Changes in dental enamel oven heated or irradiated with Er,Cr:YSGG laser. Analysis by FTIR

This study evaluated the change that occurs in dental enamel under action of oven heating or Er,Cr:YSGG laser irradiation aiming to obtain a structure more resistant to demineralization. Enamel powder was obtained from bovine teeth. Samples were subjected to oven heating at temperatures of 200, 400, 600, 800, and 1000°C or during laser irradiation with energy densities of 7.53, 10.95, and 13.74 J/cm². The infrared thermography was used to measure the surface temperature generated in the solid samples of enamel during lasers irradiation. The samples were analyzed by Fourier transform infrared spectroscopy (FTIR), which shows changes on enamel oven heated or laser irradiated, due to treatments, related to carbonates, adsorbed water and hydroxyl content. These compositional effects were more evident in lased samples. These changes may alter the material properties such as its solubility, and decrese of demineralization that is important for caries prevention.     

Low-fluence CO2 laser irradiation decreases enamel solubility

This study investigated whether subablative-pulsed CO₂ laser (10.6 μm) irradiation, using fluences lower than 1 J/cm², was capable of reducing enamel acid solubility. Fifty-one samples of bovine dental enamel were divided into three groups: control group, which was not irradiated (CG); group laser A (LA) irradiated with 0.3 J/cm²; and group laser B (LB) irradiated with 0.7 J/cm². After irradiation, the samples were subjected to demineralization in an acetate buffer solution and were then analyzed by SEM. A finite-element model was used to calculate the temperature increase. The calcium and phosphorous content in the demineralization solution were measured with an ICP-OES. ANOVA and the t-test pairwise comparison (p < 0.016) revealed that LB showed significantly lower mean Ca and P content values in the demineralization solution than other groups. A reduction in the enamel solubility can be obtained with pulsed CO₂ laser irradiation (0.7 J/cm², 135 mJ/pulse, 74 Hz, 100 μs) without any surface photomodification and a less than 2°C temperature increase at a 3-mm depth from the surface.     

Absorption and thermal study of dental enamel when irradiated with Nd:YAG laser with the aim of caries prevention

It is widely recognized that Nd:YAG can increase enamel resistance to demineralization; however, the safe parameters and conditions that enable the application of Nd:YAG laser irradiation in vivo are still unknown. The aim of this study was to determine a dye as a photoabsorber for Nd:YAG laser and to verify in vitro a safe condition of Nd:YAG irradiation for caries prevention. Fifty-eight human teeth were selected. In a first morphological study, four dyes (waterproof India ink., iron oxide, caries indicator and coal paste) were tested before Nd:YAG laser irradiation, under two different irradiation conditions: 60 mJ/pulse and 10 Hz (84.9 J/cm²); 80 mJ/pulse and 10 Hz (113.1 J/cm²). In a second study, the enamel surface and pulp chamber temperatures were evaluated during laser irradiations. All dyes produced enamel surface melting, with the exception of the caries indicator, and coal paste was the only dye that could be completely removed. All irradiation conditions produced temperature increases of up to 615.08°C on the enamel surface. Nd:YAG laser irradiation at 60 mJ/pulse, 10 Hz and 84.9 J/cm² promoted no harmful temperature increase in the pulp chamber (ANOVA, p < 0.05). Among all dyes tested, the coal paste was an efficient photoabsorber for Nd:YAG irradiation, considered feasible for clinical practice. Nd:YAG laser at 84.9 J/cm² can be indicated as a safe parameter for use in caries prevention.     

Effect of Er:YAG laser energy on the morphology of enamel/adhesive system interface

The aim of this study was to evaluate in vitro the influence of Er:YAG laser energy variation to cavity preparation on the morphology of enamel/adhesive system interface, using SEM. Eighteen molars were used and the buccal surfaces were flattened without dentine exposure. The specimens were randomly assigned to two groups, according to the adhesive system (conventional total-etching or self-etching), and each group was divided into three subgroups (bur carbide in turbine of high rotation, Er:YAG laser 250 mJ/4 Hz and Er:YAG laser 300 mJ/4 Hz) containing six teeth each. The enamel/adhesive system interface was serially sectioned and prepared for SEM. The Er:YAG laser, in general, produced a more irregular adhesive interface than the control group. For Er:YAG laser 250 mJ there was formation of a more regular hybrid layer with good tag formation, mainly in the total-etching system. However, Er:YAG laser 300 mJ showed a more irregular interface with amorphous enamel and fused areas, for both adhesive systems. It was concluded that cavity preparation with Er:YAG laser influenced on the morphology of enamel/adhesive system interface and the tissual alterations were more evident when the energy was increased.     

