Effects of multi-energy field electrodeposition on properties of Al<sub>2</sub>O<sub>3</sub>-Co composite films

Qi Yun-Kai; Yang Shu-Min; Li Xin; Xu Qin; Gu Jian-Jun

doi:10.7498/aps.71.20211313

Abstract

The multi-energy composite field micro-electrodeposition processing technology is used to prepare colorful structural coloration magnetic Al₂O₃-Co composite films each with a gradual microstructure. Under the action of the deposition electric field and the deflection electric field perpendicular to it, the microstructure, optical properties and magnetic properties of the composite films show gradual characteristics along the direction of the deflection electric field. By establishing an equivalent model of the microstructure, the mechanism of the microstructure change of the composite film is theoretically analyzed. Through software simulation, the distribution of Co ion deposition current density along the direction of the deflection electric field is quantitatively analyzed. The simulation results are consistent with the theoretical and experimental results. Through this study, we find that the micro-electrodeposition processing technology with using multi-energy field composite can control the micro-domain structure of the composite film from a microscopic point of view, and achieve the fine control of the magnetic and optical properties of the film micro-domain.

Keywords:

Authors and contacts

1.
College of Physics and Electronic Engineering, Hebei Normal University for Nationalities, Chengde 067000, China
2.
School of science, Hebei University of Technology, Tianjin 300401, China

Corresponding author: Gu Jian-Jun, jjungu@126.com

Funds: Project supported by the Natural Science Foundation of Hebei Province, China (Grant Nos. A2012101001, A2019202190) and the High-level TalentsFunded Projects of Hebei Province, China (Grant No. A2016002040).

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References

[1]	Domagalski J T, Xifre-Perez E, Tabrizi M A, Ferre-Borrull J, Marsal L F 2021 J. Colloid Interface Sci. 584 15
[2]	程自强, 石海泉, 余萍, 刘志敏 2018 物理学报 67 197302 Google Scholar Cheng Z Q, Shi H Q, Yu P, Liu Z M 2018 Acta Phys. Sin. 67 197302 Google Scholar
[3]	Zhang K X, Yao C B, Wen X, Li Q H, Sun W J 2018 RSC Adv. 46 8
[4]	Nie M, Sun H, Gao Z D, Li Q, Xue Z H, Luo J, Liao J M 2020 Electrochem. Commun. 115 106719 Google Scholar
[5]	Gu J J, Yang S M, Dong M Y, Qi Y K 2017 J. Alloys Compd. 728 25
[6]	Yang S M, Han W, Li H T, Qi Y K, Gu J J 2015 J. Electrochem. Soc. 162 E123 Google Scholar
[7]	梁玲玲, 赵艳, 冯超 2020 物理学报 69 065201 Google Scholar Liang L L, Zhao Y, Feng C 2020 Acta Phys. Sin. 69 065201 Google Scholar
[8]	Yue Y, Coburn K, Reed B, Liang H 2018 J. Appl. Electrochem. 48 3
[9]	Ali H O 2017 Int. J. Surf. Eng. Coat. 95 6
[10]	Mahmoud A T, Josep F B, Lluis F M 2020 Microchim. Acta 187 230 Google Scholar
[11]	Sergey E, Kushnir, Kirill S, Napolskii 2018 Mater. Des. 144 15
[12]	Pankaj K, Josep F B, Lluis F M 2020 Adv. Mater. Interfaces 7 22
[13]	Kirill S N, Alexey A N, Sergey E K 2020 Opt. Mater. 109 110317 Google Scholar
[14]	Mahmoud A T, Josep F B, Lluis F M 2020 Sci. Rep. 10 2356 Google Scholar
[15]	Mo R J, He L, Yan X M, Su T T, Zhou C X, Wang Z, Hong P Z 2018 Electrochem. Commun. 95 9 Google Scholar
[16]	Liudmyla R, Kateryna K, Volodymyr O, Menglei C 2021 Ukr. Chem. Journ. 86 5
[17]	Li X C, Zhang T C, Gao P C 2018 Langmuir 34 49
[18]	Liu S X, Tian J L, Zhang W 2021 Nanotechnology 32 222001 Google Scholar
[19]	Kapoor S, Ahmad H, Julien C M, Islam S S 2020 Appl. Surf. Sci. 512 145654 Google Scholar
[20]	Sistani M, Staudinger P, Greil J, Holzbauer M, Detz H, Bertagnolli E, Lugstein A 2017 Nano Lett. 17 8 Google Scholar
[21]	Fang J, Chen S, Vandenberghe W G, Fischetti M V 2017 IEEE Trans. Electron Devices 64 2758 Google Scholar
[22]	杨淑敏, 韩伟, 顾建军, 李海涛, 岂云开 2015 物理学报 64 076102 Google Scholar Yang S M, Han W, Gu J J, Li H T, Qi Y K 2015 Acta Phys. Sin. 64 076102 Google Scholar
[23]	Ruiz-Clavijo A, Caballero-Calero O, Martín-González M 2021 Nanoscale 13 4

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图 1 多能场复合电沉积装置示意图　(a) 结构示意图; (b) 电沉积示意图

Figure 1. Schematic diagram of electrodeposition device with multienergy composite field. (a) Structure schematic diagram; (b) electrodeposition diagram.

