Methods for producing single crystal mixed halide perovskites

Zhu, Kai; Zhao, Yixin

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Title: Methods for producing single crystal mixed halide perovskites

Abstract

An aspect of the present invention is a method that includes contacting a metal halide and a first alkylammonium halide in a solvent to form a solution and maintaining the solution at a first temperature, resulting in the formation of at least one alkylammonium halide perovskite crystal, where the metal halide includes a first halogen and a metal, the first alkylammonium halide includes the first halogen, the at least one alkylammonium halide perovskite crystal includes the metal and the first halogen, and the first temperature is above about 21.degree. C.

Inventors:: Zhu, Kai; Zhao, Yixin

Issue Date:: 2017-07-11

Research Org.:: National Renewable Energy Laboratory (NREL), Golden, CO (United States)

Sponsoring Org.:: USDOE

OSTI Identifier:: 1369227

Patent Number(s):: 9701696

Application Number:: 15/055,712

Assignee:: Alliance for Sustainable Energy, LLC

Patent Classifications (CPCs):: C - CHEMISTRY C07 - ORGANIC CHEMISTRY C07F - ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM

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C - CHEMISTRY C07 - ORGANIC CHEMISTRY C07F - ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
C07F7/24 - Lead compounds

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DOE Contract Number:: AC36-08G028308

Resource Type:: Patent

Resource Relation:: Patent File Date: 2016 Feb 29

Country of Publication:: United States

Language:: English

Subject:: 37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY

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                    Zhu, Kai, and Zhao, Yixin. Methods for producing single crystal mixed halide perovskites.  United States: N. p., 2017. 
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                    Zhu, Kai, & Zhao, Yixin. Methods for producing single crystal mixed halide perovskites.  United States.

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                    Zhu, Kai, and Zhao, Yixin. Tue .  
        "Methods for producing single crystal mixed halide perovskites".  United States.  https://www.osti.gov/servlets/purl/1369227.

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@article{osti_1369227,

  title        = {Methods for producing single crystal mixed halide perovskites},

  author       = {Zhu, Kai and Zhao, Yixin},

  abstractNote = {An aspect of the present invention is a method that includes contacting a metal halide and a first alkylammonium halide in a solvent to form a solution and maintaining the solution at a first temperature, resulting in the formation of at least one alkylammonium halide perovskite crystal, where the metal halide includes a first halogen and a metal, the first alkylammonium halide includes the first halogen, the at least one alkylammonium halide perovskite crystal includes the metal and the first halogen, and the first temperature is above about 21.degree. C.},

  doi          = {},

  journal      = {},
number       = ,

  volume       = ,

  place        = {United States},

  year         = {2017},

  month        = {7}

}

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Long-Range Balanced Electron- and Hole-Transport Lengths in Organic-Inorganic CH₃NH₃PbI₃
journal, October 2013

Xing, G.; Mathews, N.; Sun, S.
Science, Vol. 342, Issue 6156, p. 344-347
https://doi.org/10.1126/science.1243167

Nanocrystalline Rutile Electron Extraction Layer Enables Low-Temperature Solution Processed Perovskite Photovoltaics with 13.7% Efficiency
journal, April 2014

Yella, Aswani; Heiniger, Leo-Philipp; Gao, Peng
Nano Letters, Vol. 14, Issue 5, p. 2591-2596
https://doi.org/10.1021/nl500399m

A facile solvothermal growth of single crystal mixed halide perovskite CH₃NH₃Pb(Br_1−xCl_x)₃
journal, January 2015

Zhang, Taiyang; Yang, Mengjin; Benson, Eric E.
Chemical Communications, Vol. 51, Issue 37, p. 7820-7823
https://doi.org/10.1039/C5CC01835H

Influence of Surface Area on Charge Transport and Recombination in Dye-Sensitized TiO₂ Solar Cells
November 2006

Zhu, Kai; Kopidakis, Nikos; Neale, Nathan R.
https://doi.org/10.1021/jp065284+

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Title: Methods for producing single crystal mixed halide perovskites

Abstract

Citation Formats

Two-step dipping technique for the preparation of organic-inorganic perovskite thin films patent, February 1999

Process for forming epitaxial perovskite thin film layers using halide precursors patent, May 2001

