Interlocked MXene/rGO aerogel with excellent mechanical stability for a health-monitoring device

Shufang Zhao; Wenhao Ran; Lili Wang; Guozhen Shen

doi:10.1088/1674-4926/43/8/082601

J. Semicond. > 2022, Volume 43?>?Issue 8?> 082601

ARTICLES

Interlocked MXene/rGO aerogel with excellent mechanical stability for a health-monitoring device

Shufang Zhao^{1, 2}, Wenhao Ran^{1, 2}, Lili Wang^{1, 2,} and Guozhen Shen^{1, 2, 3,}

+ Author Affiliations

1. State Key Laboratory for Superlattices and Microstructures, Institute of Semiconductors, Chinese Academy of Sciences, Beijing 100083, China
2. Center of Materials Science and Optoelectronic Engineering, University of Chinese Academy of Sciences, Beijing 100083, China
3. School of Integrated Circuits and Electronics, Beijing Institute of Technology, Beijing 100081, China

Author Bio:

Shufang Zhao is currently a Ph.D. candidate at the Institute of Semiconductors, Chinese Academy of Sciences. Her current scientific interests focus on the design and manufacture of flexible electronic skin and artificial nerve synapses, and investigation of their fundamental properties.

Wenhao Ran is currently a Ph.D. candidate at the Institute of Semiconductors, Chinese Academy of Sciences. His current scientific interests focus on the design and preparation of low- dimensional materials and their fundamental properties.

Lili Wang is a professor in the Institute of Semiconductors, Chinese Academy of Sciences, China. She earned her B.Sc. (2010) in chemistry and Ph.D. degree in microelectronics and solid state electronics from the Jilin University in 2014. Her current research interests focus on the flexible electronics based on biological materials, 2D materials and semiconductor, including pressure sensors, electronic-skin, biosensor, photodetectors and flexible energy storage and conversion devices.

Guozhen Shen received his B.Sc. degree (1999) in chemistry from Anhui Normal University and Ph.D. degree (2003) in chemistry from the University of Science and technology of China. He joined the Institute of Semiconductors, Chinese Academy of Sciences, as a Professor in 2013. He has published more than 200 papers with a publication H-factor of 57. His current research focuses on flexible electronics and printable electronics, including transistors, photodetectors, sensors and flexible energy storage and conversion devices.

Corresponding author: Lili Wang, liliwang@semi.ac.cn; Guozhen Shen, gzshen@bit.edu.cn

DOI: 10.1088/1674-4926/43/8/082601

Abstract: Two-dimensional (2D) materials have attracted considerable interest thanks to their unique electronic/physical–chemical characteristics and their potential for use in a large variety of sensing applications. However, few-layered nanosheets tend to agglomerate owing to van der Waals forces, which obstruct internal nanoscale transport channels, resulting in low electrochemical activity and restricting their use for sensing purposes. Here, a hybrid MXene/rGO aerogel with a three-dimensional (3D) interlocked network was fabricated via a freeze-drying method. The porous MXene/rGO aerogel has a lightweight and hierarchical porous architecture, which can be compressed and expanded several times without breaking. Additionally, a flexible pressure sensor that uses the aerogel as the sensitive layer has a wide response range of approximately 0–40 kPa and a considerable response within this range, averaging approximately 61.49 kPa^–1. The excellent sensing performance endows it with a broad range of applications, including human-computer interfaces and human health monitoring.

