Name: production of single tracks of ti-6al-4v by directed energy deposition to determine the layer thickness for multilayer deposition
Uploaded: 2018-03-13T13:00:00
Description: Watch this Scientific Journal Video about Production of Single Tracks of Ti-6Al-4V by Directed Energy Deposition to Determine the Layer Thickness for Multilayer Deposition at JoVE.com

The authors would like to acknowledge the European research project belonging to the Horizon 2020 research and innovation program Borealis - the 3A energy class Flexible Machine for the new Additive and Subtractive Manufacturing on next generation of complex 3D metal parts

1. Powder Characterization
<ol>
	<li>Put 3 g of starting Ti-6Al-4V powders on a double-sided sticky carbon tape, which is located on an aluminum pin stub, and insert inside the specimen chamber of a Field-Emission Scanning Electron Microscope (FESEM) to analyze the morphology of the powder16.</li>
	<li>Measure the apparent density of the powder by filling a 30 cm3 container, and measure the weight of powder according to the ASTM-B212 standard.</li>
	<li>Perform chemical analysis of st...

<ol>
	<li>Banerjee, D., Williams, J. C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Perspectives+on+Titanium+Science+and+Technology.">Perspectives on Titanium Science and Technology.</a> Acta Mater. 61 (3), 844-879 (2013).</li><li>Peters, M., Leyens, C., Peters, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Titanium and Titanium Alloys. , (2003).</li><li>Lin, J., Lv, Y., Liu, Y., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Microstructural+evolution+and+mechanical+property+of+Ti-6Al-4V+wall+deposited+by+continuous+plasma+arc+additive+manufacturing+without+post+heat+treatment.">Microstructural evolution and mechanical property of Ti-6Al-4V wall deposited by continuous plasma arc additive manufacturing without post heat treatment.</a> J Mech Behav Biomed Mater. 69 (December 2016), 19-29 (2017).</li><li>Saboori, A., Gallo, D., Biamino, S., Fino, P., Lombardi, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=An+Overview+of+Additive+Manufacturing+of+Titanium+Components+by+Directed+Energy+Deposition:+Microstructure+and+Mechanical+Properties.">An Overview of Additive Manufacturing of Titanium Components by Directed Energy Deposition: Microstructure and Mechanical Properties.</a> Appl Sci. 7 (9), (2017).</li><li>Wu, X., Liang, J., Mei, J., Mitchell, C., Goodwin, P. 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P., Oliveira, C., Cardoso, A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Predicting+the+geometric+form+of+clad+in+laser+cladding+by+powder+using+multiple+regression+analysis+(MRA).">Predicting the geometric form of clad in laser cladding by powder using multiple regression analysis (MRA).</a> Mater Des. 29 (2), 554-557 (2008).</li><li>Kobryn, P. A., Moore, E. H., Semiatin, S. L. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=The+Effect+Of+Laser+Power+And+Traverse+Speed+On+Microstructure,+Porosity,+And+Build+Height+In+Laser-Deposited+Ti-6Al-4V.">The Effect Of Laser Power And Traverse Speed On Microstructure, Porosity, And Build Height In Laser-Deposited Ti-6Al-4V.</a> Scripta Materialia. 43, 299-305 (2000).</li><li>Bi, G., Gasser, A., Wissenbach, K., Drenker, A., Poprawe, R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Characterization+of+the+process+control+for+the+direct+laser+metallic+powder+deposition.">Characterization of the process control for the direct laser metallic powder deposition.</a> Surf Coatings Technol. 201 (6), 2676-2683 (2006).</li><li>Choi, J., Chang, Y. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Characteristics+of+laser+aided+direct+metal/material+deposition+process+for+tool+steel.">Characteristics of laser aided direct metal/material deposition process for tool steel.</a> Int J Mach Tools Manuf. 45 (4-5), 597-607 (2005).</li><li>Ruan, J., Tang, L., Liou, F. W., Landers, R. G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Direct+Three-Dimensional+Layer+Metal+Deposition.">Direct Three-Dimensional Layer Metal Deposition.</a> J Manuf Sci Eng. 132 (6), 64502-64506 (2010).</li><li>Chen, X., Tao, Z. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Maximum+thickness+of+the+laser+cladding.">Maximum thickness of the laser cladding.</a> Key Eng Mater. 46, 381-386 (1989).</li><li>Slotwinski, J. A., Garboczi, E. J., Stutzman, P. E., Ferraris, C. F., Watson, S. S., Peltz, M. A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Characterization+of+Metal+Powders+Used+for+Additive+Manufacturing.">Characterization of Metal Powders Used for Additive Manufacturing.</a> J Res Natl Inst Stand Technol. 119, 460-493 (2014).</li><li>Manfredi, D., Calignano, F., Krishnan, M., Canali, R., Ambrosio, E. P., Atzeni, E. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=From+Powders+to+Dense+Metal+Parts:+Characterization+of+a+Commercial+AlSiMg+Alloy+Processed+through+Direct+Metal+Laser+Sintering.">From Powders to Dense Metal Parts: Characterization of a Commercial AlSiMg Alloy Processed through Direct Metal Laser Sintering.</a> Materials. 6 (3), 856-869 (2013).</li></ol>

