Reference-free total reflection X-ray fluorescence analysis of semiconductor surfaces with synchrotron radiation

Total reflection X-ray fluorescence (TXRF) analysis is a well-established method to monitor lowest level contamination on semiconductor surfaces. Even light elements on a wafer surface can be excited effectively when using high-flux synchrotron radiation in the soft X-ray range. To meet current industrial requirements in nondestructive semiconductor analysis, the Physikalisch-Technische Bundesanstalt (PTB) operates dedicated instrumentation for analyzing light element contamination on wafer pieces as well as on 200- and 300-mm silicon wafer surfaces. This instrumentation is also suited for grazing incidence X-ray fluorescence analysis and conventional energy-dispersive X-ray fluorescence analysis of buried and surface nanolayered structures, respectively. The most prominent features are a high-vacuum load-lock combined with an equipment front end module and a UHV irradiation chamber with an electrostatic chuck mounted on an eight-axis manipulator. Here, the entire surface of a 200- or a 300-mm wafer can be scanned by monochromatized radiation provided by the plane grating monochromator beamline for undulator radiation in the PTB laboratory at the electron storage ring BESSY II. This beamline provides high spectral purity and high photon flux in the range of 0.078-1.86 keV. In addition, absolutely calibrated photodiodes and Si(Li) detectors are used to monitor the exciting radiant power respectively the fluorescence radiation. Furthermore, the footprint of the excitation radiation at the wafer surface is well-known due to beam profile recordings by a CCD during special operation conditions at BESSY II that allow for drastically reduced electron beam currents. Thus, all the requirements of completely reference-free quantitation of TXRF analysis are fulfilled and are to be presented in the present work. The perspectives to arrange for reference-free quantitation using X-ray tube-based, table-top TXRF analysis are also addressed.     

Characterising a Si(Li) detector element for the SIXA X-ray spectrometer

The detection efficiency and response function of a Si(Li) detector element for the SIXA spectrometer have been determined in the 500 eV to 5 keV energy range using synchrotron radiation emitted at a bending magnet of the electron storage ring BESSY, which is a primary radiation standard. The agreement between the measured spectrum and the model calculation is better than 2%.     

New plane-grating monochromators for third generation synchrotron radiation light sources

For the electron storage ring BESSY II a new type of plane-grating monochromators working with collimated light is proposed. The operation with collimated light is a well-known optical technique, which enables us to keep the focusing condition fulfilled automatically for all photon energies. The additional degree of freedom gained allows the monochromator to comply with the most different needs of the users. An additional feature of the design is the further extension of the already widely accessible energy range of a PGM towards lower photon energies.

The BESSY beamline concept, which requires an additional mirror in front of the monochromator allows the collimation of the light with the presently planned number of optical elements.     

Measurement of the Relative Intensity of 103Pd Photon Radiation

The intensity of photon radiation with energies of 20.15, 22.77, 295, and 497 keV in the decay of ¹⁰³Pd has been measured relative to the 357-keV spectral line. The results have confirmed that there is a discrepancy between the evaluated data for ¹⁰³Pd KX and gamma radiation. An interrelated system of absolute intensities for those energies is proposed.     

The applicability of radiophotoluminescence dosemeter (RPLD) for measuring medical radiation (MR) doses

The applicability of radiophotoluminescence dosimetry was determined by assessing various radiophotoluminescence dosemeter (RPLD) properties for measuring medical radiation doses from radiation sources of a continuous spectrum. The RPLD was found to be accurate for measuring doses in diagnostics (50-125 keV) and radiation therapy (6, 10 and 18 MV photons, 6 and 15 MeV electrons). The RPLD shows excellent dose linearity (R(2) > 0.99), reproducibility and batch uniformity, and minimal fading and accurate accumulated dose measurement. The dosemeter material is independent of photon energy in the diagnostic range; however, the dosemeter requires additional calibration in the mammography energy range and also for accurate dose measurement with photon or electron energies in radiation therapy. RPLD measurements with a tin filter show considerable angular dependence at angles exceeding 50° between the photon beam and the normal to the long axis of the dosemeter. The RPLD measurement accuracy at high doses can be improved with optimised pre-heating schemes.     

