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Materials, Volume 5, Issue 2 (February 2012) – 11 articles , Pages 210-363

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124 KiB  
Review
Carbon Nanomaterials: Efficacy and Safety for Nanomedicine
by Takuya Yamashita, Kohei Yamashita, Hiromi Nabeshi, Tomoaki Yoshikawa, Yasuo Yoshioka, Shin-ichi Tsunoda and Yasuo Tsutsumi
Materials 2012, 5(2), 350-363; https://doi.org/10.3390/ma5020350 - 21 Feb 2012
Cited by 55 | Viewed by 8470
Abstract
Carbon nanomaterials, including fullerenes, carbon nanohorns, and carbon nanotubes, are increasingly being used in various fields owing to these materials’ unique, size-dependent functions and physicochemical properties. Recently, because of their high variability and stability, carbon nanomaterials have been explored as a novel tool [...] Read more.
Carbon nanomaterials, including fullerenes, carbon nanohorns, and carbon nanotubes, are increasingly being used in various fields owing to these materials’ unique, size-dependent functions and physicochemical properties. Recently, because of their high variability and stability, carbon nanomaterials have been explored as a novel tool for the delivery of therapeutic molecules including peptide and nucleic acid cancer drugs. However, insufficient information is available regarding the safety of carbon nanomaterials for human health, even though such information is vital for the development of safe and effective nanomedicine technologies. In this review, we discuss currently available information regarding the safety of carbon nanomaterials in nanomedicine applications, including information obtained from our own studies; and we discuss types of carbon nanomaterials that demonstrate particular promise for safe nanomedicine technologies. Full article
(This article belongs to the Special Issue Carbon Nanotubes: Synthesis, Characterization and Applications)
1182 KiB  
Article
Challenges and Strategies in the Synthesis of Mesoporous Alumina Powders and Hierarchical Alumina Monoliths
by Sarah Hartmann, Alexander Sachse and Anne Galarneau
Materials 2012, 5(2), 336-349; https://doi.org/10.3390/ma5020336 - 20 Feb 2012
Cited by 41 | Viewed by 9137
Abstract
A new rapid, very simple and one-step sol-gel strategy for the large-scale preparation of highly porous γ-Al2O3 is presented. The resulting mesoporous alumina materials feature high surface areas (400 m2 g−1), large pore volumes (0.8 mL g [...] Read more.
A new rapid, very simple and one-step sol-gel strategy for the large-scale preparation of highly porous γ-Al2O3 is presented. The resulting mesoporous alumina materials feature high surface areas (400 m2 g−1), large pore volumes (0.8 mL g−1) and the γ-Al2O3 phase is obtained at low temperature (500 °C). The main advantages and drawbacks of different preparations of mesoporous alumina materials exhibiting high specific surface areas and large pore volumes such as surfactant-nanostructured alumina, sol-gel methods and hierarchically macro-/mesoporous alumina monoliths have been analyzed and compared. The most reproducible synthesis of mesoporous alumina are given. Evaporation-Induced Self-Assembly (EISA) is the sole method to lead to nanostructured mesoporous alumina by direct templating, but it is a difficult method to scale-up. Alumina featuring macro- and mesoporosity in monolithic shape is a very promising material for in flow applications; an optimized synthesis is described. Full article
(This article belongs to the Special Issue Advances in Porous Inorganic Materials)
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Graphical abstract

Graphical abstract
Full article ">Figure 1
<p>Schematic depiction of the formation of the nanostructured mesoporous alumina via the evaporation-induced self-assembly mechanism (EISA). The TEM image was taken from our own preparation (see experimental section) of an as-synthesized alumina material showing the 2D-hexagonally arrangement of mesopores (calcined at 400 °C for 4 h).</p> Full article ">Figure 2
<p>(<b>A</b>) Nitrogen sorption isotherm at 77 K of hexagonal mesoporous alumina with amorphous walls; (<b>B</b>) corresponding TEM image of the 2D-hexagonally arranged mesopore system; (<b>C</b>) Small X-Ray Diffraction recorded in the range showing the hexagonal arrangement; (<b>D</b>) <sup>27</sup>Al MAS NMR spectra recorded at a spinning rate of 10 kHz.</p> Full article ">Figure 3
<p>Synthesis route for the rapid preparation of disordered mesoporous γ-Al<sub>2</sub>O<sub>3</sub>.</p> Full article ">Figure 4
<p>(<b>A</b>) Nitrogen sorption isotherms at 77 K of mesoporous disordered γ-Al<sub>2</sub>O<sub>3</sub> phase calcined at 500 °C; (<b>B</b>) TEM image showing the fibrillar morphology of the material; (<b>C</b>) XRD pattern showing the peaks assigned to the γ-Al<sub>2</sub>O<sub>3</sub> phase; (<b>D</b>) <sup>27</sup>Al MAS NMR spectra for which penta-coordinated Al sites are absent as expected for a crystalline alumina phase.</p> Full article ">Figure 5
<p>Photograph of the alumina monolith after calcination at 500 °C and the corresponding SEM pictures showing its isotropic and homogeneous macroporous network (macropores ~1 µm) and its skeleton (thickness ~1 µm).</p> Full article ">Figure 6
<p>SEM images exhibiting the impact of the varying molar ratio of PEO (M<sub>V</sub> = 10<sup>6</sup>) on the resulting morphologies in the micrometre range (<b>A</b>) Al/PEO = 1/3.9 × 10<sup>−6</sup>; (<b>B</b>) Al/PEO = 1/4.5 × 10<sup>−6</sup>; (<b>C</b>) Al/PEO = 1/5.1 × 10<sup>−6</sup>.</p> Full article ">Figure 7
<p>(<b>A</b>) Typical N<sub>2</sub> sorption isotherm at 77 K for alumina monoliths and (<b>B</b>) <sup>27</sup>Al MAS NMR spectra recorded at a steady spin rate of 10 kHz of an alumina monolith (Al/PEO = 1/5.1 × 10<sup>−6</sup>).</p> Full article ">Figure 8
<p>Hydrolysis reaction of aluminium precursor.</p> Full article ">
555 KiB  
Article
Influence of Carbon Nanotubes on Thermal Stability of Water-Dispersible Nanofibrillar Polyaniline/Nanotube Composite
by Ana López Cabezas, Xianjie Liu, Qiang Chen, Shi-Li Zhang, Li-Rong Zheng and Zhi-Bin Zhang
Materials 2012, 5(2), 327-335; https://doi.org/10.3390/ma5020327 - 17 Feb 2012
Cited by 3 | Viewed by 7337
Abstract
Significant influence on the thermal stability of polyaniline (PANI) in the presence of multi-walled carbon nanotubes (MWCNTs) is reported. By means of in-situ rapid mixing approach, water-dispersible nanofibrillar PANI and composites, consisting of MWCNTs uniformly coated with PANI in the state of emeraldine [...] Read more.
