Rapid Solidification of Sn-Cu-Al Alloys for High-Reliability, Lead-Free Solder: Part I. Microstructural Characterization of Rapidly Solidified Solders

Reeve, Kathlene N.; Choquette, Stephanie M.; Anderson, Iver E.; Handwerker, Carol A.

doi:10.1007/s11661-016-3738-6

Title: Rapid Solidification of Sn-Cu-Al Alloys for High-Reliability, Lead-Free Solder: Part I. Microstructural Characterization of Rapidly Solidified Solders

Abstract

Particles of Cu _x Al _y in Sn-Cu-Al solders have previously been shown to nucleate the Cu₆Sn₅ phase during solidification. In this study, the number and size of Cu₆Sn₅ nucleation sites were controlled through the particle size refinement of Cu _x Al _y via rapid solidification processing and controlled cooling in a differential scanning calorimeter. Cooling rates spanning eight orders of magnitude were used to refine the average Cu _x Al _y and Cu₆Sn₅ particle sizes down to submicron ranges. The average particle sizes, particle size distributions, and morphologies in the microstructures were analyzed as a function of alloy composition and cooling rate. Deep etching of the samples revealed the three-dimensional microstructures and illuminated the epitaxial and morphological relationships between the Cu _x Al _y and Cu₆Sn₅ phases. Transitions in the Cu₆Sn₅ particle morphologies from faceted rods to nonfaceted, equiaxed particles were observed as a function of both cooling rate and composition. Initial solidification cooling rates within the range of 10³ to 10⁴ °C/s were found to be optimal for realizing particle size refinement and maintaining the Cu _x Al _y /Cu₆Sn₅ nucleant relationship. In addition, little evidence of the formation or decomposition of the ternary-β phase in the solidifiedmore »« less

Authors:

Reeve, Kathlene N. ^[1]; Choquette, Stephanie M. ^[2]; Anderson, Iver E. ^[2]; Handwerker, Carol A. ^[1]

Purdue Univ., West Lafayette, IN (United States)
Ames Lab. and Iowa State Univ., Ames, IA (United States)

Publication Date:: Thu Oct 06 00:00:00 EDT 2016

Research Org.:: Ames Laboratory (AMES), Ames, IA (United States)

Sponsoring Org.:: USDOE

OSTI Identifier:: 1417369

Report Number(s):: IS-J-9157
Journal ID: ISSN 1073-5623; PII: 3738; TRN: US1801048

Grant/Contract Number:: AC02-07CH11358

Resource Type:: Accepted Manuscript

Journal Name:: Metallurgical and Materials Transactions. A, Physical Metallurgy and Materials Science

Additional Journal Information:: Journal Volume: 47; Journal Issue: 12; Journal ID: ISSN 1073-5623

Publisher:: ASM International

Country of Publication:: United States

Language:: English

Subject:: 36 MATERIALS SCIENCE; intermetallics; rapid-solidification; quenching; microstructure; metallography; scanning electron microscopy; SEM

Citation Formats


                    Reeve, Kathlene N., Choquette, Stephanie M., Anderson, Iver E., and Handwerker, Carol A. Rapid Solidification of Sn-Cu-Al Alloys for High-Reliability, Lead-Free Solder: Part I. Microstructural Characterization of Rapidly Solidified Solders.  United States: N. p., 2016. 
Web.  doi:10.1007/s11661-016-3738-6.

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                    Reeve, Kathlene N., Choquette, Stephanie M., Anderson, Iver E., & Handwerker, Carol A. Rapid Solidification of Sn-Cu-Al Alloys for High-Reliability, Lead-Free Solder: Part I. Microstructural Characterization of Rapidly Solidified Solders.  United States.  https://doi.org/10.1007/s11661-016-3738-6

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                    Reeve, Kathlene N., Choquette, Stephanie M., Anderson, Iver E., and Handwerker, Carol A. Thu .  
"Rapid Solidification of Sn-Cu-Al Alloys for High-Reliability, Lead-Free Solder: Part I. Microstructural Characterization of Rapidly Solidified Solders".  United States.  https://doi.org/10.1007/s11661-016-3738-6.  https://www.osti.gov/servlets/purl/1417369.

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@article{osti_1417369,

  title        = {Rapid Solidification of Sn-Cu-Al Alloys for High-Reliability, Lead-Free Solder: Part I. Microstructural Characterization of Rapidly Solidified Solders},

  author       = {Reeve, Kathlene N. and Choquette, Stephanie M. and Anderson, Iver E. and Handwerker, Carol A.},

  abstractNote = {Particles of Cu x Al y in Sn-Cu-Al solders have previously been shown to nucleate the Cu6Sn5 phase during solidification. In this study, the number and size of Cu6Sn5 nucleation sites were controlled through the particle size refinement of Cu x Al y via rapid solidification processing and controlled cooling in a differential scanning calorimeter. Cooling rates spanning eight orders of magnitude were used to refine the average Cu x Al y and Cu6Sn5 particle sizes down to submicron ranges. The average particle sizes, particle size distributions, and morphologies in the microstructures were analyzed as a function of alloy composition and cooling rate. Deep etching of the samples revealed the three-dimensional microstructures and illuminated the epitaxial and morphological relationships between the Cu x Al y and Cu6Sn5 phases. Transitions in the Cu6Sn5 particle morphologies from faceted rods to nonfaceted, equiaxed particles were observed as a function of both cooling rate and composition. Initial solidification cooling rates within the range of 103 to 104 °C/s were found to be optimal for realizing particle size refinement and maintaining the Cu x Al y /Cu6Sn5 nucleant relationship. In addition, little evidence of the formation or decomposition of the ternary-β phase in the solidified alloys was noted. As a result, solidification pathways omitting the formation of the ternary-β phase agreed well with observed room temperature microstructures.},

  doi          = {10.1007/s11661-016-3738-6},

  journal      = {Metallurgical and Materials Transactions. A, Physical Metallurgy and Materials Science},

  number       = 12,

  volume       = 47,

  place        = {United States},

  year         = {Thu Oct 06 00:00:00 EDT 2016},

  month        = {Thu Oct 06 00:00:00 EDT 2016}

}

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Rapid Solidification of Sn-Cu-Al Alloys for High-Reliability, Lead-Free Solder: Part II. Intermetallic Coarsening Behavior of Rapidly Solidified Solders After Multiple Reflows
journal, October 2016

