Synthesis of freestanding single-crystal perovskite films and heterostructures by etching of sacrificial water-soluble layers

Lu, Di; Baek, David J.; Hong, Seung Sae; Kourkoutis, Lena F.; Hikita, Yasuyuki; Hwang, Harold Y.

doi:10.1038/nmat4749

Title: Synthesis of freestanding single-crystal perovskite films and heterostructures by etching of sacrificial water-soluble layers

Abstract

Here, the ability to create and manipulate materials in two-dimensional (2D) form has repeatedly had transformative impact on science and technology. In parallel with the exfoliation and stacking of intrinsically layered crystals^{1, 2, 3, 4, 5}, atomic-scale thin film growth of complex materials has enabled the creation of artificial 2D heterostructures with novel functionality^{6, 7, 8, 9} and emergent phenomena, as seen in perovskite heterostructures^{10, 11, 12}. However, separation of these layers from the growth substrate has proved challenging, limiting the manipulation capabilities of these heterostructures with respect to exfoliated materials. Here we present a general method to create freestanding perovskite membranes. The key is the epitaxial growth of water-soluble Sr₃Al₂O₆ on perovskite substrates, followed by in situ growth of films and heterostructures. Millimetre-size single-crystalline membranes are produced by etching the Sr₃Al₂O₆ layer in water, providing the opportunity to transfer them to arbitrary substrates and integrate them with heterostructures of semiconductors and layered compounds^{13, 14}.

Authors:

Lu, Di ^[1]; Baek, David J. ^[2]; Hong, Seung Sae ^[3]; Kourkoutis, Lena F. ^[4]; Hikita, Yasuyuki ^[5]; Hwang, Harold Y. ^[3]

Stanford Univ., Stanford, CA (United States); SLAC National Accelerator Lab., Menlo Park, CA (United States)
Cornell Univ., Ithaca, NY (United States). Baker Lab.
SLAC National Accelerator Lab., Menlo Park, CA (United States); Stanford Univ., Stanford, CA (United States)
Cornell Univ., Ithaca, NY (United States)
SLAC National Accelerator Lab., Menlo Park, CA (United States)

Publication Date:: Mon Sep 12 00:00:00 EDT 2016

Research Org.:: SLAC National Accelerator Laboratory (SLAC), Menlo Park, CA (United States)

Sponsoring Org.:: USDOE

OSTI Identifier:: 1326981

Report Number(s):: SLAC-PUB-16802
Journal ID: ISSN 1476-1122; nmat4749

Grant/Contract Number:: AC02-76SF00515

Resource Type:: Accepted Manuscript

Journal Name:: Nature Materials

Additional Journal Information:: Journal Name: Nature Materials; Journal ID: ISSN 1476-1122

Publisher:: Nature Publishing Group

Country of Publication:: United States

Language:: English

Subject:: 36 MATERIALS SCIENCE

Citation Formats


                    Lu, Di, Baek, David J., Hong, Seung Sae, Kourkoutis, Lena F., Hikita, Yasuyuki, and Hwang, Harold Y. Synthesis of freestanding single-crystal perovskite films and heterostructures by etching of sacrificial water-soluble layers.  United States: N. p., 2016. 
Web.  doi:10.1038/nmat4749.

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                    Lu, Di, Baek, David J., Hong, Seung Sae, Kourkoutis, Lena F., Hikita, Yasuyuki, & Hwang, Harold Y. Synthesis of freestanding single-crystal perovskite films and heterostructures by etching of sacrificial water-soluble layers.  United States.  https://doi.org/10.1038/nmat4749

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                    Lu, Di, Baek, David J., Hong, Seung Sae, Kourkoutis, Lena F., Hikita, Yasuyuki, and Hwang, Harold Y. Mon .  
"Synthesis of freestanding single-crystal perovskite films and heterostructures by etching of sacrificial water-soluble layers".  United States.  https://doi.org/10.1038/nmat4749.  https://www.osti.gov/servlets/purl/1326981.

