Indian Journal of Pure & Applied Physics Vol. 43, August 2005, pp. 596-601 Simple diffusion wave analyzer K Sreekumar Laboratory of Photothermal Sciences, Department of Physics, University of Kerala, Thiruvananthapuram 695 581 Received 17 December 2004; accepted 7 June 2005 A simple, cost-effective, compact and efficient photothermal diffusion wave analyzer for 1 Hz-150 kHz frequency band has been developed and analyzed. The sensitivity is 12 nV and the total error is about 1.5% at 60 dB dynamic reserve, excluding the laser intensity variation that may be corrected. The input voltage and current noises are 15nV/ Hz and 2 fA / Hz , respectively. The low power consumption of about 4 W is advantageous for long time off-line applications. The instrument has been used for the metrology of silicon wafers by radiometric simulations. Results regarding the studies on transport parameters and contamination control are presented. Keywords: Diffusion waves, Photothermal radiometry, Laser diode, Wafer metrology IPC code: H01L29/861 1 Introduction Diffusion waves arise when the classical diffusion equation is coupled to an oscillatory force function such that the time derivative is only first order. They lack wave fronts, cannot be beamed and do not travel very far, yet form the basis of several revolutionary measurement technologies1-3. The most common oscillatory driving function is a modulated light source and the method branches to photothermal (PT) diffusion wave sciences. Spectroscopy of thin film semiconductors, opaque samples and biological specimens, surface and subsurface imaging and tomography, quantum yield studies of photonic materials, characterization and quality control of semiconductors for micro and nano electronics applications are a few key areas illustrating how this unique technique leads to remarkable advances in the characterization and metrology of materials1. In this paper, we present the design, performance analysis and some applications of a laser photothermal diffusion wave analyzer (DWA). The instrument is simple, cost effective, compact and efficient with performance figures comparable with those of an average commercial assembly. This analog design needs only locally available components and very little skill for implementation compared to its digital counterpart, which is more stable and drift free. 2 Design of the DWA The essential sections of the analyzer are a modulated laser source, source of modulation with sinusoidal and orthogonal outputs, low noise ac amplifier and a lock-in or phase sensitive detector (PSD) for signal processing (Fig. 1). 2.1 Modulated laser source The source of excitation (pump) is a laser diode (LD) that can be modulated over a wide bandwidth. Circuits around U6, U7 and Q2 (Fig. 1) form a grounded-load constant current source whose output current is I L = Rf V1 / Ri Rs [A] …(1) that drives the laser diode4. Shunting MOSFET Q3 causes sinusoidal negative modulation of the laser intensity without exceeding the preset peak power of the laser diode. The photodiode (built inside LD module) current is sampled using U8 and U9 for correcting against any possible intensity fluctuations. Conventional automatic power control (APC) scheme is not employed, as at lower frequencies (say, a few Hertz) the feedback integration time needed is too long to cause overshoot in the laser current that may permanently damage the diode. The load current is adjusted using V1. The soft-start circuit (Q4 and Q5) offers protection from ON/OFF transients. The maximum diode current is about 200 mA with the present circuit and can be delivered up to a load of about 60 Ω. We have demonstrated the driver with an LNCQ-05 PS (Panasonic) laser diode (660 nm, 50 mW) whose operating current is 75 mA and threshold current is 35 mA. At 1 kHz, about 95% sinusoidal 597 Fig. 1—Circuit schematic of the DWA SREEKUMAR: SIMPLE DIFFUSION WAVE ANALYZER 598 INDIAN J PURE & APPL PHYS, VOL 43, AUGUST 2005 modulation is achieved with 0.2V (peak to peak) signal when V1 is 2V. Over a frequency band of 1 Hz-50 kHz, the total harmonic distortion is below 2%, at 100 kHz it is about 3.5% and is about 6% at 150 kHz. A multi-element glass lens with numerical aperture of 0.476 is used for collimation5. Operational trans-conductance amplifier U5 generates triangular and quadrature square wave references. The triangular signal is sine converted for laser modulation17. The integrating capacitor C is 100 nF for 1-100 Hz, 10 nF for 100-1000 Hz, 1 nF for 110 kHz and 0.1 nF up to 150 kHz. VR1 tunes the frequency. 