to evaluate depth of cure. The null
have been employed to measure the properties of the hypothesis was that the shade and consistency of the
polymerized resin composite most distant from the light resin composite would not interfere with the depth of
source.11-12 These techniques include scraping away the polymerization.
unset material and measuring the remaining specimen,
METHODS AND MATERIALS
measuring top and bottom hardness and measuring top
and bottom degree of conversion of double bonds in the The resin composites employed are shown in Table 1.
polymer.13-16 The scraping technique has been codified as Table 2 shows the amount of activation light trans-
the depth of cure measure in the ISO standard for den- mitted through a 1.3 mm thickness of each of the types
tal resins 4049.12 To define depth of cure based on top and shades. This was measured and decreased from
and bottom hardness measurements, it is common to flowable to hybrid to packable within a specific shade
calculate the ratio of bottom/top hardness and give an and from shade B1 to A3 or D3 within a material type.
arbitrary minimum value for this ratio in order to con-
Three specimens of each material type and shade, 4
sider the bottom surface as adequately cured. Values of
mm in diameter and 6 mm deep, were condensed into
0.80 and 0.85 have often been used.13-14
Teflon molds. A 1 mm metal spacer was placed over the
Manufacturers and suppliers of dental resins rarely mold to hold the tip of the activating light back 1 mm
identify the basis for recommendations about depth of from the surface of the resin. The specimens were acti-
cure as they relate to light activation. An all too com- vated for 20 seconds using a quartz halogen activation
mon recommendation is the use of some specific light light (Visilux 2, Model 5520AA, Ser No 115449, 3M
exposure time to “cure” a 2 mm thickness.15-17 It is well Dental Products, St Paul, MN, USA). Light output was
known that factors, such as resin type, filler levels, checked with a hand-held radiometer (Power and Dose
resin shade, intensity and spectrum of the activation Meter, ACCU-CAL–30, Dymax Corp, Torrington, CT,
light, influence the degree to which the bottom of a 2 USA) to ensure consistency between specimens
410 Operative Dentistry

(620mW/cm2). A 20 second light exposure using a

common quartz halogen light18 was employed to
simulate a typical clinical activation routine.
Scraping away soft material after activation and
measurement of the remaining specimen was fol-
lowed by hardness measurements starting at the
surface exposed to the light and proceeding through
the length of the specimen.12
After activation, the specimens were immediately
removed from the molds and the uncured material
scraped away with a plastic spatula. The length of
the remaining material was measured with a digi-
tal micrometer in three places and an average
length was obtained. This value was divided by two
to obtain the ISO 4049 depth of cure (DOC).12
Average values and standard deviations were calcu-
lated for the ISO DOC for each material and shade.
After the DOC was measured, the specimens were Figure 1. Depth of Cure of BISCO AELITE resin composites determined by ISO
embedded in epoxy resin and hemi-sectioned along 4049 and from Knoop Hardness using either 80% or 85% of the hardness of the
their long axis. One sectioned half of each specimen top surface.
was used for Knoop Hardness testing (KHN). A
hardness profile was obtained by measuring start-
ing at 0.5 mm from the top surface and measuring
at 0.3-mm intervals to the bottom surface or until
reliable Knoop Hardness could no longer be meas-
ured because the material was too soft. Knoop
Hardness measurements were replicated three
times at each position and an average determined.
The hardness data for each of the three specimens
was plotted against distance from the top surface,
and a linear regression analysis was performed to
estimate top hardness and rate of decline in hard-
ness with depth from the top surface. The regres-
sion analysis data was also used in subsequent cal-
culations to obtain Knoop Hardness values at spe-
cific distances from the top of the specimen.
Confidence intervals from the regression analysis
were employed to estimate error bars, when pre-
senting KHN data.
Figure 2. Percentage of top Knoop Hardness at depth of cure determined by ISO
4049.
RESULTS
Figure 1 compares the depth of cure as measured sion analyses of the KHN profile data. The resulting
with the ISO 4049 scraping technique against the KHN values were used to estimate the percentage of
depth of cure estimated from the Knoop Hardness pro- hardness at the ISO DOC compared to the top. With the
files using bottom/top hardness ratios of 0.85 and 0.80, exception of Flowable, the Knoop Hardness values of all
respectively. Using the ISO criteria,12 only the lightest materials and shades varied between 50% and 70%
shade (B1) of this resin system meets the 2.0 mm below the top surface at the ISO depth of cure.
assumption for all three types of materials. Using the
least restrictive KHN criteria of 0.8 of the top hardness, DISCUSSION
only shade B1 of the flowable yields a 2 mm depth of The null hypothesis of this study, the shade and con-
cure. In general, as expected from the light transmis- sistency not interfering with the depth of polymeriza-
sion data, the DOC is reduced with darker shades and tion of a resin composite, was rejected due to the
more heavily filled types of material. results (Figure 1). Although most clinicians would
An alternate presentation of the data is shown in assume that shade D3 is darker than shade A3, both
Figure 2. The DOC determined by the ISO technique the light transmission data and depth of cure do not
was entered into the equations obtained from regres- necessarily support this assumption. Using clinical
Moore & Others: Depth of Cure of Resin Composites 411