Metrology of pulsed radiation for 157-nm lithography

In the framework of current development in 157-nm lithography we have investigated the performance of photodetectors with emphasis to their stability and linearity. The measurements were performed in the radiometry laboratories of the Physikalisch-Technische Bundesanstalt at the Berlin electron-storage rings BESSY I and BESSY II with spectrally dispersed synchrotron radiation as well as with highly pulsed F2 laser radiation at 157 nm in combination with a cryogenic radiometer as the primary detector standard. Relative standard uncertainties of as little as 1% were achieved for the calibration of photodetectors in the spectral range of ultraviolet and vacuum-ultraviolet radiation.     

Optimisation of a secondary standard chamber for the measurement of the ambient dose equivalent, H*(10), for low photon energies

A secondary standard ionisation chamber for photon radiation for measuring an ionisation current, which is directly proportional to the conventionally true value of the ambient dose equivalent, H*(10), was optimised. The chamber was developed in the Austrian Research Centers Seibersdorf and is used successfully worldwide by dosimetry laboratories. The chamber response with respect to H*(10) for photon energies from 40 to 1,250 keV is nearly constant. For lower photon energies the response is strongly energy-dependent and does not fulfil the requirements concerning the quality of a secondary standard given in ISO 4,037-2, i.e. for energies for which the determination of the conventionally true value of H*(10) is very difficult. Considering the dose limits defined in the Directive 96/29/Euratom, in the case of whole-body irradiation the knowledge of the personal dose equivalent is of importance down to energies of approximately 12 keV. For area dosimetry, this means that the knowledge of H*(10) for energies approximately >or=12 keV is necessary. To get one secondary standard chamber for H*(10) for the whole photon energy range and to close the gap for low energies in the dissemination of the conventionally true value of H*(10), the chamber was optimised for a flat response for energies from approximately 12 to 1,250 keV.     

A novel undulator-based PGM beamline for circularly polarised synchrotron radiation at BESSY II

We present the design of a beamline for circularly polarised radiation from an elliptical double undulator to be built at BESSY II. The UE56 undulator of Sasaki type will emit simultaneously two angularly separated circularly polarised beams of opposite helicities. The undulator will, through emissions in first, third and fifth harmonics, provide circularly polarised radiation in the energy range 89–1328 eV. The beamline essentially consists of a plane grating monochromator (PGM) working with collimated light and employing only one set of optical elements for steering and monochromatising the two beams. A high energy resolution from 6000 to 13 000 can be achieved at a flux between about 10¹⁰ and 10¹² photon/s, respectively. The helicity of circular polarisation can be switched dynamically in the beamline at a high rate (>100 Hz) by use of a suitable chopper. The degree of circular polarisation of the source ranging from 78 to 100% is well preserved by the beamline. In the worst case — at the lowest energy — the degree of polarisation is reduced by 5%. In the higher energy range above 357 eV the input degree of circular polarisation can even be increased by the beamline.     

Pinhole-array x-ray spectrometer for laser-fusion experiments

A pinhole-array x-ray spectrometer for laser-fusion experiments is demonstrated. An array of approximately 300 pinholes is placed in front of a flat-crystal spectrometer, yielding target images at photon energies ~10 eV apart (for photon energies of ~4 to 5 keV). For wideband radiation the images are two dimensional, whereas when a single spectral line is used, the field of view in the direction of dispersion is limited. However, single spectral line images can have a field of view sufficient for imaging the compressed target core. We show the image at the Ti-Kalpha-line fluorescence from a Ti-doped shell, which we show to be excited by continuum radiation from the compressed core. The Kalpha image delineates the cold, compressed shell at peak compression, which can otherwise be obtained only through backlighting. In addition, the array provides spectra of high spectral resolution because of the reduction in the effective source size.     

Phase-retardation and full-polarization analysis of soft-x-ray synchrotron radiation close to the carbon K edge by use of a multilayer transmission filter

We have produced a multilayer transmission filter with 100 periods of Cr/C to achieve a significant phase retardation while maintaining good transmission for photon energies just below the carbon K edge. This device was installed into a polarimeter behind the SX700/3 monochromator at the Berlin synchrotron radiation laboratory, BESSY. The phase-retardation properties were observed as theoretically predicted. Agreement between experiment and calculation could be obtained by introduction of a rather small interface roughness in the simulation code (σ = 0.65 nm rms). An observed phase retardation of 5° was sufficient to permit, for the first time we believe, a complete and unambiguous polarization analysis of soft-x-ray synchrotron radiation (265-eV photon energy) with primary standards.     