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@article{osti_1326981,

  title        = {Synthesis of freestanding single-crystal perovskite films and heterostructures by etching of sacrificial water-soluble layers},

  author       = {Lu, Di and Baek, David J. and Hong, Seung Sae and Kourkoutis, Lena F. and Hikita, Yasuyuki and Hwang, Harold Y.},

  abstractNote = {Here, the ability to create and manipulate materials in two-dimensional (2D) form has repeatedly had transformative impact on science and technology. In parallel with the exfoliation and stacking of intrinsically layered crystals1, 2, 3, 4, 5, atomic-scale thin film growth of complex materials has enabled the creation of artificial 2D heterostructures with novel functionality6, 7, 8, 9 and emergent phenomena, as seen in perovskite heterostructures10, 11, 12. However, separation of these layers from the growth substrate has proved challenging, limiting the manipulation capabilities of these heterostructures with respect to exfoliated materials. Here we present a general method to create freestanding perovskite membranes. The key is the epitaxial growth of water-soluble Sr3Al2O6 on perovskite substrates, followed by in situ growth of films and heterostructures. Millimetre-size single-crystalline membranes are produced by etching the Sr3Al2O6 layer in water, providing the opportunity to transfer them to arbitrary substrates and integrate them with heterostructures of semiconductors and layered compounds13, 14.},

  doi          = {10.1038/nmat4749},

  journal      = {Nature Materials},

  number       = ,

  volume       = ,

  place        = {United States},

  year         = {Mon Sep 12 00:00:00 EDT 2016},

  month        = {Mon Sep 12 00:00:00 EDT 2016}

}

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Incorporating oxides with radically different physical and chemical properties into heterostructures offers tantalizing possibilities to derive new functions and structures. Recently, we have fabricated freestanding 2D oxide membranes using the water-soluble perovskite Sr₃Al₂O₆ as a sacrificial buffer layer. Here, with atomic-resolution spectroscopic imaging, we observe that direct growth of oxide thin films on Sr₃Al₂O₆ can cause complete phase transformation of the buffer layer, rendering it water-insoluble. More importantly, we demonstrate that an ultrathin SrTiO₃ layer can be employed as an effective barrier to preserve Sr₃Al₂O₆ during subsequent growth, thus allowing its integration in a wider range of oxide heterostructures.
Cited by 18
https://doi.org/10.1021/acsami.6b14106

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Freestanding crystalline $YB a_{2} C u_{3} O_{7 - x}$ heterostructure membranes

Journal Article Chen, Zhuoyu ; Wang, Bai Yang ; Goodge, Berit H. ; ... - Physical Review Materials

We report the synthesis of millimeter-sized freestanding single-crystal YBa₂Cu₃O_7–x heterostructure membranes with nanoscale thickness. On a SrTiO₃ substrate, a heteroepitaxial water-soluble sacrificial layer of Sr₃Al₂O₆ followed by an encapsulated YBa₂Cu₃O_7–x film is grown by pulsed laser deposition. A freestanding YBa₂Cu₃O_7–x heterostructure membrane is obtained by etching the sacrificial layer. As a result, its high crystalline quality is demonstrated via x-ray diffraction, electrical measurements, and scanning transmission electron microscopy.
Cited by 37
https://doi.org/10.1103/physrevmaterials.3.060801

Full Text Available

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Title: Synthesis of freestanding single-crystal perovskite films and heterostructures by etching of sacrificial water-soluble layers

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Citation Formats

Mechanisms of cement hydration journal, December 2011

Chiral magnetic order at surfaces driven by inversion asymmetry journal, May 2007

Damage-free separation of GaN thin films from sapphire substrates journal, February 1998

High-quality and efficient transfer of large-area graphene films onto different substrates journal, May 2013

Oxide Interfaces--An Opportunity for Electronics journal, March 2010

Progress, Challenges, and Opportunities in Two-Dimensional Materials Beyond Graphene journal, March 2013

Piezoelectric Nanogenerators Based on Zinc Oxide Nanowire Arrays journal, April 2006

