Endodontic Radiopacifying Application of Barium Titanate Prepared through a Combination of Mechanical Milling and Heat Treatment.

Mineral trioxide aggregates (MTA) are commonly used as endodontic filling materials but suffer from a long setting time and tooth discoloration. In the present study, the feasibility of using barium titanate (BTO) for discoloration and a calcium chloride (CaCl2) solution to shorten the setting time was investigated. BTO powder was prepared using high-energy ball milling for 3 h, followed by sintering at 700-1300 °C for 2 h. X-ray diffraction was used to examine the crystallinity and crystalline size of the as-milled and heat-treated powders. MTA-like cements were then prepared using 20-40 wt.% BTO as a radiopacifier and solidified using a 0-30% CaCl2 solution. The corresponding radiopacity, diametral tensile strength (DTS), initial and final setting times, and discoloration performance were examined. The experimental results showed that for the BTO powder prepared using a combination of mechanical milling and heat treatment, the crystallinity and crystalline size increased with the increasing sintering temperature. The BTO sintered at 1300 °C (i.e., BTO-13) exhibited the best radiopacity and DTS. The MTA-like cement supplemented with 30% BTO-13 and solidified with a 10% CaCl2 solution exhibited a radiopacity of 3.68 ± 0.24 mmAl and a DTS of 2.54 ± 0.28 MPa, respectively. In the accelerated discoloration examination using UV irradiation, the color difference was less than 1.6 and significantly lower than the clinically perceptible level (3.7). This novel MTA exhibiting a superior color stability, shortened setting time, and excellent biocompatibility has potential for use in endodontic applications.

Discoloration Improvement by Mechanically-Milled Binary Oxides as Radiopacifier for Mineral Trioxide Aggregates.

Mineral trioxide aggregates (MTA) have been widely used in endodontic treatments, but after some time, patients suffer tooth discoloration due to the use of bismuth oxide (Bi2O3) as a radiopacifier. Replacement of Bi2O3 with high energy ball-milled single (zirconia ZrO2; hafnia, HfO2; or tantalum pentoxide, Ta2O5) or binary oxide powder was attempted, and corresponding discoloration improvement was investigated in the present study. Bi2O3-free MTA is expected to exhibit superior discoloration. The radiopacity, diametral tensile strength, and discoloration of MTA-like cements prepared from the as-milled powder were investigated. Experimental results showed that MTA-like cements prepared using Ta2O5 exhibited a slightly higher radiopacity than that of HfO2 but had a much higher radiopacity than ZrO2. Milling treatment (30 min to 3 h) did not affect the radiopacities significantly. These MTA-like cements exhibited superior color stability (all measured ΔE00 < 1.0) without any perceptible differences after UV irradiation. MTA-like cements prepared using ZrO2 exhibited the best color stability but the lowest radiopacity, which can be improved by introducing binary oxide. Among the investigated samples, MTA-like cement using (ZrO2)50(Ta2O5)50 exhibited excellent color stability and the best overall performance with a radiopacity of 3.25 mmAl and a diametral tensile strength of 4.39 MPa.

Effect of synthesis time on plasmonic properties of Ag dendritic nanoforests.

The effects of synthesis time on the plasmonic properties of Ag dendritic nanoforests on Si substrate (Ag-DNF/Si) samples synthesized through the fluoride-assisted galvanic replacement reaction were investigated. The Ag-DNF/Si samples were characterized using scanning electron microscopy, energy-dispersive X-ray spectroscopy, reflection spectroscopy, X-ray diffraction and surface-enhanced Raman spectroscopy (SERS). The prolonged reaction time led to the growth of an Ag-DNF layer and etched Si hole array. SEM images and variations in the fractal dimension index indicated that complex-structure, feather-like leaves became coral-like branches between 30 and 60 min of synthesis. The morphological variation during the growth of the Ag DNFs resulted in different optical responses to light illumination, especially those of light harvest and energy transformation. The sample achieved the most desirable light-to-heat conversion efficiency and SERS response with a 30 min growth time. A longer synthesis time or thicker Ag-DNF layer on the Si substrate did not have superior plasmonic properties.

Effect of Tantalum Pentoxide Addition on the Radiopacity Performance of Bi2O3/Ta2O5 Composite Powders Prepared by Mechanical Milling.

Among the various phases of bismuth oxide, the high temperature metastable face-centered cubic δ phase attracts great attention due to its unique properties. It can be used as an ionic conductor or an endodontic radiopacifying material. However, no reports concerning tantalum and bismuth binary oxide prepared by high energy ball milling and serving as a dental radiopacifier can be found. In the present study, Ta2O5-added Bi2O3 composite powders were mechanically milled to investigate the formation of these metastable phases. The as-milled powders were examined by X-ray diffraction and scanning electron microscopy to reveal the structural evolution. The as-milled composite powders then served as the radiopacifier within mineral trioxide aggregates (i.e., MTA). Radiopacity performance, diametral tensile strength, setting times, and biocompatibility of MTA-like cements solidified by deionized water, saline, or 10% calcium chloride solution were investigated. The experimental results showed that subsequent formation of high temperature metastable ß-Bi7.8Ta0.2O12.2, δ-Bi2O3, and δ-Bi3TaO7 phases can be observed after mechanical milling of (Bi2O3)95(Ta2O5)5 or (Bi2O3)80(Ta2O5)20 powder mixtures. Compared to its pristine Bi2O3 counterpart with a radiopacity of 4.42 mmAl, long setting times (60 and 120 min for initial and final setting times) and 84% MG-63 cell viability, MTA-like cement prepared from (Bi2O3)95(Ta2O5)5 powder exhibited superior performance with a radiopacity of 5.92 mmAl (the highest in the present work), accelerated setting times (the initial and final setting time can be shortened to 25 and 40 min, respectively), and biocompatibility (94% cell viability).

