Technique Sensitivity in Bonding to Enamel

and Dentin
John M. Powers, PhD; and John W. Farah, DDS, PhD
September 2010 Issue - Expires September 30th, 2013

Compendium of Continuing Education in Dentistry

Abstract

Bonding to enamel and dentin has been among the most significant advancements in dentistry in
the last five decades; extensive research and product development has resulted in more adhesive
options. However, bonding to enamel and dentin still proves to be challenging, and selecting the
correct product for a clinical application can be confusing. An incorrect choice can lead to
insufficient bond strength. Day-to-contamination by saliva, blood, or bleaching agents, can cause
bonding agents to be technique sensitive—they may fail prematurely if steps are not followed
meticulously. This article attempts to simplify the selection process for enamel and dentinal
bonding and summarize clinically relevant bonding information that will help produce
consistently successful results.

Adhesive dentistry began in the mid 1950s when Buonocore suggested using acid on the tooth
structure surface before applying resins. A decade later, Buonocore and his colleagues suggested
that resin tag formation was essential to the establishment of a strong bond to acid-etched
enamel. From this foundational period of enamel-only bonding, modern adhesive dentistry
evolved to employ 4th-, 5th-, 6th-, and 7th-generation systems that can also bond to dentin.

Nine types of bonding agents are included in these four generations.1-5 The first two types are in
the 4th-generation systems, which were introduced in the 1990s. Both use total-etch bonding
agents (with phosphoric acid as the etching component) and separate bottles for primer and
adhesive. They are available with either light-cured or dual-cured setting types. There are also
two product types in the 5th generation systems, which advanced to contain primer and adhesive
in a single bottle. Introduced in the mid 1990s, these also use total-etch bonding agents and are
available in either light-cured or dual-cured products.

The 6th-generation systems represented a major advance when they entered the market in the
2000s: these were the first self-etch products that relied on the use of an acidic primer,
eliminating the need for phosphoric acid as a tooth surface etchant. With 6th-generation Type I,
self-etching primer and resin adhesive are applied in separate layers and available in either light-
cured or dual-cured setting products. To simplify the bonding procedure, a combined self-etch
primer and adhesive was developed to create 6th-generation Type II products, which are
available only in a light-cured type.
The 7th-generation systems—the newest to the market—were introduced in the mid 2000s.
Using a single-bottle system, these last two types of the nine types of bonding agents require the
fewest number of steps, and are available in either light-cured or dual-cured setting types (Table
1).

CATEGORIES OF BONDING AGENTS

Total-Etch Bonding Agents

Fourth-generation total-etch bonding systems transformed dentistry in the early 1990s. While
suitable for enamel-only bonding, they allowed more success in bonding to dentin, with dentinal
bond strengths of 17 MPa to 25 MPa, encouraging many dentists to switch from amalgam to
composite resin. The two components, a primer and an adhesive, are in separate bottles and must
be mixed in precise ratios before being applied in separate layers after the tooth structure is
etched with phosphoric acid. The light-cured products in 4th-generation systems typically require
four steps, including etching, rinsing and drying, primer application, and adhesive application,
while 4th-generation dual-cured products typically necessitate six steps, including etching,
rinsing and drying, mixing both components with a catalyst, applying primer, and applying
adhesive (Table 2). Examples of light-cured systems include Adper™ Scotchbond™
Multipurpose Plus (3M ESPE, www.3mespe.com), ALL-BOND 3™ (Bisco, www.bisco.com),
Bond-It® (Pentron Clinical, www.pentron.com), LuxaBond® Total-Etch (DMG America,
www.dmg-america.com), and Optibond FL (Kerr, www.kerrdental.com). Dual-cured system
products include Adper Scotchbond Multipurpose Plus, ALL-BOND 3, Bond-It, and LuxaBond
Total-Etch.