Hofstadter’s butterfly and the fractal quantum Hall effect in moiré superlattices journal, May 2013

Experimental Observation of the Quantum Anomalous Hall Effect in a Magnetic Topological Insulator journal, March 2013

Synthesis, assembly and applications of semiconductor nanomembranes journal, September 2011

Van der Waals heterostructures journal, July 2013

Electric Field Effect in Atomically Thin Carbon Films journal, October 2004

Room-temperature fabrication of transparent flexible thin-film transistors using amorphous oxide semiconductors journal, November 2004

Direct measurement of strain effects on magnetic and electrical properties of epitaxial SrRuO3 thin films journal, February 1998

Review on microfabricated micro-solid oxide fuel cell membranes journal, October 2009

Interface-Induced High-Temperature Superconductivity in Single Unit-Cell FeSe Films on SrTiO 3 journal, March 2012

Electric field control of the LaAlO3/SrTiO3 interface ground state journal, December 2008

Application of hydrogen ion beams to Silicon On Insulator material technology journal, February 1996

Emergent phenomena at oxide interfaces journal, January 2012

Influence of strain on the magnetization and magnetoelectric effect in La 0.7 A 0.3 Mn O 3 ∕ PMN − PT ( 001 ) ( A = Sr , Ca ) journal, February 2007

Graphene-Like Two-Dimensional Materials journal, January 2013

Tuning the Dimensionality of the Heavy Fermion Compound CeIn3 journal, February 2010

Interface Effect and Its Doping Dependence in La 1- x Sr x MnO 3 /SrTiO 3 Superlattices journal, November 2002

Large-scale pattern growth of graphene films for stretchable transparent electrodes journal, January 2009

Extreme selectivity in the lift‐off of epitaxial GaAs films journal, December 1987

Two-Dimensional Dielectric Nanosheets: Novel Nanoelectronics From Nanocrystal Building Blocks journal, October 2011

Mechanical Properties of Thin Single‐Crystal Gold Films journal, December 1960

Growth of Face-Centered-Cubic Metals on Sodium Chloride Substrates journal, May 1966

Microscopic origins for stabilizing room-temperature ferromagnetism in ultrathin manganite layers journal, June 2010

Tristrontium dialuminum hexaoxide: an intricate superstructure of perovskite journal, November 1990

Single-Crystalline SrRuO 3 Nanomembranes: A Platform for Flexible Oxide Electronics journal, December 2015

Ultrathin compound semiconductor on insulator layers for high-performance nanoscale transistors journal, November 2010

Ultrathin compound semiconductor on insulator layers for high performance nanoscale transistors text, January 2011

Interface induced high temperature superconductivity in single unit-cell FeSe films on SrTiO3 text, January 2012

Experimental Observation of the Quantum Anomalous Hall Effect in a Magnetic Topological Insulator text, January 2016

Electric Field Effect in Atomically Thin Carbon Films text, January 2004

Bienenstock, Cooper, and Munro Learning Rules Realized in Second-Order Memristors with Tunable Forgetting Rate journal, January 2019

Hydrogenation Dynamics of Electrically Controlled Metal–Insulator Transition in Proton‐Gated Transparent and Flexible WO 3 Transistors journal, June 2019

Synergetic Behavior in 2D Layered Material/Complex Oxide Heterostructures journal, December 2018

Ferroelectric Domain Wall Motion in Freestanding Single‐Crystal Complex Oxide Thin Film journal, December 2019

Conductive Oxide Interfaces for Field Effect Devices journal, June 2019

Stimulating Oxide Heterostructures: A Review on Controlling SrTiO 3 ‐Based Heterointerfaces with External Stimuli journal, August 2019

Atomic Scale Understanding of the Epitaxy of Perovskite Oxides on Flexible Mica Substrate journal, December 2019

Giant Uniaxial Strain Ferroelectric Domain Tuning in Freestanding PbTiO 3 Films journal, April 2020