In this work, the focus was on the slicing thickness setting in the DED process of Ti-6Al-4V, according to the geometry of melt pool characteristics. For this purpose, a two-step protocol was defined and utilized. The first part of the protocol was an optimization of process parameters for single scan deposition and, during this step, the optimum parameters were achieved and the melt pool geometries were measured. In the second part of the protocol, the specific energy density of specimens at the optimum parameters was c...

Ti-6Al-4V is the most commonly used Ti alloy in the aerospace, aircraft, automotive, and biomedical industries because of its high strength-to-weight ratio, excellent fracture toughness, low specific gravity, excellent corrosion resistance, and heat treatability. However, its further developments in other applications are challenging, owing to its low thermal conductivity and high reactivity features, which result in its poor machinability. Moreover, due to the heat hardening phenomena during the cutting, a specific heat treatment must be undertaken1,2,3,4.
Nonetheless, additive manufacturing (AM) technologies showed great potential to be used as new manufacturing techniques that can reduce the price and energy consumption, and address some of the current challenges in the fabrication of Ti-6Al-4V alloy.
Additive manufacturing techniques are known as innovative and can fabricate a near net shape component in a layer-by-layer fashion. A layer-by-layer additive manufacturing approach, which slices a Computer Aided Design (CAD) model into thin layers and then builds the component layer by layer, is fundamental for all AM methods. In general, additive manufacturing of metallic materials can be divided into four different processes: powder bed, powder feed (blown powder), wire feed, and other routes3,5,6.
Directed Energy Deposition (DED) is a class of additive manufacturing and is a blown powder process that fabricates three-dimensional (3D) near net shape solid parts from a CAD file similar to other AM methods. In contrast with other techniques, DED can not only be used as a manufacturing method, but also can be employed as a repairing technique for high value parts. In the DED process, metallic powder or wire material is fed by a carrier gas or motors into the melt pool, which is generated by the laser beam on either the substrate or previously deposited layer. The DED process is a promising advanced manufacturing process that is capable of decreasing the buy-to-fly ratio, and also is capable of repairing high value parts that previously were prohibitively expensive to replace or irreparable7.
In order to achieve the desired geometric dimensions and material properties, it is vital to establish appropriate parameters8. Several studies have been undertaken to elucidate the relationship between the process parameters and the final properties of the deposited sample. Peyre et al.9 built some thin walls with different process parameters, and then characterized them by using 2D and 3D profilometry. They showed that layer thickness and melt pool volume affect the roughness parameters noticeably. Vim et al.10 proposed a model in order to analyze the relation between the process parameters and geometrical characteristics of a single cladding layer (clad height, clad width, and depth of penetration).
To date, several studies on DED of Ti alloys have been reported, most of which focused on the influence of the combination of parameters on properties of massive samples11,12,4. Rasheedat et al. studied the effect of scan speed and powder flow rate on the resulting properties of the laser metal deposited Ti-6Al-4V alloy. They found that by increasing the scan speed and powder flow rate the microstructure changed from Widmanst&#228;tten to a martensitic microstructure, which results in an increment of surface roughness and the microhardness of deposited specimens7. Nevertheless, less attention has been paid to designing the layer thickness setting. Choi et al. have investigated the correlation between the layer thickness and process parameters. They have found that the main sources of error between the present height and the actual height are the powder mass flow rate and layer thickness setting13. Their studies did not properly implement layer thickness setting because they involved lengthy and inaccurate processes in the layer thickness setting. Ruan et al. have investigated the effect of laser scanning speed on the deposited layer height at a constant laser power and powder feeding rate14. They have proposed some empirical models for layer thickness setting which were obtained under specific processing conditions, and thus the layer thickness setting may not be precise due to the utilization of specific process parameters15. In contrast to previous works, the layer thickness setting process proposed in this manuscript is a rapid method which can be performed without wasting time and materials.
The main focus of this work is to develop a rapid method for the determination of layer thickness based on the characteristics of the single tracks of the Ti-6Al-4V alloy at optimum DED process parameters. Thereafter, the optimal process parameters are employed to determine a layer thickness and fabricate high-density Ti-6Al-4V blocks without wasting time and materials.

