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Bonding to enamel and dentin

Pardis Tarighi

Principles of adhesion
Adhesion = attachment of one substance to another-forces/energies Adherend Adherent= bonding agent-adhesive system Durability= time period that bond remains effective Mode of failure in tensile or shear load cohesive/adhesive Requirements at interface: contact-wetting
Enamel>dentin>smear layer Contaminated enamel=28 dyn/cm Surface tension-energy

Theories of adhesion
Mechanical (roughness and micromechanical interlocks) enamel Primary(ionic-covalent) Adsorption (chemical) Secondary(hydrogen-valence) Diffusion (mobile molecules) Electrostatic (electrical double layer)

Factors affecting adhesion to tooth

Physiochemical properties of adherend and adhesive Structural properties of adherend being heterogenous Surface contamination External stresses Oral invironment

4% 1%

12% 18% 70%

95% inorganic 12% 2% 25% 50% water organic


25% Inorganic=HAP Volumes more important to adhesion Dentin: heterogeneous



Dentin structure

Number of tubules: 20000 near DEJ-45000 near pulp Diameter: 0.8 at DEJ-2.5 near pulp Intertubular dentin: less mineralized Organic membrane=lamina limitans Superficial dentin: 96% intertubular-3%peritubular1%dentinal fluid Near pulp: 66% peritubular-12% intertubular-22%fluid Outward fluid pressure: 25-30 mmHg

In sclerotic dentin: obstruction of tubules by apposition of peritubular dentin Refractive index like intertubular: glasslike appearance Low permeability and less receptive to adhesives

Smear layer
Any debris, calcific in nature, produced by reduction or instrumentation of dentin, enamel or cementum or as a contaminant that precludes interaction with the underlying pure tooth tissue

Characteristics: Attachment to surface by frictional heat and shear forces(weak-brittle) Most effective conditioners: EDTA-acids(citric-polyacrylic-lactic-phosphoric) Thickness:0.5-2/smear plug=1-10 Reduces dentinal permeability by 86%(with acid removal increases by 90%)

Strategies towards smear layer

Dentinal fluid

Removal (etch & rinse)

Postoperative sensitivity Pulpal irritation

Penetrate (self etch approach)

Alternative technologies of cavity preparation

Sono abrasion Air abrasion Diamond coated tip Little effect on gingival tissue Ultrasonic energy Reduces heat, vibration and Thinner smear noise layer Main disadvantage: dust Main advantage: less risk of damage Laser ablation to adjacent tooth Er:YAG,Nd:YAG Thermomechanical microexplosions No smear layer(just denatured collagen fibrils) Rough but not demineralized surface Possible cracks and weak dentin(3-4) No specific advantage

Dentinal wetness
Diameter and length of tubules Viscosity of fluid Pressure gradiant Substances dissolved Surface area for diffusion

1)internal wetness

permeability is more in : coronal-near pulp hornproximal Interference with polymerization of adhesive-depth of penetration
2)External wetness

Wetting of adhesive
Ideal adhesive: Sufficiently wet the solid surface (CA less than 15hydrophilic monomers like HEMA)

Low enough viscosity to penetrate microporosities (polarity-solubility of monomer similar to


Displace air and moistue during bonding (ethanolaceton)

2.9-7.1% Contraction stresses up to 7MPa New technologies for lower shrinkage (besides c-factor and filler content) : ring opening Silorane based composite(siloxane+oxirane) shrink less than 1%vol e.g :Filtek LS Compensations:
1-flow (contraction stress>elastic limit)
in autocure 2-sandwich technique/cervical sealing 3-glass or ceramic blocks/prepolymerized resin 4-cavity design 5-hygroscopic expansion long time after bond failure Overcompensation (microfilled:2/5 times) 6-elasticity(YM):elastic bonding concept of 125 slow curing rate-rapid bond/ air bubbles

Polymerization contraction of restorative resins

Initial polymerization
Orientation of curing light? Autocure: start at dentinal wall (heat) Chemical polymerization at surface of dentin (gluma 2000) glycin-collagen Water-triggered polymerization 4META/MMA-TBB e.g: Super Bond D-liner/AmalgamBond Other mechanical considerations:
Thermal and mechanical stresses cause pumping action on the fluid in the gap between resin composite and tooth structure Biocompatibility Fusayama: acid penetration to dentin=10 (odontoblost blocks) Some adhesives have antimicrobial effect(MDPB) but not after polymerization

