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Saturable Absorption in Suspensions of Single-Digit Detonation Nanodiamonds Gennady M. Mikheev,*,† Roman Yu. Krivenkov,† Tatyana N. Mogileva,† Konstantin G. Mikheev,† Nicholas Nunn,‡ and Olga A. Shenderova‡ †

Institute of Mechanics UB RAS, 34, str. T. Baramzinoy, Izhevsk 426067, Russia Adámas Nanotechnologies, Inc., 8100 Brownleigh Drive, Suite 120, Raleigh, North Carolina 27617, United States

‡

ABSTRACT: Highly nonlinear optical properties of nanocarbon materials make them perspective candidates for saturable absorption (SA) applications, characterized by a short-term decrease in the optical medium absorption at high incident light intensity. The nonlinear optical properties and SA of aqueous suspensions of 5 nm detonation nanodiamonds (DNDs) have been studied by the z-scan technique under irradiation with nanosecond laser pulses at wavelengths of 532 and 1064 nm. The saturation intensity and nonlinear absorption coefficient describing the SA were obtained for concentrations of DND suspensions ranging between 0.5 and 5 wt %. It was concluded that the single-digit DND suspensions are suitable for optical limiting only at relatively high intensities of incident radiation, with saturation intensities of ∼5.9 and 14.1 MW/cm2 for 532 and 1064 nm incident excitation, respectively.

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INTRODUCTION One of the interesting phenomena of nonlinear optics is saturable absorption (SA), which is characterized by a shortterm decrease in the optical medium absorption at high incident light pulse intensity. SA is a well-known phenomenon and is based on an electronic transition between two energy levels. When incident light intensity is sufficiently high, the rate of decay of excited electrons to the ground state is insufficient to compensate for the depletion of the ground state, and the absorption subsequently saturates.1 Considering the wide range of applications where SA materials can be used, it is desirable to have a set of SA materials that can absorb at different wavelengths (e.g., in the visible or infrared spectral regions), possess different dynamic responses (how fast they recover), and demonstrate saturation at various intensities. SA is widely used in laser technology for high-speed optical modulators of optical losses placed in laser cavities. In the past decade, SA has been intensively studied in single-walled carbon nanotubes (CNTs)2−9 and graphene10−20 due to the possibility of using these carbon nanomaterials for producing picosecond and femtosecond laser pulses in the infrared spectral region. However, performance in the visible spectral region of most current saturable absorbers needs to be improved to advance the operation of passively Q-switched/mode-locked visible pulsed fiber lasers.21 Detonation nanodiamonds (DNDs) are another form of carbon nanomaterials,22−24 which are currently being considered as a promising material for various optical applications.25−30 Previously we reported on the SA of DNDs in aqueous suspensions with an average aggregate sizes of ∼35, 50, and 110 nm upon excitation by femtosecond laser pulses at 795 nm.31 The SA in aqueous suspensions of DNDs was characterized by an anomalously high saturation intensity. © 2017 American Chemical Society

Typically, operation regimes requiring high saturation intensity are not desirable due to fast degradation of the SA material. Indeed, recently it was reported that under intense laser irradiation of suspensions of onion-like carbon or multiwalled CNTs in N,N-dimethylformamide32,33 and suspensions of multiwalled CNTs in tetrahydrofuran34 the sp2 nanocarbon species reacted with molecules of the solvents, resulting in the formation of new compounds and irreversibly changing the optical properties of the suspensions. On the contrary, aqueous suspensions of nanodiamonds are resistant to mechanical and chemical degradation under periodic laser irradiation of high intensity.35 The aim of this work is to extend the SA study of DNDs to aqueous suspensions of fully disaggregated 5 nm DND particles upon excitation by nanosecond laser pulses at the wavelengths of 532 and 1064 nm.

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EXPERIMENTAL METHODS DNDs were prepared at a vendor site by detonation of an oxygen-deficient explosive mixture of trinitrotoluene with hexogen (50:50 wt %) in a closed steel chamber using CO2 cooling media. The product, detonation soot, is a mixture of up to 30 wt % of diamond particulates with other carbon allotropes as well as metallic impurities. DNDs were purified by oxidation of the soot in a mixture of nitric-sulfuric acids in the presence of sulfur oleate at high temperature. The residual content of incombustible impurities in DNDs was estimated to be 1 wt %. These DNDs received from the vendor were additionally purified with HCl at Adamas Nanotechnologies, reducing the Received: January 23, 2017 Revised: March 29, 2017 Published: March 29, 2017 8630

