Mid-infrared Black Phosphorus Surface-emitting Laser with an Open

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Mid-infrared Black Phosphorus Surfaceemitting Laser with an Open Micro-cavity Yuanqing Huang, Jiqiang Ning, Hongmei Chen, Yijun Xu, Xu Wang, Xiaotian Ge, Cheng Jiang, Xing Zhang, Jianwei Zhang, Yong Peng, Zengli Huang, Yongqiang Ning, Kai Zhang, and Ziyang Zhang ACS Photonics, Just Accepted Manuscript • DOI: 10.1021/acsphotonics.9b00096 • Publication Date (Web): 15 May 2019 Downloaded from http://pubs.acs.org on May 15, 2019

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Mid-infrared Black Phosphorus Surface-emitting Laser with an Open Micro-cavity Yuanqing Huang1,4†, Jiqiang Ning2†, Hongmei Chen1, Yijun Xu1, Xu Wang1, Xiaotian Ge2, Cheng Jiang1, Xing Zhang3, Jianwei Zhang3, Yong Peng4, Zengli Huang2, Yongqiang Ning3*, Kai Zhang1* and Ziyang Zhang1* 1Key

Laboratory of Nanodevices and Applications & i-Lab, Suzhou Institute of Nano-Tech and Nano-Bionics, Chinese Academy of Sciences, Suzhou 215123, China. 2Vacuum

Interconnected Nanotech Workstation, Suzhou Institute of Nano-Tech and Nano-Bionics, Chinese Academy of Sciences, Suzhou 215123, China. 3State

Key Laboratory of Luminescence and Applications, Changchun Institute of Optics, Fine Mechanics and Physics, Chinese Academy of Sciences, Changchun 130033, China. 4School

of Physical Sciences and Technology, Electron Microscopy Centre of Lanzhou University, Lab of Magnetism and Magnetic Materials of the Ministry of Education, Lanzhou University, 730000 Lanzhou, People’s Republic of China † These authors contributed equally to this work.

Abstract The compact and low cost surface-emitting lasers in 3-5 μm mid-infrared (MIR) range are highly desirable for important applications such as gas detection, noninvasive medical diagnosis and infrared scene projection. Due to the intrinsic noisy of general narrow-bandgap semiconductors, the MIR is a challenging region for photonics. Here, we demonstrate the first black phosphorus (BP) based MIR surface-emitting laser operating at room temperature fabricated with BP as the active gain materials embedded into a SiO2/Si3N4 open micro-cavity on silicon. Optically pumped lasing at ~3765 nm is successfully realized in the demonstrated device by significantly increased luminescence efficiency in the BP lamellar structure and resolving the general issues for processing BP and other two-dimensional materials as gain medium with the specific design of open cavity. This is the first demonstration of BP based light emitting device, and thus paves a pathway towards monolithic integration of Si-photonics in the MIR range. Keywords: Black phosphorus; Mid-infrared light sources; Surface-emitting lasers; Open cavity; Lamellar structure.

