3D OXIDES

Saint-Genis-Pouilly, France

3D OXIDES

Saint-Genis-Pouilly, France

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A chemical gas phase deposition process comprises steps of providing a high vacuum chamber, and inside the high vacuum chamber: positioning a substrate surface; positioning a mask parallel to the substrate surface, whereby the mask comprises one or more openings; adjusting a gap of determined dimension between the substrate surface and the mask; and orienting a plurality of chemical precursor beams of at least one precursor species towards the mask with line of sight propagation, each of the plurality of chemical precursor beams being emitted from an independent punctual source, and molecules of the chemical precursor pass through the one or more mask openings to impinge onto the substrate surface for deposition thereon. At least a part of the chemical precursor molecules decompose on the substrate surface at a decomposition temperature. The process further comprises adjusting a temperature of the substrate surface greater or equal to the chemical precursor molecule decomposition temperature, thereby remaining greater than a mask temperature, and maintaining the mask temperature below the decomposition temperature, thereby causing a decomposition of the chemical precursor and a growth of a film on the substrate surface, but not on the mask; and heating the substrate surface using a heating device.


A chemical gas phase deposition process comprises steps of providing a high vacuum chamber, and inside the high vacuum chamber: positioning a substrate surface; positioning a mask parallel to the substrate surface, whereby the mask comprises one or more openings; adjusting a gap of determined dimension between the substrate surface and the mask; and orienting a plurality of chemical precursor beams of at least one precursor species towards the mask with line of sight propagation, each of the plurality of chemical precursor beams being emitted from an independent punctual source, and molecules of the chemical precursor pass through the one or more mask openings to impinge onto the substrate surface for deposition thereon. At least a part of the chemical precursor molecules decompose on the substrate surface at a decomposition temperature. The process further comprises adjusting a temperature of the substrate surface greater or equal to the chemical precursor molecule decomposition temperature, thereby remaining greater than a mask temperature, and maintaining the mask temperature below the decomposition temperature, thereby causing a decomposition of the chemical precursor and a growth of a film on the substrate surface, but not on the mask; and heating the substrate surface using a heating device.


Wagner E.,3D OXIDES | Sandu C.S.,3D OXIDES | Sandu C.S.,Ecole Polytechnique Federale de Lausanne | Harada S.,3D OXIDES | And 3 more authors.
Thin Solid Films | Year: 2015

Chemical Beam Vapour Deposition is a gas phase deposition technique, operated under high vacuum conditions, in which evaporated chemical precursors are thermally decomposed on heated substrates to form a film. In the particular equipment used in this work, different chemical beams effuse from a plurality of punctual precursor sources with line of sight trajectory to the substrate. A shadow mask is used to produce 3D-structures in a single step, replicating the apertures of a stencil as deposits on the substrate. The small gap introduced between substrate and mask induces a temperature difference between both surfaces and is used to deposit selectively solely on the substrate without modifying the mask, taking advantage of the deposition rate dependency on temperature. This small gap also enables the deposition of complex patterned structures resulting from the superposition of many patterns obtained using several precursor beams from different directions through a single mask aperture. A suitable process parameter window for precursor flow and substrate temperature is evidenced to maximize resolution. © 2015 Elsevier B.V.


Eisenberg D.,University of Amsterdam | Stroek W.,University of Amsterdam | Geels N.J.,University of Amsterdam | Sandu C.S.,3D OXIDES | And 3 more authors.
Chemistry - A European Journal | Year: 2016

Replacing platinum as an oxygen reduction catalyst is an important scientific and technological challenge. Herein we report a simple synthesis of a complex carbon with very good oxygen reduction reaction (ORR) activity at pH 13. Pyrolysis of magnesium nitrilotriacetate yields a carbon with hierarchical micro/meso/macro porosity, resulting from in situ templating by spontaneously forming MgO nanoparticles and from etching by pyrolysis gases. The mesopores are lined with highly graphitic shells. The high ORR activity is attributed to a good balance between high specific surface area and mass transport through the hierarchical porosity, and to improved electronic conductivity through the graphitic shells. This novel carbon has a high surface area (1320 m2g-1), and high nitrogen content for a single precursor synthesis (∼6 %). Importantly, its synthesis is both cheap and easily scalable. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.


Dabirian A.,Ecole Polytechnique Federale de Lausanne | Kuzminykh Y.,Ecole Polytechnique Federale de Lausanne | Kuzminykh Y.,Empa - Swiss Federal Laboratories for Materials Science and Technology | Wagner E.,3D Oxides | And 4 more authors.
Thin Solid Films | Year: 2014

Chemical vapour deposition (CVD) processes depend on the availability of suitable precursors. Precursors that deliver a stable vapour pressure are favourable in classical CVD processes, as they ensure process reproducibility. In high vacuum CVD (HV-CVD) process vapour pressure stability of the precursor is of particular importance, since no carrier gas assisted transport can be used. The dimeric Nb2(OEt)10 does not fulfil this requirement since it partially dissociates upon heating. Dimethylamino functionalization of an ethoxy ligand of Nb(OEt)5 acts as an octahedral field completing entity and leads to Nb(OEt)4(dmae). We show that Nb(OEt)4(dmae) evaporates as monomeric molecule and ensures a stable vapour pressure and, consequently, stable flow. A set of HV-CVD experiments were conducted using this precursor by projecting a graded molecular beam of the precursor onto the substrate at deposition temperatures from 320 °C to 650 °C. Film growth rates ranging from 8 nm·h- 1 to values larger than 400 nm·h- 1 can be obtained in this system illustrating the high level of control available over the film growth process. Classical CVD limiting conditions along with the recently reported adsorption-reaction limited conditions are observed and the chemical composition, and microstructural and optical properties of the films are related to the corresponding growth regime. Nb(OEt)4(dmae) provides a large process window of deposition temperatures and precursor fluxes over which carbon-free and polycrystalline niobium oxide films with growth rates proportional to precursor flux are obtained. This feature makes Nb(OEt)4(dmae) an attractive precursor for combinatorial CVD of niobium containing complex oxide films that are finding an increasing interest in photonics and photoelectrochemical water splitting applications. The adsorption-reaction limited conditions provide extremely small growth rates comparable to an atomic layer deposition (ALD) process indicating that HV-CVD has the potential to be an alternative to ALD for growth of ultrathin films on low aspect ratio substrates. © 2014 Elsevier B.V.


