bluuebunny/crossref_metadata_2025 huggingface dataset:
An Optical System for Measuring the Burning Rate of Solid Propellant Strands
Authors: Eisenreich N. , Kugler H. P. , Sinn F.
Published: December 2004

An optical system is described for measuring the burning rate of solid propellant strands. It consists of a bomb equipped with quartz windows, an objective, a photo diode array and a data acquisition and processing unit. A Simultaneous observation of the burning in possible by other optical and spectroscopic methods.

The system is tested by recording the pressure dependence of the burning rates of typical propellants. The results are compared to those obtained by the standard Crawford method. The advantages of the optical system are due to the easier handling in sample preparation and the assessment of a distribution of the burning rate.
Experiments of Initiation of Covered, but Unconfined HE Charges under different test conditions by shaped charge jets
Authors: Held M.
Published: December 2004

The initiation behavior of TNT/RDX 35/65 high explosive charges under the impact of the jet from a 44 mm diameter shaped charge with 7.8 mm/m̈s jet tip velocity, which has previously perforated a 100 mm thick barrier is reported. In these tests,

the high explosive charge under test was divided into different sections by transverse air gaps, with the first section being in contact with the barrier, or

the 100 mm thick barrier was sub‐divided in such a way that one part of it was in contact with the high explosive charge under test, or

various air gaps, ranging from 0.5 mm to 450 mm, were made between the acceptor charge and the barrier.
The Initiation Threshold Sensitivity of HNS Explosive as a Function of its Grain Size
Authors: Hasman E. , Gvishi M. , Solomonovici A.
Published: December 2004

The initiation threshold sensitivity of HNS versus explosive grain size has been measured, using an electric gun, with two flyer thicknesses. The initiation threshold, (kinetic energy of flyer plate), versus explosive grain size shows that the threshold curve increases dramatically at grain size over 5.4 m̈m (for flyer thickness 76.2 m̈m at explosive density 1.6 g/cm3). Minimum critical energies were calculated to be 12.15 ± 0.5 J/cm2 and less than 7.0 J/cm2, for flyer thicknesses 76.2 m̈m and 20.0 m̈m, respectively.
Combustion Wave Structure of AP Composite Propellants
Authors: Yano Y. , Miyata K. , Kubota N. , Sakamoto S.
Published: December 2004

The combustion mechanism of ammonium perchlorate (AP) composite propellants were studied. The oxidizer‐rich propellants tested were made with excess concentrations of AP particles. The pressure deflagration limit of propellant decreases with increasing the concentration of binder. The combustion wave consists of two reaction regions I and II: the region I is the zone of AP monopropellant flame and the region II is the zone of diffusion flame. The heat flux feedback from the gas phase to the burning surface increases as pressure increases, and the heat flux is responsible for the burning rate characteristics.
Measurement of the smoke density of endburning double base propellant grains before and after burnout
Authors: Pröbster M. , Huber W. , Strecker R. , v. Taeuffenbach G.
Published: December 2004

The formation of smoke during firing of DB‐endburners is dependant on the chemical composition of the employed inhibitor. Measurements, which correlate the observed attenuation of light in the exhaust gas before and after burnout with the composition of the inhibitor, are described. The binders used were polyurethane resins with oxamide as filler and unsaturated polyester with Lithopone, respectively.
Chemiluminescence Study on Thermal Decomposition of Nitrate Esters (PETN and NC)
Authors: Kimura J.
Published: December 2004

Measurements of chemiluminescence (CL) during heating of nitrate esters (PETN and NC) have been conducted in the temperature range between 40 °C and 90 °C in an inert atmosphere. Faint light was emitted from the condensed‐phase in steady‐state fashion. This new finding implies that the thermal decomposition of nitrate esters is accompanied by some oxidation reactions. Spectral analysis of the CL showed that the light‐emitting species will be the first excited triplet of carbonyl‐containing products and singlet oxygen. The low‐temperature CL phenomena observed for PETN and NC are represented by Arrhenius law, providing the activation energy of 63 kJ/mol (= 15 kcal/mol). Kinetic analysis of the CL has led to the result that the formation of peroxy radicals, which can be produced by oxidation of the primary products of nitrate ester bond (RONO2) cleavage, predominates a consecutive series of radical reactions of the CL.
X‐Ray Microanalysis on the Surface and Cross‐Section of burning‐interrupted aluminum particle and foil in high pressure atmospheres
Authors: Tokui H. , Iwama A.
Published: December 2004

In order to deduce the burning characteristics of aluminum (Al) particle in solid propellant, a model experiment has been carried out with Al spheres of 3 mm ∼4 mm dia. in the oxidizing atmospheres at elevated pressures. As one of the investigation items, X‐ray microanalysis for the burning‐interrupted Al spheres was conducted along the straight lines crossing cap‐like Al2O3 islands attached on unburned Al.

