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Matthew S. G. Feuer, Alejandro R.-P. Montblanch, Mohammed Y. Sayyad, Carola M. Purser, Ying Qin, Evgeny M. Alexeev, Alisson R. Cadore, Barbara L. T. Rosa, James Kerfoot, Elaheh Mostaani, Radosław Kalȩba, Pranvera Kolari, Jan Kopaczek, [Kenji Watanabe](https://orcid.org/0000-0003-3701-8119), [Takashi Taniguchi](https://orcid.org/0000-0002-1467-3105), Andrea C. Ferrari, Dhiren M. Kara, Sefaattin Tongay, Mete Atatüre

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[Identification of Exciton Complexes in Charge-Tunable Janus W<sub>Se</sub><sup>S</sup> Monolayers](https://mdr.nims.go.jp/datasets/9696fc06-68d2-4fbe-85f9-90d54ddfcb76)

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Identification of Exciton Complexes in Charge-Tunable Janus WSeS MonolayersIdentification of Exciton Complexes in Charge-Tunable Janus WSeS MonolayersMatthew S. G. Feuer,# Alejandro R.-P. Montblanch,# Mohammed Y. Sayyad,# Carola M. Purser,Ying Qin, Evgeny M. Alexeev, Alisson R. Cadore, Barbara L. T. Rosa, James Kerfoot, Elaheh Mostaani,Radosław Kalȩba, Pranvera Kolari, Jan Kopaczek, Kenji Watanabe, Takashi Taniguchi, Andrea C. Ferrari,Dhiren M. Kara, Sefaattin Tongay,* and Mete Atatüre*Cite This: ACS Nano 2023, 17, 7326−7334 Read OnlineACCESS Metrics & More Article Recommendations *sı Supporting InformationABSTRACT: Janus transition-metal dichalcogenide monolayersare artificial materials, where one plane of chalcogen atoms isreplaced by chalcogen atoms of a different type. Theory predictsan in-built out-of-plane electric field, giving rise to long-lived,dipolar excitons, while preserving direct-bandgap optical tran-sitions in a uniform potential landscape. Previous Janus studieshad broad photoluminescence (>18 meV) spectra obfuscatingtheir specific excitonic origin. Here, we identify the neutral andthe negatively charged inter- and intravalley exciton transitions inJanus WSeS monolayers with ∼6 meV optical line widths. Weintegrate Janus monolayers into vertical heterostructures,allowing doping control. Magneto-optic measurements indicate that monolayer WSeS has a direct bandgap at the K points.Our results pave the way for applications such as nanoscale sensing, which relies on resolving excitonic energy shifts, and thedevelopment of Janus-based optoelectronic devices, which requires charge-state control and integration into verticalheterostructures.KEYWORDS: Janus transition-metal dichalcogenides, WSeS monolayers, 2D materials, layered materials, charge tunable, excitonsLayered materials are solids with strong intralayer bondsbut only weak van der Waals coupling between layers.1These materials have a range of electronic,2 optical,3,4,5and topological6 properties and can be combined in verticalheterostructures with pristine atomic interfaces, despitemismatched lattice parameters.7−9 Direct-bandgap semicon-ducting transition-metal dichalcogenide (TMD) monolayers(1Ls) are a class of layered material, which are particularlyinteresting due to their optoelectronic properties.10−5 Opticalexcitation creates excitons, i.e., bound electron−hole pairs, atthe K and K′ direct-bandgap edges,13,14 while the strong spin−orbit interaction and broken inversion symmetry leads tocoupling of spin and valley degrees of freedom.15 Hetero-structures comprising two different TMD monolayers can havea type-II band alignment,16,17 which localizes electrons in one1L and holes in the other.18 This charge separation results inexcitons with a permanent electric dipole moment19 and longlifetime (up to 0.2 ms),20 due to a reduced overlap of electronand hole wave functions.21 While such stacking configurationsenable tunability with layer angle and introduce emergentmoire ́ physics,22 they are also susceptible to an inhomogeneouspotential landscape due to spatial variations in layer separationand twist angle.23,24Janus TMDs (J-TMD) are a class of layered materials25 thatpromise Rashba splitting;26,27 piezoelectric response;28,29 andlong-lived, dipolar excitons30 in an intrinsically uniformpotential landscape. To form a Janus 1L, a conventional 1L-TMD, such as 1L-WSe2, is altered to create 1L-WSeS with Seatoms on one face and S atoms on the other, effectively placinga WSe2/WS2 interface within the 1L. This artificially modifiedatomic ordering breaks the out-of-plane crystal symmetry andresults in an in-built electric field,31 which, when experiencedby excitons, displaces the electron and hole wave functions.321L-Janus were experimentally reported recently in refs 33 and34. The next steps include the identification and control ofexciton charge states in J-TMDs. One challenge is the broadReceived: October 26, 2022Accepted: March 29, 2023Published: April 14, 2023Articlewww.acsnano.org© 2023 The Authors. Published byAmerican Chemical Society7326https://doi.org/10.1021/acsnano.2c10697ACS Nano 2023, 17, 7326−7334Downloaded via NATL INST FOR MATLS SCIENCE (NIMS) on May 7, 2023 at 06:06:02 (UTC).See https://pubs.acs.org/sharingguidelines for options on how to legitimately share published articles.https://pubs.acs.org/action/doSearch?field1=Contrib&text1="Matthew+S.