<table>
	<tbody>
		<tr>
			<td>Ti-6Al-4V powder</td>
			<td>Xi&#8217;Tianrui new material</td>
			<td></td>
			<td>As starting material</td>
		</tr>
		<tr>
			<td>ISOMET precision cutter</td>
			<td>Bohler</td>
			<td></td>
			<td>To cut the samples</td>
		</tr>
		<tr>
			<td>Polishing machine</td>
			<td>Presi</td>
			<td></td>
			<td>To polish the samples</td>
		</tr>
		<tr>
			<td>EpoFix resin</td>
			<td>Presi</td>
			<td></td>
			<td>To mount the samples</td>
		</tr>
		<tr>
			<td>Diamond paste</td>
			<td>Presi</td>
			<td></td>
			<td>For polishing</td>
		</tr>
		<tr>
			<td>Optical Microscope</td>
			<td>Leica</td>
			<td></td>
			<td>Microstructural observation</td>
		</tr>
		<tr>
			<td>Field emission scanning electron microscope</td>
			<td>Merlin-Zeiss</td>
			<td></td>
			<td>Microstructural observation</td>
		</tr>
		<tr>
			<td>Stereo microscope</td>
			<td>Leica</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>LEC1- CS444 ANALYSER</td>
			<td>IncoTest</td>
			<td></td>
			<td>Chemical analysis</td>
		</tr>
		<tr>
			<td>LEC3 - ELTRA OHN2000 ANALYSER</td>
			<td>IncoTest</td>
			<td></td>
			<td>Chemical analysis</td>
		</tr>
		<tr>
			<td>LEC2 - LECO TC436AR ANALYSER</td>
			<td>IncoTest</td>
			<td></td>
			<td>Chemical analysis</td>
		</tr>
		<tr>
			<td>ICP</td>
			<td>IncoTest</td>
			<td></td>
			<td>Chemical analysis</td>
		</tr>
		<tr>
			<td>IRB 4600</td>
			<td>ABB</td>
			<td></td>
			<td>Antropomorphic robot</td>
		</tr>
		<tr>
			<td>GTV PF</td>
			<td>GTV</td>
			<td></td>
			<td>Powder feeding system</td>
		</tr>
		<tr>
			<td>YW 52</td>
			<td>Precitec</td>
			<td></td>
			<td>Laser head</td>
		</tr>
		<tr>
			<td>Nozzles</td>
			<td>IRIS</td>
			<td></td>
			<td>Nozzle for feeding powders</td>
		</tr>
		<tr>
			<td>YLS 3000</td>
			<td>IPG Photonics</td>
			<td></td>
			<td>Laser source</td>
		</tr>
	</tbody>
</table>

production of single tracks of ti-6al-4v by directed energy deposition to determine the layer thickness for multilayer deposition

Directed Energy Deposition (DED), which is an additive manufacturing technique, involves the creation of a molten pool with a laser beam where metal powder is injected as particles. In general, this technique is employed to either fabricate or repair different components. In this technique, the final characteristics are affected by many factors. Indeed, one of the main tasks in building components by DED is the optimization of process parameters (such as laser power, laser speed, focus, etc.) which is usually carried out through an extensive experimental investigation. However, this sort of experiment is extremely lengthy and costly. Thus, in order to accelerate the optimization process, an investigation was conducted to develop a method based on the melt pool characterizations. In fact, in these experiments, single tracks of Ti-6Al-4V were deposited by a DED process with multiple combinations of laser power and laser speed. Surface morphology and dimensions of single tracks were analyzed, and geometrical characteristics of melt pools were evaluated after polishing and etching the cross-sections. Helpful information regarding the selection of optimal process parameters can be achieved by examining the melt pool features. These experiments are being extended to characterize the larger blocks with multiple layers. Indeed, this manuscript describes how it would be possible to quickly determine the layer thickness for the massive deposition, and avoid over or under-deposition according to the calculated energy density of the optimum parameters. Apart from the over or under-deposition, time and materials saving are the other great advantages of this approach in which the deposition of multilayer components can be started without any parameter optimization in terms of layer thickness.

For the experimental studies, irregular Ti-6Al-4V powder with an average size of 50 - 150 &#181;m and apparent density of 1.85 g/cm3 was employed as depositing material (Figure 1). The chemical analysis of the powder confirmed that the oxygen and nitrogen contents of the powder did not change before and after the deposition process, while in both cases the oxygen content was higher than the standard oxygen content of Ti-6Al-4V powder for additive m...

Watch this Scientific Journal Video about Production of Single Tracks of Ti-6Al-4V by Directed Energy Deposition to Determine the Layer Thickness for Multilayer Deposition at JoVE.com

Production of Single Tracks of Ti-6Al-4V by Directed Energy Deposition to Determine the Layer Thickness for Multilayer Deposition

In this research, a rapid method based on melt pool characterization is developed to estimate the layer thickness of Ti-6Al-4V components produced by directed energy deposition.

