Top-view analysis of ultrafast differential scanning calorimetry data

Cheng Qi; Sun Yong-Hao; Wang Wei-Hua

doi:10.7498/aps.73.20232027

Abstract

Ultrafast differential scanning calorimetry is the third-generation technique of differential thermal-analysis. It can fast heat up to 60000 K/s or fast cool down to 40000 K/s, so its temperature-changing rate spans five orders of magnitude, and permit repeating experiments on compounds or materials with a melting point lower than 1000 ℃. The unique rate of temperature change allows it to record structural changes of sample in milliseconds, producing a significant number of data. A “top-view” graph is suggested in this study for data analysis. It basically projects the heat flow onto a plane of variables such as temperature, rate or time and uses color contrast to describe the intensity change of heat flow. The issues with “side-view” graphs, where it is a challenge to discern rate or time from several curves, are successfully resolved by this novel technique. It can also realize a comparison of the kinetics among several co-existing physical events. Using an Au-based metallic glass as an example material, this work collects the data from four “side-view” graphs in literature, replots the data on “top-view” graphs, and compares pros and cons. Any substance or material to be examined by utilizing fast differential scanning calorimetry can be examined through using the “top-view” approach. It is useful not only for data analysis but also for constructing processing maps for novel materials, finding new structural transitions, and examining the kinetic behaviors of physical phenomena. All the data presented in this paper are openly available at https://doi.org/ 10.57760/sciencedb.j00213.00012.

Keywords:

Authors and contacts

1.
Beijing National Laboratory for Molecular Sciences, College of Chemistry and Molecular Engineering, Institute of Physical Chemistry, Peking University, Beijing 100871, China
2.
Key Laboratory of Extreme Conditions Physics, Institute of Physics, Chinese Academy of Sciences, Beijing 100190, China
3.
Songshan Lake Materials Lab, Dongguan 523808, China

Corresponding author: Sun Yong-Hao, ysun58@iphy.ac.cn

Funds: Project supported by the National Natural Science Foundation of China (Grant No. 92263103) and the National Key Technology Research and Development Program of China (Grant No. 2018YFA0703603).

