1

Seminar by

Dr. N. JAMINI
POST GRADUATE STUDENT

SRI RAMACHANDRA DENTAL COLLEGE AND HOSPITAL

CHENNAI

ACID ETCHING

CONTENTS
1. INTRODUCTION
2. HISTORY
3. THE IDEAL DENTIN STRUCTURE
4. ACID ETCHING ON ENAMEL
5. CONDITIONING OF DENTIN
6. CHALLENGES IN DENTIN BONDING
7. OBJECTIVES
8. EFFECTS OF ACID CONDITIONED DENTIN
9. CONDITIONING OF DENTIN
10. FACTORS AFFECTING DENTIN CONDITIONING
11. ROLE OF HYBRID LAYER
12. ROLE OF WATER IN BONDING PROCESS
13. DENTIN PERMEABILITIES
14. MOIST VERUS DRY DENTIN SURFACES
15. BIOCOMPATIBILITY
16. PRIMING (SELF ETCH, TOTAL ETCH)
17. EFFECT OF ETCHING ON PRIMARY TEETH
18. APPLICATIONS OF THE ACID CONDITIONERS
19. FACTORS TAKEN INTO CONSIDERATION
20. DISADVANTAGES
21. PROBLEMS

3
INTRODUCTION
During the last decades clinicians have been confronted with a continuous and fairly
rapid turnover in adhesive materials. It started in the mid- 60s with the advent of first
commercialized restorative resin composites, followed in the early 70s with the
introduction of the acid etch technique in clinical practice. [Operative dentistry
supplement 2001: 6 ; 119-144]
The bonding of restorative materials to teeth typically involves the use of acids to
demineralize their surfaces. Changes in the surface due to acid treatment include the
gross removal of smear layer, an increase in both permeability, micro porosity and
chemical modifications of the surface composition. [Dental material 2002; 18; 26-35]
Bonding to enamel is now considered a durable and predictable clinical procedure.
The acid etch technique relies on the micro mechanical retention obtained on the
enamel surface by an acidic etchant and subsequent penetration of a blend of
polymerizable monomers into the interprismatic spaces to form enamel resin tags
(Gwinnett and matsui 1967)
In contrast, dentin bonding has become one of the most challenging topics of
restorative dentistry. Recent developments in dentin bonding technology involve the
simultaneous etching of enamel and dentin with acids. Dentin etching has become
most common in Japan since the late 70s [Operative dentistry; 2000;25; 144-186].
A significant advance in dentin bonding was made by kanca who reasoned that if
appropriate, chemically compatible, resin formulation was added following a total
etch of the mineralized dental tissues [Esthetics].The evolution of adhesive systems
has resulted in bond strengths to dentin that are very close to that of the celebrated
union of enamel.
Possibly, in the not too distant future, dental adhesion will involve only one
application of a self-etching system capable of satisfactorily bonding both to enamel
and to dentin [Quintessence Int 2002; 33; 213 214]

4
HISTORY:
Adhesive dentistry originated from a simple clinical experiment and the vision and
dedication of a unique dental scientist. In 1955, Buonocore reported the self-curing,
methyl-methacrylate resin could be durably bonded to the enamel of human incisor
teeth. Phosphoric acid was the agent of choice and was applied to the enamel
surface for 30 seconds at a concentration of 85%.
The first clinical trails of the method were concerned with the sealing of pits and
fissures of molar teeth to prevent their decay. (Dental adhesives John Gwinneth)
FUSAYAMA et al [1979] introduced the concept of Total etching advocating the
treatment of both enamel and dentin with phosphoric acid prior to bonding. This
technique has become relatively popular in Japan, but initially met with resistance in
the USA. (Esthetics dentistry and ceramic restoration, Bernaud Touati]
Between 1982 and 1985, Nakabayashi described micro mechanical bonding
mechanism of dentin bonding agents. He introduced the concepts of hybridization
(Operating Dentistry 2003 28; (3); 287- 295). A significant step in improving the bond
to dentin through smear layer removal came from the work of Bowen. He showed an
improvement in bond strength of dentin with a combination of ferric oxalate
conditioning and resin priming of the dentin surface.
The primers consisted of a comonomer of N- Tolyl glycineglycidil metharylate (NTGGMA) and a coupling agent derived from an addut of pyromellitic acid dianhydriate
and 2 hydroxyethyl methacrylate (PMDM). The oxalate was changed to the
Aluminium salt to avoid staining invivo associated with the ferricion. The bonding
procedure was clinically demanding and has since been simplified.
Further more, it has been documented that the presence of nitric acid in the oxalate
conditioner was responsible for the improvements in bond strengths. Other products
entered the market place were designed to remove dentin smear layer. The
conditioning agents ranged from the chelation of EDTA (Gluma, Bayer) to the
incorporation of maleic acid in a resin primer. (Scotchbond 2, 3m (Dental adhesives)

5
Perdiago and others (1998), found the application of Aqua Prep to dried dentin
surfaces to restore the bond strengths of acetone-based water free dentin adhesives
to the same level as bonding to moist substrates. They have shown that rewetting
the etched dentin with an aqueous HEMA solution re-established the level of bond
strength obtained to moist dentin and severed as an effective means to reopen the
interfibrillar spaces for penetration of resin.
Pilo and others (2001) concluded that pretreatment of etched dentin with either a
disinfectant (2% chlorhexidise gluconate, tubulicid [2% EDTA and 1% benzylkonium
chloride] or rewetting (Aquaprep 35% Hema) may have a positive effect on the shear
bond strength of resin to dentin. Duke and Rhodes (2001) evaluated the effect of
desensitizers (vivadent and Gluma) used as rewetting agents on dentin shear bond
strength.
Vivadent > 5% Glutaraldehyde and 35% polyethylene glycol dimethacrylate
Gluma > Solution of glutaraldehyde and HEMA [Operative dentistry; 2003;28-3;
287-296]

THE IDEAL DENTIN STRUCTURE: (Tencate)

Dentin is the hard tissue portion of the pulp-dentin complex and forms the bulk of the
tooth. Dentin is formed by cells, the odontoblasts, which differentiate from the
ectomesenchymal cells of the dental papillal following an organizing influence
emanating from the cells of dental epithelium. The odontoblasts produce an organic
matrix that becomes mineralized to form dentin.
COMPOSITION OF DENTIN:
70%

Inorganic material

20%

Organic material

10%

Water

Inorganic component consist mainly of hydroxyapatite and the organic phase is type
I

collagen

with

fractional

inclusions

of

glycominoglycans,

Phosphoproteins, glycoproteins and other plasma proteins.

proteoglycans,

STRUCTURE OF DENTIN:
In human teeth, three types of dentin can be recognized.
PRIMARY DENTIN :
Primary dentin forms most of the tooth and outlines the pulp chamber of the fully
formed tooth. The outer layer of primary dentin, called mantle dentin, differs from the
rest of the primary dentin. This layer is the first layer formed by newly differentiated
odontoblasts. It is approximately 150 nm wide and has an organic matrix consisting
of ground substance and loosely packed coarse collagen fibrils. This matrix is slightly
(4%) less mineralized than the rest of the primary dentin.
SECONDARY DENTIN
Secondary dentin is the dentin formed after root formation has been completed.
Secondary dentin has an incremental pattern and a tubular structure though less
regular, forms the most continuous part with that of the primary dentin

TERTIARY DENTIN
Tertiary dentin (also referred to as reactive, reparative, or irregular secondary dentin)
is produced in reaction to noxious stimuli, such as caries or restorative dental
procedures. Unlike primary or secondary dentin, which is formed along the entire
pulp-dentin border, tertiary dentin is produced only by the odontoblasts directly
affected by the stimulus.

PREDENTIN
Predentin is a layer of variable thickness (10 to 47 1-um) that lines the innermost
pulpal portion of the dentin. It is an unmineralized dentin matrix, and consists of
collagen and proteoglycans.
HISTOLOGY OF PRIMARY DENTIN
When the dentin is viewed microscopically, several structural features can be
identified. These include the dentinal tubules, intra-and intertubular dentin, areas of

7
deficient calcification called interglobular dentin, incremental growth lines, an area
seen solely in the root portion of the tooth known as the granular layer of Tomes, and
finally, the cells of dentin, the odontoblasts.
DENTINAL TUBULES
Dentinal tubules are small, canal-like spaces within the dentin filled with tissue fluid
and occupied by odontoblast processes. The dentinal tubules are tapered in outline,
measuring approximately 2.5 m in diameter near the pulp, 1.2 m in the midportion
of the dentin, and 900 m near the dentino enamel junction. In coronal dentin, there
are approximately 20,000 tubules per square millimeter near the enamel and 45,000
per square millimeter near the pulp. This increase in number per unit volume is
associated with a crowding of the odontoblasts as the pulp space becomes smaller.
The terminal part of the tubules branches, resulting in an increased number of
tubules per unit length in mantle dentin. This terminal branching is especially profuse
in root dentin. Dentinal tubules also have lateral extensions that branch from the
main tubule at intervals of 1 to 2 m along its length.
FEATURES OF DENTINAL TUBULES
It is filled with Dentinal Fluid.
It is under constant Pulpal pressure.
Responsible for intrinsic wetness of the prepared Dentin surface.
Connected by lateral branches
No. per unit area on pulpal and superficial surface - 4:1
INTRATUBULAR DENTIN (PERITUBULAR DENTIN)
Around the dentinal tubule is a hypermineralized ring of dentin, which is readily
apparent when non- demineralized ground sections of dentin cut at right angles to
the tubules are examined under the light microscope. This hypermineralized (40%
more than intertubular dentin) collar of dentin, which can also be demonstrated by
electron microscopy, electron microprobe analysis, and soft x-ray film, was originally
called peritubular dentin at the time of its discovery about 30 years ago, and this
term is now widely used.

8
Acid etching removes peritubular dentin. Matrix from the wall of the tubule results in
hybridized resin tag (2-4um)
FEATURES OF PERTIBULAR DENTIN
It is highly mineralized
It is twice as thick as in superficial
Constricts the tubules at the DEJ.
It has got a very delicate organic matrix.
Results in a funnel shaped resin tag.
INTERTUBULAR DENTIN
Dentin located between the dentinal tubules is called intertubular dentin. It
represents the prime secretory product of the odontoblasts and consists of a tightly
interwoven network of type I collagen fibrils, measuring between 50 and 200 nm in
diameter, in which apatite crystals are deposited. The collagen fibrils are aligned
roughly at right angles to the dentinal tubules, and the apatite crystals, averaging
100 nm in length, are generally orientated with their long axis parallel to the collagen
fibril.