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3-5 μm MIR spectral region lying in an atmospheric window is not only important for free-space communication, but also crucial for wide-ranging applications in bio-medical imaging1, security inspection2, gas detection3, and so on because of the spectral "fingerprints" of abundant molecular vibrations in this range4. Following the first demonstration of quantum cascade lasers (QCLs)5 based on intersubband transitions, the research field of MIR light sources has experienced tremendous growth and QCL has emerged as the vital choice6-9. However, QCLs are featured with complex structures and expensive epitaxy growth, and the intersubband selection rules lead to polarized emission in the growth direction, which makes surface emission not suitable for QCL10. Development of reliable light-emitting devices on silicon is strongly desired for high-bandwidth chip-to-chip optical interconnect technologies. There have many progresses utilizing direct bandgap III-V11 or group-IV GeSn lasers12 as the light sources through direct-growth or wafer-bonding on Si, but it remains rare and very challenging for the MIR regime. The rising of 2D semiconductors makes some promise for breakthrough in optoelectronics, which are characterized with atomic perfect crystalline structures free of dangling bonds and defects. More importantly, 2D materials are constructed by van der Waals interactions which allows versatile integrations with various substrates including Si. Point- and edge-emitting light emitters have been realized by using 2D transition metal dichalcogenides (TMDCs)13-15. In comparison with point- and edge-emitting light emitters, surface-emitting emitters have many advantages, such as (i) monolithic and high-yield fabrication, (ii) extremely low threshold and small power consumption, (iii) high speed modulation capability at low driving current levels, (iv) easy packaging. Recently, a 636.5 nm vertical cavity surface-emitting laser (VCSEL) is achieved with the direct bandgap monolayer WS2 embedded in a SiO2 micro-cavity16. As a novel member of 2D semiconductors, BP has attracted great interests for infrared optics and optoelectronics due to its high mobility17, 18, large current on/off ratios19, anisotropic properties20 and the intrinsic thickness-dependent direct bandgap from 0.3 to 1.5 eV, covering the range from visible to MIR21-23. These unique features of BP have been well explored for fabricating high mobility transistors24-26 and broadband infrared photodetectors27-29. However, there is no report on BP based light emitters yet to date, due to the low luminescence efficiency and the serious challenge of processing BP to be a gain material. In this study, MIR surface-emitting lasers with a vertical waveguide micro-cavity were fabricated by employing BP as the gain medium. The laser cavity is surface-coated with distributed Bragg reflectors (DBR) mirrors, which provides an ideal media to precisely position the BP gain material and confine the light emission. However, in constructing such a DBR cavity for BP, there lies a great difficulty that the DBR mirrors cannot be directly grown on BP because of the severe damage of BP during the growth processes. As seen in Figure 1, with increasing the thickness of Si3N4 capping layer, the BP was damaged more and more severely, from wrinkling (in Figure 1b) to splitting (in Figure 1c), and finally completely destroyed into small pieces (in Figure 1d), which is believed to be one of the main issues in fabricating BP based light emitting devices.

Materials and methods BP gain materials were grown by a mineralizer-assisted gas-phase transformation method. During the growth, red P, Sn, SnI4 were enclosed in evacuated silica glass tubes as the precursors.


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Rather than the self-condensed bulk BP crystals for densely squeezed layered (DSL) BP, lamellar structure BP was grown on insulating substrates (like silicon) coated with designed alloy nuclei such as Au3SnP7. The details of the growth and characteristics of lamellar BP will be described elsewhere. The fabrication of the waveguide micro-cavity of the BP surface-emitting laser devices were made by standard optical lithography, and dry and wet etching process. The SiO2/Si3N4 DBR mirrors were deposited by Plasma Enhanced Chemical Vapor Deposition. The BP films were exfoliated from as-grown lamellar BP samples and cut into a uniform size of ~200×350 µm2, and very gently transferred onto the top of the bottom DBR on silicon. The MIR PL measurements of the BP materials and the optical characteristic of the BP based surface-emitting laser devices were performed with a 130 fs, 76 MHz Ti: sapphire laser operating at 740 nm. The excitation laser was directed to the sample with a reflective objective and the emitted MIR light was collected with a lens pair and fed into an infrared monochromator (Zolix Omni-λ300i) equipped with a mercury cadmium telluride (MCT) detector.

Figure 1. The microscopic images of the morphology of BP after capping with Si3N4 layers with different thickness, (a) no capping; (b) 100 nm Si3N4 layer capping; (c) 200 nm Si3N4 layer capping; and (d) 400 nm Si3N4 layer capping.