+G.+Feuer"&field2=AllField&text2=&publication=&accessType=allContent&Earliest=&ref=pdfhttps://pubs.acs.org/action/doSearch?field1=Contrib&text1="Alejandro+R.-P.+Montblanch"&field2=AllField&text2=&publication=&accessType=allContent&Earliest=&ref=pdfhttps://pubs.acs.org/action/doSearch?field1=Contrib&text1="Mohammed+Y.+Sayyad"&field2=AllField&text2=&publication=&accessType=allContent&Earliest=&ref=pdfhttps://pubs.acs.org/action/doSearch?field1=Contrib&text1="Carola+M.+Purser"&field2=AllField&text2=&publication=&accessType=allContent&Earliest=&ref=pdfhttps://pubs.acs.org/action/doSearch?field1=Contrib&text1="Ying+Qin"&field2=AllField&text2=&publication=&accessType=allContent&Earliest=&ref=pdfhttps://pubs.acs.org/action/doSearch?field1=Contrib&text1="Ying+Qin"&field2=AllField&text2=&publication=&accessType=allContent&Earliest=&ref=pdfhttps://pubs.acs.org/action/doSearch?field1=Contrib&text1="Evgeny+M.+Alexeev"&field2=AllField&text2=&publication=&accessType=allContent&Earliest=&ref=pdfhttps://pubs.acs.org/action/doSearch?field1=Contrib&text1="Alisson+R.+Cadore"&field2=AllField&text2=&publication=&accessType=allContent&Earliest=&ref=pdfhttps://pubs.acs.org/action/doSearch?field1=Contrib&text1="Barbara+L.+T.+Rosa"&field2=AllField&text2=&publication=&accessType=allContent&Earliest=&ref=pdfhttps://pubs.acs.org/action/doSearch?field1=Contrib&text1="James+Kerfoot"&field2=AllField&text2=&publication=&accessType=allContent&Earliest=&ref=pdfhttps://pubs.acs.org/action/doSearch?field1=Contrib&text1="Elaheh+Mostaani"&field2=AllField&text2=&publication=&accessType=allContent&Earliest=&ref=pdfhttps://pubs.acs.org/action/doSearch?field1=Contrib&text1="Rados%C5%82aw+Kale%CC%A7ba"&field2=AllField&text2=&publication=&accessType=allContent&Earliest=&ref=pdfhttps://pubs.acs.org/action/doSearch?field1=Contrib&text1="Rados%C5%82aw+Kale%CC%A7ba"&field2=AllField&text2=&publication=&accessType=allContent&Earliest=&ref=pdfhttps://pubs.acs.org/action/doSearch?field1=Contrib&text1="Pranvera+Kolari"&field2=AllField&text2=&publication=&accessType=allContent&Earliest=&ref=pdfhttps://pubs.acs.org/action/doSearch?field1=Contrib&text1="Jan+Kopaczek"&field2=AllField&text2=&publication=&accessType=allContent&Earliest=&ref=pdfhttps://pubs.acs.org/action/doSearch?field1=Contrib&text1="Kenji+Watanabe"&field2=AllField&text2=&publication=&accessType=allContent&Earliest=&ref=pdfhttps://pubs.acs.org/action/doSearch?field1=Contrib&text1="Takashi+Taniguchi"&field2=AllField&text2=&publication=&accessType=allContent&Earliest=&ref=pdfhttps://pubs.acs.org/action/doSearch?field1=Contrib&text1="Andrea+C.+Ferrari"&field2=AllField&text2=&publication=&accessType=allContent&Earliest=&ref=pdfhttps://pubs.acs.org/action/doSearch?field1=Contrib&text1="Dhiren+M.+Kara"&field2=AllField&text2=&publication=&accessType=allContent&Earliest=&ref=pdfhttps://pubs.acs.org/action/doSearch?field1=Contrib&text1="Dhiren+M.+Kara"&field2=AllField&text2=&publication=&accessType=allContent&Earliest=&ref=pdfhttps://pubs.acs.org/action/doSearch?field1=Contrib&text1="Sefaattin+Tongay"&field2=AllField&text2=&publication=&accessType=allContent&Earliest=&ref=pdfhttps://pubs.acs.org/action/doSearch?field1=Contrib&text1="Mete+Atatu%CC%88re"&field2=AllField&text2=&publication=&accessType=allContent&Earliest=&ref=pdfhttps://pubs.acs.org/action/showCitFormats?doi=10.1021/acsnano.2c10697&ref=pdfhttps://pubs.acs.org/doi/10.1021/acsnano.2c10697?ref=pdfhttps://pubs.acs.org/doi/10.1021/acsnano.2c10697?goto=articleMetrics&ref=pdfhttps://pubs.acs.org/doi/10.1021/acsnano.2c10697?goto=recommendations&?ref=pdfhttps://pubs.acs.org/doi/10.1021/acsnano.2c10697?goto=supporting-info&ref=pdfhttps://pubs.acs.org/doi/10.1021/acsnano.2c10697?fig=agr1&ref=pdfhttps://pubs.acs.org/toc/ancac3/17/8?ref=pdfhttps://pubs.acs.org/toc/ancac3/17/8?ref=pdfhttps://pubs.acs.org/toc/ancac3/17/8?ref=pdfhttps://pubs.acs.org/toc/ancac3/17/8?ref=pdfwww.acsnano.org?ref=pdfhttps://pubs.acs.org?ref=pdfhttps://pubs.acs.org?ref=pdfhttps://doi.org/10.1021/acsnano.2c10697?urlappend=%3Fref%3DPDF&jav=VoR&rel=cite-ashttps://www.acsnano.org?ref=pdfhttps://www.acsnano.org?ref=pdfhttps://creativecommons.org/licenses/by/4.0/https://creativecommons.org/licenses/by/4.0/https://acsopenscience.org/open-access/licensing-options/18-meV photoluminescence (PL) line shape for the narrowestreported emission in J-TMDs, achieved via hexagonal boronnitride (hBN) encapsulation.35 The second challenge isfeasible integration of J-TMDs into electrically gated devices.Here, we address the above challenges, and identify neutraland negatively charged exciton transitions in 1L-WSeS usingreflectance contrast (RC) and PL spectroscopy. To confirmthe Janus conversion of a 1L exfoliated from flux-grown WSe2bulk crystal,36 we perform Raman and PL spectroscopy overthe flake. By encapsulating 1L-WSeS in hBN, we are able tomeasure the narrowest emission (5.9 meV line width) reportedto-date from J-TMDs. This spectral narrowing is key to solvingthe essential challenge