The

ground

substance

consists

of

phosphoproteins,

proteoglycans,

glycosaminoglycans, carboxyglutamate-containing proteins, glycoproteins, and some

plasma proteins. During acid etching, mineral content removed in intertubular dentin
(Approx 2-7um) results in formation of resin tag and hybrid layer.
INTERGLOBULAR DENTIN
Interglobular dentin is the term used to describe areas of unmineralized or
hypomineralized dentin that persist within mature dentin. The name describes areas
where the globular areas of mineralization (calcospherites) have failed to fuse into a
homogeneous mass. They are especially prevalent in human teeth in which there
has been a deficiency in vitamin D or exposure to high levels of fluoride at the time of
dentin formation. Interglobular dentin is seen most frequently in the circumpulpal
dentin just below the mantle dentin, where the pattern of mineralization is largely
globular.

INCREMENTAL LINES
Dentin formation proceeds rhythmically, with alternating phases of activity and
quiescence. These phases are represented in formed dentin as incremental lines
that, although often not clearly detectable, can, best be seen in longitudinal ground
sections of teeth. These incremental lines run at right angles to the dentinal tubules
and generally mark the normal rhythmic linear pattern of dentin deposition in an
inward and root- ward direction
Another type of incremental pattern found in dentin is formed by the contour lines of
Owen.As originally described by Owen, the contour lines result from a coincidence of
the secondary curvatures between neighboring dentinal tubules. However, other
lines, having the same deposition but caused by accentuated deficiencies in
mineralization, are now more generally known as contour lines of Owen.
GRANULAR LAYER OF TOMES
When dentin is viewed under transmitted light in ground sections, and only in ground
section, a granular-appearing area, the granular layer of Tomes, can be seen just
below the surface of the dentin where the root of the tooth is covered by cementum.
AGE AND FUNCTIONAL CHANGES
Reparative Dentin
Reparative dentin is formed by the replacement (or) secondary odontoblast in
response to irritation caused by attrition, abrasion, erosion, trauma, dental caries,
some operative procedures and other irritants.
Dead Tracts
This is a type of reaction dentin, which appears to result from irritation of greater
severity. The odontoblast process in the whole length of the injured tubule
degenerates and at the same time is sealed off at the pulpal end by a deposit of
reactionary dentin.

10
In dried ground section of normal dentin the odontoblast processes disintegrate and
the empty tubules are filled with air. They appear black in transmitted and white in
reflected light.
Sclerotic Dentin
Sclerotic dentin results from aging or mild irritation (such as slowly advancing caries)
and causes a change in the composition of the primary dentin. The peritubular dentin
becomes wider, gradually filling the tubules with calcified material, progressing from
the dentino enamel junction pulpally. These areas are harder, denser, less sensitive,
and more protective of the pulp against subsequent irritations. The deposition of
intratubular dentin, as a result of aging or in response to attrition, results in a
progressive reduction in the tubule lumen, and if continued, obliterates the tubule. If
this occurs in several tubules in adjacent areas, the dentin assumes a glassy
appearance. The term used to describe this progressive deposition and obliteration
of the tubule is SCLEROSIS, resulting in sclerotic dentin.

Dentin Characteristics Change With Depth

Both primary and secondary dentin contains tubules. The circumference of the
dentin at the most peripheral part of the crown or root is much greater than that of
the final circumference of the pulp chamber or root canal space this results in the
odontoblasts being much more crowded as they approach their final position, thus
leading to the appearance of a columnar layer of odontoblasts, especially over the
pulp horns. The convergence of odontoblasts towards the pulp creates a unique
structural organization, with functional consequences. The convergence has been
estimated to be 4:1.
The number of tubules per unit area and the radius of the tubules increases in the
direction from the dentino-enamel junction to the pulp, thus the area occupied by
tubule lumina also increases.
Pashley (1984) calculated the area occupied by tubule lumina at the dentino-enamel
junction to be approximately 1% of the total surface area of the dentino-enamel
junction and 22% of the pulp. As this area is occupied by dentinal fluid, which is 95%

11
water. (Pashley 1996), the surface area figures are also approximately equal to the
tubule water content of these regions.
Therefore, the water content or wetness of dentin increases 20 fold from superficial
to deep dentin. This factor has clinical implications, in terms of dentin bonding of
restorative materials to deep dentin the water completes with resin monomers for
surface collagen fibrils (Pashley 1997).

Fluid Flow
In clinical conditions there is an outward fluid flow across exposed dentin in response
to the low but positive pulpal tissue pressure. The composition of this fluid is
uncertain, but must have an ion product of calcium and phosphate, which is above or
near the solubility product constants for a number of forms of Calcium phosphate
(Pashley 1996).
This would in turn lead to the formation of mineral deposits in dentinal tubules which
have many forms (Mjor 1985), as the dentinal fluid moves outwards, larger amounts
of mineral ions are presented to the walls of tubules than would occur in sealed
tubules. Indeed, Shellis (1994) used this principle to reduce the depth of
demineralization in vitro under stimulated caries forming conditions, by using a
supersaturated surrogate dentinal fluid, which was perfused through the pulp
chamber. When examined microscopically, translucent bands resembling sclerotic
dentin were sometimes observed.
Clinically, patients who complain of dentin sensitivity report that a cold stimulus elicits
a greater response than evaporative, tactile or osmotic stimulation. Outward direct
fluid movement (in response to cold) is far more effective in activating pulpal
mechanoreceptors than is the inward movement of fluid.
The Pulpo-Dentinal Complex
Dentin and pulp are embroyologically, histologically and functionally united and there
is much evidence to support the concept of viewing the dentin and pulp as a
functionally coupled unit, which acts as an integrated system.

12

As soon as the tissues, which normally cover dentin, are lost, normal
compartmentalization between the tissues is also lost and they become functionally
continuous. The pulp responds to the stimuli generated by the loss of dentinal
covering, in the short term, by mounting an outward movement of fluid and
macromolecules.The long-term response to the stimulus is the production of tertiary
dentin, which is a biological response to reduce the permeability of the dentin of the
pulp dentin complex.
ACID ETCHING ON ENAMEL:
DEFINITION
The enamel in preparation for a micro mechanical attachment with resin. ( Graham
J.Mount, W.R.Hume)
The enamel surface covered by an organic pellicle, which makes bonding difficult
because of its low reactivity. Etching enamel with phosphoric acid raises the critical
surface tension, increases the bonding area and roughness allowing the hydrophobic
resins to penetrate the porosities of the dry etched enamel. (Aschhiem

dale;

Esthetic Dentistry; 2nd edition)

OBJECTIVES
1. To remove the contaminants.
2. To raise the energy and reactivity of the enamel surfaces.
STEPS IN ACID ETCH TECHNIQUE
ENAMEL PROPHYLAXIS:
Thorough dental prophylaxis for removing material A!ba and plaque is an important
component of the conditioning regime. It has been observed that prophylaxis alone
can double the bond strength,
The prophylaxis pastes, devoid of oils, flavouring agents and fluorides are
recommended for this purpose. After cleaning, the enamel is thoroughly washed with
water, the treatment dried and carefully isolated from oral fluids.

13
APPLICATION OF ETCHANT
Ever since Buonocore used phosphoric acid in the form of liquid or gel alternative
acids and varying etching times. The acid is applied by one of several means
including a cotton pellet brush or mini sponge.
Beginning with Buonocore's use , 85% phosphoric acid have been used to etch
enamel, (Sturdevant). Application of 50% phosphoric acid for 60 secs result in the
formation of a mono calcium phosphate dihydrate precipitate that can be rinsed off.
However, 20% phosphoric acid may create a dicalcium phosphate dihydrate
precipitate that cannot be easily removed and may interfere with adhesion.
Sliverstone found that the applications of 30% to 40% phosphoric acid resulted in
very retentive enamel surfaces.
Recent studies has shown that shorter etching time produce the same adhesive
strength than the originally suggested 60 seconds ( Journal of operative dentistry
1986; 11:111). Morphologic studies has shown significant differences in etching
results based on the viscosity of etchant.
Liquid or thin gel produced similar etch pattern than thick gel but thin gel seemed to
have

the

best

defined

etched

pattern

Journal

of

prosthetic

dentistry

1989;65:522).Etching for too long produces insoluble reaction products and a weak
bond. An Etching time of 60 seconds was originally recommended for permanent
enamel using 30% to 40% phosphoric acid. (Sturdevant).
WASHING : (Vimal sikiri)
Following acid application for a stipulated period, the area is thoroughly washed for
10-15 seconds to remove the reaction products of acid and mineral hydroxy apattite.
Studies have concluded a 2 to 5 secs rinse of the tooth surface should sufficiently
cleanse gel- etched enamel resulting in adequate shear bond strength.( Journal of
prosthetic dentistry 1989 ; 62 : 522). Rinsing for 1 second from a smooth enamel
surface resulted no micro leakage ( Ronald E Goldstein)
DRYING :
The teeth are thoroughly dried with a oil free compressed air. An effectively etched
surface on drying gives a matt white or frosted appearance. Even a minor exposure

14
to saliva, blood or oil can restrict the potential for resin tag formation and bonding. All
measures should therefore be taken to prevent any contamination. If accidental
contamination occurs, the procedure should be repeated.
EFFECTS OF ETCHING ON ENAMEL:

Removes residual pellicle exposure to the inorganic crystallite component of

enamel.

Creates a porous layer with the depth of the pores ranging from 5-10 m

Increases as the wettublity and surface area of the enamel substrate.

Raises the surface energy of enamel with creation of reactive polar sites.