Key words: flexible electronic, MXene/rGO, interlocking structure, high performance, healthcare monitoring

References

[1]	Cao M, Su J, Fan S, et al. Wearable piezoresistive pressure sensors based on 3D graphene. Chem Eng J, 2021, 406, 126777 doi: 10.1016/j.cej.2020.126777
[2]	Jin X, Li L, Zhao S, et al. Assessment of occlusal force and local gas release using degradable bacterial cellulose/Ti₃C₂T_x MXene bioaerogel for oral healthcare. ACS Nano, 2021, 15, 18385 doi: 10.1021/acsnano.1c07891
[3]	Wang L, Chen S, Li W, et al. Grain-boundary-induced drastic sensing performance enhancement of polycrystalline-microwire printed gas sensors. Adv Mater, 2019, 31, 1804583 doi: 10.1002/adma.201804583
[4]	Wu J, Huang D, Ye Y, et al. Theoretical study of a group IV p–i–n photodetector with a flat and broad response for visible and infrared detection. J Semicond, 2020, 41, 122402 doi: 10.1088/1674-4926/41/12/122402
[5]	Zhong B, Jiang K, Wang L, et al. Wearable sweat loss measuring devices: From the role of sweat loss to advanced mechanisms and designs. Adv Sci, 2022, 9, 2103257 doi: 10.1002/advs.202103257
[6]	Geng R, Gong Y. High performance active image sensor pixel design with circular structure oxide TFT. J Semicond, 2019, 40, 022402 doi: 10.1088/1674-4926/40/2/022402
[7]	Zhao S, Ran W, Wang D, et al. 3D dielectric layer enabled highly sensitive capacitive pressure sensors for wearable electronics. ACS Appl Mater Interfaces, 2020, 12, 32023 doi: 10.1021/acsami.0c09893
[8]	Mak P I. Lab-on-COS-an in-vitro diagnostic (IVD) tool for a healthier society. J Semicond, 2020, 41, 110301 doi: 10.1088/1674-4926/41/11/110301
[9]	Zhang Z, Chen C, Fei T, et al. Wireless communication and wireless power transfer system for implantable medical device. J Semicond, 2020, 41, 102403 doi: 10.1088/1674-4926/41/10/102403
[10]	Chen T, Zhang S H, Lin Q H, et al. Highly sensitive and wide-detection range pressure sensor constructed on a hierarchical-structured conductive fabric as a human-machine interface. Nanoscale, 2020, 12, 21271 doi: 10.1039/D0NR05976E
[11]	Wang L, Jiang K, Shen G. A perspective on flexible sensors in developing diagnostic devices. Appl Phys Lett, 2022, 119, 150501 doi: 10.1063/5.0057020
[12]	Li L, Wang D, Zhang D, et al. Near-infrared light triggered self-powered mechano-optical communication system using wearable photodetector textile. Adv Funct Mater, 2021, 31, 2104782 doi: 10.1002/adfm.202104782
[13]	Kang K, Jung H, An S, et al. Skin-like transparent polymer-hydrogel hybrid pressure sensor with pyramid microstructures. Polymers, 2021, 13, 3272 doi: 10.3390/polym13193272
[14]	Qi K, Zhou Y, Ou K, et al. Weavable and stretchable piezoresistive carbon nanotubes-embedded nanofiber sensing yarns for highly sensitive and multimodal wearable textile sensor. Carbon, 2020, 170, 464 doi: 10.1016/j.carbon.2020.07.042
[15]	Wang G, Wang Z, Wu Y, et al. A robust stretchable pressure sensor for electronic skins. Org Electron, 2020, 86, 105926 doi: 10.1016/j.orgel.2020.105926
[16]	Torad N L, Ding B, El-Said WA, et al. Mof-derived hybrid nanoarchitectured carbons for gas discrimination of volatile aromatic hydrocarbons. Carbon, 2020, 168, 55 doi: 10.1016/j.carbon.2020.05.013
[17]	Bai H, Li C, Shi G. Functional composite materials based on chemically converted graphene. Adv Mater, 2011, 23, 1089 doi: 10.1002/adma.201003753