使用单能X射线辐射装置对CdTe探测效率的实验刻度

CdTe探测器对单能平行光子源的绝对测量之前,需要进行效率刻度。利用MCNP5蒙特卡罗模拟程序建立CdTe探测器物理模型,模拟计算了10~260keV能量段能点的本征探测效率,在10~60keV能量段探测效率高于75%。用单能X射线装置和HPGe探测器对CdTe探测器本征探测效率进行了实验刻度。结果表明,在10~100keV能量范围内CdTe探测器的模拟效率与实验效率趋势一致,最大误差不超过5.6%。因为Te元素在27keV和32keV处会产生逃逸峰,导致探测效率在这2个能量处有明显下降趋势。用241Am和133Ba放射源对CdTe探测器进行效率刻度验证,在能量为59.54keV和81keV放射源标定的探测效率与单能X射线辐射装置测量值相符。     

Precise dose evaluation using a commercial phototransistor as a radiation detector

An experimental arrangement and a circuitry based on an NPN phototransistor-type silicon radiation detector have been used for evaluating the X-ray beam dose in the diagnostic range. The circuitry was built to allow alteration of the electric field in the phototransistor internal structure, with some devices that have an available base connection. By changing the transistor base bias it is possible to alter its operation point to obtain a response gain from the selected photon energy range. In this way we have made an electronic energy-domain discretisation and we are investigating a model to calculate the dose contribution from each energy discretised into 10 keV steps. The method has been tested in filtered radiation beams generated from an HF-160 Pantak X-ray unit and compared with the usual dosimetry method. Our results have demonstrated that it is possible to make such a dose deconvolution from 40 to 140 keV energies by controlling the phototransistor base bias properly.     

Hard X-ray polarization measured with a Compton polarimeter at synchrotron radiation facility

A hard X-ray polarimeter with CdTe detectors has been developed for measurement of the degree of X-ray polarization at synchrotron radiation facilities. It utilizes 90° Compton scattering from the low Z targets. Measurements were performed at both facilities of the beamline BL38B1 in SPring-8 and the beamline BL14A in KEK-PF. The degrees of X-ray polarization for 20 keV X-rays are 99% and 82% at the BL38B1 in SPring-8 and BL14A in KEK-PF, respectively. The polarization degrees in the energy range of 15 and 40 keV correspond to 99.6±0.2% and 96.1±0.2% at the beamline BL38B1 in SPring-8. The analyzing power of the polarimeter was estimated by the Monte Carlo simulation with EGS4. The synchrotron radiation facilities provide highly polarized X-ray beams at energies above 15 keV.     

Measurement of energy and direction distribution of neutron and photon fluences in workplace fields

Within the EU Project EVIDOS, a spectrometer with 24 silicon detectors mounted on the surface of a polyethylene sphere is used for the determination of the energy and direction distribution of neutrons and photons. It has been characterized with respect to neutron radiation with energies from thermal up to 15 MeV and to photon radiation with energies from 65 keV to 6 MeV. The first measurements described here were performed in the simulated workplace field, CANEL, at Cadarache, with the purpose of checking the instrument and the unfolding procedures.     

Induction of chromosome aberration in human lymphocytes and its dependence on X ray energy

The variations of dose response with X ray energy observed with the human lymphocyte dicentric assay is examined. In order to determine reliably the initial slopes (RBEm) many cells need to be analysed at low doses. Insufficient analysis may explain some reported interlaboratory differences in fitted dose-response coefficients. One such discrepancy at 150 kVp, E = 70 keV is examined. Data are also presented for an X ray spectrum of 80 kVp, E = 58 keV. Over the photon energy range 20 keV X rays to 1.25 MeV gamma rays RBEm varies by about a factor of 5, with the lower energies being more effective. This is consistent with microdosimetric theory. By contrast, in radiological protection a radiation weighting factor of 1.0 is assumed for all photons when assessing the risk of inducing cancer at low doses. The measured variations of biological effect with photon energy have led to suggestions that the lower energies, as used for some diagnostic radiology, carry a greater risk per unit dose than is normally assumed by those involved in radiological protection. Interpretation of the data reported in this paper does not support this view.     

