Preparation and electrochemical properties of nano-diamond/vertical graphene composite three-dimensional electrodes

Jiang Mei-Yan; Wang Ping; Chen Ai-Sheng; Chen Cheng-Ke; Li Xiao; Lu Shao-Hua; Hu Xiao-Jun

doi:10.7498/aps.71.20220715

Abstract

Diamond/graphene composite three-dimensional electrode has attracted extensive attention because of its low background current, wide potential window from diamond component, and high electrochemical activity from graphite component. In this work, by using the hot wire chemical vapor deposition method, nano diamonds are embedded in the vertical graphene sheet on the surface of single particle layer of nano diamond by regulating the short-term growth time to form a composite three-dimensional electrode. The results show that the electrode exhibits a wide potential window (3.59 V) and a very low background current (1.27 mA/cm²) when nano-diamond crystals grow on the top of the vertical graphene sheet. The composite structure of nano-diamond crystals coated with graphite on the top of the graphene sheet is the key to broadening the potential window and reducing the background current. With the increase of growth time, the vertical graphene sheet grows and nano-diamond grains are embedded into the lamellae, and a novel nano-diamond/graphene composite vertical lamellae structure is constructed. The ordered graphite structure increases the electrochemical active area to 677.19 μC/cm² and the specific capacitance to 627.34 μF/cm². The increase of graphite components makes the potential window narrow, and the embedded nano-diamond crystals effectively reduce the background current. This study provides a new method for preparing three-dimensional nanodiamond/graphene composite electrodes by hot wire chemical vapor deposition, and provides a new idea for fully exploiting the synergistic effect of diamond/graphene composite films.

Keywords:

Authors and contacts

College of Materials Science and Engineering, Zhejiang University of Technology, Hangzhou 310014, China

Corresponding author: Hu Xiao-Jun, huxj@zjut.edu.cn

Funds: Project supported by the Joint key Funds of National Natural Science Foundation of China (Grant No. U1809210), the National Key R&D Program of China (Grant No. 2016YFE0133200), the National International Science Technology Cooperation Program of China (Grant No. 2014DFR51160), the One Belt and One Road International Cooperation Project from the Key Research and Development Program of Zhejiang Province, China (Grant No. 2018C04021), the National Natural Science Foundation of China (Grant Nos. 50972129, 50602039, 11504325, 52002351, 52102052), and the Natural Science Foundation of Zhejiang Province, China (Grant Nos. LQ15A040004, LY18E020013, LGC21E020001).

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References

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Cited By

图 1 不同生长时间下复合薄膜的FESEM形貌和截面图, 内插图为对应样品的静态水接触角图 (a), (e), (i) 1.5 min; (b), (f), (j) 2 min; (c), (g), (k) 2.5 min; (d), (h), (l) 3 min

Figure 1. FESEM images for frontal and cross-sectional morphologies of composite films under different growth times, the inset images show the static water contact angle diagram from the corresponding samples under different growth times: (a), (e), (i) 1.5 min; (b), (f), (j) 2 min; (c), (g), (k) 2.5 min; (d), (h), (l) 3 min.

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图 2 (a) 样品在800到2000 cm^–1波数的可见光Raman光谱及拟合曲线; (b) 样品在2200到3100 cm^–1波数的可见光Raman光谱; (c) 样品的Raman光谱拟合结果演化图

Figure 2. Visible Raman spectra of the samples at the range of (a) 800–2000 cm^–1 and (b) 2200–3100 cm^–1. (c) The evolution of several typical parameters from the Raman fitting results.

DownLoad: Full-Size Img PowerPoint

图 3 不同生长时间样品的低倍, 高倍和对应白框选定区域的放大图, 及其对应区域的FFT图 (a), (e) 1.5 min; (b), (f) 2 min; (c), (g) 2.5 min; (d), (h) 3 min. (e1)—(h1), (e2)—(h2) 图(e)—(h)中对白框选定区域的放大图以及其相应的对应区域的FFT图

Figure 3. The low- and high-magnificent TEM images with inset corresponding FFTs from samples under different growth times: (a), (e) 1.5 min; (b), (f) 2 min; (c), (g) 2.5 min; (d), (h) 3 min. (e1)–(h1), (e2)–(h2) are enlarged images and corresponding FFTs of the selected areas in the corresponding white boxes in Figure (e)–(h).

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图 4 不同生长时间的NDs-VGs-SPL薄膜电极(a)在1 M KCl体系中的电势窗口和背景电流和(b)在 1 mM K₃Fe(CN)₆+1 M KCl 体系中以 100 mV/s 扫速下的循环伏安图. 图(a)和图(b)插入的表格列出了扫描速度为100 mV/s时的相应参数

Figure 4. Cyclic voltammetry curves for NDs-VGs-SPL electrodes in 1 M KCl solution (a) and in 1 mM K₃Fe(CN)₆+ 1 M KCl solution (b). The inset tables are their corresponding parameters under the scanning rate of 100 mV/s.