Adhesion to enamel and dentin

1990: selective enamel etching replaced by total etch 2phases of adhesion to tooth: removal of CaPh/hybridization (infiltration+polymerization) Classification of adhesives: scientificchronologic

Classification and examples

Etch and rinse adhesives Self etch adhesives

3step (4th generation) All bond2/clearfil liner bond /denthesive/optibond FL/ permaquick/scotchbond MP

2step (6th generation) AdheSE/ clearfil SE/ clearfil protect bond /ProBond/scotchbond2/ Syntac/Solobond Plus 1step (7th generation) AdmiraBond/ Promp L pop/ Futurabond/ one-up bond/ Gbond/ibond/xeno

2step (5th generation) Excite/Gluma2000/ optibond solo plus/ prime&bond NT/ single bond(scotch bond1)

Etch and rinse approach

Still most effective-gold standard Macrotag (intertubular)/microtag (intratubular) Most critical step: primer Major enamel retention
wetting of exposed fibrils-displacement of moisture-transforming hyrophil to hydrophobe

Adhesive resin: polymerization-stabilizing hybrid layer and

resin tags-MA double bonds

True chemical bonding is unlikely

Acid etchants
Phosphoric acid:30-40% at least 15 sec/rinse5-10sec All acids rinsed off except: nitric acid(mirage ABC enhanced) Other etchants: maleic(scotchbond mp)-citric( clearfil CA/amalgambond)-oxalic acid( gluma2000) Etched enamel: surface energy=72dyn/cm (etched dentin=44.8) Removes 10 from surface-microporous layer=5-50 Effect of etchant: type-concentration-time-form(gel)-rinse-method(rubbing)structure (on dentin, also distance between tubules: closer=deeper) Bond strength to etched enamel: 20 Mpa Aggressive etch on dentin: groove-funnel Oxygen inhibited layer(15 ) on top of adhesive layer provides double MMA bonds

Collapse risk

Hybrid layer

Top: amorphus denatured collagen NaOCl/chx Middle: cross sectioned fibrils with electronlucent spaces(10-20nm) with occasional mineral crystals Base layer: gradual transition to unaltered dentin imperfect resin penetration : nanoleakage Degree of polymerization inside hybrid layer: mode-site of initial polymerizationdegree of available double carbon bonds Resin tag=polymerized resin extensions More important in enamel/in dentin presence of intertubular dentin is critical

15% of bond strength

Tubule wall hybridization

Lateral tubule branches

3step vs 2step etch&rinse

Marginal integrity Bond durability Optibond solo vs FL( clV)/ VanMeerbeek 2010:
best bond durability for mild 2step self etch (hydrophobic resin layer on top of hydrophilic SE primer)(clearfil SE bond)

Single bond vs scotch bond mp

3tep: -best long term results -Risk of overetching/ contamination/ therapeutic agents(ph.acid-solvent free adhesive-low mol. Weigh therapeutics in adhesive) 2step: -controlled solvent evaporation -More technique sensitive -Risk of too thin bonding/overetch -Sensitive to dentin wetness

Self etch approach

Modifying smear layer/thinner(100nm-4) Total etch Acidic functional monomers hydrolytic degredation Monomers to which carboxylic(4MET) or phosphate acid(Phenyl P/10MDP) groups are added Reduced post operative sensitivity

Etching aggressiveness in SE:

Strong: PH of 1 or less/like ph.acid/3-4 hybrid layer/shag carpet Mediately strong: PH=1-2/1-2/gradual transition of hybrid layer e.g: adheSE/optibond solo plus / ibond/xenoIII Mild: PH=2/1/ thinner hybrid layer/preservation of HAP=possible chemical bond(4-MET/phenyl-p/10-MDP) Ultramild: PH>2.5/100nm
Remained HAP crystals may retard marginal leakage Main disadvantage: weak bond to enamel

Shag carpet

One step self etch adhesives

Disadvantages: Low bond strength Hydrophilicity Phase separation(HEMA-free): water-tree nanolaekage/(clearfil S3 contains HEMA)
Poly-HEMA hydrogel?

