PEGDA, acrylonitrile, and HMP were measured at the mass shown in Table 1 and mixed with polyacrylamide (PAA) solution (10 g/L). After dissolution, nitrogen gas was purged to the solution to remove oxygen for 1 min. The solution was added to a petri dish and sealed at the nitrogen atmosphere. A UV lamp at the wavelength of 365 nm was irradiated to the solution for polymerization for one hour at room temperature in a dark room. The heat flux was set at 0.72 × 10−3 W/cm2. After the polymerization, the obtained membrane was washed with water repeatedly. The membrane without added PAA was also prepared with the same procedure for comparison. The porosity of the membrane was determined by the weight change before and after the membrane was immersed in water. To determine the elastic modulus of the membrane, the dynamic ultra micro hardness tester (DUH-211S, Shimadzu, Kyoto, Japan) was performed three times.
Duh 211
Manufactured by Shimadzu
Sourced in Japan
The DUH-211 is a differential thermal analyzer (DTA) that measures the thermal properties of materials. It can detect phase changes, chemical reactions, and other thermal events in a sample as it is heated or cooled. The DUH-211 provides data on the temperature and heat flow of the sample relative to a reference material.
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15 protocols using duh 211
1
Synthesis and Characterization of PEGDA-Based Membranes
2
Microhardness and Elastic Modulus Measurement
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For each sample, MH and Eit* measurements were performed using a digital dynamic ultra-microhardness tester (DUH-211S, Shimadzu, Kyoto, Japan) with a Vickers indenter tip under a 500 mN load, at 70.0670 mN/s loading speed for 5 s of holding time. Five indentations were made in the central region of each sample with 100 μm between each one. Mean MH and Eit* measurements were obtained for each sample.
The MH value (N/mm2 ) is defined as the maximum force (F max) divided by the surface area of the indenter, multiplied by the squared penetration depth (h):
The Eit* value was calculated according to the following equation:
Here v and vi are Poisson's coefficient (defined as the property between the specific transverse and longitudinal deformations) of the sample and indenter, respectively, and Ei is the elastic modulus of the indenter.
The MH value (N/mm
The Eit* value was calculated according to the following equation:
Here v and vi are Poisson's coefficient (defined as the property between the specific transverse and longitudinal deformations) of the sample and indenter, respectively, and Ei is the elastic modulus of the indenter.
3
Nanoindentation for Material's Young's Modulus
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Nanoindentation was carried out to determine the specimen’s Young’s modulus by applying the load-unload method [19 (link)–21 (link)]. The polished specimen was indented (loaded-unloaded) using a three-faced Berkovich tip by Shimadzu DUH-211S. The parameters involved were test force, loading speed, and hold time of 300 mN, 14.01 mN/sec and 5 s, respectively. The specimen was indented and the arithmetic average of three different indentations of the same level served to determine Young’s modulus. The sample’s 0.189 Poisson’s ratio was extracted from the CRC Materials Science and Engineering handbook and placed in DUH software to calculate Young’s modulus [22 ].
4
Nanomechanical Properties of PEF and PEF/GNP
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The nanomechanical properties of the amorphous and semicrystalline neat PEF and PEF/GNP nanocomposite materials were studied by nanoindentation testing. The nanoindentation measurements, using a dynamic ultra-microhardness tester DUH-211S (Shimadzu Co., Kyoto, Japan), were conducted using a 100 nm-radius triangular pyramid indenter tip (Berkovich-type indenter) at room temperature (23 °C). The nanoindenter was loaded onto the surface of the films until a load peak of 20 mN was reached, and this was held for 3 s. Subsequently, the nanoindenter was unloaded, leading to the value of zero. The indentation depth was recorded as a function of load and the maximum load was applied to the nanoindenter during the creep time. In this study, the basic mechanical properties that were determined were the hardness and elastic modulus of the amorphous and semicrystalline neat PEF and their PEF/GNP nanocomposite samples using the Oliver and Pharr method and previous work [59 (link),60 (link),61 (link),62 (link),63 (link),64 ,65 (link)]. The average value of ten measurements taken at different locations was used to calculate these properties. Moreover, the creep displacement was investigated during the nanoindentation testing.
5
Bone Microindentation Characterization
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Microindentation was used to test the bone local changes in elastic modulus and
hardness with the modified protocols previously described in Kaya et
al. (30 (link)). Microindentation enables
the measurement of the region consisting of numerous canaliculi and at least one
osteocyte nearby. Vickers hardness and elastic modulus of the bone sections were
measured using a microhardness tester (DUH-211S; Shimadzu, Tokyo, Japan). The region
of interest was set at the central part of trabecular bone section at least 20
µm away from the boundary. A total of 10 impressions were performed in each
bone section. With modified protocol of previous reports (31 (link)), the test was conducted with a load of 100 mN for 20 s,
loading speed of 6.6 mN/s, minimum force of 0.2 mN, and Poisson’s ratio of
0.200.
hardness with the modified protocols previously described in Kaya et
al. (30 (link)). Microindentation enables
the measurement of the region consisting of numerous canaliculi and at least one
osteocyte nearby. Vickers hardness and elastic modulus of the bone sections were
measured using a microhardness tester (DUH-211S; Shimadzu, Tokyo, Japan). The region
of interest was set at the central part of trabecular bone section at least 20
µm away from the boundary. A total of 10 impressions were performed in each
bone section. With modified protocol of previous reports (31 (link)), the test was conducted with a load of 100 mN for 20 s,
loading speed of 6.6 mN/s, minimum force of 0.2 mN, and Poisson’s ratio of
0.200.