2.2 Signal processing: Phase sensitive or lock-in detection The principle of PSD is well discussed in literature and it has been shown that for the detection to be free from harmonic errors (fundamental only response) with a square wave reference (as in the present case), the signal should be sinusoidal6. The sinusoidal laser modulation is advantageous in this regard. The front end is a high performance instrumentation amplifier U1 with gain 10. The overall stable gain of the cascaded amplifier can be varied from 0.01 to 104 so that the full-scale (FS) input sensitivity is adjustable from 1 V to 1 μV. The 50 and 100 Hz notch filters (optional) are included for suppressing line frequency components17. Spice simulation shows that at 1 kHz, the input voltage noise is about 15nV/ Hz and current noise is about 2 fA / Hz for a gain of 10. The achieved common mode rejection ratio (CMRR) is about 75 dB and it decreases by 20 dB/decade (approximately) above 1 kHz. Ground loop minimizing techniques like floating guard, double-shielded cabling etc. may be used for improving CMRR (Ref. 7). The gain linearity error is less than 1% over the entire bandwidth. The suitably amplified signal is subjected to phase sensitive detection in U2 for in-phase detection. The second order low pass filter around U3 has variable time constant determined by R with equivalent noise bandwidth 1/ 8 RCT . The slew rate and offset current considerations of U3 limit the time constant between 1 ms and 50 s and U4 provides sufficient output expansion. A similar section is used for quadrature detection. The operating frequency is limited at the lower end by the stability of the signal generator and the upper end pump signal distortion and amplifier bandwidth are the major factors. 3 Performance Analysis 3.1 Dynamic reserve and output stability The transfer function of the detection system, assuming gain 2 of U2, is VO (rms ) = 2Gac GdcVS cos φ [V] …(2) where Gac and Gdc are the ac and dc gains, respectively, φ is the phase of the signal with respect to the reference and VS is the signal amplitude. For calculating the dynamic reserve (DR), we have considered the value of an asynchronous voltage that causes 5% deviation in the FS output. The ratio of this asynchronous amplitude to the signal amplitude for FS reading is the DR. For an FS input of 10 mV (amplitude) the said asynchronous input (from a signal generator) is 10 V (amplitude) and the DR is 60 dB. With 10 mV (rms) input, the DC gain required for an output FS display of 10.00 (rms) is 500. DR can be increased by decreasing ac gain while increasing dc gain, keeping their product constant. Output stability is principally determined by the drift in the output-offset voltage of U2, which is about 5 μV/°C (Ref. 8). For a change of 10°C in the operating temperature, this causes about 0.35% error for 60 dB DR. 3.2 Total error, sensitivity and power consumption of the DWA The total error is evaluated with time constant 10 s and 1μV FS range for 60 dB DR over 10°C change in operating temperature. 15nV/ Hz input noise contributes about 2 nV (rms) output noise after low pass filtering (equivalent noise bandwidth is 1/80Hz ) and the error is about 0.2%. After 60 s, the exponential convergence of the filter adds about 0.3% error. The gain error is 1% and the drift is 0.35%. Orthogonality and DC gain errors are negligible. The rms of these uncorrelated error is about 1.2% and the sensitivity is 12 nV. The drift in the laser intensity for 5 hours continuous operation is about 2% (may be compensated using the photodiode) and the total error of the analyzer amounts to be about 2.5%. The power consumption of the DWA is about 4 W enabling battery based operation. This ensures more safety to the LD, improved DR, portability and the feasibility of long time (off-line) operation. SREEKUMAR: SIMPLE DIFFUSION WAVE ANALYZER 4 Some Applications of the DWA: Photothermal Radiometry (PTR) of Si Wafers 4.1 Theory of PTR of semiconductors When a semiconducting material is excited with a harmonically modulated beam of super band-gap light, thermal and plasma waves are generated, the former arises from direct lattice heating and the latter from the periodically generated excess carriers diffusing away from the source (charge plasma diffusion wave), until they recombine with opposite carriers or defects/impurity centers after an average life-time (τ)9-11. Each recombining photo-excited carrier is equivalent to a blackbody radiator and the amplitude and phase of the corresponding IR emission is a complex function of the carrier density (Δn) which depends on the diffusion coefficient (D), surface recombination velocity (s) and life-time (τ) of the concerned carrier type. The quantitative noncontacting evaluation of these parameters is essential at different stages of the production line of micro and nano electronic devices. The technique has been emerging as an innovative metrology tool in the micro and nano electronic industrial scenario12,13. It has been established that for a good quality (defect free) silicon wafer, above a few hundreds of Hertz, the plasma wave content dominates the slow thermal wave contribution9-11. For a wafer of thickness L with unpolished back surface having strong optical absorption at the front (illuminated) surface, the PTR signal can be simplified to yield S= CN (1 − e − σL ) 2 [W] Dσ( Dσ + s ) (1 + Re −2σL ) …(3) where CN is an instrumental constant, σ = (1 + j ω τ) / Dτ [m−1] …(4) 599 4.2 Experimental Details The infrared emission is collected using two offaxis parabolic mirrors (Fig. 2) and detected with an HgCdTe element (2-12 μm) of 1 mm2 active area. The laser spot size is made 3.5×5 mm (approximately) by adjusting the collimating lens so that the onedimensionality criterion is ensured to satisfy the model (spot diameter > detector size). The germanium window blocks the pump laser component. The