Results and discussion To overcome the obstacle mentioned above, we have developed an open cavity architecture specific for BP as well as other 2D materials which are prone to be damaged during processing. The geometry and fabrication procedure of the micro-cavity are schematically illustrated in Figure 2a. The top waveguide structure is fabricated with a sapphire substrate where a cubic hole (500 μm long, 500 μm wide and 3 μm deep) was defined by optical lithography and etching processes. 6 pairs of 462 nm Si3N4/660 nm SiO2 layers were deposited by PECVD into the cubic hole to form the top DBR with 96.0 % reflectivity. The thickness of sapphire above the DBR is about 450 μm. Because sapphire is highly transmissive in the wavelength range of 1000 to 4000 nm, the thickness of the sapphire above the DBR structure has little effect on the emission performance of the laser device. We have varied the thickness from 300 to 600 μm, and no detectable effect on the light emission can be observed. The bottom waveguide is obtained by depositing 8 pairs 462 nm Si3N4/660 nm SiO2 on a Si substrate as the DBR with 98.8 % reflectivity. A BP film of 1 µm thick and 200 × 350 μm2 large was gently transferred onto the bottom DBR with a blue Nitto tape. The top waveguide structure was flipped over, and then bonded together with the bottom part to


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sandwich the BP gain medium. The finalized device is schematically depicted in Figure 2b, and the photographs (the top ones) and corresponding optical microscopic images (the bottom ones) of the actual devices are shown in Figure 2c. The dark square at the finger is the bottom waveguide structure with the BP film loaded and the bright one is the final bonded device. The BP configurations can be seen clearly in the optical images.

Figure 2. The schematic diagram of the fabrication process and the microscopic images of BP surface-emitting laser. (a) Schematically depicts the fabrication process of the BP surface-emitting laser device with an open cavity design, where the top DBR waveguide structure is fabricated within a sapphire substrate (light yellow) following the steps of cubic hole etching, DBR deposition in the hole and substrate reversal for bonding, and the bottom component is prepared on a silicon substrate (light blue) following the steps of DBR deposition, BP transfer with a blue Nitto tape (blue) and the tape removal, and the top and bottom parts are finally bonded together to obtain the laser device. (b) Illustrates the schematic geometry of the finalized laser device. (c) Presents the photographs of the bottom waveguide with the BP film loaded (the dark square on the finger) and the final device with the top and bottom parts bonded together (the bright square on the finger), and the optical microscopic images of the BP film on the bottom waveguide without capping (the bright one) and the BP film with the top waveguide covered (the dark one).

High quality BP films were employed as the gain materials for the MIR surface-emitting lasers. As shown in Figure 3a, Raman spectrum shows three characteristic peaks of BP located at 364, 438 and 465 cm-1, corresponding to the A1g, B2g and A2g vibration modes24, respectively. High crystallinity of the BP films was well confirmed by the X-ray diffraction (XRD) measurements (Figure 3b). The sharp peaks at 2θ = 16.9°, 34.17° and 52.32° are ascribed to the diffractions from the (020), (040) and (060) crystal plane, respectively indicating a layered structure of BP30. The P 2p XPS core level spectrum of the BP films displays the peaks for P 2p1/2 and P 2p3/2 states located at 130.2 eV and 131 eV (Figure 3c). The peaks near 132 eV resulting from PxOy species disappear in the XPS spectrum, suggesting that the BP films are free from oxidation. It is worth to note that, the BP films employed for the laser devices reproduced from our as-grown lamellar BP are different from those conventional BP crystals (the growth and detailed description of the lamellar BP will be described elsewhere). As schematically shown in Figure 3d, the lamellar BP utilized in our work consists of alternating BP atomic layer units separated with nanoscaled air gaps rather