Layered organic-inorganic perovskites having metal-deficient inorganic frameworks patent, August 2002

Tandem photovoltaic cell patent, October 2013

Perovskite complex oxide and method of producing the same patent-application, September 2004

Organic Semiconductor Device patent-application, December 2010

Redox Material For Thermochemical Water Splitting, And Method For Producing Hydrogen patent-application, December 2011

Heterojunction Device patent-application, August 2012

Active Materials For Electro-Optic Devices And Electro-Optic Devices patent-application, January 2014

Light Absorbing Oxide Materials for Photovoltaic and Photocatalytic Applications and Devices patent-application, March 2014

Hybrid Organic Solar Cell With Perovskite Structure As Absorption Material And Manufacturing Method Thereof patent-application, November 2014

Optoelectronic Device Comprising Perovskites patent-application, May 2015

Optoelectronic Devices With Organometal Perovskites With Mixed Anions patent-application, May 2015

Optoelectronic Device patent-application, September 2015

Mechanism of Charge Recombination in Dye-Sensitized Nanocrystalline Semiconductors: Random Flight Model April 2002

Silicon heterojunction solar cell with passivated hole selective MoO x contact journal, March 2014

Effect of Different Hole Transport Materials on Recombination in CH3NH3PbI3 Perovskite-Sensitized Mesoscopic Solar Cells journal, April 2013

Interpretation of the Time Constants Measured by Kinetic Techniques in Nanostructured Semiconductor Electrodes and Dye-Sensitized Solar Cells journal, February 2004

Sequential deposition as a route to high-performance perovskite-sensitized solar cells journal, July 2013

Planar Heterojunction Perovskite Solar Cells via Vapor-Assisted Solution Process journal, December 2013

High voltage and efficient bilayer heterojunction solar cells based on an organic–inorganic hybrid perovskite absorber with a low-cost flexible substrate journal, January 2014

Structure of Methylammonium Lead Iodide Within Mesoporous Titanium Dioxide: Active Material in High-Performance Perovskite Solar Cells journal, December 2013

An Inorganic Hole Conductor for Organo-Lead Halide Perovskite Solar Cells. Improved Hole Conductivity with Copper Iodide journal, December 2013

All-solid-state dye-sensitized solar cells with high efficiency journal, May 2012

MAPbI3-xClx Mixed Halide Perovskite for Hybrid Solar Cells: The Role of Chloride as Dopant on the Transport and Structural Properties journal, November 2013

Perovskite-Based Hybrid Solar Cells Exceeding 10% Efficiency with High Reproducibility Using a Thin Film Sandwich Approach journal, December 2013

Enhanced Extraction Rates through Gap States of Molybdenum Oxide Anode Buffer journal, April 2013

Dynamic Response of Dye-Sensitized Nanocrystalline Solar Cells: Characterization by Intensity-Modulated Photocurrent Spectroscopy journal, December 1997

Efficient organometal trihalide perovskite planar-heterojunction solar cells on flexible polymer substrates journal, November 2013

Solution Deposition-Conversion for Planar Heterojunction Mixed Halide Perovskite Solar Cells journal, May 2014

Effect of Annealing Temperature on Film Morphology of Organic-Inorganic Hybrid Pervoskite Solid-State Solar Cells journal, February 2014

Impedance Spectroscopic Analysis of Lead Iodide Perovskite-Sensitized Solid-State Solar Cells journal, December 2013

High Open-Circuit Voltage Solar Cells Based on Organic–Inorganic Lead Bromide Perovskite journal, March 2013

Chloride Inclusion and Hole Transport Material Doping to Improve Methyl Ammonium Lead Bromide Perovskite-Based High Open-Circuit Voltage Solar Cells journal, January 2014

Morphological Control for High Performance, Solution-Processed Planar Heterojunction Perovskite Solar Cells journal, September 2013

n-Type Transition Metal Oxide as a Hole Extraction Layer in PbS Quantum Dot Solar Cells journal, August 2011

The emergence of perovskite solar cells journal, July 2014

Development of MoOx thin films as back contact buffer for CdTe solar cells in substrate configuration journal, May 2013

Efficient inorganic–organic hybrid heterojunction solar cells containing perovskite compound and polymeric hole conductors journal, May 2013

