Enhanced Force Measurement Techniques to Extend Optical Trapping towards Nanoscale Manipulation

Arvind Balijepalli Thomas W. LeBrun and Jason J. Gorman

Manufacturing Engineering Laboratory National Institute of Standards and Technology Gaithersburg Maryland E-mail: {arvind, lebrun, gorman}@nist.gov

Satyandra K. Gupta

Department of Mechanical Engineering University of College Park College Park, Maryland E-mail: skgupta@umd.edu

AbstractWe have developed a new force measurement technique based on the random thermal motion of a nanoparticle in an optical trap. We demonstrate this method, in one-dimension, through numerical simulations and laboratory experiments. We show that computer simulations successfully recover the prole of the optical trapping force, beyond the inection point of the trapping potential for a range of particle sizes. We show, through laboratory experiments, that this technique is effective in recovering higher order terms, in a power series expansion of the trapping force, beyond the widely reported linear trap stiffness. We also show that the rst order (stiffness) term in our series expansion is consistent with values reported in the literature. Keywordsoptical trapping; optical trapping potential; FokkerPlanck equation; Simulations; Brownian Motion1

I. I NTRODUCTION The development of complex three-dimensional nanodevices has been hindered by the lack of effective techniques to prototype and test functional devices. Optical trapping could allow the assembly of heterogeneous components at the nanoscale and has long been used to manipulate larger spherical particles. The manipulation of non-spherical particles has been demonstrated with optical tweezers [1], but the effective controlled manipulation of particles at the nanoscale requires a better understanding of the behavior of weakly bound nanoparticles in an optical trap, as well as new techniques to characterize the trapping force exerted on trapped nanoparticles. Existing force measurement methods assume a linear trapping force in a region very close to the center of a strong trap and were developed for large micrometer sized particles [2]. These techniques are incomplete for use with nanoparticles, which experience large excursions from the trap center on account of Brownian motion and optical binding forces that are not well approximated by a simple spring. Therefore, new force measurement techniques are required for the use of optical tweezers in precise nanoscale assembly. The thermal motion of nanoparticles in an optical trap poses considerable challenges, not just to the accurate control and
1 This material is declared a work of the U.S. Government and is not subject to copyright protection in the United States. Approved for public release; distribution is unlimited.

placement of nanoparticles, but also in some cases to the formation of stable traps [3]. One method to overcome this problem is the suppression of Brownian motion using active feedback control techniques [4], which require an accurate estimate of the trapping force to function effectively. We have previously developed one such force measurement technique [5], suitable for use with nanoparticles, where we apply a rapid step to a particle conned in an optical trap and estimate the trapping force from the response of the particle to this step input. Here, we develop a new force measurement technique, which utilizes the random thermal motion of a particle, initially conned within the trap, to sample and recover the trapping force beyond the inection point of the trapping potential. The inection point is used as a point of reference in our measurements to indicate a point on the force curve, which lies sufciently away from the trap center so that the trapping force can no longer be approximated by a spring stiffness. Finally, our force measurement technique is a generalization of a force measurement method, which uses the equipartition theorem to relate the spring stiffness of an optical trap to the thermal energy using the relationship 1 < x2 >= 1 kb T , 2 2 where is the spring constant of the optical trap, < x2 > is the variance of the particle distribution in the trap, kb is Boltzmanns constant and T is the temperature [6]. This force measurement technique is demonstrated using numerical simulations and laboratory experiments. The details of the force measurement are discussed next, followed by results and conclusions. II. M ETHODS A small particle initially conned in an optical trap undergoes a constant random movement due to Brownian motion. This particle eventually escapes the trap after a nite time, dependent on the depth of the potential, particle size and temperature. For an ensemble of particles, initially located close to the center of an optical trap, the time-evolution of the probability density function (PDF) W (x, t), a function of position x and time t, is described by the Fokker-Planck equation [7], given for a one-dimensional system by (1), where D = kB T is the diffusion constant, = 6a is the Stokes drag coefcient for a spherical particle with radius

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a in a uid with viscosity , kB is Bolztmanns constant and T is the temperature of the uid. The force from the optical trap is given by F (x) = x U (x), where U (x) is the conservative component of the optical trapping potential, while non-conservative scattering components of the trapping force are ignored. 1 1 2 W (x, t) = [W (x, t) F (x)] + W (x, t) t x D x2 (1)

TABLE I S IMULATION PARAMETERS Diameter (d) Potential Depth () Simulation Time-step (kB T) (ps) (nm) 150 0.211 50 0.500 50 200 300 1.687 100 Fluid medium: water at T =293 deg K Beam-diameter 2=800 nm for all cases

