An in-situ phosphorus source for the synthesis of Cu3P and the subsequent conversion to Cu3PS4 nanoparticle clusters

Sheets, Erik J.; Stach, Eric A.; Yang, Wei -Chang; Balow, Robert B.; Wang, Yunjie; Walker, Bryce C.; Agrawal, Rakesh

doi:10.1557/jmr.2015.333

Title: An in-situ phosphorus source for the synthesis of Cu₃P and the subsequent conversion to Cu₃PS₄ nanoparticle clusters

Abstract

The search for alternative earth abundant semiconducting nanocrystals for sustainable energy applications has brought forth the need for nanoscale syntheses beyond bulk synthesis routes. Of particular interest are metal phosphides and derivative I-V-VI chalcogenides including copper phosphide (Cu₃P) and copper thiophosphate (Cu₃PS₄). Herein, we report a one-pot, solution-based synthesis of Cu₃P nanocrystals utilizing an in-situ phosphorus source: phosphorus pentasulfide (P₂S₅) in trioctylphosphine (TOP). By injecting this phosphorus source into a copper solution in oleylamine (OLA), uniform and size controlled Cu₃P nanocrystals with a phosphorous-rich surface are synthesized. The subsequent reaction of the Cu₃P nanocrystals with decomposing thiourea forms nanoscale Cu₃PS₄ particles having p-type conductivity and an effective optical band gap of 2.36 eV.

Authors:

Sheets, Erik J. ^[1]; Stach, Eric A. ^[2]; Yang, Wei -Chang ^[1]; Balow, Robert B. ^[1]; Wang, Yunjie ^[1]; Walker, Bryce C. ^[1]; Agrawal, Rakesh ^[1]

Purdue Univ., West Lafayette, IN (United States)
Brookhaven National Lab. (BNL), Upton, NY (United States)

Publication Date:: Sun Sep 20 00:00:00 EDT 2015

Research Org.:: Brookhaven National Laboratory (BNL), Upton, NY (United States)

Sponsoring Org.:: USDOE Office of Science (SC), Basic Energy Sciences (BES)

OSTI Identifier:: 1225436

Report Number(s):: BNL-108511-2015-JA
Journal ID: ISSN 0884-2914; KC0403020

Grant/Contract Number:: SC00112704

Resource Type:: Accepted Manuscript

Journal Name:: Journal of Materials Research

Additional Journal Information:: Journal Name: Journal of Materials Research; Journal ID: ISSN 0884-2914

Publisher:: Materials Research Society

Country of Publication:: United States

Language:: English

Subject:: 14 SOLAR ENERGY; nanoparticles; Cu₃P; copper phosphate; solar conversion; Center for Functional Nanomaterials

Citation Formats


                    Sheets, Erik J., Stach, Eric A., Yang, Wei -Chang, Balow, Robert B., Wang, Yunjie, Walker, Bryce C., and Agrawal, Rakesh. An in-situ phosphorus source for the synthesis of Cu3P and the subsequent conversion to Cu3PS4 nanoparticle clusters.  United States: N. p., 2015. 
Web.  doi:10.1557/jmr.2015.333.

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                    Sheets, Erik J., Stach, Eric A., Yang, Wei -Chang, Balow, Robert B., Wang, Yunjie, Walker, Bryce C., & Agrawal, Rakesh. An in-situ phosphorus source for the synthesis of Cu3P and the subsequent conversion to Cu3PS4 nanoparticle clusters.  United States.  https://doi.org/10.1557/jmr.2015.333

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                    Sheets, Erik J., Stach, Eric A., Yang, Wei -Chang, Balow, Robert B., Wang, Yunjie, Walker, Bryce C., and Agrawal, Rakesh. Sun .  
"An in-situ phosphorus source for the synthesis of Cu3P and the subsequent conversion to Cu3PS4 nanoparticle clusters".  United States.  https://doi.org/10.1557/jmr.2015.333.  https://www.osti.gov/servlets/purl/1225436.