XPS studies of short pulse laser interaction with copper

The effect of laser ablation on copper foil irradiated by a short 30 ns laser pulse was investigated by X-ray photoelectron spectroscopy. The laser fluence was varied from 8 to 16.5 J/cm² and the velocity of the laser beam from 10 to 100 mm/s. This range of laser fluence is characterized by a different intensity of laser ablation. The experiments were done in two kinds of ambient atmosphere: air and argon jet gas.The chemical state and composition of the irradiated copper surface were determined using the modified Auger parameter (α′) and O/Cu intensity ratio. The ablation atmosphere was found to influence the size and chemical state of the copper particles deposited from the vapor plume. During irradiation in air atmosphere the copper nanoparticles react with oxygen and water vapor from the air and are deposited in the form of a CuO and Cu(OH)₂ thin film. In argon atmosphere the processed copper surface is oxidized after exposure to air.     

Modification of Cd1−xMnxTe crystal surface layers by nanopulsed laser irradiation

The surface modification of Cd_1−xMn_xTe (x = 0-0.3) crystal wafers under pulsed laser irradiation has been studied. The samples were irradiated by a Q-switched ruby laser with pulse duration of 80 ns. Optical diagnostics of laser-induced thermal processes were carried out by means of time-resolved reflectivity measurements at wavelengths 0.53 and 1.06 μm. Laser irradiation energy density, E varied in the range of 0.1-0.6 J/cm². Morphology of irradiated surface was studied using scanning electron microscopy. The energy density whereby the sample surface starts to melt, depends on Mn content and is equal to 0.12-0.14 J/cm² for x ≤ 0.2, in the case of x = 0.3 this value is about 0.35 J/cm². The higher Mn content leads to higher melt duration. The morphology of laser irradiated surface changes from a weakly modified surface to a single crystal strained one, with an increase in E. Under irradiation with E in the range of 0.21-0.25 J/cm², the oriented filamentary crystallization is observed. The Te inclusions on the surface are revealed after the irradiation of samples with small content of Mn.     

Caries resistance of lased human root surface with 10.6 μm CO2 laser-thermal,morphological, and microhardness analysis

Although the cariostatic effects of CO₂ laser on enamel have been shown, its effects on root surface demineralization remains uncertain. The objectives of this in vitro research was to establish safe parameters for a pulsed 10.6 μm CO₂ laser and to evaluate its effect on morphological features of the root surface, as well as on the reduction of root demineralization. Ninety-five human root surfaces were randomly divided into five groups: G1-No treatment (control); G2—2.5 J/cm²; G3—4.0 J/cm²; G4—5.0 J/cm²; and G5—6.0 J/cm². Intrapulpal temperature was evaluated during root surface irradiation by a thermocouple and morphological changes were evaluated by SEM. After the surface treatment, the specimens were submitted to a 7-day pH-cycling model. Subsequently, the cross-sectional Knoop microhardness values were measured. For all irradiated groups, intrapulpal temperature changes were less than 1.5°C. Scanning electron microscopy images indicated that fluences as low as 4.0 J/cm² were sufficient to induce morphological changes in the root surface. Additionally, for fluences reaching or exceeding 4.0 J/cm², laser-induced inhibitory effects on root surface demineralization were observed. It was concluded that laser energy density in the range of 4.0 to 6.0 J/cm² could be applied to a dental root to reduce demineralization of this surface without compromising pulp vitality.     

Accumulation morphology on the surface of stainless steel irradiated by a nanosecond Nd:YAG pulsed laser

In this study, results in the irradiation of stainless steel AISI 304 in air with nanosecond laser pulses at laser irradiation power density 4×10⁷ W/cm² are reported. Laser processing parameters, such as wavelengths 532 and 1064 nm, pulse duration 20 ns and repetition rate 10 Hz were used. It is shown that the surface morphology of the stainless steel is related to the number of pulses applied to the same spot. The following surface morphological changes were observed: (i) occurrence of the micro-grains microstructures at wavelengths 532 and 1064 nm after 10 000 pulses irradiation and (ii) occurrence of vermiform-like microstructures at wavelength 1064 nm after 1000 pulses irradiation. Generally, it is concluded that irradiation due to several consecutive pulses caused significant damage and enhanced the stainless steel surface roughness.     