If the probability density function W (x, t) is known, then (1) reduces to a rst order differential equation in F (x), which can then be solved to recover the trapping force. By constructing the probability density function W (x, t) from the position trajectories of several particles, obtained either from simulations or laboratory experiments and substituting it into the Fokker-Planck equation, we can recover the optical trapping force. This is performed by rst calculating the histogram, normalized by bin width, of the particle positions at each time-step, which yields the PDF of particle positions as it changes with time. We can then calculate the optical trapping force F (x), by substituting W (x, t) into (1), integrating both sides over position and rearranging the terms as shown in (2), where we can set the constant of integration to be zero by dening x = 0 to be the minimum of the trapping potential. F (x) =
t W (x, t)dx D x W (x, t) W (x, t)

A. Simulation Results We demonstrate the thermodynamic force measurement method using data generated using a one-dimensional Brownian dynamics simulation [5], for an ensemble of particles initially located at the center of a Gaussian optical trapping potential. Three separate simulations are performed for silica microspheres with diameters of 150 nm, 200 nm and 300 nm x2 x in a Gaussian potential (F (x) = x U (x) = 2 e 22 ) with beam size, = 400 nm and potential depth (). We rst set the potential depth for the 200 nm particle to be 1 kB T and 2 then scale the potential depth of the 150 nm and 300 nm with volume [8]. While this approximation is only rigorously valid for very small particles, it provides sufcient accuracy for our current measurements. The simulation parameters for each of the three cases are summarized in Tab. I. The simulation runs at a time-step of 50 ps and 100 ps, depending on particle size and the output is sampled uniformly at 1 s to collect a timeseries of position for each particle. The simulation is repeated for 600 000 particles and we perform the analysis by grouping the data into groups of 50 000, resulting in 12 independent force measurements for each case. We initialize each simulation with a distribution of particle positions, obtained by numerically solving the Fokker-Planck equation, given in (1), up to a time when the particles in the ensemble completely ll the trap and have substantially leaked out. This is done to reduce the amount of computation time required to complete the simulation. Moreover, using the Fokker-Planck equation, to initialize the simulation, in this manner does not affect the outcome of the calculation. The simulations allow us to quantify the effect of stochastic noise from individual particle trajectories, on the measurement - an important effect that must be taken into account to use this technique in the laboratory. At the start of each simulation, the particles in the ensemble are located at the center of the optical trap and the PDF is a sharp peak. As the simulation progresses, we nd that the ensemble of particles ll the trap in a very short time, typically a few milliseconds, and then slowly leaks outside the trap over a longer time-scale. A representative position distribution for 200 nm diameter particles, calculated over a spatial range of 10 with a bin width of 160 nm, is shown in the inset of Fig. 1 at t = 2.00001 s. From the plot, we see a central peak close to zero, which represents the particle distribution inside the optical trap, with a standard deviation of approximately 400 nm and exponentially decaying tails in the region where the particle has left the trap and undergoes nearly free particle

(2)

We are interested in calculating the trapping force at long times, where the probability distribution can be assumed to be in a quasi-steady state. In such an approximation, the rst term in the numerator of (2) is negligible, resulting in the simplied expression for the trapping force shown in (3), which is just the Einstein-Smoluchowski relationship (in a quasi-steady state) with drift velocity vd . F (x) = kB T
x W (x, t)

W (x, t)

kB T vd D

(3)

The trapping force is calculated numerically, for simulation as well as laboratory data, by evaluating the expression in (4) to obtain the derivative of the PDF, with bin size x and substituting the results into (3). It is important to note that the results of the numerical derivative must be kept aligned with W (x, t). W (x + x, t) W (x x, t) W (x, t) x 2 x III. R ESULTS The force measurement technique described in the previous section is validated using data generated from numerical simulations of optical trapping, as well as experimental data measured using an optical tweezers instrument. The results of these measurements are described next. (4)

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TABLE II S IMULATION R ESULTS Diameter Pct Rel ErrSE Pct Rel ErrSE (nm) Measurement time, t = 2.00001 s 150 10.494 2.341 23.393 1.561 200 3.435 0.992 20.088 0.637 300 2.968 0.176 20.023 0.113 Measurement time, t = 7.000005 s 200 3.839 1.1629 11.152 0.564