Effects of Milling Time, Zirconia Addition, and Storage Environment on the Radiopacity Performance of Mechanically Milled Bi2O3/ZrO2 Composite Powders.

Mineral trioxide aggregate (MTA) typically consists of Portland cement (75 wt.%), bismuth oxide (20 wt.%), and gypsum (5 wt.%) and is commonly used as endodontic cement. Bismuth oxide serving as the radiopacifying material reveals the canal filling effect after clinical treatment. In the present study, bismuth/zirconium oxide composite powder was prepared by high energy ball milling of (Bi2O3)100-x (ZrO2)x (x = 5, 10, 15, and 20 wt.%) powder mixture and used as the radiopacifiers within MTA. The crystalline phases of the as-milled powders were examined by the X-ray diffraction technique. The radiopacities of MTA-like cements prepared by using as-milled composite powders (at various milling stages or different amount of zirconia addition) were examined. In addition, the stability of the as-milled powders stored in an ambient environment, an electronic dry box, or a glove box was investigated. The experimental results show that the as-milled powder exhibited the starting powder phases of Bi2O3 and ZrO2 and the newly formed δ-Bi7.38Zr0.62O2.31 phase. The longer the milling time or the larger the amount of the zirconia addition, the higher the percentage of the δ-Bi7.38Zr0.62O2.31 phase in the composite powder. All the MTA-like cements prepared by the as-milled powder exhibited a radiopacity higher than 4 mmAl that is better than the 3 mmAl ISO standard requirement. The 30 min as-milled (Bi2O3)95(ZrO2)5 composite powder exhibited a radiopacity of 5.82 ± 0.33 mmAl and degraded significantly in the ambient environment. However, storing under an oxygen- and humidity-controlled glove box can prolong a high radiopacity performance. The radiopacity was 5.76 ± 0.08 mmAl after 28 days in a glove box that was statistically the same as the original composite powder.

Effect of Oxygen Concentration and Tantalum Addition on the Formation of High Temperature Bismuth Oxide Phase by Mechanochemical Reaction.

High-temperature face-centered cubic bismuth oxide phase is a material of great interest given its unique properties. In the present study, α-Bi2O3 and tantalum powders were used as the starting powders for the formation of high-temperature bismuth oxide phase via mechanochemical synthesis by high energy ball milling. (Bi2O3)80(Ta)20 and (Bi2O3)95(Ta)5 in weight concentrations were milled in either an oxygen-free argon-filled glove box environment or an ambient atmosphere to investigate the effects of oxygen concentration and tantalum addition. The as-milled powders were examined using X-ray diffraction, scanning electron microscopy with energy-dispersive spectroscopy, and differential scanning calorimetry to reveal the structural evolution. The experimental results showed that for (Bi2O3)95(Ta)5 powder mixtures milled within the glove box, tantalum gradually reacted with the α-Bi2O3 phase and formed a ß-Bi7.8Ta0.2O12.2 phase. For (Bi2O3)80(Ta)20 milled under the same conditions, Ta and α-Bi2O3 mechanochemically reacted to form δ-Bi3TaO7 and bismuth after 10 min of high energy ball milling, whereas milling (Bi2O3)80(Ta)20 under the ambient atmosphere with a much higher oxygen concentration accelerated the mechanochemical reaction to less than five minutes of milling and resulted in the formation of high-temperature δ-Bi3TaO7 phase.

A High Performance Impedance-based Platform for Evaporation Rate Detection.

This paper describes the method of a novel impedance-based platform for the detection of the evaporation rate. The model compound hyaluronic acid was employed here for demonstration purposes. Multiple evaporation tests on the model compound as a humectant with various concentrations in solutions were conducted for comparison purposes. A conventional weight loss approach is known as the most straightforward, but time-consuming, measurement technique for evaporation rate detection. Yet, a clear disadvantage is that a large volume of sample is required and multiple sample tests cannot be conducted at the same time. For the first time in literature, an electrical impedance sensing chip is successfully applied to a real-time evaporation investigation in a time sharing, continuous and automatic manner. Moreover, as little as 0.5 ml of test samples is required in this impedance-based apparatus, and a large impedance variation is demonstrated among various dilute solutions. The proposed high-sensitivity and fast-response impedance sensing system is found to outperform a conventional weight loss approach in terms of evaporation rate detection.