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@article{osti_1225436,

  title        = {An in-situ phosphorus source for the synthesis of Cu3P and the subsequent conversion to Cu3PS4 nanoparticle clusters},

  author       = {Sheets, Erik J. and Stach, Eric A. and Yang, Wei -Chang and Balow, Robert B. and Wang, Yunjie and Walker, Bryce C. and Agrawal, Rakesh},

  abstractNote = {The search for alternative earth abundant semiconducting nanocrystals for sustainable energy applications has brought forth the need for nanoscale syntheses beyond bulk synthesis routes. Of particular interest are metal phosphides and derivative I-V-VI chalcogenides including copper phosphide (Cu3P) and copper thiophosphate (Cu3PS4). Herein, we report a one-pot, solution-based synthesis of Cu3P nanocrystals utilizing an in-situ phosphorus source: phosphorus pentasulfide (P2S5) in trioctylphosphine (TOP). By injecting this phosphorus source into a copper solution in oleylamine (OLA), uniform and size controlled Cu3P nanocrystals with a phosphorous-rich surface are synthesized. The subsequent reaction of the Cu3P nanocrystals with decomposing thiourea forms nanoscale Cu3PS4 particles having p-type conductivity and an effective optical band gap of 2.36 eV.},

  doi          = {10.1557/jmr.2015.333},

  journal      = {Journal of Materials Research},

  number       = ,

  volume       = ,

  place        = {United States},

  year         = {Sun Sep 20 00:00:00 EDT 2015},

  month        = {Sun Sep 20 00:00:00 EDT 2015}

}

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Works referencing / citing this record:

A Directed Route to Colloidal Nanoparticle Synthesis of the Copper Selenophosphate Cu ₃ PSe ₄
journal, February 2020

Lee, Jennifer M.; Kraynak, Leslie A.; Prieto, Amy L.
Angewandte Chemie International Edition, Vol. 59, Issue 8
DOI: 10.1002/anie.201911385

Pure phase synthesis of Cu ₃ PS ₄ and Cu ₆ PS ₅ Cl for semiconductor applications
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Graeser, Brian; Agrawal, Rakesh
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A Directed Route to Colloidal Nanoparticle Synthesis of the Copper Selenophosphate Cu ₃ PSe ₄
journal, January 2020

Lee, Jennifer M.; Kraynak, Leslie A.; Prieto, Amy L.
Angewandte Chemie, Vol. 132, Issue 8
DOI: 10.1002/ange.201911385

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Title: An in-situ phosphorus source for the synthesis of Cu3P and the subsequent conversion to Cu3PS4 nanoparticle clusters

Abstract

Citation Formats

The good reactivity of lithium with nanostructured copper phosphide journal, January 2008

A Mild One-Step Solvothermal Route to Metal Phosphides (Metal=Co, Ni, Cu) journal, January 2000

Converting Metals into Phosphides A General Strategy for the Synthesis of Metal Phosphide Nanocrystals journal, February 2007

Electronic and optical properties of potential solar absorber Cu3PSe4 text, January 2012

Solvothermal syntheses of Cu3P via reactions of amorphous red phosphorus with a variety of copper sources journal, April 2005

Kinetics of Thermal Decomposition of Thiourea journal, July 2004

Metal-Dependent Interplay between Crystallization and Phosphorus Diffusion during the Synthesis of Metal Phosphide Nanoparticles journal, October 2012

Size-Tunable, Hexagonal Plate-like Cu 3 P and Janus-like Cu–Cu 3 P Nanocrystals journal, December 2011

Photoelectronic properties of Cu3PS4 and Cu3PS3Se single crystals journal, August 1983

Trioctylphosphine as Both Solvent and Stabilizer to Synthesize CdS Nanorods journal, June 2009

