Abstract
To develop low-power, non-volatile computing-in-memory device using ferroelectric transistor technologies, ferroelectric channel materials with scaled thicknesses are required. Two-dimensional semiconductors, such as molybdenum disulfide (MoS2), equipped with sliding ferroelectricity could provide an answer. However, achieving switchable electric polarization in epitaxial MoS2 remains challenging due to the absence of mobile domain boundaries. Here we show that polarity-switchable epitaxial rhombohedral-stacked (3R) MoS2 can be used as a ferroelectric channel in ferroelectric memory transistors. We show that a shear transformation can spontaneously occur in 3R MoS2 epilayers, producing heterostructures with stable ferroelectric domains embedded in a highly dislocated and unstable non-ferroelectric matrix. This diffusionless phase transformation process produces mobile screw dislocations that enable collective polarity control of 3R MoS2 via an electric field. Polarization–electric-field measurements reveal a switching field of 0.036 V nm−1 for shear-transformed 3R MoS2. Our sliding ferroelectric transistors are non-volatile memory units with thicknesses of only two atomic layers and exhibit an average memory window of 7 V with an applied voltage of 10 V, retention times greater than 104 seconds and endurance greater than 104 cycles.
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Acknowledgements
This work was supported by the National Science and Technology Council (NSTC) of Taiwan through grant 111-2124-M-003-005 (Y.-W.L.), 111-2119-M-008-003-MBK (Y.-W.L.), 110-2634-F-009-027 (C.-L.L.), 110-2112-M-A49-013-MY3 (C.-L.L.) and 110-2112-M-A49-022-MY2 (C.-L.L.). Y.-W.L. thanks the Taiwan Consortium of Emergent Crystalline Materials (TCECM) for its financial support. C.-L.L. thanks the Center for Semiconductor Technology Research (CSTR) for its financial support (the CSTR is from The Featured Areas Research Center Program within the framework of the Higher Education Sprout Project by the Ministry of Education (MOE) in Taiwan). T.H.Y. thanks C. R. Kao at Materials Science and Engineering, National Taiwan University, for his insightful comments on dislocation analyses and the phase transformation model. We thank Y.-M. Chang in The Instrumentation Center at National Tsing Hua University for her skilled TEM operation. We are grateful for technical support on SPEM data acquisition from Y.-C. Kuo, S.-H. Hsieh and C.-H. Chen at National Synchrotron Radiation Research Center (NSRRC) and K.-H. O. Yang at National Taiwan University.
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Contributions
T.H.Y. and B.-W.L. contributed equally to this work. T.H.Y. and Y.-W.L. conceived the idea and devised the project. H.-C.H. and Yi-Cheng Chen conducted the material growth. L.Y. and M.W. performed the DFT simulation to deduce the sliding mechanism. T.H.Y., H.-C.H., W.-H.C., H.-C.L. and Y.-C. Chang prepared samples for material characterizations. F.-X.C. and Y.-H.K. performed the scanning tunnelling microscope spectroscopy analysis and the cycling I–V measurement. S.-Z.H. and Yi-Chun Chen conducted PFM investigations and analysed the data. P.-Y.L. conducted the HRTEM and SADP investigation. T.H.Y. did the dislocation analysis and verified the formation and sliding mechanisms of domain boundaries. T.H.Y., H.-C.L. and W.-H.C. designed and fabricated MISM capacitors and FETs. T.H.Y., B.-W.L. and T.-H.K. performed the field-effect measurements. Y.-J.H. supported the FET fabrication and data analysis. T.H.Y., B.-W.L., T.-H.K. and J.-H.C. conducted the P–E measurements, and K.-S.L. examined the validity and interpretation of the results. T.H.Y. and B.-W.L. performed the PUND measurements, and Z.-F.L. and M.-H.L. assisted with the data analysis and interpretation. T.H.Y. and Y.-S.K. did the Wulff net simulation. T.H.Y., H.-C.H., Y.-F.C. and T.-H.L. performed the Raman and PL analyses. T.H.Y. and H.-C.H. conducted the SPEM investigation. H.-C.H. and A.C.C. conducted the AFM analyses. The manuscript was written by T.H.Y., B.-W.L., H.-C.H., K.B.S. and F.-X.C. with detailed discussion with all authors and was revised by C.-L.L., M.W. and Y.-W.L. The overall project was supervised by Y.-W.L.