The application of Raman and anti-stokes Raman spectroscopy for in situ monitoring of structural changes in laser irradiated titanium dioxide materials

The use of Raman and anti-stokes Raman spectroscopy to investigate the effect of exposure to high power laser radiation on the crystalline phases of TiO₂ has been investigated. Measurement of the changes, over several time integrals, in the Raman and anti-stokes Raman of TiO₂ spectra with exposure to laser radiation is reported. Raman and anti-stokes Raman provide detail on both the structure and the kinetic process of changes in crystalline phases in the titania material. The effect of laser exposure resulted in the generation of increasing amounts of the rutile crystalline phase from the anatase crystalline phase during exposure. The Raman spectra displayed bands at 144 cm⁻¹ (A1g), 197 cm⁻¹ (Eg), 398 cm⁻¹ (B1g), 515 cm⁻¹ (A1g), and 640 cm⁻¹ (Eg) assigned to anatase which were replaced by bands at 143 cm⁻¹ (B1g), 235 cm⁻¹ (2 phonon process), 448 cm⁻¹ (Eg) and 612 cm⁻¹ (A1g) which were assigned to rutile. This indicated that laser irradiation of TiO₂ changes the crystalline phase from anatase to rutile. Raman and anti-stokes Raman are highly sensitive to the crystalline forms of TiO₂ and allow characterisation of the effect of laser irradiation upon TiO₂. This technique would also be applicable as an in situ method for monitoring changes during the laser irradiation process.     

Nanostructures on SiC surface created by laser microablation

Silicon carbide (SiC), as it is well-known, is inaccessible to usual methods of technological processing. Consequently, it is important to search for alternative technologies of processing SiC, including laser processing, and to study the accompanying physical processes. The work deals with the investigation of pulsed laser radiation influence on the surface of 6H-SiC crystal. The calculated temperature profile of SiC under laser irradiation is shown. Structural changes in surface and near-surface layers of SiC were studied by atomic force microscopy images, photoluminescence, Raman spectra and field emission current-voltage characteristics of initial and irradiated surfaces. It is shown that the cone-shaped nanostructures with typical dimension of 100-200 nm height and 5-10 nm width at the edge are formed on SiC surface under nitrogen laser exposure (λ = 0.337 μm, t_p = 7 ns, E_p = 1.5 mJ). The average values of threshold energy density 〈W_thn〉 at which formation of nanostructures starts on the 0 0 0 1 and surfaces of n-type 6H-SiC(N), nitrogen concentration n_N ≅ 2 × 10¹⁸ cm⁻³, are determined to be 3.5 J/cm² and 3.0 J/cm², respectively. The field emission appeared only after laser irradiation of the surface at threshold voltage of 1000 V at currents from 0.7 μA to 0.7 mA. The main role of the thermogradient effect in the processes of mass transfer in prior to ablation stages of nanostructure formation under UV laser irradiation (LI) was determined. We ascertained that the residual tensile stresses appear on SiC surface as a result of laser microablation. The nanostructures obtained could be applied in the field of sensor and emitting extreme electronic devices.     

High level compressive residual stresses produced in aluminum alloys by laser shock processing

Laser shock processing (LSP) has been proposed as a competitive alternative technology to classical treatments for improving fatigue and wear resistance of metals. We present a configuration and results for metal surface treatments in underwater laser irradiation at 1064 nm. A convergent lens is used to deliver 1.2 J/cm² in a 8 ns laser FWHM pulse produced by 10 Hz Q-switched Nd:YAG, two laser spot diameters were used: 0.8 and 1.5 mm.Results using pulse densities of 2500 pulses/cm² in 6061-T6 aluminum samples and 5000 pulses/cm² in 2024 aluminum samples are presented. High level of compressive residual stresses are produced −1600 MPa for 6061-T6 Al alloy, and −1400 MPa for 2024 Al alloy. It has been shown that surface residual stress level is higher than that achieved by conventional shot peening and with greater depths. This method can be applied to surface treatment of final metal products.     

Laser Shock Processing of 6061-T6 Al alloy with 1064 nm and 532 nm wavelengths

Laser Shock Processing (LSP) has been proposed as a competitive alternative technology to classical treatments for improving fatigue and wear resistance of metals. We present a configuration and results in the LSP concept for metal surface treatments in underwater laser irradiation at 532 nm and 1064 nm. The purpose of the work is to compare the effect of both wavelengths on the same material. A convergent lens is used to deliver 1.2 J/pulse (1064 nm) and 0.9 J/pulse (532 nm) in a 8 ns laser FWHM pulse produced by 10 Hz Q-switched Nd:YAG laser with spots of a 1.5 mm in diameter moving forward along the work piece. A LSP configuration with experimental results using a pulse density of 2500 pulses/cm² and 5000 pulses/cm² in 6061-T6 aluminum samples are presented. High level compressive residual stresses are produced using both wavelengths. It has been shown that surface residual stress level is comparable to that achieved by conventional shot peening, but with greater depths. This method can be applied to surface treatment of final metal products.     