Epitaxial Liftoff of Wafer‐Scale VO 2 Nanomembranes for Flexible, Ultrasensitive Tactile Sensors journal, April 2019

Nanoporous Films and Nanostructure Arrays Created by Selective Dissolution of Water-Soluble Materials journal, September 2018

Liquid–Solid Interfacial Assemblies of Soft Materials for Functional Freestanding Layered Membrane–Based Devices toward Electrochemical Energy Systems journal, April 2019

Rectifying Effect of the Sr 3 Al 2 O 6 /Ga 2 O 3 Heterojunction journal, September 2019

Strain Tuning in Complex Oxide Epitaxial Films Using an Ultrathin Strontium Aluminate Buffer Layer journal, January 2018

Assembly and Self-Assembly of Nanomembrane Materials-From 2D to 3D journal, January 2018

Freestanding crystalline oxide perovskites down to the monolayer limit journal, June 2019

Heterogeneous integration of single-crystalline complex-oxide membranes journal, February 2020

Epitaxial growth and layer-transfer techniques for heterogeneous integration of materials for electronic and photonic devices journal, October 2019

Enhanced bending-tuned magnetic properties in epitaxial cobalt ferrite nanopillar arrays on flexible substrates journal, January 2018

Fabrication of ultralong perovskite structure nanotubes journal, January 2018

Recent progress on flexible inorganic single-crystalline functional oxide films for advanced electronics journal, January 2019

Development of oxide heteroepitaxy for soft technology journal, January 2018

A versatile patterning process based on easily soluble sacrificial bilayers journal, August 2017

Stressor-layer-induced elastic strain sharing in SrTiO 3 complex oxide sheets journal, February 2018

Strain-induced resistance change in V 2 O 3 films on piezoelectric ceramic disks journal, March 2019

Non-Ohmic conduction in exfoliated La 0.7 Ca 0.3 MnO 3 thin films journal, January 2020

Spark plasma sintering of bulk SrAl 2 O 4 -Sr 3 Al 2 O 6 eutectic glass with wide-band optical window journal, April 2018

Erasable and recreatable two-dimensional electron gas at the heterointerface of SrTiO 3 and a water-dissolvable overlayer journal, August 2019

Extreme tensile strain states in La 0.7 Ca 0.3 MnO 3 membranes journal, April 2020

Super-elastic ferroelectric single-crystal membrane with continuous electric dipole rotation journal, October 2019

A general approach to obtain soft x-ray transparency for thin films grown on bulk substrates text, January 2017

A general approach to obtain soft x-ray transparency for thin films grown on bulk substrates text, January 2017

Nanoporous Films and Nanostructure Arrays Created by Selective Dissolution of Water-Soluble Materials. journalarticle, January 2018

A general approach to obtain soft x-ray transparency for thin films grown on bulk substrates journal, October 2017

Synergetic Behavior in 2D Layered Material/Complex Oxide Heterostructures text, January 2019

Stressor-Layer-Induced Elastic Strain Sharing in SrTiO3 Complex Oxide Sheets text, January 2020

Nanostructural Tailoring to Induce Flexibility in Thermoelectric Ca3Co4O9 Thin Films journal, July 2017

Heteroepitaxial vertical perovskite hot-electron transistors down to the monolayer limit journal, November 2019

Two-dimensional limit of crystalline order in perovskite membrane films journal, November 2017

Erasable and recreatable two-dimensional electron gas at the heterointerface of SrTiO 3 and a water-dissolvable overlayer journal, August 2019

Nanoporous Films and Nanostructure Arrays Created by Selective Dissolution of Water-Soluble Materials. journalarticle, January 2018

Mechanisms of cement hydration
journal, December 2011

Chiral magnetic order at surfaces driven by inversion asymmetry
journal, May 2007

Damage-free separation of GaN thin films from sapphire substrates
journal, February 1998

High-quality and efficient transfer of large-area graphene films onto different substrates
journal, May 2013

Oxide Interfaces--An Opportunity for Electronics
journal, March 2010

Progress, Challenges, and Opportunities in Two-Dimensional Materials Beyond Graphene
journal, March 2013