[18]	Sun J, Du S. Application of graphene derivatives and their nanocomposites in tribology and lubrication: A review. RSC Adv, 2019, 9, 40642 doi: 10.1039/C9RA05679C
[19]	Pan H. Ultra-high electrochemical catalytic activity of MXenes. Sci Rep, 2016, 6, 32531 doi: 10.1038/srep32531
[20]	Zhao L, Wang Z, Li Y, et al. Designed synthesis of chlorine and nitrogen co-doped Ti₃C₂ MXene quantum dots and their outstanding hydroxyl radical scavenging properties. J Mater Sci Technol, 2021, 78, 30 doi: 10.1016/j.jmst.2020.10.048
[21]	Kamath K, Adepu V, Mattela V, et al. Development of Ti₃C₂T_x/MoS_{2 x}Se_{2(1– x)} nanohybrid multilayer structures for piezoresistive mechanical transduction. ACS Appl Electron Mater, 2021, 3, 4091 doi: 10.1021/acsaelm.1c00583
[22]	Sun J, Du H, Chen Z, et al. MXene quantum dot within natural 3D watermelon peel matrix for biocompatible flexible sensing platform. Nano Res, 2022, 15, 3653 doi: 10.1007/s12274-021-3967-x
[23]	Gong S, Schwalb W, Wang Y, et al. A wearable and highly sensitive pressure sensor with ultrathin gold nanowires. Nat Commun, 2014, 5, 3132 doi: 10.1038/ncomms4132
[24]	Ma Y, Yue Y, Zhang H, et al. 3D synergistical MXene/reduced graphene oxide aerogel for a piezoresistive sensor. ACS Nano, 2018, 12, 3209 doi: 10.1021/acsnano.7b06909
[25]	Tian Y, Han J, Yang J, et al. A highly sensitive graphene aerogel pressure sensor inspired by fluffy spider leg. Adv Mater Interfaces, 2021, 8, 2100511 doi: 10.1002/admi.202100511
[26]	Wang L, Zhang M, Yang B, et al. Thermally stable, light-weight, and robust aramid nanofibers/Ti₃AlC₂ MXene composite aerogel for sensitive pressure sensor. ACS Nano, 2020, 8, 10633 doi: 10.1021/acsnano.0c04888
[27]	Zhai J, Zhang Y, Cui C, et al. Flexible waterborne polyurethane/cellulose nanocrystal composite aerogels by integrating graphene and carbon nanotubes for a highly sensitive pressure sensor. ACS Sustain Chem Eng, 2021, 9, 14029 doi: 10.1021/acssuschemeng.1c03068
[28]	Wei S, Qiu X, An J, et al. Highly sensitive, flexible, green synthesized graphene/biomass aerogels for pressure sensing application. Compos Sci Technol, 2021, 7, 20,108730 doi: 10.1016/j.compscitech.2021.108730
[29]	Xu Q, X Chang, Zhu Z, et al. Flexible pressure sensors with high pressure sensitivity and low detection limit using a unique honeycomb-designed polyimide/reduced graphene oxide composite aerogel. RSC Adv, 2021, 11, 11760 doi: 10.1039/D0RA10929K
[30]	Wang D, Wang L, Shen G. Nanofiber/nanowires-based flexible and stretchable sensors. J Semicond, 2020, 41, 041605 doi: 10.1088/1674-4926/41/4/041605
[31]	Wei S J. Reconfigurable computing: a promising microchip architecture for artificial intelligence. J Semicond, 2020, 41, 020301 doi: 10.1088/1674-4926/41/2/020301
[32]	Wang K, Lou Z, Wang L, et al. Bioinspired interlocked structure-induced high deformability for two-dimensional titanium carbide (MXene)/natural microcapsule-based flexible pressure sensors. ACS Nano, 2019, 13, 9139 doi: 10.1021/acsnano.9b03454
[33]	Dong K, Wang Z L. Self-charging power textiles integrating energy harvesting triboelectric nanogenerators with energy storage batteries/supercapacitors. J Semicond, 2021, 42, 101601 doi: 10.1088/1674-4926/42/10/101601