Efficient Inorganic–Organic Hybrid Perovskite Solar Cells Based on Pyrene Arylamine Derivatives as Hole-Transporting Materials journal, December 2013

High Open-Circuit Voltage Solid-State Dye-Sensitized Solar Cells with Organic Dye journal, June 2009

Solvent engineering for high-performance inorganic–organic hybrid perovskite solar cells journal, July 2014

Role of the Selective Contacts in the Performance of Lead Halide Perovskite Solar Cells journal, January 2014

Organic-Inorganic Hybrid Materials as Semiconducting Channels in Thin-Film Field-Effect Transistors journal, October 1999

High Efficiency Solid-State Sensitized Solar Cell-Based on Submicrometer Rutile TiO2 Nanorod and CH3NH3PbI3 Perovskite Sensitizer journal, May 2013

Organolead Halide Perovskite: New Horizons in Solar Cell Research journal, February 2014

Organometal Halide Perovskites as Visible-Light Sensitizers for Photovoltaic Cells journal, May 2009

Efficient Hybrid Solar Cells Based on Meso-Superstructured Organometal Halide Perovskites journal, October 2012

Synthesis and Characterization of Organic−Inorganic Perovskite Thin Films Prepared Using a Versatile Two-Step Dipping Technique journal, January 1998

Additive Enhanced Crystallization of Solution-Processed Perovskite for Highly Efficient Planar-Heterojunction Solar Cells journal, March 2014

Efficient planar heterojunction perovskite solar cells by vapour deposition journal, September 2013

Perovskite solar cells with a planar heterojunction structure prepared using room-temperature solution processing techniques journal, December 2013

Trap-limited recombination in dye-sensitized nanocrystalline metal oxide electrodes journal, May 2001

Liquid Exfoliation of Layered Materials journal, June 2013

Chemical Management for Colorful, Efficient, and Stable Inorganic–Organic Hybrid Nanostructured Solar Cells journal, March 2013

Organometal Perovskite Light Absorbers Toward a 20% Efficiency Low-Cost Solid-State Mesoscopic Solar Cell journal, July 2013

Enhanced Crystallinity in Organic–Inorganic Lead Halide Perovskites on Mesoporous TiO2 via Disorder–Order Phase Transition journal, July 2014

Mixed-Organic-Cation Perovskite Photovoltaics for Enhanced Solar-Light Harvesting journal, February 2014

High-quality bulk hybrid perovskite single crystals within minutes by inverse temperature crystallization journal, July 2015

Perovskites by Design: A Toolbox of Solid-State Reactions journal, April 2002

Perovskite Solar Cells Keep On Surging journal, May 2014

Hole-conductor-free perovskite organic lead iodide heterojunction thin-film solar cells: High efficiency and junction property journal, February 2014

Perovskites: The Emergence of a New Era for Low-Cost, High-Efficiency Solar Cells journal, October 2013

Electron-Hole Diffusion Lengths Exceeding 1 Micrometer in an Organometal Trihalide Perovskite Absorber journal, October 2013

High performance organic light emitting diodes using substoichiometric tungsten oxide as efficient hole injection layer journal, May 2012

Low-Temperature Processed Electron Collection Layers of Graphene/TiO2 Nanocomposites in Thin Film Perovskite Solar Cells journal, December 2013

Retarding the crystallization of PbI 2 for highly reproducible planar-structured perovskite solar cells via sequential deposition journal, January 2014

Long-Range Balanced Electron- and Hole-Transport Lengths in Organic-Inorganic CH3NH3PbI3 journal, October 2013

Nanocrystalline Rutile Electron Extraction Layer Enables Low-Temperature Solution Processed Perovskite Photovoltaics with 13.7% Efficiency journal, April 2014

A facile solvothermal growth of single crystal mixed halide perovskite CH3NH3Pb(Br1−xClx)3 journal, January 2015

Influence of Surface Area on Charge Transport and Recombination in Dye-Sensitized TiO2 Solar Cells November 2006

Two-step dipping technique for the preparation of organic-inorganic perovskite thin films
patent, February 1999

Process for forming epitaxial perovskite thin film layers using halide precursors
patent, May 2001

