Nanoscale chemical tomography of buried organic–inorganic interfaces in the chiton tooth

Gordon, Lyle M.; Joester, Derk

doi:10.1038/nature09686

Cited by 255 publications

(212 citation statements)

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“…x-y plane: 0.2 nm 119 z direction: 0.05 nm 119 • Single atom sensitivity 153 • Reconstruction artifacts can occur due to the quantum nature of the atom, field penetration at the apex of the needle, an aspherical apex, changes in the evaporation order or different evaporation rates of different elements 154 • In heterogeneous structures, surface electric field variations can lead to local magnification effects and the trajectory of different elements overlapping 154 • Thermal artifacts can occur under high laser fluence 154 • Atom probe specimens have large surface area to volume ratios, making them sensitive to the processing environment 155 Electron energy loss spectroscopy (EELS) STEM-EELS uses a 100-300 keV kinetic energy electron beam, which is inelastically scattered when interacting with electron clouds surrounding atoms. Energy distribution of transmitted electron beam measured using a magnetic prism to separate electrons by energy, and the energy spectrum is recorded.…”

Section: Atom Probe Tomography (Apt)mentioning

confidence: 99%

Perovskite-Inspired Photovoltaic Materials: Toward Best Practices in Materials Characterization and Calculations

et al. 2017

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ABSTRACT:Recently, there has been an explosive growth in research based on hybrid lead-halide perovskites for photovoltaics owing to rapid improvements in efficiency. The advent of these materials for solar applications has led to widespread interest in understanding the key enabling properties of these materials. This has resulted in renewed interest in related compounds and a search for materials that may replicate the defect-tolerant properties and long lifetimes of the hybrid lead-halide perovskites. Given the rapid pace of development of the field, the rises in efficiencies of these systems have outpaced the more basic understanding of these materials. Measuring or calculating the basic properties, such as crystal/electronic structure and composition, can be challenging because some of these materials have anisotropic structures, and/or are composed of both heavy metal cations and volatile, mobile, light elements. Some consequences are beam damage during characterization, composition change under vacuum, or compound effects, such as the alteration of the electronic structure through the influence of the substrate. These effects make it challenging to understand the basic properties integral to optoelectronic operation. Compounding these difficulties is the rapid pace with which the field progresses. This has created an ongoing need to continually evaluate best practices with respect to characterization and calculations, as well as to identify inconsistencies in reported values to determine if those inconsistencies are rooted in characterization methodology or materials synthesis. This article describes the difficulties in characterizing hybrid lead-halide perovskites and new materials, and how these challenges may be overcome. 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60 2 challenges discussed. The focus in this article is on crystallography, composition measurements, photoemission spectroscopy and calculations on perovskites and new, related absorbers. We suggest how some of the important artifacts could be avoided and how the reporting for each technique could be streamlined between groups to ensure reproducibility as the field progresses.

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Section: Atom Probe Tomography (Apt)mentioning

confidence: 99%

Perovskite-Inspired Photovoltaic Materials: Toward Best Practices in Materials Characterization and Calculations

et al. 2017

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“…Laser pulsing heats the specimen tip surface, lowering the required electric field for field evaporation and, consequently, reducing premature specimen failure from stresses generated by the electric field. We discuss here the rapidly improving analysis capabilities for self-assembled monolayers [11][12][13], polymers [14][15][16], and the complex architecture of a tooth biomineral nanocomposite [17].…”

Section: Early Workmentioning

confidence: 99%

Organic Materials and Organic/Inorganic Heterostructures in Atom Probe Tomography

et al. 2012

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Nano-scale organic/inorganic interfaces are key to a wide range of materials. In many biominerals, for instance bone or teeth, outstanding fracture toughness and wear resistance can be attributed to buried organic/ inorganic interfaces. Organic/inorganic interfaces at very small length scales are becoming increasingly important also in nano and electronic materials. For example, functionalized inorganic nanomaterials have great potential in biomedicine or sensing applications. Thin organic films are used to increase the conductivity of LiFePO4 electrodes in lithium ion batteries, and solid electrode interphases (SEI) form by uncontrolled electrolyte decomposition. Organics play a key role in dye-sensitized solar cells, organic photovoltaics, and nano-dielectrics for organic field-effect transistors. The interface between oxide semiconductors and polymer substrates is critical in emergent applications, for example, flexible displays.