DOI: 10.1021/acs.jpcc.7b00656 J. Phys. Chem. C 2017, 121, 8630−8635

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that is, any peaks in the absorbance spectrum are absent. The insert in Figure 1b shows the particle size distribution obtained by the dynamic light scattering technique using a Malvern Zetasizer Nano ZS instrument. It can be seen that the distribution is bimodal with peaks corresponding to 5 and 18 nm, where nearly 70% of all nanoparticles have diameters varying between 3.5 and 10 nm. Experiments were carried out using a well-known z-scan technique with an open aperture36 on an automated z-scan system with a monochromatic laser pump37 (Figure 2). Single-

metal content to 0.4 wt %. Purified DNDs were suspended in deionized (DI) water by sonication and processed in a Retsch (Haan, Germany) planetary mill for 4 h using 300 μm zirconia beads. After milling, the product was treated at 400 °C in air for 3 h to remove residual graphitic carbon. After the treatment, the product was resuspended in DI water at 1% w/v by sonication. Centrifugation at 25 000g forces for 2 h was used to extract DND particles with 5 nm in diameter, as measured by the dynamic light scattering (DLS) technique. The suspensions exhibited negative zeta potentials (ζ = −45 mV) at neutral pH. The size distributions and ζ potential were measured at 25 °C using a Zetasizer (Nano-ZS series, Malvern, U.K). The sample was concentrated to 1−5 wt % batches. The X-ray diffraction pattern of DNDs shown in Figure 1 was acquired using 0.1541 nm CuKα radiation on a D2

Figure 2. Schematic of the z-scan experimental set up.

frequency radiation of the fundamental or second-harmonics of a 1 Hz single-mode YAG:Nd3+-laser served as the laser pump. The M2 parameter characterizing the laser beam quality, measured by a profile meter BC 106-VIS (Thorlabs), was equal to 1.03. The diameters of the laser beams at wavelengths of 1064 and 532 nm measured at 1/e2 of the maximal intensity were 1.7 and 1.3 mm, respectively. The durations of the laser pulses (τp) at 1064 and 532 nm, measured using a high-speed photodetector SIR-5 (Thorlabs) and digital oscilloscope TDS7704B (TEKTRONIX) with a bandwidth of 7 GHz, were 21.2 and 13.6 ns, respectively. Laser light was focused by a lens with a focal length of 192 mm (the point z = 0 corresponds to the waist of the focused beam), with the diameters (2w0) of the laser beam waist at 1064 and 532 nm being equal to 173 and 117 μm, respectively, and the Rayleigh lengths (z0) being of 22.0 and 20.2 mm, respectively (z0 = πw02/λ, where λ is wavelength). The laser pulse energy was measured using a PM100USB device with ES111C pyroelectric measuring head (Thorlabs). Measurements were performed by the open-aperture z-scan configuration shown in Figure 2. The nonlinear transmittance T of the optical cuvette filled with suspension was measured as a function of the cuvette position z along the focused laser beam axis. The path length of the suspension was 1 mm. To eliminate the effect of interference of reflected beams from the front and rear sides of the cuvette on the z-scan results, the cuvette was inclined at an angle of 45° to the z axis37 (see Figure 2). The nonlinear transmittance was determined according to the equation T(z/z0) = Eout(z/z0)/Ein, where Eout(z/z0) is the energy of the laser pulses at the output of the cuvette located at a distance z/z0 from the beam waist and Ein is the input laser pulses energy.

Figure 1. (a) X-ray diffraction pattern of the DNDs and HRTEM image of a nanodiamond particle projected along the [011] zone axis (inset) and (b) optical density spectra of aqueous DND suspensions at nanoparticle concentrations of (1) 0.25, (2) 0.5, (3) 1, and (4) 2.5 wt % and the volumetric size distribution of nanoparticles (inset).

PHASER (Bruker) diffractometer. One can observe the diamond reflections from the {111}, {220}, and {311} planes at 2θ = 43.9, 75.3, and 91.5° respectively. The insert in Figure 1a demonstrates a high-resolution transmission electron microscopy (HRTEM) image of a single DND particle, where the interplanar spacing is ∼0.2 nm, consistent with the {111}-type planes of crystalline diamond. HRTEM experiments were performed on a JEOL 4000EX microscope operated at 400 kV. Figure 1b shows the absorbance spectra of the studied suspensions with different particles concentrations C, measured relative to a glass cuvette containing distilled water. One can see that the optical density of the suspensions monotonically decreases with an increase in the excitation light wavelength;

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RESULTS AND DISCUSSION Figure 3 shows the normalized transmittance Tn(z/z0) of the 2.5 wt % DND suspension as a function of input laser pulse energy (Ein) at wavelengths of 532 and 1064 nm, where Tn(z/ z0) = T(z/z0)/T0, and T0 is linear transmittance. The obtained dependences Tn(z/z0) are symmetric relative to the point z/z0 8631