Layered organic-inorganic perovskites having metal-deficient inorganic frameworks
patent, August 2002

Tandem photovoltaic cell
patent, October 2013

Perovskite complex oxide and method of producing the same
patent-application, September 2004

Organic Semiconductor Device
patent-application, December 2010

Redox Material For Thermochemical Water Splitting, And Method For Producing Hydrogen
patent-application, December 2011

Heterojunction Device
patent-application, August 2012

Active Materials For Electro-Optic Devices And Electro-Optic Devices
patent-application, January 2014

Light Absorbing Oxide Materials for Photovoltaic and Photocatalytic Applications and Devices
patent-application, March 2014

Hybrid Organic Solar Cell With Perovskite Structure As Absorption Material And Manufacturing Method Thereof
patent-application, November 2014

Optoelectronic Device Comprising Perovskites
patent-application, May 2015

Optoelectronic Devices With Organometal Perovskites With Mixed Anions
patent-application, May 2015

Optoelectronic Device
patent-application, September 2015

Mechanism of Charge Recombination in Dye-Sensitized Nanocrystalline Semiconductors: Random Flight Model
April 2002

Silicon heterojunction solar cell with passivated hole selective MoO _x contact
journal, March 2014

Effect of Different Hole Transport Materials on Recombination in CH₃NH₃PbI₃ Perovskite-Sensitized Mesoscopic Solar Cells
journal, April 2013

Interpretation of the Time Constants Measured by Kinetic Techniques in Nanostructured Semiconductor Electrodes and Dye-Sensitized Solar Cells
journal, February 2004

Sequential deposition as a route to high-performance perovskite-sensitized solar cells
journal, July 2013

Planar Heterojunction Perovskite Solar Cells via Vapor-Assisted Solution Process
journal, December 2013

High voltage and efficient bilayer heterojunction solar cells based on an organic–inorganic hybrid perovskite absorber with a low-cost flexible substrate
journal, January 2014

Structure of Methylammonium Lead Iodide Within Mesoporous Titanium Dioxide: Active Material in High-Performance Perovskite Solar Cells
journal, December 2013

An Inorganic Hole Conductor for Organo-Lead Halide Perovskite Solar Cells. Improved Hole Conductivity with Copper Iodide
journal, December 2013

All-solid-state dye-sensitized solar cells with high efficiency
journal, May 2012

MAPbI_3-xCl_x Mixed Halide Perovskite for Hybrid Solar Cells: The Role of Chloride as Dopant on the Transport and Structural Properties
journal, November 2013

Perovskite-Based Hybrid Solar Cells Exceeding 10% Efficiency with High Reproducibility Using a Thin Film Sandwich Approach
journal, December 2013

Enhanced Extraction Rates through Gap States of Molybdenum Oxide Anode Buffer
journal, April 2013

Dynamic Response of Dye-Sensitized Nanocrystalline Solar Cells: Characterization by Intensity-Modulated Photocurrent Spectroscopy
journal, December 1997

Efficient organometal trihalide perovskite planar-heterojunction solar cells on flexible polymer substrates
journal, November 2013

Solution Deposition-Conversion for Planar Heterojunction Mixed Halide Perovskite Solar Cells
journal, May 2014

Effect of Annealing Temperature on Film Morphology of Organic-Inorganic Hybrid Pervoskite Solid-State Solar Cells
journal, February 2014

Impedance Spectroscopic Analysis of Lead Iodide Perovskite-Sensitized Solid-State Solar Cells
journal, December 2013

High Open-Circuit Voltage Solar Cells Based on Organic–Inorganic Lead Bromide Perovskite
journal, March 2013

Chloride Inclusion and Hole Transport Material Doping to Improve Methyl Ammonium Lead Bromide Perovskite-Based High Open-Circuit Voltage Solar Cells
journal, January 2014

Morphological Control for High Performance, Solution-Processed Planar Heterojunction Perovskite Solar Cells
journal, September 2013

n-Type Transition Metal Oxide as a Hole Extraction Layer in PbS Quantum Dot Solar Cells
journal, August 2011

The emergence of perovskite solar cells
journal, July 2014

Development of MoOx thin films as back contact buffer for CdTe solar cells in substrate configuration
journal, May 2013