The number of steps and requirements for exact component measurements of 4th-generation
systems can be difficult to perform chairside, increasing the risk for error. This led to the
development of 5th-generation dental adhesives, characterized by single-bottle bonding agents
with no mixing, minimizing the possibility for error.3 Suitable for application to uncut enamel,
but with impressive dentinal bond strengths of 20 MPa to 25 MPa, these simpler systems
combine the primer/adhesive monomer, which is applied in one or more layers after tooth
etching with phosphoric acid. Fifth-generation light-cured systems typically require etching,
rinsing and drying, and primer/adhesive application, while the dual-cured systems necessitate an
additional step of mixing with a catalyst (Table 2).3 Light-cured 5th-generation bonding agents
include Adper Single Bond Plus (3M ESPE), ONE STEP PLUS (Bisco), and Optibond® Solo
Plus (Kerr). Dual-cured 5th-generation bonding agents include Bond-1 (Pentron Clinical),
ExciTE® DSC (Ivoclar Vivadent, www.ivoclarvivadent.com), and Prime & Bond® NT™
(DENTSPLY Caulk, www.dentsply.com).

Self-Etch Bonding Agents

The first self-etch bonding agents were introduced in the 2000s as 6th-generation systems.3 With
the use of an acidic primer as the tooth surface etchant, they eliminate the need for etching with
phosphoric acid, as well as subsequent rinsing and drying. Without the phosphoric acid etching,
postoperative sensitivity is lower than with the 4th- and 5th-generation total-etch bonding
agents.1-3 However, dentinal bond strengths are sacrificed slightly, typically between 18 MPa and
23 MPa. While phosphoric acid is eliminated for dentinal bonding in 6th-generation systems, it
continues to be used when bonding to uncut enamel.

The 6th-generation is classified into Type I and Type II. The first has a self-etching primer and a
resin adhesive, which are applied in separate layers, while Type II combines the self-etching
primer and adhesive to simplify bonding even further. This method of application creates an
important difference between Type I and Type II: with Type I, the bonding surface is neutral in
pH because the resin adhesive is applied over the acidic primer, while the Type II surface is
acidic because the acidic primer and adhesive are applied as one component.

The light-cured 6th-generation Type I takes two steps, including application of separate primer
and adhesive, while the dual-cured agents require three steps, mixing with a catalyst and
applying primer and adhesive (Table 2). (However, for both of these, an additional first step of
etching with phosphoric acid may be needed if bonding to uncut enamel.) Light-cured 6th-
generation Type I bonding agents include Adper Scotchbond SE Self-Etch Adhesive, Clearfil™
SE BOND (Kuraray America, www.kuraraydental.com), Clearfil SE PROTECT (Kuraray
America), FL-Bond II (SHOFU, www.shofu.com), and frog (SDI-North America,
www.sdi.com.au). Examples of dual-cured 6th-generation Type I bonding agents are AdheSE®
(Ivoclar Vivadent), Clearfil LINER BOND 2V (Kuraray America), Contax™ (DMG America),
and Nano-Bond® (Pentron Clinical).

The Type II bonding agents are available with light-cured settings only and typically need only
mixing and applying primer–adhesive to complete (Table 2). Examples of light-cured 6th-
generation Type II bonding agents include Adper Prompt L-Pop Self-Etch Adhesive (3M ESPE),
ALL-BOND SE® (Bisco), and Brush & Bond™ (Parkell, www.parkell.com).

Just as 5th-generation bonding agents simplified previous systems, 7th-generation bonding

agents integrated 6th-generation materials into a single-bottle system. Introduced in the mid
2000s, 7th-generation self-etching bonding agents have the fewest number of steps when
bonding to dentin, providing dentinal bond strengths of 18 MPa to 25 MPa. The light-cured
agents require no mixing, with the application of a primer–adhesive as the only step, while dual-
cured products typically require mixing with a catalyst (Table 2). (With both light-cured and
dual-cured products, an additional first step of etching with phosphoric acid is used if bonding to
uncut enamel.) Examples of light-cured 7th-generation bonding agents are AdheSE One F
(Ivoclar Vivadent), BOND FORCE (Tokuyama Dental/Tokuyama America, www.tokuyama-
us.com), Clearfil S3 BOND (Kuraray America), G-BOND (GC America, www.gcamerica.com),
go! (SDI-North America), Optibond® All-In-One (Kerr), and Xeno® IV (DENTSPLY Caulk).
Dual-cured 7th generation bonding agents include Clearfil DC BOND (Kuraray America),
Futurabond DC (VOCO America, www.voco.com), and Xeno IV DC (DENTSPLY Caulk).