frequency scan width is 200 Hz to 100 kHz, which is the plasma-dominating region. The PTR amplitude has been recorded at 10 kHz for different pump powers and between 10 and 40 mW, a linear response has been observed. This ensures a linear carrier generation, which is essential for the successful application of the above theory14. Figure 3(a & b) shows the PTR amplitude (⎜S⎪) and phase [tan−1(ImS/ReS)] data against the modulation frequency sweep and the best fit curves from the center of a boron doped (10-15 Ωcm), p-Si wafer of thickness 500±20 μm at 300 K. Simultaneous fitting of the amplitude and phase eliminates multi-pair solutions in the determination of τ and s. The best-fit values are D=17 (±2.2%) cm2/s, s=105 (±2.4%) cm/s, and τ=240 (±1.6%) μs. Wafer annealing is an important process at different device fabrication stages and heavy metal ions (contaminants) diffusing into the wafer during annealing act as recombination centers influencing τ that in turn deteriorates the device performance. We have intentionally annealed the above wafer at 800°C for 1 hour. The SiO2 layer thus grown has an approximate thickness of 0.3 μm. This has been etched using an HF:H2O (6:1) solution (etch rate is 1200 Å/minute) and then rinsed in distilled water15. The complete removal of SiO2 is verified by resistance measurement. Figure 4 shows the quadrature frequency response of the PTR signal from unannealed and annealed is the complex plasma wave vector associated with the excess carrier concerned and R= Dσ − s Dσ + s …(5) The real and imaginary components of S are available at the in-phase and quadrature output of the DWA, from which the amplitude and phase can be calculated. Fig. 2—Experimental arrangement for photothermal radiometry 600 INDIAN J PURE & APPL PHYS, VOL 43, AUGUST 2005 (a) (b) wafers whose peak (at fC) roughly indicates the corresponding carrier life-time according to the relation 2πf C τ = 1 , which may be used as a guessparameter for simulation10. Simultaneous amplitudephase simulation shows that the once annealed wafer has τ=105 (±1.5%) μs, s=132 (±2%) cm/s and D=17.3 (±2.2%) cm2/s. After two cycles of annealing, τ=34 (±1.5%) μs and s=180 (±2.2%) cm/s without considerable change in D. The result is in close agreement with the fact that annealing is a source of Si wafer contamination due to heavy metals and ions (life-time killers) from the furnace atmosphere. At 660 nm, the optical absorption length is about 1.5 μm and the dynamics of near surface excess carriers are reflected in the PTR response. In all the above measurements, data have been collected from the center of the wafer with peak pump power of about 35 mW. For typical microelectronic grade Si wafers, the reported values of τ, D and s are, respectively, in the range 1-1000 μs, 10-40 cm2/s and 1-500 cm/s16. At low modulation frequencies less than fC (say, 500 Hz), well in the plasma-dominating region, these values correspond to a real valued σ and R becomes 1. Now if L > diffusion length Dτ , Eq. (3) simplifies to S ∝ τ/ D Fig. 3—(a) Experimental and simulated PTR amplitude against modulation frequency. The crowded portion is due to the logarithmic scale; (b) experimental and simulated PTR phase against modulation frequency …(6) It has been reported16 and verified in our experiment that D is the least sensitive parameter to processing and surface conditioning. Thus, S can be a measure of τ if properly calibrated by actual simulation. We have applied this technique to three different points radially outwards for a wafer of D=7.6 (±2.2%) cm/s2 and τ=110 (±2%) μs at the center and the τ values are compared (Table 1) with those obtained from simulation at these points. The deviation may be due to the approximations made. The fall in τ outwards may be related to the crystal growth process and is consistent with the literature16. Table 1⎯ Minority carrier lifetime estimated at radial points by simulation (error <±2.4%) and amplitude measurement at 500 Hz Fig. 4—PTR Quadrature response of the annealed and unannealed wafers Distance between the centers of wafer and laser spot cm Simulated lifetime μs Measured lifetime μs 1 2 3 88 70 47 67 62 35 SREEKUMAR: SIMPLE DIFFUSION WAVE ANALYZER 5 Results and Discussion A cost-effective, simple, compact and efficient diffusion wave analyzer has been designed, developed and analyzed. The rough estimate is about 150 Dollars. For further cost reduction, an active LD, typically of 630-700 nm at 30 mW, may be collected from a damaged laser printer or CD writer. The instrument is a general-purpose photothermal/ photoacoustic analyzer. The major source of error is the drift in the demodulator chip. The analyzer has been used for the metrology Si wafers and estimated parameters are in good agreement with the literature values. The quadrature channel has been used for the fast estimation of minority carrier life-time, which is a crucial parameter in device modeling. At 660 nm, the absorption length in Si is about 1.5 μm and the measured parameters are those of the near surface excess carriers. The instrument has been used for contamination analysis too. For probing deep lying carriers, higher wavelengths may be used. 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