6
Nanohardness Analysis of Eroded Enamel
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Following the analysis of surface loss, samples were cross-sectioned, exposing the inner surface of the enamel. One half of each enamel slab was randomly selected and embedded in acrylic resin. After, the enamel surface was exposed by flattening and polishing (800, 1,200, 2,400 and 4,000 grit of Al 2 O 3 papers). The polished specimen was then ultrasonically washed in deionized water for 3 min. Nanohardness measurements of the "near-surface demineralized zone" of the enamel section were performed with a Berkovich tip attached to an Ultra-Microhardness Tester (DUH-211S, Shimadzu, Tokyo, Japan) using a load of 25 mN, by a blinded-operator (operator P.M.A.N.). Loading and unloading speeds were set at 0.01mN/µs. For each specimen, three columns of 10 indentations each were made, one in the central region of the in situ eroded dental enamel and the other two columns at a 300-µm distance from both sides of the central row of indentations (right and left). The indentations were made at 1 µm (P1), 2 µm (P2), 3 µm (P3), 4 µm (P4), 5 µm (P5), 6 µm (P6), 7 µm (P7), 8 µm (P8), 9 µm (P9) and 10 µm (P10) from the outer surface of eroded enamel. The mean values of all 3 measuring points at each distance from the surface were averaged.
7
Dentin Hardness and Elasticity Evaluation
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After polishing the samples, the restored dentin blocks were examined by a dynamic ultra micro hardness tester (DUH-211S; Shimadzu, Kyoto, Japan) to check the HMV (Martens hardness obtained with the Vickers indenter) and elastic modulus (Eit values) of dentin under a load of 3 mN at a speed of 0.2926 mN/s, for 5 s, at the following distances from restorative interface: 10 µm, 30 µm, 50 µm and 70 μm m. Three indentations in all the studied regions were made with a Vickers tip. The HMV value (N/mm 2 ) was defined as the maximum force (F max) divided by the surface area of the indenter x squared penetration depth (h):
The Eit value was calculated according to the equation:
where v and vi are the Poisson's coefficient (defined as the property between the transverse and longitudinal specific deformations) of the sample and the indenter, respectively, and Ei is the elastic modulus of the indenter. The reduced Eit (Er) was calculated by the equation:
where A is the designed area for contact printing, S is the material stiffness obtained from the slope of the unloading curve, and π is 3.14.
In this study, HMV and Eit values were automatically calculated by the equipment software.
The Eit value was calculated according to the equation:
where v and vi are the Poisson's coefficient (defined as the property between the transverse and longitudinal specific deformations) of the sample and the indenter, respectively, and Ei is the elastic modulus of the indenter. The reduced Eit (Er) was calculated by the equation:
where A is the designed area for contact printing, S is the material stiffness obtained from the slope of the unloading curve, and π is 3.14.
In this study, HMV and Eit values were automatically calculated by the equipment software.
8
Comprehensive Material Characterization Protocol
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XRD measurements were performed by Rigaku X-ray diffractometer (SmartLab (3)). SEM measurements were confirmed by Regulus8100 (Hitachi). Water contact angles were measured in air by Dataphysics OCA20. TGA measurements were checked by Q500-TA. Hardness was measured by a nanoindentation instrument (DUH-211, SHIMADZU, Japan) with a pyramidal indenter (pyramidal indenter, TOKYO DIAMOND Tools MFG. Co., Ltd., Japan). AFM measurements were supported by the instrument BRUKER ICON-XR, and measured with RTESPA-300 type tips. High-Resolution Ultraviolet Photoemission Spectra (UPS) were measured by an integrated ultrahigh vacuum system equipped with a multi-technique surface analysis system (VG ESCALAB MK II spectrometer). Infrared Spectroscopy (IR) was measured by VERTEX 80 V-ATR. The photolithography and oxygen reactive ion etching (RIE) process was achieved by Plasmalab Oxford 80 Plus system.
9
Nano-Indentation Hardness and Elasticity of 3Y-TZP
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Indentation hardness and modulus of elasticity (E-modulus) were evaluated by a nano-indentation technique using a dynamic ultra-micro hardness tester (DUH-211; Shimadzu, Kyoto, Japan). Half of the specimens (n = 6) prepared for this analysis were subjected to autoclaving under the same conditions as described above, and the remaining 6 specimens were used without autoclaving. The specimen, fixed in the device using metal strips, was loaded via the Berkovich indenter at a rate of 14 mN/s up to 500 mN. After reaching the maximum load, the force was maintained for 15 s and then unloading was performed at the same rate. Based on the load-displacement curve, nano-indentation hardness and E-modulus were calculated using the device software. For the calculation of E-modulus, Poisson’s ratio of 3Y-TZP was assumed to be 0.3, according to the literature [25 ].
10
PLA Filament Mechanical Properties
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The mechanical performance of neat PLA and PLA/Joncryl filaments was investigated through nanoindentation testing. The hardness of the samples was measured with a dynamic ultra-microhardness tester DUH-211 (Shimadzu Co., Kyoto, Japan) using a 100 nm radius triangular pyramid indenter tip (Berkovich-type indenter). During the indentation test, a controlled load (P) with a peak load of 30 mN was applied through a diamond tip on the surface of the filaments. This peak load was held for 3 s. The indentation depth was recorded as a function of load. Subsequently, the indenter was unloaded to a load of zero. The maximum indentation load was applied to the indenter during the creep time. The modulus and hardness were obtained as the average value of ten measurements.
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