of spectrally resolving and assigning theoptical transitions to specific exciton charge configurations.Furthermore, we provide physical insights into the excitonicorigin of the different optical transitions, by extracting the gfactors and trion binding energies. The gate controldemonstrated here is a necessary step for future integrationinto optoelectronic devices and excitonic experiments with J-TMDs.Figure 1. Optical characterization of the Janus 1L-WSeS device. (a) Illustration of the device. Janus 1L-WSeS (inset) is encapsulated in ML-hBN(blue) and electrically contacted by FLG (black). The device is on a n+2 Si (purple)/SiO2 (orange) substrate. Au contacts (yellow) allow avoltage to be applied between the FLG and Si. (b) Optical image of the device. 1L-WSeS is outlined in red, the top and bottom ML-hBN inblue, and FLG in black. (c) Raman map of the device, in the region highlighted by the white box in (b), acquired at room temperature using2.33 eV optical excitation. The color coding shows the relative intensity between the 1L-WSe2 E′ + A1′ Raman mode (254 cm−1), with 100%in blue, and the Janus 1L-WSeS A11 Raman mode (284 cm−1), with 100% in yellow. Regions with no 1L-TMD are shown in black. The arrowindicates conversion from 1L-WSe2 to 1L-WSeS . Raman spectra from unconverted, partially converted, and fully converted locations areshown below the Raman map, with the color shading indicating the Raman modes above. (d) PL map of the device in the region highlightedby the white box in (b), acquired at 4 K using 2.33 eV optical excitation. The color coding shows the relative integrated PL emissionintensity between the 1L-WSe2 (1.63 to 1.75 eV), with 100% in blue, and Janus 1L-WSeS (1.77 to 1.91 eV), with 100% in yellow, spectralbands. Regions with no 1L-TMD are shown in black. The arrow indicates conversion from 1L-WSe2 to 1L-WSeS . Representative normalizedPL spectra from unconverted, partially converted, and fully converted locations are shown below the PL map, with the color shadingindicating the spectral bands above.ACS Nano www.acsnano.org Articlehttps://doi.org/10.1021/acsnano.2c10697ACS Nano 2023, 17, 7326−73347327https://pubs.acs.org/doi/10.1021/acsnano.2c10697?fig=fig1&ref=pdfhttps://pubs.acs.org/doi/10.1021/acsnano.2c10697?fig=fig1&ref=pdfhttps://pubs.acs.org/doi/10.1021/acsnano.2c10697?fig=fig1&ref=pdfhttps://pubs.acs.org/doi/10.1021/acsnano.2c10697?fig=fig1&ref=pdfwww.acsnano.org?ref=pdfhttps://doi.org/10.1021/acsnano.2c10697?urlappend=%3Fref%3DPDF&jav=VoR&rel=cite-asRESULTS AND DISCUSSIONDevice Characterization. Figure 1a is an illustration ofone of our Janus devices. The doped Si substrate is used as aback gate, separated from the 1L-Janus by SiO2 and multilayerhBN (ML-hBN). A parent 1L-WSe2 is exfoliated andsubsequently transfered onto the ML-hBN. The 1L-WSe2 isthen converted into a Janus 1L-WSeS , with Se atoms on thebottom and S atoms on the top, by following a room-temperature in-situ conversion technique (see Methods andSupplementary Notes S1, S2).37,38 An additional ML-hBNtransferred on top of the converted 1L-WSeS encapsulates theflake, and a top gate of few-layer graphene (FLG) electricallycontacts the 1L-WSeS . Figure 1b shows an optical microscopeimage of the device, where the 1L-WSeS is outlined in red, thebottom and top hBN in blue, and the FLG in black.Figure 1c shows a Raman spectroscopy map of the device,acquired at room temperature using 2.33 eV optical excitation,in the region highlighted by the white box in Figure 1b. Thecolor code indicates the relative intensity between thecharacteristic 1L-WSe2 E′ + A1′ Raman mode (blue)39 andthe Janus 1L-WSeS A11 Raman mode (yellow),40 withrepresentative Raman spectra from regions with differentdegrees of Janus conversion shown below the Raman map (seeS3). The Raman spectra from the large region (∼400 μm2) offully converted Janus 1L-WSeS evidence that the convertedregion is not a disordered alloy.37,40,41Figure 1d shows a PL map, acquired at a temperature of 4 Kusing 2.33 eV optical excitation, in the same region of thedevice as in Figure 1c. Similar to Figure 1c, the color codeshows the relative PL emission intensity between the distinct1L-WSe2 (blue) and Janus 1L-WSeS (yellow) spectral bands.37,42The PL map correlates with the Raman map in Figure 1c,which validates our assignment of the Janus 1L-WSeS spectralband. Therefore, we focus on the exciton emission in thespatial region of full Janus conversion.Identification of the Neutral Exciton. Encapsulation inhBN reduces the line widths of PL peaks in conventional 1L-TMDs,43−45 thus allowing for the identification of excitonicspecies.46,47 Figure 2a compares a representative PL spectrumat 4 K from our ML-hBN encapsulated 1L-WSeS device (redcurve) to the spectrum from unencapsulated 1L-WSeS on a Si/SiO2 substrate (blue curve). The unencapsulated 1L-WSeS has abroad spectrum, with a full width at half-maximum (FWHM)on the order 30 meV, on par with the narrowest line widthreported to-date for unencapsulated Janus TMDs.38 Incontrast, encapsulation with hBN