Significant influence on the thermal stability of polyaniline (PANI) in the presence of multi-walled carbon nanotubes (MWCNTs) is reported. By means of in-situ rapid mixing approach, water-dispersible nanofibrillar PANI and composites, consisting of MWCNTs uniformly coated with PANI in the state of emeraldine salt, with a well-defined core-shell heterogeneous structure, were prepared. The de-protonation process in PANI occurs at a lower temperature under the presence of MWCNTs on the polyaniline composite upon thermal treatment. However, it is found that the presence of MWCNTs significantly enhances the thermal stability of PANI’s backbone upon exposure to laser irradiation, which can be ascribed to the core-shell heterogeneous structure of the composite of MWCNTs and PANI, and the high thermal conductivity of MWCNTs. Full article
(This article belongs to the Special Issue Carbon Nanotubes: Synthesis, Characterization and Applications)
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Figure 1

Figure 1
<p>(<b>a</b>) Schematic structure of polyaniline in emeraldine base (PANI-ES) and outer-shell of multi-walled carbon nanotube (MWCNT) and high-resolution scanning electron microscopy (HRSEM) image of (<b>b</b>) nanofibrillar <b>(</b>nf-) PANI; (<b>c</b>) nf-PANI/MWCNT-20wt% and (<b>d</b>) nf-PANI/MWCNT-50wt%. The insets are the optical microscopy images of the films (nf-PANI (b) and nf-PANI/MWCNT-20% (c)) with 200 × 160 μm.</p> Full article ">Figure 2
<p>Raman spectra from the bright and dark region of nf-PANI after being baked in air at (<b>a</b>) 150 °C in air and (<b>b</b>) at 200 °C and those of nf-PANI/MWCNT-20wt% baked at (<b>c</b>) 100 °C and (<b>d</b>) 150 °C, respectively.</p> Full article ">Figure 3
<p>Raman spectra of nf-PANI, nf-PANI/MWCNT-20wt%, nf-PANI/MWCNT-50wt%, and MWCNT collected with 514 nm wavelength laser line at different powers of (<b>a</b>) 0.3; (<b>b</b>) 1.5 and (<b>c</b>) 3mW, respectively; (<b>d</b>) Raman spectra of nf-PANI/MWCNT-20wt% obtained on a fixed spot with variable laser power from 0.3 mW to 3 mW and subsequently back to 0.3 mW.</p> Full article ">Figure 4
<p>Temperature dependence Raman spectra of (<b>a</b>) nf-PANI; (<b>b</b>) nf-PANI/MWCNT-20wt%; and (<b>c</b>) nf-PANI/MWCNT-50wt% in which the thin films were baked in air before Raman measurement.</p> Full article ">
308 KiB  
Article
Synthesis and Properties of Poly(Isothianaphthene Methine)s with Chiral Alkyl Chain
by Yu Innami, Hirotsugu Kawashima, Rafaël H. L. Kiebooms, Hideaki Aizawa, Kiyoto Matsuishi and Hiromasa Goto
Materials 2012, 5(2), 317-326; https://doi.org/10.3390/ma5020317 - 16 Feb 2012
Cited by 7 | Viewed by 7182
Abstract
We synthesized poly(isothianaphthene methine)s with chiral alkyl chains in the substituent. Resultant polymers are soluble in THF and CHCl3. Structure of the polymers was characterized with FT-IR, FT-Raman, and UV-Vis-NIR optical absorption spectroscopy. They showed low-bandgap both in solution and in [...] Read more.
We synthesized poly(isothianaphthene methine)s with chiral alkyl chains in the substituent. Resultant polymers are soluble in THF and CHCl3. Structure of the polymers was characterized with FT-IR, FT-Raman, and UV-Vis-NIR optical absorption spectroscopy. They showed low-bandgap both in solution and in a form of film. Optical activity of the polymers was confirmed with optical rotatory dispersion. Doping effects on the polymer were also examined with UV-Vis-NIR spectroscopy and ESR measurement. Full article
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Figure 1

Figure 1
<p>FT-IR spectra of (–)-poly1 and (+)-poly2.</p> Full article ">Figure 2
<p>FT-Raman spectra of (–)-poly1 and (+)-poly2.</p> Full article ">Figure 3
<p>UV-Vis-NIR absorption spectra of (–)-poly1 and (+)-poly2 in solution (0.03 mM in THF) (solid line) and cast films (dashed line).</p> Full article ">Figure 4
<p>UV-Vis-NIR absorption spectra of (–)-poly1 (<b>a</b>) and (+)-poly2 (<b>b</b>) in THF solution with iodine doping.</p> Full article ">Figure 5
<p>ORD spectra of (–)-poly1 and (+)-poly2 in cast films.</p> Full article ">Figure 6
<p>(<b>a</b>) ESR spectra of (–)-poly1 in bulk state with vapor phase iodine doping; (<b>b</b>) g-Value; (<b>c</b>) intensity, and peak width of (–)-poly1 with vapor phase iodine doping for 0–50 min.</p> Full article ">Figure 7
<p>Synthetic routes to poly(isothianaphthene methine)s with chiral side chains. DIAD = diisopropyl azodicarboxylate.</p> Full article ">
421 KiB  
Review
Sorbate Transport in Carbon Molecular Sieve Membranes and FAU/EMT Intergrowth by Diffusion NMR
by Robert Mueller, Rohit Kanungo, Amrish Menjoge, Mayumi Kiyono-Shimobe, William J. Koros, Steven A. Bradley, Douglas B. Galloway, John J. Low, Sesh Prabhakar and Sergey Vasenkov
Materials 2012, 5(2), 302-316; https://doi.org/10.3390/ma5020302 - 14 Feb 2012
Cited by 3 | Viewed by 7620
Abstract
In this paper we present and discuss selected results of our recent studies of sorbate self-diffusion in microporous materials. The main focus is given to transport properties of carbon molecular sieve (CMS) membranes as well as of the intergrowth of FAU-type and EMT-type [...] Read more.