Reeve, Kathlene N.; Choquette, Stephanie M.; Anderson, Iver E.
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Works referencing / citing this record:

Beta-Tin Grain Formation in Aluminum-Modified Lead-Free Solder Alloys
journal, October 2017

Reeve, Kathlene N.; Handwerker, Carol A.
Journal of Electronic Materials, Vol. 47, Issue 1
DOI: 10.1007/s11664-017-5819-8

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Title: Rapid Solidification of Sn-Cu-Al Alloys for High-Reliability, Lead-Free Solder: Part I. Microstructural Characterization of Rapidly Solidified Solders

Abstract

Citation Formats

Heterogeneous nucleation of βSn on NiSn4, PdSn4 and PtSn4 journal, June 2014

Nucleation and Growth of Cu-Al Intermetallics in Al-Modified Sn-Cu and Sn-Ag-Cu Lead-Free Solder Alloys journal, January 2015

Heterogeneous nucleation of Cu6Sn5 in Sn–Cu–Al solders journal, January 2015

Ordering and structural vacancies in non-stoichiometric Cu–Al γ brasses journal, December 1991

The Cu–Sn phase diagram, Part I: New experimental results journal, March 2013

The constitution of the copper-rich copper-aluminium-tin alloys, with special reference to ternary compound formation journal, June 1954

Liquid demixing and microstructure formation in ternary Al–Sn–Cu alloys journal, July 2008

Isothermal transformation of β-phase in Cu-rich Cu-Al-Sn alloys journal, May 2013

Phase equilibria in the Cu-rich portion of the Cu–Al binary system journal, January 1998

The Cu–Sn phase diagram part II: New thermodynamic assessment journal, March 2013

Crystal perfection in a noncentrosymmetric alloy. Refinement and test of twinning of the γ-Cu 9 Al 4 structure journal, May 1978

The effect of Cu6Sn5 whisker precipitates in bulk 60sn-40pb solder journal, May 1987

Controlling Bulk Cu6Sn5 Nucleation in Sn0.7Cu/Cu Joints with Al Micro-alloying journal, October 2015

Re-investigation of phase equilibria in the system Al–Cu and structural analysis of the high-temperature phase η1-Al1−δCu journal, November 2011

Experimental Study of Phase Equilibria in the System Cu-Al-Sn journal, May 2013

Interstitial Diffusion of Copper in Tin journal, July 1967

Influence of Composition on the Morphology of Primary Cu6Sn5 in Sn-4Cu Alloys journal, September 2012

Development of Sn-Ag-Cu-X Solders for Electronic Assembly by Micro-Alloying with Al journal, March 2012

The aluminium-copper system journal, January 1985

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Heterogeneous nucleation of βSn on NiSn4, PdSn4 and PtSn4
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Nucleation and Growth of Cu-Al Intermetallics in Al-Modified Sn-Cu and Sn-Ag-Cu Lead-Free Solder Alloys
journal, January 2015

Heterogeneous nucleation of Cu6Sn5 in Sn–Cu–Al solders
journal, January 2015

Ordering and structural vacancies in non-stoichiometric Cu–Al γ brasses
journal, December 1991

The Cu–Sn phase diagram, Part I: New experimental results
journal, March 2013

The constitution of the copper-rich copper-aluminium-tin alloys, with special reference to ternary compound formation
journal, June 1954

Liquid demixing and microstructure formation in ternary Al–Sn–Cu alloys
journal, July 2008

Isothermal transformation of β-phase in Cu-rich Cu-Al-Sn alloys
journal, May 2013

Phase equilibria in the Cu-rich portion of the Cu–Al binary system
journal, January 1998

The Cu–Sn phase diagram part II: New thermodynamic assessment
journal, March 2013

Crystal perfection in a noncentrosymmetric alloy. Refinement and test of twinning of the γ-Cu ₉ Al ₄ structure
journal, May 1978

The effect of Cu6Sn5 whisker precipitates in bulk 60sn-40pb solder
journal, May 1987

Controlling Bulk Cu6Sn5 Nucleation in Sn0.7Cu/Cu Joints with Al Micro-alloying
journal, October 2015

Re-investigation of phase equilibria in the system Al–Cu and structural analysis of the high-temperature phase η1-Al1−δCu
journal, November 2011

Experimental Study of Phase Equilibria in the System Cu-Al-Sn
journal, May 2013

Interstitial Diffusion of Copper in Tin
journal, July 1967

Influence of Composition on the Morphology of Primary Cu6Sn5 in Sn-4Cu Alloys
journal, September 2012

Development of Sn-Ag-Cu-X Solders for Electronic Assembly by Micro-Alloying with Al
journal, March 2012

The aluminium-copper system
journal, January 1985

Rapid Solidification of Sn-Cu-Al Alloys for High-Reliability, Lead-Free Solder: Part II. Intermetallic Coarsening Behavior of Rapidly Solidified Solders After Multiple Reflows
journal, October 2016

Beta-Tin Grain Formation in Aluminum-Modified Lead-Free Solder Alloys
journal, October 2017