Cu 3 P Binary Phosphide: Synthesis via a Wet Mechanochemical Method and Electrochemical Behavior as Negative Electrode Material for Lithium-Ion Batteries journal, September 2012

Synthesis and Characterization of Copper Arsenic Sulfide Nanocrystals from Earth Abundant Elements for Solar Energy Conversion journal, March 2015

Converting Metals into Phosphides: A General Strategy for the Synthesis of Metal Phosphide Nanocrystals. journal, May 2007

Facile synthesis of SERS active Ag nanoparticles in the presence of tri-n-octylphosphine sulfide journal, March 2011

Synthesis, characterization and electrochemical properties of copper phosphide (Cu3P) thick films prepared by solid-state reaction at low temperature: a probable anode for lithium ion batteries journal, August 2005

Trioctylphosphine A General Phosphorus Source for the Low-Temperature Conversion of Metals into Metal Phosphides journal, August 2007

Inverse Design of High Absorption Thin-Film Photovoltaic Materials journal, August 2012

Synthesis of InP nanofibers from tri(m-tolyl)phosphine: an alternative route to metal phosphidenanostructures journal, January 2010

Photoluminescence Analysis of Thin-Film Solar Cells book, January 2016

Crystal growth of metal-phosphorus-sulfur compounds by vapor transport journal, June 1970

Generalized Synthesis of Metal Phosphide Nanorods via Thermal Decomposition of Continuously Delivered Metal−Phosphine Complexes Using a Syringe Pump journal, June 2005

The Crystal Structure of Cu3P. journal, January 1972

Ternary chalcogenide systems X: The quasiternary system Ag2S-Cu2S-P4S10 journal, June 1991

Trioctylphosphine: A General Phosphorus Source for the Low-Temperature Conversion of Metals into Metal Phosphides. journal, October 2007

Recent developments in synthetic approaches to transition metal phosphide nanoparticles for magnetic and catalytic applications journal, July 2008

Elucidating the Surface Chemistry of Zinc Phosphide Nanoparticles Through Ligand Exchange journal, July 2014

Earth-abundant Cu-based chalcogenide semiconductors as photovoltaic absorbers journal, January 2013

Electronic and optical properties of potential solar absorber Cu 3 PSe 4 journal, October 2011

Metal sulphide-tetraphosphorusdekasulphide phase diagrams journal, December 1992

Transition metal phosphide hydroprocessing catalysts: A review journal, May 2009

Thermodynamic Analysis of Decomposition of Thiourea and Thiourea Oxides journal, September 2005

Cu 3- x P Nanocrystals as a Material Platform for Near-Infrared Plasmonics and Cation Exchange Reactions journal, January 2015

Refinement of the crystal structures of Cu3PS4 and Cu3SbS4 and a comment on normal tetrahedral structures journal, January 2002

A Directed Route to Colloidal Nanoparticle Synthesis of the Copper Selenophosphate Cu 3 PSe 4 journal, February 2020

Pure phase synthesis of Cu 3 PS 4 and Cu 6 PS 5 Cl for semiconductor applications journal, January 2018

A Directed Route to Colloidal Nanoparticle Synthesis of the Copper Selenophosphate Cu 3 PSe 4 journal, January 2020

Title: An in-situ phosphorus source for the synthesis of Cu₃P and the subsequent conversion to Cu₃PS₄ nanoparticle clusters

The good reactivity of lithium with nanostructured copper phosphide
journal, January 2008

A Mild One-Step Solvothermal Route to Metal Phosphides (Metal=Co, Ni, Cu)
journal, January 2000

Converting Metals into Phosphides A General Strategy for the Synthesis of Metal Phosphide Nanocrystals
journal, February 2007

Electronic and optical properties of potential solar absorber Cu3PSe4
text, January 2012

Solvothermal syntheses of Cu3P via reactions of amorphous red phosphorus with a variety of copper sources
journal, April 2005