In this paper we present and discuss selected results of our recent studies of sorbate self-diffusion in microporous materials. The main focus is given to transport properties of carbon molecular sieve (CMS) membranes as well as of the intergrowth of FAU-type and EMT-type zeolites. CMS membranes show promise for applications in separations of mixtures of small gas molecules, while FAU/EMT intergrowth can be used as an active and selective cracking catalyst. For both types of applications diffusion of guest molecules in the micropore networks of these materials is expected to play an important role. Diffusion studies were performed by a pulsed field gradient (PFG) NMR technique that combines advantages of high field (17.6 T) NMR and high magnetic field gradients (up to 30 T/m). This technique has been recently introduced at the University of Florida in collaboration with the National Magnet Lab. In addition to a more conventional proton PFG NMR, also carbon-13 PFG NMR was used. Full article
(This article belongs to the Special Issue Diffusion in Micropores)
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Figure 1

Figure 1
<p>SEM image of a representative particle of FAU/EMT intergrowth.</p> Full article ">Figure 2
<p>Examples of PFG NMR attenuation curves measured for methane diffusion in 6FDA/BPDA using proton (■) and carbon-13 (<math display="inline"> <semantics> <mrow> <mstyle mathcolor="red"> <mo>●</mo> </mstyle> </mrow> </semantics> </math>) PFG NMR. The measurements were performed for the effective diffusion time of 9 ms at T = 321 K. The 13-interval and PGSTE LED PFG NMR pulse sequences were used for proton and carbon-13 measurements, respectively. The line shows the result of fitting both attenuation curves by Equation (1) with n = 1.</p> Full article ">Figure 3
<p>Dependences of the methane self-diffusion coefficient on the root MSD at <span class="html-italic">T</span> = 297 K for 6FDA/BPDA (■), Matrimid Sample 1 (<math display="inline"> <semantics> <mrow> <mstyle mathcolor="red"> <mo>●</mo> </mstyle> </mrow> </semantics> </math>), and Matrimid Sample 2 (<math display="inline"> <semantics> <mrow> <mstyle mathcolor="blue"> <mo>▼</mo> </mstyle> </mrow> </semantics> </math>). The data was obtained using Equation (1) with <span class="html-italic">n</span> = 1 and Equation (2).</p> Full article ">Figure 4
<p>Temperature dependences of the methane self-diffusion coefficient measured by PFG NMR for the effective diffusion time 9 ms in 6FDA/BPDA (■), Matrimid Sample 1 (<math display="inline"> <semantics> <mrow> <mstyle mathcolor="red"> <mo>●</mo> </mstyle> </mrow> </semantics> </math>), and Matrimid Sample 2 (<math display="inline"> <semantics> <mrow> <mstyle mathcolor="blue"> <mo>▼</mo> </mstyle> </mrow> </semantics> </math>). Lines show the fit to the Arrehenius law (Equation (3)).</p> Full article ">Figure 5
<p>(<b>a</b>) Proton PFG NMR attenuation curves measured by the 13-interval PFG NMR sequence for diffusion of isooctane in the FAU/EMT intergrowth at <span class="html-italic">T</span> = 264 K for the following effective diffusion times: 6.0 ms (■), 10.5 ms (<math display="inline"> <semantics> <mrow> <mstyle mathcolor="red"> <mo>●</mo> </mstyle> </mrow> </semantics> </math>), 20.5 ms (<math display="inline"> <semantics> <mrow> <mstyle mathcolor="green"> <mo>▲</mo> </mstyle> </mrow> </semantics> </math>), and 40.5 ms (<math display="inline"> <semantics> <mrow> <mstyle mathcolor="blue"> <mo>▼</mo> </mstyle> </mrow> </semantics> </math>). The lines show the initial slopes of the attenuation curves; (<b>b</b>) Proton PFG NMR attenuation curves measured by the 13-interval PFG NMR sequence for diffusion of isooctane in the FAU/EMT intergrowth at <span class="html-italic">T</span> = 289 K for the following effective diffusion times: 5.7 ms (■), 10.2 ms (<math display="inline"> <semantics> <mrow> <mstyle mathcolor="red"> <mo>●</mo> </mstyle> </mrow> </semantics> </math>), 40.1 ms (<math display="inline"> <semantics> <mrow> <mstyle mathcolor="blue"> <mo>▼</mo> </mstyle> </mrow> </semantics> </math>), 80.1 ms (<math display="inline"> <semantics> <mrow> <mstyle mathcolor="#FF33CC"> <mo>□</mo> </mstyle> </mrow> </semantics> </math>), and 120.1 ms (<math display="inline"> <semantics> <mrow> <mstyle mathcolor="maroon"> <mo>○</mo> </mstyle> </mrow> </semantics> </math>). The lines show the best fit curves of the measured data by Equation (1) with <span class="html-italic">n</span> = 2.</p> Full article ">
1707 KiB  
Article
Carbon Nanotubes: Solution for the Therapeutic Delivery of siRNA?
by D. Lynn Kirkpatrick, Michelle Weiss, Anton Naumov, Geoffrey Bartholomeusz, R. Bruce Weisman and Olga Gliko
Materials 2012, 5(2), 278-301; https://doi.org/10.3390/ma5020278 - 13 Feb 2012
Cited by 52 | Viewed by 9967
Abstract
Carbon nanotubes have many unique physical and chemical properties that are being widely explored for potential applications in biomedicine especially as transporters of drugs, proteins, DNA and RNA into cells. Specifically, single-walled carbon nanotubes (SWCNT) have been shown to deliver siRNA to tumors [...] Read more.