Fig. 1. (Color online) The characterization of the interlocked MXene/rGO aerogel composite. (a) Schematic illustration of the fabrication procedure of interlocked MXene/rGO aerogel. SEM images of interlocked MXene/rGO aerogel: (b) high magnification and (c) low magnification. (d) Optical image of interlocked MXene/rGO aerogel with lightweight feature placed on the dandelion. (e) Compressive stress-strain curves of the interlocked MXene/rGO aerogel at 12% strain under different cycles. (f) Structure change of interlocked MXene/rGO aerogel during the compression process and (g) the corresponding illustration of current change.

DownLoad: Full-Size Img PowerPoint

Fig. 2. (Color online) The sensing performance of the interlocked MXene/rGO aerogel-based pressure sensor. (a) Illustration of flexible pressure sensor. (b) The I–V curves of the flexible sensor. (c) Dynamic measurement of the sensor response with increased pressure from 0 to 1.1 kPa. (d) Sensitivity curves. Inset show the comparison of sensing properties of MXene/rGO aerogel and flat aerogel. (e) Current responses to loading/unloading 5.5 kPa on the sensor. The inserts give response time and recovery time of the sensor.

DownLoad: Full-Size Img PowerPoint

Fig. 3. (Color online) Sensing-performance of the interlocked MXene/rGO aerogel-based pressure sensor at different bending states. (a) The I–T curve with the bending angle increased from 30° to 90°. (b) The real-time I–T curve of the sensor in the 90° repeated bending-straightening process. (c) Response and recovery time under different cycles. (d) The bending stability test of the sensor under bending and releasing state.

DownLoad: Full-Size Img PowerPoint

Fig. 4. (Color online) MXene/rGO aerogel-based pressure sensor as a wearable device for health monitoring. (a) The pressure-sensitive response to the bending motion of a forefinger (inset: photograph of the device fastened to back of a forefinger with different bending angles). (b) Three cycles of bending the finger at 90°. (c) Human pulse (inset: photograph of the device placed onto a wrist). (d) The enlarged waveform of one of the pulses in (c).

DownLoad: Full-Size Img PowerPoint

Table 1. Comparison of pressure sensor performance.

Device	Sensitivity (kPa^–1)	Pressure range (kPa)	τ_rise (ms)	Τ_decay (ms)	Ref.
MXene/rGO	61.49	0–40	68	40	Our work
MXene/ANFs	6.75	–	320	98	[26]
Carbon nanotubes (CNTs)/graphene/waterborne polyurethane (WPU)/ cellulose nanocrystal (CNC) composite aerogels (CNTs/graphene/WC)	0.25	0.112–10	120		[27]
MXene/reduced graphene oxide (MX/rGO)	22.56	0.115–0.97	243	231	[24]
Graphene/biomass aerogels	13.89	<12	120	840	[28]
Polyimide (PI)/reduced graphene oxide (rGO) aerogel	1.33	<20	60	70	[29]