It was clarified that, on the way of burning, in the case of Al sphere and plausibly on the burning surface of the particle also, there exist numerous Al2O3 islands, large and small, floating on molten Al sea; but even on the sea part, which seemed pure Al only, the surface is covered mostly with Al2O3 film. The similar analysis was applied to the Al foils ignited with Joule heating. It was witnessed, however, that contrary to the sphere surface there remains still neat Al in the vicinity of burning‐interrupted surface. This fact may introduce low ignition temperature (933 K ∼ 963 K) and high deflagration velocity along the surface (for example. 2500 mm/s, with test piece of 0.11 mm thick, 5 mm wide; 8 MPaO2 ) with Al foils.
Aging of Pyrotechnik Compositions. The investigation of chemical changes by IR spectroscopy and x‐ray diffraction
Authors: Barišin D. , Batinić‐Haberle I.
Published: December 2004

The aging of tracers, containing different amounts of Mg, Sr(NO3)2, KClO4, Al‐Mg alloy and organic binder, was conducted under the conditions of 50.0% and 98.5% relative humidities at 75 °C, and of 98.5% relative humidity at 25 °C. IR spectroscopy and X‐ray diffraction were used for investigation of chemical changes. At the lower humidity no detectable changes were observed. Tracer of metauoxidant ratio >1 exhibits decreased stability, changing significantly under the conditions of higher humidity, even at room temperature. In the reaction sequence of aging process (Mg(OH)2) and SrCO3 are formed, with concomitant decrease in Mg and Sr(NO3)2 content. Alloy changes only slightly, and the content of KClO4 and binder remains unchanged. Interaction between metal and nitrate is considered to be essential in the process of chemical aging.
The Effect of the Liner Metallurgical State on the shaped charge jet break‐up time
Authors: Hirsch Eitan
Published: December 2004

The effect of the liner metallurgical state on the shaped charge jet break‐up time has been widely investigated experimentaly but the experimental results were never explained by a model sufficiently detailed to even explaining them qualitatively. The model presented here shows for the first time a direct mathematical connection between the Vpl break‐up parameter and the processes which affect the liner metallurgical state during the initial stages of the flow: the drive of the liner by the explosive and the jet formation. The model shows how both the deformation energy heating the sliding shear bands during the localization process and the rate of the instability growing in the plastic flow during this process, combine to determine the Vpl parameter. This parameter is then shown to be both the velocity of the information of the plastic deformation and the component of the maximum slide velocity allowable to shear band in the elongation direction. The model predicts the shaped charge jet segment normalised length over diameter (L/D) distribution with good accuracy. It also explains the pattern of shear bands observed on the surface of jet segments recovered by Zernow, including their width. Furthermore, the model is strongly supported by its ability to show good agreement between measurements of aluminum dynamical elongation obtained in different ways, which were so far believed to be unrelated. When the jet temperature measurements by Von Holle and Trimble are reinterpreted in view of the model it is found that the average jet temperature is lower than the value they found and the temperature basically agrees with Racah's predictions.
Carbon resistor gauges for measuring shock and detonation pressures. I. Principles of functioning and calibration
Authors: Austing James L. , Tulis Allen J. , Hrdina Donald J. , Baker Douglas E. , Martinez Ricardo
Published: December 2004

The state of the art relative to the measurement of shock and detonation pressures of the magnitude generaled by condensed high explosives is reviewed. Carbon resistors have been shown to provide a relatively inexpensive and direct method for such measurements, provided adequate calibration data are available. The gauge is fabricated by heat‐sealing the carbon resistor (470 Ω, 0.125 W) into a suitable plastic material such as polystyrene; when subjected to a strong shock wave, the gauge undergoes compression and the conductivity increases in proprtion to the magnitude of the pressure. The present investigation was concerned with the experimental derivation of calibration equations relating the pressure (in gigapascal) as a function of the conductivity change ΔG (in siemens). The point of inflaction occurring at approximately 2.36 GPa, corresponding to 0.02082 S, is in agreement with previous observations in the literature. Additional experiments are being planned to resolve a problem concerning oscillatory ringing in the gauge voltage records.
Stabilizer reactions in cast double base rocket propellants. Part I: HPLC Determination of Stabilizers and their derivatives in a propellant containing the stabilizer mixture para‐nitro‐N‐methylaniline and 2‐nitrodiphenylamine aged at 80°C and 90°C
Authors: Bellerby J. M. , Sammour M. H.
Published: December 2004