[1]	瓦格纳M著 (陆立华译) 2011 热分析应用基础 (上海: 东华大学出版社) 第1页 Wagner M (translated by Lu L H) 2011 Thermal Analysis in Practice (Shanghai: Dong Hua University Press) p1
[2]	Ravisankar R, Naseerutheen A, Rajalakshmi A, Raja Annamalai, G, Chandrasekaran A 2014 Spectrochim. Acta A 129 201 Google Scholar
[3]	刘振海, 陆立明, 唐远望 2012 热分析简明教程 (北京: 科学出版社) 第1页 Liu Z H, Lu L M, Tang Y W 2012 A Concise Coursebook of Thermal Analysis (Beijing: Science Press) p1
[4]	Boersma S L 1955 J. Amer. Ceram. 38 281 Google Scholar
[5]	Watson E S, O’Neill M J, Justin J, Brenner N 1964 Anal. Chem. 36 1233 Google Scholar
[6]	Reading M, Elliott D, Hill V L 1993 J. Therm. Anal. 40 949 Google Scholar
[7]	Schick C, Mathot V 2016 Fast Scanning Calorimetry (Switzerland: Springer Nature
[8]	Cheng Q, Sun Y H, Orava J, Bai H Y, Wang W H 2022 Acta Mater. 230 117834 Google Scholar
[9]	Cheng Q, Han X L, Kaban I, Soldatov I, Wang W H, Sun Y H, Orava J 2020 Scripta Mater. 183 61 Google Scholar
[10]	Cheng Q, Wang P F, Jiang H Y, Gu L, Orava J, Sun Y H, Bai H Y, Wang W H 2021 Phys. Rev. B 103 L100203 Google Scholar
[11]	Shen J, Lu Z, Wang J Q, Lan S, Zhang F, Hirata A, Chen M W, Wang X L, Wen P, Sun Y H, Bai H Y, Wang W H 2020 J. Phys. Chem. Lett. 11 6718 Google Scholar
[12]	Shen J, Sun Y H, Orava J, Bai H Y, Wang W H 2022 Acta Mater. 225 117588 Google Scholar
[13]	江海河 2001 光电子技术与信息 14 1 Jiang H H 2001 Opto-Electronics Tech. Info. 14 1
[14]	Schroers J, Lohwongwatana B, Johnson W L, Peker A 2007 Mater. Sci. Eng. A 449 235
[15]	Schorers J, Lohwongwatana B, Johnson W L, Peker A 2005 Appl. Phys. Lett. 87 061912 Google Scholar
[16]	Cardinal S, Qiao J C, Pelletier J M 2014 Mater. Sci. Forum 783 1901
[17]	Zhang W, Guo H, Chen M W, Saotome Y, Qin C L, Inoue S 2009 Scripta Mater. 61 744 Google Scholar
[18]	Na J H, Han K H, Garrett G R, Launey M F, Demetriou M D, Johnson W L 2019 Sci. Rep. 9 3269 Google Scholar
[19]	Rizzi P, Corazzari I, Fiore G, Fenoglio I, Fubini B, Kaciulis S, Battezzati L 2013 Cor. Sci. 77 135 Google Scholar
[20]	Eisenbart M, Klotz U E, Busch R, Gallino I 2014 J. Alloys Compd. 615 S118 Google Scholar
[21]	Eisenbart M, Klotz U E, Busch R, Gallino I 2014 Cor. Sci. 85 258 Google Scholar
[22]	Ivanov Y P, Meylan C M, Panagiotopoulos N T, Georgorakis K, Greer A L 2020 Acta Mater. 196 52 Google Scholar
[23]	Schawe J E K, Löffler J F 2019 Nat. Commun. 10 1337 Google Scholar
[24]	Cheng Q, Sun Y H, Orava J, Wang W H 2023 Mater. Today Phys. 31 101004 Google Scholar
[25]	Song L J, Xu W, Huo J T, Wang J Q, Wang X M, Li R W 2018 Intermetallics 93 101 Google Scholar
[26]	Song L J, Gao M, Xu W, Huo J T, Wang J Q, Li R W, Wang W H, Perepezko J H 2020 Acta Mater. 185 38 Google Scholar
[27]	Schawe J E K, Löffler J F 2022 Acta Mater. 226 117630
[28]	Zhang L J, Wang C H, Wu H Y, Wang L M, Yi J, Zhai Q J, Gao Y L, Zhao B G 2024 Thermochim. Acta 731 179643 Google Scholar
[29]	Song L J, Gao Y R, Zou P, Xu W, Gao M, Zhang Y, Huo J T, Li F S, Qiao J C, Wang L M, Wang J Q 2023 Proc. Natl. Acad. Sci. 120 e2302776120 Google Scholar
[30]	Lisio V D, Gallino I, Riegler S S, Frey M, Neuber N, Kumar G, Schroers J, Busch R, Cangialosi D 2023 Nat. Commun. 14 4698 Google Scholar
[31]	Pogatscher S, Leutenegger D, Schawe J E K, Uggowitzer P J, Löffler J F 2016 Nat. Commun. 7 11113 Google Scholar
[32]	Kissinger H E 1956 Journal of Research of the National Bureau of Standards 57 217 Google Scholar
[33]	汪卫华 2023 非晶态物质—常规物质第四态(第二卷) (北京: 科学出版社) 第279页 Wang W H 2023 Amorphous Matter: The Forth Conventional Matter (Vol. 2) (Beijing: Science Press) p279

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图 1 FDSC实验的温控程序(T_q代表熔体温度, T_a代表退火温度, φ_c代表冷却速率, φ_h代表加热速率, t_a代表退火时间; 双箭头代表变量可以调节的方向)

Figure 1. Thermal protocol of FDSC experiments (T_q is quenching temperature, T_a is annealing temperature, φ_c is cooling rate, φ_h is heating rate, t_a is annealing time; double arrows indicate directions of change for variables).

DownLoad: Full-Size Img PowerPoint

图 2 FDSC结果的三维形貌图、侧视图和俯视图 (h' 代表被φ_h约化后的热流, 数据来源于参考文献[23])

Figure 2. 3D morphology, side and top views of typical FDSC results (h' is φ_h-normalized heat flow, reproduced from Ref. [23]).

