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46 protocols using bis gma

1

Resin Polymer Viscosity Measurement

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Bis-GMA (Aldrich, St. Louis, MO, USA) and TEGDMA (Aldrich) were mixed at the mass ratios of 3:7, 4:6, 5:5, 6:4 and 7:3, respectively, followed by benzoyl peroxide (BPO) (Aldrich) being added at 0.5 wt% in relation to the total weight of Bis-GMA and TEGDMA. In parallel, the mixture of UDMA (Aldrich) and TEGDMA was prepared at the mass ratio of 6:4. These dimethacrylate mixtures were submitted to viscosity measurement by applying Brookfield DV-II+Pro digital viscometer (Middleboro, MA, USA) at room temperature.
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2

Hydrophilic Dental Adhesive Formulation

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The model adhesive consisted of HEMA (Sigma-Aldrich, St. Louis, MO, USA) and BisGMA (Sigma-Aldrich, St. Louis, MO, USA) with a mass ratio of 45/55 (HEMA/BisGMA). The photoinitiators used were as follows: 0.5 wt% camphorquinone (CQ) as a hydrophobic photosensitizer, 0.5 wt% ethyl-4-(dimethylamino)benzoate (EDMAB) as a hydrophobic reducing agent, and 1.0 wt% diphenyliodonium hexafluorophosphate (DPIHP) as a hydrophilic coinitiator (all from Sigma-Aldrich, St. Louis, MO, USA). The neat resins were prepared in brown glass vials and stirred for 48 h to form a homogeneous solution [15 (link)].
D2O (99.9%; Sigma-Aldrich, St. Louis, MO, USA) was added into the neat resins in variable amounts: 0 wt%, 10 wt%, and 16 wt%, based on [5 (link)]. These concentrations of D2O were added according to a ternary phase diagram [16 (link)]. D2O (heavy water) was used instead of water to avoid coincidence of the peaks at the spectrum in the FTIR [16 (link)].
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3

Polymer Composite Mixtures Synthesis

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Eight recipes of polymer mixtures with different ratios and compositions were obtained according to Table 1. Two types of Bis-GMA were used: a commercially available one, Bis-GMAimp (Sigma-Aldrich, Merck, Kenilworth, NJ, USA), and Bis-GMA (2018), manufactured at “Raluca Ripan” Institute for Research in Chemistry, Cluj-Napoca, Romania [20 (link),21 (link)]. All other organic substances and initiation system were used from Sigma-Aldrich, Darmstadt, Germany.
The inorganic phase was synthesized in our laboratory (UBB-ICCRR, Babes-Bolyai University, Raluca Ripan Institute of Research in Chemistry). Glass filler with BaF2 (size 2–6 nm) was obtained by the conventional melting method, and the graphene containing 0.5% Ag was obtained by Hummer’s method from graphite [22 (link)].
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4

Resin Composite Formulations: Mechanical Blending

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Three experimental resin composite formulations were mechanically blended using a centrifugal mixing device (SpeedMixer, DAC 150.1 FVZ-K, Hauschild Engineering, Hamm, North Rhine-Westphalia, Germany). As described in Table 1, the organic resin matrix of all formulations consisted on 60 wt% of Bis-GMA (Sigma-Aldrich Inc., St Louis, MO, USA) combined with 40 wt% of diluent monomer(s). The IBOMA (Sigma-Aldrich Inc.) was used as a diluent monomer for Bis-GMA, alone or in combination with TEGDMA (Sigma-Aldrich Inc.) (1:1). TEGDMA alone as the only diluent monomer was used as control. The chemical structure of each monomer is illustrated in Figure 1. To the resin matrix, 65 wt% of filler particles was added, in which, 13 wt% was 0.05 μm fumed silica (Aerosil OX50, Nippon Aerosil Co. Ltd., Yokkaichi, Tokyo, Japan) and 52 wt% was 0.7 μm BaBSiO 2 glass (Esstech Inc., Essington, PA, USA). A 1:4 filler ratio of silica and glass was used in order to assign proper handling properties to the composites. The photo-initiator system used in all formulations was 0.5 wt% of camphorquinone (Sigma-Aldrich Inc.) combined with 1 wt% of 2-(dimethylamino)ethyl methacrylate, DMAEMA (Sigma-Aldrich Inc.).
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5

