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Aby Joseph Report
Aby Joseph Report
Aby Joseph Report
Submitted by
Aby Joseph
Undergraduate Student (3rd year)
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2. Experimental details
2.1. Reflectivity beamline at Indus-1
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15 16 18
4.2. Summary
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Appendix References
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Acknowledgements
I would like to thank Dr. M. H. Modi (RRCAT, Indore) for this opportunity to work under him. I am grateful to him for a productive and memorable summer internship at RRCAT.
I am also grateful to Mr. Rajkumar Gupta and Mr. Amol Singh (RRCAT, Indore) who played an important role in the experimental work related to this project and also gave their valuable suggestions.
I would also like to express my gratitude to Dr. G. S. Lodha (RRCAT, Indore) for this opportunity to work at RRCAT and his guidance and motivation.
I would also like to express my gratitude to Prof. Dr. Pankaj Srivastava (IIT Delhi) for giving me this opportunity to do my summer internship at RRCAT.
1. Introduction
Thin foils of different materials are used in x-ray region as an absorber and edge filters. Absorbers of different thicknesses are primarily used to reduce the incident intensity. Edge filters are used to selectively absorb high energy spectrum coming from wide energy sources such as synchrotrons, laboratory based x-ray generator etc. Aluminium and Silicon are very important filter materials. Al has a wide bandpass (170 800 ) and is very good for visible light rejection. This filter provides visible light rejection in the range of 10-9. This filter is more durable and easier to process than many other filter materials. Aluminium filters are used to obtain high resolution pictures of the sun in the soft x-ray region of the electromagnetic spectrum. [1]
It is important to characterize the performance of these foils, especially near the absorption edges. The primary aim of this project was to analyse the transmission curve of Al and Si filters (1500 and 1200 thick respectively), in the soft x-ray region (105 360 ). For the simulations, the parameters are initially considered as: 1500 foil thickness, standard optical constants and zero roughness. Based on the modifications required in the initial assumptions regarding the different parameters of the filter we expected to characterize the filter and give possible reasons why certain parameters (eg. thickness distribution between filter material and oxide layer) were different from the values initially assumed.
A thorough understanding of the methodology involved in calculating the reflectivity and transmission through thin films was required before analysing the experimental data. A detailed study of the Parratt formalism [2] and its mathematical derivation was undertaken. The simulation code written in MATLAB was used to understand the behaviour of the reflectivity and transmission of thin films as a function of angle and wavelength, their dependence on thickness of layer and roughness and the effect of oxide layer on a transmission filter.
The project work is carried out on reflectivity beamline at Indus-1 synchrotron source. The report is divided into four parts: The first part covers basic aspects of synchrotron radiation and Indus-1 . The second part covers the details of the experimental work, basic aspects of the beamline and details of transmission measurement. The third part discusses the methodology 4
used in calculating the reflectivity and transmission through thin film. The basic equations leading up to the Parratt formalism [2] are discussed and a complete derivation of the same is given in the Appendix. The fourth part describes the data analysis of transmission measurements of Si and Al filters including the interpretations of the results.
1.1.1 Bending Magnet Radiation Accelerated charged particles emit electromagnetic radiation. For a charged particle moving in a curved trajectory at relativistic speed the radiation emitted is isotropic (uniform in all directions) in the moving frame of reference of the electron. However, in the laboratory frame of reference, the beam of radiation is highly collimated. This can be seen by solving electron equation of motion in moving frame of reference of electron and Lorentz transforming the results to the laboratory frame of reference. The radiation emitted in the range -/4 < ` < /4 is beamed in the direction of motion of the
1(/)2 1
).
Figure 1.1: The left and right pictures show the distribution of emitted radiation form an accelerated charged particle (relativistic) in the frames S and S` respectively. S and S` are the laboratory and the moving frames of reference respectively. (images taken from [13]).
Synchrotron Radiation sources provide several advantages over other sources: High intensity photon beam (high flux) is available and allows rapid experiments or use of weakly scattering crystals. A broad spectrum of radiation with wide tunability (from microwaves to hard x-rays) is available. Highly collimated beam with small angular divergence (high brilliance). Both linear and circularly polarized light are available. Pulsed light emission with pulse durations as low as tens of picoseconds allows resolution of processes on the same time scale.