The optics beamline at the Swiss Light Source

We present the successful installation and the performance of a new beamline for optics and instrumentation research and developments at the Swiss Light Source. The beamline covers the photon energy range from 5.5 to 22.5 keV at a bending magnet with a cryogenically cooled Si(1 1 1) channel cut monochromator followed by a bendable toroidal mirror with 1:1 focusing. Monochromator and focusing mirror can be retracted independently to allow monochromatic and pink beam mode with and without focusing. In focused monochromatic mode we measured a usable photon flux of at 11 keV within a focus of (FWHM v×h). The higher order contamination has been determined with absorption foils. We measured 0.025% of second order light at 9 keV and 17% of third order contamination at 6 keV. In pink beam mode we measured with a thermopile sensor a radiation power of 10.6 W for 1 mrad acceptance.     

The use of the Monte Carlo simulation technique for the design of an H*(10) dosemeter based on TLD-100

The thermoluminescence (TL) detector material LiF:Mg,Ti (TLD-100) and appropriate filter materials were combined in order to design a passive dosemeter measuring the operational quantity ambient dose equivalent, H*(10), for monitoring low-dose external photon radiation fields. Using the Monte Carlo simulation technique, optimisations of energy dependent conversion coefficients from air kerma free-in-air compared to ICRU and ISO proposed values. h*K(10), were performed by varying dosemeter detector positioning. geometrical arrangements, and filter materials. Deviations smaller than 5% compared to h*K(10) between 30 keV and 2.5 MeV of primary photon energies were achieved by a dosemeter design consisting of a 15 microm Sn metal layer and a 5 mm PMMA layer surrounding the LiF detector. Subsequently performed free-air verification experiments carried out in well defined standard photon radiation fields showed an obviously TL-specific effect. An underestimation up to -15% of the modelled data at low photon energies was observed.     

Intercomparison measurements of extremity dosemeters in beta and/or photon radiation fields

Beta dosimetry, especially at the extremities, is gaining in importance due to the increasing use of beta particle sources, e.g. in brachytherapy. The dosimetric properties of personal dosemeters to be worn on the extremities and capable of measuring the personal dose equivalent, Hp(0.07), in beta and/or photon radiation fields were investigated within the scope of intercomparison measurements organised by the PTB in two steps. The results were evaluated on the basis of recommendations from the German Commission on Radiological Protection (SSK). In the first step 10 types of dosemeter were investigated in beta particle fields in a range of mean energies from 0.06 MeV to 0.8 MeV. In the second step, five selected beta dosemeter types were exposed to beta particles and, in addition, to photons and to mixtures of both. Three dosemeters fulfill the requirements for the whole range of mean beta energy used for the intercomparison and meet the requirements for photon radiation from 8 keV to 662 keV.     

X reference radiation qualities produced with tube voltages above 300 kV for the calibration and testing of dosemeters

In the international standard ISO 4037-1, only X reference radiation qualities produced with tube voltages of up to 300 kV and with mean photon energies of lower than 250 keV are defined. Higher energy reference photon fields are given with a mean energy only from 662 keV (S-Cs) upwards. To close this energy gap, four new X radiation qualities, produced with tube voltages of 350 kV and 400 kV, were realised. The filtration of two of these qualities-called N-350 and N-400-was chosen in such a way that they agree with the specifications of the narrow-spectrum series (N-series) defined in ISO 4037-1. The other qualities which have been created-called H-350 and H-400-can be assigned to the high air-kerma rate series (H-series). The fluence spectra of these qualities were measured by using X-ray spectrometry. The values of 23 characteristic parameters were determined and compared with the ISO specifications for X-ray reference fields.     

Bremsstrahlung radiation from high-energy electrons in wide gas-filled gaps

Electric discharge in wide interelectrode gaps filled with air at atmospheric pressure have been experimentally studied using applied voltage pulses with amplitudes up to 800 kV and a front width within 150–200 ns. The discharge was accompanied by the emission of a 10–20-ns-long pulse of radiation with photon energies above 5 keV. It is established that this emission is related to the generation of runaway electrons from the heads of anode-directed streamers. The calculated spectrum of the observed bremsstrahlung radiation exhibits a maximum at photon energies about 15 kV, which is due to the absorption of photons by the molecules of a gas in which the discharge takes place.