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than the DSL structure as unconventional BP crystals. The distinct structural difference of these two types of BP was clearly revealed by the cross-sectional scanning electron microscope (SEM) images, where regular nano-gaps in between BP atomic layers are observed in the lamellar BP in contrast to the seamless crystalline facet of the DSL BP. Figure S1a displays a typical transmission electron microscope (TEM) image of a lamellar BP flake, showing its obvious layered structure. Figure S1b shows a high resolution TEM (HRTEM) image, illustrating an orthorhombic crystal structure with two sets of interplanar spacing of 3.3 and 4.2 Å, respectively. The selected area electron diffraction (SAED) pattern in Figure S1c is well indexed to an orthorhombic structure and reveal the single-crystal nature of the material. Significantly, as shown in Figure 3e, the PL intensity excited from the lamellar BP is in the order of 3-4 times stronger than that from the DSL BP with the same thickness of ~1 µm. And, the PL spectrum of the lamellar BP exhibits a much narrower full width at half maximum (FWHM) of 355 nm than the 540 nm width of the DSL BP. The improved PL emission of the lamellar BP relatively to the DSL BP is probably due to the separate laminated layer structure, where the regular nano-gaps in between the multilayer BP crystals result in a constructive interference of the emission. This unique structural characteristic is promising for fabricating surface-emitting laser devices as demonstrated in this work.

Figure 3. Characterizations of the BP gain materials employed for the MIR surface-emitting lasers. (a)-(c) Raman, XRD and XPS measurements of the BP gain medium. (d) Schematic and cross-sectional SEM images of the lamellar BP utilized in our work compared with conventional DSL BP. The lamellar BP is derived from a novelly developed BP, with regular nano-gaps distributed among multilayer BP crystalline layers, that is different from DSL BP reproduced from BP bulk crystals. (e) MIR PL spectra of the lamellar BP relative to DSL BP. The PL intensity excited from the lamellar BP is in the order of 3-4 times stronger than that from the DSL BP with the same thickness of ~1 µm. And, the PL spectrum of the lamellar BP exhibits a much narrower FWHM of 355 nm rather than the 540 nm of the DSL BP.

The optical pumping of the BP laser was performed at RT with a Ti: sapphire laser operating at 740 nm and the emission was measured with the setup schematically shown in Figure 4c which


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also depicts the BP band structure illustrating the photon excitation and band edge emission processes as well as the lamellar BP gain material (~1 µm thick, comprised of ~100 BP/air alternating atomic layer pairs). The simulated and measured reflectivity spectra of the DBR mirrors are shown in Figure S2. The typical DBR mirror consists of alternating layers of 1/4 λ-thick dielectrics with different refractive indexes, and Figure S2a presents the simulated reflectivity spectra at normal incidence of the DBR mirrors with 4, 6, 8 pairs (labeled NC) of Si3N4 and SiO2, exhibiting the peak reflectivity at 3700 nm, the stop band of 1250 nm at full width at half-maximum, and peak reflectivity of 82.1%, 96.0%, and 98.8%, respectively. Figure S2b shows the measured reflectivity spectrum of a DBR mirror with 8 pairs of Si3N4 and SiO2, indicating a high reflectivity plateau from 3450 to 3850 nm which covers the whole PL spectrum of the lamellar BP. The emission spectra from the BP laser device measured at different pumping powers are shown in Figure 4a. At 50 mW, a 190 nm broad emission centered at 3836 nm is obtained. With increased pumping power, the emission exhibits a blue shift to ~3824 nm at the power of 700 mW, due to the redistribution of photo generated carriers towards higher energetic states with the increased pumping power. When the pumping power goes to 800 mW, a very sharp emission peak at 3794 nm with only 9 nm in width, emerges from the broad emission, indicating the occurrence of the stimulated emission. This is further confirmed by the nonlinear response characteristic of the peak intensity versus the pumping power as shown in Figure 4b, where the obvious onset of stimulated emission has been observed. Further increasing the pumping power, the intensities of the broad band and the lasing peak are both enhanced, as depicted in Figure 4a. When the pumping power gets larger than 850 mW, the spontaneous emission band is completely suppressed and the only sharp stimulated emission peak at 3765 nm dominates the spectrum. The lasing peak also exhibits a blue-shift behavior with increased pumping level which is in accordance with the power-dependent behavior of the spontaneous emission band30, 31. However, further increasing excitation power has led to a drop of the emission intensity. The main reason may be attributed to the significant heating effect, and we believe if the air separation in between each BP unit layers could be replaced by high thermal conductivity materials, the device performance could be further improved32.


