Application of the Box–Behnken design in the response surface methodology for the precipitation of Ni/Ni oxalate composite anodes

Mehmet Feryat Gulcan; Billur Deniz Karahan; Ozgul Keles

doi:10.1007/s10800-023-01846-7

Application of the Box–Behnken design in the response surface methodology for the precipitation of Ni/Ni oxalate composite anodes

Mehmet Feryat Gulcan
, Billur Deniz Karahan^*
, Ozgul Keles

^*Corresponding author for this work

Department of Metallurgical and Materials Engineering

Istanbul Technical University
Istanbul Medipol University

Research output: Contribution to journal › Article › peer-review

5 Citations (Scopus)

Abstract

In this work, first, using the Box–Behnken method, the temperature, oxalic acid/nickel mole ratio, and stirring duration are optimized to maximize the precipitation efficiency of nickel oxalate. Then, ANOVA is used to study the statistically significant parameters and their interactions. At 42.5 °C, with a 1.25 oxalic acid/nickel mole ratio and a 135 min stirring duration, 99.94% precipitation efficiency is achieved. A good agreement (R ² = 0.9535) between the predicted and experimental values is reported. Then, this obtained nickel oxalate hydrate is heat-treated at 290 °C for 3 h in a vacuum and turned into a composite made of anhydride oxalate and metallic nickel. The possible use of this composite as an anode material is first investigated: it delivers a capacity of 552.24 mAh g⁻¹ after 100 cycles under a load of 100 mA g⁻¹. Cyclic voltammetry is utilized to probe its lithiation mechanism. The structural and morphological properties of the composite are cited as a reason for its good cycling performance. Graphical abstract: [Figure not available: see fulltext.].

Original language	English
Pages (from-to)	1193-1205
Number of pages	13
Journal	Journal of Applied Electrochemistry
Volume	53
Issue number	6
DOIs	https://doi.org/10.1007/s10800-023-01846-7
Publication status	Published - Jun 2023

Bibliographical note

Publisher Copyright:
© 2023, The Author(s), under exclusive licence to Springer Nature B.V.

Funding

The authors thank Prof Dr Sebahattin Gürmen, Prof. Dr. Yasemin Yüksel Durmaz and Erhan Demirel for their supports. Finally, thanks are due to Istanbul Medipol University-Regenerative and Restorative Medicine Research Center for SEM and XRD characterizations.

Funders
Istanbul Medipol University-Regenerative and Restorative Medicine Research Center

UN SDGs

This output contributes to the following UN Sustainable Development Goals (SDGs)

SDG 7 Affordable and Clean Energy

Keywords

Composite powder
Electrode material
Lithium-ion batteries
Precipitation
Response surface methodology

Access to Document

10.1007/s10800-023-01846-7

Cite this

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title = "Application of the Box–Behnken design in the response surface methodology for the precipitation of Ni/Ni oxalate composite anodes",

abstract = "In this work, first, using the Box–Behnken method, the temperature, oxalic acid/nickel mole ratio, and stirring duration are optimized to maximize the precipitation efficiency of nickel oxalate. Then, ANOVA is used to study the statistically significant parameters and their interactions. At 42.5 °C, with a 1.25 oxalic acid/nickel mole ratio and a 135 min stirring duration, 99.94\% precipitation efficiency is achieved. A good agreement (R 2 = 0.9535) between the predicted and experimental values is reported. Then, this obtained nickel oxalate hydrate is heat-treated at 290 °C for 3 h in a vacuum and turned into a composite made of anhydride oxalate and metallic nickel. The possible use of this composite as an anode material is first investigated: it delivers a capacity of 552.24 mAh g−1 after 100 cycles under a load of 100 mA g−1. Cyclic voltammetry is utilized to probe its lithiation mechanism. The structural and morphological properties of the composite are cited as a reason for its good cycling performance. Graphical abstract: [Figure not available: see fulltext.].",

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doi = "10.1007/s10800-023-01846-7",

language = "English",

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AU - Gulcan, Mehmet Feryat

AU - Karahan, Billur Deniz

AU - Keles, Ozgul

PY - 2023/6

Y1 - 2023/6

N2 - In this work, first, using the Box–Behnken method, the temperature, oxalic acid/nickel mole ratio, and stirring duration are optimized to maximize the precipitation efficiency of nickel oxalate. Then, ANOVA is used to study the statistically significant parameters and their interactions. At 42.5 °C, with a 1.25 oxalic acid/nickel mole ratio and a 135 min stirring duration, 99.94% precipitation efficiency is achieved. A good agreement (R 2 = 0.9535) between the predicted and experimental values is reported. Then, this obtained nickel oxalate hydrate is heat-treated at 290 °C for 3 h in a vacuum and turned into a composite made of anhydride oxalate and metallic nickel. The possible use of this composite as an anode material is first investigated: it delivers a capacity of 552.24 mAh g−1 after 100 cycles under a load of 100 mA g−1. Cyclic voltammetry is utilized to probe its lithiation mechanism. The structural and morphological properties of the composite are cited as a reason for its good cycling performance. Graphical abstract: [Figure not available: see fulltext.].

AB - In this work, first, using the Box–Behnken method, the temperature, oxalic acid/nickel mole ratio, and stirring duration are optimized to maximize the precipitation efficiency of nickel oxalate. Then, ANOVA is used to study the statistically significant parameters and their interactions. At 42.5 °C, with a 1.25 oxalic acid/nickel mole ratio and a 135 min stirring duration, 99.94% precipitation efficiency is achieved. A good agreement (R 2 = 0.9535) between the predicted and experimental values is reported. Then, this obtained nickel oxalate hydrate is heat-treated at 290 °C for 3 h in a vacuum and turned into a composite made of anhydride oxalate and metallic nickel. The possible use of this composite as an anode material is first investigated: it delivers a capacity of 552.24 mAh g−1 after 100 cycles under a load of 100 mA g−1. Cyclic voltammetry is utilized to probe its lithiation mechanism. The structural and morphological properties of the composite are cited as a reason for its good cycling performance. Graphical abstract: [Figure not available: see fulltext.].

KW - Composite powder

KW - Electrode material

KW - Lithium-ion batteries

KW - Precipitation

KW - Response surface methodology

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IS - 6

ER -

Application of the Box–Behnken design in the response surface methodology for the precipitation of Ni/Ni oxalate composite anodes

Abstract

Bibliographical note

Funding

UN SDGs

Keywords

Access to Document

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