diffusive motion. Fig. 1 shows the mean trapping force and standard deviation as a function of the particles displacement, for three particle sizes, using the trapping force analysis technique described in Sec. II. The solid line in the gure is a least squares t to the trapping force data to obtain an estimate of the trap parameters, and . We see from the gure, that we are able to obtain the trapping force beyond the inection point of the trapping potential for all three particle sizes. The results of a least squares t to the force data from each of the three simulations are summarized in Tab. II, which gives the percent relative errors and the standard errors for the trap parameters for well depth () and beam size (). The results, especially the errors in , highlight the importance of the time at which the trapping force is calculated. At the top of the table, the trapping force is calculated from the PDF, W (x, 2.00001), approximately two seconds after the start of the simulations and the force is calculated to a distance 800 nm from the trap center. We see from (3) that the force calculation involves a division by W (x, ts ), therefore at short times, when the probability of nding the particle far away from the center of the trap is small, the force calculation is only numerically stable close to the trap center. On the other hand, at large times as more particles exit the trap, the estimate of the trapping force away from the center of the trap improves. Therefore at very short times, we expect to estimate only the trap stiffness (the rst term in a power series expansion of the force about the trap center) and progressively estimate higher order terms at longer times. Eventually, at very long measurement times we can expect to recover the trapping force prole beyond the inection points of the potential. Here we calculate the trapping force only at two separate times, but this can be extended to the full time range of the simulation to further improve the measurement. Already, at t = 2.00001 s, we are able to recover the trapping force beyond the inection points of the potential, but we see relatively large errors in the t parameter . However, by running a simulation for 200 nm diameter particles to approximately seven seconds (W (x, 7.00005)), the error in the t parameters reduces to 11.152 0.564 for . B. Laboratory Results We also demonstrate this force measurement technique, in one-dimension, in the laboratory using an optical tweezers instrument. The position of the particle is recorded using

Fig. 1. The trapping force as a function of displacement from the trap center, calculated using numerical simulations of glass microspheres in an optical trap. The solid lines are the input force to the simulation and data points indicat the trapping force calculated from the simulation output.

a two-dimensional detector, however based on our previous results [5], it is reasonable to ignore the projection of the particle position on the second detection axis, as well as any out-of-plane motion in this measurement. Two lasers are used in the experiment - a laser with a wavelength of 1064 nm (J20I-8S-12K/BL-106C, Spectra Physics)2 is used for trapping and manipulating nanoparticles, while a diode laser with a wavelength of 640 nm (iFLEX2000, Point Source) is used for fast back focal plane detection [9] of the particle position. The trapping laser is ber launched from a polarization maintaining single mode ber. The beam is split using a non-polarizing beam splitter and then passed through a piezo-electric tip-tilt mirror (PI-S-330.10, Physik Instrumente) or an acousto-optic modulator (LS-110XYNIR, Isomet), which can each scan the beam independently along the X and Y axes. We use the beam path passing along the PI tip-tilt mirror in all our measurements. A telescope is used to expand the beam to ll the back aperture of the microscope objective (Plan Apo 60X/1.40NA oil immersion, Nikon). The telescope and tip-tilt mirror are xed so that the back entrance aperture of the microscope objective forms a conjugate plane with the tip-tilt mirror [10]. The detection laser is also launched from a polarization maintaining ber and is combined with the trapping beam using a dichroic mirror (Model Z640BCM, Chroma Technology Corp.). The trapping and detection beams pass through a second oneto-one telescope before they enter the microscope objective and then pass through the sample cell. When the detection laser exits the sample cell, it is collected by an aspheric lens and reected by a dichroic mirror to pass through a second lens before arriving at the quadrant photo-diode (QPD), which senses the deection of the detection beam due to the motion of the trapped nanoparticle (QPD-2901, New Focus).
2 Certain commercial entities, equipment, or materials may be identied in this document in order to describe an experimental procedure or concept adequately. Such identication is not intended to imply recommendation or endorsement by the National Institute of Standards and Technology, nor is it intended to imply that the entities, materials, or equipment are necessarily the best available for the purpose.

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0.3 0.2 Trapping Force HpNL

0.1 0.

8 106 6 106 4 106 2 106 0

-0.1 -0.2 -0.3 -200

-100

-200 -100 0 0 100 Displacement HnmL

100

200 200

Fig. 2. Optical trapping force calculated for a trapped 1.5 m particle in a weak optical trap. Inset: Probability density function of the particles position in the trap.