1.2.1
Indus-1
Synchrotron
Radiation Source
Indus-1 is a 450 MeV electron storage ring at RRCAT. It provides a broad
10 100
electromagnetic
spectrum
Wavelength
1000
10000
extending from far infrared to soft xray region with a critical wavelength
Figure 1.2: Spectrum of photon flux of Indus-1 450 MeV electron storage ring
of 61 . The machine provides high flux in the soft x-ray/vacuum ultraviolet radiation (10 < < 1000 ) as shown in Fig 1.2. Since the wavelengths considered are relatively shorter, one can explore physical structure of materials with much better resolution than that offered by visible light. Also, this wavelength range covers many absorption thresholds of various elements. [5]
Because the refractive index is less than unity, it is possible to reflect the radiation completely (Snells law). The value of critical angle increases with wavelength ( = /) and it
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from the surface of a material below a certain angle of incidence known as critical angle the reflectivity drops rapidly and the fall is proportional to 1/ 4 where q= sin . Soft x-
lies in the range of a few degrees for soft x-rays (10 A < < 300 A). Above the critical angle,
rays are important due to the numerous atomic resonances of different materials lying in this region, which makes it possible to exploit these wavelengths for elemental identification. [5]
101 2.5
extinction coefficient
10-1
2.0
10-3
1.5
1-
1-
defined as = 1 + , where In the x-ray region, the refractive index is unity, and imaginary part (beta) is absorption index. The terms delta and beta are called optical constants. In soft x-ray region their typical values lie in the range ~10-2 10-3. The inner atomic electrons of atoms contribute to the absorption of x-rays which gives a series of jumps in the absorption index at
10-5
1.0
10-7
10 100 Wavelength ()
0.5 1000
Figure 1.3: Real (1-) and imaginary () part of the refractive index n for Mo. The real part slightly deviates form unity whereas the absorption index decreases rapidly at lower wavelengths (Ref. [5]).
energies given by the binding energies of these electrons. A typical characteristics of optical constants in x-ray region is shown in Figure 1.3. 7
2. Experimental Details
2.1 Reflectivity beamline at Indus-1
The reflectivity beamline comprised of pre and post focusing toroidal mirrors and a toroidal grating monochromator. The beamline provides monochromatic radiation in 40-1000
wavelength region with high flux and moderate spectral resolution. This beamline is used for characterization of optical elements (mirrors, gratings, thin films, multilayers, detectors, absorption edge filters etc.) in the soft x-ray/ vacuum ultra violet region. [6].
Monochromatic radiation from the TGM is comprised of higher harmonics. A filter wheel mechanism has been incorporated in the beamline just after the exit slit of the monochromator to introduce an appropriate transmission filter in the SR beam path. Various filters such as Al, Si, B Indium grown on Ni mesh of 87% transmission are used to suppress the higher harmonic contents in the beamline [6].
.For this project measured data of transmission filters was used to understand the transmission characteristics of Al and Si filters near the absorption edges. The transmission measurements were carried out in the wavelength range of 100 360 in step of 0.3. This range includes the absorption edge of both materials (124 and 170 for Si and Al respectively).
The starting point is the set of Fresnel formulas for refraction and transmission coefficients at the boundary between two materials of refractive indices n1 and n2. The electromagnetic wave is incident at an angle 1 (from normal) with an angle of refraction 2. The final expressions used for the simulations consider only s-polarization.
12 = 1 cos 1 2 cos 2 1 cos 1 + 2 cos 2 2 1 cos 1
12 =
(3.1) (3.2)
1 cos 1 + 2 cos 2
Figure 3.1: Schematic of multilayer film showing reflected and transmitted amplitudes just above each interface.
Tn and Rn are the amplitudes of the electric field just above the nth interface.
The basic equations relating the amplitude of forward running waves and backward running waves of the nth interface with that of the n-1th interface are given below. They are used to derive a recursion formalism to get the expression for transmitted field at the bottom of the last interface. +2 = 0 since there is no backscattered wave (from air medium) at the N+1th interface. Considering N layers,
+2 = 0
For +1 we consider the contribution of the +1 wave which propagates upto the Nth interface, gets reflected, and travels the same distance back. The phase term is therefore 2 instead of as given in Spiller [8]. (where, =
2
cos
(3.7) (3.8)
Roughness For considering the effect of roughness of the interfaces the reflection and transmission coefficients at each interface are modified by multiplying by an exponential factor. The literature [7] gives two sets of modification factors depending on the case considered. The set
, +1 = , +1 2 , , +1
, +1 = , +1 +( , , +1 )
(3.9) (3.10) 10
following expressions:
, +1 = , +1 2 ,
2
However, Tolan et al [7] states that while the above set of expressions is valid in the case of
As can be seen, the transmission coefficient is now modified and , +1 < | , +1 |. However,
, +1 = , +1 ( , , +1 )
(3.11) (3.12)
it was observed that in the case of multilayer films, increasing the roughness () of certain interfaces decreased the transmission while doing the same for certain other interfaces increased the overall transmission. We believe that this is due to the interference of the reflected waves from the different interfaces of the multilayer film.