Wagner E.,ABCD Technology | Sandu C.S.,ABCD Technology | Harada S.,3D Oxides | Pellodi C.,University of Applied Sciences and Arts Western Switzerland | And 3 more authors.
ACS Combinatorial Science | Year: 2016

An innovative deposition system has been developed to construct complex material thin films from single-element precursors by chemical beam vapor deposition (CBVD). It relies on well distributed punctual sources that emit individually controlled precursor beams toward the substrate under high vacuum conditions combined with well designed cryo-panel surfaces that avoid secondary precursor sources. In this configuration the impinging flows of all precursors can be calculated at any substrate point considering the controlled angular distribution of the emitted beams and the ballistic trajectory of the molecules. The flow simulation is described in details. The major advantage of the deposition system is its ability to switch between several possible controlled combinatorial configurations, in which the substrate is exposed to a wide range of flow compositions from the different precursors, and a uniform configuration, in which the substrate is exposed to a homogeneous flow, even on large substrates, with high precursor use efficiency. Agreement between calculations and depositions carried out in various system configurations and for single, binary, or ternary oxides in mass transfer limited regime confirms that the distribution of incoming precursors on the substrate follows the theoretical models. Additionally, for some selected precursors and in some selected conditions, almost 100% of the precursor impinging on the substrate is incorporated to the deposit. The results of this work confirm the potentialities of CBVD both as a research tool to investigate efficiently deposition processes and as a fabrication tool to deposit on large surfaces. © 2016 American Chemical Society.


Sandu C.S.,3D OXIDES | Wagner E.,3D OXIDES | Harada S.,3D OXIDES | Benvenuti G.,3D OXIDES | And 4 more authors.
Thin Solid Films | Year: 2016

Chemical beam vapour deposition (CBVD) is a thin film deposition technique operated under high vacuum conditions in which film growth occurs through the thermally activated chemical decomposition of precursor molecules at the substrate surface. This technique was used in a combinatorial mode to investigate the influence of Si doping on the properties of Nb-doped TiO2 films, a well-known transparent conductive oxide material. The ternary oxide system (Si, Nb, Ti, O) displays good intermiscibility between the elements. By adding a Si precursor flow gradient to homogeneous Ti and Nb precursor flows, it was demonstrated that the resistivity of deposited films increased by over 5 orders of magnitude (from 1 to 100,000 Ω·cm) with Si doping levels between 2 and 21at.%. Meanwhile, only a slight variation of the refractive index of about 10% was observed. A fundamental film morphology study showed that the conductivity variation was due to Si segregation at the grain boundaries of the conductive Nb:TiO2 structure. © 2016


PubMed | University of Amsterdam, University of Texas at Austin and 3D OXIDES
Type: Journal Article | Journal: Chemistry (Weinheim an der Bergstrasse, Germany) | Year: 2016

Replacing platinum as an oxygen reduction catalyst is an important scientific and technological challenge. Herein we report a simple synthesis of a complex carbon with very good oxygen reduction reaction (ORR) activity at pH13. Pyrolysis of magnesium nitrilotriacetate yields a carbon with hierarchical micro/meso/macro porosity, resulting from in situ templating by spontaneously forming MgO nanoparticles and from etching by pyrolysis gases. The mesopores are lined with highly graphitic shells. The high ORR activity is attributed to a good balance between high specific surface area and mass transport through the hierarchical porosity, and to improved electronic conductivity through the graphitic shells. This novel carbon has a high surface area (1320m(2) g(-1) ), and high nitrogen content for a single precursor synthesis (6%). Importantly, its synthesis is both cheap and easily scalable.


PubMed | Ecole Polytechnique Federale de Lausanne, 3D Oxides, ABCD Technology and University of Applied Sciences and Arts Western Switzerland
Type: Journal Article | Journal: ACS combinatorial science | Year: 2016

An innovative deposition system has been developed to construct complex material thin films from single-element precursors by chemical beam vapor deposition (CBVD). It relies on well distributed punctual sources that emit individually controlled precursor beams toward the substrate under high vacuum conditions combined with well designed cryo-panel surfaces that avoid secondary precursor sources. In this configuration the impinging flows of all precursors can be calculated at any substrate point considering the controlled angular distribution of the emitted beams and the ballistic trajectory of the molecules. The flow simulation is described in details. The major advantage of the deposition system is its ability to switch between several possible controlled combinatorial configurations, in which the substrate is exposed to a wide range of flow compositions from the different precursors, and a uniform configuration, in which the substrate is exposed to a homogeneous flow, even on large substrates, with high precursor use efficiency. Agreement between calculations and depositions carried out in various system configurations and for single, binary, or ternary oxides in mass transfer limited regime confirms that the distribution of incoming precursors on the substrate follows the theoretical models. Additionally, for some selected precursors and in some selected conditions, almost 100% of the precursor impinging on the substrate is incorporated to the deposit. The results of this work confirm the potentialities of CBVD both as a research tool to investigate efficiently deposition processes and as a fabrication tool to deposit on large surfaces.

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