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Extended data
Extended Data Fig. 1 Controllable synthesis of ST-3R MoS2 epilayers.
a, CVD setup for ST-3R MoS2 synthesis. A two-step CVD synthesis was performed at 800 °C for 3 min and 670 °C for 17 min, respectively. The higher temperature selected for the first step was to intensively vaporize MoO3, which was subsequently brought to the growth substrate by an Ar carrier gas. An additional SiO2/Si substrate was placed in front of the MoO3 powders for gas flow modulation. b, Clarification of the growth conditions for ST-3R MoS2 epilayers by changing temperatures and duration times of the MoO3 zone. The MoS2 flakes produced with different thermal histories, denoted in different color lines, are shown in (c-f). c, ST-3R bilayer MoS2 flakes via a two-step synthesis: 800 °C for 3 min (1st step) and 670 °C for 17 min (2nd step). Scale bar, 20 µm. d, Monolayer MoS2 via a two-step synthesis: 800 °C for 2 min (1st step) and 670 °C for 17 min (2nd step). The Mo amount in this condition is insufficient to promote vertical growth. e, Concentric growth of 3R MoS2 epilayers via a one-step synthesis at 800 °C for 20 min, showing 3R MoS2 flakes commonly observed in CVD synthesis. f, Nucleation of MoS2 does not take place via a one-step synthesis at 670 °C for 20 min. Scale bars in (d-f), 10 µm. The results of (c-f) suggest that the first duration mainly determined the Mo supply for MoS2 growth at 800 °C. However, the growth under the continuous Mo supply at 800 °C led to ordinary concentric-bilayer MoS2. A confined Mo amount and relatively low temperature is a key condition for the ST-3R bilayer MoS2 growth. g, Optical micrographs showing morphological evolutions of ST-3R MoS2 bilayers grown on SiO2/Si substrates with the increasing duration time at 670 °C. The bottom panel illustrates the corresponding growth stages. The epilayer growth can be divided into three stages: (1) formation of six primary dendrites with the preferred orientations along the armchair directions, (2) formation of multiple secondary dendrites based on the primary dendrites, and (3) coalescence of parallelly-oriented dendrites to form a merged epilayer triangle. Scale bars, 20 μm. i, AFM topography image of the marked bilayer region in the optical micrograph (h) of an ST-3R MoS2 flake, showing a monolayer step height of about 0.7 nm for the epitaxial nanoribbons. Scale bar, 10 μm.
Extended Data Fig. 2 Growth mechanism of ST-3R MoS2 homoepitaxy.
a, Polar plots of the formation energies of MoS2 edges as a function of chiral angle χ (0° ≤ χ ≤ 360°) under a Mo-deficient environment. The interior red triangle represents the final equilibrium shape of a MoS2 epilayer. The 0° corresponds to the armchair direction. b, Schematic of surface and edge diffusion for a MoS3 monomer on 1H-MoS2 surface. The stacking configuration between the 2nd layer and the underlying MoS2 layer is 3R stacking. The enlarged illustration shows possible migration pathways of a MoS3 monomer adsorbed on top of the Mo site, where the black dashed arrows denote the hopping paths for every single hopping event while the red solid arrows are the effective paths of two consecutive hopping events which possess the equivalent vectors parallel to the \(\langle \bar{1}\,2\,\bar{1}\,0\rangle\) (armchair) directions. TMo, the top site of Mo atoms from the 1st layer. H, the hollow site. c, Arrhenius relation of the hopping rates of a MoS3 monomer for the surface and edge diffusion. d, Tuning dimensionality of bilayer nanoribbons by changing the 2nd (tempering) temperature, as denoted by black dashed lines in (c), clearly showing that the bilayer ribbons became thinner with decreasing the temperature. The observed behavior is reasonable since the decrease in growth temperature increased the difference in the diffusion rates between surface diffusion and edge diffusion. The more limited the ability of edge relaxation is, the higher the degree of fractal growth and the thinner the bilayer ribbons turn out.
