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Ultrastructural Analysis by Scanning Electron Microscopy of Dental Structures Conditioning with Ortophosphoric Acid and ER.CR - YSGG Laser Irradiation

MetadataDetails
Publication Date2017-02-15
JournalRevista de Chimie
AuthorsCătălina Iulia Săveanu, Oana Dragos, Vlad Dănilă, Corina Cheptea
Citations2
AnalysisFull AI Review Included

Technical Analysis & Documentation: MPCVD Diamond for Precision Surface Modification Studies

Section titled “Technical Analysis & Documentation: MPCVD Diamond for Precision Surface Modification Studies”

6CCVD specializes in providing ultra-high purity, custom-engineered CVD diamond materials for applications requiring extreme mechanical, thermal, and optical properties, including precision surface modification and ablation research. This analysis bridges the advanced sample preparation techniques detailed in the attached research with 6CCVD’s unique material and customization capabilities.


  • Comparative Surface Preparation: The study successfully compared the morphological effects of standard 35% Phosphoric Acid (H₃PO₄) etching versus Erbium, Chromium: Yttrium Scandium Gallium Garnet (Er, Cr: YSGG) LASER irradiation on human dentin structure.
  • Optimal Laser Parameters: Er, Cr: YSGG laser treatment at 3 W power (with 15 Hz frequency and 30% water/60% air cooling) was identified as the optimal setting to improve dentin micromorphology for subsequent material adhesion.
  • Superior Laser Performance: Laser treatment demonstrated better control over demineralization and smear layer removal compared to acid etching times exceeding 10 seconds, which caused severe demineralization and destruction of the underlying dentine support structure.
  • Importance of Power Control: Varying laser power confirmed that low power (0-4 W) increased surface roughness (improving adhesion), while higher power (>4 W) decreased roughness, indicating a critical relationship between power and controlled ablation/modification.
  • Prerequisite Precision Polishing: Sample preparation required meticulous surface finishing using diamond discs and abrasive pastes, achieving a final smoothness of 0.25 ”m, highlighting the necessity of ultra-precision material processing foundational to this research.
  • Targeted Application: The work focuses on optimizing surface conditioning parameters to achieve strong hybridization layers and effective adhesion of restorative nanomaterials.

ParameterValueUnitContext
Laser TypeEr, Cr: YSGGN/ABiolase Waterlase-MD
Optimal Laser Power3WFor best micromorphology/adhesion improvement
Laser Frequency15HzUsed in conjunction with 3W power
Laser Medium30% Water / 60% AirN/ACooling and hydration medium
Etching Agent35%H₃PO₄Orthophosphoric Acid concentration
Optimal Etching Time5 - 10sAcid action time for favorable adhesion
Sample Polishing Finish0.25”mFinal grit size using abrasive paste
SEM InstrumentJSM 6390SN/AJEOL Scanning Electron Microscope
EDS Element: Carbon (C K)0.277keVMass% 56.76; Atom% 69.50
EDS Element: Calcium (Ca K)3.690keVMass% 11.29; Atom% 4.14 (Key mineral component)
Severe Demineralization Threshold> 10sH₃PO₄ etching time causing matrix destruction

The experiment involved strict control over material preparation and surface conditioning to evaluate ultrastructural changes via SEM/EDS.

  1. Sample Preparation:

    • Human premolar and molar samples were sectioned mesial-distal in the longitudinal direction.
    • Samples were ground using diamond discs and SiC paper (400, 600, 1200, 2400 grit).
    • Samples were polished further using gums and abrasive paste to a 0.25 ”m finish under continuous irrigation.
  2. Conditioning Groups (5 Groups):

    • GR. 1-4 (Acid Etching): Conditioned with 35% H₃PO₄ for 5 s, 10 s, 15 s, and 20 s, followed by a 10 s rinse with distilled water.
    • GR. 5 (Laser Irradiation): Conditioned using the Er, Cr: YSGG laser (Biolase Waterlase-MD) at 3 W / 15 Hz, utilizing a 30% water and 60% air cooling medium.
  3. Post-Conditioning Storage:

    • All conditioned teeth were stored in saline solution for 48 hours.
  4. Characterization:

    • Ultrastructure was analyzed using Scanning Electron Microscopy (SEM).
    • Elemental composition was analyzed using Energy-Dispersive X-ray Spectroscopy (EDS).

This research demonstrates a core engineering challenge: achieving precise, repeatable, and non-destructive surface modification on hard, composite materials. 6CCVD’s MPCVD diamond expertise directly supports researchers and engineers replicating or extending these high-precision surface studies on advanced materials, or utilizing diamond as a tooling/ablation reference standard.