perception of relative darkness of shades may not restoration, it is the opinion of the authors that the
result in adequate compensation if the clinician varies kind of testing reported in this study should be done by
activation time to compensate for shade variation. If the manufacturers and suppliers of dental resin com-
manufacturers use ISO 404912 to justify recommenda- posites for all of their types of materials and shades,
tions for curing times and depths of cure, the data in and the information be supplied to the dentist so that
Figure 2 suggest a bottom hardness far below 80% of the placement technique can be modified to ensure rea-
the top surface, with accompanying decreases in other sonable properties for the full bulk of a resin composite
mechanical properties. Since it has been shown that restoration.
even a well polymerized resin composite can release
some residual monomers and other reactive species,19 (Received 13 June 2007)
it is reasonable to conclude that more substances
would elute from poorly polymerized resin at the bot-
tom of the restoration. These substances have the References
potential to irritate soft tissues and pulp, stimulate 1. Cook WD (1980) Factors affecting the depth of cure of UV-
the growth of bacteria and promote allergic reac- polymerized composites Journal of Dental Research 59(5)
800-808.
tions.7,20-21
2. Rock WP (1974) The use of ultra-violet radiation in dentistry
The parameters used in this experiment are proba- British Dental Journal 136(11) 455-458.
bly conservative compared to actual clinical situa-
3. Yearn JA (1985) Factors affecting cure of visible light activat-
tions. Based on measured light output, the curing
ed composites International Dental Journal 35(3) 218-225.
light used would rank as a good quartz halogen acti-
vation light. The 1 mm distance between the light tip 4. Ruyter IE & Oysaed H (1982) Conversion in different depths
of ultraviolet and visible light activated composite materials
and resin surface is probably the minimum that is Acta Odontologica Scandinavica 40(3) 179-192.
clinically feasible. Most recommendations for incre-
5. Shortall AC, Wilson HJ & Harrington E (1995) Depth of cure
mental buildup and curing of a dental resin suggest 2
of radiation-activated composite restoratives—influence of
mm thick layers.18,22 This depth of cure is obtained for shade and opacity Journal of Oral Rehabilitation 22(5) 337-
only one type and shade of material tested, using the 342.
least conservative hardness criteria. None of the sam-
6. Ferracane JL, Mitchem JC, Condon JR & Todd R (1997) Wear
ple groups met the 0.85 hardness ratio for a 2.0 mm and marginal breakdown of composites with various degrees of
thickness. The ISO criteria significantly inflated the cure Journal of Dental Research 76(8) 1508-1516.
depth of cure compared to hardness data for all mate- 7. Sideridou ID & Achilias DS (2005) Elution study of unreacted
rials tested.23 Even using this criteria, some of the Bis-GMA, TEGDMA, UDMA, and Bis-EMA from light-cured
types of material and shades did not have a DOC of dental resins and resin composites using HPLC Journal of
2.0 mm. The results of this investigation are in dis- Biomedical Materials Research. Part B, Applied Biomaterials
agreement with some studies that have shown that 2- 74(1) 617-626.
mm increments are well polymerized24-25 but agree 8. Nomoto R, Asada M, McCabe JF & Hirano S (2006) Light
with other studies that show inefficiency of polymer- exposure required for optimum conversion of light activated
ization at a 2 mm depth.26 This study evaluated the resin systems Dental Materials 22(12) 1135-1142.
same brand of materials, which is a limitation with 9. Kawaguchi M, Fukushima T & Miyazaki K (1994) The rela-
respect to generalizing the conclusions. However, the tionship between cure depth and transmission coefficient of
objective was to show what happens to the depth of visible-light-activated resin composites Journal of Dental
cure when composite formulation and shade are var- Research 73(2) 516-521.
ied over a wide range from the standpoint of resin 10. Shortall AC, Wilson HJ & Harrington E (1995) Depth of cure
composites intended for different clinical applications. of radiation-activated composite restoratives—influence of
shade and opacity Journal of Oral Rehabilitation 22(5) 337-342.
Clearly, studies should be done to evaluate the behav-
ior of other brands of resin composite. 11. Yap AU, Soh MS & Siow KS (2002) Effectiveness of composite
cure with pulse activation and soft-start polymerization
CONCLUSIONS Operative Dentistry 27(1) 44-49.

