Phase Stability and Stoichiometry in Thin Film Iron Pyrite: Impact on Electronic Transport Properties
The use of pyrite FeS2 as an earth-abundant, low-cost, nontoxic thin film photovoltaic hinges on improved understanding and control of certain physical and chemical properties. Phase stability, phase purity, stoichiometry, and defects, are central in this respect, as they are frequently implicated i...
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| Published in | ACS applied materials & interfaces Vol. 7; no. 25; pp. 14130 - 14139 |
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| Main Authors | , , , , , , , , , , |
| Format | Journal Article |
| Language | English |
| Published |
United States
American Chemical Society
01.07.2015
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| Subjects | |
| Online Access | Get full text |
| ISSN | 1944-8244 1944-8252 1944-8252 |
| DOI | 10.1021/acsami.5b03422 |
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| Abstract | The use of pyrite FeS2 as an earth-abundant, low-cost, nontoxic thin film photovoltaic hinges on improved understanding and control of certain physical and chemical properties. Phase stability, phase purity, stoichiometry, and defects, are central in this respect, as they are frequently implicated in poor solar cell performance. Here, phase-pure polycrystalline pyrite FeS2 films, synthesized by ex situ sulfidation, are subject to systematic reduction by vacuum annealing (to 550 °C) to assess phase stability, stoichiometry evolution, and their impact on transport. Bulk probes reveal the onset of pyrrhotite (Fe1−δS) around 400 °C, rapidly evolving into the majority phase by 425 °C. This is supported by X-ray photoelectron spectroscopy on (001) crystals, revealing surface Fe1−δS formation as low as 160 °C, with rapid growth near 400 °C. The impact on transport is dramatic, with Fe1−δS minority phases leading to a crossover from diffusive transport to hopping (due to conductive Fe1−δS nanoregions in an FeS2 matrix), followed by metallicity when Fe1−δS dominates. Notably, the crossover to hopping leads to an inversion of the sign, and a large decrease in magnitude of the Hall coefficient. By tracking resistivity, magnetotransport, magnetization, and structural/chemical parameters vs annealing, we provide a detailed picture of the evolution in properties with stoichiometry. A strong propensity for S-deficient minority phase formation is found, with no wide window where S vacancies control the FeS2 carrier density. These findings have important implications for FeS2 solar cell development, emphasizing the need for (a) nanoscale chemical homogeneity, and (b) caution in interpreting carrier types and densities. |
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| AbstractList | The use of pyrite FeS2 as an earth-abundant, low-cost, nontoxic thin film photovoltaic hinges on improved understanding and control of certain physical and chemical properties. Phase stability, phase purity, stoichiometry, and defects, are central in this respect, as they are frequently implicated in poor solar cell performance. Here, phase-pure polycrystalline pyrite FeS2 films, synthesized by ex situ sulfidation, are subject to systematic reduction by vacuum annealing (to 550 °C) to assess phase stability, stoichiometry evolution, and their impact on transport. Bulk probes reveal the onset of pyrrhotite (Fe1−δS) around 400 °C, rapidly evolving into the majority phase by 425 °C. This is supported by X-ray photoelectron spectroscopy on (001) crystals, revealing surface Fe1−δS formation as low as 160 °C, with rapid growth near 400 °C. The impact on transport is dramatic, with Fe1−δS minority phases leading to a crossover from diffusive transport to hopping (due to conductive Fe1−δS nanoregions in an FeS2 matrix), followed by metallicity when Fe1−δS dominates. Notably, the crossover to hopping leads to an inversion of the sign, and a large decrease in magnitude of the Hall coefficient. By tracking resistivity, magnetotransport, magnetization, and structural/chemical parameters vs annealing, we provide a detailed picture of the evolution in properties with stoichiometry. A strong propensity for S-deficient minority phase formation is found, with no wide window where S vacancies control the FeS2 carrier density. These findings have important implications for FeS2 solar cell development, emphasizing the need for (a) nanoscale chemical homogeneity, and (b) caution in interpreting carrier types and densities. The use of pyrite FeS2 as an earth-abundant, low-cost, nontoxic thin film photovoltaic hinges on improved understanding and control