Piezoelectric Nanogenerators Based on Zinc Oxide Nanowire Arrays
journal, April 2006

Hofstadter’s butterfly and the fractal quantum Hall effect in moiré superlattices
journal, May 2013

Experimental Observation of the Quantum Anomalous Hall Effect in a Magnetic Topological Insulator
journal, March 2013

Synthesis, assembly and applications of semiconductor nanomembranes
journal, September 2011

Van der Waals heterostructures
journal, July 2013

Electric Field Effect in Atomically Thin Carbon Films
journal, October 2004

Room-temperature fabrication of transparent flexible thin-film transistors using amorphous oxide semiconductors
journal, November 2004

Direct measurement of strain effects on magnetic and electrical properties of epitaxial SrRuO3 thin films
journal, February 1998

Review on microfabricated micro-solid oxide fuel cell membranes
journal, October 2009

Interface-Induced High-Temperature Superconductivity in Single Unit-Cell FeSe Films on SrTiO ₃
journal, March 2012

Electric field control of the LaAlO3/SrTiO3 interface ground state
journal, December 2008

Application of hydrogen ion beams to Silicon On Insulator material technology
journal, February 1996

Emergent phenomena at oxide interfaces
journal, January 2012

Influence of strain on the magnetization and magnetoelectric effect in ${La}_{0.7} A_{0.3} Mn O_{3} ∕ PMN − PT (001)$ $(A = Sr, Ca)$
journal, February 2007

Graphene-Like Two-Dimensional Materials
journal, January 2013

Tuning the Dimensionality of the Heavy Fermion Compound CeIn3
journal, February 2010

Interface Effect and Its Doping Dependence in La _{1- x} Sr _x MnO ₃ /SrTiO ₃ Superlattices
journal, November 2002

Large-scale pattern growth of graphene films for stretchable transparent electrodes
journal, January 2009

Extreme selectivity in the lift‐off of epitaxial GaAs films
journal, December 1987

Two-Dimensional Dielectric Nanosheets: Novel Nanoelectronics From Nanocrystal Building Blocks
journal, October 2011

Mechanical Properties of Thin Single‐Crystal Gold Films
journal, December 1960

Growth of Face-Centered-Cubic Metals on Sodium Chloride Substrates
journal, May 1966

Microscopic origins for stabilizing room-temperature ferromagnetism in ultrathin manganite layers
journal, June 2010

Tristrontium dialuminum hexaoxide: an intricate superstructure of perovskite
journal, November 1990

Single-Crystalline SrRuO ₃ Nanomembranes: A Platform for Flexible Oxide Electronics
journal, December 2015

Ultrathin compound semiconductor on insulator layers for high-performance nanoscale transistors
journal, November 2010

Ultrathin compound semiconductor on insulator layers for high performance nanoscale transistors
text, January 2011

Interface induced high temperature superconductivity in single unit-cell FeSe films on SrTiO3
text, January 2012

Experimental Observation of the Quantum Anomalous Hall Effect in a Magnetic Topological Insulator
text, January 2016

Electric Field Effect in Atomically Thin Carbon Films
text, January 2004

Bienenstock, Cooper, and Munro Learning Rules Realized in Second-Order Memristors with Tunable Forgetting Rate
journal, January 2019

Hydrogenation Dynamics of Electrically Controlled Metal–Insulator Transition in Proton‐Gated Transparent and Flexible WO ₃ Transistors
journal, June 2019

Synergetic Behavior in 2D Layered Material/Complex Oxide Heterostructures
journal, December 2018

Ferroelectric Domain Wall Motion in Freestanding Single‐Crystal Complex Oxide Thin Film
journal, December 2019

Conductive Oxide Interfaces for Field Effect Devices
journal, June 2019

Stimulating Oxide Heterostructures: A Review on Controlling SrTiO ₃ ‐Based Heterointerfaces with External Stimuli
journal, August 2019