PATTERN OF ETCHING:
Silverstone et al (1975) studied the morphological changes in SEM produced on the
acid etched enamel surface. Exposure of human enamel to conditioning solutions
produces 3 basic etching patterns.(Robert G. Craig and John M. powers)
Type I: (Preferential prism center etching)
Etching pattern involves the preferential removal of enamel prism cores with prisms,
peripheries remaining relatively intact, resulting in a honey comb appearance. The
average diameter of the hollowed prism core is measured as about 3m. This is the
most commonest type of etching pattern.
Type II: (Preferential prism pheriphery etching)
The peripheral regions of the prism are dissolved preferentially, leaving the prism
cores relatively intact, resulting in a cobblestone appearance.
Type III: (Mixed)
Etching pattern is less distinct and includes areas resembling type I and type II
patterns as well as regions in which the etching pattern appears unrelated to prism

15
morphology. This type of etching in general is associated with the presence of
prismless enamel and appears as a generalized surface roughening.
Alternative acids have been tried as enamel etchants; mainly phyruvic acid and
sulphuric acid. 2% sulphuric acid used for 30 seconds has shown to be as effective
as phosphoric acid, where as higher sulphuric acid concentrations produce heavy
crystal deposits which interfere with the bonding and cannot be washed away easily.
With the present concept of total etch techniques, acids such as 10% maleic acid,
10% citric acid, 10% phosphoric acid, 2.5% oxalic acids and 2.5% Nitric acid are
used to etch enamel and dentin simultaneously (Quintessence !nt 2002; 33; 213224)
FACTORS AFFECTING ETCHING ON ENAMEL:
Time:
Increase time application
High fluoride content and primary teeth require longer etching time. Etching for too
long produces insoluble reaction products and a week bond (Aschhein dale;
Esthetics dentistry).
Shorter etching time:
C.J. Guba et al (1994) highlighted that etching times and etchant consistency were
not critical to enamel bond strengths, it yields acceptable bone strength, conserves
enamel and saves time.
Acid concentration:
An interesting and important phenomenon is the existence of an inverse relationship
between the etching effect of phosphoric acid and it's concentration. The
concentrations of acid, producing consistent, more evenly distributed relatively deep
etch pattern, appear to be in the range of 30 to 50%.

16

CONDITIONING OF DENTIN
Etching of enamel and dentin together for 15 secs called as Total etch or Unitech is
the most successful way of managing by smear layer. It was introduced by
Fusuyama et al in 1979 and it is now commonly practiced. Acid 35-37% phosphoric
acid.
Acid etching of dentin removes the mineral phase and increases the porosities of
these tissues enormously. In superficial dentin, the surface of dentin changes from
one in which only 1% of surface area is porous (the porosity resulting from the
presence of dentinal tubules) before etching to a condition in which 13.4% of the
surface area consisting of water filling tubules that can serve as avenue for
infiltration of suitable monomers.
The remaining 86.6% of the surface consists of demineralized intertubular dentin that
has spaces around delivery collagen fibril. Thus acid etching converts a solid surface
into a porous non-solid surface.
ACID ETCHED DENTIN

ADVANTAGES
1. Dentinal Tubules opened
2. Collagen exposed in the
intertubular dentin

DISADVANTAGES
Surface energy is lowered.

Before etching
1% Surface area
(Dentinal Tubule)
Intertubular Dentin

17
After Etching
13.4% of surface area
(Water Filled tubule) al
Tubule)
86.6% of surface area
demieneralized dentin

The surface energy of the substrate is low and use of primer increases the surface
energy to provide a good bonding.
Factors affecting the depth of dentin etching and monomer infiltration.

Concentration of acid

Duration of etching

Type of Preparation

Polymer Thickened or silica thickened.

Concentration of acid used

Ideal concentration of phosphoric acid used 35 to 37%

> 40%

Calcium salts are less dissolved

Etch patterns with poorer definition

< 27%

Calcium salts are less dissolved

Cannot be easily removed

Duration of etching
Ideal during of etching 15-20 Sec.
Increased Duration
Type of Preparation
Greater collapse of collagen due to
Thickening
agents used are
collagen deneturation
1. Silica Gel
2. Polymers
Decreased
Silica Gel - monomer
Higher pHinfiltration
(Alkaline)
polymer - Decrease pH(acidic)
Increased depth of etching

Decreased Duration
Insufficient depth of etching

18

MICROSCOPIC APPEARANCE OF ETCHED ENAMEL

Clinically a uniform dull appearance is an indication that the tooth surface has been
adequately etched.
Silverstone in 1974 showed that etched enamel surface under polarized light
resulted in 3 zones.
1. Etched Zone
2. Qualitative Zone
3. Quantitative Zone
1. Etched Zone
This is the narrow zone of enamel at about 10m in depth, that is removed by
etching. The fully reacted mineral crystals are removed resulting in the exposure of
more reactive surface. This increased surface area and a reduced surface tension
allows resin to wet in the etched surface more readily.
2. Qualitative Zone:
This zone is about 20m in depth and it is rendered porous during acid etching of the
enamel when identified qualitatively using polarized light.
3. Quantitative Zone:
This third zone is almost up to 20m depth. It is qualitatively indistinguishable from
adjacent enamel and can be detected with quantitative polarized light. In human
enamel, the pores may be spherical, elongated or sometimes as large chamber that
are connected to smaller channels called ink bottle systems.

19
Microscopic appearance of etched dentin
High resolution scanning electron microscopy reveals 3 distinct zones within the
demineralized dentin.
Upper zone - consists of residual smear layer or denatured collagen and residual
silica particles. (for silica containing gel)
Intermediate Zone - consists of randomly oriented collagen fibres separated from
each other by uniform spacing.
Bottom zone - otherwise referred to as Hiatus has fewer collagen fibres and mineral
inclusion. This hiatus was observed in all polymer thickened specimens, in 90% of
specimens etched with aqueous phosphoric acid and 60% of specimens etched with
silica thickened gels.
CHALLENGES IN DENTIN BONDING: [Sturdevant)
Bonding to enamel is a relatively simple process, without major technical
requirements or difficulties. Bonding to dentin, on the other hand, presents a much
greater challenge. Several factors account for this difference between enamel and
dentin bonding. Whereas enamel is a highly mineralized tissue composed of more
than 90% (by volume) hydroxyapatite, dentin contains a substantial proportion of
water and organic material, primarily Type I collagen. Dentin also contains a dense
network of tubules that connect the pulp with the dentin-enamel junction. The tubules
are lined by a cuff of hypermineralized dentin called peritubular dentin. The lessmineralized intertubular dentin contains collagen fibrils with the characteristic
collagen banding. The intertubular dentin is penetrated by submicron channels,
which allow the passage of tubular liquid and fibers between neighboring tubules,
forming intertubular anastomoses.
Dentin is an intrinsically hydrated tissue, penetrated by a maze of 1 to 2.5 um
diameter fluid-filled dentin tubules. Movement of fluid from the pulp to the dentin
enamel junction is a result of a slight but constant pulpal pressure.
Dentinal tubules enclose cellular extensions from the odontoblasts and therefore are
in direct communication with the pulp. Inside the tubule lumen, other fibrous organic
structures (the lamina Limitans) can be observed, these substantially decrease the
functional radius of the tubule,

20

The relative area occupied by dentin tubules decreases with increasing distance
from the pulp. The number of tubules decreases from about 45,000 per mm 2 close to
the pulp, to about 20,000 per mm2 near the dentin-enamel junction.The tubules
occupy an area of only 1% of the total surface near the dentin-enamel junction,
whereas they comprise 22% of the surface close to the pulp. The average tubule
diameter ranges from 0.63 m at the periphery to 2.37 m near the pulp. Adhesion
can be affected by the remaining dentin thickness after tooth preparation. Bond
strengths are generally less in deep dentin than in superficial dentin. Nonetheless,
some dentin adhesives, such as those based on the 4-META monomer, do not seem
to be affected by dentin depth.
Whenever tooth structure is prepared with a bur or other instrument, residual organic
and inorganic components form a "smear layer" of debris on the surface. The smear
layer fills the orifices of dentin tubules (forming smear plugs) and decreases dentin
permeability by up to 86%. The composition of the smear layer is basically
hydroxyapatite and altered denatured collagen. This altered collagen may even
acquire a gelatinized consistency as a result of the friction and heat created by the
preparation procedure. "Submicron porosity of the smear layer still allows for
diffusion of dentinal fluid.
The removal of the smear layer and smear plugs with acidic solutions may result in
an increase of the fluid flow onto the exposed dentin surface. This fluid may interfere
with adhesion, because hydrophobic resins do not adhere to hydrophilic substrates
even if resin tags are formed in the dentin tubules.
Several additional factors affect dentin permeability. Besides the use of
vasoconstrictors in local anesthetics,which decrease pulpal pressure and fluid flow in
the tubules, other factors such as the radius and length of the tubules, the viscosity
of dentin fluid, the pressure gradient, the molecular size of the substances dissolved
in the tubular fluid, and the rate of removal of substances by the blood vessels in the
pulp affect permeability. All of these variables make dentin a dynamic substrate and
consequently a very difficult substrate for bonding.

21
OBJECTIVES:
(ESTHETICS DIRECT ADHESIVE RESTORATION ON FRACTURED ANTERIOR TEETH)

According to pashley acid etching of vital dentin has the following objectives.

To remove the intrinsic smear layer to facilitate adhesion to the under lying
dentin matrix.

To expose the peritubular and the inter tubular dentin.

To clean the dentin surface removing biofilms.

To demineralize the surface dentin matrix to permit the adhesive system to

infiltrate into the intertubular dentin.

EFFECTS OF ACID CONDITIONED DENTIN

The principal effects of conditioning of dentin may be classified as

Physical changes

Chemical changes

Physical changes
Increases or decreases in the thickness and morphology of smear layer changes in
the shape of dentinal tubules.
Chemical changes
a. Modification of the fraction of organic matter
b. Decalcification of the inorganic portion
EFFECTS OF ACID CONDITIONS:
In an experiment on monkey, dentin wall demineralized with a phosphoric acid jelly
etchant for 60 secs was completely re-mineralized after 4 months. This results
indicates that etching did not result in deleterious effect upon either the collagen
fibers or the odontoblast processes, because the presence of collagen fibers
maintaining their proper cross bonded structure as a base for apatite crystals to
attach to and of the vital odontoblast processes to supply the calcium phosphate
from the pulp is essential for remineralization of dentin.

