Ut-Battelle, Inc.

University of Pennsylvania

The University of Tennessee Research Foundation

Sergei V Kalinin

Stephen Jesse

Dawn A Bonnell

Rodolfo Antonio Alvarez

Albina Y Borisevich

Rama K Vasudevan

Petro Maksymovych

Raymond Robert Unocic

Bobby G Sumpter

Ho Nyung Lee

Yongtao Liu

Arthur P Baddorf

Ondrej E Dyck

Kyle P Kelley

Maxim A Ziatdinov

Jacob D Hinkle

Nina Balke

Kevin Roccapriore

Nancy Johnston Dudney

Alan T Johnson

Olga S Ovchinnikova

Hans M Christen

Alexei L Gruverman

Junsoo Shin

Anton V Ievlev

Nikolay Borodinov

Vincent Meunier

Edgar Karapetian

Mark Kachanov

Alex Belianinov

Rui Shao

Suhas Somnath

Marcus Freitag

Liam F Collins

Brian J Rodriguez

Andrew R Lupini

Yunseok Kim

Evgheni Strelcov

Qian He

Amit Kumar

Alexander Tselev

Maxim P Nikiforov

Systems are provided for machine learning-driven operation of instrumentation with human in the loop. The systems use a model with learnt model parameters to define points for physical-characteristic measurements once the model is trained. The systems use active learning, which considers selection, reinforcement and/or adjustment inputs from the instrumentation's user, to enable describing a relationship between local features of sample-surface structure shown in image patches and determined representations of physical-characteristic measurements.

Machine learning-driven operation of instrumentation with human in the loop

Systems, methods and programs are provided for automated science experiments which use a model with learnt model parameters to define points for physical-characteristic measurements once the model is trained. The systems, methods and programs use active learning which enables describing a relationship between local features of sample-surface structure shown in image patches and determined representations of physical-characteristic measurements.

Science-driven automated experiments

A system and method (referred to as the system) fabricates controllable atomic assemblies in two and three dimensions. The systems identify by a non-invasive imager, a local atomic structure, distribution of vacancies, and dopant atoms and modify, by a microscopic modifier, the local atomic structure, via electron beam irradiation. The systems store, by a knowledge base, cause-and-effect relationships based on a non-invasive imaging and electron scans. The systems detect, by detectors, changes in the local atomic structure induced by the electron irradiation; and fabricate, a modified atomic structure by a beam control software and feedback.

Atomic-scale e-beam sculptor

Techniques for generating full-spatial resolution, full spectral resolution image(s) from a 3D spectral-data cube for any spectral value within a given spectral range are provided without requiring the acquisition of all full-spatial resolution, full spectral resolution data by an instrument. The 3D spectral-data cube is generated from a limited number of full-spatial resolution, sparse spectral resolution data and a sparse-spatial resolution, full-spectral resolution data of the same area of the sample. The use of the 3D spectral-data cube reduces the data acquisition time.

Pan-sharpening for microscopy

A system and method (referred to as a method) to fabricate nanorobots. The method generates a pixel map of an atomic object and identifies portions of the atomic object that form a nanorobot. The method stores those identifications in a memory. The method adjusts an electron beam to a noninvasive operating level and images the portions of the atomic object that form the nanorobot. The method executes a plurality of scanning profiles by the electron beam to form the nanorobot and detects nanorobot characteristics and their surroundings via the electron beam in response to executing the plurality of scanning profiles.

Beam controlled nano-robotic device

A method for sculpting crystalline oxide structures for bulk nanofabrication is provided. The method includes the controlled electron beam induced irradiation of amorphous and liquid phase precursor solutions using a scanning transmission electron microscope. The atomically focused electron beam includes operating parameters (e.g., location, dwell time, raster speed) that are selected to provide a higher electron dose in patterned areas and a lower electron dose in non-patterned areas. Concurrently with the epitaxial growth of crystalline features, the present method includes scanning the substrate to provide information on the size of the crystalline features with atomic resolution. This approach provides for atomic level sculpting of crystalline oxide materials from a metastable amorphous precursor and the liquid phase patterning of nanocrystals.

Bulk nanofabrication with single atomic plane precision via atomic-level sculpting of crystalline oxides

Microwave AC conductivity may be improved or tuned in a material, for example, a dielectric or semiconductor material, by manipulating domain wall morphology in the material. Domain walls may be created, erased or reconfigured to control the AC conductivity, for example, for crafting circuit elements. The density and placement of domain walls may increase or decrease the AC conductivity and may control AC conduction pathways through the material. An electric potential applied to the material's surface may create a desired pattern of domain walls to meet desired AC conductivity criteria. Incline angle of the domain walls may be modified relative to a crystallographic axis of the material to temporarily or permanently modify or gate AC conductivity of the material. For example, the AC conductivity of the material may be gated by domain wall incline angle to increase, decrease or throttle current flowing through the material for an electronic circuit element.