DOI: 10.1021/acs.jpcc.7b00656 J. Phys. Chem. C 2017, 121, 8630−8635

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deviate from the corresponding approximate curves. This can be explained by the effect of nonlinear light scattering39−43 and reverse SA,44−46 leading to the optical limiting, the contribution of which was not taken into account in the eq 2. Indeed, additional experiments demonstrated that a small dip against a background of relatively big peak in the laser beam waist area appears on the Tn(z/z0) dependence curve when a pulse energy was increased to 130 μJ. At higher laser pulses energies, the depth of the dip further increases. Figure 4 shows the parameters Isat,2, α0,2, and αns,2 as a function of the concentration C at the wavelength of 532 nm of

Figure 3. Normalized transmittances of the 2.5 wt % DND suspension as a function of the parameter z/z0 at (a) 532 and (b) 1064 nm excitation, obtained by z-scanning at different laser pulses energies.

= 0, and that demonstrates SA in aqueous DND suspensions at visible and infrared regions of the optical spectrum. To approximate the experimental dependences shown in Figure 3, one can use the following equations describing the propagation of the light pulse in the DND medium that exhibits the SA (see, e.g., refs 1, 5, 14, and 38)

d I (z ) = − αI (z ) d z α = αns +

α0 1 + I /Isat

(1)

(2)

where I (z) is the incident radiation intensity, αns is the linear absorption factor (the sum of absorption between different energy levels) not involved to SA, α0 is the absorption factor characterizing the SA at infinitesimal incident radiation intensity, and Isat is the saturation intensity (the intensity necessary to reduce the absorption coefficient to half of the initial value, considering αns = 0).6 A solution of the system of eqs 1 and 2 provides the expression for the normalized transmittance Tn ⎡ I /I + 1 + α0/αns ⎤−α0 / αns Tn = ⎢ out sat ⎥ ⎣ Iin/Isat + 1 + α0/αns ⎦

Figure 4. (a) Absorption factor α0,2, characterizing the SA at infinitesimal incident radiation intensity. (b) Linear absorption factor αns,2 not associated with the SA. (c) Saturation intensity Isat,2 as a function of nanoparticles concentration C in the suspension, measured at 532 nm.

the second harmonic of YAG:Nd3+ laser. It can be seen that the α0,2 and αns,2 data obtained for various C can be approximated by the linear relationships α0,2 = k0,2C and αns,2 = kns,2C,where k0,2 = 0.248 cm−1 wt %−1 and kns,2 = 3.34 cm−1 wt %−1. This means that the absorption factors α0,2 and αns,2 are directly proportional to the concentration C, but the ratio R2 = α0,2/αns,2 = 0.068 does not depend on C. From Figure 4 one can see that Isat,2 is independent of C within experimental error. Indeed, in the stationary case, according to Svelto,1 the following equation for a two-level system is valid

(3)

where Iin and Iout are the input and output radiation intensities respectively and Iin = Ein/(τpS(z)), where S(z) is the crosssectional area of the laser beam as a function of the coordinate z. It is clear that the relation ln T0 = −(αns + α0) is true, and, besides, in a first approximation, we can assume that Iout = T0· Iin. This allows one to use eq 3 to approximate the experimental data shown in Figure 3a,b, with two unknown parameters Isat,i and α0,i, where i = 1, 2 (Isat,1 and Isat,2 are the saturation intensities at 1064 and 532 nm, respectively, and α0,1 and α0,2 are the parameters α0 at 1064 and 532 nm, respectively). Figure 3a shows that the experimental data Tn(z/z0), obtained at Ein = 5.7 and 13 μJ are well described by eq 3. The experimental data obtained at larger values of Ein = 33 μJ and Ein = 84 μJ slightly

Isat = ΔE/(2στ )

(4)

where ΔE is the energy of the quantum transition, σ is the absorption cross-section, and τ is the lifetime of the upper energy state. Obviously, the absorption cross-section as well as the lifetime of the upper energy state of the electron transition is not dependent on the concentration of the nanoparticles in the liquid. Therefore, Isat is also independent of C. The average value of Isat,2 is equal to 5.9 MW/cm2. As a result of 8632

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≈ 1. Materials intended for use as saturable absorbers for modelocking must have a small Isat, wherein the R factor should be as large as possible. At nanosecond excitation, the saturation intensities for suspensions of DNDs and single-walled CNTs are almost the same; however, the R factor for DND suspension is significantly lower than 1. This means that DND suspensions are less suitable for creating a passive Qswitch than graphene or single-walled CNTs. However, the obtained results are important for the characterization of nonlinear optical properties of DNDs and may be useful in other nonlinear optical applications where high robustness of nanodiamond particles under high-intensity irradiation is important. The experimental results obtained in this work suggest the possibility of using aqueous DND suspensions to shorten the duration and remove the pedestal (“tail”) of the nanosecond laser pulses over a wide spectral range of 532− 1064 nm.