for the 1.5 m diameter microspheres, we calculate the optical trapping force as a function of displacement from the trap center, also shown in Fig. 2. We expect the trapping force to exhibit some non-linear behavior away from the center of the trap and therefore we use higher order terms when performing a least squares t to the force data. Since the trapping force is an odd function for a symmetric trap, we t a third order polynomial to the force data of the form F (x) = k0 + k1 x + k2 x2 + k3 x3 and recover the t parameters k0 = 1.643 103 pN , k1 = 1.412 pN/m, k2 = 0.609 pN/m2 and k3 = 6.283 pN/m3 . By using a power spectrum method (a commonly used technique to estimate the stiffness of an optical trap) on the same data set, we calculate the stiffness of the optical trap to be = 1.09 pN/m [4]. This value is consistent with those reported in the literature [11], but differs by 23 % with the rst term (k1 ) of the series expansion (or trap stiffness) using our force method. IV. C ONCLUSIONS We have developed a new force measurement technique based on the thermal noise experienced by a particle in an optical trap and demonstrated this method using numerical simulations and laboratory experiments. When measuring the optical trapping force beyond the inection point of the potential, the relative errors in the measurements of trap strength and trap width were found to be acceptable. Moreover, in laboratory experiments, the rst term in the series expansion of the trapping force is consistent with trap stiffness values published in the literature. R EFERENCES
[1] Agarwal, R., Ladavac, K., Roichman, Y., Yu, G., Lieber, C., and Grier, D., 2005. Manipulation and assembly of nanowires with holographic optical traps. OPTICS EXPRESS, 13(22), pp. 89068912. [2] Visscher, K., and Block, S., 1998. Versatile optical traps with feedback control. Method Enzymol, 298, pp. 460489. [3] Hansen, P., Bhatia, V., Harrit, N., and Oddershede, L., 2005. Expanding the optical trapping range of gold nanoparticles. Nano Letters, 5(10), pp. 19371942. [4] Gorman, J. J., LeBrun, T., and Balijepalli, A., 2009. Control of optically trapped particles for brownian motion suppression. Accepted to be published in the IEEE Transactions on Control Systems Technology. [5] Balijepalli, A., Lebrun, T., Gorman, J., and Gupta, S., 2008. Methods to directly measure the trapping potential in optical tweezers. In Proceedings of SPIE, Vol. 70380V. [6] Capitanio, M., Romano, G., Ballerini, R., Giuntini, M., Pavone, F., Dunlap, D., and Finzi, L., 2002. Calibration of optical tweezers with differential interference contrast signals. Review of Scientic Instruments, 73(4), pp. 16871696. [7] Risken, H., 1996. The Fokker-Planck Equation: Methods of Solution and Applications. Springer. [8] Davis, T. J., 2007. Brownian diffusion of nano-particles in optical traps. Optics Express, 15(5), pp. 27022712. [9] Lang, M., Asbury, C., Shaevitz, J., and Block, S., 2002. An automated two-dimensional optical force clamp for single molecule studies. Biophysical Journal, 83(1), pp. 491501. [10] Fallman, E., and Axner, O., 1997. Design for fully steerable dual-trap optical tweezers. Applied Optics, 36(10), pp. 21072113. [11] Rohrbach, A., 2005. Stiffness of optical traps: Quantitative agreement between experiment and electromagnetic theory. Physical Review Letters, 95(16), p. 168102.

We use a two-step calibration process, described in detail in our previous work [5], to calibrate the response of the QPD. At the end of the calibration procedure, we obtain a mapping that converts the position measurement of the QPD in volts to the position of the particle in micrometers. Next, we create a stationary trap by moving the PI tip-tilt mirror to the center of its range and ensuring that it is properly aligned with the detection beam. We control the intensity of the trapping beam using an electro-optic modulator (Model 350-80/Power Supply: M302RM, ConOptics Inc.) and reduce the beam power until the particle remains in the trap for only a few minutes at a time. The position of the particle in the trap, measured by the QPD in one-dimension, is rst sent through a low-pass lter with a cutoff frequency of 5.28 kHz and then recorded, with a sampling rate of 20 kH, using a National Instruments LabView-based data acquisition system. An important difference between the simulation and laboratory results is that in the laboratory measurements, as currently performed, the particle always remains trapped. Therefore, we expect to only recover the trapping force in a region near the center of the trap. However, on account of using a weak trap, we can expect large enough deviations away from the trap center so that we may recover one or more higher order terms for the optical trapping force, beyond a linear stiffness value. These measurements will be extended in the future to more closely resemble the simulations and thereby allow us to recover the full trapping potential. The force measurement is performed using 1.5 m (Catalog #8150; Duke Scientic) silica microspheres. In each case, the beam power is reduced until the particle distribution broadens and the particle remains conned in the trap for only a few minutes. A single position trajectory is then recorded for two minutes. The inset in Fig. 2 shows the distribution of particle positions for a trapped 1.5 m microsphere, with the standard deviation calculated to be 51 nm. By applying the force analysis method described previously to the PDF, constructed

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