Carbon nanotubes have many unique physical and chemical properties that are being widely explored for potential applications in biomedicine especially as transporters of drugs, proteins, DNA and RNA into cells. Specifically, single-walled carbon nanotubes (SWCNT) have been shown to deliver siRNA to tumors in vivo. The low toxicity, the excellent membrane penetration ability, the protection afforded against blood breakdown of the siRNA payload and the good biological activity seen in vivo suggests that SWCNT may become universal transfection vehicles for siRNA and other RNAs for therapeutic applications. This paper will introduce a short review of a number of therapeutic applications for carbon nanotubes and provide recent data suggesting SWCNT are an excellent option for the delivery of siRNA clinically. Full article
(This article belongs to the Special Issue Carbon Nanotubes: Synthesis, Characterization and Applications)
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Graphical abstract

Graphical abstract
Full article ">Figure 1
<p>(<b>a</b>) AFM length analyses of siRNA/SWCNT complexes sonicated for 15 seconds, 1 min or 5 min; (b,c) AFM (red) and DLS (blue) length distribution and means of processed samples of (<b>b</b>) siRNA/<span class="html-italic">l</span>-PEG/SWCNT; (<b>c</b>) siRNA/<span class="html-italic">br</span>-PEG/SWCNT.</p> Full article ">Figure 2
<p>Atomic force microscopy of SWCNT complexed to (<b>a</b>) siRNA; (<b>b</b>) siRNA followed by <span class="html-italic">l</span>-PEG-5000; (<b>c</b>) siRNA followed by exposure to 1% bovine serum albumin (BSA). Diameters: SWCNT ~1 nm; siRNA coated ~1 to 3 nm; linear (<span class="html-italic">l</span>) or branched (<span class="html-italic">br</span>)-PEG 5000 coating ~4 to 6 nm; BSA ~7 to 10 nm.</p> Full article ">Figure 3
<p>HyperChem model of (<b>a</b>) siRNA complexed to SWCNT and (<b>b</b>) human serum albumin complexed to SWCNT with diameter distances labeled.</p> Full article ">Figure 4
<p>(<b>a</b>) Cy-3-siRNA complexed to SWCNT is not fluorescent (lane 3); (<b>b</b>) H2122 NSCLC cells in culture exposed to Cy-3-siRNA/SWCNT 1 µg/mL for 6 h. Cells were washed and examined by bright field and fluorescent microscopy. Top views illustrate left: the H2122 cells in culture (10.6 pix/µm); right: intracellular Cy-3-siRNA by visible fluorescence (10.6 pix/µm); and bottom views left: illustrate the same H2122 cells in culture (2 pix/µm); right: the intracellular SWCNT by NIR fluorescence (2 pix/µm) in the same cells. All cells in culture contained both the siRNA and SWCNT. Control cells not exposed to Cy-3 siRNA/SWCNT complex showed no fluorescence under either condition (data not shown).</p> Full article ">Figure 5
<p>MiaCaPa-2 cells exposed to: (<b>a</b>) Cy-3-siRNA/SWCNT for 1 h. SWCNT NIR fluorescence in red and Cy-3-siRNA fluorescence in green showing siRNA distribution throughout the cells; (<b>b</b>) Cy-3-siRNA using liposomal delivery for 1 h with same amount siRNA as in (a). Green fluorescence showing the focused lipid delivery of siRNA at 1 h.</p> Full article ">Figure 6
<p>siRNA remaining after exposure to ribonuclease (10 units RNAseONE<sup>TM</sup> Ribonuclease) at 37 °C for 1, 2 and 3 h in solutions of free siRNA in 64 µM PEG or siRNA complexed to SWCNT with 64 µM PEG. No treatment (NT) controls were incubated at 37 °C for 3 h. Resulting solutions were separated on agarose gels and the siRNA quantified using CareStream <span class="html-italic">In Vivo</span> MS FX PRO imager.</p> Full article ">Figure 7
<p>siRNA/SWCNT complexes produce time dependent target knockdown <span class="html-italic">in</span> <span class="html-italic">vitro</span> and <span class="html-italic">in vivo</span>. (<b>a</b>) MiaPaCa-2 cells <span class="html-italic">in vitro</span> with 10% FCS were exposed to siTrx(13nM)/SWCNT at times shown with Western blotting performed at 72 h. Control well: siTrx without SWCNT; (<b>b</b>) siTrx/PEG13µM/SWCNT (39 µg SWCNT, ~0.8 mg/kg siRNA) was injected into tail vein of mice bearing large MiaPaCa-2 tumors. Mice were sacrificed at 24, 48 and 72 h, tumors excised and Western blotted; (<b>c</b>) MiaPaCa-2 tumors from mice treated weekly for 4 weeks with 35 µg SWCNT carrying single siEGFR or dual payload siEGFR+siKRAS (0.8 mg/kg siRNA) (<a href="#materials-05-00278-f008" class="html-fig">Figure 8</a>(A)), excised and Western blotted 96 h following 4th treatment; (<b>d</b>) NIR microscopy of SWCNT in tumor slice at 24 h. Arrows identify SWCNT in tumor with corresponding characteristic NIR spectra used to distinguish SWCNT from biological fluorescing features.</p> Full article ">Figure 8
<p><span class="html-italic">In vivo</span> antitumor activity is robust with biweekly administration. Mice (8 or n) bearing MiaPaCa-2 human pancreatic tumors were treated with 35 µg siRNA/PEG 8 µM/SWCNT complexes delivering ~0.8 mg/kg siRNAs targeting EGFR, KRAS or both via tail vein injection. (<b>a</b>) Weekly for 4 weeks: *Days 15 to 23, significant difference in mean tumor growth rate siKRAS/SWCNT <span class="html-italic">vs</span> vehicle plus siRNA Control, <span class="html-italic">P</span> = 0.05; (<b>b</b>) Biweekly for 4 weeks produced a significant difference for siKRAS-, siEGFR- and the dual siEGFR/siKRAS/SWCNT treated groups from vehicle siRNA control. The siRNA control (weekly) is shown with the biweekly data since only one animal was evaluable for the siRNA control (biweekly); (<b>c</b>) Hematology and blood chemistry showed no difference when performed 24 h after final injection following weekly administration for 4 weeks. Vehicle control was siRNA and PEG 8 µM in 0.9% saline. ( <span class="html-fig-inline" id="materials-05-00278-i001"> <img alt="Materials 05 00278 i001" src="/materials/materials-05-00278/article_deploy/html/images/materials-05-00278-i001.png"/></span> normal mouse range). NT = non-treatment control; S = SWCNT control; E = siEGFR/SWCNT; K = siKRAS/SWCNT; E K = siEGFR/siKRAS/SWCNT. Subset of data is shown; (<b>d</b>) No weight loss was observed in animals treated weekly or biweekly (not shown).</p> Full article ">Figure 8 Cont.