Surface morphology of thin lysozyme films produced by matrix-assisted pulsed laser evaporation (MAPLE)

Thin films of the protein, lysozyme, have been deposited by the matrix-assisted pulsed laser evaporation (MAPLE) technique. Frozen targets of 0.3-1.0 wt.% lysozyme dissolved in ultrapure water were irradiated by laser light at 355 nm with a fluence of 2 J/cm². The surface quality of the thin lysozyme films of different thickness deposited on 7 mm × 7 mm Si-〈1 0 0〉-wafers was investigated with scanning electron microscopy and atomic force microscopy. Already at comparatively low thickness, ∼20 nm, the substrate is covered by intact lysozyme molecules and fragments. The concentration of lysozyme in the ice matrix apparently does not play any significant role for the morphology of the film. The morphology obtained with MAPLE has been compared with results for direct laser irradiation of a pressed lysozyme sample (i.e. pulsed laser deposition (PLD)).     

Raman and IR reflection micro‐spectroscopic study of Er:YAG laser treated permanent and deciduous human teeth

Permanent and deciduous human teeth treated by a dental Er‐doped yttrium‐aluminium‐garnet pulse laser (λ = 2940 nm) as well as by classical drilling tools under conditions typical of the clinical practice were studied by ultraviolet Raman and Fourier transform infrared (FTIR) reflection microspectroscopy. Enamel was analyzed by both spectroscopic methods, whereas dentine was studied only by FTIR reflection because of the high level of photoluminescence continuum background even when a wavelength of 325 nm was used in inelastic light scattering experiments. The applied energy and pulse frequency of the dental laser varied between 200 and 500 mJ and between 10 and 30 Hz, respectively. The most important result is that after the laser treatment, the hydroxyapatite structure in both permanent and deciduous enamel is preserved: the apatite Ca‐P‐O framework remains intact, and the content of channel OH^‐ groups is not changed within experimental uncertainties. The calcium‐phosphate framework of dentine also exhibits negligible laser‐induced changes. The only alterations in enamel induced by laser as well as by mechanical drilling are reduction of the amount of CO₃^2‐ in apatite and changes in the protein conformation. The laser impact on the organic material and carbonate groups is strongest for laser power of 8 W; for powers of 4 or 5 W, the combination of higher pulse energy and lower pulse frequency has less impact than the combination of lower energy and higher frequency. No differences between deciduous and permanent teeth in their resistivity to laser irradiation with λ = 2940 nm were detected. Copyright © 2013 John Wiley & Sons, Ltd.     

Simultaneous three-photon absorption induced ultraviolet upconversion in Pr:Y2SiO5 crystal by femtosecond laser irradiation

Near-infrared to ultraviolet upconversion luminescence was observed in the Pr³⁺:Y₂SiO₅ crystal with 120 fs, 800 nm infrared laser irradiation. The observed emissions at around 270 nm and 305 nm could be assigned to 5d → 4f transitions of Pr³⁺ ions. The relationship between the upconversion luminescence intensity and the pump power of the femtosecond laser reveals that the UV emission belongs to simultaneous three-photon absorption induced upconversion luminescence.     

Gold coatings on polyethyleneterephthalate nano-patterned by F2 laser irradiation

In this work we present periodic surface structures generated by linearly polarized F₂ laser light (157 nm) on polyethyleneterephthalate (PET). Atomic force microscopy was used to study the topological changes induced by the laser irradiation. The laser irradiation induces the formation of periodic ripple structures with a width of ca 130 nm and a height of about 15 nm in the fluence range 3.80-4.70 mJ/cm² and the roughness of the polymer surface increases due to the presence of these periodic structures. Subsequently, the laser modified PET foils were coated with a 50 nm thick gold layer by sputtering. After Au deposition on the PET foils with ripple structure, the roughness of surface decreases in comparison to PET with ripples without Au coating. For 50 nm thick Au layers, the ripple structure is not directly transferred to the gold coating, but it has an obvious effect on the grain size of the coating. With considerably thinner Au layers, the ripple structures are smoothened but preserved.     

