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DOE OSTI2013

Differentiation within autologous fibrin scaffolds of porcine dermal cells with the mesenchymal stem cell phenotype

Porcine mesenchymal stem cells (pMSCs) are an attractive source of cells for tissue engineering because their properties are similar to those of human stem cells. pMSCs can be found in different tissues but their dermal origin has not been studied in depth. Additionally, MSCs differentiation in monolayer cultures requires subcultured cells, and these cells are at risk of dedifferentiation when implanting them into living tissue. Following this, we attempted to characterize the MSCs phenotype of porcine dermal cells and to evaluate their cellular proliferation and differentiation in autologous fibrin scaffolds (AFSs). Dermal biopsies and blood samples were obtained from 12 pigs. Dermal cells were characterized by flow cytometry. Frozen autologous plasma was used to prepare AFSs. pMSC differentiation was studied in standard structures (monolayers and pellets) and in AFSs. The pMSCs expressed the CD90 and CD29 markers of the mesenchymal lineage. AFSs afforded adipogenic, osteogenic and chondrogenic differentiation. The porcine dermis can be proposed to be a good source of MSCs with adequate proliferative capacity and a suitable expression of markers. The pMSCs also showed optimal proliferation and differentiation in AFSs, such that these might serve as a promising autologous and implantable material for use in tissue engineering. -- Highlights: ► Low fibrinogen concentration provides a suitable matrix for cell migration and differentiation. ► Autologous fibrin scaffolds is a promising technique in tissue engineering. ► Dermal cells are an easily accessible mesenchymal stem cell source. ► Fibrin scaffolds afforded adipogenic, osteogenic and chondrogenic differentiation.

60 APPLIED LIFE SCIENCES↗

DOE OSTI2016

Manipulating mammalian cell by phase transformed titanium surface fabricated through ultra-short pulsed laser synthesis

Developing cell sensitive indicators on interacting substrates that allows specific cell manipulation by a combination of physical, chemical or mechanical cues is a challenge for current biomaterials. Hence, various fabrication approaches have been created on a variety of substrates to mimic or create cell specific cues. However, to achieve cell specific cues a multistep process or a post-chemical treatment is often necessitated. So, a simple approach without any chemical or biological treatment would go a long way in developing bio-functionalized substrates to effectively modulate cell adhesion and interaction. The present investigation is aimed to study the manipulative activity induced by phase transformed titanium surface. An ultra-short laser is used to fabricate the phase transformed titanium surface where a polymorphic titanium oxide phases with titanium monoxide (TiO), tri-titanium oxide (Ti{sub 3}O) and titanium dioxide (TiO{sub 2}) have been synthesized on commercially pure titanium. Control over oxide phase transformed area was demonstrated via a combination of laser scanning time (laser pulse interaction time) and laser pulse widths (laser pulse to pulse separation time). The interaction of phase transformed titanium surface with NIH3T3 fibroblasts and MC3T3-E1 osteoblast cells developed a new bio-functionalized platforms on titanium based biomaterials to modulate cell migration and adhesion. The synthesized phase transformed titanium surface on the whole appeared to induce directional cues for cell migration with unique preferential cell adhesion unseen by other fabrication approaches. The precise bio-functionalization controllability exhibited during fabrication offers perceptible edge for developing a variety of smart bio-medical devices, implants and cardiovascular stents where the need in supressing specific cell adhesion and proliferation is of great demand. - Highlights: • Generation of titanium oxide phase transformed surface by ultra-short pulsed laser synthesis is presented here. • Laser pulse to pulse separation time variation results in polymorphic titanium oxide phases. • The approach enables site specific mammalian cell adhesion and migration. • This method paves way for developing smart titanium based biomedical devices such as implants and biosensors.