CLINICAL APPLICATIONS
Each generation is recommended for a specific clinical application: 4th-generation systems are
considered best for composite cores; 5th-generation systems are ideal for bonding of anterior and
posterior composites and cementation of veneers with resin cements; 6th-generation bonding
agents are recommended for bonding of posterior composites; light-cured 7th-generation
bonding agents are ideal for bonding of posterior composites; and dual-cured 7th-generation
bonding agents are suggested for bonding of esthetic posts and ceramic restorations with resin
cement (Table 3).3

 
COMPONENTS IN BONDING AGENTS
Etchant

To understand how an etchant works, it is important to define the smear layer, which is the layer
of debris on the surface of dental tissues created by cutting a tooth. Depending on the surface
preparation, the smear layer can vary in thickness, roughness, and degree of attachment to the
underlying tooth structure. It must be removed, modified, or penetrated by resin to allow for
bonding between the tooth and restorative material. In 4th- and 5th-generation total-etch
products, the etchant used to remove the smear layer completely is phosphoric acid. In self-etch
products, a primer–adhesive penetrates and re-precipitates the smear layer. Self-etching primers
are acidic monomers that combine the etchant with the primer or primer–adhesive. While some
acidic primers are based mainly on lower concentrations of phosphoric acid (typically 35% to
37%), some have pH levels higher than phosphoric acid.

Primer

The primer promotes good wetting of enamel and dentin.1-5 It is composed of hydrophilic
monomers, usually carried in a water-soluble solvent (such as acetone, ethanol, or water) to
promote good flow and penetration into hydrophilic dentin. The most extensive penetration
possible is important because this influences the resulting bond strength. Self-etch bonding
agents use primers that are also acidic to assist in the penetration of the smear layer; refrigeration
can extend shelf life.

Adhesives

The adhesive creates the bond between enamel or dentin and resin composite restorative material
or resin cement.1-5 Adhesives are mostly hydrophobic, dimethacrylate monomers that are
compatible with monomers used in both the primer and the resin composite. This compatibility
helps the adhesive act as the link between the hydrophilic primer and the hydrophobic resin
composite. The primer–adhesives used in 7th-generation bonding agents are acidic because they
must penetrate the tooth’s smear layer.

Initiator and Accelerator

Proper curing—the crosslinking of enamel or dentin and resin bonds until a solid bond is formed
—is essential for providing good retention and sealing. The crosslinking reaction begins with an
initiator, and an accelerator activates the initiator to promote curing at room temperature. The
initiator and accelerator are required in both light- or dual-cured settings.1-5 In light-activated
products, these components are typically camphorquinone and organic amine.

Filler

Fillers are submicron glass particles and nanofillers ranging from 0.5% to 40% by weight,1-5
which help to control handling. In addition, fillers may improve bonding strength and increase
film thickness of the adhesive layer, which creates more of a buffer and reduces the risk of
postoperative sensitivity.