Efficient inorganic–organic hybrid heterojunction solar cells containing perovskite compound and polymeric hole conductors
journal, May 2013

Efficient Inorganic–Organic Hybrid Perovskite Solar Cells Based on Pyrene Arylamine Derivatives as Hole-Transporting Materials
journal, December 2013

High Open-Circuit Voltage Solid-State Dye-Sensitized Solar Cells with Organic Dye
journal, June 2009

Solvent engineering for high-performance inorganic–organic hybrid perovskite solar cells
journal, July 2014

Role of the Selective Contacts in the Performance of Lead Halide Perovskite Solar Cells
journal, January 2014

Organic-Inorganic Hybrid Materials as Semiconducting Channels in Thin-Film Field-Effect Transistors
journal, October 1999

High Efficiency Solid-State Sensitized Solar Cell-Based on Submicrometer Rutile TiO₂ Nanorod and CH₃NH₃PbI₃ Perovskite Sensitizer
journal, May 2013

Organolead Halide Perovskite: New Horizons in Solar Cell Research
journal, February 2014

Organometal Halide Perovskites as Visible-Light Sensitizers for Photovoltaic Cells
journal, May 2009

Efficient Hybrid Solar Cells Based on Meso-Superstructured Organometal Halide Perovskites
journal, October 2012

Synthesis and Characterization of Organic−Inorganic Perovskite Thin Films Prepared Using a Versatile Two-Step Dipping Technique
journal, January 1998

Additive Enhanced Crystallization of Solution-Processed Perovskite for Highly Efficient Planar-Heterojunction Solar Cells
journal, March 2014

Efficient planar heterojunction perovskite solar cells by vapour deposition
journal, September 2013

Perovskite solar cells with a planar heterojunction structure prepared using room-temperature solution processing techniques
journal, December 2013

Trap-limited recombination in dye-sensitized nanocrystalline metal oxide electrodes
journal, May 2001

Liquid Exfoliation of Layered Materials
journal, June 2013

Chemical Management for Colorful, Efficient, and Stable Inorganic–Organic Hybrid Nanostructured Solar Cells
journal, March 2013

Organometal Perovskite Light Absorbers Toward a 20% Efficiency Low-Cost Solid-State Mesoscopic Solar Cell
journal, July 2013

Enhanced Crystallinity in Organic–Inorganic Lead Halide Perovskites on Mesoporous TiO₂ via Disorder–Order Phase Transition
journal, July 2014

Mixed-Organic-Cation Perovskite Photovoltaics for Enhanced Solar-Light Harvesting
journal, February 2014

High-quality bulk hybrid perovskite single crystals within minutes by inverse temperature crystallization
journal, July 2015

Perovskites by Design: A Toolbox of Solid-State Reactions
journal, April 2002

Perovskite Solar Cells Keep On Surging
journal, May 2014

Hole-conductor-free perovskite organic lead iodide heterojunction thin-film solar cells: High efficiency and junction property
journal, February 2014

Perovskites: The Emergence of a New Era for Low-Cost, High-Efficiency Solar Cells
journal, October 2013

Electron-Hole Diffusion Lengths Exceeding 1 Micrometer in an Organometal Trihalide Perovskite Absorber
journal, October 2013

High performance organic light emitting diodes using substoichiometric tungsten oxide as efficient hole injection layer
journal, May 2012

Low-Temperature Processed Electron Collection Layers of Graphene/TiO₂ Nanocomposites in Thin Film Perovskite Solar Cells
journal, December 2013

Retarding the crystallization of PbI ₂ for highly reproducible planar-structured perovskite solar cells via sequential deposition
journal, January 2014

Long-Range Balanced Electron- and Hole-Transport Lengths in Organic-Inorganic CH₃NH₃PbI₃
journal, October 2013

Nanocrystalline Rutile Electron Extraction Layer Enables Low-Temperature Solution Processed Perovskite Photovoltaics with 13.7% Efficiency
journal, April 2014

A facile solvothermal growth of single crystal mixed halide perovskite CH₃NH₃Pb(Br_1−xCl_x)₃
journal, January 2015

Influence of Surface Area on Charge Transport and Recombination in Dye-Sensitized TiO₂ Solar Cells
November 2006