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图 2 氧化铝薄膜和Al₂O₃-Co复合薄膜数码照片及XRD图谱　(a) 氧化电压20 V, 氧化时间11 min条件下制备的氧化铝薄膜数码照片; (b) 沉积电压12 V, 沉积时间60 s, 偏转电场120 V/m条件下制备的Al₂O₃-Co复合薄膜数码照片; (c) 图2(b) 所示薄膜的XRD图谱

Figure 2. Digital photos of alumina film and Al₂O₃-Co composite film and XRD diffraction pattern: (a) Digital photo of alumina film oxidized with a voltage of 20 V for 11 min; (b) digital photo of Al₂O₃-Co composite film deposited with a voltage of 12 V for 60 s and deflection field of 120 V/m; (c) XRD diffraction pattern of Al₂O₃-Co composite film shown in Fig. 2(b).

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图 3 Al₂O₃-Co复合薄膜SEM表面和截面照片 (a)−(c)分别对应图2(b)所示薄膜A到C的位置.

Figure 3. SEM surface and cross-sectional images of Al₂O₃-Co composite film: (a)−(c) corresponding to positions A to C in Fig. 2(b).

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图 4 Al₂O₃-Co复合薄膜的结构模型 (a)−(c)分别对应图2(b)所示薄膜的A到C的位置

Figure 4. The structural models of Al₂O₃-Co composite film: (a)−(c) corresponding to positions A to C in Fig. 2(b).

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图 5 图2(b)所示Al₂O₃-Co复合薄膜反射光谱

Figure 5. The reflection spectrum of Al₂O₃-Co composite film shown in Fig.2 (b).

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图 6 Al₂O₃-Co复合薄膜沿径向电流密度分布曲线

Figure 6. The curve of deposition current density along the radial of Al₂O₃-Co composite film shown in Fig.2 (b).

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图 7 Al₂O₃-Co复合薄膜区域划分示意图和单位面积沉积率曲线　(a) Al₂O₃-Co复合薄膜沿径向不同区域划分示意图; (b) 不同划分区域单位面积沉积率曲线

Figure 7. Partition diagram and curve of per unit area deposition rate of Al₂O₃-Co composite film: (a) Diagram of different regions along the radial direction of Al₂O₃-Co composite film shown in Fig.2 (b); (b) the curve of deposition rate per unit area via divided regions.

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图 8 图2(b)所示Al₂O₃-Co复合薄膜表面Co离子分布仿真图

Figure 8. Diagram of Co ion distribution on Al₂O₃-Co composite film surface shown in Fig.2 (b).

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图 9 室温下Al₂O₃-Co复合薄膜磁化曲线a−c对应图2(b)所示薄膜A到C位置

Figure 9. Hysteresis loops of different positions on Al₂O₃-Co composite film at room temperature. Curves a−c correspond to positions A to C in Fig. 2(b).

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图 10 Al₂O₃-Co复合薄膜数码照片　(a) 氧化电压20 V氧化时间14 min, 沉积电压12 V, 偏转电场120 V/m, 沉积时间分别为30, 40, 50, 60 s; (b) 氧化电压20 V氧化时间分别为12, 13, 14和15 min, 沉积电压12 V, 沉积时间为60 s, 偏转电场120 V/m

Figure 10. Digital photos of Al₂O₃-Co composite films: (a) The films were oxidized with a voltage of 20 V for 14 min. Then they were deposited with a voltage of 12 V for 30, 40, 50, 60 s and deflection field of 120 V/m; (b) the films were oxidized with a voltage of 20 V for 12, 13, 14 and 15 min. Then they were deposited with a voltage of 12 V for 60 s and deflection field of 120 V/m.

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图 11 Al₂O₃-Co复合薄膜数码照片　(a) 氧化电压20 V氧化时间14 min, 沉积电压为11, 12, 13 V, 沉积时间为60 s, 偏转电场120 V/m; (b) 氧化电压20 V氧化时间为14 min, 沉积电压12 V, 沉积时间为60 s, 偏转电场分别为100, 120 and 140 V/m

Figure 11. Digital photos of Al₂O₃-Co composite films: (a) The films were oxidized with a voltage of 20 V for 14 min. Then they were deposited with voltage 11, 12, 13 V for 60 s and deflection field of 120 V/m; (b) the films were oxidized with a voltage of 20 V for 14 min. Then they were deposited with a voltage 12 V for 60 s and deflection field of 100, 120 and 140 V/m.

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表 1 图2(b)所示薄膜不同区域参数表

Table 1. The parameters of different regions shown in Fig. 2(b).