Reverse phase high performance liquid chromatography (HPLC) employing an acctonitrile/methanol/water (45/10/45) mobile phase has been used to separate and quantitate the stabilizaers para‐nitro‐N‐methylaniline, (pNMA) and 2‐nitrodiphenylamine, (2NDPA) and their derivatives in a mixed‐stabilizer cast double hase rocket propellant composition undergiong acceterated aging at 80°C adn 90°C. Quantitative measurements show that pNMA is converted almost cntirely into N‐nitroso‐pNMA during the carly stages of aging and that this derivative persists for the remainder of the aging period. 2NDPA, on the other hand, reacts more slowly to give both N‐nitroso and C‐nitro derivatives.
Shock Initiation of Sheet Explosive
Authors: Yadav H. S. , Nath T. , Sundaram S. G. , Kamath P. V. , Kulkarni M. W.
Published: December 2004

The shock sensitivity of a typical sheet explosive RDX‐WAX (90:10) has been experimentally determined with gap test arrangement by measuring free surface velocity in different thicknesses of the barrier and shock and particle velocity of non‐reactive shock wave in the sheet explosive with Pin Oscillography Technique. It has been found that a shock wave, generated by a point‐initiated cylindrical explosive in contact with an aluminium barrier of diameter nearly twice the diameter of the charge, attenuates exponentially and a 6.5 mm thick sheet explosive, of density 1.28 g/cm3 and velocity of detonation 6.43 mm/μs, detonates with 50% probability by a shock wave of 11 kbar pressure in the explosive.
The thermal stability of the polymorphs of hexanitrohexaazaisowurtzitane, part II
Authors: Foltz M. Frances , Coon Clifford L. , Garcia Frank , Nichols Albert L.
Published: December 2004

Solid‐solid phase transitions in the α‐, β‐, γ‐, and ϵ‐polymorphs of 2,4,6,8,10,12‐hexanitrohexaazaisowurtzitane (HNIW) have been studied as a function of temperature. Techniques employed include differential scanning calorimetry (DSC), differential thermal analysis/thermogravimetric analysis (DTA/TGA), and hot stage microscope analysis. Fourier transform infrared spectroscopy (FTIR) was used to identify results of polymorphic conversion. Results corroborate those(2) of Part I that the existence of multiple α‐hydrate phases complicates definition of the HNIW P‐T phase diagram. A high temperature endothermic DSC response was determined by FTIR spectroscopy to be the β → γ transition, not a conversion to a new high temperature “delta” phase. The role of water in the shifting this conversion to higher temperature is discussed.
Estimation and prediction of the heats of formation for non‐aromatic polynitro compounds on the basis of the QSPR approach
Authors: Sukhachev Dmitrii V. , Pivina Tatyana S. , Volk Fred S.
Published: December 2004

The analysis of “Quantitative Structure‐Property Relationship”(QSPR), concerning the heat of formation in the condensed state, is performed for non‐aromatic polynitrocompounds. The QSPR approach and our original computer program “EMMA”(Efficient Modelling of Molecular Activity) are used. This approach is based on the construction of optimal linear regression models involving physical‐chemical, topological, informational, and substructural indices; it can be used as an alternative to traditional additive schemes for evaluating physical‐chemical characteristics of energetic materials. On the basis of the QSPR method, the “structure‐heat of formation (ΔH°f)” relationship is revealed for a data base of non‐aromatic polynitrocompounds, and ΔH°f is predicted for some hypothetic substances.
Stabilizer reactions in cast double base rocket propellants. Part VI: Reactions of propellant stabilizers with the known propellant decomposition products NO2, HNO2, and HNO3
Authors: Sammour M. H. , Bellamy A. J.
Published: December 2004