22
A.J.Gwinnett and M.D.Jendresen (1978) have concluded from their experiments and
observations that the surface of acid conditioned eroded dentin is significantly
different from that of acid conditioned normal dentin. They further observed that the
depth of penetration of resin is also less in acid treated eroded dentin where many
tubules remain partially occluded by intratubular insoluble deposits.
Ruse and Smith (1991) found by X-ray photo electron microscopy that when
common conditioning agents were used, the outermost surface contains only 10% or
less of the calcium and phosphorus which is present initially. They concluded that the
treatment of dentin with acidic conditioners leaves the surface so depleted of calcium
and enriched by organic residues mat subsequently placed bonding systems should
be based upon agents able to interact with organic components of dentin. Bonding
agents that rely on chelation to calcium are unlikely to be successful when applied to
acid etched dentin unless they penetrate into the demineralized matrix to reach
normal, mineralized dentin.
Acid etching of dentin is not harmless but represents one more source of acute
irritation to the pulpo dentin complex in addition to the vibratory, thermal, mechanical
and evaporative stimuli that accompany cavity preparation. However, it is not as
irritating as has been previously thought.
Nakabayashi (1982) introduced the concept of hybridization. The technique consists
of applying an acid, ranging in concentration from 10% to 30% to the surface of
dentin. Within 15 minutes the acid selectively dissolves away the inorganic
component of the dentin to a depth of 5 to 10 microns. It then flows in the dentinal
tubule for up to 100 microns at which point it diffuses laterally into the peri-tubular
dentin for up to 10 microns.
As in the previous case the calcium component is selectively eliminated. Then these
spaces are replaced by an insoluble resin component that completely encapsulates
all exposed collagenous fiber. He also reported that dentin conditioning by citric acid
containing ferric chloride followed by a dentin bonding agent containing 4 META was
effective method of dentinal bonding.

23
Concerning the bonding mechanism, he proposed that diffusion and impregnation of
monomers into the subsurface of pretreated dentinal substrate and their
polymerization, creating a hybrid layer of resin reinforced dentin. This newly formed
hybrid layer may be thought of as an admixture of polymer and dentinal components,
creating a resin dentin composite. This technique not only enhances the shear bond
strength of the resin to the dentin but also increases the potential against micro
leakage and postoperative sensitivity.
Nakabayashi (1985) suggested that the acidic treatment partially demineralized a
zone of the dentin near the surface, facilitating an infiltration process of compatible
monomers. The polymerized resin forms a reinforced zone of dentin on which a resin
based restorative material can be bonded. The bond strength is not dependent upon
interlocking at the dentinal tubules.
Kurosaki et al (1987) found that etching of dentin of the clinical cavity floor allows the
chemically adhesive composite resin to produce resin tags of tapered, cylindrical or
tubular form as well as impregnated dentinal layers. These changes will considerably
improve the bond strength as well as the tubule aperture seal.
CONDITIONING OF DENTIN (Vimal K.Sikri)
Conditioning of dentin may be done by several means
1) Chemical
a. Acids
b. Calcium chelators
2) Thermal
a. Lasers
3) Mechanical
a. Abrasion

Conditioning of dentin is defined as an alteration of the dentin surface including the

smear layer with the objective of producing a substrate capable of micromechanical
and possibly chemical bonding at a dentin adhesive. The principal effects of
conditioning on dentin can be physical or chemical. Physical effects are the

24
increases or decreases in the thickness and morphology of the smear layer and also
the dentinal tubules whereas chemical effects are modifications of the fraction of
organic matter and decalcification of the inorganic portion. Conditioning can be
performed by chemical, thermal or mechanical means.
CHEMICAL CONDITIONERS
They remove the smear layer and expose a micro porous scaffold of collagen fibrils
thus increasing the microporosity of intertubular dentin. Because this collagen matrix
is normally supported by the inorganic dentinal fraction, demineralization causes it to
collapse. On the intertubular dentin the exposed collagen fibrils are randomly
oriented and are often covered by an amorphous phase with relatively few micro
porosities and variable thickness.
Etchants thickened with silica leave residual silica particles deposited on the surface,
but the silica does not appear to plug the intertubular microporosities. Sometimes
fibrous structures probably remnants of odontoblastic processes are pulled out of the
tubules and smeared over the surface.
With aggressive acid etchants / hypertonic acids the acid may tend to pull the
collagen fibers away from the intact dentin / unaffected dentin leaving a submicron
space termed as hiatus. With increasing aggressiveness of the conditioning agent a
circumferential groove may be formed at the tubule orifice separating a cuff of
mineralized peritubular dentin from the surrounding intertubular dentin. Alternatively
the mineralized peritubular dentin may be completely dissolved to form a funnel
shape.
Historically several acids have been researched as dentin conditioners. These
include hydrochloric, oxalic, pyruvic acid, phosphoric, citric and nitric acids. The
hydrogen ions from these acids diffuse into the dentin while etching. If one assumes
that the self diffusion coefficient of hydrogen ions in free solution at room
temperature is 1 x 10-6 cm2 / sec, one can calculate the distance that the hydrogen
ions can diffuse into dentin as the square root of the product of the diffusion
coefficient of hydrogen and time.

25
Moreover the hydrogen ions don't diffuse as much as calculated as their diffusion is
restricted by dentin. The surface reactions are violent as carbonate is converted to
carbon dioxide and as calcium and phosphate is liberated. These products may be
liberated faster than they can diffuse from the site leading to formation of reaction
products that may limit further penetration of protons. Further the hypertonic
solutions when osmotically draw the fluid from the dentin towards the surface could
restrict the inward proton diffusion.
The removal of the smear layer and de mineralization of the dentin matrix may
facilitate bonding through a number of mechanisms. They are:
1. Removal of loose smear layer debris and exposure of dentin matrix.
2. Exposure of collagen fibrils and their epsilon - Ammo groups that may catalyze
HEMA polymerization.
3. Exposure of intact collagen that serves as a scaffold for the creation of resin
collagen hybrid layer.
Phosphoric acid
It was the first dentin conditioner that was successfully used to remove the smear
layer, etch the dentin and restore it with adhesive composite resin by Fusayama and
Others (1979).

This helps by removing the surface dentin, leaving a clean, well-

defined etching pattern where the tubules are enlarged into funnel shape.
Phosphoric acid is the acid of choice currently for the etching purpose. However
controversy remains about the optimal concentration of H 3P04. The most widely used
concentrations used in clinical practice exceed 30% H 3P04.
Chow and Brown (1973) demonstrated that the application of H 3P04 solutions greater
than 27% resulted in the formation of mono calcium phosphate monohydrate, which
is readily soluble and would be completely washed away in the clinical situation. If
the reaction product is not completely removed after the etching procedure it may
interfere with the bonding of composite resins to etched enamel / dentine surfaces.
When H3P04 was used in concentrations less than 27% dicalcium phosphate
dihydrate was formed which is less soluble, and it may interfere with the bonding of
composite to enamel.
Total etch / all etch technique

26
Fusayama pioneered the research of total etching establishing the protocol for
simultaneous etching of dentin and enamel with phosphoric acid in 1979.
Kurarya's original Clearfil New bond system accomplishes the total etch using 37%
phosphoric acid for 60 seconds. Bisco system uses 10% phosphoric acid for 15
seconds in all etch technique. A 10% solution appears to result in a slightly better
bond strength than higher concentrations (Kanca 1991).
Nitric acid
It is stronger than phosphoric acid.
a. Easily removes the smear layer
b. Used in concentration of 2.5%, it causes tunneling of the orifices of dentin to a
depth of 5 m in 40 seconds. Nitric acid conditioners are highly adhesive and
provide good tubule seals.
Citric acid
10% citric acid is used for the purpose of removing the smear layer. It has been
reported by Nakabayashi (1989) that such treatment tends to lower the porosity or
permeability of the demineralized surface, possibly by denaturing the collagen. The
10% citric acid plus 3% ferric chloride combination was developed by Nakabayashi
(1984).The divalent cations seem to stabilize the dentin matrix during its
demineralization by citric acid. This combination was found to be particularly effective
for methacrylate based adhesives containing 4-META.
Ferric ions appear to be necessary since the citric acid alone yields poor results with
this system. The higher bond strengths of 4 Methacryl oxyethyl trimellitic
anhydride/methyl methacrylatetetra butyl borane oxidized (4-META/MMA-TBB)
products conditioned by 10% citric acid and 3% ferric chloride solution can also be
achieved by substituting cupric chloride for the ferric ions. Eg. Super bond C and B
Metabond and Amalgambond.
10% citric acid and 20% calcium chloride. This has been introduced by Kuraray in
the latest generation of Clearfil liner bond system.

This high concentration of

calcium may stabilize collagen during surface etching. It also decreases the extent of

27
the demineralization of hydroxyapatitie by a common ion effect. Here the depth of
decalcification is about 8 microns compared to the phosphoric acid etching which
results in 16-micron depth of decalcification (Inokoshi and Other 1989).
Pyruvic acid
Pyruvic acid and pyruvic acid buffered with glycine have been reported to
satisfactorily acid etch both enamel and dentin (Asmussen and Munksgaard 1988).
When using the Gluma bonding system Glycine was used to adjust the pH and
perhaps to facilitate polymerization reactions.
Calcium Chelators
Chelators are used to remove the smear layer without decalcification or significant
physical changes to the underlying substrate as opposed to the strong acid etchants.
EDTA
Brannstrom's (1980) concerns that bacteria might be incorporated into smear layers
and infect the dentin surfaces of cavities led him to develop a dentin conditioners
containing 0.1% Ethylene diamine tetracetic acid and 0.15 Benzalkonium chloride as
a surface active disinfectant. This agent was marketed under the name "Tubulicid".
It is scrubbed on the surface of the smear layer for a few seconds and then left
passively for another 60 seconds followed by additional scrubbing. Such treatment
removes the smear layer and generally leaves the smear plug intact. The dilute
solution of EDTA removes some calcium that is thought to be important in the
mechanism of bonding. This was probably responsible for the fall in bond strength.
EDTA was developed for use in the Gluma system by Munksgaard and Asmussen in
1984. It removes the smear layer but does not form significant surface concavity nor
are the funnel shaped changes associated with phosphoric acid evident. The smear
plugs in the dentinal tubules are not fully removed by 30 seconds application of the
conditioners.
Thermal conditioning:
The recent trend is to use lasers in conditioning of dentin. These may serve as a
potential alternative to acids for conditioning of dentin. It is speculated that lasers

28
cause recrystallization of dentin resulting in a fungi form appearance that contributes
to increased micro retention or possible chemical adhesion of a restorative material
to the tooth structure. Further, they remove the organic elements, leaving behind an
apatite substance in a new alpha form. The carbonized black spot that results after
lasing is easily washed off with water. Studies have confirmed increased bond
strengths with lased dentin compared to those with unlased dentin.
FACTORS AFFECTING DENTIN CONDITIONING
Time
Duration of application
Brannstrom and his colleagues achieved good bonds of resin to dentin using a fivesecond application of 37% phosphoric acid (Brannstrom, Johnson and Nordenvall,
1979). Perhaps 30 seconds of 5% Phosphoric acid would have been equally
effective.
The same agent may remove the smear layer in five seconds, can cause
considerable decalcification if left in place for 30 seconds and pulpal damages may
begin to appear while using less concentrated acids with higher molecular weights
and shorter time intervals.
Tagarni and Others (1999) Compared a series of acids for their ability to clear
tubules of smear layers and smear plugs by measuring the increase in the hydraulic
conductance of smear layer-covered dentin as a function of etching time.
Presumably, the same amount of demineralization was occurring in intertubular
dentin. Blosser and others (1989) reported that etching normal dentin for 20-30
seconds with 2.6% nitric acid was as effective as it was at removing the smear layer
and opening up dentinal tubules as 50 or 60 seconds of etching.
Etching times may also need to be adjusted when attempting to etch sclerotic dentin
such as excavated carious dentin or abraded cervical root surfaces. Dluke and
Lindemuth (1990-1991) have shown that carious dentin is much less etchable and
more resistant to acid attack than normal dentin.