Microwave AC conductivity of domain walls

Apparatus and methods are described for scanning probe microscopy and spectroscopy based on acquisition of full probe response. The full probe response contains valuable information about the probe-sample interaction that is lost in traditional scanning probe microscopy and spectroscopy methods. The full probe response is analyzed post data acquisition using fast Fourier transform and adaptive filtering, as well as multivariate analysis. The full response data is further compressed to retain only statistically significant components before being permanently stored.

Full information acquisition in scanning probe microscopy and spectroscopy

A system and method for electrochemical force microscopy are provided. The system and method are based on a multidimensional detection scheme that is sensitive to forces experienced by a biased electrode in a solution. The multidimensional approach allows separation of fast processes, such as double layer charging, and charge relaxation, and slow processes, such as diffusion and faradaic reactions, as well as capturing the bias dependence of the response. The time-resolved and bias measurements can also allow probing both linear (small bias range) and non-linear (large bias range) electrochemical regimes and potentially the de-convolution of charge dynamics and diffusion processes from steric effects and electrochemical reactivity.

Electrochemical force microscopy

Scanning probe microscopy may include a method for generating a band excitation (BE) signal and simultaneously exciting a probe at a plurality of frequencies within a predetermined frequency band based on the excitation signal. A response of the probe is measured across a subset of frequencies of the predetermined frequency band and the excitation signal is adjusted based on the measured response.

Band excitation method applicable to scanning probe microscopy

An excitation voltage biases an ionic conducting material sample over a nanoscale grid. The bias sweeps a modulated voltage with increasing maximal amplitudes. A current response is measured at grid locations. Current response reversal curves are mapped over maximal amplitudes of the bias cycles. Reversal curves are averaged over the grid for each bias cycle and mapped over maximal bias amplitudes for each bias cycle. Average reversal curve areas are mapped over maximal amplitudes of the bias cycles. Thresholds are determined for onset and ending of electrochemical activity. A predetermined number of bias sweeps may vary in frequency where each sweep has a constant number of cycles and reversal response curves may indicate ionic diffusion kinetics.

Real space mapping of oxygen vacancy diffusion and electrochemical transformations by hysteretic current reversal curve measurements

A method and system for probing mobile ion diffusivity and electrochemical reactivity on a nanometer length scale of a free electrochemically active surface includes a control module that biases the surface of the material. An electrical excitation signal is applied to the material and induces the movement of mobile ions. An SPM probe in contact with the surface of the material detects the displacement of mobile ions at the surface of the material. A detector measures an electromechanical strain response at the surface of the material based on the movement and reactions of the mobile ions. The use of an SPM tip to detect local deformations allows highly reproducible measurements in an ambient environment without visible changes in surface structure. The measurements illustrate effective spatial resolution comparable with defect spacing and well below characteristic grain sizes of the material.

Real space mapping of ionic diffusion and electrochemical activity in energy storage and conversion materials

An approach for the thermomechanical characterization of phase transitions in polymeric materials (polyethyleneterephthalate) by band excitation acoustic force microscopy is developed. This methodology allows the independent measurement of resonance frequency, Q factor, and oscillation amplitude of a tip-surface contact area as a function of tip temperature, from which the thermal evolution of tip-surface spring constant and mechanical dissipation can be extracted. A heating protocol maintained a constant tip-surface contact area and constant contact force, thereby allowing for reproducible measurements and quantitative extraction of material properties including temperature dependence of indentation-based elastic and loss moduli.

Spatially resolved quantitative mapping of thermomechanical properties and phase transition temperatures using scanning probe microscopy

Methods and apparatus are described for scanning probe microscopy. A method includes generating a band excitation (BE) signal having finite and predefined amplitude and phase spectrum in at least a first predefined frequency band; exciting a probe using the band excitation signal; obtaining data by measuring a response of the probe in at least a second predefined frequency band; and extracting at least one relevant dynamic parameter of the response of the probe in a predefined range including analyzing the obtained data. The BE signal can be synthesized prior to imaging (static band excitation), or adjusted at each pixel or spectroscopy step to accommodate changes in sample properties (adaptive band excitation). An apparatus includes a band excitation signal generator; a probe coupled to the band excitation signal generator; a detector coupled to the probe; and a relevant dynamic parameter extractor component coupled to the detector, the relevant dynamic parameter extractor including a processor that performs a mathematical transform selected from the group consisting of an integral transform and a discrete transform.

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Knoxville, TN, United States of America

Sergei V Kalinin