The reactions of stabilizers with the individual reactive species known to be generated during double base propellant decomposition, viz. NO2, HNO2 and HNO3, have been thoroughly investigated in an attempt to obtain information on the reactions that take place in these propellant systems. It was found that the various stabilizers differ in their behaviour towards these reactive species, and this should help to give a clearer picture of the chemistry occuring during aging of double base propellants.
Plateau Burning Characteristics of AP Based Azide Composite Propellants
Authors: Oyumi Yoshio , Anan Toshiyuki , Bazaki Hakobu , Harada Tadamasa
Published: December 2004

The site and mechanism by which iron oxide catalyst acted to enhance burning rate and produced plateau burning behavior at high pressure was studied. The condensed phase chemistry study was conducted by isothermal thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC), and rapid‐scan FTIR spectroscopic technique. Uncatalyzed ammonium perchlorate (AP) based azide composite propellant showed unstable combustion at relatively lower pressure region. The heat balance at the buring surface would be unstable at these pressures. However, iron oxide altered the burning property of the propellant and enhanced the burning rate with the plateau‐mesa burning characteristics. Such pressure insensitiveness of the burning rate indicated that the condensed phase chemistry played important role in the catalytic mechanism of action. According to the microrocket motor tests, physical effect, melted fuel binder covered the AP particles and prevented the further decomposition of AP, had not affected the plateau burning. Fe2O3 was more effective on the burning rate augmentation than Fe3O4. However, the pressure exponent of the burning rate point of view Fe3O4 was favored catalyst to the propellant used here.
Carbon resistor gauges for measuring shock and detonation pressures. III. Revised calibration data and relationships
Authors: Austing James L. , Tulis Allen J. , Joyce Richard P. , Foxx Carl E. , Hrdina Donald J. , Bajzek Thomas J.
Published: December 2004

For many years, carbon resistors have formed the basis for measurement of shock and detonation pressures associated with condensed explosives. The gauge is fabricated by heat‐sealing the resistor into a plastic material such as polystyrene. When subjected to a strong shock wave, the resistance decreases, and the resulting increase in conductance is a function of the magnitude of the pressure. The present investigation was concerned with the experimental derivation of revised calibration equations, which was necessitated by the need to incorporate a terminating resistor into the gauge circuitry. The use of this resistor decreased the effect of standing waves and eliminated oscillatory ringing in the recorded signal. Typical records over a wide range of pressures are presented. An error analysis of the recorded data showed that the uncertainty in the measured pressure was of the same order of magnitude as the uncertainty in the interpretation of the recorded voltage from which the conductance was computed. An extensive discussion of the relevancy of the experimental data is presented, and the need for additional calibration experiments is stressed.
On the inconsistency of the asymmetric‐sandwich gurney formula when used to model thin plate propulsion
Authors: Hirsch Eitan
Published: December 2004

The asymmetric sandwich Gurney formula is used extensively worldwide during explosive reactive armor and shaped‐charge war‐head design, in either its original form(1,2) or its extended form used to model implosion configurations(3–5). It is therefore very important to realize that calculations may contradict physical observations when the formula is used to calculate the velocity of thin plates having mass which is smaller than half the explosive mass per unit area. This inconsistency between calculation and experimental results is explained as resulting from the failure of the assumption made in deriving all the Gurney formulas that the velocity distribution of the explosive products is a linear function of the expansion coordinate.
An Analysis of the Influence of Detonator Parameters on the propagation of shock waves in an inert medium
Authors: Cudzilo Stanislaw , Maranda Andrzej , Nowaczewski Jerzy , Trzciński Waldemar
Published: December 2004

The effect of mass, diameter and type of detonator on parameters of shock waves generated in plexiglas block is examined by experimental and theoretical means. The quantities connected with the shock wave, such as, the mean velocity of the shock wave front, the profile of mass velocity behind this front, and the mean velocity of free surface of the loaded block are measured.