approximation of the z-scan experimental data obtained at 1064 nm (Figure 3b), it was determined that Isat,1 = 14.1 MW/cm2, α0,1 = k0,1C, and αns,1 = kns,1C, where k0,1 = 0.0535 cm−1 wt %−1 and kns,1 = 0.751 cm−1 wt %−1. We can see again that the ratio R1 = α0,1/αns,1 = 0.070 does not depend on the concentration of nanoparticles in suspension. Upon comparison of the parameters determined at 532 and 1064 nm, it follows that the SA in the studied DND suspension is more pronounced in the visible than in the infrared spectral region. Approximating the results obtained at the wavelengths of 532 and 1064 nm by a linear function, it can be predicted that Isat ≈ 10 MW/cm2 at 795 nm, the commonly used wavelength of femtosecond lasers. It should be noted that the saturation intensities of aqueous DND suspensions are of the same order of magnitude as that measured for single-walled CNTs (see, e.g., refs 6 and 38). Equation 3 can also be used for analysis of the experimental results of SA observed in aqueous DND suspensions with average particle sizes of 50 nm with femtosecond excitation.31 As a result, it was established that at 795 nm femtosecond excitation, Isat = 88 ± 11 GW/cm2, which practically coincides with the value of Isat, obtained for free-standing graphene polymer composite films irradiated using 1030 nm laser pulses with duration of 340 fs.47 It should be noted that besides graphene, the SA was observed in other 2D nanomaterials such as layered molybdenum dichalcogenide semiconductors MoX2 (X = S, Se, Te)48 and black phosphorus nanosheets.20,49 In accordance with Zhang et al.20 at the same linear absorption and excitation conditions, suspensions of black phosphorus nanosheets suspensions show better SA response than suspensions of graphene and MoS2. In our experiments, the laser pulse duration is more than 105 times longer than that reported previously,31 and the value of Isat is ∼9 × 103 times less than that obtained at femtosecond laser excitation. The inverse proportional dependence of the saturation intensities ratio on the ratio of exciting laser pulse duration can be associated with nanosecond time scale relaxation of the upper excited state of the quantum transition. Indeed, DNDs have numerous defects, vacancies of different nature, and surface groups,26,27 which contribute to broadband luminescence.28,50,51 The SA in the studied DND suspensions may occur as a result of electronic transitions of dimer chains (so-called Pandey chains) fixed on the surface of a nanodiamond particle52 or luminescence quantum transitions. According to Smith et al.,53 the lifetime of the upper state of excited luminescent NV centers of nanodiamonds can reach up to 25 ns, which can lead to Isat decreasing by several orders of magnitude upon the transition from femtosecond to nanosecond excitation laser pulses. Another important nonlinear parameter characterizing SA is the ratio54 R=

exp( −αnsL) − exp[−(αns + α0)L] 1 − exp( −αnsL)

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CONCLUSIONS Impulse nonlinear bleaching of 5 nm detonation nanodiamond suspensions due to saturable absorption was observed under irradiation with nanosecond laser pulses at 532 and 1064 nm excitation. The saturable absorption was observed over a wide range of nanoparticle concentrations. It was found that the saturation intensity at 532 and 1064 nm is 5.9 and 14.1 MW/ cm2, respectively. The ratio of the saturable loss to the nonsaturable loss does not depend on the DND concentration in the suspensions and was found to be ∼0.07 at both 532 and 1064 nm excitation wavelengths. The results obtained indicate that the 5 nm DND suspensions are suitable for optical limiting only at relatively high intensities of the incident radiation. Because of the robust nature of diamond particles, they can withstand high-intensity laser impulses without degradation, and operational regimes with high saturation intensities become possible.

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AUTHOR INFORMATION

Corresponding Author

*Tel: +7(3412)218955. E-mail: [email protected]. ORCID

Gennady M. Mikheev: 0000-0003-3607-5795 Notes

The authors declare no competing financial interest.

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ACKNOWLEDGMENTS This work was financially supported by RFBR (project No 1642-180147). REFERENCES

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(5)

of the saturable loss, {exp (−αns L) − exp [−(αns+α0) L]}, to the nonsaturable loss, {1 −exp (−αns L)}, where L is the SA material thickness. At low losses, eq 5 is transformed into the expression R = α0/αns. According to the results obtained above (Figure 4), R does not depend on the concentration. In our case, the ratio of the saturable loss to the nonsaturable loss, R1 and R2, found at 1064 and 532 nm was 0.070 and 0.068, respectively. Thus the relationships R1 ≈ R2 ≪ 1 are true. In accordance with Yamashita et al.54 for graphene and CNTs, R 8633

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