allows us to resolve multiplespectral features with significantly reduced line widths (<10meV).The peaks labeled 1, 2, 3, and X0 are present in the 1L-WSeSPL spectra across the whole device (see S3), indicating thatthese arise from intrinsic excitonic transitions. Since thehighest-energy PL peak in both 1L-WSe2 and 1L-WS2 stemsfrom neutral excitons,43 the peak at 1.893 eV is a likelycandidate for the neutral exciton, X0, in 1L-WSeS . To verify this,we directly probe excitonic absorption resonances using RCspectroscopy (see Methods).14Figure 2b shows a RC spectrum from our 1L-WSeS device(black curve) and the PL spectrum from the same location(red curve). The RC signal shows a strong feature at 1.893 eV,which confirms our assignment of X0. The lowest observed PLFWHM of the Janus X0 transition is 5.9 meV in our device, thelowest reported to date. The X0 transition is present in both PLand RC across the fully converted Janus region (see S3), withan average PL transition energy of 1.890(1) eV and an averageFWHM of 8.4(4) meV over 11 measured locations.Power-dependent PL measurements (see S4) providefurther evidence that X0 is the neutral exciton transition asits intensity scales linearly with power over the measured range15 nW to 50 μW (corresponding to 3 Wcm−2 to 104 Wcm−2).We note that in the spectral range 1.750 to 1.825 eV we alsoobserve PL peaks with linear power dependences at low powerand that saturate in the range 50 to 500 nW (10 to 100Wcm−2). This suggests the presence of localized defectsdisplaying quantum light emission.20,48,49Density functional theory (DFT) calculations of the 1L-WSeSband structure (see S5) show that, similar to conventional W-based TMDs (1L-WSe2 and 1L-WS2),50−52 1L-WSeS is direct-bandgap at the K points, with a spin ordering such that theupper valence band is opposite in spin to the lower spin-splitconduction band. The spin ordering in the conduction bandallows for both a negatively charged intervalley trion (Xinter− ),with the two electrons in different valleys, and an intravalleytrion (Xintra− ), with the two electrons in the same valley. Bycombining DFT and quantum Monte Carlo calculations wepredict the binding energies of the Coulomb-exchange splitXinter− and Xintra− to be 26 and 32 meV, respectively, relative tothe neutral exciton in free-standing 1L-WSeS .Voltage-Controlled Generation of Charged Excitons.To measure the charged excitonic transitions of 1L-WSeS , wetune its doping by applying a voltage V between the 1L-WSeSFigure 2. Photoluminescence and reflectance contrast spectra ofhBN-encapsulated 1L-WSeS . (a) PL spectrum from the encapsulated1L-WSeS device (red curve) compared to the PL spectrum fromunencapsulated 1L-WSeS (blue curve). The spectra are normalizedto the same peak height. The peaks labeled 1, 2, and 3 are presentacross the device. The inset shows the magnified PL spectrumaround X0. (b) RC spectrum (black curve, left axis) from theencapsulated 1L-WSeS device compared to the PL spectrum at thesame location (red curve, right axis). The black dashed linedenotes the X0 transition energy, 1.893 eV. All spectra wereacquired at 4 K, in the neutral-doping regime, and the PL spectraunder 2.33 eV excitation.ACS Nano www.acsnano.org Articlehttps://doi.org/10.1021/acsnano.2c10697ACS Nano 2023, 17, 7326−73347328https://pubs.acs.org/doi/suppl/10.1021/acsnano.2c10697/suppl_file/nn2c10697_si_001.pdfhttps://pubs.acs.org/doi/suppl/10.1021/acsnano.2c10697/suppl_file/nn2c10697_si_001.pdfhttps://pubs.acs.org/doi/suppl/10.1021/acsnano.2c10697/suppl_file/nn2c10697_si_001.pdfhttps://pubs.acs.org/doi/suppl/10.1021/acsnano.2c10697/suppl_file/nn2c10697_si_001.pdfhttps://pubs.acs.org/doi/suppl/10.1021/acsnano.2c10697/suppl_file/nn2c10697_si_001.pdfhttps://pubs.acs.org/doi/suppl/10.1021/acsnano.2c10697/suppl_file/nn2c10697_si_001.pdfhttps://pubs.acs.org/doi/10.1021/acsnano.2c10697?fig=fig2&ref=pdfhttps://pubs.acs.org/doi/10.1021/acsnano.2c10697?fig=fig2&ref=pdfhttps://pubs.acs.org/doi/10.1021/acsnano.2c10697?fig=fig2&ref=pdfhttps://pubs.acs.org/doi/10.1021/acsnano.2c10697?fig=fig2&ref=pdfwww.acsnano.org?ref=pdfhttps://doi.org/10.1021/acsnano.2c10697?urlappend=%3Fref%3DPDF&jav=VoR&rel=cite-asand the Si substrate. Figure 3a shows the RC derivative signalas we vary the doping density, n (Methods). Similar dopingdependence is observed on a second device (see S2). In theoperational range of voltages, only the n-doped regime isaccessible, due to an intrinsic n-doping ∼3 × 1012 cm−2. Thepreviously identified X0 transition, here at 1.896 eV, dominatesthe RC signal between +21 to +17 V, corresponding to chargeneutrality. As we decrease the voltage, and n-dope the 1L-WSeS ,lower energy transitions appear, which are analogous to thetransitions observed in the n-doped regime for 1L-WSe2.53−55Figure 3b presents the RC derivative at 19, 7, and −10 V.The neutral exciton, X0, is shown in the line cut at 19 V.Between +17 to +5 V, we see a doublet, which we identify asXinter− and Xintra− in the line cut at 7 V with peaks at 1.864 and1.857 eV. We find an average binding