To replicate the ultra-smooth surfaces necessary for high-magnification SEM analysis or to use diamond as a superior optical/mechanical substrate for laser interaction studies, 6CCVD recommends:

6CCVD MaterialApplication Rationale
Optical Grade SCD (Single Crystal Diamond)Required for studies involving precision laser ablation (like Er: YAG/YSGG). SCD offers exceptional purity, high thermal conductivity, and unmatched surface quality (Ra < 1 nm polishing capability), ideal for eliminating spurious scattering effects often seen in biological or composite samples.
PCD (Polycrystalline Diamond) WafersSuitable for large-area testing (up to 125 mm diameter) where high throughput laser processing or scaled-up abrasion/erosion tests are needed.
Boron-Doped Diamond (BDD)If the subsequent application involves electrochemical analysis or sensor integration related to the etched surface, BDD provides a stable, electrically conductive platform.

The success of the reported methodology hinges on repeatable sample preparation and achieving defined surface morphologies (e.g., controlling roughness for adhesion). 6CCVD excels in providing the critical material foundations for such precision work:

  • Ultra-Precision Polishing: While the paper achieved a 0.25 ”m finish on dentin, 6CCVD provides Ra < 1 nm polishing on Single Crystal Diamond and Ra < 5 nm on inch-size Polycrystalline Diamond. This level of atomic-scale flatness is critical for baseline calibration in laser-material interaction studies.
  • Custom Dimensions and Substrates: 6CCVD can supply SCD or PCD in specific dimensions and thicknesses (SCD: 0.1 ”m - 500 ”m; Substrates up to 10 mm), enabling custom mounting and setup for specialized ablation chambers.
  • Advanced Micro-structuring: We offer custom laser cutting and etching services to define precise test areas, apertures, or micro-channels on diamond surfaces, analogous to the controlled tubule exposure sought in the paper.
  • Integrated Metalization Services: For studies requiring subsequent bonding, adhesion measurement, or electrical contacts (often necessary in micro-sensor integration or bonding layer analysis), 6CCVD provides in-house metalization using materials like Au, Pt, Pd, Ti, W, and Cu, allowing for complex thin-film structures to be deposited directly onto the diamond substrate.

The relationship between surface roughness, laser power, and adhesion—a key finding of the research—is a complex parameter space. 6CCVD’s in-house PhD-level engineering team specializes in the material science of diamond surface chemistry and mechanical finishing. We can assist researchers with:

  1. Material Selection: Determining the optimal CVD diamond grade (e.g., optical vs. electronic) required for specific laser wavelengths and power densities (e.g., Er, Cr: YSGG lasers commonly operate at 2.78 ”m).
  2. Ablation Studies: Consulting on diamond substrate preparation for high-power laser ablation tests and optimizing surface finish to study damage mechanisms or controlled micro-patterning.
  3. Hybrid Layer Formation: Advising on optimal metalization schemes and polishing protocols for projects involving creating stable hybrid interfaces between diamond and subsequent thin-film composites or restorative materials.

For custom specifications or material consultation, visit 6ccvd.com or contact our engineering team directly.

View Original Abstract

This study evaluated the ultra-morphological effects of ortophosforic acid and Er.Cr: YSGGLASER on human dentin by means of a field emission in-lens scanning electron microscope. The study was conducted in vitro on human teeth extracted for orthodontic or periodontal reasons, after obtaining informed consent of patients. The samples were sectioned mesial-distal in the longitudinal direction (diamond discs) finished 400, 600, 1200 and 2400 grit SiC paper, polished with gums and abrasive paste 6, 3, 1 and 0,25 mm under continuous irrigation. The samples were divided in five groups depending on the type of conditioning as follows: GR.1= 5 s; GR.2= 10 s; GR.3= 15 s; GR.4= 20 s; GR.5= Er,Cr: YSGGlaser irradiating at 30% water and 60% air at 3W/15 Hz. The materials used for conditioning the teeth were SEïżœ35% (Scotchbondïżœ Etchant Phosphoric Acid -3M ESPE-Seefeld, Germany) and MG6-MZ6 tipswith Er, Cr: YSGGlaser (Biolase Waterlase-MD), according to manufacturerïżœs instructions. The specimens were prepared for observation under SEM with ïżœ1,000 and ïżœ4,000 magnifications. The acid type, concentration and time of action determines dentin demineralization and modifying or removing smear layer. Er.Cr: YSGG laser treatment of non-carious dentin, a laser power of 3 W is found to be the optimal to improve the micromorphology of dentin.