To perform an numerical analysis of the shock wave parameters mentioned above on type and size of detonator the problem is considered of acting of detonation products of an explosive charge on a block of inert material. In this goal, the active mass of charge is determined and, next, the model assumptions and mathematical formulation of the problem of penetration of pressure pulse into inert medium are presented. The results of computer simulation and experimental data are compared.
LX‐17 Corner‐Turning
Authors: Souers P. Clark , Andreski Henry G. , Cook Charles F. , Garza Raul , Pastrone Ron , Phillips Dan , Roeske Frank , Vitello Peter , Molitoris John D.
Published: December 2004

We have performed a series of highly‐instrumented experiments examining corner‐turning of detonation. A TATB booster is inset 15 mm into LX‐17 (92.5% TATB, 7.5% kel‐F) so that the detonation must turn a right angle around an air well. An optical pin located at the edge of the TATB gives the start time of the corner‐turn. The breakout time on the side and back edges is measured with streak cameras. Three high‐resolution X‐ray images were taken on each experiment to examine the details of the detonation. We have concluded that the detonation cannot turn the corner and subsequently fails, but the shock wave continues to propagate in the unreacted explosive, leaving behind a dead zone. The detonation front farther out from the corner slowly turns and eventually reaches the air well edge 180° from its original direction. The dead zone is stable and persists 7.7 μs after the corner‐turn, although it has drifted into the original air well area. Our regular reactive flow computer models sometimes show temporary failure but they recover quickly and are unable to model the dead zones. We present a failure model that cuts off the reaction rate below certain detonation velocities and reproduces the qualitative features of the corner‐turning failure.
Atomic Force Microscopy study of hexagonal boron nitride film growth on 6H‐SiC (0001)
Authors: Chen Wei , Ping Loh Kian , Lin Ming , Liu Rong , Wee Andrew T. S.
Published: December 2004

Boron nitride thin films with their unique mechanical and electrical properties are of interest for various applications and have been grown on a number of different substrates. The cover picture from this issue's Editor's Choice [1] shows an Atomic Force Microscopy topography of a hexagonal BN film grown on 6H‐SiC substrate by Plasma Enhanced Chemical Vapor Deposition at 600 °C. Interesting stress‐relief features developed on the non‐reactive substrate. The corresponding author Kian Ping Loh is Assistant Professor at the National University of Singapore. His research is devoted to the growth of diamond and boron nitride thin films and the fabrication of nanocrystalline diamond and boron nitride nanotubes.

As a follow‐up to the recent special issue on ‘Physics of Organic Semiconductors’ [2], Detlef Berner gives insights into organic light emitting diode functioning by coordinated experiment and simulation in his Review Article [3].

The present issue also sees the start of our rapid research letters, the fastest peer‐reviewed publication medium in solid state physics. For more information see www.pss‐rapid.com and the Editorial by the Editor‐in‐Chief Martin Stutzmann on page 7 [4].
Synthesis and Radiochemical Labeling of N‐(2,6‐Diisopropylacetanilido)‐Iminodiacetic Acid and Its Analogues under Microwave Irradiation: A Hepatobiliary Imaging Agent
Authors: Park Sang Hyun , Gwon Hui Jeong , Park Jeong Sook , Park Kyung Bae
Published: December 2004

This paper describes a fast and convenient procedure for the synthesis of 2,6‐diisopropylacetanilidoiminodiacetic acid and its analogues and radiochemical labeling with 99mTc. They were synthesized in large scale under microwave irradiation in very short reaction times. A microwave reactor offers a rapid and efficient methodology for the formation of a considerable range of IDA derivatives. The method is expected to be applicable to the preparation of radiopharmaceuticals.
Microwave‐assisted aza‐Baylis‐Hillman Reaction. Preparation of Poly(ethylene Glycol) Supported α‐methylene‐β‐Aminoester
Authors: Ribière Patrice , Yadav‐Bhatnagar Neerja , Martinez Jean , Lamaty Frédéric
Published: December 2004

The aza‐Baylis Hillman is a practical method for the preparation of α‐methylene‐β‐aminoesters. A soluble polymer supported version of this reaction has been developed. The reaction was shown to proceed in the absence of solvent under microwave activation. In the presence of 3‐hydroxyquinuclidine, the reaction time was reduced from 3–12 h under thermal conditions to 30 min under microwave irradiation. A small library of PEG‐supported aminoesters was generated.
Microwave‐assisted Synthesis of a 3‐Aminoimidazo[1,2‐a]‐pyridine/pyrazine Library by Fluorous Multicomponent Reactions and Subsequent Cross‐coupling Reactions
Authors: Lu Yimin , Zhang Wei
Published: December 2004