In the simulation code, Eqs. (3.9) and (3.10) were used because it led to the intuitive behaviour of a decrease in the overall transmission on increasing the roughness parameter ().
Simulations for the cases discussed above helps to understand the basic phenomena involved in reflection and transmission through thin films.
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Effect of thickness of film on transmission In Figure 3.2, the wavelength is fixed and the thickness of the film is varied. A thicker film will have higher absorption and we see how the curve is lower for higher thicknesses. The critical
1.0 0.9 0.8 0.7 0.6 0.5 0.4 0.3 0.2 0.1 0.0
angle by
is
approximately
2.
given In
Transmission
below the critical angle and increases suddenly at the critical angle and then saturates towards some value as the case of normal incidence is approached. As shown in Figure 3.2, for higher thicknesses the graph is as
Figure. 3.2: Transmission curve for wavelength=200 . The thickness of silicon film is varied.
characteristic behaviour near critical angle is not very apparent. The transition from low to high transmission (near the critical angle) is relatively smoother. A possible explanation is that at lower thicknesses there is less absorption, and the field penetration is much more.
3.1.2 Case II Transmission vs. Wavelength The calculated transmission values of Si and Al filters near the respective absorption edges (124 and 170 ) for different angles of incidence are shown in Figures 3.3 3.6.
Silicon (case I) and Aluminium (case II) (both with oxide layers on both sides) Densities: Si (2.33 g/cm3), SiO2 (2.2 g/cm3) Al (2.699 g/cm3), Al2O3 (3.97 g/cm3) Wavelength range 50 200 Thicknesses Si or Al film: 500 Oxide layer: 50 on both sides
12
0.8 0.6
0.8 0.6
Transmission
Transmission
5 15 30 60 90
120 160 200 240 280 320 360 Wavelength () Figure 3.3: Transmission vs. Wavelength for Si as a function of angle of incidence
0.12
Delta (deviation from real part of refractive index) Beta (imaginary part of refractive index)
0.08
Delta (deviation from real part of refractive index) Beta (imaginary part of refractive index)
0.08
Delta/Beta
0.04
Delta/Beta
0.04
0.00
0.00
-0.04
120 160 200 240 280 320 360 Wavelength () Figure 3.4: Optical constants for Si
120 160 200 240 280 320 360 Wavelength () Figure 3.6: Optical constants for Al
As can be observed from Figures 3.3 3.6, in general, the transmission increases when beta decreases and it decreases when beta increases. Thus the transmission strongly depends on the absorption (characterized by beta). The transmission changes abruptly at the respective absorption edges (124 and 170 ) due to the abrupt changes in the values of the optical constants (particularly beta) at the same wavelengths.
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Incident beam
Transmitted beam
Detector
Oxide Film
Oxide
Our aim was to fit the experimental curve by running simulations considering similar structure and try to understand why various deviations from initial assumptions of the composition of the film were required. This would give us a better understanding of the basic phenomena involved and a deeper insight into the actual composition of the filter.
For the simulations, we considered a film (Si and Al) of particular thickness surrounded by oxide layer on both sides
0.8
Transmission
0.6
simulated
curve
was
obtained
0.4
considering the thickness of the film as given by the manufacturer (1200 for Si and 1500 for Al filter) and standard
0.2
120
160
200
240
280
320
360
Wavelength () Figure 4.2: Simulated transmission curve without considering the contribution of higher harmonics
optical constants (obtained from CXRO website [12]). There was a large
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discrepancy between the simulated and experimental curves. Because of the huge difference in the calculated values and the experimental ones, we suspected that the thicknesses of the respective layers were very different from that initially assumed (SiO2 (0 ) Si (1200 ) SiO2 (0 )). The simulation curve obtained from these preliminary considerations is given in Figure 4.2.
The absorption edge of Si is at 124 . A small apparent edge at around 250 (roughly twice 124 ), indicates that higher harmonics are present in the incident beam coming from the TGM of the beamline.