Synthesis and Characterization of Dental Monomers

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Ethyl 4-(dimethylamino)benzoate (EDB) and diphenyliodonium hexafluorophosphate (DPI) were purchased from Sigma-Aldrich and their chemical structures are shown in Scheme 2. Bis-GMA and TEGDMA were obtained from Sigma-Aldrich and used with the highest purity available (Scheme 2); Bis-GMA and TEGDMA were selected as benchmarked monomers for free radical polymerization processes.
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6

Synthesis and Characterization of Bioactive Dental Composites

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Bisphenol A–glycidyl methacrylate (BisGMA) and triethylene glycol dimethacrylate (TEGDMA) were purchased from Merck, Darmstadt, Germany. An identical resin matrix containing 60:40 weight ratio of BisGMA: TEGDMA with a photoinitiator system (camphorquinone (0.2 wt %; Merck) and ethyl-4-dimethylamino benzoate (0.8 wt %; Merck)) was used for all materials. Resin was heated to 60 °C prior to admixture of fillers.
Four types of fillers were used in this study, as shown in Table 1.
The materials were mixed in the absence of blue light using an asymmetrical centrifugal mixer (Speed Mixer TM DAC 150 FVZ, Hauschild & Co KG, Hamm, Germany) at gradually increasing speed up to 2700 rpm.
Eight experimental resin composites were prepared, divided into two groups:

Group testing the bimodal approach with 65 wt % total filler load and

Group testing the trimodal approach with 70 wt % total filler load used for investigating 1, 5, and 10 wt % Cu-MBGN composites with silica fillers.

Each group contained both inert control (silica and microfillers; 10-Si and 15-Si) and bioactive control (45S5 BG and microfillers, 10-BG and 15-BG) in adequate amounts corresponding to the total filler load (Table 2).
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7

LiNbO3-Modified Dental Adhesive Formulation

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A dental adhesive was formulated by mixing two methacrylate monomers: bisphenol A glycerolate dimethacrylate (Bis-GMA, Aldrich Chemical Company, St. Louis, Missouri, USA) at 66.66 wt.% and 2-hydroxyethyl methacrylate (HEMA, Aldrich Chemical Company) at 33.33%. Camphorquinone (1 mol%) and ethyl 4-dimethylaminobenzoate (1 mol%) were also used as the photoinitiator and co-initiator, respectively. Butylated hydroxytoluene was used (1 wt.%) as a stabilizer for the inhibition of spontaneous polymerization. These three reagents were also purchased from Aldrich Chemical Company. The adhesive formulated was used as the experimental LiNbO3-free control adhesive. LiNbO3 was incorporated in experimental adhesive resins at different concentrations (1 wt.%, 2 wt.%, and 5 wt.%). The particles of LiNbO3 were milled and sieved (>0.125 mm) and characterized via laser diffraction (CILAS 1180, Orleans, France) for particle size. A light-curing unit (Radii Cal, SDI, Australia) was used for specimens’ photoactivation at 1200 mW/cm2. Experimental adhesives were evaluated as illustrated in Figure 2.
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8