This study tested one brand of composite in flowable, 12. ISO Standard (2000) ISO 4049 Polymer based filling, restora-
tive and luting materials International Organization for
hybrid and packable formulations in three shades (B1, Standardization 3rd edition 1-27.
A3 and D3) and indicates that the materials did not
13. Bouschlicher MR, Rueggeberg FA & Wilson BM (2004)
achieve a 2 mm depth of cure with 20 second light expo-
Correlation of bottom-to-top surface microhardness and con-
sure when the bottom hardness of the specimens was version ratios for a variety of resin composite compositions
measured. Despite using the ISO standard for depth of Operative Dentistry 29(6) 698-704.
cure, not all materials met the DOC criteria at a 2 mm
14. Aravamudhan K, Rakowski D & Fan PL (2006) Variation of
thickness. Since the clinician has no way of monitoring depth of cure and intensity with distance using LED curing
the degree of cure of the bottom of a resin composite lights Dental Materials 22(11) 988-994 Epub 2006.
412 Operative Dentistry

15. Rueggeberg FA, Caughman WF, Curtis JW Jr & Davis HC 21. Lee SY, Huang HM, Lin CY & Shih YH (1998) Leached com-
(1993) Factors affecting cure at depths within light-activated ponents from dental composites in oral simulating fluids and
resin composites American Journal of Dentistry 6(2) 91-95. the resultant composite strengths Journal of Oral
16. Jain P & Pershing A (2003) Depth of cure and microleakage Rehabilitation 25(8) 575-588.
with high-intensity and ramped resin-based composite curing 22. Aguiar FH, Lazzari CR, Lima DA, Ambrosano GM &
lights Journal of the American Dental Association 134(9) Lovadino JR (2005) Effect of light curing tip distance and
1215-1223. resin shade on microhardness of a hybrid resin composite
17. Rueggeberg FA, Ergle JW & Mettenburg DJ (2000) Brazilian Oral Research 19(4) 302-306. Epub 2006 Feb 14.
Polymerization depths of contemporary light-curing units 23. DeWald JP & Ferracane JL (1987) A comparison of four
using microhardness Journal of Esthetic Dentistry 12(6) 340- modes of evaluating depth of cure of light-activated compos-
349. ites Journal of Dental Research 66(3) 727-730.
18. Caldas DB, de Almeida JB, Correr-Sobrinho L, Sinhoreti MA 24. Lindberg A, Peutzfeldt A & van Dijken JW (2005) Effect of
& Consani S (2003) Influence of curing tip distance on resin power density of curing unit, exposure duration, and light
composite Knoop Hardness number, using three different guide distance on composite depth of cure Clinical Oral
light curing units Operative Dentistry 28(3) 315-320. Investigation 9(2) 71-76 Epub 2005 Apr 7.
19. Tanaka K, Taira M, Shintani H, Wakasa K & Yamaki M 25. Rueggeberg FA, Ergle JW & Mettenburg DJ (2000)
(1991) Residual monomers (TEGDMA and Bis-GMA) of a set Polymerization depths of contemporary light-curing units
visible-light-cured dental composite resin when immersed in using microhardness Journal of Esthetic Dentistry 12(6) 340-
water Journal of Oral Rehabilitation 18(4) 353-362. 349.
20. Lee SY, Greener EH & Menis DL (1995) Detection of leached 26. Fan PL, Schumacher RM, Azzolin K, Geary R & Eichmiller
moieties from dental composites in fluids simulating food and FC (2002) Curing-light intensity and depth of cure of resin-
saliva Dental Materials 11(6) 348-353. based composites tested according to international standards
Journal of the American Dental Association 133(4) 429-434.