energy relative to X0 of33.4(5) meV and 39.9(3) meV for Xinter− and Xintra− , respectively,over seven measured locations. We attribute the difference inbinding energies of these trions compared to our calculationsto a difference in dielectric environment caused by ML-hBNencapsulation.56 The exchange splitting between the negativetrion transitions of 6.4(6) meV is in good agreement with ourcalculations.At increased n-doping, below 5 V, the Xinter− and Xintra− peaksvanish and a single peak, labeled X−′ in the linecut at −10 V inFigure 3b, dominates the derivative of the RC spectrum. TheX−′ peak initially appears at 1.845 eV and redshifts by 10 meVbetween +5 and −17 V. An excitonic transition with a similardoping dependence has previously been observed in 1L-WSe254,55,57 and attributed to excitons bound to intervalleyplasmons.57,58 We expect this peak in 1L-WSeS to be similar inorigin, due to the similarity in its behavior with the transitionobserved in 1L-WSe2.Magnetic-Field Dependence of Janus Excitons. Wenext probe the exciton g factors by applying an out-of-planemagnetic field, B, and measuring the Zeeman energy splittingof the exciton transitions. We send unpolarized light to thedevice and detect the RC spectra with both σ+ and σ− circularpolarizations. The left-aligned panels (a, c, e, and g) in Figure 4display the RC derivative spectra for each excitonic transitionmeasured at B = 3 T magnetic field, with the right-circular (σ+)and left-circular (σ−) polarizations shown by the blue and redcurves, respectively. The splitting ΔE as a function of B isshown in the right-hand panels (b, d, f, and h) of Figure 4.Linear fits give the magnitude of the exciton transition gfactors, where ΔE = −gμBB (μB = 58 μeV T−1 is the Bohrmagneton).Figure 4a presents the RC derivative spectra for X0 at 3 T,showing a well-resolved splitting. Figure 4b shows ΔE for X0 asa function of magnetic field, for both RC and PL. From thelinear fit we extract similar g factors of 4.5(2) and 4.14(6) forRC and PL, respectively. For conventional 1L-TMDs, g factors∼4 have typically been assigned to bright excitons in the K andK′ valleys, with valley, orbital, and spin contributing to themagnetic moment.59,60 The measured g factors are consistentwith 1L-WSeS having a direct-bandgap at the K points.The g factors of the negatively charged trions dependstrongly on doping, ranging from 3 to 13 for voltages from 8 to14 V (see S6). For conventional 1L-TMDs, a similardependence and resulting trion g factors greater than 4 havebeen attributed to many-body interactions with the Fermi seaof electrons.61,62 We expect a similar origin of the observeddoping-dependent trion g factor in 1L-WSeS . Figure 4c−f showsRC derivative spectra and splittings as a function of magneticfield for the negative trions at example voltages. We findexample g factors of 5.7(7) for Xinter− and 5.4(6) for Xintra− at thevoltages presented. The Xinter− and Xintra− transitions additionallyshow evidence of the thermalization of the excess charge, asobserved in conventional W-based 1L-TMDs.46,60,63 Beyond∼3 T, this leads to only a single polarization being observablefor each negative trion.Figure 4g shows the polarization-resolved RC derivativespectrum for the X−′ transition at 3 T. Figure 4h displays theRC splitting of X−′ as a function of magnetic field, which givesa g factor ∼ 4.1(4), consistent with the interpretation of X−′ asthe exciton bound to intervalley plasmons and dressed bymany-body interactions.54,55,57Figure 3. Charge dependence of the reflectance contrast spectrumof 1L-WSeS . (a) RC derivative with varying electron doping densityn (left axis) and applied voltage (right axis) at 4 K. (b) RCderivative spectra at the voltages corresponding to the dashedwhite linecuts in panel (a) at 19, 7, and −10 V. The excitonictransitions X0, Xinter− , Xintra− , and X−′ are labeled.ACS Nano www.acsnano.org Articlehttps://doi.org/10.1021/acsnano.2c10697ACS Nano 2023, 17, 7326−73347329https://pubs.acs.org/doi/suppl/10.1021/acsnano.2c10697/suppl_file/nn2c10697_si_001.pdfhttps://pubs.acs.org/doi/suppl/10.1021/acsnano.2c10697/suppl_file/nn2c10697_si_001.pdfhttps://pubs.acs.org/doi/10.1021/acsnano.2c10697?fig=fig3&ref=pdfhttps://pubs.acs.org/doi/10.1021/acsnano.2c10697?fig=fig3&ref=pdfhttps://pubs.acs.org/doi/10.1021/acsnano.2c10697?fig=fig3&ref=pdfhttps://pubs.acs.org/doi/10.1021/acsnano.2c10697?fig=fig3&ref=pdfwww.acsnano.org?ref=pdfhttps://doi.org/10.1021/acsnano.2c10697?urlappend=%3Fref%3DPDF&jav=VoR&rel=cite-asCONCLUSIONSWe identified several excitonic complexes in Janus 1L-WSeS : X0,Xinter− , Xintra− , and X−′ and measured their g factors by integratinga hBN encapsulated 1L-WSeS into a charge-control device.Integrating J-TMDs into vertical heterostructures is key for thefuture development of nanoscale optoelectronic devices,64,65while resolving few-meV exciton line widths and identifyingthe exciton spectrum determines the suitability of J-TMDs forsensing.66,67 Future work includes identifying the transitionsthat give rise to the as-yet unidentified PL