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Figure 4. Characterizations of the BP gain materials employed for the MIR surface-emitting lasers. (a) Presents the emission spectra of the BP laser device acquired at room temperature by pumping with a femtosecond pulsed laser of 740 nm at different powers. (b) Illustrates the dependence of the emission peak intensity on the pumping laser power, and (c) Schematically depicts the optical pumping and emission collection configure for the BP laser device measurements, the scheme of the optical excitation of the BP with 740 nm light and the band edge emission of the 3765 nm wavelength, and laminate structure of the BP material, respectively.

Conclusion In summary, BP has been demonstrated as an effective gain material for MIR lasing. The realization of the BP based surface-emitting laser represents a significant step forward to compact and low cost MIR light sources on silicon. Further development and extension of this work will be focused on improving the device performance by optimizing the uniformity, quality, luminescence efficiency and scalable production capability of BP, introducing new composites like black PxAs(1-x)33 as the gain materials to realize lasing in longer MIR wavelength ranges.

Authority information Corresponding Authors *Email: [email protected]. *E-mail: [email protected] *E-mail: [email protected]

Notes The authors declare no competing financial interest. Acknowledgements We acknowledge the financial support from the Natural Science Foundation of China (Grant


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Nos. 61875222, 61875223, 11874390), and the open project of the State Key Laboratory of Luminescence and Applications. We thank the Nanofabrication facility for device fabrication in Suzhou Institute of Nano-Tech and Nano-Bionics, Chinese Academy of Sciences. Supporting Information： The Supporting Information is available free of charge on the ACS Publications website. Transmission electron microscopy images of the lamellar black phosphorus, and the simulated and measured reflectivity of distributed Bragg reflectors mirrors.

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Title: Mid-infrared black phosphorus surface-emitting laser with an open micro-cavity Authors: Yuanqing Huang1,4†, Jiqiang Ning2†, Hongmei Chen1, Yijun Xu1, Xu Wang1, Xiaotian Ge2, Cheng Jiang1, Xing Zhang3, Jianwei Zhang3, Yong Peng4, Zengli Huang2, Yongqiang Ning3*, Kai Zhang1*, Ziyang Zhang1*

1Key

Laboratory of Nanodevices and Applications & i-Lab, Suzhou Institute of Nano-Tech and Nano-Bionics, Chinese Academy of Sciences, Suzhou 215123, China. 2Vacuum

Interconnected Nanotech Workstation, Suzhou Institute of Nano-Tech and Nano-Bionics, Chinese Academy of Sciences, Suzhou 215123, China. 3State

Key Laboratory of Luminescence and Applications, Changchun Institute of Optics, Fine Mechanics and Physics, Chinese Academy of Sciences, Changchun 130033, China. 4School

of Physical Sciences and Technology, Electron Microscopy Centre of Lanzhou University, Lab of Magnetism and Magnetic Materials of the Ministry of Education, Lanzhou University, 730000 Lanzhou, People’s Republic of China † These authors contributed equally to this work. We demonstrate the first black phosphorus (BP) based mid-infrared (MIR) surface-emitting laser operating at room temperature fabricated with BP as the active gain materials embedded into a SiO2/Si3N4 open micro-cavity on silicon. Optically pumped lasing at ~3765 nm is successfully realized in the demonstrated device by significantly increased luminescence efficiency in the BP lamellar structure and resolving the general issues for processing BP and other two-dimensional materials as gain medium with the specific design of open cavity.

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Mid-infrared Black Phosphorus Surface-emitting Laser with an Open

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