Kinetics of Thermal Decomposition of Thiourea
journal, July 2004

Metal-Dependent Interplay between Crystallization and Phosphorus Diffusion during the Synthesis of Metal Phosphide Nanoparticles
journal, October 2012

Size-Tunable, Hexagonal Plate-like Cu ₃ P and Janus-like Cu–Cu ₃ P Nanocrystals
journal, December 2011

Photoelectronic properties of Cu3PS4 and Cu3PS3Se single crystals
journal, August 1983

Trioctylphosphine as Both Solvent and Stabilizer to Synthesize CdS Nanorods
journal, June 2009

Cu ₃ P Binary Phosphide: Synthesis via a Wet Mechanochemical Method and Electrochemical Behavior as Negative Electrode Material for Lithium-Ion Batteries
journal, September 2012

Synthesis and Characterization of Copper Arsenic Sulfide Nanocrystals from Earth Abundant Elements for Solar Energy Conversion
journal, March 2015

Converting Metals into Phosphides: A General Strategy for the Synthesis of Metal Phosphide Nanocrystals.
journal, May 2007

Facile synthesis of SERS active Ag nanoparticles in the presence of tri-n-octylphosphine sulfide
journal, March 2011

Synthesis, characterization and electrochemical properties of copper phosphide (Cu3P) thick films prepared by solid-state reaction at low temperature: a probable anode for lithium ion batteries
journal, August 2005

Trioctylphosphine A General Phosphorus Source for the Low-Temperature Conversion of Metals into Metal Phosphides
journal, August 2007

Inverse Design of High Absorption Thin-Film Photovoltaic Materials
journal, August 2012

Synthesis of InP nanofibers from tri(m-tolyl)phosphine: an alternative route to metal phosphidenanostructures
journal, January 2010

Photoluminescence Analysis of Thin-Film Solar Cells
book, January 2016

Crystal growth of metal-phosphorus-sulfur compounds by vapor transport
journal, June 1970

Generalized Synthesis of Metal Phosphide Nanorods via Thermal Decomposition of Continuously Delivered Metal−Phosphine Complexes Using a Syringe Pump
journal, June 2005

The Crystal Structure of Cu3P.
journal, January 1972

Ternary chalcogenide systems X: The quasiternary system Ag2S-Cu2S-P4S10
journal, June 1991

Trioctylphosphine: A General Phosphorus Source for the Low-Temperature Conversion of Metals into Metal Phosphides.
journal, October 2007

Recent developments in synthetic approaches to transition metal phosphide nanoparticles for magnetic and catalytic applications
journal, July 2008

Elucidating the Surface Chemistry of Zinc Phosphide Nanoparticles Through Ligand Exchange
journal, July 2014

Earth-abundant Cu-based chalcogenide semiconductors as photovoltaic absorbers
journal, January 2013

Electronic and optical properties of potential solar absorber Cu ₃ PSe ₄
journal, October 2011

Metal sulphide-tetraphosphorusdekasulphide phase diagrams
journal, December 1992

Transition metal phosphide hydroprocessing catalysts: A review
journal, May 2009

Thermodynamic Analysis of Decomposition of Thiourea and Thiourea Oxides
journal, September 2005

Cu _{3- x} P Nanocrystals as a Material Platform for Near-Infrared Plasmonics and Cation Exchange Reactions
journal, January 2015

Refinement of the crystal structures of Cu3PS4 and Cu3SbS4 and a comment on normal tetrahedral structures
journal, January 2002

A Directed Route to Colloidal Nanoparticle Synthesis of the Copper Selenophosphate Cu ₃ PSe ₄
journal, February 2020

Pure phase synthesis of Cu ₃ PS ₄ and Cu ₆ PS ₅ Cl for semiconductor applications
journal, January 2018

A Directed Route to Colloidal Nanoparticle Synthesis of the Copper Selenophosphate Cu ₃ PSe ₄
journal, January 2020