Higher diffraction orders from the grating monochromator generate higher harmonics. Thus the transmission at a single wavelength actually consists of the transmission at the wavelengths , /2, /3 and so on, with different fractional weightages for each harmonic. The fractional composition of these higher harmonic wavelengths depends on several factors, including the grating diffraction efficiency, detector responsivity, mirror reflectivity etc. The quantitative details of higher harmonics components in the incident beam of the reflectivity beamline are previously characterized [11]. Therefore effect of higher harmonics in measured data on the beamline can be taken into account accordingly. In the present report the
fractional composition of higher harmonics was considered. The higher harmonic data obtained was interpolated in the wavelength range 115 360 .
1.0 0.8
Because the transmission at a particular wavelength is actually a weighted sum of the transmission at , /2 and /3 (corresponding to the 1st, 2nd and 3rd harmonics), the following procedure was followed to consider the
Transmission
simulated experimental
200 240 280 320 360 Wavelength () Figure 4.3: Simulated transmission curve after considering the contribution of higher harmonics
were calculated for the ranges: (I) 105 360 , (II) 52 180 and (III) 35
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second and third ranges are simply 1/2 and 1/3 of that of the first range. The three 120 corresponding to the 1st, 2nd and 3rd harmonics respectively. The extremum of the transmission curves were then added after multiplying with the corresponding weighting factors obtained from previous studies [11]. The final curve obtained is shown in Figure 4.3.
As we can see from Figure 4.3, after considering the contribution of higher harmonics the overall shape of the simulated transmission curve is similar to that of the experimental one. We now need to take care of the significant vertical shift between the simulated and experimental curves.
Thickness Thickness of film and oxide layer:- It was observed that, in the case of Si, increasing the Si film thickness had a significant effect on the vertical extent of the transmission curve near the
1.0 0.8
as shown in the inset of Figure 4.4, is the difference between the maxima and minima of transmission near the
Transmission
the oxide layer thickness brought the transmission curve down but had little effect on the vertical extent of the same. (Figure 4.4). The thickness distribution
120
160
Figure 4.4: Effect of considering 100 oxide layer on both sides of 1200 Si film
320
360
(between oxide and film layers) was changed keeping the total thickness of the filter around 1200 (for Si filter).
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Optical constants Imaginary part of refractive index (beta):- Proportional increases in the beta and thickness of two means an increase in the total absorption = (where is the imaginary part of any layer led to an almost similar effect on the transmission curve. An increase in either of the
4
refractive index and x is the thickness of layer). The logarithm of total absorption is linearly
proportional to both beta and thickness of layer. However, a change in either of these two parameters led to slightly different effects on the features on the transmission curve. These features are predominantly due to the interference between the reflected waves from multiple interfaces. Thus a change in the thickness of a layer would have a significant impact on the wavy features seen on the transmission curve; and the effect of a change in beta would be somewhat different in this respect.
Deviation from real part of refractive index (delta):- In the case of Si (with thicknesses as given in Table 4.1), it was observed that changing the delta values (even up to three times the standard values) had very little effect on the transmission curve.
However, during preliminary investigations (when the thickness of the pure Si layer was much larger ~1200 ) it was observed that increasing the delta by a significant amount (2-3 times original value) brought about wavy features onto the transmission curve. Since the experimental curve did not show such features it was considered appropriate to smoothen out the same in the simulated curves by increasing the roughness of the layers. However, as mentioned previously, the thickness distribution was greatly modified (Table 4.1 and 4.2) from that initially assumed. It was not seen necessary to make the above mentioned changes to the delta values in this case
A brief digression regarding the quantification of roughness of interfaces in the case of transmission is given below:
Roughness Detailed discussion on the quantification of roughness is given in Section 3. In the case of normal angle of incidence, the roughness was seen to have negligible effect on the transmission when the roughness parameter () was increased even up to 10 20 .
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It was observed that to match the simulation with experiment, considerably thick oxide layers had to be incorporated. The total thickness considered is around 1140 (Table 4.1 and Figure 4.5).
Silicon filter (finalized parameters) SiO2 (330 ) Si (480 ) SiO2 (330 ) Standard values (unchanged) (CXRO [12]) Si (2.33 g/cm3), SiO2 (2.2 g/cm3)
simulated experimental
Thickness Thickness of film and oxide layer: - In the case of Aluminium, it was observed that the effect of increasing the oxide layer thickness was different from that of Si. In this case, an increase in the oxide layer thickness not only brought the transmission curve down, it also significantly reduced the vertical extent of the curve (unlike the effect observed in case of Si). 18
Finalizing the thickness distribution:- Due to the behaviour mentioned above fixing the thicknesses of the film and oxide layer for Aluminium filter was a more dynamic process than that of Silicon filter. The best possible combination of thicknesses is found to be that as given in Table 4.2.