29
The application of strong acids (i.e ferric chloride/citric acid or phosphoric acid) to a
dentin surface for 15 secs significantly gave higher bond strength values than 60
secs applications. Applying weak acids (maleic acid or EDTA) to dentin for 15 secs
significantly decreased the bond strength values compared to 60 secs applications.
Shortening of application time of conditioning agents :
In 1977, Brannstrom and Nordenvall noted demonstrable difference between
dentinal surfaces etched for 15 seconds or two minutes and recommended shorter
etching times. This appeared to be the beginning of a new phase in dentin
conditioning.
Concentration:
Y. Benderli (1999) studied the effect of various dentin acid treatment on tensile bond
strength of composite to dentin. He concluded that the application of strong acids
such as ferric chloride or phosphoric acid to dentin surface for 15 secs, gave
significantly higher bond strength values than for 60 secs application. He also stated
that when weak acids such as maleic acid was applied for 15 secs to dentin showed
decreased bond strength values compared with 60 secs application. This is because
weak acids remove the smear layer after an increase in the etching time.
On the other hand the strong acids remove the smear layer in 15 secs. When
applied for a long time (60 secs.), they removed both smear layer and peritubular
dentin.
Effect of additives
Additives to the acid solution can affect the rate of removal of smear layer and plugs.
Addition of 55% HEMA to 2.5% maleic acid more than double the time required to
reach maximum permeability even though the measured pH is the same.
This might be explained by absorption of HEMA on the Hydroxyapatitie crystals,
thereby protecting them from dissolution. Permeability has also been shown to
decrease when Aluminium or ferric oxalate is added to nitric acid conditioning
solution.

30
Viscosity
The viscosity of the solutions used to etch has a significant effect on the amount of
demineralization. Many etchants are purposely thickened to improve handling and
limit their distribution on teeth. However, free diffusion slows down as viscosity is
increased so that it gets more etching time than liquids.
According to study conducted by C.J. Guba (1994), when three etchants of different
viscosities were compared under the scanning electron microscope, the liquid and
thin gel produced a more even etch pattern than a thick gel. In addition the thin gel
appeared to produce the most well defined pattern of three conditioners.
Molecular weight
An other important variable is the molecular weight or size of the etchant, since
diffusion varies inversely with the molecular weight, while this does not vary much for
many acids. (Molecular weights: nitric acid, 63; phosphoric acid. 98; citric acid, 192).
It is more significant with polyacrylic acids, which can have molecular weights that
vary from 5000 to 25000 or higher, which decreases their diffusion coefficients. If
they were also viscous, then both effects would summate to limit their etching
effects.
ROLE OF THE HYBRID LAYER [STURDEVANT]
The role of the hybrid layer in dentin bonding is somewhat controversial. Data from
one vitro study indicated that resin infiltration or "hybridization" of the dentinal tubules
and intertubular dentin accounts for a substantial proportion of the bond of resin to
dentin. On the other hand, data from another study suggested that the collagen layer
offers no quantitative contribution to the interfacial bond strength. Studies of various
adhesive systems report different results. A study with Prime and Bond 2.1 (Dentsply
Caulk, Milford, Del-aware) indicated that the removal of collagen fibers may actually
increase bond strengths of resin to dentin. Studies with One-Step (Bisco, Inc.,
Schaumburg/ Illinois) indicated that the hybrid layer might not play any important role
in the establishment of bond strengths. For a multi bottle adhesive system, All-Bond
2 (Bisco, Inc., Schaumburg, Illinois), one study reported that the presence or
absence of the hybrid layer did not affect fracture toughness of resin-dentin

31
interfaces. In the case of All-Bond 2, a different mechanical behavior of the adhesive
interface would be expected. The Young's modulus of the adhesive resin is 1.8 GPa,
while the Young's modulus of the All-Bond 2-infiltrated hybrid layer was estimated to
be 3,6 GPa. Dentin has a Young's modulus in the range of 11 to 18 GPa. Therefore
the presence of the collagen layer would presumably allow for the establishment of a
stress-relieving layer at the interface.
A study using a self-etching primer demonstrated that dentin bond strengths did not
vary from 1 day to 6 months to 1 year in teeth subjected to occlusal function. It also
showed that porosity in the hybrid layer increased significantly at 1 year, due to loss
of resin between the collagen fibers. Since these results were obtained with a hybrid
layer being created by a self-etching primer, they cannot be generalized to total-etch
adhesives. However, they do support the theory that collagen may play an important
role in the strength of the resin-dentin interface.
For most dentin adhesives, the ultramorphologic characterization of the transition
between the hybrid layer and the unaffected dentin suggests that there is an abrupt,
shift from hybrid tissue to mineralized tissue, without any empty space or pathway
that could result in leakage. The demarcation line seems to consist of hydroxyapatite
crystals embedded in the resin from the hybrid layer.
ROLE OF WATER IN THE BONDING PROCESS (Vimal Sikri)
When prepared dentin is acid etched, the smear layer and plugs are removed and
the underlying 2-7 m layer of dentin is demineralized. Solutions used for etching are
generally acidic and contain water to ionize the acids and dissolve the extracted
minerals. Post-etching rinsing with water removes this dissolved mineral and leaves
a demineralized dentin surface covered with water. About 70% the demineralized
dentin is occupied with water areas from where the mineral has been removed. This
water is responsible for maintaining the collagen in an expanded state and thereby
preserving the spaces needed for infilteration of resin. In other words, water acts as
a plasticizer for collagen and keeps it in a soft state. If the dentin is dried and
exposed to air, water evaporates leaving collagen in a collapsed stiffened state
because of surface tension forces. This reduces the ability of the subsequently
applied agents to penetrate collagen web. Also when the collagen fibrils are brought

32
closer, secondary forces start becoming active between adjacent peptide chains in
the collagen triple helix, which is not possible when water is present, thereby
increasing the stiffness or modulus of elasticity for collagen. Total demineralization
with air drying results in as much as 65 volume percent shrinkage. Upon addition of
water, the collagen network re-expands to about 100 percent of its original volume. It
is believed that a critical water concentration exists that prevents the collapse of
network or allows re-expansion of the dried dentin over a period of 10.30 seconds.
When non-aqueous primers are applied on to dry dentin, the collagen is not rewetted
by water and the network continues to exist in a collapsed stiffened state with little or
no resin penetration because of the reduced porosity around collagen fibrils. Instead
the resin is limited to the surface of collapsed layer. On the other hand when water
based primers are applied to air dried, shrunken and demineralized dentin, two
events may occur
(i)

If the water concentration of the primer is low, water soluble resin monomer
and/ or organic solvent will stiffen the collagen meshwork faster than the water.
It can plasticize the collagen and it will not completely re-expand.

(ii)

If the water content of the primer is large enough to plasticize the collagen
faster than the resin-solvent, stiffens in the hydrophilic resin monomers and
infilterate the network as it is gradually expanding. As a result more complete
penetration can be expected with this self rewetting effect of water based
primers used on dry dentin.

Excessive water in the primer should be avoided as it dilutes the monomer

concentration drastically. In dry bonding technique, water free acetone based
primers are used, they do not effectively infiltrate the exposed collagen network
because of absence of water, forming the so called hybridoid regions. Well-infiltrated
areas under these primers are seen to be more electron and found only superficially
along the walls tubules and along the course of their lateral branches.
When the dentin is kept moist, the collagen network is maintained in an expanded
state and the inter fibrillar spaces are left open. Bonding to this moist surface could
be efficient only if water within the dentin is completely eliminated and replaced by
monomers during subsequent priming step. An effective wet bonding technique
advocates use of primers that contain hydrophilic resin monomers dissolved in water

33
miscible organic solvents like acetone and ethanol. On application of such primers
on wet dentin, the water from it diffuses into the organic solvent, while the latter
diffuses into the demineralized dentin matrix and tubules carrying with it the
polymerizable monomers. The water is hence gradually lost as the solvents and
resin monomers move further around the collagen fibrils. This probably explains the
better bonding ability in the wet bonding technique (Gwinnett, 1992 and Kanca,
1992). If the water inside the collagen network is not completely displaced,
polymerization of resin inside the hybrid layer may be affected or the remaining
water will compete for space with resin inside the demineralized dentin. When the
water from dentin is not completely removed by hydrophilic monomer, the
phenomenon is referred to as over-wetting phenomenon. In such overwet
conditions, excess moisture decreases the concentration of organic solvents in the
primer, thereby lowering the solubility of monomers. The monomers are present in
the form of globules over the water layer. This is more common in the dentin tubules
where high content of water is present than in the intertubular dentin. They may
present as 'blister like' structures on the dentin surface with water being trapped
beneath the resin layer. Many resin globules have been demonstrated inside the
water droplets as well as tubules. An interesting feature occurred when the tubule
orifice was blocked with water. No resin tags formed but several globules were
present in the lumen. It is concluded that a critical amount of water is prudent for
good bonding but an over-wet condition decreases bond strength by lack of resin
tags and formation of blister like structures at the interface.
The primer solvent should be either water or water miscible agent. The commonly
used solvents are:

Acetone (used in Prime and Bond NT, Bisco One step)

Ethanol (used in Optibond solo, 3M Single bond)

Water (used in Scotchbond Multipurpose Plus)

Acetone has a relatively high vapor pressure value (184 mm Hg at 20"C) compared
to ethanol (43.9 mm Hg at 20C) and water (17.5 mm Hg at 20C). A higher vapor

34
pressure will allow the solvent to evaporate more easily. As the solvent evaporates,
the viscosity of the dentin bonding agent increases, which decreases the ability of
the bonding system to penetrate around the exposed collagen fibers and the opened
dentinal tubules consequently inhibiting the proper bond formation.
DENTIN PERMEABILITIES
Permeability refers to the ease with which a substance can move into or across a
diffusion barrier. There are two types of dentinal permeabilities.