Short shelf life

AD concept
Why certain acids adhere rather than decalcify tooth? Solubility of calcium salt Oxalic acid=PH:0.6/adheres Maleic acid=PH:0.9/decalcifies

Glass ionomer adhesive

The only true self adhesive material Conditioner needed when: thick, compact smear layer/10-20sec/ cleansing effect-partial demineralization and increased surface areachemical interaction of acid with HAP Self etch with high molecular weight polymer

Chronological classification
1st generation: Buonocore1956 GPDM-hydrochloric acid etched dentin/2 -3MPa /unstable in waterhydrophobe bifunctional monomers: NPG-GMA(1st dentin bonding agent/chelation) 2nd generation: 1978-Clearfil Bond system to Scotchbond/phosphorous esters of MA derivatives/surface wetting+ionic interaction/ 56MPa/hydrolytic unstability-bonding to smear layer

3rd generation: Japanese philosophy of etching/Clearfil New Bond(HEMA+10MDP) chelating agents to remove smear layer: NPGGMA/ferric-Ca-Al oxalate or phosphate/4META( polymer weight)/ 10% citric acid+3%ferric chloride and 35%HEMA+4META-MMA-TBB( C&B Metabond/ Superbond D-liner/Amalgambond plus)/ EDTA( Gluma/Denthesive)/ scotchprep(2.5%maleic acid+55%HEMA and unfilled bis-GMA+HEMA): Scotchbond2(SE adhesive precursor)/ Universalbonds

4th generation: conditioner instead of etchant/ total etch approach with30-40% ph.acid/3 step etch&rinse/bonding agent=adhesive system e.g :
All Bond2-OptiBond FL-Permaquick-Scotchbond mp

5th generation(one bottle): excite-one step-optibond

solo-prime&bond-single bond(scotchbond1)

6th generation: similar to 2nd generation/ 1- SE primer+adhesive (AdheSE-Clearfil SE and protect bondoptibond solo plus SE) 2-one step 2component with mixing (Adper promp L pop-one up bond F-Xeno III)
7th generation: one bottle no mixing (Gbond-ibondXeno IV-Clearfil S3)

Isolation: etch&rinse/salive proteins/dental arch Pulp protection SE on enamel: Prime&bond NT/Clearfil SE bond- at least30sec rubbing Wet vs dry bonding Dilutes primer Uncomplete replacement by primer Phase separation Primer application: 15sec-multiple layers-active rubbing-gentle air drying Adhesive: brush thinning-100
Air drying= 65% volume reduction

Clinical notes

Current concepts about adhesion

Resin-dentin bond is less durable than resinenamel bond: organic content dependency Immidiate bond strength/5.7yrs(average) Exposed collagen fibrils from incomplete resin infiltration: creep(pashley2003)-cyclic fatiguerupture(fung2009) -hydrolysis

Factors compromising durability of resin-dentin bond

1.Hydrolytic degradation by water sorption : Collagen collapse wet bonding hydrophilic adhesives hydrolysis after solvent vapor monomer concentration water evaporation
Plasticization of polymer Phase separation
Bis2.Incomplete infiltration of resin monomers : GMA/ incomplete water replacement-GAG hydrogels HEMA 3.Collagenolysis by endogenous MMPs and cathespins (Zn&Ca dependent/acidic invironment)

Strategies to prevent bonding degradation

1) Increasing degree of conversion and esterase resistance of hydrophilic adhesives: hydrophilic photoinitiators- cross linking of fuctional groups after infiltration (ideal adhesive= hydrophil
before infiltration/hydrophobe after polymerization)/ helps

reduce phase separation-not resin infiltration

2) Collagenolytic enzymes inhibitors : CHXgalardin- PV phosphonic acid-BACMDPB(protect bond)/ collagen cross linking(hemopexin/fibronectin-like domains) :glutaraldehyde,genipin,proanthrocianidine,car bodiimide (still mechanical properties like E.M

demineralized dentim/ cathepsin active/electrosta tic bond/E.M

3)Ethanol wet bonding

Removes water without shrinkage Prevents collagen collapse (reduced fibrillar diameter and increased interfibrillar spaces) Prevents phase separation of hydrophobic resin monomers Homogenous distribution of hydrophobic resins Inhibits MMP activation(water absence) Method of application: 1-100%/1min before (technique sensitive) 2-progressive replacement( clinically impractical) For long durability better to use hydrophobic adhesives
Tert-butanol: miscible with water/resin-better stability than ethanol-less technique sensitive

4)Biomimetic remineralization of bond

Enzyme exclusion in mineralized dentin Heterogenous nucleation of ca-ph. phases(seed crystallites)/top-down approach Polyanionic analogs of acidic matrix proteins/bottom-up/3-4 months