Microwave and fluorous technologies are employed to increase reaction speed and reduce separation time in solution‐phase parallel synthesis of a substituted 3‐aminoimidazo[1,2‐a]pyridine and 3‐aminoimidazo[1,2‐a]pyrazine library. Multicomponent reactions of perfluorooctanesulfonyl‐tagged benzaldehydes with 2‐aminopyridines (or 2‐aminopyrazines) and isocyanides are followed by Pd‐catalyzed cross‐coupling reactions with boronic acids or thiols to form biaryls or aryl sulfides. Reaction mixtures are purified by fluorous solid‐phase extraction (F‐SPE) or crystallization.
Improved depth resolution in Auger depth profiling of multilayered thin films by reactive ion sputtering
Authors: Blattner R. J. , Nadel S. , Evans C. A. , Braundmeier A. J. , Magee Charles W.
Published: December 2004

Reactive ion sputtering (N) is shown to improve depth resolution significantly in conventional Auger electron spectroscopy depth profiling of multilayered metallic thin film samples as compared to standard argon ion bombardment. Layer modulations on the order of the escape depth of the Auger electrons are shown to be discernible by conventional Auger depth profiling in a texturing‐prone situation (microscopically modulated thin film samples) when N is used as the sputtering species. Oxygen ion sputtering was observed to give greater improvement in depth resolution than nitrogen, but was also observed to have a deleterious influence on instrument performance. Increasing the N ion energy from 2 to 5 Ke V was found to degrade depth resolution slightly.
The coadsorption method in Auger electron spectroscopy: Applications to the analysis of contaminated nickel surfaces
Authors: Oda O. , Read G. E.
Published: December 2004

Three examples of applications of the coadsorption technique using a metal monolayer ‘étalon’ in AES are described. They concern adsorption of tin on nickel (100) surfaces partially contaminated with lead, phosphorus or oxygen. The results extend an earlier account and point to some new phenomena (desorption stimulated by the metal vapour, complex variations in sticking probability, multiplayer growth, adsorbate diffusion) that can be examined using this technique.
Studies of the metal–support interaction in coprecipitated nickel on alumina methanation catalysts using X‐ray photoelectron spectroscopy (XPS)
Authors: Shalvoy R. B. , Davis B. H. , Reucroft P. J.
Published: December 2004

Characterization studies on a series of coprecipitated alumina‐supported nickel methanation catalysts by X‐ray photoelectron spectroscopy are described. Binding energies and spectral shapes have been determined for several standard compounds (Ni, NiO, Ni(OH)2, NiAl2O4, Al2O3) to provide background information for interpreting the catalyst spectra. The results indicate that the surface regions of the fresh (unreduced) catalysts are composed primarily of amorphous NiAl2O4 with some NiO particles present either within the pores of the support or covered by a NiAl2O4 layer. In comparison with similarly prepared silica‐supported catalysts, reducibility is more difficult indicating the presence of stronger support interactions.
Calculations of the backscattering factor for L3MM Auger transitions
Authors: Jabłoński Aleksander
Published: December 2004

The single scattering Monte Carlo algorithm of Murata, Matsukawa and Shimizu and the Gryziński ionization cross‐section were used in calculations of the backscattering factor r. The calculations were based on two definitions of r. Generally, the backscattering factor was defined as the ratio of the Auger electron current recorded by the analyser to the current that would be recorded in the ideal case of no backscattering and no energy loss. The usual definition, involving the energy distribution of backscattered electrons, was also used. The calculations were performed for L3MM Auger transitions of elements with atomic numbers between 23 and 32. The primary energy ranged from 3 to 10 keV. The difference in backscattering factors resulting from both definitions varied from 0.1% to 10%, decreasing with the primary energy increase. The single scattering Monte Carlo algorithm can also be used in simulation of electron scattering in binary alloys. This makes possible the calculation of the backscattering factor as a function of the solid composition. The calculations were performed for L3MM Auger transitions of Cr, Cu, Fe and Ni in Au/Ni, Cr/Fe, Cr/Pd, Cu/Ni and Ni/Pd binary alloys. It was found that the backscattering factor varies almost linearly with mass fraction. The dependence on concentration is more pronounced when the difference in atomic numbers of alloy components is larger. The relative sensitivity factors, calculated for Cu/Ni and Cr/Fe binary alloys, are practically independent of composition, but depend on the primary energy.
X‐ray photoelectron spectroscopy studies of polymer surfaces, 4—further studies of the chromic acid etching of low density polyethylene
Authors: Briggs D. , Zichy V. J. I. , Brewis D. M. , Comyn J. , Dahm R. H. , Green M. A. , Konieczko M. B.
Published: December 2004