Transdentinal
(Movement of fluid within tubules)

Intratubular
(Fluid transport from surface to
tubule)

Constant Wetness of surface

Resin has to permeate

Formation of resin tag.

Outward fluid movement from pulp

(Pulpal pressure)

Primer

Increase the surface energy of

the substrate

Better Wetability of the adhesive

resin

MOIST VERSUS DRY DENTIN SURFACES

Earlier, after acid etching, the cavity was rinsed with water and dried with air to
remove the excess water. But this can collapse the collagen fibril network.
Acid etched dentin

35

Air dried

Collapse of collagen

No hybrid layer

Moist

Over wet

Collapse maintained

Swelling of collagen

Optimal hybrid layer

Lesser space available

for resin penetration

John Kanca and Gwinett introduced the Moist bonding technique where in the
etched dentin is not dried before the application of the bonding agent. The surface is
blot dried with the help of blotting paper or tissue, only to remove the excess water.
The presence of water within the collagen fibres, prevents it from collapsing.

Dry vs. Moist Bonding : [STURDEVANT]

Vital dentin is inherently wet, therefore, complete drying of dentin is difficult to
achieve clinically. Water has been considered an obstacle for attaining an effective
adhesion of resins to dentin. With that in mind, research has shifted toward
development of dentin adhesives compatible with humid environments. Most newer
adhesives combine hydrophilic and hydrophobic monomers in the same bottle,
dissolved in an organic solvent such as ethanol or acetone. The "wet-bonding"
technique prevents the spatial alterations (i.e., collagen collapse) that occur upon
drying demineralized dentin. Such alterations may prevent the monomers from
penetrating the labyrinth of nanochannels formed by dissolution of hydroxyapatite
crystals between collagen fibers. The use of adhesive systems on moist dentin is
made possible by incorporation of the organic solvents acetone or ethanol in the
primers or adhesives. Because the solvent can displace water from both the dentin
surface and the moist collagen network, it promotes the infiltration of resin
monomers throughout the nanospaces of the dense collagen web. The "wet

36
bonding" technique has been shown repeatedly to enhance bond strengths because
water preserves the porosity of collagen network available for monomer
interdiffusion. If the dentin surface is dried with air, the collagen undergoes
immediate collapse and prevents resin monomers from penetrating.
The clinician must be aware that pooled moisture, should not remain on the tooth,
because excess water can dilute the primer and render it less effective glistening
hydrated surface is preferred. Many clinicians, however, still dry the tooth preparation
after rinsing away the etching gel to check for the classic etched enamel
appearance. Because it is clinically impossible to dry enamel without simultaneously
drying dentin, the dentin collagen collapses easily upon air- drying, resulting in the
closing of micropores in the exposed intertubular collagen. For acetone-based,
water-free dentin bonding systems, the etched dentin surface must be rewetted
before applying the adhesive. Rewetting the dried etched dentin with water or with
aqueous rewetting agents has been demonstrated to restore bond strength values
and to raise the collapsed collagen network to a level similar to a "wet bonding"
technique. Some authors have suggested that the inclusion of water in the
composition of some adhesives may result in rewetting of the collagen fibers in areas
that are not left fully moist, thus opening the interfibrillar spaces to the infiltration of
the priming resin. Therefore the simultaneous inclusion of both an organic solvent
and water may be fundamental for the best infiltration of some adhesives into
demineralized dentin. This could result in a less technique-sensitive procedure.
When etched dentin is dried using an air syringe, bond strengths decrease
substantially, especially for acetone and ethanol-based dentin adhesive systems
when water is removed, the elastic characteristics of collagen may be lost. The
collapse of the collagen fibers upon drying may therefore be a result of the changes
in the molecular arrangement. While in a wet state, wide gaps separate the collagen
molecules from each other, in a dry state, the molecules are arranged more
compactly. This is because extrafibrillar spaces in hydrated Type I collagen are filled
with water, while dried collagen has fewer extrafibrillar spaces open for the
penetration of the monomers included in the adhesive systems. Water removal also
may permit additional hydrogen bonds to form between collagen molecules that were
previously bonded to water molecules, leaving no interfibrillar space.

37

During air-drying, water that occupies the interfibrillar spaces, previously filled with
hydroxyapatite crystals is lost by evaporation, resulting in a decrease of the volume
of the collagen network to approximately one third of its original volume. When airdried demineralized dentin is rewet with water, the collagen matrix may re expand
and recover its primary dimensions to the levels of the original hydrated state. This
spatial re expansion occurs because the spaces between fibers are refilled with
water and because Type I collagen itself is capable of undergoing expansion upon
rehydration. The stiffness of decalcified dentin increases when the tissue is
dehydrated either chemically in water-miscible solvents or physically in air. The
increase in stiffness is reversed when specimens are rehydrated in water. Therefore,
rewetting dentin after air-drying to check for the enamel frosty aspect may be an
acceptable clinical procedure.
In spite of numerous research papers focused on the low bond strengths associated
with air-dried dentin the ultrastructural effects of drying dentin collagen during clinical
procedures are not fully understood. Under the SEM, areas of detachment with
incomplete peritubular hybridization have been observed, along with deficient
penetration of the adhesive into the tubules. The adhesive does not seem to
penetrate etched dried intertubular dentin. Under the TEM, collagen fibers coalesce
into a structure without individualized interfibrillar spaces. Rewetting re expands this
collapsed collagen.
Clinically, it is very difficult to either assess or standardize the ideal amount of
moisture that should be left on the dentin surface before the application of the
adhesive system. Ideally, water should form a uniform layer without pooling
(overwet) and without dry areas (over-dried). Therefore air-drying with an air-water
syringe after rinsing off the etching gel is not recommended because it cannot
produce a uniform layer of water on the surface. A recent study demonstrated that
the excess water after rinsing the etching gel can be removed with a damp cotton
pellet, a disposable brush, or a tissue paper without adversely affecting bond
strengths.

38
MQ AI Qahtani et al evaluated the effect on shearbond strength of rewetting dry
dentin with 2 desensitizers. He compared the effect of rewetting dried dentin with 2
commercial desensitizing agents (protect and Hurriseal) on the dentin shear bond
strength of 3 total etch dentin bonding agents (syntac single component, optibond
solo plus and prime and bond NT) and compared both to applying these same
bonding agents to moist dentin and dry dentin. There was no significant difference in
bond strength between the controls, dry and hurrieal protect means shows lower
shear bond strength.(Operative dentistry; 2003; 28-3; 287-296)
Moist Vs dry Y. Nakaokiet et al evaluated the effect of residual water on dentin bond
strength and hybridization of a one bottle adhesive system. This research
investigated the effect of wet and dry conditions of phosphoric acid etched dentin on
resin bonding and determined the optimum moisture condition for resin bonding
using an etchant based one bottle adhesive system. Boline dentin surfaces were
etched with 35% phosphoric acid and rinsed with water. Under four wet and dry
conditions (Overwet, blot dry, one-second dry and desiccated ) resin, composite was
bonded using single bond. Tensile bond strength was measured.
The blot dry group and one second dry group revealed significantly higher bond
strength than the desiccated and over wet groups. The formation of hybrid layers
approximately 5m thick (over wet and blot dry), 2m (one second dry) and item
(desiccated) were observed. (Operative dentistry, 2002; 27; 563-568)
Erik Christian Munksgaard et al compared wet or dry , normal or deproteinized
dentin surfaces as substrate for dentin adhesives. (Acta odontol scand 2002; 60; 6064)
Human dentin were
a) Acid-etched and blot dried for 1 sec (wet),
b) As (a) but dried with air for l0 sec (dry).
c) Acid-etched and treated with hypochlorite and then dried for 1 sec.
d) As (c) but dried with our for 10 sec eight dentin adhesives were used in each
group for bond strength measurement. Normal etched dentin showed a

39
reduction in strength of 14-15 MPa for three of the adhesives when tested dry
instead of wet.
It was hypothesized that low techniques sensibility of an adhesives may be linked to
its ability to wet and adhere to collapsed collagen fibres and to the surface for the
underlying mineralized tissue comparisons of bond strengths obtained by using dried
or wet acid-etched dentin and dried. Wet acid-etched and deproteinized dentin may
be useful for evaluating the efficiencies of dentin adhesives.
BIOCAMPATIBILITY:
It has been suggested that conditioning agents (etching agents used on dentin)
should be:
Isotonic to avoid osmotic pressure changes in dentinal tubules
Of neutral pH or at least between pH 5.5 and pH 8.0.
Nontoxic to dentin, pulp and gingival tissue.
Compatible with the chemistry of the materials it will contact.
Water soluble and easily removed.
Unable to deplete the enamel or dentin chemically.
Able to enhance the surface chemically in preparation for bonding.
PRIMING (Self Etch, Total Etch)
The Key element for adhesion is the intimate bond that develops between the
adhesive and substrate.
Dentin

Hydrophilic

Composite

Hydrophobic

Intermediary with both the groups PRIMER. Primer usually HEMA (Hydroxyethyl
Methacrylate), is a part of bonding agent that has both the hydrophilic and
hydrophobic group so as to achieve bonding. Adhesive agent is applied after the
application of the primer followed by the placement of composite resin. Solvents are
substances which help to carry the primer into the dentin.
The solvent can be
Acetone
Alcohol (ethanol)