60 APPLIED LIFE SCIENCES↗

DOE OSTI2019

Characterization of Complex Interactions at the Gas–Solid Interface with in Situ Spectroscopy: The Case of Nitrogen-Functionalized Carbon

Interactions at the gas-solid interface drive physicochemical processes in many energy and environmental applications; yet, the challenges associated with characterization and development of these dynamic interactions in complex systems limit progress in developing effective materials. Thus, structure-property-performance correlations greatly depend on the development of advanced techniques and analysis methods for the investigation of gas-solid interactions. In this work, adsorption behavior of O 2 and humidified O 2 on nitrogen-functionalized carbon (N-C) materials was investigated to provide a better understanding of the role of nitrogen species in the oxygen reduction reaction (ORR). N-C materials were produced by solvothermal synthesis and N-ion implantation, resulting in a set of materials with varied nitrogen amount and speciation in carbon matrices with different morphologies. Adsorption behavior of the N-C samples was characterized by in situ diffuse reflectance infrared Fourier-transform spectroscopy (DRIFTS) and ambient pressure X-ray photoelectron spectroscopy (AP-XPS) experiments. A novel analysis approach for the interpretation of AP-XPS data was developed, allowing both the determination of overall adsorption behavior of each N-C material and identification of which nitrogen species were responsible for adsorption. The complementary information provided by in situ DRIFTS and AP-XPS suggests that O 2 adsorption primarily takes place on either electron-rich nitrogen species like pyridine, hydrogenated nitrogen species, or graphitic nitrogen. Adsorption of O 2 and H 2 O occurs competitively on solvothermally prepared N-Cs, whereas adsorption of H 2 O and O 2 occurs at different sites on N-ion implanted N-Cs, highlighting the importance of tuning the composition of N-C materials to promote the most efficient ORR pathway.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2015

Instability of Hydrogenated TiO2

Hydrogenated TiO2 (H-TiO2) is toted as a viable visible light photocatalyst. We report a systematic study on the thermal stability of H-implanted TiO2 using X-ray photoelectron spectroscopy (XPS), ultraviolet photoelectron spectroscopy (UPS), Rutherford backscattering spectrometry (RBS) and nuclear reaction analysis (NRA). Protons (40 keV) implanted at a ~2 atom % level within a ~120 nm wide profile of rutile TiO2(110) were situated ~300 nm below the surface. NRA revealed that this H-profile broadened preferentially toward the surface after annealing at 373 K, dissipated out of the crystal into vacuum at 473 K, and was absent within the beam sampling depth (~800 nm) at 523 K. Photoemission showed that the surface was reduced in concert with these changes. Similar anneals had no effect on pristine TiO2(110). The facile bulk diffusivity of H in rutile, as well as its activity toward interfacial reduction, significantly limits the utilization of H-TiO2 as a photocatalyst. This work was supported by the US Department of Energy, Office of Science, Office of Basic Energy Sciences, Division of Chemical Sciences, Geosciences & Biosciences. Pacific Northwest National Laboratory (PNNL) is a multiprogram national laboratory operated for DOE by Battelle. The research was performed using the Environmental Molecular Sciences Laboratory (EMSL), a national scientific user facility sponsored by the Department of Energy's Office of Biological and Environmental Research and located at Pacific Northwest National Laboratory.

diffusion↗

DOE OSTI2023

Emergent Magnetism with Continuous Control in the Ultrahigh-Conductivity Layered Oxide PdCoO 2

The current challenge to realizing continuously tunable magnetism lies in our inability to systematically change properties, such as valence, spin, and orbital degrees of freedom, as well as crystallographic geometry. Here, we demonstrate that ferromagnetism can be externally turned on with the application of low-energy helium implantation and can be subsequently erased and returned to the pristine state via annealing. We find that this high level of continuous control is made possible by targeting magnetic metastability in the ultrahigh-conductivity, nonmagnetic layered oxide PdCoO 2 where local lattice distortions generated by helium implantation induce the emergence of a net moment on the surrounding transition metal octahedral sites. These highly localized moments communicate through the itinerant metal states, which trigger the onset of percolated long-range ferromagnetism. The ability to continuously tune competing interactions enables tailoring precise magnetic and magnetotransport responses in an ultrahigh-conductivity film and will be critical to applications across spintronics.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