peaks as well asmeasuring the excitonic spectrum in the positively dopedregime. An immediate next step is measuring the out-of-planeelectric dipole moment of excitons in 1L-WSeS by applying anout-of-plane electric field in a capacitor-like device structure.The predicted permanent electric dipole moment of ∼0.2 Dfor the Janus X031,68 means that the resulting Stark shift ∼4meV at 1 V/nm would be resolved with our ∼6 meV linewidths.METHODSFabrication. We build our device by following a multistepprocess: first, the bottom ML-hBN is mechanically exfoliated onto aSi/SiO2 (90 nm oxide thickness) substrate. Second, a parent 1L-WSe2is mechanically exfoliated from a flux-zone grown36 bulk WSe2 crystaland deposited on the bottom ML-hBN by polydimethylsiloxane(PDMS) transfer. Third, the 1L-WSe2 undergoes AFM flattening69and subsequent conversion to a Janus 1L-WSeS by using the selectiveepitaxial atomic replacement (SEAR) method,37 while recording time-resolved Raman spectroscopy measurements in-situ to achievedeterministic conversion.38 Fourth, the top ML-hBN and FLG aresequentially deposited on the 1L-WSeS by PDMS transfer, withannealing to 150 °C and AFM flattening after each layer is deposited.The FLG is mechanically exfoliated from graphite sourced from HQGraphene. Fifth, Au contacts are deposited using standard electron-beam lithography procedures.AFM topography (Bruker Icon) is used to confirm the layerthicknesses, and Raman spectroscopy (Horiba LabRam Evolution) isused to characterize the various constituents of the heterostructure,along with confirming the conversion from 1L-WSe2 to 1L-WSeS (seeS1).Optical Measurements. All 4 K measurements are taken in aclosed-cycle cryostat (AttoDRY 1000 from Attocube Systems AG),equipped with an 8 T superconducting magnet.Excitation and collection light pass through a home-built confocalmicroscope in reflection geometry, with a 0.81 numerical aperture(NA) apochromatic objective (LT-APO/NIR/0.81 from AttocubeSystems AG). The PL measurements use continuous-wave excitationfrom a 2.33 eV laser (Ventus 532 from Laser Quantum Ltd.), with theexcitation powers measured on the sample and the optical intensitycalculated from the optical spot size given by the 0.81 NA. The PLFigure 4. Magnetic field dependence of the excitonic complexes in 1L-WSeS . (a) RC derivative spectrum with σ+ (blue) and σ− (red) polarizedcollection at B = 3 T for X0 (at 19 V). (b) The energy splitting ΔE between X0 peaks in σ+ and σ− detected light as a function of magneticfield. The left panel shows the average splitting measured with RC in the neutral regime (splitting averaged between 18 to 20 V at eachmagnetic field). The right panel shows the splitting of X0 measured with PL. The solid curve is a linear fit to ΔE = −gμBB, and the g factorsare displayed for both RC and PL. (c) Same measurement as in (a) but for Xinter− at 12.5 V. (d) ΔE as a function of magnetic field for Xinter− at12.5 V. (e,f) Same as in (c) and (d) but for Xintra− at 9 V. (g,h) Same as in (c) and (d) but for the X−′ peak at −20 V. All measurements werecarried out at 4 K.ACS Nano www.acsnano.org Articlehttps://doi.org/10.1021/acsnano.2c10697ACS Nano 2023, 17, 7326−73347330https://pubs.acs.org/doi/suppl/10.1021/acsnano.2c10697/suppl_file/nn2c10697_si_001.pdfhttps://pubs.acs.org/doi/10.1021/acsnano.2c10697?fig=fig4&ref=pdfhttps://pubs.acs.org/doi/10.1021/acsnano.2c10697?fig=fig4&ref=pdfhttps://pubs.acs.org/doi/10.1021/acsnano.2c10697?fig=fig4&ref=pdfhttps://pubs.acs.org/doi/10.1021/acsnano.2c10697?fig=fig4&ref=pdfwww.acsnano.org?ref=pdfhttps://doi.org/10.1021/acsnano.2c10697?urlappend=%3Fref%3DPDF&jav=VoR&rel=cite-assignal is sent to a 150-line grating spectrometer (PrincetonInstruments Inc.).The RC measurements use broadband light (Thorlabs mountedLED M660L4, nominal wavelength 660 nm, FWHM 20 nm). Thereflected light is collected in the confocal microscope discussed aboveand the spectra are recorded on the same 150-line gratingspectrometer as for PL. RC is calculated by comparing the spectrumreflected from the heterostructure in a region with the 1L-WSeS , R, andwithout 1L-WSeS , R0. RC as a function of emission energy E is thengiven by=+ER E R ER E R ERC( )( ) ( )( ) ( )00The negative derivative of the RC spectrum, −d(RC)/dE,highlights the excitonic transitions and suppresses the RC back-ground.54,70,71 To obtain the derivative RC spectrum, we first smooththe raw RC spectrum using a spline fit and then take the derivative ofthe resultant spline.Gate-Voltage to Layer-Doping Conversion. The dopingdensity n (charge per unit area) is calculated from the appliedvoltage V (Keithley 2400 SMU), by using the gate capacitance, C=n V n CV q( ) ( / )i eThe intrinsic doping, ni, is the doping density at zero applied voltage,and the magnitude of the electron charge is qe = 1.6 × 10−19 C.The voltage is applied across both the ML-hBN and SiO2 and thegate capacitance can be derived by combining the dielectric layers ofML-hBN and SiO2 in series=+Cd d0SiO2 hBNhBN SiO2 SiO2 hBNThe relative dielectric constants of SiO2 and hBN