40
Water
TOTAL-ETCH ADHESIVES:
Total-etch adhesives involve a separate etch-and-rinse phase. In their initial
configuration, the conditioning step is followed by a priming step and application of
the adhesive resin, resulting in three-step total-etch adhesives. Two-step total-etch
adhesives combine the primer and adhesive resin into one application.
Bonding to acid-etched enamel theoretically requires an air-dried surface to allow the
photo-polymerizable hydrophobic bonding agent to be drawn by capillary attraction
into the pits created by acid-etching. As a result, two kinds of tag-like resin
extensions are formed. Macro-tags are circularly formed between enamel prism
peripheries. Microtags are formed at the cores of enamel prisms where the resin
cures into a multitude of distinct crypts of dissolved hydroxyapatite crystals. Although
most research dealing with adhesive techniques lately has focused mainly on
bonding to dentin, the importance of enamel bonding effectiveness may not be
neglected with the development of new adhesive systems. The bond to enamel
remains the best that can be clinically achieved. Preserving adjacent enamel as
much as possible, therefore, remains one of the most important guidelines when
preparing cavities for adhesive restorations.
The underlying mechanism of adhesion to dentin is alike for the three- and two-step
total-etch adhesives. The dentin smear layer produced during cavity preparation is
removed by the etch-and-rinse phase, which concurrently results in a 3-5 m deep
demineralization of the dentin surface. Collagen fibrils are nearly completely
uncovered from hydroxyapatite and form a micro-retentive network for micromechanical interlocking of monomers. This interlock was first described by
Nakabayashi, in 1982 and is commonly referred to as hybrid layer (Van Meerbeek
and others 1992, Hybridization - resin tags seal the unplugged dentin tubules and
offer additional retention through hybridization of the tubule orifice wall.)
Three specific ultra-morphologic features have been described as resulting from this
hybridization process. A shag-carpet appearance stands for the loose organization

41
of collagen fibrils that are directed towards the adhesive resin and often unraveled
into their micro-fibrils. This feature typically appears when the dentin surface after
being acid-etched, has been actively scrubbed with an acidic primer solution. A
similar pattern of deeply tufted collagen fibrils has been observed to result from
citric-acid burnishing of root surfaces as part of a tissue-regenerative periodontal
treatment. The physical rubbing action combined with the chemical action of the citric
acid was found to enhance the removal of acidically-dissolved inorganic dentin
material and surface debris. This resulted in a deeply tufted collagen fibril surface
topography, similar to the appearance of a shag carpet. In this way, the dentinal root
surface became more receptive to the attachment of cells from new connective
tissue-formation. Likewise, the combined mechanical/chemical action of rubbing the
acid etched dentin with an acidic primer probably dissolves additional mineral while
fluffing and separating the entangled collagen, at the surface This active rubbing
application is thought to promote infiltration of monomers into the loosened collagen
scaffold by a kind of massaging " effect.
A second typical hybridization characteristic has been termed as tubule-wall
hybridization and represents the extension of the hybrid layer into the tubule wall
area. Resin-tag formation in the opened tubules is circularly surrounded by a
hybridized tubule-orifice wall that is thought to be favorable in hermetically sealing
the pulpo dentinal complex against microleakage and the potential subsequent
ingress of microganisms. This effect may be especially protective when the bond
fails either at the bottom or top of the hybrid layer, which are considered as the two
weak links in the micromechanical attachment. Then, the resin tags usually break off
at the hybrid layer surface keeping the dentin tubules and thus the direct connection
to the pulp sealed. In particular, the resin-tag necks at the top 5-10 m of the tubule
orifices are thought to contribute most to retention and sealing effectiveness. The
actual length of the resin tags most-probably be regarded as being secondary
importance.
Thirdly lateral tubule hybridization has been described as the formation of a tiny
hybrid layer into the walls of lateral tubule brandies. This micro-version of a hybrid
layer typically surrounds a central core of resin called a micro resin tag

42
The clinical application procedure of the newest generation of one bottle or two-step
total-etch adhesives might be simpler due to the reduction by one step, the eventual
application time may not have been substantially reduced as compared ''to
conventional three-step systems. In conventional three-step systems, the primer
should assure efficient wetting-of the exposed collagen fibrils, displace any residual
surface moisture, transform a hydrophilic into a hydrophobia tissue state and
sufficiently carry monomers into the interfibrillar channels. The adhesive resin should
fill up the remaining pores between the collagen fibrils, form resin tags that seal the
opened dentinal tubules, initiate and advance the polymerization reaction, stabilize
the formed hybrid layer and resin tags and provide sufficient methacrylate double
bonds for co-polymerization with the successively applied restorative resin. In
simplified one-bottle systems, the functions of the primer and the adhesive resin
should be perfectly combined. As a consequence, higher technique sensitivity has
often been ascribed to the use of these one-bottle systems As these combined
primer/ adhesive resin solutions have a higher solvent-to-monomer ratio, a realistic
risk exists that such adhesives are applied in a too thin layer. To achieve adequate
bonding, it is of major importance, however, that the one-bottle solution is abundantly
applied. Monomers should be sufficiently supplied not only to saturate the exposed
collagen fibril network, but also to establish a satisfactorily thick resin layer on top of
the hybrid layer. Such a distinct resin layer must be regarded as a flexible,
intermediate shock-absorber.
ELASTIC BONDING CONCEPT
The adhesive resin placed over the surface should be preferentially brush thinned
rather than air thinned to provide an optimal thickness of 100 m. Such a thick layer,
due to high elasticity act as a stress relaxation buffer. This is called Elastic Bonding
Concept.
Advantage of Elastic Bonding Concept
1)

Counteracts the polymerization contraction stress.

2)

Absorbs Mastigatory forces.

3)

Aids in Tooth flexure effect.

4)

Prevents Thermal cycling shock.

43
In light of the elastic bonding concept, it is expected that this shock-absorber may
help to protect the adhesive joint against early failure caused by the shrinking
composite cured on top. Therefore, when using one-bottle adhesives, it is
recommended to apply multiple layers to ensure a sufficiently thick resin film on top
of the hybrid layer. They are particularly necessary when using primer/adhesive resin
combinations with high acetone content. The so called nanofiller added to certain
one-bottle adhesives (Prime and Bond NT, Dentsply, Excite, Vivadent) may also help
to establish a uniform resin film that stabilizes the hybrid layer. After priming, the
surface should appear glossy without so called dry spots, the clinical indication that
resin was adequately and sufficiently applied. Especially in the latter respect, the
addition of nanofiller must be regarded as-beneficial, rather than perceived that the
nanofiller would infiltrate the exposed collagen fibril network and thus reinforce the
hybrid layer, as has been hypothetically claimed. TEM (Transmission Electron
Microscopy) of unstained sections has clearly demonstrated that the collagen fibril
network mostly filters out the nanofiller, holding them at the hybrid layer surface.
Besides, it is not obvious that pen tration of the nanofiller in the hybrid layer would
strengthen the bond or improve the bond stability.
Hybrid layer
The structure formed in dental hard tissues (enamel, dentin, cementum by
demineralization of the surface and subsurface followed by infiltration of monomers
and subsequent polymerization is called Hybrid layer.
Hybridization
Hybridization is the process of creating a hybrid layer in dental hard tissue.
Acid Etching of Dentin

Increase of Transdentinal permeability

Mineral content removed in intertubular Dentin ( App-2-7m )

Formation of Resin Tag + Hybrid layer

44
Good Hybridization is achieved when there is an even and a homogeneous hybrid
layer formation (5-8). The cohesive strength of the bonding should be sufficient to
give good bond strength.
Hybridized Resin Tag
Acid etching removes the peritubular dentinal matrix from the wall of the tubule.
Increased permeability of tubule walls

High affinity of adhesive monomer

Diffusion of monomer into surrounding demineralized dentin

Polymerisation

Hybridized Resin tag (Top 2-4m)

Seals the tubules + Resin retention.

The bond strength is dependent on the cross sectional area of the tag rather than the
volume.
The interaction of tissues and biomaterials at biological interfaces is extremely
important, but it is very difficult to connect natural tissue with artificial material to
solve this problem, a liquid must be first used to form an intimate contact between
the biomaterial (monomer) and the solid hard tissue, when the liquid penetrates and
is converted to a solid via polymerization. This is the approach that is selected in the
attempt to provide retention of biocompatible monomer with tooth substrate.
The Dentinal Tubules are in different directions towards the pulp and the penetration
of resins into the dentinal tubules may generate mechanical retention, providing a

45
NON PARALLEL RETENTION.

Hence there will be no possible path for removal,

unless some of the resin tags fracture.

Hybrid layer contributes to dentin bonding in the following ways:
1.

Good bond strength

2.

It acts as a semipermeable membrane and prevents noxious

stimuli from

invading pulp
3.

Lessens the risk of micro leakage

4.

Decrease the incidence of secondary caries

5.

Reduces postoperative sensitivity.

Dentin Bonding = Hybrid layer + Resin Tags

Under ideal conditions, hybrid layer formation would be the major bonding
mechanism in superficial dentin with little contribution from Resin Tags (since there is
few tubules available in superficial dentin to form tags), while in deep dentin resin
tags contribute most of the bond strength, with a reduced contribution of hybrid layer
Hybridoid Layer or Ghost Hybrid Layer
Hybridoid layer occurs due to incorrect

application

procedures whereby voids

and porosities occur within resin-infiltrated demineralized dentin.

John Perdigao et al in 1999 showed that air-drying dentin prior to application of
primer and adhesive, results in incomplete peritubular hybridization and deficient
penetration of the adhesive into the tubules. Under SEM, the collagen fibres
appeared coalesced into a structure without individualized interfibrillar spaces. The
lower third of this hybridoid structure displayed a few areas with collagen bonding
indicating that the structural changes are less severe close to the transition to
unaffected dentin. The non-infiltrated spaces (100-150m wide) were observed
detaching from the peritubular areas at the transition between normal and
demineralized dentin.

Reverse Hybrid layer

In reverse hybrid layer formation, acid etching removes the smear layer and exposes
the collagen fibrils of dentin matrix, followed by application of sodium hypochlorite.