Directed Energy Deposition (DED), which is an additive manufacturing technique, involves the creation of a molten pool with a laser beam where metal ...

The overall goal of this procedure is to determine the effects of different directed energy deposition process parameters on the layer thickness and other melt pool characteristics to identify the optimal parameters for fabrication of larger metallic parts. Directed energy deposition is an additive manufacturing technology for creating metallic parts with medium-large dimensions from metallic powders. Each powder requires process parameters to produce high-density, defect-free parts.Conventional process parameters optimization often involves waste from over/under-deposition caused by assumption for layer height. The main advantage of this technique is that it is time and cost saving. This optimization method is based on production and characterization of single tracks from metallic powders.When handling the titanium six-four powder, wear a respiratory mask, powder-free disposable nitrile gloves, and protective plastic glasses. To begin characterization of the fresh, irregular titanium six-four powder, fix double-sided adhesive carbon tape to an aluminum pin stub for a field emission scanning electron microscope. Apply three grams of the titanium six-four powder to the sticky carbon tape.Place the pin in the specimen chamber of the FESEM, and evaluate the morphology of the powder. Then, fill a 30 cubic centimeter pre-weighed container with the titanium six-four powder. Weigh the filled container, and calculate the apparent density of the powder.Perform chemical analysis of the starting powder using combustion analysis and ICP-MS. To begin titanium six-four powder loading, open the powder-feeding system hopper. Remove residual powders with an extractor fan.Tightly close the top cap of the hopper to prevent gas leakage. Then, clean the titanium six-four sheet with ethanol-soaked paper towels. Measure the weight of the sheet with a centesimal balance.Place the sheet on the marked location of the working area. Mount a powder-feeding nozzle on the laser head so that the angle between the nozzle and laser is 35 degrees. Ensure that the nozzle is clean.Then, move the robot to the starting point in the working area. Manually adjust the nozzle position until the vertical distance between the metal alloy sheet and the nozzle tip is five millimeters. Then, turn on the guide laser.Insert a thin rod through the nozzle to touch the working area. Check if the guide laser spot and the tip of the rod are coincident. Manually adjust the nozzle as needed to align the guide laser and metal rod, retaining the 35-degree angle between the nozzle and laser and a five millimeter vertical distance between the nozzle tip and the alloy sheet.This manual adjustment of the nozzle should be done very carefully because the deposition of the nozzle can significantly affect the geometry of the melt pool. Connect the nozzle to the powder-feeding system, being careful not to disturb the nozzle alignment. Next, open the robot calibration data in the control software.Load the code onto the robot, and address any detected code errors. Use the laser control software to enable the laser source module. Manually enable the robot motors from the robot control cabinet.Verify that the safety LED is illuminated. Then, select the deposition process file from the program list, and load the working path into the main robot routine. Set the laser power and robot speed to the desired values, and apply the parameters.Once the code has been successfully loaded onto the robot controller, launch the robot routine from the robot control software to deposit the single tracks in an automated process. When the routine has finished, use forceps to pick up the sample from the working area. Remove residual powder from the sample surface with an ethanol-soaked paper towel.Perform elemental analysis on used titanium four powder and on a deposited alloy block. Examine deposited single tracks under a stereo microscope at 5X magnification. Then, use a precision cutting machine to cut cross-sections of single tracks from the middle of the deposited tracks.Place the clean, dry cross-section specimens in mounting cups. Mix together 10 grams of resin and six grams of liquid hardener to each sample. Pour each resin mixture over a specimen.Allow the resin to cure for 30 minutes at room temperature. Then, fix a specimen on a polishing machine. First, grind the specimen with 500, 800, and 1, 200 grit silicon carbide paper.Then, polish the specimen with three micron and one micron diamond paste in sequence. The grinding and polishing step should be done carefully in order to have scratch-free surfaces for optical microscopy and melt pool size measurements. Grind and polish every specimen in this way.Then, evaluate the shape and porosity of each polished surface under an optical microscope. Acquire images of the melt pool features at 10X magnification, and analyze the images with image processing software. The chemical compositions of titanium six-four powders in both components were evaluated before and after deposition.The oxygen and nitrogen contents were greater in the irregular titanium six-four powder than in the standard powder used in additive manufacturing. The oxygen and nitrogen contents of the bulk components increased after deposition, but no significant composition change was observed in the used powder. Increasing the laser power significantly increased the height of single tracks up to a point, after which the power delivered to the melt pool was too great to positively affect deposition height.Increasing the laser scanning speed decreased the energy input to the melting pool and the powder delivery rate, resulting in decreasing deposition height. Correspondingly, deposition height was found to increase linearly both with specific energy density and with power feed density. These relationships were used to determine the process parameters required to produce layers of a specific height.Specimens were produced at different powers with an assumed layer height of 0.6 millimeters using the conventional method, resulting in over-and under-deposition. When parameters optimized for a consistent layer thickness were used, greater dimensional accuracy was achieved in a single attempt. In direct energy deposition, powders are directly deposited on a substrate, are melted under a laser and quickly solidified.The solid is created layer by layer, limiting waste by using only as much powder as needed. This method can help answer key questions in the additive manufacturing field about optimization of the process parameters, such as laser power and laser speed. Characterization of single tracks allowed working conditions to be defined for the shown deposition height.This kind of process parameter optimization is a fundamental step in the development of a new directed energy deposition instrument. After watching this video, you should have a good understanding of how to determine desired step parameter for multilayer deposition by this directed energy deposition technique without wasting time and material.