are ϵSiO2 = 3.972 andϵhBN = 3.8,73 respectively. ϵ0 = 8.85 × 1012 Fm−1 is the vacuumpermittivity.The thickness of SiO2 is dSiO2 = 90 nm and that of hBN is dhBN = 27nm (see S1). The intrinsic doping density is ni = 3 × 1012 cm−2,determined by setting the doping density to n = 0 when thereflectance contrast signal from the neutral exciton vanishes (17 V),54where positive n indicates electron doping.ASSOCIATED CONTENT*sı Supporting InformationThe Supporting Information is available free of charge athttps://pubs.acs.org/doi/10.1021/acsnano.2c10697.Device characterization; Gate-dependent measurementsin device 2; Spectral mapping and homogeneity; Power-dependent measurements; Band structure calculations;Magnetic-field dependent measurements (PDF)AUTHOR INFORMATIONCorresponding AuthorsSefaattin Tongay − Materials Science and Engineering, Schoolfor Engineering of Matter, Transport and Energy, ArizonaState University, Tempe, Arizona 85287, United States;orcid.org/0000-0001-8294-984X;Email: sefaattin.tongay@asu.eduMete Atatüre − Cavendish Laboratory, University ofCambridge, Cambridge CB3 0HE, U.K.; orcid.org/0000-0003-3852-0944; Email: ma424@cam.ac.ukAuthorsMatthew S. G. Feuer − Cavendish Laboratory, University ofCambridge, Cambridge CB3 0HE, U.K.Alejandro R.-P. Montblanch − Cavendish Laboratory,University of Cambridge, Cambridge CB3 0HE, U.K.Mohammed Y. Sayyad − Materials Science and Engineering,School for Engineering of Matter, Transport and Energy,Arizona State University, Tempe, Arizona 85287, UnitedStatesCarola M. Purser − Cavendish Laboratory, University ofCambridge, Cambridge CB3 0HE, U.K.; CambridgeGraphene Centre, University of Cambridge, Cambridge CB30FA, U.K.Ying Qin − Materials Science and Engineering, School forEngineering of Matter, Transport and Energy, Arizona StateUniversity, Tempe, Arizona 85287, United StatesEvgeny M. Alexeev − Cambridge Graphene Centre, Universityof Cambridge, Cambridge CB3 0FA, U.K.; CavendishLaboratory, University of Cambridge, Cambridge CB3 0HE,U.K.; orcid.org/0000-0002-8149-6364Alisson R. Cadore − Cambridge Graphene Centre, Universityof Cambridge, Cambridge CB3 0FA, U.K.Barbara L. T. Rosa − Cambridge Graphene Centre, Universityof Cambridge, Cambridge CB3 0FA, U.K.James Kerfoot − Cambridge Graphene Centre, University ofCambridge, Cambridge CB3 0FA, U.K.; orcid.org/0000-0002-6041-4833Elaheh Mostaani − Cambridge Graphene Centre, University ofCambridge, Cambridge CB3 0FA, U.K.Radosław Kaleb̧a − Cavendish Laboratory, University ofCambridge, Cambridge CB3 0HE, U.K.Pranvera Kolari − Materials Science and Engineering, Schoolfor Engineering of Matter, Transport and Energy, ArizonaState University, Tempe, Arizona 85287, United StatesJan Kopaczek − Materials Science and Engineering, School forEngineering of Matter, Transport and Energy, Arizona StateUniversity, Tempe, Arizona 85287, United States;orcid.org/0000-0003-4851-9568Kenji Watanabe − Research Center for Functional Materials,National Institute for Materials Science, Tsukuba 305-0044,Japan; orcid.org/0000-0003-3701-8119Takashi Taniguchi − International Center for MaterialsNanoarchitectonics, National Institute for Materials Science,Tsukuba 305-0044, Japan; orcid.org/0000-0002-1467-3105Andrea C. Ferrari − Cambridge Graphene Centre, Universityof Cambridge, Cambridge CB3 0FA, U.K.; orcid.org/0000-0003-0907-9993Dhiren M. Kara − Cavendish Laboratory, University ofCambridge, Cambridge CB3 0HE, U.K.Complete contact information is available at:https://pubs.acs.org/10.1021/acsnano.2c10697Author Contributions#M.S.G.F., A.R.-P.M., and M.Y.S. contributed equally to thiswork.Author ContributionsA.R.-P.M., M.S.G.F., A.C.F., D.M.K., and M.A. conceived andmanaged the project; M.Y.S., Y.Q., P.K., J.K., and S.T. providedthe bulk WSe2 crystals and carried out the Janus SEARconversion; K.W. and T.T. provided hBN crystals; A.R.C.,B.L.T.R., and J.K. fabricated the devices; E.M. performed thecalculations; M.S.G.F., A.R.-P.M., C.M.P., E.M.A., R.K.,D.M.K., and M.A. performed the optical measurements andanalyzed the results. All authors participated in the discussionof the results and the writing of the manuscript.ACS Nano www.acsnano.org Articlehttps://doi.org/10.1021/acsnano.2c10697ACS Nano 2023, 17, 7326−73347331https://pubs.acs.org/doi/suppl/10.1021/acsnano.2c10697/suppl_file/nn2c10697_si_001.pdfhttps://pubs.acs.org/doi/10.1021/acsnano.2c10697?goto=supporting-infohttps://pubs.acs.org/doi/suppl/10.1021/acsnano.2c10697/suppl_file/nn2c10697_si_001.pdfhttps://pubs.acs.org/action/doSearch?field1=Contrib&text1="Sefaattin+Tongay"&field2=AllField&text2=&publication=&accessType=allContent&Earliest=&ref=pdfhttps://orcid.org/0000-0001-8294-984Xhttps://orcid.org/0000-0001-8294-984Xmailto:sefaattin.tongay@asu.eduhttps://pubs.acs.org/action/doSearch?field1=Contrib&text1="Mete+Atatu%CC%88re"&field2=AllField&text2=&publication=&accessType=allContent&Earliest=&ref=pdfhttps://orcid.org/0000-0003-3852-0944https://orcid.org/0000-0003-3852-0944mailto:ma424@cam.ac.ukhttps://pubs.acs.org/action/doSearch?field1=Contrib&text1="Matthew+S.+G.