Aluminium filter (finalized parameters) Al2O3 (70 ) Al (1450 ) Al2O3 (70 ) Standard values (unchanged) (CXRO [12]) Al (2.699 g/cm3), Al2O3 (3.97 g/cm3)
Transmission
simulated experimental
As can be seen in the transmission curves of Figure 4.5 and 4.6, there is a small horizontal shift (2.0 for Si and 2.7 for Al) between the simulated and experimental curve. This shift is particularly apparent near the absorption edge. This small shift is observed in experimental curves due to a small inevitable error in the calibration.
4.2 Summary
The Parrat formalism [2] was studied and intermediate steps were derived to understand the xray reflection and transmission phenomena through thin films. Effect of roughness, thickness, 19
angle of incidence on transmission behaviour of thin films was studied in detail. Experimental data of Al and Si thin foils were used to explain their transmission behaviour by detailed theoretical analysis. It was observed that there is significant contribution of higher harmonic content in the experimental results of transmission though filters. Thus this factor was included in the simulations. In transmission calculations, it was observed that, in the case of Si, increasing the Si film thickness had a significant effect on the vertical extent of the transmission curve near the absorption edge. Also, proportional increases in the beta and thickness of any layer led to an almost similar effect on the transmission curve. In the case of normal angle of incidence, the roughness was seen to have negligible effect on the transmission when the roughness parameter () was increased even up to 10 20 . It was observed that there is significant amount of oxide layer in the case of Silicon filter (330 on both sides), and a relatively less amount in the case of Aluminium filter (70 on both sides). The total thickness, however, remained approximately same as given by the manufacturer (1140 and 1590 for Si and Al filters respectively). The experimental curve was fitted reasonably well with the calculated values for the range of wavelengths from the absorption edge of the respective materials (Si 124 and Al 170 ) to about 200-220 for the two filters with parameters as given in Tables 4.1 and 4.2.
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Appendix
Figure 5.1: Schematic of multilayer film showing reflected and transmitted amplitudes just above each interface.
+2 = 0 since there is no backscattered wave (from air medium) at the N+1th interface.
+2 = 0
(5.1)
+2 = +1 +1,+2 +1 = +1,+2 =
2
+1 = +1 +1,+2 cos
1= =>
+1
+1
,+1 + =
1+ +1 , +1 2
, +1
+1 +1
2 +1,
(+1, = ,+1 )
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+1
=>
= ,+1 +
+1
1+ +1 , +1 2
, +1 +1
+1
2 +1,
= ,+1 +
+1
+1,
(++ ,+ )
,+ ++
(1 , +1 2 ) +1 2 1+ +1 , +1 2
However, the Parratt formalism [2] gives the following expression for :
(++ ,+ )
(5.10)
The two expressions (5.9 and 5.10) are equivalent and give the same results for transmission calculations. The difference between the two is that in one the individual thicknesses of the layers are considered, while in the other the cumulative sum of the layers upto the nth interface is considered (i.e. z-coordinate). Both expressions were used to run simulations of transmission through multilayer films and the results obtained were the same.
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References
1. Forbes R. Powell, Optical Engineering, Vol. 29 No. 6, 614-624 (1990). 2. L.G. Parratt, Phys. Rev. 95, 359 (1954) 3. David Attwood, Soft X-ray and Extreme Ultraviolet Radiation, Cambridge University Press. 4. Jens Als-Nielson, Elements of Modern X-ray Physics, Wiley (2nd edition, 2011) 5. Mohammed H.Modi, Surfaces and Interface Studies in X-ray Mirrors, PhD Thesis, RRCAT Indore, India (2003) 6. R.V. Nandedkar, Current Science, Vol. 82, No. 3, 298-304 (2002) 7. M. Tolan, X-Ray Scattering from Soft-Matter Thin Films, Springer (1999) 8. E. Spiller, Soft X-Ray Optics, SPIE Optical Engineering Press (1994) 9. D. K. G. de Boer, Phys. Rev. B, Vol. 44 number 2, 498 (1991) 10. V. Holy, X-Ray Scattering from Thin Films, Springer Tracts in Modern Physics, Vol. 149, Springer (1998) 11. Mohammed H. Modi, Applied Optics, Vol. 51, No. 16, 3552-3557 (2012) 12. http://www.cxro.lbl.gov/ 13. http://asd.gsfc.nasa.gov/Volker.Beckmann/school/download/Longair_Radiation2.pdf
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