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Engineering

Harvesting Solar Energy by Means of Charge-Separating Nanocrystals and Their Solids

Conjoining different semiconductor materials in a single nano-composite provides synthetic means for the development of novel optoelectronic materials offering a superior control over the spatial distribution of charge carriers across material interfaces. As this study demonstrates, a combination of donor-acceptor nanocrystal (NC) domains in a single nanoparticle can lead to the realization of efficient photocatalytic1-5 materials, while a layered assembly of donor- and acceptor-like nanocrystals films gives rise to photovoltaic materials.
Initially the paper focuses on the synthesis of composite inorganic nanocrystals, comprising linearly stacked ZnSe, CdS, and Pt domains, which jointly promote photoinduced charge separation. These structures are used in aqueous solutions for the photocatalysis of water under solar radiation, resulting in the production of H2 gas. To enhance the photoinduced separation of charges, a nanorod morphology with a linear gradient originating from an intrinsic electric field is used5. The inter-domain energetics are then optimized to drive photogenerated electrons toward the Pt catalytic site while expelling the holes to the surface of ZnSe domains for sacrificial regeneration (via methanol). Here we show that the only efficient way to produce hydrogen is to use electron-donating ligands to passivate the surface states by tuning the energy level alignment at the semiconductor-ligand interface. Stable and efficient reduction of water is allowed by these ligands due to the fact that they fill vacancies in the valence band of the semiconductor domain, preventing energetic holes from degrading it. Specifically, we show that the energy of the hole is transferred to the ligand moiety, leaving the semiconductor domain functional. This enables us to return the entire nanocrystal-ligand system to a functional state, when the ligands are degraded, by simply adding fresh ligands to the system4.
To promote a photovoltaic charge separation, we use a composite two-layer solid of PbS and TiO2 films. In this configuration, photoinduced electrons are injected into TiO2 and are subsequently picked up by an FTO electrode, while holes are channeled to a Au electrode via PbS layer6. To develop the latter we introduce a Semiconductor Matrix Encapsulated Nanocrystal Arrays (SMENA) strategy, which allows bonding PbS NCs into the surrounding matrix of CdS semiconductor. As a result, fabricated solids exhibit excellent thermal stability, attributed to the heteroepitaxial structure of nanocrystal-matrix interfaces, and show compelling light-harvesting performance in prototype solar cells7.

A general strategy for the development of charge-separating semiconductor nanocrystal composites deployable for solar energy production is presented. We show that assembly of donor-acceptor nanocrystal domains in a single nanoparticle geometry gives rise to a photocatalytic function, while bulk-heterojunctions of donor-acceptor nanocrystal films can be used for photovoltaic energy conversion.

Conjoining different semiconductor materials in a single nano-composite provides synthetic means for the development of novel optoelectronic materials ...

Fabrication of Nano-engineered Transparent Conducting Oxides by Pulsed Laser Deposition

Nanosecond Pulsed Laser Deposition (PLD) in the presence of a background gas allows the deposition of metal oxides with tunable morphology, structure, density and stoichiometry by a proper control of the plasma plume expansion dynamics. Such versatility can be exploited to produce nanostructured films from compact and dense to nanoporous characterized by a hierarchical assembly of nano-sized clusters. In particular we describe the detailed methodology to fabricate two types of Al-doped ZnO (AZO) films as transparent electrodes in photovoltaic devices: 1) at low O2 pressure, compact films with electrical conductivity and optical transparency close to the state of the art transparent conducting oxides (TCO) can be deposited at room temperature, to be compatible with thermally sensitive materials such as polymers used in organic photovoltaics (OPVs); 2) highly light scattering hierarchical structures resembling a forest of nano-trees are produced at higher pressures. Such structures show high Haze factor (&gt;80%) and may be exploited to enhance the light trapping capability. The method here described for AZO films can be applied to other metal oxides relevant for technological applications such as TiO2, Al2O3, WO3 and Ag4O4.