DownLoad: CSV

[1]	Cao M, Su J, Fan S, et al. Wearable piezoresistive pressure sensors based on 3D graphene. Chem Eng J, 2021, 406, 126777 doi: 10.1016/j.cej.2020.126777
[2]	Jin X, Li L, Zhao S, et al. Assessment of occlusal force and local gas release using degradable bacterial cellulose/Ti₃C₂T_x MXene bioaerogel for oral healthcare. ACS Nano, 2021, 15, 18385 doi: 10.1021/acsnano.1c07891
[3]	Wang L, Chen S, Li W, et al. Grain-boundary-induced drastic sensing performance enhancement of polycrystalline-microwire printed gas sensors. Adv Mater, 2019, 31, 1804583 doi: 10.1002/adma.201804583
[4]	Wu J, Huang D, Ye Y, et al. Theoretical study of a group IV p–i–n photodetector with a flat and broad response for visible and infrared detection. J Semicond, 2020, 41, 122402 doi: 10.1088/1674-4926/41/12/122402
[5]	Zhong B, Jiang K, Wang L, et al. Wearable sweat loss measuring devices: From the role of sweat loss to advanced mechanisms and designs. Adv Sci, 2022, 9, 2103257 doi: 10.1002/advs.202103257
[6]	Geng R, Gong Y. High performance active image sensor pixel design with circular structure oxide TFT. J Semicond, 2019, 40, 022402 doi: 10.1088/1674-4926/40/2/022402
[7]	Zhao S, Ran W, Wang D, et al. 3D dielectric layer enabled highly sensitive capacitive pressure sensors for wearable electronics. ACS Appl Mater Interfaces, 2020, 12, 32023 doi: 10.1021/acsami.0c09893
[8]	Mak P I. Lab-on-COS-an in-vitro diagnostic (IVD) tool for a healthier society. J Semicond, 2020, 41, 110301 doi: 10.1088/1674-4926/41/11/110301
[9]	Zhang Z, Chen C, Fei T, et al. Wireless communication and wireless power transfer system for implantable medical device. J Semicond, 2020, 41, 102403 doi: 10.1088/1674-4926/41/10/102403
[10]	Chen T, Zhang S H, Lin Q H, et al. Highly sensitive and wide-detection range pressure sensor constructed on a hierarchical-structured conductive fabric as a human-machine interface. Nanoscale, 2020, 12, 21271 doi: 10.1039/D0NR05976E
[11]	Wang L, Jiang K, Shen G. A perspective on flexible sensors in developing diagnostic devices. Appl Phys Lett, 2022, 119, 150501 doi: 10.1063/5.0057020
[12]	Li L, Wang D, Zhang D, et al. Near-infrared light triggered self-powered mechano-optical communication system using wearable photodetector textile. Adv Funct Mater, 2021, 31, 2104782 doi: 10.1002/adfm.202104782
[13]	Kang K, Jung H, An S, et al. Skin-like transparent polymer-hydrogel hybrid pressure sensor with pyramid microstructures. Polymers, 2021, 13, 3272 doi: 10.3390/polym13193272
[14]	Qi K, Zhou Y, Ou K, et al. Weavable and stretchable piezoresistive carbon nanotubes-embedded nanofiber sensing yarns for highly sensitive and multimodal wearable textile sensor. Carbon, 2020, 170, 464 doi: 10.1016/j.carbon.2020.07.042
[15]	Wang G, Wang Z, Wu Y, et al. A robust stretchable pressure sensor for electronic skins. Org Electron, 2020, 86, 105926 doi: 10.1016/j.orgel.2020.105926
[16]	Torad N L, Ding B, El-Said WA, et al. Mof-derived hybrid nanoarchitectured carbons for gas discrimination of volatile aromatic hydrocarbons. Carbon, 2020, 168, 55 doi: 10.1016/j.carbon.2020.05.013
[17]	Bai H, Li C, Shi G. Functional composite materials based on chemically converted graphene. Adv Mater, 2011, 23, 1089 doi: 10.1002/adma.201003753
[18]	Sun J, Du S. Application of graphene derivatives and their nanocomposites in tribology and lubrication: A review. RSC Adv, 2019, 9, 40642 doi: 10.1039/C9RA05679C
[19]	Pan H. Ultra-high electrochemical catalytic activity of MXenes. Sci Rep, 2016, 6, 32531 doi: 10.1038/srep32531
[20]	Zhao L, Wang Z, Li Y, et al. Designed synthesis of chlorine and nitrogen co-doped Ti₃C₂ MXene quantum dots and their outstanding hydroxyl radical scavenging properties. J Mater Sci Technol, 2021, 78, 30 doi: 10.1016/j.jmst.2020.10.048
[21]	Kamath K, Adepu V, Mattela V, et al. Development of Ti₃C₂T_x/MoS_{2 x}Se_{2(1– x)} nanohybrid multilayer structures for piezoresistive mechanical transduction. ACS Appl Electron Mater, 2021, 3, 4091 doi: 10.1021/acsaelm.1c00583