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图 5 不同生长时间下复合薄膜电极在0.1—0.5 V/s扫描速率下1 mol/L KOH体系中的循环伏安曲线　(a) NDs-VGs-SPL-1.5; (b) NDs-VGs-SPL-2; (c) NDs-VGs-SPL-2.5; (d) NDs-VGs-SPL-3

Figure 5. Cyclic voltammetry curves for NDs-VGs-SPL electrodes of (a) NDs-VGs-SPL-1.5, (b) NDs-VGs-SPL-2, (c) NDs-VGs-SPL-2.5, (d) NDs-VGs-SPL-3 in 1 M KOH solution under the scanning rate of 0.1–0.5 V/s.

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图 6 (a) 不同生长时间下复合薄膜电极在100 mV/s扫描速率下循环伏安曲线; (b) 复合薄膜电极对应的电容柱状图

Figure 6. (a) Cyclic voltammetry curves for NDs-VGs-SPL electrodes in 1 M KOH solution under the scanning rate of 100 mV/s; (b) capacitance histograms corresponding to NDs-VGs-SPL electrodes.

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表 1 Raman光谱拟合结果汇总

Table 1. Summary of the data from the fitted Raman spectra.

样品	1332 /arb. units	D' /arb. units	G /arb. units	FWHM_G /cm^–1	D' /arb. units	2D /arb. units	I_TPA/I_SUM	I_2D/I_G
1.5 min	0.22	0.58	0.43	90.56	—	0.17	0.44	0.40
2.0 min	—	0.84	0.73	44.85	0.26	0.57	0.35	0.65
2.5 min	—	0.85	0.48	34.12	0.22	0.31	0.30	0.63
3.0 min	—	0.92	0.66	33.40	0.21	0.76	0.28	1.14
注: 表格中“—”符号表示Raman光谱中未检测到此峰位.