We describe the experimental method to deposit nanostructured oxide thin films by nanosecond Pulsed Laser Deposition (PLD) in the presence of a background gas. By using this method Al-doped ZnO (AZO) films, from compact to hierarchically structured as nano-tree forests, can be deposited.

Nanosecond Pulsed  Laser Deposition (PLD) in the presence of a background gas allows the deposition  of metal oxides with tunable morphology, structure, ...

Casting Protocols for the Production of Open Cell Aluminum Foams by the Replication Technique and the Effect on Porosity

Metal foams are interesting materials from both a fundamental understanding and practical applications point of view. Uses have been proposed, and in many cases validated experimentally, for light weight or impact energy absorbing structures, as high surface area heat exchangers or electrodes, as implants to the body, and many more. Although great progress has been made in understanding their structure-properties relationships, the large number of different processing techniques, each producing material with different characteristics and structure, means that understanding of the individual effects of all aspects of structure is not complete. The replication process, where molten metal is infiltrated between grains of a removable preform material, allows a markedly high degree of control and has been used to good effect to elucidate some of these relationships. Nevertheless, the process has many steps that are dependent on individual &#8220;know-how&#8221;, and this paper aims to provide a detailed description of all stages of one embodiment of this processing method, using materials and equipment that would be relatively easy to set up in a research environment. The goal of this protocol and its variants is to produce metal foams in an effective and simple way, giving the possibility to tailor the outcome of the samples by modifying certain steps within the process. By following this, open cell aluminum foams with pore sizes of 1&#8211;2.36 mm diameter and 61% to 77% porosity can be obtained.

Replication is one of the processing techniques used for the production of porous metal sponges. In this paper one implementation of the method for the production of open celled porous aluminum is shown in detail.

Metal foams are interesting materials from both a fundamental understanding and practical applications point of view. Uses have been proposed, and in many ...

Making Record-efficiency SnS Solar Cells by Thermal Evaporation and Atomic Layer Deposition

Tin sulfide (SnS) is a candidate absorber material for Earth-abundant, non-toxic solar cells. SnS offers easy phase control and rapid growth by congruent thermal evaporation, and it absorbs visible light strongly. However, for a long time the record power conversion efficiency of SnS solar cells remained below 2%. Recently we demonstrated new certified record efficiencies of 4.36% using SnS deposited by atomic layer deposition, and 3.88% using thermal evaporation. Here the fabrication procedure for these record solar cells is described, and the statistical distribution of the fabrication process is reported. The standard deviation of efficiency measured on a single substrate is typically over 0.5%. All steps including substrate selection and cleaning, Mo sputtering for the rear contact (cathode), SnS deposition, annealing, surface passivation, Zn(O,S) buffer layer selection and deposition, transparent conductor (anode) deposition, and metallization are described. On each substrate we fabricate 11 individual devices, each with active area 0.25 cm2. Further, a system for high throughput measurements of current-voltage curves under simulated solar light, and external quantum efficiency measurement with variable light bias is described. With this system we are able to measure full data sets on all 11 devices in an automated manner and in minimal time. These results illustrate the value of studying large sample sets, rather than focusing narrowly on the highest performing devices. Large data sets help us to distinguish and remedy individual loss mechanisms affecting our devices.

Tin sulfide (SnS) is a candidate material for Earth-abundant, non-toxic solar cells. Here, we demonstrate the fabrication procedure of the SnS solar cells employing atomic layer deposition, which yields 4.36% certified power conversion efficiency, and thermal evaporation which yields 3.88%.

Tin sulfide (SnS) is a candidate absorber material for Earth-abundant, non-toxic solar cells. SnS offers easy phase control and rapid growth by congruent ...

Formation of Thick Dense Yttrium Iron Garnet Films Using Aerosol Deposition

Aerosol deposition (AD) is a thick-film deposition process that can produce layers up to several hundred micrometers thick with densities greater than 95% of the bulk. The primary advantage of AD is that the deposition takes place entirely at ambient temperature; thereby enabling film growth in material systems with disparate melting temperatures. This report describes in detail the processing steps for preparing the powder and for performing AD using the custom-built system. Representative characterization results are presented from scanning electron microscopy, profilometry, and ferromagnetic resonance for films grown in this system. As a representative overview of the capabilities of the system, focus is given to a sample produced following the described protocol and system setup. Results indicate that this system can successfully deposit 11 &#181;m thick yttrium iron garnet films that are &#160;&#62; 90% of the bulk density during a single 5 min deposition run. A discussion of methods to afford better control of the aerosol and particle selection for improved thickness and roughness variations in the film is provided.

