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Laser Refrigeration of Hydrothermal Nanocrystals in Physiological Media

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Laser Refrigeration of Hydrothermal Nanocrystals in Physiological Media Laser refrigeration of hydrothermal nanocrystals in physiological media Paden B. Rodera,1, Bennett E. Smithb,1, Xuezhe Zhoua,1, Matthew J. Cranec, and Peter J. Pauzauskiea,d,2 aDepartment of Materials Science & Engineering, University of Washington, Seattle, WA 98195; bDepartment of Chemistry, University of Washington, Seattle, WA 98195; cDepartment of Chemical Engineering, University of Washington, Seattle, WA 98195; and dFundamental & Computational Sciences Directorate, Pacific Northwest National Laboratory, Richland, WA 99354 Edited by Qihua Xiong, Nanyang Technological University, Singapore, Singapore, and accepted by the Editorial Board October 13, 2015 (received for review June 9, 2015) Coherent laser radiation has enabled many scientific and techno- contrast with anti-Stokes processes, optomechanical laser refrig- logical breakthroughs including Bose–Einstein condensates, ultra- eration has also been demonstrated based on a novel mechanism fast spectroscopy, superresolution optical microscopy, photothermal of angular momentum transfer between a circularly polarized laser therapy, and long-distance telecommunications. However, it has and a birefringent crystal (23). remained a challenge to refrigerate liquid media (including phys- To date, laser refrigeration of nanocrystals in aqueous media iological buffers) during laser illumination due to significant back- has not been reported stemming primarily from the large NIR ground solvent absorption and the rapid (∼ps) nonradiative α j ∼ optical absorption coefficient of water ( H2O 975 nm 0.5/cm) (24). vibrational relaxation of molecular electronic excited states. Here It has remained an open question whether these known cooling we demonstrate that single-beam laser trapping can be used to materials could act to refrigerate aqueous media and undergo induce and quantify the local refrigeration of physiological media hypothesized cold Brownian motion (CBM) (25, 26), or whether by >10 °C following the emission of photoluminescence from solvent heating from the background absorption coefficient of upconverting yttrium lithium fluoride (YLF) nanocrystals. A simple, water would overwhelm the cooling of individual YLF crystals. low-cost hydrothermal approach is used to synthesize polycrystalline Furthermore, it is not obvious a priori that YLF crystals made particles with sizes ranging from <200 nm to >1 μm. A tunable, near- through hydrothermal processing would have sufficiently low infrared continuous-wave laser is usedtoopticallytrapindividualYLF background impurity levels to achieve laser cooling (27, 28). In crystals with an irradiance on the order of 1 MW/cm2.Heatistrans- this work, we demonstrate the local laser refrigeration of hydro- ported out of the crystal lattice (across the solid–liquid interface) by + thermal YLF nanocrystals dispersed within several different anti-Stokes (blue-shifted) photons following upconversion of Yb3 aqueous media including deionized water, heavy water (D2O), electronic excited states mediated by the absorption of optical and physiological electrolytes. Refrigeration >10 °C below am- phonons. Temperatures are quantified through analysis of the bient conditions is observed in PBS following anti-Stokes pho- cold Brownian dynamics of individual nanocrystals in an inhomo- toluminescence from optically trapped (29), rare-earth–doped YLF geneous temperature field via forward light scattering in the back nanocrystals undergoing CBM. focal plane. The cold Brownian motion (CBM) analysis of individual YLF crystals indicates local cooling by >21 °C below ambient con- Results and Discussion 3+ ditions in D2O, suggesting a range of potential future applications Pioneering efforts to cool Yb :YLF materials in vacuo have including single-molecule biophysics and integrated photonic, relied on the growth of high-purity YLF single crystals using an electronic, and microfluidic devices. Significance laser refrigeration | nanocrystal | hydrothermal | physiological | anti-Stokes Although the laser refrigeration of bulk crystals has recently dvances in cryogenic sciences have enabled several obser- shown to cool below cryogenic temperatures (∼90 K) in vac- Avations of new low-temperature physical phenomena including uum, to date the laser refrigeration of physiological media has – superconductivity (1), superfluidity (2), and Bose Einstein con- not been reported. In this work, a low-cost hydrothermal densates (3). Heat transfer is critical in numerous fields of science synthetic approach is used to prepare nanocrystals that are and technology including thermal management within integrated capable of locally refrigerating physiological buffers (PBS, microelectronics (4–6), photonic (7, 8) and microfluidic (9) cir- DMEM) upon near-infrared illumination. Optical tweezers are cuits, and the regulation of metabolic processes (9–11). In 1929, used in tandem with cold Brownian motion analysis to observe + Pringsheim (12) proposed that solid-state materials could experi- the refrigeration of individual (Yb3 )-doped nanocrystals >10 °C ence refrigeration if they exhibited biased emission of anti-Stokes below ambient conditions. The ability to optically generate (blue-shifted) radiation relative to a fixed optical excitation wave- local refrigeration fields around individual nanocrystals prom- length. Epstein et al. (13) experimentally demonstrated this concept ises to enable precise optical temperature control within in- first in 1995 using rare-earth–doped fluoride glass materials. Optical tegrated electronic/photonic/microfluidic circuits, and also refrigeration of a condensed phase with a rhodamine dye by anti- thermal modulation of basic biomolecular processes, including Stokes radiation has previously been reported (14–16) but the the dynamics of motor proteins. results remain controversial (17, 18). More recently, it has been + shown that rare-earth–doped yttrium lithium fluoride (Yb3 : Author contributions: P.J.P. designed research; P.B.R., B.E.S., X.Z., and M.J.C. performed research; P.B.R., X.Z., and P.J.P. contributed new reagents/analytic tools; P.B.R., B.E.S., YLF) crystals grown in high-temperature Czochralski reactors X.Z., M.J.C., and P.J.P. analyzed data; and P.B.R., B.E.S., X.Z., and P.J.P. wrote the paper. ∼ (19) can be cooled to cryogenic temperatures ( 90 K) (20) in The authors declare no conflict of interest. vacuo using continuous-wave near-infrared (NIR) laser excita- This article is a PNAS Direct Submission. Q.X. is a guest editor invited by the Editorial tion. Furthermore, the laser refrigeration of doped yttrium alu- Board. 3+ minum garnet (Yb :YAG) materials has recently been reported in 1P.B.R., B.E.S., and X.Z. contributed equally to this work. air at atmospheric pressure (21). Anti-Stokes photoluminescence 2To whom correspondence should be addressed. Email: [email protected]. has also been reported (22) to cool cadmium sulfide (CdS) nano- This article contains supporting information online at www.pnas.org/lookup/suppl/doi:10. ribbons in vacuo by as much as 40 °C below room temperature. In 1073/pnas.1510418112/-/DCSupplemental. 15024–15029 | PNAS | December 8, 2015 | vol. 112 | no. 49 www.pnas.org/cgi/doi/10.1073/pnas.1510418112 Downloaded by guest on September 28, 2021 Fig. 1. Synthesis and characterization of YLF crystals. (A) Schematic of Scheelite crystal structure of YLF with I41/a space group symmetry. (B) SEM image of 3+ 3+ a faceted (Yb )0.1(Y )0.9 LiF4 particle exhibiting TTB morphology. (Scale bar, 1 μm.) (C) Powder XRD pattern of YLF crystals following hydrothermal synthesis indicating a pure Scheelite crystal phase. (Inset) Schematic of TTB morphology relative to YLF’s unit cell. (D) Bright-field TEM image of an in- + dividual Yb3 :YLF grain. (Scale bar, 200 nm.) (Inset) High-resolution TEM image taken from the indicated region. (Scale bar, 2 nm.) (E) HAADF image of the YLF grain in B showing regions of high contrast suggesting the presence of polycrystalline domains. (Inset) SAED from the indicated region. (F)X-ray fluorescence compositional-analysis spectrum of an individual YLF crystal taken within the TEM confirming the elemental crystalline composition in- cludingY,Yb,andFspecies. SCIENCES APPLIED PHYSICAL air- and moisture-free Czochralski process (30). In the experi- to pump the E4–E5 resonance and subsequently cannot initiate ments reported here, a low-cost modified hydrothermal synthesis upconversion-mediated cooling (Fig. 3B). + (31) of Yb3 :YLF is used to prepare crystals shown in Fig. 1. The CBM analysis discussed above is limited to reporting local Scanning electron microscopy (SEM) reveals that YLF crystals solvent temperatures, but it does not provide information on the exhibit a truncated tetragonal bipyramidal (TTB) morphology (Fig. internal lattice temperature of optically trapped YLF nanocrystals. + 1B). X-ray diffraction shows that the YLF crystal has a Scheelite It is well known that codoping YLF crystals with both Yb3 and + structure (Fig. 1C). Bright-field/high-angle annular-dark-field Er3 ions leads to a thermalized Boltzmann distribution between 2 4 3+ (HAADF) transmission electron microscope (TEM) imaging (Fig. the E2 ( H11/2) and E1 ( S3/2) manifolds of Er and an intense 1 D and E) and electron diffraction suggest that the TTB materials green upconversion emission that is visible to the unaided eye are polycrystalline and likely form through an oriented attachment (showninFig.4A). This upconversion process is enabled by the (32) process of nanocrystalline grains (Fig. 1E, Inset). long (ms) photoluminescence
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