Borate Glass Resin Composite Fabrication

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Borate glass containing 70% boron oxide, 26% strontium oxide and 4% sodium oxide (mole fraction) was synthesized as per MacDonald et al., and sieved to retrieve <25 μm particles [35 (link)]. Particle size distribution was verified using a laser particle size analyzer, in aqueous dispersant (Mastersizer 3000, Malvern, Malvern, Worcs, UK), and confirmed as d10 = 3.38 μm, d50 = 12.1 μm, d90 = 26.4 μm. A series of 15 two-paste resins (Figure 9, Table 1) were fabricated through varying mixtures of HEMA (Aldrich Chemistry, USA), TEGDMA (Aldrich Chemistry, St. Louis, MO, USA), and BisGMA (Aldrich Chemistry, USA). Benzyl peroxide (BPO, Sigma Aldrich, St. Louis, MO, USA) and N,N-Bis(2-hydroxyethyl)-p-toluidine (DHEPT, Aldrich Chemistry, St. Louis, MO, USA) were added to paste one and two respectively, for each composition, to form a chemical initiation system [54 ]. Resin components were shielded from light to prevent photo initiation of benzoyl peroxide, and placed in a shaking incubator at (37 °C, 2 Hz) overnight to reduce resin viscosity and allow for mixing. Resin mixtures were refrigerated until further use, and hand spatulated with the appropriate weight of glass to form both paste components as needed.
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9

Modified Clay Nanocomposites Synthesis

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The monomers triethylene glycol dimethacrylate (TEGDMA), 95%, and 2,2-Bis[p-(2′-hydroxy-3′-methacryloxypropoxy)phenylene]propane (Bis-GMA) were both provided by Aldrich, Taufkirchen, Germany. Co-initiator 2-(Dimethylamino)ethylmethacrylate (DMAEMA), 99%, and initiator camphorquinone, 98%, were purchased from J&K Scientific GmbH, (Lommel, Belgium). Commercially available OMMT, Nanomer® I.34MN, produced by Nanocor Company (Hoffman Estates, IL, USA) and supplied by Aldrich (Taufkirchen, Germany), is an –onium ion modified clay containing 25 to 30 wt % methyl dixydroxyethyl hydrogenated tallow ammonium ion. OMMTs with different intercalating organomodifiers, such as cetyltrimethylammonium chloride (MMT-CTAC), dimethylaminooctadecyl methacrylate (MMT-DMAODM), dimethylaminohexadecyl methacrylate (MMT-DMAHDM), as well as two surface modified analogs, with 3-(trimethoxysilyl)propyl methacrylate, S.MMT-CTAC, and S.MMT-DMAHDM were all prepared in our previous works [49 (link),50 (link)]. The specific chemical structures of all MMT organomofidiers are represented in Figure 1. All other chemicals used were of reagent grade.
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10

Synthesis and Characterization of Dental Composites

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The monomers triethyleneglycol dimethacrylate (TEGDMA), 95%, and 2,2-bis[4-(2-hydroxy-3methacrylyloxy-propoxy)-phenyl] propane (Bis-GMA) were both provided by Aldrich (Sigma-Aldrich Chemie, Taufkirchen, Germany). Co-initiator 2-(Dimethylamino) ethylmethacrylate (DMAEMA), 99%, and initiator camphorquinone, 98%, were purchased from J&K (J&K Scientific, Lommel, Belgium). Commercially available OMMTS with the trade name Nanomer ® I.34MN (Nanocor, Hoffman Estates, IL, USA) and Cloisite ® 20A were supplied by Aldrich (Sigma-Aldrich Chemie) and BYK Additives & Instruments (BYK-Chemie, Wesel, Germany) respectively. They are -onium ion modified clays containing methyl dihydroxyethyl hydrogenated tallow and dimethyl dehydrogenated tallow quaternary ammonium ions respectively. Another OMMT with dimethylaminooctadecyl methacrylate as intercalating organomodifier (MMT-DMAODM) prepared in our previous work was also used 32) . The specific chemical structures of all MMT organomofidiers are represented in Table 1. Phosphate buffered saline (PBS) 10× was provided by Aldrich (Sigma-Aldrich Chemie) and diluted to a 1× working solution. All other chemicals used were of reagent grade.
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