+Feuer"&field2=AllField&text2=&publication=&accessType=allContent&Earliest=&ref=pdfhttps://pubs.acs.org/action/doSearch?field1=Contrib&text1="Alejandro+R.-P.+Montblanch"&field2=AllField&text2=&publication=&accessType=allContent&Earliest=&ref=pdfhttps://pubs.acs.org/action/doSearch?field1=Contrib&text1="Mohammed+Y.+Sayyad"&field2=AllField&text2=&publication=&accessType=allContent&Earliest=&ref=pdfhttps://pubs.acs.org/action/doSearch?field1=Contrib&text1="Carola+M.+Purser"&field2=AllField&text2=&publication=&accessType=allContent&Earliest=&ref=pdfhttps://pubs.acs.org/action/doSearch?field1=Contrib&text1="Ying+Qin"&field2=AllField&text2=&publication=&accessType=allContent&Earliest=&ref=pdfhttps://pubs.acs.org/action/doSearch?field1=Contrib&text1="Evgeny+M.+Alexeev"&field2=AllField&text2=&publication=&accessType=allContent&Earliest=&ref=pdfhttps://orcid.org/0000-0002-8149-6364https://pubs.acs.org/action/doSearch?field1=Contrib&text1="Alisson+R.+Cadore"&field2=AllField&text2=&publication=&accessType=allContent&Earliest=&ref=pdfhttps://pubs.acs.org/action/doSearch?field1=Contrib&text1="Barbara+L.+T.+Rosa"&field2=AllField&text2=&publication=&accessType=allContent&Earliest=&ref=pdfhttps://pubs.acs.org/action/doSearch?field1=Contrib&text1="James+Kerfoot"&field2=AllField&text2=&publication=&accessType=allContent&Earliest=&ref=pdfhttps://orcid.org/0000-0002-6041-4833https://orcid.org/0000-0002-6041-4833https://pubs.acs.org/action/doSearch?field1=Contrib&text1="Elaheh+Mostaani"&field2=AllField&text2=&publication=&accessType=allContent&Earliest=&ref=pdfhttps://pubs.acs.org/action/doSearch?field1=Contrib&text1="Rados%C5%82aw+Kale%CC%A7ba"&field2=AllField&text2=&publication=&accessType=allContent&Earliest=&ref=pdfhttps://pubs.acs.org/action/doSearch?field1=Contrib&text1="Pranvera+Kolari"&field2=AllField&text2=&publication=&accessType=allContent&Earliest=&ref=pdfhttps://pubs.acs.org/action/doSearch?field1=Contrib&text1="Jan+Kopaczek"&field2=AllField&text2=&publication=&accessType=allContent&Earliest=&ref=pdfhttps://orcid.org/0000-0003-4851-9568https://orcid.org/0000-0003-4851-9568https://pubs.acs.org/action/doSearch?field1=Contrib&text1="Kenji+Watanabe"&field2=AllField&text2=&publication=&accessType=allContent&Earliest=&ref=pdfhttps://orcid.org/0000-0003-3701-8119https://pubs.acs.org/action/doSearch?field1=Contrib&text1="Takashi+Taniguchi"&field2=AllField&text2=&publication=&accessType=allContent&Earliest=&ref=pdfhttps://orcid.org/0000-0002-1467-3105https://orcid.org/0000-0002-1467-3105https://pubs.acs.org/action/doSearch?field1=Contrib&text1="Andrea+C.+Ferrari"&field2=AllField&text2=&publication=&accessType=allContent&Earliest=&ref=pdfhttps://orcid.org/0000-0003-0907-9993https://orcid.org/0000-0003-0907-9993https://pubs.acs.org/action/doSearch?field1=Contrib&text1="Dhiren+M.+Kara"&field2=AllField&text2=&publication=&accessType=allContent&Earliest=&ref=pdfhttps://pubs.acs.org/doi/10.1021/acsnano.2c10697?ref=pdfwww.acsnano.org?ref=pdfhttps://doi.org/10.1021/acsnano.2c10697?urlappend=%3Fref%3DPDF&jav=VoR&rel=cite-asNotesThe authors declare no competing financial interest.This work has previously been submitted to a preprintserver:74 Feuer, M. S. G.; Montblanch, A. R. P.; Sayyad, M.;Purser, C. M.; Qin, Y.; Alexeev, E. M.; Cadore, A. R.; Rosa, B.L. T.; Kerfoot, J.; Mostaani, E.; Kalba, R.; Kolari, P.; Kopaczek,J.; Watanabe, K.; Taniguchi, T.; Ferrari, A. C.; Kara, D. M.;Tongay, S.; Atature, M. Identification of exciton complexes in acharge-tunable Janus WSeS monolayer. arXiv, October 13,2022, arXiv:2210.06930. DOI: 10.48550/arXiv.2210.06930(accessed March 22, 2023).ACKNOWLEDGMENTSWe acknowledge funding from the EU Quantum Technology(2D-SIPC) and Graphene Flagships; EU Grants CHARM andGraph-X; ERC Grants PEGASOS, Hetero2D, GSYNCOR, andGIPT; and EPSRC Grants EP/K01711X/1, EP/K017144/1,EP/N010345/1, EP/L016087/1, EP/X015742/1, and EP/V000055/1. M.S.G.F. acknowledges the EPSRC DoctoralTraining Programme. D.M.K. acknowledges support of a RoyalSociety university research fellowship URF\R1\180593. S.T.acknowledges primary support from DOE-SC0020653 (mate-rials synthesis), NSF CMMI 1825594 (NMR and TEMstudies), NSF DMR-2206987 (magnetic measurements), NSFCMMI-1933214, NSF 1904716, NSF 1935994, NSF ECCS2052527, DMR 2111812, and CMMI 2129412 (scalability ofJanus layers). K.W. and T.T. acknowledge support from theJSPS KAKENHI (Grant Numbers 19H05790, 20H00354 and21H05233).REFERENCES(1) Novoselov, K. S.; Jiang, D.; Schedin, F.; Booth, T.; Khotkevich,V.; Morozov, S.; Geim, A. K. Two-dimensional atomic crystals. Proc.Natl. Acad. Sci. U. S. A. 2005, 102, 10451−10453.(2) Radisavljevic, B.; Radenovic, A.; Brivio, J.; Giacometti, V.; Kis, A.Single-layer MoS2 transistors. Nat. Nanotechnol. 2011, 6, 147−150.(3) Palacios-Berraquero, C.; Kara, D. M.; Montblanch, A. R.-P.;Barbone, M.; Latawiec, P.; Yoon, D.; Ott, A. K.; Loncar, M.; Ferrari,A. C.; Atatüre, M. Large-scale quantum-emitter arrays in atomicallythin semiconductors. Nat. Commun. 2017, 8, 1−6.(4) Ferrari, A. 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