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map

[1]	Lesiak B, Kövér L, Tóth J, Zemek J, Jiricek P, Kromka A, Rangam N 2018 Appl. Surf. Sci. 452 223 Google Scholar
[2]	Zhai Z, Huang N, Jiang X 2022 Curr. Opin. Electrochem. 32 100884 Google Scholar
[3]	Chen C K, He Z, Xu A, Li X, Jiang M, Xu T, Yan B, Hu X 2021 Funct. Diamond 1 117 Google Scholar
[4]	胡衡, 胡晓君, 白博文, 陈小虎 2012 61 148101 Google Scholar Hu H, Hu X J, Bai B W, Chen X H 2012 Acta Phys. Sin. 61 148101 Google Scholar
[5]	潘金平, 胡晓君, 陆利平, 印迟 2010 59 7410 Google Scholar Pan J P, Hu X J, Lu L P, Yin C 2010 Acta Phys. Sin. 59 7410 Google Scholar
[6]	胡晓君, 李荣斌, 沈荷生, 何贤昶, 邓文, 罗里熊 2004 53 2014 Google Scholar Hu X J, Li R B, Shen H S, He X C, Deng W, Luo L X 2004 Acta Phys. Sin. 53 2014 Google Scholar
[7]	Yang N, Yu S, Macpherson J V, Einaga Y, Zhao H, Zhao G, Swain G M, Jiang X 2019 Chem. Soc. Rev. 48 157 Google Scholar
[8]	Gao F, Nebel C E 2016 ACS Appl. Mater. Interfaces 8 28244 Google Scholar
[9]	Watanabe T, Honda Y, Kanda K, Einaga Y 2014 Phys. Status Solidi A 211 2709 Google Scholar
[10]	Sun Y, Wu Q, Xu Y, Bai H, Li C, Shi G 2011 J. Mater. Chem. 21 7154 Google Scholar
[11]	Wei M, Terashima C, Lv M, Fujishima A, Gu Z Z 2009 Chem. Commun. 24 3624 Google Scholar
[12]	蒋梅燕, 朱政杰, 陈成克, 李晓, 胡晓君 2019 68 148101 Google Scholar Jiang M Y, Zhu Z J, Chen C K, Li X, Hu X J 2019 Acta Phys. Sin. 68 148101 Google Scholar
[13]	王锐, 胡晓君 2014 63 148102 Google Scholar Wang R, Hu X J 2014 Acta Phys. Sin. 63 148102 Google Scholar
[14]	Sobaszek M, Siuzdak K, Ryl J, Sawczak M, Gupta S, Carrizosa S B, Ficek M, Dec B, Darowicki K, Bogdanowicz R 2017 J. Phys. Chem. C 121 20821 Google Scholar
[15]	Shen A, Zou Y, Wang Q, Dryfe R A W, Huang X, Dou S, Dai L, Wang S 2014 Angew. Chem. Int. Ed. 53 10804 Google Scholar
[16]	Kamata T, Kato D, Ida H, Niwa O 2014 Diamond Relat. Mater. 49 25 Google Scholar
[17]	Garcia-Segura S, Vieira dos Santos E, Martínez Huitle C A 2015 Electrochem. Commun. 59 52 Google Scholar
[18]	Ayres Z J, Borrill A J, Newland J C, Newton M E, Macpherson Julie. V 2016 Anal. Chem. 88 974 Google Scholar
[19]	Cobb S J, Ayres Z J, Macpherson J V 2018 Annu. Rev. Anal. Chem. 11 463 Google Scholar
[20]	Vlasov I, Lebedev O I, Ralchenko V G, Goovaerts E, Bertoni G, Van Tendeloo G, Konov V I 2007 Adv. Mater. 19 4058 Google Scholar
[21]	Arenal R, Bruno P, Miller D J, Bleuel M, Lal J, Gruen D M 2007 Phys. Rev. B 75 195431 Google Scholar
[22]	Sankaran K J, Kurian J, Chen H C, Dong C L, Lee C Y, Tai N H, Lin I N 2012 J. Phys. D:Appl. Phys. 45 365303 Google Scholar
[23]	Shang N, Papakonstantinou P, Wang P, Zakharov A, Palnitkar U, Lin I N, Chu M, Stamboulis A 2009 ACS Nano 3 1032 Google Scholar
[24]	Shalini J, Sankaran K J, Dong C L, Lee C Y, Tai N H, Lin I N 2013 Nanoscale 5 1159 Google Scholar
[25]	Shalini J, Lin Y C, Chang T H, Sankaran K J, Chen H C, Lin I N, Lee C Y, Tai N H 2013 Electrochim. Acta 92 9 Google Scholar
[26]	Zhai Z, Huang N, Yang B, Wang C, Liu L, Qiu J, Shi D, Yuan Z, Lu Z, Song H, Zhou M, Chen B, Jiang X 2019 J. Phys. Chem. C 123 6018 Google Scholar
[27]	Yu S, Sankaran K J, Korneychuk S, Verbeeck J, Haenen K, Jiang X, Yang N 2019 Nanoscale 11 17939 Google Scholar
[28]	邢丽丹, 谢启明, 李伟善 2020 69 228205 Google Scholar Xing L D, Xie Q M, Li W S 2020 Acta Phys. Sin. 69 228205 Google Scholar
[29]	Wu, Yang 2002 Nano Lett. 2 355 Google Scholar
[30]	Tzeng Y, Chen W L, Wu C, Lo J Y, Li C Y 2013 Carbon 53 120 Google Scholar
[31]	Banerjee D, Sankaran K J, Deshmukh S, Ficek M, Bhattacharya G, Ryl J, Phase D M, Gupta M, Bogdanowicz R, Lin I N, Kanjilal A, Haenen K, Roy S S 2019 J. Phys. Chem. C 123 15458 Google Scholar
[32]	Zhai Z, Leng B, Yang N, Yang B, Liu L, Huang N, Jiang X 2019 Small 15 1901527 Google Scholar
[33]	Zhou M, Zhai Z, Liu L, Zhang C, Yuan Z, Lu Z, Chen B, Shi D, Yang B, Wei Q, Huang N, Jiang X 2021 Appl. Surf. Sci. 551 149418 Google Scholar
[34]	Jiang M Y, Ma W C, Han S J, Chen C K, Fan D, Li X, Hu X J 2020 J. Appl. Phys. 127 015301 Google Scholar
[35]	Jiang M Y, Zhang Z Q, Chen C K, Ma W C, Han S J, Li X, Lu S H, Hu X J 2020 Carbon 168 536 Google Scholar
[36]	Jiang M Y, Chen C K, Wang P, Guo D F, Han S J, Li X, Lu S H, Hu X J. 2022 PNAS 119 2201451119 Google Scholar
[37]	Chen C K, Fan D, Xu H J, Jiang M Y, Li X, Lu S H, Ke C C, Hu X J. 2022 Carbon 196 466 Google Scholar
[38]	胡晓君, 仰宗春 2015 中国专利 ZL 201510149374.4 [2017-04-12] Hu X J, Yang Z C 2015 Chin. Patent ZL 201510149374.4 [2017-04-12]
[39]	Klauser F, Steinmüller Nethl D, Kaindl R, Bertel E, Memmel N 2010 Chem. Vap. Deposition 16 127 Google Scholar
[40]	Malard L M, Pimenta M A, Dresselhaus G, Dresselhaus M S 2009 Phys. Rep. 473 51 Google Scholar
[41]	Cançado L G, Jorio A, Ferreira E H M, Stavale F, Achete C A, Capaz R B, Moutinho M V O, Lombardo A, Kulmala T S, Ferrari A C 2011 Nano Lett. 11 3190 Google Scholar
[42]	Shimada T, Sugai T, Fantini C, Souza M, Cançado L G, Jorio A, Pimenta M A, Saito R, Grüneis A, Dresselhaus G, Dresselhaus M S, Ohno Y, Mizutani T, Shinohara H 2005 Carbon 43 1049 Google Scholar
[43]	Ferrari A C, Robertson J. Resonant 2001 Phys. Rev. B 64 075414 Google Scholar
[44]	Vora H, Moravec T J 1981 J. Appl. Phys. 52 6151 Google Scholar
[45]	Konyashin I, Frost D J, Sidorenko D, Orekhov A, Obraztsova E A, Sviridova T A 2020 Diamond Relat. Mater. 109 108017 Google Scholar

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Vol. 71, Issue 19 - 2022-10-05

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