DOE OSTI2011

Ion-beam mixing in crystalline and amorphous germanium isotope multilayers

Gallium (Ga) implantation induced self-atom mixing in crystalline and amorphous germanium (Ge) is investigated utilizing isotopically controlled Ge multilayer structures grown by molecular beam epitaxy. The distribution of the Ga ions and the ion-beam induced depth-dependent mixing of the isotope structure was determined by means of secondary ion mass spectrometry. Whereas the distribution of Ga in the crystalline and amorphous Ge is very similar and accurately reproduced by computer simulations based on binary collision approximation (BCA), the ion-beam induced self-atom mixing is found to depend strongly on the state of the Ge structure. The experiments reveal stronger self-atom mixing in crystalline than in amorphous Ge. Atomistic simulations based on BCA reproduce the experimental results only when unphysically low Ge displacement energies are assumed. Analysis of the self-atom mixing induced by silicon implantation confirms the low displacement energy deduced within the BCA approach. This demonstrates that thermal spike mixing contributes significantly to the overall mixing of the Ge isotope structures. The disparity observed in the ion-beam mixing efficiency of crystalline and amorphous Ge indicates different dominant mixing mechanisms. We propose that self-atom mixing in crystalline Ge is mainly controlled by radiation enhanced diffusion during the early stage of mixing before the crystalline structure turns amorphous, whereas in an already amorphous state self-atom mixing is mediated by cooperative diffusion events.

36 MATERIALS SCIENCE↗

DOE OSTI2012

Molecular dynamics simulations of damage production by thermal spikes in Ge

Molecular dynamics simulation techniques are used to analyze damage production in Ge by the thermal spike process and to compare the results to those obtained for Si. As simulation results are sensitive to the choice of the inter-atomic potential, several potentials are compared in terms of material properties relevant for damage generation, and the most suitable potentials for this kind of analysis are identified. A simplified simulation scheme is used to characterize, in a controlled way, the damage generation through the local melting of regions in which energy is deposited. Our results show the outstanding role of thermal spikes in Ge, since the lower melting temperature and thermal conductivity of Ge make this process much more efficient in terms of damage generation than in Si. The study is extended to the modeling of full implant cascades, in which both collision events and thermal spikes coexist. Our simulations reveal the existence of bigger damaged or amorphous regions in Ge than in Si, which may be formed by the melting and successive quenching induced by thermal spikes. In the particular case of heavy ion implantation, defect structures in Ge are not only bigger, but they also present a larger net content in vacancies than in Si, which may act as precursors for the growth of voids and the subsequent formation of honeycomb-like structures.

36 MATERIALS SCIENCE↗

DOE OSTI2012

Controlling Dopant Profiles in Hyperdoped Silicon by Modifying Dopant Evaporation Rates During Pulsed Laser Melting

We describe a method to control the sub-surface dopant profile in 'hyperdoped' silicon fabricated by ion implantation and pulsed laser melting. Dipping silicon ion implanted with sulfur into hydrofluoric acid prior to nanosecond pulsed laser melting leads to a tenfold increase in the rate of sulfur evaporation from the surface of the melt. This results in an 80% reduction of the near-surface dopant concentration, effectively embedding the hyperdoped region in a layer up to 180 nm beneath the surface. This method should facilitate the development of blocked impurity band devices.

14 SOLAR ENERGY↗

DOE OSTI2012

Positron annihilation studies of fluorine-vacancy complexes in Si and SiGe

The formation of fluorine-vacancy (FV) complexes in strained Si-SiGe-Si multilayer structures and relaxed SiGe layers of varying Ge content has been investigated using variable-energy positron annihilation spectroscopy, including Doppler-broadened spectra ratio curves. It has been found that in all sample types there are two distinct regions defined only by the damage created by the implanted F ions. The first, shallower region (from the surface to a depth of {approx}200 nm) was found to contain a mixture of undecorated vacancies and FV complexes; there is no correlation between the vacancy or F concentration in this region and the Ge content. The multi-layer samples may also have O contamination that is not present in the relaxed samples. The second region (at depths {approx}200-440 nm) contains primarily FV complexes in all samples. In the multi-layer samples secondary ion mass spectrometry (SIMS) results show peaks of F accumulating in, or at the interfaces of, each SiGe multi-layer; the FV complexes, however, are distributed over depths similar to those in the relaxed samples, with some localization at the SiGe layer located within the second region. The positron response is primarily to FV complexes formed by the F implant in all samples. The F: FV ratios are approximately 3-7: 1 in the relaxed samples. Positrons appear to be relatively insensitive to the largest of the F SIMS peaks which lies beyond the second region. This is probably because the F has filled all the open volume at the SiGe layer, leaving no positron trapping sites.