46
This not only removes the exposed collagen fibrils but also solubilizes the fibrils
down into the underlying mineralized matrix to create submicron porosities within the
mineral phase.
Self-etching adhesive
Alternative to total etch system is the self etching primers (SEP's) that include a
phosphonated resin molecule that performs two functions simultaneously etching
and priming of dentin and enamel. The SEP does not remove the smear layer, but
fixes it and exposes about 0.5 to 1 m of intertubular collagen because of its acidity
(pH=1.25 -1.40). The acid primer (AP) further impregnates the smear plug and
prepares the pathway for the penetration of subsequently placed fluid resin (R) into
the micro channel that permeate the smear plug. The fluid resin with the
demineralized dentin and collagen fibrils form the hybrid layer.
The self etching adhesives available are
1.

Two step self etch adhesive (AP+R)

2.

One step self etch adhesive (or) All in one adhesive (APR.)

Based on the pH they are classified as:

1) Mild self etch adhesive pH = 2
2) Strong self etch adhesive pH < 1.
The mild self etch adhesives provide only submicron hybrid layers and the collegen
fibrils are not completely deprived from hydroxyapatite (in contrast to total etch
adhesive)
Residual hydroxyapatite crystals

Bond with specific carboxyl or phosphate groups of functional monomer (4 Met

based two step self etch adhesive)
Better resist hydrolytic degradation process. The strong self-etching adhesives bond
in manner similar total etch adhesive. The hydroxyapatite crystals are fully removed

47
and hence there is no chemical interaction between hydroxyapatite and functional
monomers.
Advantage of self etching primers (SEP)
1)

Simultaenous demineralization and resin infiltration

2)

No post conditioning rinsing

3)

Not sensitive to diverse dentin wetness conditions.

4)

Less technique sensitive.

Effect of self etching primer phosphoric acid etchant on bonding to bur-prepared

dentin-M ogata et al evaluated the effect of dentin conditioner on tensile bond
strength to dentin prepared with different types of burs.
A self etching primer system, mac-bond II and a phosphoric acid etching system
single bond used for conditioning. For Mac bond II and single bond there were no
statistically significant differences among the groups prepared with steel burs and
the control.
Phosphoric acid treated and bur-prepared dentin surfaces shown scratches left by
the abrasive paper (or) burs. Dentinal tubules that were also observed over the
entire surface. Macbond II primer treated surface, the smear layer on the dentin
surface and the smear plugs in the dentinal tubules were

removed(Operative

dentistry, 2002, 27, 447-454)

EFFECT OF ETCHING ON PRIMARY TEETH
Silverstone (1974) found that a 60sec application of an unbuffered solution of 37%
phosphoric acid produced the most favorable conditions for bonding. Pukes et al
(1984) and Eidelman et al (1984) showed, respectively, that a 20 sec etch provided
similar leakage resistance and retention rates when compared to a 60 sec etch. This
has very obvious implications for the management of young children when scaling
their teeth and therefore upon the success of the sealant itself. Acid etching has two
distinct actions on human enamel. Firstly, it removes superficial plaque, debris and a
very shallow layer of enamel, including chemically inert enamel crystallites.

48
Secondly, it renders the enamel surface more porous. A honey-combed latticework is
produced within the remaining superficial enamel, where enamel tags are left
projecting in different planes and at different angles.
There is differential demineralization of the prisms because the primary attack occurs
on the cores of enamel rods to produce the microspaces. However, this depends on
the incident angulation of the enamel rods to the tooth surface. On an average, the
etching is about 25m deep in permanent teeth. It was thought that the outer prism
less layer of primary enamel prevented the penetration of resins in the surface of
etched primary enamel.
There is no universal agreement that prism less enamel occurs in all surfaces of all
primary teeth (Silverstone 1970).To obtain a pattern of etching comparable to that
found in permanent teeth, Silverstone and Dogan (1976) found it necessary to etch
for 120 seconds. However, Redford et al (1986) looked at the effect of different etch
times on the sealant bond strength, etch depth and pattern, on primary teeth. They
found that the bond strength was no greater at 60 or 120 seconds than at 15 or 30
seconds, but the standard deviation was greater at the two shorter times; the etch
depth was not very different at the three shorter times but was five times greater at
120 seconds. They felt unable to recommend an etch time for primary enamel of less
than 60 second because of the greater variability of bond strength at 15 and 20
seconds. Our clinical experience is of good results with a 30 seconds etch.
The Purpose of this study was to evaluate in vitro the effect of a phosphoric acid
etchant containing benzalkonium chloride on the dentin/adhesive interface in primary
teeth. The teeth had caries lesions involving enamel and dentin, and were stored in
92% lutaraldehyde soln for 2-4 hours. The teeth were divided into 5 groups of five
teeth each. The specimens were observed with an SEM for assessment of the
morphology of the bonded interface.
Interface was observed to determine the presence or absence of hybrid layer
formation, resin tags and gaps. In the groups treated with only benzalkonium
chloride solutions, spaces were observed in the resin/dentin interface. Similar
findings were observed in the control group, which received no treatment on the

49
dentin primer application in these groups neither resin tag nor hybrid layer formation
was observed. The presence of an amorphous layer, which was an unremoved
smear layer was noted.
The group treated with 35% phosphoric acid showing hybrid layer formation (8.15
m) this layer was linked intimately with the peritubular and intertubular dentin. Tags
formation was observed towards the pulp under the hybrid layer. In these specimens
the gaps were not observed between the dentin layer and bonding material. The total
removed of the smear layer was observed using 37% phosphoric acid with
benzalkonium chloride. A hybrid layer ( 7.32 m) and resin tags attached to this
layer were observed similar to the group in which the 3.5% phosphoric acid was
used. The samples showed total removal of the smear layer and no gaps were
observed in the dentin/adhesive interface.(JOURNAL OF CLINICAL PAEDIATRIC
DENTISTRY; 2000; vol24; No3;2-5-209)
APPLICATIONS OF THE ACID CONDITIONERS
Acid etch technique is now widely used for most composite restorations as a
means of aiding retention and reducing or preventing micro leakage. For class-4
cavities the acid etches technique has replaced the gold inlay as the treatment of
choice for restoring the tooth contours and function.
Bonding of resins using the acid etch technique has also been used as a means
of splinting teeth which have been weakened by cavity preparation.
Fissure sealants are now widely used for preventing pit and fissure caries. Resin
systems are now used for attaching orthodontic brackets. Composites are gaining
in popularity for the attachment of bridges. The principle of the resin-bonded
system is that the composite bonds mechanically to the etched enamel of the
tooth and also to the surface of the cast alloy framework of the bridge.
Another application of the acid etch technique is the attachment of acrylic or
porcelain labial veneers in order to improve the appearance of stained, discolored
or misshapened teeth.

50

FACTORS TAKEN INTO CONSIDERATION

While evaluating whether an etching technique is good or bad, one must remember
that subtle changes in technique and methods can cause important changes in
results, and that the following factors must be taken into consideration:

Type of acid

Concentration

Time interval of application

Active (rubbing, scrubbing) or passive (soaking) application.

Cavity preparation or just exposed superficial dentin

Consideration of Remaining Dentin Thickness (RDT)

Presence or absence of sclerotic dentin and reparative dentin

Age of the patient and species and age of experimental dentin

Pulpal responses to subsequent type of restoration .

Condensation of amalgam

Self -cured composite resin, placed under pressure.

Visible - light cured composite resin placed incrementally

DISADVANTAGES OF ACID CONDITIONERS

There are a number of disadvantages to acid etching of dentin. These include:
Increasing dentin permeability
Increasing dentin wetness
Increasing the potential for pulpal irritation by leakage of microbial products
Increased potential for denaturation of collagen and/or reducing the porosity of the
demineralized matrix by precipitation of calcium and phosphate ions.
There is also the danger that adhesive resins will not penetrate into the matrix as
deeply as the acidic conditioners. This may leave an intrinsically weak zone that may

51
give high bond strengths initially, but weaken over several years due to slow
hydrolysis of exposed, unprotected collagen.
THE PROBLEM OF ETCHING: [Clarks Clinical dentistry]
ETCHING AGENTS

Originally, the use of strong acids in cavity primers and propping agents for long
periods of time {1 to 2 minutes) in contact with dentin, tended to do more harm than
good.
Although pretreatment of enamel with certain acid solution; which has no effect on
the pulp, has been accepted as an effective means to improve bonding of resinous
materials, acid pretreatment of dentin has gained no such acceptance. Etching of
enamel does not harm the pulp because the effects of the acid would have to
penetrate the entire thickness of the enamel before reaching dentin. In addition, the
superficial dentin is usually gnarled and tubular which reduces permeability.
However, the situation is quite different when etching agents contact exposed dentin.
Since the etching agents are either phosphoric acid or citric acid and, like acids from
any source they can harm the pulp if they approach or contact it. Peritubular dentin
(sclerotic dentin) is rapidly dissolved by the strong acid etching agents and can
return the dentinal tubules to their original diametric dimension, with increasing
permeability and susceptibility to toxic substances.
A one minute treatment of the dentinal walls of a cavity preparation with 50%
phosphoric acid followed by a ZOE restoration produced pulp reactions resembling
those induced by unlined silicate cements after 24 to 72 hours. The etching agent
increased the permeability of dentin fourfold. If an irritating restorative material
contacts such permeable dentin the ability of the irritating ingredients to reach the
pulp is accentuated. This etching opened the tubules to such an extent that the
pulpal lesions were larger and the infiltration of inflammatory cells greater than when
no preparative agent was used. Despite such information being available, a 50%
aqueous solution of citric acid, applied for I to 3 minutes, is still being suggested as a
means of removing debris from cavity preparations.

52

Even when a composite with a low percentage of methacrylic acid and possessing a
so-called neutral pH was applied to cavity preparations after citric acid pretreatment.
The average pulp response increased. Similar results occurred when dentin was
etched with 50% phosphoric acid containing 7% zinc oxide prior to filling with an
ultraviolet light curable resin composite.
Bastos and colleagues found no significant differences on the shear bond strength of
a microfill composite resin compared to enamel whether they etched 15, 30, 60
seconds, or 30 seconds followed by washing and then an additional etching for 30
seconds with 37% phosphoric acid.
The direct application of orthophosphoric acid (H 3PO4)) to dentin of vervet monkeys
elicited a severe pulpal response. Similar findings were reported in a subsequent
study in which this acid was applied to human teeth prior to composite restoration.