Atomic Scale Understanding of the Epitaxy of Perovskite Oxides on Flexible Mica Substrate
journal, December 2019

Giant Uniaxial Strain Ferroelectric Domain Tuning in Freestanding PbTiO ₃ Films
journal, April 2020

Epitaxial Liftoff of Wafer‐Scale VO ₂ Nanomembranes for Flexible, Ultrasensitive Tactile Sensors
journal, April 2019

Nanoporous Films and Nanostructure Arrays Created by Selective Dissolution of Water-Soluble Materials
journal, September 2018

Liquid–Solid Interfacial Assemblies of Soft Materials for Functional Freestanding Layered Membrane–Based Devices toward Electrochemical Energy Systems
journal, April 2019

Rectifying Effect of the Sr ₃ Al ₂ O ₆ /Ga ₂ O ₃ Heterojunction
journal, September 2019

Strain Tuning in Complex Oxide Epitaxial Films Using an Ultrathin Strontium Aluminate Buffer Layer
journal, January 2018

Assembly and Self-Assembly of Nanomembrane Materials-From 2D to 3D
journal, January 2018

Freestanding crystalline oxide perovskites down to the monolayer limit
journal, June 2019

Heterogeneous integration of single-crystalline complex-oxide membranes
journal, February 2020

Epitaxial growth and layer-transfer techniques for heterogeneous integration of materials for electronic and photonic devices
journal, October 2019

Enhanced bending-tuned magnetic properties in epitaxial cobalt ferrite nanopillar arrays on flexible substrates
journal, January 2018

Fabrication of ultralong perovskite structure nanotubes
journal, January 2018

Recent progress on flexible inorganic single-crystalline functional oxide films for advanced electronics
journal, January 2019

Development of oxide heteroepitaxy for soft technology
journal, January 2018

A versatile patterning process based on easily soluble sacrificial bilayers
journal, August 2017

Stressor-layer-induced elastic strain sharing in SrTiO ₃ complex oxide sheets
journal, February 2018

Strain-induced resistance change in V ₂ O ₃ films on piezoelectric ceramic disks
journal, March 2019

Non-Ohmic conduction in exfoliated La _0.7 Ca _0.3 MnO ₃ thin films
journal, January 2020

Spark plasma sintering of bulk SrAl ₂ O ₄ -Sr ₃ Al ₂ O ₆ eutectic glass with wide-band optical window
journal, April 2018

Erasable and recreatable two-dimensional electron gas at the heterointerface of SrTiO ₃ and a water-dissolvable overlayer
journal, August 2019

Extreme tensile strain states in La _0.7 Ca _0.3 MnO ₃ membranes
journal, April 2020

Super-elastic ferroelectric single-crystal membrane with continuous electric dipole rotation
journal, October 2019

A general approach to obtain soft x-ray transparency for thin films grown on bulk substrates
text, January 2017

A general approach to obtain soft x-ray transparency for thin films grown on bulk substrates
text, January 2017

Nanoporous Films and Nanostructure Arrays Created by Selective Dissolution of Water-Soluble Materials.
journalarticle, January 2018

A general approach to obtain soft x-ray transparency for thin films grown on bulk substrates
journal, October 2017

Synergetic Behavior in 2D Layered Material/Complex Oxide Heterostructures
text, January 2019

Stressor-Layer-Induced Elastic Strain Sharing in SrTiO3 Complex Oxide Sheets
text, January 2020

Nanostructural Tailoring to Induce Flexibility in Thermoelectric Ca₃Co₄O₉ Thin Films
journal, July 2017

Heteroepitaxial vertical perovskite hot-electron transistors down to the monolayer limit
journal, November 2019

Two-dimensional limit of crystalline order in perovskite membrane films
journal, November 2017

Erasable and recreatable two-dimensional electron gas at the heterointerface of SrTiO ₃ and a water-dissolvable overlayer
journal, August 2019

Nanoporous Films and Nanostructure Arrays Created by Selective Dissolution of Water-Soluble Materials.
journalarticle, January 2018