This report describes the use of a custom-built system to perform aerosol deposition of thick films of yttrium iron garnet onto sapphire substrates at RT. The deposited films are characterized using scanning electron microscopy, profilometry, and ferromagnetic resonance to give a representative overview of the capabilities of the technique.

Aerosol deposition (AD) is a thick-film deposition process that can produce layers up to several hundred micrometers thick with densities greater than 95% ...

Synthesis and Characterization of High c-axis ZnO Thin Film by Plasma Enhanced Chemical Vapor Deposition System and its UV Photodetector Application

In this study, zinc oxide (ZnO) thin films with high c-axis (0002) preferential orientation have been successfully and effectively synthesized onto silicon (Si) substrates via different synthesized temperatures by using plasma enhanced chemical vapor deposition (PECVD) system. The effects of different synthesized temperatures on the crystal structure, surface morphologies and optical properties have been investigated. The X-ray diffraction (XRD) patterns indicated that the intensity of (0002) diffraction peak became stronger with increasing synthesized temperature until 400 oC. The diffraction intensity of (0002) peak gradually became weaker accompanying with appearance of (10-10) diffraction peak as the synthesized temperature up to excess of 400 oC. The RT photoluminescence (PL) spectra exhibited a strong near-band-edge (NBE) emission observed at around 375 nm and a negligible deep-level (DL) emission located at around 575 nm under high c-axis ZnO thin films. Field emission scanning electron microscopy (FE-SEM) images revealed the homogeneous surface and with small grain size distribution. The ZnO thin films have also been synthesized onto glass substrates under the same parameters for measuring the transmittance.
For the purpose of ultraviolet (UV) photodetector application, the interdigitated platinum (Pt) thin film (thickness ~100 nm) fabricated via conventional optical lithography process and radio frequency (RF) magnetron sputtering. In order to reach Ohmic contact, the device was annealed in argon circumstances at 450 oC by rapid thermal annealing (RTA) system for 10 min. After the systematic measurements, the current-voltage (I-V) curve of photo and dark current and time-dependent photocurrent response results exhibited a good responsivity and reliability, indicating that the high c-axis ZnO thin film is a suitable sensing layer for UV photodetector application.

We offered a method to directly synthesize high c-axis (0002) ZnO thin film by plasma enhanced chemical vapor deposition. The as-synthesized ZnO thin film combined with Pt interdigitated electrode was used as sensing layer for ultraviolet photodetector, showing a high performance through a combination of its good responsivity and reliability.

In this study, zinc oxide (ZnO) thin films with high c-axis (0002) preferential orientation have been successfully and effectively synthesized onto ...

Integration of Light Trapping Silver Nanostructures in Hydrogenated Microcrystalline Silicon Solar Cells by Transfer Printing

One of the potential applications of metal nanostructures is light trapping in solar cells, where unique optical properties of nanosized metals, commonly known as plasmonic effects, play an important role. Research in this field has, however, been impeded owing to the difficulty of fabricating devices containing the desired functional metal nanostructures. In order to provide a viable strategy to this issue, we herein show a transfer printing-based approach that allows the quick and low-cost integration of designed metal nanostructures with a variety of device architectures, including solar cells. Nanopillar poly(dimethylsiloxane) (PDMS) stamps were fabricated from a commercially available nanohole plastic film as a master mold. On this nanopatterned PDMS stamps, Ag films were deposited, which were then transfer-printed onto block copolymer (binding layer)-coated hydrogenated microcrystalline Si (&#181;c-Si:H) surface to afford ordered Ag nanodisk structures. It was confirmed that the resulting Ag nanodisk-incorporated &#181;c-Si:H solar cells show higher performances compared to a cell without the transfer-printed Ag nanodisks, thanks to plasmonic light trapping effect derived from the Ag nanodisks. Because of the simplicity and versatility, further device application would also be feasible thorough this approach.

A viable transfer printing-based methodology to introduce plasmonic metal nanostructures in solar cells is described. Using nanopillar poly(dimethylsiloxane) stamps, an Ag-based ordered nanodisk array was integrated with standard hydrogenated microcrystalline Si solar cells, which led to improved device performances due to plasmonic light trapping.

One of the potential applications of metal nanostructures is light trapping in solar cells, where unique optical properties of nanosized metals, commonly ...