<p><span class="html-italic">In vivo</span> antitumor activity is robust with biweekly administration. Mice (8 or n) bearing MiaPaCa-2 human pancreatic tumors were treated with 35 µg siRNA/PEG 8 µM/SWCNT complexes delivering ~0.8 mg/kg siRNAs targeting EGFR, KRAS or both via tail vein injection. (<b>a</b>) Weekly for 4 weeks: *Days 15 to 23, significant difference in mean tumor growth rate siKRAS/SWCNT <span class="html-italic">vs</span> vehicle plus siRNA Control, <span class="html-italic">P</span> = 0.05; (<b>b</b>) Biweekly for 4 weeks produced a significant difference for siKRAS-, siEGFR- and the dual siEGFR/siKRAS/SWCNT treated groups from vehicle siRNA control. The siRNA control (weekly) is shown with the biweekly data since only one animal was evaluable for the siRNA control (biweekly); (<b>c</b>) Hematology and blood chemistry showed no difference when performed 24 h after final injection following weekly administration for 4 weeks. Vehicle control was siRNA and PEG 8 µM in 0.9% saline. ( <span class="html-fig-inline" id="materials-05-00278-i001"> <img alt="Materials 05 00278 i001" src="/materials/materials-05-00278/article_deploy/html/images/materials-05-00278-i001.png"/></span> normal mouse range). NT = non-treatment control; S = SWCNT control; E = siEGFR/SWCNT; K = siKRAS/SWCNT; E K = siEGFR/siKRAS/SWCNT. Subset of data is shown; (<b>d</b>) No weight loss was observed in animals treated weekly or biweekly (not shown).</p> Full article ">Figure 9
<p>SWCNT complexed with siRNA and with excipients to modify the circulation time. (<b>a</b>) siRNA/<span class="html-italic">l</span>-PEG (400 µM)/SWCNT, t<sub>1/2</sub> = 8–10 min; (<b>b</b>) siRNA/<span class="html-italic">l</span>-PEG (1600 µM)/SWCNT; t<sub>1/2</sub> = 2.6 h; (<b>c</b>) <span class="html-italic">br-</span>PEG/SWCNT: t<sub>1/2</sub> = 25 h.</p> Full article ">Figure 10
<p>Relative SWCNT content in (<b>a</b>) spleen and (<b>b</b>) liver at 12, 24, 48 h and 1 week after mice received single bolus of 100 µg SWCNT solubilized in 3% pluronic displayed by fluorescence spectra.</p> Full article ">Figure 11
<p>Preparation of siRNA/SWCNT or siRNA/PEG/SWCNT complexes.</p> Full article ">
3948 KiB  
Review
Ceramic Laser Materials
by Jasbinder Sanghera, Woohong Kim, Guillermo Villalobos, Brandon Shaw, Colin Baker, Jesse Frantz, Bryan Sadowski and Ishwar Aggarwal
Materials 2012, 5(2), 258-277; https://doi.org/10.3390/ma5020258 - 9 Feb 2012
Cited by 159 | Viewed by 12608
Abstract
Ceramic laser materials have come a long way since the first demonstration of lasing in 1964. Improvements in powder synthesis and ceramic sintering as well as novel ideas have led to notable achievements. These include the first Nd:yttrium aluminum garnet (YAG) ceramic laser [...] Read more.
Ceramic laser materials have come a long way since the first demonstration of lasing in 1964. Improvements in powder synthesis and ceramic sintering as well as novel ideas have led to notable achievements. These include the first Nd:yttrium aluminum garnet (YAG) ceramic laser in 1995, breaking the 1 KW mark in 2002 and then the remarkable demonstration of more than 100 KW output power from a YAG ceramic laser system in 2009. Additional developments have included highly doped microchip lasers, ultrashort pulse lasers, novel materials such as sesquioxides, fluoride ceramic lasers, selenide ceramic lasers in the 2 to 3 μm region, composite ceramic lasers for better thermal management, and single crystal lasers derived from polycrystalline ceramics. This paper highlights some of these notable achievements. Full article
(This article belongs to the Special Issue Laser Materials)
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Figure 1

Figure 1
<p>Thermal conductivity <span class="html-italic">versus</span> dopant concentration for crystals (Adapted from R. Gaume 2002 [<a href="#B4-materials-05-00258" class="html-bibr">4</a>], P. Koopmann [<a href="#B6-materials-05-00258" class="html-bibr">6</a>], F. Patel [<a href="#B7-materials-05-00258" class="html-bibr">7</a>], A. Tunnermann [<a href="#B8-materials-05-00258" class="html-bibr">8</a>] and T. Yamakasi [<a href="#B9-materials-05-00258" class="html-bibr">9</a>]).</p> Full article ">Figure 2
<p>Ceramization process for converting powder into a transparent ceramic.</p> Full article ">Figure 3
<p>Practical fabrication of ceramics.</p> Full article ">Figure 4
<p>Transmission plot of the optically polished ceramics fabricated from our co-precipiated 10% Yb:Lu<sub>2</sub>O<sub>3</sub> and commercial powders, respectively.</p> Full article ">Figure 5