Solvent

The most commonly used solvents are acetone, ethanol, and water. The solvent affects the
evaporation rate:1-5 acetone evaporates quickly and requires the shortest drying time; ethanol
evaporates more slowly and requires moderate drying time; and water evaporates very slowly
and needs the longest drying time. The extent of dryness (promoted by the amount of air applied
to the teeth with a three-way syringe) strongly influences the resultant bond strength. A
somewhat moist dentin surface is needed for optimal bonding, with over-wet or over-dry
conditions weakening bonds: over-wet conditions could result in water remaining in the adhesive
layer, while over-drying could cause reduced penetration of adhesive, collapse of the dentin fiber
network, and shrinkage of collagen fibers. One recently introduced product—Bond-1® SF
Solvent Free SE Adhesive (Pentron Clinical)—is solvent-free, reportedly eliminating common
technique-sensitive issues, such as under-drying or over-drying.6

Other Ingredients

Fluoride, desensitizers, and antimicrobial ingredients are also used in the process of adhesive
bonding.1-5 Whether these ingredients affect bonding has not yet been demonstrated clinically.

MECHANISMS OF BONDING
Total-Etch Systems

In 4th- and 5th-generation bonding agents, application of phosphoric acid, followed by rinsing,
completely removes the smear layer and plugs.1,2 The 4th-generation separate primer and
adhesive or the 5th-generation primer–adhesive combination fills in the dentinal tubules and
interacts with collagen fibers to form a hybrid layer.

Self-Etch Systems

Sixth- and 7th-generation bonding agents use the smear layer as a bonding substrate.3-5 The 6th-
generation acidic primer or the 7th-generation primer–adhesive combination demineralizes the
smear layer and the top layer of the underlying dentin surface.7 They also infiltrate collagen
fibers and copolymerize, minimizing voids and potential leakage. Because the etched surface is
not rinsed, the demineralized smear layer is incorporated into the hybrid layer, which is typically
thicker than the hybrid layer formed with 4th- and 5th-generation systems, ranging from 0.5 μm
to 5 μm.7 This somewhat thicker hybrid layer works as a buffer to minimize postoperative
sensitivity.

MINIMIZING TECHNIQUE SENSITIVITY

Variations in tooth structure and contaminants can reduce the strength of bonding agents.
Managing these variables minimizes technique sensitivity.

Tooth Structure

It has been established that tooth structure variations can affect adhesive bond strength. For
example, in vitro bond strengths to carious tooth structure are generally lower than to noncarious
tooth structure, while in vitro bond strengths to primary tooth structure are generally lower than
to permanent tooth structure.8,9 Bond strengths to deep dentin can be 50% lower than bond
strengths to superficial dentin.10 Application of additional layers of resin may be necessary to
obtain a glossy surface and increase bond strength. Dentin prepared with an Erbium: YAG laser
has no smear layer,11 and etching with phosphoric acid is not necessary. Application of self-etch
bonding agents might require several layers to obtain a glossy surface.

With uncut enamel, two techniques could be used to remove the enamel pellicle and prepare it
for bonding: the pumice technique and the pre-etch method. Pumice can be used on uncut enamel
to improve the bond strength by 3 MPa to 14 MPa, depending on the bonding product used
(Table 4).12 In the pre-etch technique, phosphoric acid is applied to enamel before tooth
preparation. This approach eliminates the need to etch uncut enamel and avoids possible
contamination of dentin with phosphoric acid. Both techniques are effective on unrestored teeth,
as well as on teeth with old amalgams that need replacement.

Most manufacturers of self-etching bonding agents recommend the use of phosphoric acid to
etch uncut enamel before application of the self-etching primer or self-etching adhesive. Even so,
there may be only a small improvement of up to 3 MPa in bond strength—or even a slight
decrease in strength (Table 5). If the phosphoric acid also etches dentin, the bond strength of the
self-etching adhesive to dentin may be reduced, especially with 6th-generation Type II and 7th-
generation bonding agents. This reduction may occur if the self-etching adhesive fails to
penetrate completely the additional demineralized dentin produced by the phosphoric acid etch.
To prevent this, apply extra coats of bonding agent to obtain a shiny surface as needed.
 

Contaminants

Many common contaminants of the tooth surface can weaken adhesive bonds. The first is water,
so overly wet dentin must dry before application of the bonding agent. Saliva, blood, and plasma
are other tooth surface contaminants, with blood being more detrimental to bond strength than
saliva.13-16 To prevent weak bonding, rinse contaminated areas with water (and dry sufficiently)
or re-etch before bonding.