DownLoad: Full-Size Img PowerPoint

图 3 铸态Au基非晶合金的超快加热曲线　(a) 侧视图; (b) 俯视图; (c) 低热流强度下的俯视图. 方块和圆圈分别代表焓过冲和晶化的峰值温度; 信息数据来源于文献[22]. 注: 由于文献[22]未能提供部分曲线上完整的晶化峰或熔化峰信息, 所以部分热流曲线不连续

Figure 3. Ultrafast heating curves of the as-cast Au-based metallic glass: (a) Side view; (b) top view; (c) top view under low heat flux intensity. Squares and circles represent peak temperatures of enthalpy overshoot and crystallization; reproduced from Ref. [22]. Note: Due to the lack of a complete crystallization peak or a complete melting peak on some heat-flow curves in Ref. [22], some of the presented appear discontinuous.

DownLoad: Full-Size Img PowerPoint

图 4 退火态Au基非晶合金的超快加热曲线　(a) 侧视图; (b) 俯视图. 圆圈代表晶化峰值温度, 数据来源于参考文献[27]

Figure 4. Ultrafast heating curves of the annealed Au-based metallic glass: (a) Side view; (b) top view. Circles represent the peak temperature of crystallization, reproduced from Ref. [27].

DownLoad: Full-Size Img PowerPoint

图 5 化学均匀型(CHG)和自掺杂型(SDG) Au基非晶合金的超快加热曲线　(a) CHG样品的侧视图; (b) SDG样品的侧视图; (c) CHG样品的俯视图; (d) SDG样品的俯视图. 三角、空心圆和实心圆分别代表焓过冲、晶化和熔化的峰值温度, 数据来源于参考文献[23]

Figure 5. Ultrafast heating curves of the chemically-homogeneous-glass (CHG) and self-doped glass (SDG) of the Au-based metallic glass: (a) Side view of CHG; (b) side view of SDG; (c) top view of CHG; (d) top view of SDG. Triangles, circles and dots denote peak temperatures of enthalpy overshoot, crystallization and melting, respectively, reproduced from Ref. [23].

DownLoad: Full-Size Img PowerPoint

图 6 退火态Au基非晶合金的超快加热曲线　(a)侧视图; (b)俯视图. 圆圈代表焓过冲的峰值温度, 数据来源于参考文献[29]

Figure 6. Ultrafast heating curves of the annealed Au-based metallic glass: (a) Side view; (b) top view. Circles represent the peak temperatures of enthalpy overshoot, reproduced from Ref. [29].

DownLoad: Full-Size Img PowerPoint

DownLoad: Full-Size Img PowerPoint

表 1 Au基化学均匀型玻璃(CHG)和自掺杂型玻璃(SDG)的α弛豫、晶化和熔化激活能

Table 1. Activation energy of Au-based CHG and SDG metallic glasses for their α relaxation, crystallization and melting