区域		A	B	C
氧化铝模板厚度/nm		290	290	290
氧化铝-Co复合薄膜厚度/nm		305	295	290
结构模型	Co层厚度/nm	15	5	0
	Co纳米线密度/(%)	30	60	100
	孔洞底部Co纳米线长度/nm	160	160	160
	孔洞顶部Co纳米线长度/nm	25	15	0
等效结构模型	Co层等效厚度/nm	14	5	0
	Co纳米线长度/nm	66	102	160
	未填充纳米孔洞长度/nm	225	188	130
	干涉级别	2	1	1
	反射波长/nm	392	632	629
	对应颜色	红紫色	橙黄色	橙红色
平均折射率		n(air-Al₂O₃)=1.55 n(Co)=2.09 n(Co-Al₂O₃)=1.69

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表 2 复合薄膜区域划分面积和20 us末各区域粒子数统计表

Table 2. Partition areas of the film and particle statistics at the end of 20 μs.

区域	S1	S2	S3	S4	S5	S6	S7	S8	S9	S10
面积/mm²	6.3	11.1	13.5	14.8	15.5	15.5	14.8	13.5	11.1	6.3
粒子数/个	3	11	29	39	38	53	49	84	98	87

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[1]	Domagalski J T, Xifre-Perez E, Tabrizi M A, Ferre-Borrull J, Marsal L F 2021 J. Colloid Interface Sci. 584 15
[2]	程自强, 石海泉, 余萍, 刘志敏 2018 物理学报 67 197302 Google Scholar Cheng Z Q, Shi H Q, Yu P, Liu Z M 2018 Acta Phys. Sin. 67 197302 Google Scholar
[3]	Zhang K X, Yao C B, Wen X, Li Q H, Sun W J 2018 RSC Adv. 46 8
[4]	Nie M, Sun H, Gao Z D, Li Q, Xue Z H, Luo J, Liao J M 2020 Electrochem. Commun. 115 106719 Google Scholar
[5]	Gu J J, Yang S M, Dong M Y, Qi Y K 2017 J. Alloys Compd. 728 25
[6]	Yang S M, Han W, Li H T, Qi Y K, Gu J J 2015 J. Electrochem. Soc. 162 E123 Google Scholar
[7]	梁玲玲, 赵艳, 冯超 2020 物理学报 69 065201 Google Scholar Liang L L, Zhao Y, Feng C 2020 Acta Phys. Sin. 69 065201 Google Scholar
[8]	Yue Y, Coburn K, Reed B, Liang H 2018 J. Appl. Electrochem. 48 3
[9]	Ali H O 2017 Int. J. Surf. Eng. Coat. 95 6
[10]	Mahmoud A T, Josep F B, Lluis F M 2020 Microchim. Acta 187 230 Google Scholar
[11]	Sergey E, Kushnir, Kirill S, Napolskii 2018 Mater. Des. 144 15
[12]	Pankaj K, Josep F B, Lluis F M 2020 Adv. Mater. Interfaces 7 22
[13]	Kirill S N, Alexey A N, Sergey E K 2020 Opt. Mater. 109 110317 Google Scholar
[14]	Mahmoud A T, Josep F B, Lluis F M 2020 Sci. Rep. 10 2356 Google Scholar
[15]	Mo R J, He L, Yan X M, Su T T, Zhou C X, Wang Z, Hong P Z 2018 Electrochem. Commun. 95 9 Google Scholar
[16]	Liudmyla R, Kateryna K, Volodymyr O, Menglei C 2021 Ukr. Chem. Journ. 86 5
[17]	Li X C, Zhang T C, Gao P C 2018 Langmuir 34 49
[18]	Liu S X, Tian J L, Zhang W 2021 Nanotechnology 32 222001 Google Scholar
[19]	Kapoor S, Ahmad H, Julien C M, Islam S S 2020 Appl. Surf. Sci. 512 145654 Google Scholar
[20]	Sistani M, Staudinger P, Greil J, Holzbauer M, Detz H, Bertagnolli E, Lugstein A 2017 Nano Lett. 17 8 Google Scholar
[21]	Fang J, Chen S, Vandenberghe W G, Fischetti M V 2017 IEEE Trans. Electron Devices 64 2758 Google Scholar
[22]	杨淑敏, 韩伟, 顾建军, 李海涛, 岂云开 2015 物理学报 64 076102 Google Scholar Yang S M, Han W, Gu J J, Li H T, Qi Y K 2015 Acta Phys. Sin. 64 076102 Google Scholar
[23]	Ruiz-Clavijo A, Caballero-Calero O, Martín-González M 2021 Nanoscale 13 4

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Effects of multi-energy field electrodeposition on properties of Al₂O₃-Co composite films

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Corresponding author: Gu Jian-Jun, jjungu@126.com

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Effects of multi-energy field electrodeposition on properties of Al2O3-Co composite films

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Corresponding author: Gu Jian-Jun, jjungu@126.com

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Effects of multi-energy field electrodeposition on properties of Al₂O₃-Co composite films