Electrospray Deposition of Uniform Thickness Ge23Sb7S70 and As40S60 Chalcogenide Glass Films

Solution-based electrospray film deposition, which is compatible with continuous, roll-to-roll processing, is applied to chalcogenide glasses. Two chalcogenide compositions are demonstrated: Ge23Sb7S70 and As40S60, which have both been studied extensively for planar mid-infrared (mid-IR) microphotonic devices. In this approach, uniform thickness films are fabricated through the use of computer numerical controlled (CNC) motion. Chalcogenide glass (ChG) is written over the substrate by a single nozzle along a serpentine path. Films were subjected to a series of heat treatments between 100 &#176;C and 200 &#176;C under vacuum to drive off residual solvent and densify the films. Based on transmission Fourier transform infrared (FTIR) spectroscopy and surface roughness measurements, both compositions were found to be suitable for the fabrication of planar devices operating in the mid-IR region. Residual solvent removal was found to be much quicker for the As40S60 film as compared to Ge23Sb7S70. Based on the advantages of electrospray, direct printing of a gradient refractive index (GRIN) mid-IR transparent coating is envisioned, given the difference in refractive index of the two compositions in this study.

Electrospray Deposition of Uniform Thickness Ge23Sb7S70 and As40S60 Chalcogenide Glass Films

A method of uniform thickness solution-derived chalcogenide glass film deposition is demonstrated using computer numerical controlled motion of a single-nozzle electrospray.

Solution-based electrospray film deposition, which is compatible with continuous, roll-to-roll processing, is applied to chalcogenide glasses. Two ...

High Temperature Fabrication of Nanostructured Yttria-Stabilized-Zirconia (YSZ) Scaffolds by In Situ Carbon Templating Xerogels

We demonstrate a method for the high temperature fabrication of porous, nanostructured yttria-stabilized-zirconia (YSZ, 8 mol% yttria - 92 mol% zirconia) scaffolds with tunable specific surface areas up to 80 m2&#183;g-1. An aqueous solution of a zirconium salt, yttrium salt, and glucose is mixed with propylene oxide (PO) to form a gel. The gel is dried under ambient conditions to form a xerogel. The xerogel is pressed into pellets and then sintered in an argon atmosphere. During sintering, a YSZ ceramic phase forms and the organic components decompose, leaving behind amorphous carbon. The carbon formed in situ serves as a hard template, preserving a high surface area YSZ nanomorphology at sintering temperature. The carbon is subsequently removed by oxidation in air at low temperature, resulting in a porous, nanostructured YSZ scaffold. The concentration of the carbon template and the final scaffold surface area can be systematically tuned by varying the glucose concentration in the gel synthesis. The carbon template concentration was quantified using thermogravimetric analysis (TGA), the surface area and pore size distribution was determined by physical adsorption measurements, and the morphology was characterized using scanning electron microscopy (SEM). Phase purity and crystallite size was determined using X-ray diffraction (XRD). This fabrication approach provides a novel, flexible platform for realizing unprecedented scaffold surface areas and nanomorphologies for ceramic-based electrochemical energy conversion applications, e.g. solid oxide fuel cell (SOFC) electrodes.

High Temperature Fabrication of Nanostructured Yttria-Stabilized-Zirconia YSZ Scaffolds by In Situ Carbon Templating Xerogels

A protocol for fabricating porous, nanostructured yttria-stabilized-zirconia (YSZ) scaffolds at temperatures between 1,000 &#176;C and 1,400 &#176;C is presented.

We demonstrate a method for the high temperature fabrication of porous, nanostructured yttria-stabilized-zirconia (YSZ, 8 mol% yttria - 92 mol% zirconia) ...

Fabrication of Ultra-thin Color Films with Highly Absorbing Media Using Oblique Angle Deposition

Ultra-thin film structures have been studied extensively for use as optical coatings, but performance and fabrication challenges remain.&#160; We present an advanced method for fabricating ultra-thin color films with improved characteristics. The proposed process addresses several fabrication issues, including large area processing. Specifically, the protocol describes a process for fabricating ultra-thin color films using an electron beam evaporator for oblique angle deposition of germanium (Ge) and gold (Au) on silicon (Si) substrates.&#160; Film porosity produced by the oblique angle deposition induces color changes in the ultra-thin film. The degree of color change depends on factors such as deposition angle and film thickness. Fabricated samples of the ultra-thin color films showed improved color tunability and color purity. In addition, the measured reflectance of the fabricated samples was converted into chromatic values and analyzed in terms of color. Our ultra-thin film fabricating method is expected to be used for various ultra-thin film applications such as flexible color electrodes, thin film solar cells, and optical filters. Also, the process developed here for analyzing the color of the fabricated samples is broadly useful for studying various color structures.

We present a detailed method for fabricating ultra-thin color films with improved characteristics for optical coatings. The oblique angle deposition technique using an electron beam evaporator allows improved color tunability and purity. Fabricated films of Ge and Au on Si substrates were analyzed by reflectance measurements and color information conversion.

Ultra-thin film structures have been studied extensively for use as optical coatings, but performance and fabrication challenges remain.&#160; We present ...