Extended Data Fig. 3 Shear-transformation-induced 3R polytypic domains and domain boundaries.
a, b, Extended dark-field (top) and bright-field (bottom) TEM images taken with the \((1\,0\,\bar{1}\,0)\) diffraction spot, revealing AB and BA lamellae in the AA-matrix. All the lamellar domains show the preferred orientation along the zigzag directions, which is roughly perpendicular to the growth direction of bilayer nanoribbons. Scale bars, 100 nm. c, Schematic of AB and BA stacking faults forming in the instable AA matrix, where the domain boundaries constitute a pair of Shockley partial dislocations (SPD) with \(\mathop{{b}}\limits^{{\rightharpoonup }}\parallel \langle 10\bar{1}0\rangle\) that is decomposed from a basal dislocation \(\mathop{{b}}\limits^{{\rightharpoonup }}\parallel \langle \bar{1}\,2\,\bar{1}\,0\rangle\). ML refers to monolayer, while BL to bilayer. d, A diffraction pattern from the ST-3R bilayer nanoribbon shown in (e). e, Tilted dark-field TEM image obtained by filtering the \((10\bar{1}0)\) diffraction spot of MoS2, where a BA lamella is embedded in an AA matrix. f, g, Dark-field TEM images from the same region in (e), taken with \({\mathop{{g}}\limits^{{\rightharpoonup }}}_{1}=(2\bar{1}\bar{1}0)\) and \({\mathop{{g}}\limits^{{\rightharpoonup }}}_{2}=(1\,\bar{2}\,1\,0)\) diffraction spots denoted in (d), respectively. Based on the criterion \(\mathop{g}\limits^{\rightharpoonup }\cdot \mathop{b}\limits^{\rightharpoonup }=0\) that is satisfied to make dislocations disappear, the domain boundary \({\mathop{{b}}\limits^{{\rightharpoonup }}}_{1}\) disappears with \({\mathop{{g}}\limits^{{\rightharpoonup }}}_{1}=(2\bar{1}\bar{1}0)\) while the domain boundary \({\mathop{{b}}\limits^{{\rightharpoonup }}}_{2}\) disappears with \({\mathop{g}\limits^{\rightharpoonup }}_{2}=(1\bar{2}10)\). This suggests that BA-AA domain boundaries constitute a pair of Shockley partial dislocations with \(\mathop{b}\limits^{\rightharpoonup }\parallel \langle 10\bar{1}0\rangle\), and the resultant BA domain is a Shockley stacking fault forming in the AA matrix. Scale bars, 20 nm.
Extended Data Fig. 4 Extended STEM-ADF image analysis of shear-transformation-induced 3R domain boundaries.
a, b, STEM-ADF images taken from two neighboring regions in a 3R nanoribbon, showing a BA-AA domain boundary. (M: moiré-like transition zone. PSD: partial screw dislocation). The Burgers vectors of the M zone and the PSD site are parallel to the\(\langle 10\bar{1}0\rangle\) direction. Scale bars, 2 nm. c, Enlarged image showing the transition of atomic-stacking configuration between the AA and BA domains in (b). Scale bar, 1 nm. d, e, STEM-ADF images taken from the regions far from the domain boundary shown in (b). No noticeable lattice misalignment is found in the separated domains. Scale bars, 2 nm.
Extended Data Fig. 5 Diffraction patterns and STEM-ADF images of different 3R stacking domains.
a–c, SADPs taken from monolayer, AB-stacking bilayer, and AA-stacking bilayer regions, respectively. The corresponding intensity profiles were extracted along the white dashed square in each SADP image of (a-c), which are consistent with simulated SADPs of 3R stacking polytypes by Kim et al. (Ref. 21). d, e, STEM-ADF images showing atomic arrangements of AB and BA domains, respectively. Scale bars, 2 nm. f, g, Intensity profiles extracted from the red and purple dashed squares in the bilayer and monolayer regions in (d,e).