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“…APT is specifically adept at characterizing nanomaterials with internal organic-inorganic interfaces, due to its elemental sensitivity and spatial accuracy. We recently demonstrated this capability in biological minerals in the magnetite cusp of the chiton tooth [4] and vertebrate bone and dentin [5].…”

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Towards Atom Probe Tomography of Hybrid Organic-Inorganic Nanoparticles

Gordon¹,

Cohen²,

Joester³

2013

Microsc Microanal

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Surface functionalization of inorganic nanoparticles is widely used to modify material properties for a variety of applications including medical therapies and diagnostics. While inorganic nanoparticles may be characterized via electron microscopy and X-ray scattering, study of hybrid nanomaterials and, in particular, buried interfaces is very challenging. Here we discuss the application of atom probe tomography (APT) to imaging organic-inorganic interfaces of biological nanoparticles, ferritin, as a model system. Ferritin is a structurally well-characterized protein, critical across biology to store some 4500 iron atoms and transport iron as mineralized Fe (III) [1]. This 24-subunit 12 nm protein has a spherical 8 nm core into which Fe (II) enters and is subsequently oxidized.APT is uniquely capable of providing the necessary chemical and structural insight at the atomic scale by directly probing the location and chemical identity of the atoms within a small sample of material. APT consists of a field-ion microscope coupled to a time-of-flight mass spectrometer, providing chemical and three-dimensional positional information of ions successively field evaporated from a sharp sample. The advent of ultraviolet laser pulsing has widely enlarged the scope of APT to include a range of insulating materials, including hybrid organic-inorganic materials [3]. APT is specifically adept at characterizing nanomaterials with internal organic-inorganic interfaces, due to its elemental sensitivity and spatial accuracy. We recently demonstrated this capability in biological minerals in the magnetite cusp of the chiton tooth [4] and vertebrate bone and dentin [5].We report here on the characterization of native equine spleen ferritin using APT. Greene et al. recently used APT to analyse ferritin as a model for characterizing biological materials using APT. In this work, researchers used a solidified organic/salt matrix, which contained numerous ferritin complexes [6]. These APT tips of dense ferritin/salt deposits were able to undergo APT, providing a proof of concept through mass spectrometry results. However, they were unable to characterize individual proteins and their experiments suffered from drastic tip bending, preventing meaningful reconstructions [6]. To image individual ferritin protein complexes, we deposited a dilute solution of native equine spleen ferritin onto a silicon post coated with Au-Pd (Figure 1) [7]. Further encapsulation of the adsorbed molecules with Au-Pd and subsequent focused ion beam milling allowed for the fabrication of APT sample tips. This method allowed for a small number of ferritin complexes to be characterized. This work not only allows for resolution and characterization of ferritin, but also shows our ability to use APT to characterize discrete nanoparticles.Atom probe tomography characterizes ferritin as spherical accumulations of iron and oxygen surrounded by carbon and nitrogen. Creating an isoconcentration surface we can identify the iron-rich core within the ferritin protein (Figure ...

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Nanoscale chemical tomography of buried organic–inorganic interfaces in the chiton tooth

Cited by 255 publications

References 39 publications

Perovskite-Inspired Photovoltaic Materials: Toward Best Practices in Materials Characterization and Calculations

Perovskite-Inspired Photovoltaic Materials: Toward Best Practices in Materials Characterization and Calculations

Organic Materials and Organic/Inorganic Heterostructures in Atom Probe Tomography

Towards Atom Probe Tomography of Hybrid Organic-Inorganic Nanoparticles

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