<p>Demonstration of lower scattering loss in ceramic Nd:YAG (Quarles [<a href="#B12-materials-05-00258" class="html-bibr">12</a>]).</p> Full article ">Figure 6
<p>Laser damage threshold for rare earth doped and undoped YAG ceramics compared with single crystal YAG (Adapted from Ueda <span class="html-italic">et al.</span> [<a href="#B17-materials-05-00258" class="html-bibr">17</a>]).</p> Full article ">Figure 7
<p>Results of the first Nd:YAG ceramic laser (Adapted from [<a href="#B20-materials-05-00258" class="html-bibr">20</a>]).</p> Full article ">Figure 8
<p>Results for first Nd:YAG laser to break 1 KW output power (Adapted from [<a href="#B22-materials-05-00258" class="html-bibr">22</a>]).</p> Full article ">Figure 9
<p>Highly doped Yb:YAG ceramic lasers (Adapted from [<a href="#B23-materials-05-00258" class="html-bibr">23</a>]).</p> Full article ">Figure 10
<p>Combining a 2.5% Yb:Y<sub>2</sub>O<sub>3</sub> ceramic behind a 1.8% Yb:Sc<sub>2</sub>O<sub>3</sub> ceramic in a laser cavity to demonstrate (<b>a</b>) spectral broadening from nonlinear gain and (<b>b</b>) pulsed lasing with 53 fs pulses (Adapted from [<a href="#B25-materials-05-00258" class="html-bibr">25</a>]).</p> Full article ">Figure 11
<p>Lasing results for 5%-Yb<sup>3+</sup>:0.65CaF<sub>2</sub>-0.35SrF<sub>2</sub> ceramic compared with a single crystal (Adapted from [<a href="#B27-materials-05-00258" class="html-bibr">27</a>]).</p> Full article ">Figure 12
<p>(<b>a</b>) The laser results for ceramic Cr<sup>2+</sup>:ZnSe made by hot pressing ceramics (HPC) and by chemical diffusion of CrSe into CVD ZnSe (CTD) (after [<a href="#B28-materials-05-00258" class="html-bibr">28</a>]); and (<b>b</b>) a 15 W commercial source available from IPG [<a href="#B29-materials-05-00258" class="html-bibr">29</a>].</p> Full article ">Figure 13
<p>Laser performance of various types of composite elements (Adapted from [<a href="#B30-materials-05-00258" class="html-bibr">30</a>]).</p> Full article ">Figure 14
<p>(<b>a</b>) Graded laser ceramics showing distribution of Nd ions before and after sintering and (<b>b</b>) better thermal management during lasing (Adapted from [<a href="#B31-materials-05-00258" class="html-bibr">31</a>]).</p> Full article ">Figure 15
<p>(<b>a</b>) Tape cast ceramic composite laser material and (<b>b</b>) laser result (Adapted from Messing [<a href="#B32-materials-05-00258" class="html-bibr">32</a>]).</p> Full article ">Figure 16
<p>(<b>a</b>) Shows conversion of a ceramic into a single crystal by seeding a highly doped (3.6 at%) Nd:YAG with a single crystal YAG on either side and (<b>b</b>) the laser results highlighting improved slope efficiency for a single crystal produced from the ceramic, in this case containing 2.4 at% Nd (Adapted from Ikesue [<a href="#B30-materials-05-00258" class="html-bibr">30</a>]).</p> Full article ">Figure 17
<p>Output power <span class="html-italic">versus</span> absorbed power for a 10% Yb:Lu<sub>2</sub>O<sub>3</sub> ceramic laser using a 5% output coupler. Pumping was with a diode operating at 975 nm.</p> Full article ">Figure 18
<p>Thin disk laser using a 200 μm thick 9% Yb:YAG as the active medium and with a 1 mm thick undoped YAG cap (after [<a href="#B39-materials-05-00258" class="html-bibr">39</a>]).</p> Full article ">Figure 19
<p>Different solid state laser configurations used for high power demonstrations: (<b>a</b>) heat capacity laser [<a href="#B41-materials-05-00258" class="html-bibr">41</a>] (<b>b</b>) end-pumped slab laser [<a href="#B42-materials-05-00258" class="html-bibr">42</a>] and (<b>c</b>) thinzag slab laser [<a href="#B43-materials-05-00258" class="html-bibr">43</a>].</p> Full article ">Figure 20
<p>Large Nd:YAG ceramic laser slabs for the heat capacity laser (Adapted from [<a href="#B41-materials-05-00258" class="html-bibr">41</a>]).</p> Full article ">Figure 21
<p>Evolution of laser output power <span class="html-italic">versus</span> year for YAG ceramics.</p> Full article ">
386 KiB  
Article
Molecular Beam-Thermal Desorption Spectrometry (MB-TDS) Monitoring of Hydrogen Desorbed from Storage Fuel Cell Anodes
by Rui F. M. Lobo, Diogo M. F. Santos, Cesar A. C. Sequeira and Jorge H. F. Ribeiro
Materials 2012, 5(2), 248-257; https://doi.org/10.3390/ma5020248 - 6 Feb 2012
Cited by 5 | Viewed by 6597
Abstract
Different types of experimental studies are performed using the hydrogen storage alloy (HSA) MlNi3.6Co0.85Al0.3Mn0.3 (Ml: La-rich mischmetal), chemically surface treated, as the anode active material for application in a proton exchange membrane fuel cell (PEMFC). The [...] Read more.