Extended Data Fig. 6 Evolution of experimental P-E loops of ST-3R MoS2 capacitor and mathematical modeling.
a, P-E loops of the ST-3R MoS2 capacitor at increasing \({{\rm{E}}}_{{{\rm{MoS}}}_{2}}\) ranges, from 0.027 V nm−1 to 0.217 V nm−1. \({{\rm{E}}}_{{{\rm{MoS}}}_{2}}\) is the effective field across the ST-3R MoS2 layer (Supplementary Note 3). b, The experimental and simulated P-E loops, from the corrected Miller et al. model, at \({{\rm{E}}}_{{{\rm{MoS}}}_{2}}\) = 0.109 V nm−1. To consider the asymmetric polarization switching due to the different top and bottom interfacial structures of the ST-3R MoS2 capacitor (top: hBN/MoS2, bottom: graphene/MoS2), the corrected Miller model is used to simulate the P-E loops4,5. c, The experimental data and corrected Miller model estimation of the P-E loops at \({{\rm{E}}}_{{{\rm{MoS}}}_{2}}\) = 0.217 V nm−1. d, Electric-field dependence of 2Ps and 2Pr, extracted from a.
Extended Data Fig. 7 Temperature-dependent electrical measurements of ST-3R MoS2 FETs.
The SiO2 dielectric thickness for the FETs presented is 300 nm. The applied E fields (defined by applied voltages/the SiO2 thickness) range from 0.033–0.33 V nm−1, which is quantitatively close to that used for the FETs with the 30 nm-thick SiO2 dielectric. a, Transfer characteristics at |VDS|=1 V at increasing VGS sweep ranges, from ±10 V to ±100 V, measured in vacuum and at 298 K. b, Temperature-dependent transfer characteristics at |VDS|=1 V at VGS range of ±100 V. c, The temperature-dependent changes of the Ion/Ioff ratio and the memory window (VMW).
Extended Data Fig. 8 Concerns of long-term retention arising from charge trapping.
Retention of the program and erase currents of an ST-3R MoS2 FET with floating gate at |VDS|=1 V, for a, an as-fabricated device measured in ambient conditions, b, a vacuum-annealed device measured in ambient conditions, and c, a vacuum-annealed device measured in an N2 atmosphere, respectively. The annealing was conducted at 100 °C for 30 min. Gate pulses of 10 V and −10 V at 1 s were used for the program and erase operations, respectively.
Extended Data Fig. 9 Statistical analysis on memory performance of ST-3R MoS2 FETs.
a, The dual-sweep IDS-VGS transfer curves repeated for 50 cycles from an ST-3R MoS2 FET device. Cumulative distribution of (b) VMV and (c) the on/off ratio of 50 ST-3R MoS2 FET devices. The bias conditions, |VDS| = 1 V and VGS range = ±10 V, are used to ensure that the FETs reach a maximum VMV and a maximum Ion/Ioff ratio between the program and erase states. The distribution in each graph is fitted with a normal curve. The statistical distribution shows that VMV is around 7 V, and the highest value can reach around 8–9 V. The on-off current ratio between the program and erase states is about 104 and with an average of 6.10 × 103.
Supplementary information
Supplementary Information
Supplementary Notes 1–6, Figs. 1–14 and Tables 1–3.
Source data
Source Data Fig. 1
Fig. 1a reaction path data.
Source Data Fig. 2
Fig. 2a–c, e–g raw data.
Source Data Fig. 3
Fig. 3b–f, raw data.
Source Data Extended Data Fig. 1
Extended Data Fig. 1h AFM raw data.
Source Data Extended Data Fig. 6
Extended Data Fig. 6a, PE loops; Fig, 6b, PE simulation; Fig. 6c, PE simulation; Fig. 6d, Ps Pr E.
Source Data Extended Data Fig. 7
Extended Data Fig. 7a, I–V curves; Fig. 7b I–V T curves; Fig. 7c, VMV and on/off ratio; Fig. 7c, analysis raw data.
Source Data Extended Data Fig. 8
Extended Data Fig. 8a, Retention; Fig. 8b, Retention; Fig. 8c, Retention.
Source Data Extended Data Fig. 9
Extended Data Fig. 9a, 50 cycles; Fig. 9b, 50 VMV; Fig. 9c, 50 on/off ratio; Fig. 9c, I–V curves.
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Yang, T.H., Liang, BW., Hu, HC. et al. Ferroelectric transistors based on shear-transformation-mediated rhombohedral-stacked molybdenum disulfide. Nat Electron 7, 29–38 (2024). https://doi.org/10.1038/s41928-023-01073-0
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DOI: https://doi.org/10.1038/s41928-023-01073-0
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