Ultra fast melting process in femtosecond laser crystallization of thin a-Si layer

In this paper, we investigated the mechanism of crystallization induced by femtosecond laser irradiation for an amorphous Si (a-Si) thin layer on a crystalline Si (c-Si) substrate. The fundamental, SHG, THG wavelength of a Ti:Sapphire laser was used for the crystallization process. To investigate the processed areas we performed Laser Scanning Microscopy (LSM), Transmission Electron Microscopy (TEM) and Imaging Pump-Probe measurements. Except for 267 nm femtosecond laser irradiation, the crystallization occurred well. The threshold fluences for the crystallization using 800 nm and 400 nm femtosecond laser irradiations were 100 mJ/cm² and 30 mJ/cm², respectively. TEM observation revealed that the crystallization occurred by epitaxial growth from the boundary surface between the a-Si layer and c-Si substrate. The melting depths estimated by Imaging Pump-Probe measurements became shallower when the shorter wavelength was used.     

Bioglass thin films for biomimetic implants

Pulsed laser deposition (PLD) method was used to obtain bioglass (BG) thin film coatings on titanium substrates. An UV excimer laser KrF* (λ = 248 nm, τ = 25 ns) was used for the multi-pulse irradiation of the BG targets with 57 or 61 wt.% SiO₂ content (and Na₂O-K₂O-CaO-MgO-P₂O₅ oxides). The depositions were performed in oxygen atmosphere at 13 Pa and for substrates temperature of 400 °C. The PLD films displayed typical BG of 2-5 μm particulates nucleated on the film surface or embedded in. The PLD films stoichiometry was found to be the same as the targets. XRD spectra have shown, the glass coatings obtained, had an amorphous structure. One set of samples, deposited in the same conditions, were dipped in simulated body fluids (SBFs) and subsequently extracted one by one after several time intervals 1, 3, 7, 14 and 21 days. After washing in deionized water and drying, the surface morphology of the samples and theirs composition were investigated by scanning electron microscopy (SEM), X-ray diffraction (XRD), IR spectroscopy (FTIR) and energy dispersive X-ray analysis (EDX). After 3-7 days the Si content substantially decreases in the coatings and PO₄³⁻ maxima start to increase in FTIR spectra. The XRD spectra also confirm this evolution. After 14-21 days the XRD peaks show a crystallized fraction of the carbonated hydroxyapatite (HAP). The SEM micrographs show also significant changes of the films surface morphology. The coalescence of the BG droplets can be seen. The dissolution and growth processes could be assigned to the ionic exchange between BG and SBFs.     

Preparation of the La0.8Sr0.2MnO3 films on STO and LAO substrates by excimer laser-assisted metal organic deposition using the KrF laser

La_0.8Sr_0.2MnO₃ films were prepared on SrTiO₃ (STO) and LaAlO₃ (LAO) substrates using excimer laser-assisted metal organic deposition (ELAMOD). For the LAO substrate, no epitaxial La_0.8Sr_0.2MnO₃ film was obtained by laser irradiation in the fluence range from 60 to 110 mJ/cm² with heating at 500 °C. On the other hand, an epitaxial La_0.8Sr_0.2MnO₃ film on the STO substrate was formed by laser irradiation in the fluence range from 60 to 100 mJ/cm² with heating at 500 °C. To optimize the electrical properties for an IR sensor, the effects of the laser fluence, the irradiation time and the film thickness on the temperature dependence of the resistance and temperature coefficient of resistance (TCR: defined as 1/R·(dR/dT)) of the LSMO films were investigated. An LSMO film on the STO substrate that showed the maximum TCR of 3.9% at 265 K was obtained by the ELAMOD process using the KrF laser.     

Characterization of Ti6Al4V implant surface treated by Nd:YAG laser and emery paper for orthopaedic applications

A more noble and biocompatible Ti alloy was achieved at fluence of 140 J cm⁻² where the implant indicated a higher degree of hardness (825HV), higher corrosion resistance (−0.21 V) and highest hydrophilicity (i.e. θ_c = 37°) compared with 70° of the control sample. These values corresponded to 58 and 39 mN m⁻¹ of surface tension respectively. The laser treated samples at 140 J cm⁻² showed higher wettability characteristics than mechanically roughened surface. Cell growth and their spreading condition in a specific area were analyzed by SEM and Image J Program software. Clearly, more cells were attached (1.2 × 10⁵) to and spread (488 μm²) over the surface at 140 J cm⁻² than in any other condition. Pathologically, the treated samples indicated no sign of infection.