36 MATERIALS SCIENCE↗

DOE OSTI2012

Integration of a broad beam ion source with a high-temperature x-ray diffraction vacuum chamber

Here, the integration of a low energy, linearly variable ion beam current density, mechanically in situ adjustable broad beam ion source with a high-temperature x-ray diffraction (XRD) vacuum chamber is reported. This allows in situ XRD investigation of phase formation and evolution processes induced by low energy ion implantation. Special care has been taken to an independent adjustment of the ion beam for geometrical directing towards the substrate, a 15 mm small ion source exit aperture to avoid a secondary sputter process of the chamber walls, linearly variable ion current density by using a pulse length modulation (PLM) for the accelerating voltages without changing the ion beam density profile, nearly homogeneous ion beam distribution over the x-ray footprint, together with easily replaceable Kapton{sup Registered-Sign} windows for x-rays entry and exit. By combining a position sensitive x-ray detector with this PLM-modulated ion beam, a fast and efficient time resolved investigation of low energy implantation processes is obtained in a compact experimental setup.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

DOE OSTI2012

Kinetic Monte Carlo simulation of dopant-defect systems under submicrosecond laser thermal processes

An innovative Kinetic Monte Carlo (KMC) code has been developed, which rules the post-implant kinetics of the defects system in the extremely far-from-the equilibrium conditions caused by the laser irradiation close to the liquid-solid interface. It considers defect diffusion, annihilation and clustering. The code properly implements, consistently to the stochastic formalism, the fast varying local event rates related to the thermal field T(r,t) evolution. This feature of our numerical method represents an important advancement with respect to current state of the art KMC codes. The reduction of the implantation damage and its reorganization in defect aggregates are studied as a function of the process conditions. Phosphorus activation efficiency, experimentally determined in similar conditions, has been related to the emerging damage scenario.

36 MATERIALS SCIENCE↗

DOE OSTI2012

Microwave ECR plasma electron flood for low pressure wafer charge neutralization

Modern ion implanters typically use dc arc discharge Plasma Electron Floods (PEFs) to neutralize wafer charge. The arc discharge requires using at least some refractory metal hardware, e.g. a thermionically emitting filament, which can be undesirable in applications where no metallic contamination is critical. rf discharge PEFs have been proposed to mitigate contamination risks but the gas flows required can result in high process chamber pressures. Axcelis has developed a microwave electron cyclotron resonance (ECR) PEF to provide refractory metals contamination-free wafer neutralization with low gas flow requirement. Our PEF uses a custom, reentrant cusp magnet field providing ECR and superior electron confinement. Stable PEF operation with extraction slits sized for 300 mm wafers can be attained at Xe gas flows lower than 0.2 sccm. Electron extraction currents can be as high as 20 mA at absorbed microwave powers < 70 W. On Axcelis' new medium current implanter, plasma generation has proven robust against pressure transients caused by, for example, photoresist outgassing by high power ion beams. Charge monitor and floating potential measurements along the wafer surface corroborate adequate wafer charge neutralization for low energy, high current ion beams.

43 PARTICLE ACCELERATORS↗

DOE OSTI2013

Deep levels generated by thermal oxidation in p-type 4H-SiC

Thermal oxidation is an effective method to reduce deep levels, especially the Z{sub 1/2}-center (E{sub C}-0.67 eV), which strongly suppresses carrier lifetimes in n-type 4H-SiC epilayers. The oxidation, however, simultaneously generates other deep levels, HK0 (E{sub V}+0.79 eV) and HK2 (E{sub V}+0.98 eV) centers, within the lower half of the bandgap of SiC, where the HK0 center is a dominant deep level with a concentration of about 1 Multiplication-Sign 10{sup 13} cm{sup -3} after oxidation. By comparing deep levels observed in three sets of p-type 4H-SiC: oxidized, electron-irradiated, and C{sup +}- or Si{sup +}-implanted samples, we find that the HK0 and HK2 centers are complexes including carbon interstitials such as the di-carbon interstitial or di-carbon antisite. Other defects observed in p-type 4H-SiC after electron irradiation or after C{sup +}/Si{sup +} implantation are also studied.