Different types of experimental studies are performed using the hydrogen storage alloy (HSA) MlNi3.6Co0.85Al0.3Mn0.3 (Ml: La-rich mischmetal), chemically surface treated, as the anode active material for application in a proton exchange membrane fuel cell (PEMFC). The recently developed molecular beam—thermal desorption spectrometry (MB-TDS) technique is here reported for detecting the electrochemical hydrogen uptake and release by the treated HSA. The MB-TDS allows an accurate determination of the hydrogen mass absorbed into the hydrogen storage alloy (HSA), and has significant advantages in comparison with the conventional TDS method. Experimental data has revealed that the membrane electrode assembly (MEA) using such chemically treated alloy presents an enhanced surface capability for hydrogen adsorption. Full article
(This article belongs to the Special Issue Recent Advances in Hydrogen Storage Materials)
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Graphical abstract

Graphical abstract
Full article ">Figure 1
<p>Molecular beam—thermal desorption mass spectrometer (MB-TDS) (Adapted from [<a href="#B6-materials-05-00248" class="html-bibr">6</a>]).</p> Full article ">Figure 2
<p>Particle size distribution of the mechanically pulverized HSA and of the HSAs ball-milled in different media.</p> Full article ">Figure 3
<p>Working stabilities of the HSA anode membrane electrode assembly (MEA) in comparison with Pt/C MEA at a constant current load of 40 mA/cm<sup>2</sup> (operating conditions: electrode area 1 cm<sup>2</sup>, pressure P<sub>H<sub>2</sub></sub> = P<sub>O<sub>2</sub></sub> = 2 atm; working temperature T<sub>cell</sub> = 25 °C, wetting temperature T<sub>anode</sub> = T<sub>cathode</sub> = 40 °C).</p> Full article ">Figure 4
<p><span class="html-italic">U-i</span> and <span class="html-italic">P-i</span> characteristics for the HSA anode MEA and for the Pt/C anode MEA. Operating conditions: A = 1 cm<sup>2</sup>, <math display="inline"> <semantics> <mrow> <msub> <mi>P</mi> <mrow> <msub> <mi>H</mi> <mn>2</mn> </msub> </mrow> </msub> </mrow> </semantics> </math> = <math display="inline"> <semantics> <mrow> <msub> <mi>P</mi> <mrow> <msub> <mi>O</mi> <mn>2</mn> </msub> </mrow> </msub> </mrow> </semantics> </math> = 2 atm, <span class="html-italic">T</span><sub>cell</sub> = <span class="html-italic">T</span><sub>anode</sub> = <span class="html-italic">T</span><sub>cathode</sub> = 60 °C. Open symbols refer to the RH scale.</p> Full article ">Figure 5
<p>MB-TDS spectrum of two (previously electrochemical) charged hydrogenated MlNi<sub>3.6</sub>Co<sub>0.85</sub>Al<sub>0.3</sub>Mn<sub>0.3</sub> alloys submitted to a heating rate of 1 °C/min. The HSA (I) has a larger absorbed hydrogen mass than HSA (II). Adapted from [<a href="#B6-materials-05-00248" class="html-bibr">6</a>].</p> Full article ">Figure 6
<p>p-c-T isotherms for HSA.</p> Full article ">Figure 7
<p>Cell performance of HSA-MEA anode at different temperatures.</p> Full article ">
483 KiB  
Article
Aligned Layers of Silver Nano-Fibers
by Andrii B. Golovin, Jeremy Stromer and Liubov Kreminska
Materials 2012, 5(2), 239-247; https://doi.org/10.3390/ma5020239 - 1 Feb 2012
Cited by 3 | Viewed by 6449
Abstract
We describe a new dichroic polarizers made by ordering silver nano-fibers to aligned layers. The aligned layers consist of nano-fibers and self-assembled molecular aggregates of lyotropic liquid crystals. Unidirectional alignment of the layers is achieved by means of mechanical shearing. Aligned layers of [...] Read more.
We describe a new dichroic polarizers made by ordering silver nano-fibers to aligned layers. The aligned layers consist of nano-fibers and self-assembled molecular aggregates of lyotropic liquid crystals. Unidirectional alignment of the layers is achieved by means of mechanical shearing. Aligned layers of silver nano-fibers are partially transparent to a linearly polarized electromagnetic radiation. The unidirectional alignment and density of the silver nano-fibers determine degree of polarization of transmitted light. The aligned layers of silver nano-fibers might be used in optics, microwave applications, and organic electronics. Full article
(This article belongs to the Special Issue Photonic Materials and Applications)
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Graphical abstract

Graphical abstract
Full article ">Figure 1
<p>(Color online) (<b>a</b>) Shearing setup with the layer of silver nano-fibers (1), doctor blade (2) with applied force F, droplet of the colloidal dispersion (3), and bare borosilicate glass plate (4); (<b>b</b>) The microspore texture of Sample No. 1 with dried silver nano-fibers NGAP NF Ag-3101-W, which was captured between crossed polarizer (P) and analyzer (A). Vector S depicts the direction of shearing.</p> Full article ">Figure 2
<p>(Color online) (<b>a</b>) and (<b>b</b>) Textures of Sample No. 2 (dried silver nano-fibers with the infrared dye IR-806) placed between crossed polarizer P and analyzer A, with two different orientations of shearing direction S with respect to P and A; (<b>c</b>) Absorption spectra of Sample No. 2 (black line) and same for reference film of dried infrared dye IR-806 (red line) measured with visible and near-infrared lights linearly polarized along (∥) and orthogonally (⊥) to the shearing direction S; (<b>d</b>) Infrared absorption spectrum of the longitudinal plasmon calculated for the silver nano-fibers NGAP NF Ag-3101-W.</p> Full article ">Figure 3
<p>(Color online) (<b>a</b>) and (<b>b</b>) Textures of Sample No. 3 (concentrated silver nano-fibers with the infrared dye IE-806) placed between crossed polarizer P and analyzer A, with two different orientations of shearing direction S with respect to P and A; (<b>c</b>) Absorption spectra of Samples 3, (blue lines) measured with lights linearly polarized along (∥) and orthogonally (⊥) to the shearing direction S.</p> Full article ">Figure 4
<p>(Color online) (<b>a</b>) Dichroic ratio and (<b>b</b>) degree of polarization of reference layer of IR-806 (red), Samples No. 2 (black), and Samples No. 3 (blue).</p> Full article ">
2046 KiB  
Article
Optical Properties of Mg, Fe, Co-Doped Near-Stoichiometric LiTaO3 Single Crystals
by Wei Tse Hsu, Zhi Bin Chen, Chien Cheng Wu, Ravi Kant Choubey and Chung Wen Lan
Materials 2012, 5(2), 227-238; https://doi.org/10.3390/ma5020227 - 30 Jan 2012
Cited by 26 | Viewed by 7311
Abstract
Mg, Fe co-doped near-stoichiometric lithium tantalite (SLT) single crystals were grown by employing the zone-leveling Czochralski (ZLCz) technique. The optical properties, holographic parameters, as well as the composition of the grown crystals were measured. It was found that the Li/Ta ratio decreased with [...] Read more.