[22]	Sun J, Du H, Chen Z, et al. MXene quantum dot within natural 3D watermelon peel matrix for biocompatible flexible sensing platform. Nano Res, 2022, 15, 3653 doi: 10.1007/s12274-021-3967-x
[23]	Gong S, Schwalb W, Wang Y, et al. A wearable and highly sensitive pressure sensor with ultrathin gold nanowires. Nat Commun, 2014, 5, 3132 doi: 10.1038/ncomms4132
[24]	Ma Y, Yue Y, Zhang H, et al. 3D synergistical MXene/reduced graphene oxide aerogel for a piezoresistive sensor. ACS Nano, 2018, 12, 3209 doi: 10.1021/acsnano.7b06909
[25]	Tian Y, Han J, Yang J, et al. A highly sensitive graphene aerogel pressure sensor inspired by fluffy spider leg. Adv Mater Interfaces, 2021, 8, 2100511 doi: 10.1002/admi.202100511
[26]	Wang L, Zhang M, Yang B, et al. Thermally stable, light-weight, and robust aramid nanofibers/Ti₃AlC₂ MXene composite aerogel for sensitive pressure sensor. ACS Nano, 2020, 8, 10633 doi: 10.1021/acsnano.0c04888
[27]	Zhai J, Zhang Y, Cui C, et al. Flexible waterborne polyurethane/cellulose nanocrystal composite aerogels by integrating graphene and carbon nanotubes for a highly sensitive pressure sensor. ACS Sustain Chem Eng, 2021, 9, 14029 doi: 10.1021/acssuschemeng.1c03068
[28]	Wei S, Qiu X, An J, et al. Highly sensitive, flexible, green synthesized graphene/biomass aerogels for pressure sensing application. Compos Sci Technol, 2021, 7, 20,108730 doi: 10.1016/j.compscitech.2021.108730
[29]	Xu Q, X Chang, Zhu Z, et al. Flexible pressure sensors with high pressure sensitivity and low detection limit using a unique honeycomb-designed polyimide/reduced graphene oxide composite aerogel. RSC Adv, 2021, 11, 11760 doi: 10.1039/D0RA10929K
[30]	Wang D, Wang L, Shen G. Nanofiber/nanowires-based flexible and stretchable sensors. J Semicond, 2020, 41, 041605 doi: 10.1088/1674-4926/41/4/041605
[31]	Wei S J. Reconfigurable computing: a promising microchip architecture for artificial intelligence. J Semicond, 2020, 41, 020301 doi: 10.1088/1674-4926/41/2/020301
[32]	Wang K, Lou Z, Wang L, et al. Bioinspired interlocked structure-induced high deformability for two-dimensional titanium carbide (MXene)/natural microcapsule-based flexible pressure sensors. ACS Nano, 2019, 13, 9139 doi: 10.1021/acsnano.9b03454
[33]	Dong K, Wang Z L. Self-charging power textiles integrating energy harvesting triboelectric nanogenerators with energy storage batteries/supercapacitors. J Semicond, 2021, 42, 101601 doi: 10.1088/1674-4926/42/10/101601

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Received: 14 January 2022 Revised: 09 March 2022 Online: Accepted Manuscript: 21 April 2022Uncorrected proof: 22 April 2022Corrected proof: 18 July 2022Published: 01 August 2022

Two-dimensional (2D) materials have attracted considerable interest thanks to their unique electronic/physical–chemical characteristics and their potential for use in a large variety of sensing applications. However, few-layered nanosheets tend to agglomerate owing to van der Waals forces, which obstruct internal nanoscale transport channels, resulting in low electrochemical activity and restricting their use for sensing purposes. Here, a hybrid MXene/rGO aerogel with a three-dimensional (3D) interlocked network was fabricated via a freeze-drying method. The porous MXene/rGO aerogel has a lightweight and hierarchical porous architecture, which can be compressed and expanded several times without breaking. Additionally, a flexible pressure sensor that uses the aerogel as the sensitive layer has a wide response range of approximately 0–40 kPa and a considerable response within this range, averaging approximately 61.49 kPa^–1. The excellent sensing performance endows it with a broad range of applications, including human-computer interfaces and human health monitoring.

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Interlocked MXene/rGO aerogel with excellent mechanical stability for a health-monitoring device

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