Residual oxygen from home or office bleaching can also lower bond strength to dentin.1,2 Wait 1
week after bleaching before performing a bonding procedure. (Note that the color of bleached
teeth may rebound during this time as the teeth rehydrate.)

Various desensitizers have also been found to lower in vitro dentinal bond strengths by more
than 50%.17 In this case, opt for noneugenol temporary cements for provisional restorations,
because eugenol-based materials can lower bond strength to dentin.13,14 If a eugenol-based
material must be used, the tooth should be pumiced before bonding.

Residual chemicals from hemostatic agents containing ferric sulfate, aluminum chloride, or other
chemicals can lower bond strength to dentin.18 To improve bond strength, rinse contaminated
areas for at least 10 sec with water and dry sufficiently before bonding. Areas contaminated with
ferric sulfate should be re-etched with phosphoric acid before bonding. Remineralizing agents
such as CPP-ACP and NovaMin® (NovaMin Technologies, www.novamin.com) may provide
stronger bonding.

BONDING TIPS
Ceramic Crowns, Inlays, and Onlays

For maximum bonding success, verify that the bonding agent is compatible with the resin cement
used. Use dual-cured adhesives with opaque ceramic restorations, especially if they will only be
cured once, after the restoration is placed. Light-cured adhesives can be used with opaque
ceramic restorations if they are cured before the restoration is placed; however, this could create
a thicker adhesive/cement layer and affect fit. Bonding agents with acetone should be used soon
after dispensing.1-5

Core Materials/Fiber-Reinforced Esthetic Posts

Choosing the correct curing method is important for strong bonding of esthetic posts. Dual-cured
activators are available with some 5th-generation bonding agents and should be used with self-
and dual-cured resin core materials.9 Sixth-generation Type I bonding agents are generally
compatible with self-cured composite cores or resin cements. The tooth is primed, the adhesive is
applied, and then the composite core is placed. Sixth-generation Type II and 7th-generation
bonding agents are generally not compatible with self-cured composite cores or resin cements,
because the acidity of the bonding agent can interfere with the setting of the composite. Light-
cured bonding agents may be difficult to activate properly for cementation of esthetic posts; in
this case, the use of dual-cured bonding agents is recommended.

Posterior Composites

Controlling the evaporation of solvent is key to strong bonding of posterior composites. Most
bonding agents should be used within 3 min of dispensing to minimize the effect of solvent
evaporation. Carefully follow instructions on application time and the use of air to thin the
adhesive and evaporate the solvent. With less volatile solvents, such as water and ethanol, more
air is needed to evaporate the solvent. Another concern is that some bonding agents etch the
surface of the metal matrix band, making removal difficult: this etching can be prevented by
placing a separating agent (wax) on the surface of the metal band.

Veneers

The appropriate curing technique to use for optimal bonding depends on the thickness of
veneers. For veneers less than 1 mm thick, a one-step light-curing technique—in which one
applies the bonding agent, followed by the resin cement, the veneer, and then the light cure—is
recommended.19 For veneers more than 1 mm thick, use a two-step light-curing technique,
applying the bonding agent and light cure, then applying the resin cement, veneer, and light cure
again. Instructions for some resin cements (such as RelyX™ Veneer [3M ESPE]) recommend
the additional application of the bonding agent to the veneer without separate light curing before
cementation.

CONCLUSION
The choice of an adhesive system depends on the clinical application: 4th-generation systems are
recommended for bonding of composite cores; 5th-generation systems are best for bonding of
anterior and posterior composites and cementation of veneers with resin cements; 6th-generation
systems are suggested for bonding of posterior composites; light-cured 7th-generation systems
are advised for bonding of posterior composites; and dual-cured 7th-generation bonding systems
are recommended for bonding of esthetic posts and ceramic restorations with resin cement.