Mg, Fe co-doped near-stoichiometric lithium tantalite (SLT) single crystals were grown by employing the zone-leveling Czochralski (ZLCz) technique. The optical properties, holographic parameters, as well as the composition of the grown crystals were measured. It was found that the Li/Ta ratio decreased with the doping of Mg and Fe ions. A red shift was observed in absorption spectrum for the Mg, Fe co-doped crystals compared to the undoped and Mg-doped ones. The effect of the iron ions (Fe2+ and Fe3+) was further discussed based on the specified absorption bands. Moreover, the occupation mechanism for the defects was discussed by using the IR absorption spectrum, which was attributed to the FeTa3− defects in the highly Fe-doped crystal. In addition, the holographic parameters were also found to be improved with a higher Fe/Ta ratio in the crystals. Full article
(This article belongs to the Special Issue Advanced Materials for Modern Holographic Applications)
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Figure 1

Figure 1
<p>Photograph of the as grown stoichiometric lithium tantalite (SLT) crystals.</p> Full article ">Figure 2
<p>Absorption spectra of the as grown crystals (A).</p> Full article ">Figure 3
<p>Absorption spectra of the as grown (A) and oxidized (O) crystals.</p> Full article ">Figure 4
<p>Infrared absorption spectra of the as grown crystals.</p> Full article ">Figure 5
<p>Variation of (<b>a</b>) lattice constants and (<b>b</b>) volume of the unit cell with the increasing Fe concentration in the crystals.</p> Full article ">
330 KiB  
Article
Stresses and Displacements in Functionally Graded Materials of Semi-Infinite Extent Induced by Rectangular Loadings
by Hong-Tian Xiao and Zhong-Qi Yue
Materials 2012, 5(2), 210-226; https://doi.org/10.3390/ma5020210 - 30 Jan 2012
Cited by 10 | Viewed by 6210
Abstract
This paper presents the stress and displacement fields in a functionally graded material (FGM) caused by a load. The FGM is a graded material of Si3N4-based ceramics and is assumed to be of semi-infinite extent. The load is a [...] Read more.
This paper presents the stress and displacement fields in a functionally graded material (FGM) caused by a load. The FGM is a graded material of Si3N4-based ceramics and is assumed to be of semi-infinite extent. The load is a distributed loading over a rectangular area that is parallel to the external surface of the FGM and either on its external surface or within its interior space. The point-load analytical solutions or so-called Yue’s solutions are used for the numerical integration over the distributed loaded area. The loaded area is discretized into 200 small equal-sized rectangular elements. The numerical integration is carried out with the regular Gaussian quadrature. Weak and strong singular integrations encountered when the field points are located on the loaded plane, are resolved with the classical methods in boundary element analysis. The numerical integration results have high accuracy. Full article
(This article belongs to the Special Issue Advances in Functionally Graded Materials)
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Figure 1

Figure 1
<p>Functionally Graded Material (FGM) half-space subjected to loads on a rectangular area (<span class="html-italic">a</span> = 2 mm, <span class="html-italic">b</span> = 1 mm).</p> Full article ">Figure 2
<p>Variation of elastic modulus in layers for actual measured modulus.</p> Full article ">Figure 3
<p>The mesh of loading area with 200 eight-noded elements and 661 nodes.</p> Full article ">Figure 4
<p>Normalized displacements (<b>a</b>) u<sub>x</sub>; (<b>b</b>) u<sub>y</sub>; (<b>c</b>) u<sub>z</sub> along <span class="html-italic">y</span> = 0.5 mm at z = 0, 0.125, 0.225 mm for the loading area h = 0 mm.</p> Full article ">Figure 4 Cont.
<p>Normalized displacements (<b>a</b>) u<sub>x</sub>; (<b>b</b>) u<sub>y</sub>; (<b>c</b>) u<sub>z</sub> along <span class="html-italic">y</span> = 0.5 mm at z = 0, 0.125, 0.225 mm for the loading area h = 0 mm.</p> Full article ">Figure 5
<p>Normalized stresses (<b>a</b>) σ<sub>xx</sub>; (<b>b</b>) σ<sub>yy</sub>; (<b>c</b>) σ<sub>zz</sub> along y = 0.5 mm at z = 0, 0.125, 0.225 mm for the loading area h = 0 mm.</p> Full article ">Figure 5 Cont.
<p>Normalized stresses (<b>a</b>) σ<sub>xx</sub>; (<b>b</b>) σ<sub>yy</sub>; (<b>c</b>) σ<sub>zz</sub> along y = 0.5 mm at z = 0, 0.125, 0.225 mm for the loading area h = 0 mm.</p> Full article ">Figure 6
<p>Normalized stresses (<b>a</b>) σ<sub>xx</sub>; (<b>b</b>) σ<sub>yy</sub>; (<b>c</b>) σ<sub>zz</sub> along y = 0.5 mm at z = 0, 0.125, 0.225 mm for the loading area h = 0 mm.</p> Full article ">Figure 6 Cont.
<p>Normalized stresses (<b>a</b>) σ<sub>xx</sub>; (<b>b</b>) σ<sub>yy</sub>; (<b>c</b>) σ<sub>zz</sub> along y = 0.5 mm at z = 0, 0.125, 0.225 mm for the loading area h = 0 mm.</p> Full article ">Figure 7
<p>Normalized displacements (<b>a</b>) u<sub>x</sub>; (<b>b</b>) u<sub>y</sub>; (<b>c</b>) u<sub>z</sub> along y = 0.5 mm at z = 0, 0.13, 0.225 mm for the loading area h = 0.13 mm.</p> Full article ">Figure 7 Cont.
<p>Normalized displacements (<b>a</b>) u<sub>x</sub>; (<b>b</b>) u<sub>y</sub>; (<b>c</b>) u<sub>z</sub> along y = 0.5 mm at z = 0, 0.13, 0.225 mm for the loading area h = 0.13 mm.</p> Full article ">Figure 8
<p>Normalized stresses (<b>a</b>) σ<sub>xx</sub>; (<b>b</b>) σ<sub>yy</sub>; (<b>c</b>) σ<sub>zz</sub> along y = 0.5 mm at z = 0, 0.13, 0.225 mm for the loading area h = 0.13 mm.</p> Full article ">Figure 8 Cont.
<p>Normalized stresses (<b>a</b>) σ<sub>xx</sub>; (<b>b</b>) σ<sub>yy</sub>; (<b>c</b>) σ<sub>zz</sub> along y = 0.5 mm at z = 0, 0.13, 0.225 mm for the loading area h = 0.13 mm.</p> Full article ">Figure 9
<p>Normalized stresses (<b>a</b>) σ<sub>xy</sub>; (<b>b</b>) σ<sub>xz</sub>; (<b>c</b>) σ<sub>yz</sub> along y = 0.5 mm at z = 0, 0.13, 0.225 mm for the loading area h = 0.13 mm.</p> Full article ">Figure 9 Cont.
<p>Normalized stresses (<b>a</b>) σ<sub>xy</sub>; (<b>b</b>) σ<sub>xz</sub>; (<b>c</b>) σ<sub>yz</sub> along y = 0.5 mm at z = 0, 0.13, 0.225 mm for the loading area h = 0.13 mm.</p> Full article ">
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