of certain physical and chemical properties. Phase stability, phase purity, stoichiometry, and defects, are central in this respect, as they are frequently implicated in poor solar cell performance. Here, phase-pure polycrystalline pyrite FeS2 films, synthesized by ex situ sulfidation, are subject to systematic reduction by vacuum annealing (to 550 °C) to assess phase stability, stoichiometry evolution, and their impact on transport. Bulk probes reveal the onset of pyrrhotite (Fe(1-δ)S) around 400 °C, rapidly evolving into the majority phase by 425 °C. This is supported by X-ray photoelectron spectroscopy on (001) crystals, revealing surface Fe(1-δ)S formation as low as 160 °C, with rapid growth near 400 °C. The impact on transport is dramatic, with Fe(1-δ)S minority phases leading to a crossover from diffusive transport to hopping (due to conductive Fe(1-δ)S nanoregions in an FeS2 matrix), followed by metallicity when Fe(1-δ)S dominates. Notably, the crossover to hopping leads to an inversion of the sign, and a large decrease in magnitude of the Hall coefficient. By tracking resistivity, magnetotransport, magnetization, and structural/chemical parameters vs annealing, we provide a detailed picture of the evolution in properties with stoichiometry. A strong propensity for S-deficient minority phase formation is found, with no wide window where S vacancies control the FeS2 carrier density. These findings have important implications for FeS2 solar cell development, emphasizing the need for (a) nanoscale chemical homogeneity, and (b) caution in interpreting carrier types and densities. The use of pyrite FeS2 as an earth-abundant, low-cost, nontoxic thin film photovoltaic hinges on improved understanding and control of certain physical and chemical properties. Phase stability, phase purity, stoichiometry, and defects, are central in this respect, as they are frequently implicated in poor solar cell performance. Here, phase-pure polycrystalline pyrite FeS2 films, synthesized by ex situ sulfidation, are subject to systematic reduction by vacuum annealing (to 550 °C) to assess phase stability, stoichiometry evolution, and their impact on transport. Bulk probes reveal the onset of pyrrhotite (Fe(1-δ)S) around 400 °C, rapidly evolving into the majority phase by 425 °C. This is supported by X-ray photoelectron spectroscopy on (001) crystals, revealing surface Fe(1-δ)S formation as low as 160 °C, with rapid growth near 400 °C. The impact on transport is dramatic, with Fe(1-δ)S minority phases leading to a crossover from diffusive transport to hopping (due to conductive Fe(1-δ)S nanoregions in an FeS2 matrix), followed by metallicity when Fe(1-δ)S dominates. Notably, the crossover to hopping leads to an inversion of the sign, and a large decrease in magnitude of the Hall coefficient. By tracking resistivity, magnetotransport, magnetization, and structural/chemical parameters vs annealing, we provide a detailed picture of the evolution in properties with stoichiometry. A strong propensity for S-deficient minority phase formation is found, with no wide window where S vacancies control the FeS2 carrier density. These findings have important implications for FeS2 solar cell development, emphasizing the need for (a) nanoscale chemical homogeneity, and (b) caution in interpreting carrier types and densities.The use of pyrite FeS2 as an earth-abundant, low-cost, nontoxic thin film photovoltaic hinges on improved understanding and control of certain physical and chemical properties. Phase stability, phase purity, stoichiometry, and defects, are central in this respect, as they are frequently implicated in poor solar cell performance. Here, phase-pure polycrystalline pyrite FeS2 films, synthesized by ex situ sulfidation, are subject to systematic reduction by vacuum annealing (to 550 °C) to assess phase stability, stoichiometry evolution, and their impact on transport. Bulk probes reveal the onset of pyrrhotite (Fe(1-δ)S) around 400 °C, rapidly evolving into the majority phase by 425 °C. This is supported by X-ray photoelectron spectroscopy on (001) crystals, revealing surface Fe(1-δ)S formation as low as 160 °C, with rapid growth near 400 °C. The impact on transport is dramatic, with Fe(1-δ)S minority phases leading to a crossover from diffusive transport to hopping (due to conductive Fe(1-δ)S nanoregions in an FeS2 matrix), followed by metallicity when Fe(1-δ)S dominates. Notably, the crossover to hopping leads to an inversion of the sign, and a large decrease in magnitude of the Hall coefficient. By tracking resistivity, magnetotransport, magnetization, and structural/chemical parameters vs