Bonding mechanism and ultrastructural interfacial analysis of a single-step adhesive to dentin

Kunio Ikemura, Franklin Chi Meng Tay, Toshiya Hironaka, Takeshi Endo, David Henry Pashley

Research output: Contribution to journalArticle

37 Citations (Scopus)

Abstract

Objectives. to characterize the interaction of 4-acryloxyethyltrimellitic acid (4-AET), a key ingredient in a commercial all-in-one adhesive (Reactmer Bond) with dentin apatite, to measure the solubility of 4-AET calcium (4-AETCa), and to examine the ultrastructure of the resin-dentin interface bonded by this adhesive. Methods. solubility of synthesized 4-AETCa in several solutions was measured. Flattened bovine dentin blocks were treated with 0.1wt% NaOCl for 10 min, or 5.0wt% NaOCl for 10 min, or 30 min. Fourier transform infrared analysis using attenuated total reflection (FT-IR/ATR) was performed on these four substrates before and after treatment with a 4-AET mixture (4-AET/HEMA: 40/60wt%). Undemineralized, unstained sections of human sound dentin that were bonded with the same comonomers were examined by transmission electron microscopy (TEM). Results. the respective solubilities of the 4-AETCa in water, 2-hydroxyethyl methacrylate (HEMA; 100wt%) and HEMA/water (70/30wt%) were 0.023, 0.003 and 0.014 mol/l after 2 min. The IR analysis indicated that Ca-carboxylate (new bands: νC=O:1580 and 1413 cm-1) was formed on all dentin specimens following application of 4-AET, with or without NaOCl pretreatment. TEM showed a 1 μm thick hybrid layer with some remnant apatite crystallites that were encapsulated by a layer of less electron-dense material. Significance. the results suggest that ionized carboxyl groups in 4-AET may interact with Ca2+ from apatite crystallites within the partially demineralized hybrid layer to form an insoluble calcium salt (4-AETCa) that may aid in bonding this resin system to dentin.

Original languageEnglish (US)
Pages (from-to)707-715
Number of pages9
JournalDental Materials
Volume19
Issue number8
DOIs
StatePublished - Dec 1 2003

Fingerprint

Dentin
Adhesives
beta-Aminoethyl Isothiourea
Calcium
Apatites
Acids
Apatite
Solubility
Transmission Electron Microscopy
Crystallites
Resins
Transmission electron microscopy
Water
Fourier Analysis
4-acryloxyethyltrimellitic acid
Fourier transforms
Salts
Acoustic waves
Electrons
Infrared radiation

Keywords

  • Ca-carboxylate
  • Dentin apatite
  • FT-IR/ATR
  • Transmission electron microscopy

ASJC Scopus subject areas

  • Materials Science(all)
  • Dentistry(all)
  • Mechanics of Materials

Cite this

Bonding mechanism and ultrastructural interfacial analysis of a single-step adhesive to dentin. / Ikemura, Kunio; Tay, Franklin Chi Meng; Hironaka, Toshiya; Endo, Takeshi; Pashley, David Henry.

In: Dental Materials, Vol. 19, No. 8, 01.12.2003, p. 707-715.

Research output: Contribution to journalArticle

Ikemura, Kunio ; Tay, Franklin Chi Meng ; Hironaka, Toshiya ; Endo, Takeshi ; Pashley, David Henry. / Bonding mechanism and ultrastructural interfacial analysis of a single-step adhesive to dentin. In: Dental Materials. 2003 ; Vol. 19, No. 8. pp. 707-715.
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AU - Ikemura, Kunio

AU - Tay, Franklin Chi Meng

AU - Hironaka, Toshiya

AU - Endo, Takeshi

AU - Pashley, David Henry

PY - 2003/12/1

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AB - Objectives. to characterize the interaction of 4-acryloxyethyltrimellitic acid (4-AET), a key ingredient in a commercial all-in-one adhesive (Reactmer Bond) with dentin apatite, to measure the solubility of 4-AET calcium (4-AETCa), and to examine the ultrastructure of the resin-dentin interface bonded by this adhesive. Methods. solubility of synthesized 4-AETCa in several solutions was measured. Flattened bovine dentin blocks were treated with 0.1wt% NaOCl for 10 min, or 5.0wt% NaOCl for 10 min, or 30 min. Fourier transform infrared analysis using attenuated total reflection (FT-IR/ATR) was performed on these four substrates before and after treatment with a 4-AET mixture (4-AET/HEMA: 40/60wt%). Undemineralized, unstained sections of human sound dentin that were bonded with the same comonomers were examined by transmission electron microscopy (TEM). Results. the respective solubilities of the 4-AETCa in water, 2-hydroxyethyl methacrylate (HEMA; 100wt%) and HEMA/water (70/30wt%) were 0.023, 0.003 and 0.014 mol/l after 2 min. The IR analysis indicated that Ca-carboxylate (new bands: νC=O:1580 and 1413 cm-1) was formed on all dentin specimens following application of 4-AET, with or without NaOCl pretreatment. TEM showed a 1 μm thick hybrid layer with some remnant apatite crystallites that were encapsulated by a layer of less electron-dense material. Significance. the results suggest that ionized carboxyl groups in 4-AET may interact with Ca2+ from apatite crystallites within the partially demineralized hybrid layer to form an insoluble calcium salt (4-AETCa) that may aid in bonding this resin system to dentin.

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KW - Transmission electron microscopy

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