Bonding to enamel and dentin can be challenging because different tooth substrates and
contaminants cause bonding agents to be technique sensitive and result in decreases in bond
strength of as much as 50%. However, understanding the characteristics of bonding agent
components and how to manage possible pitfalls in bonding can produce better results. As
bonding agents improve, the dentist will also experience less technique sensitivity, while
obtaining excellent bond strengths to enamel and dentin.

DISCLOSURE
The authors have a financial interest in Dental Consultants, Inc., and are editors of The Dental
Advisor. They have received grant or research support from 3M ESPE, Kuraray America, and
GC America.

REFERENCES
1. Powers JM, Sakaguchi R, eds. Craig’s Restorative Dental Materials. 12th ed. St. Louis, MO:
Mosby Elsevier; 2006.

2. Powers JM, Wataha JC, eds. Dental Materials–Properties and Manipulation. 9th ed. St.
Louis, MO: Mosby Elsevier; 2008.

3. Farah JW, Powers JM, eds. Bonding agents—2008. Dental Advisor. 2008;25(5):1-9.

4. Farah JW, Powers JM, eds. 7th-generation bonding agents. Dental Advisor. 2009;26(6):1-6.

5. Powers JM, O’Keefe KL. Update on seventh-generation bonding agents. Inside Dentistry.
2009;5(2):52-56.

6. Farah JW, Powers JM. Innovations in prevention: fluoride varnish and calcium phosphates.
Dental Advisor. 2010;27(2):12.

7. Pinzon LM, Reis A, Saiz E, et al. Interfacial structure and nanomechanical properties of self-
etch adhesive systems over-time [abstract]. J Dent Res. 2007;86(spec iss A):116.
8. Xie J, Flaitz CM, Hicks MJ, Powers JM. Bond strength of composite to sound and artificial
carious dentin. Am J Dent. 1996;9(1):31-33.

9. Agostini FG, Kaaden C, Powers JM. Bond strength of self-etching primers to enamel and
dentin of primary teeth. Pediatr Dent. 2001;23(6):481-486.

10. O’Keefe KL, Powers JM. Adhesion of resin composite core materials to dentin. Int J
Prosthodont. 2001;14(5):451-456.

11. Trajtenberg CP, Pereira PNR, Powers JM. Resin bond strength and micromorphology of
human teeth prepared with an Erbium: YAG laser. Trans Academy of Dental Materials.
2001;15:171.

12. O’Keefe KL, Uceda-Gomez N, Pinzon LM, Powers JM. Bond strength of self-etching
adhesives to pre-treated enamel. Dental Advisor Research Report. 2005;(2):1.

13. Powers JM, Finger WJ, Xie J. Bonding of composite resin to contaminated human enamel
and dentin. J Prosthodont. 1995;4(1):28-32.

14. Xie J, Powers JM, McGuckin RS. In vitro bond strength of two adhesives to enamel and
dentin under normal and contaminated conditions. Dent Mater. 1993;9(5):295-299.

15. Pinzon LM, O’Keefe KL, Powers JM. Bond strength of composite with self-etching
adhesives to blood-contaminated dentin [abstract]. J Dent Res. 2003;82(spec iss A):570.

16. Pinzon LM, O’Keefe KL, Powers JM. Adhesion of composite with self-etching primer to
saliva-contaminated moist and dry dentin. Trans Academy of Dental Materials. 2002;16:336.

17. Li D, O’Keefe KL, Powers JM. Effect of dentin desensitizers on bond strength on deep
dentin [abstract]. J Dent Res. 2000;79(spec iss A):509.

18. O’Keefe KL, Pinzon LM, Powers JM. Effect of astringent contamination on bond strength of
self-etching adhesives to dentin [abstract]. J Dent Res. 2003;82(spec iss A):25.

19. Steffer MR, O’Keefe KL, Powers JM. Bonding porcelain veneers with light-cured adhesives
[abstract]. J Dent Res. 2005;85(spec iss A):1824.