物理过程 CHG的激活能E_a/(kJ·mol^–1) SDG的激活能E_a/(kJ·mol^–1) 相对变化

α弛豫 110±11 85±7 –23%

结晶 94±13 105±5 12%

熔化 430±43 380±26 –12%

DownLoad: CSV

[1]	瓦格纳M著 (陆立华译) 2011 热分析应用基础 (上海: 东华大学出版社) 第1页 Wagner M (translated by Lu L H) 2011 Thermal Analysis in Practice (Shanghai: Dong Hua University Press) p1
[2]	Ravisankar R, Naseerutheen A, Rajalakshmi A, Raja Annamalai, G, Chandrasekaran A 2014 Spectrochim. Acta A 129 201 Google Scholar
[3]	刘振海, 陆立明, 唐远望 2012 热分析简明教程 (北京: 科学出版社) 第1页 Liu Z H, Lu L M, Tang Y W 2012 A Concise Coursebook of Thermal Analysis (Beijing: Science Press) p1
[4]	Boersma S L 1955 J. Amer. Ceram. 38 281 Google Scholar
[5]	Watson E S, O’Neill M J, Justin J, Brenner N 1964 Anal. Chem. 36 1233 Google Scholar
[6]	Reading M, Elliott D, Hill V L 1993 J. Therm. Anal. 40 949 Google Scholar
[7]	Schick C, Mathot V 2016 Fast Scanning Calorimetry (Switzerland: Springer Nature
[8]	Cheng Q, Sun Y H, Orava J, Bai H Y, Wang W H 2022 Acta Mater. 230 117834 Google Scholar
[9]	Cheng Q, Han X L, Kaban I, Soldatov I, Wang W H, Sun Y H, Orava J 2020 Scripta Mater. 183 61 Google Scholar
[10]	Cheng Q, Wang P F, Jiang H Y, Gu L, Orava J, Sun Y H, Bai H Y, Wang W H 2021 Phys. Rev. B 103 L100203 Google Scholar
[11]	Shen J, Lu Z, Wang J Q, Lan S, Zhang F, Hirata A, Chen M W, Wang X L, Wen P, Sun Y H, Bai H Y, Wang W H 2020 J. Phys. Chem. Lett. 11 6718 Google Scholar
[12]	Shen J, Sun Y H, Orava J, Bai H Y, Wang W H 2022 Acta Mater. 225 117588 Google Scholar
[13]	江海河 2001 光电子技术与信息 14 1 Jiang H H 2001 Opto-Electronics Tech. Info. 14 1
[14]	Schroers J, Lohwongwatana B, Johnson W L, Peker A 2007 Mater. Sci. Eng. A 449 235
[15]	Schorers J, Lohwongwatana B, Johnson W L, Peker A 2005 Appl. Phys. Lett. 87 061912 Google Scholar
[16]	Cardinal S, Qiao J C, Pelletier J M 2014 Mater. Sci. Forum 783 1901
[17]	Zhang W, Guo H, Chen M W, Saotome Y, Qin C L, Inoue S 2009 Scripta Mater. 61 744 Google Scholar
[18]	Na J H, Han K H, Garrett G R, Launey M F, Demetriou M D, Johnson W L 2019 Sci. Rep. 9 3269 Google Scholar
[19]	Rizzi P, Corazzari I, Fiore G, Fenoglio I, Fubini B, Kaciulis S, Battezzati L 2013 Cor. Sci. 77 135 Google Scholar
[20]	Eisenbart M, Klotz U E, Busch R, Gallino I 2014 J. Alloys Compd. 615 S118 Google Scholar
[21]	Eisenbart M, Klotz U E, Busch R, Gallino I 2014 Cor. Sci. 85 258 Google Scholar
[22]	Ivanov Y P, Meylan C M, Panagiotopoulos N T, Georgorakis K, Greer A L 2020 Acta Mater. 196 52 Google Scholar
[23]	Schawe J E K, Löffler J F 2019 Nat. Commun. 10 1337 Google Scholar
[24]	Cheng Q, Sun Y H, Orava J, Wang W H 2023 Mater. Today Phys. 31 101004 Google Scholar
[25]	Song L J, Xu W, Huo J T, Wang J Q, Wang X M, Li R W 2018 Intermetallics 93 101 Google Scholar
[26]	Song L J, Gao M, Xu W, Huo J T, Wang J Q, Li R W, Wang W H, Perepezko J H 2020 Acta Mater. 185 38 Google Scholar
[27]	Schawe J E K, Löffler J F 2022 Acta Mater. 226 117630
[28]	Zhang L J, Wang C H, Wu H Y, Wang L M, Yi J, Zhai Q J, Gao Y L, Zhao B G 2024 Thermochim. Acta 731 179643 Google Scholar
[29]	Song L J, Gao Y R, Zou P, Xu W, Gao M, Zhang Y, Huo J T, Li F S, Qiao J C, Wang L M, Wang J Q 2023 Proc. Natl. Acad. Sci. 120 e2302776120 Google Scholar
[30]	Lisio V D, Gallino I, Riegler S S, Frey M, Neuber N, Kumar G, Schroers J, Busch R, Cangialosi D 2023 Nat. Commun. 14 4698 Google Scholar
[31]	Pogatscher S, Leutenegger D, Schawe J E K, Uggowitzer P J, Löffler J F 2016 Nat. Commun. 7 11113 Google Scholar
[32]	Kissinger H E 1956 Journal of Research of the National Bureau of Standards 57 217 Google Scholar
[33]	汪卫华 2023 非晶态物质—常规物质第四态(第二卷) (北京: 科学出版社) 第279页 Wang W H 2023 Amorphous Matter: The Forth Conventional Matter (Vol. 2) (Beijing: Science Press) p279

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