annealing, we provide a detailed picture of the evolution in properties with stoichiometry. A strong propensity for S-deficient minority phase formation is found, with no wide window where S vacancies control the FeS2 carrier density. These findings have important implications for FeS2 solar cell development, emphasizing the need for (a) nanoscale chemical homogeneity, and (b) caution in interpreting carrier types and densities. The use of pyrite FeS₂ as an earth-abundant, low-cost, nontoxic thin film photovoltaic hinges on improved understanding and control of certain physical and chemical properties. Phase stability, phase purity, stoichiometry, and defects, are central in this respect, as they are frequently implicated in poor solar cell performance. Here, phase-pure polycrystalline pyrite FeS₂ films, synthesized by ex situ sulfidation, are subject to systematic reduction by vacuum annealing (to 550 °C) to assess phase stability, stoichiometry evolution, and their impact on transport. Bulk probes reveal the onset of pyrrhotite (Fe₁₋δS) around 400 °C, rapidly evolving into the majority phase by 425 °C. This is supported by X-ray photoelectron spectroscopy on (001) crystals, revealing surface Fe₁₋δS formation as low as 160 °C, with rapid growth near 400 °C. The impact on transport is dramatic, with Fe₁₋δS minority phases leading to a crossover from diffusive transport to hopping (due to conductive Fe₁₋δS nanoregions in an FeS₂ matrix), followed by metallicity when Fe₁₋δS dominates. Notably, the crossover to hopping leads to an inversion of the sign, and a large decrease in magnitude of the Hall coefficient. By tracking resistivity, magnetotransport, magnetization, and structural/chemical parameters vs annealing, we provide a detailed picture of the evolution in properties with stoichiometry. A strong propensity for S-deficient minority phase formation is found, with no wide window where S vacancies control the FeS₂ carrier density. These findings have important implications for FeS₂ solar cell development, emphasizing the need for (a) nanoscale chemical homogeneity, and (b) caution in interpreting carrier types and densities. |
| Author | Zhang, Xin Yan, Yuqi Scott, Tom Aydil, Eray S Leighton, Chris Losovyj, Yaroslav Socha, Tyler Nielsen, David Manno, Michael Johnson, Melissa Dowben, Peter |
| AuthorAffiliation | Department of Chemistry University of Minnesota Department of Physics and Astronomy Indiana University Department of Chemical Engineering and Materials Science University of NebraskaLincoln |
| AuthorAffiliation_xml | – name: University of NebraskaLincoln – name: Department of Chemistry – name: Indiana University – name: Department of Physics and Astronomy – name: University of Minnesota – name: Department of Chemical Engineering and Materials Science |
| Author_xml | – sequence: 1 givenname: Xin surname: Zhang fullname: Zhang, Xin – sequence: 2 givenname: Tom surname: Scott fullname: Scott, Tom – sequence: 3 givenname: Tyler surname: Socha fullname: Socha, Tyler – sequence: 4 givenname: David surname: Nielsen fullname: Nielsen, David – sequence: 5 givenname: Michael surname: Manno fullname: Manno, Michael – sequence: 6 givenname: Melissa surname: Johnson fullname: Johnson, Melissa – sequence: 7 givenname: Yuqi surname: Yan fullname: Yan, Yuqi – sequence: 8 givenname: Yaroslav surname: Losovyj fullname: Losovyj, Yaroslav – sequence: 9 givenname: Peter surname: Dowben fullname: Dowben, Peter – sequence: 10 givenname: Eray S surname: Aydil fullname: Aydil, Eray S email: aydil@umn.edu – sequence: 11 givenname: Chris surname: Leighton fullname: Leighton, Chris email: leighton@umn.edu |
| BackLink | https://www.ncbi.nlm.nih.gov/pubmed/26087015$$D View this record in MEDLINE/PubMed |
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| Keywords | stoichiometry photovoltaic devices doping pyrite charge transport thin films phase stability |
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| Snippet | The use of pyrite FeS2 as an earth-abundant, low-cost, nontoxic thin film photovoltaic hinges on improved understanding and control of certain physical and... The use of pyrite FeS₂ as an earth-abundant, low-cost, nontoxic thin film photovoltaic hinges on improved understanding and control of certain physical and... |
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| SubjectTerms | annealing crystals photovoltaic cells physicochemical properties pyrite stoichiometry X-ray photoelectron spectroscopy |
| Title | Phase Stability and Stoichiometry in Thin Film Iron Pyrite: Impact on Electronic Transport Properties |
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