X‐ray photoelectron spectroscopy (XPS) has been used to study the chemical modification of low density polyethylene, high density polyethylene and polypropylene using a very mild treatment with chromic‐sulphuric acid or treatment with concentrated sulphuric acid. The treatment of low density polyethylene with CrO3‐water has been studied in detail by XPS and multiple internal reflection infrared spectroscopy. In all cases surface modification has been correlated with adhesion level to an epoxide adhesive. The XPS data are also used to discuss the adhesion of metals to CrO3‐water etched polymers and the effect of surface contaminants on adhesion to epoxides.
An alternative to the relative sensitivity factor approach to quantitative SIMS analysis
Authors: Morgan A. E.
Published: December 2004

Measurements have been made of positive secondary ion currents from oxygen bombardment of glass standards, obtained either from NBS or specially prepared in this laboratory. By using one fitting parameter, the ionization temperature Ti, a semi‐quantitative analysis (accurate to within a factor of 2–3) is possible on any one of these standards. This approach, whilst achieving an accuracy comparable to that obtainable using relative sensitivity factors, does not restrict the analysis to those elements for which sensitivity factors are available. Further, change of sample matrix, which can alter sensitivity factors in a seemingly puzzling fashion, can easily be rationalized and accommodated through variation in Ti. Values of Ti for 16 binary oxides lie between 5500 and 9500 K. The Ti value for a more complex matrix can be estimated on a proportional basis from these binary oxide results.
An X‐ray photoelectron spectroscopic study of gold containing a bulk antimony impurity
Authors: Proctor A. , Sherwood P. M. A.
Published: December 2004

The paper reports the detection by XPS of a bulk antimony impurity in a gold foil sample, as a result of its surface segregation upon heating in vacuo at 600 °C. The O 1s spectra indicate at least two possible oxygen species present in the vicinity of the gold surface. The interaction of the surface segregated antimony with oxygen does not appear to be as is reported for calcium impurities, the antimony showing the binding energy corresponding to metal. Also the amount of surface segregated antimony impurity does not seem to be as dependent as calcium impurities on previously adsorbed or gas‐phase oxygen. The use of the carbon 1s peak rather than the gold 4f peaks is found to be a more reliable calibration reference.
The use of plasmon‐loss peaks in studying the epitaxial silicon on alumina interface
Authors: Thomas J. H. , Hofmann S.
Published: December 2004

Intense plasmon‐loss features excited by kilovolt electron beams used in AES have been used to study the Si on Al2O3 interface. Variable electron beam energies provide a means of continuously varying the electron escape depth and subsequently removing this contribution from the plasmon‐depth profiles. Parametrically varying the ion energy extrapolation of the interface width to zero ion energy yields an intrinsic interface width of 13±4 å, or about six Si atom layers.
Sputter‐depth profiling in AES: Dependence of depth resolution on electron and ion beam geometry
Authors: Duncan S. , Smith R. , Sykes D. E. , Walls J. M.
Published: December 2004

The precise geometrical relationship between the ion and electron beams and the sample affects the depth resolution of sputter‐depth profiles in AES. A theory is presented which predicts this instrumental depth resolution by considering the shape of the ion‐eroded crater and the corresponding orientation of the electron beam. The variation in depth resolution is analysed for a range of conditions including (a) varying ion and electron beam diameter (b) the angular orientation of the electron and ion beam and (c) the effect of misalignment of the two beams.
Preparation of brittle thermoset specimens for surface characterization by contact angles
Authors: Bystry F. A. , Penn L. S.
Published: December 2004

A convenient and accurate method for surface analysis by contact angle studies is described. The specimen developed is particularly useful for brittle thermoset materials which must be prepared in a simple regular geometry for wetting force measurement by the Wilhelmy method. The procedure involves dip‐coating wires to make smooth cylindrical specimens of cured thermoset resin for wettability (contact angle) analysis. The results from this type specimen were cross‐checked with cast film specimen results to ensure that measured contact angles were material properties and were not influenced by geometry or presence of wire substrate. Results are presented for some modified and unmodified brittle thermoset resins showing changes in surface energetics.
Analysis of the auger electron line shape to determine the composition of CuNi alloys
Authors: Pamler W. , Röll K.
Published: December 2004

The quantitative analysis of alloys by Auger electron spectroscopy combined with ion beam sputtering becomes difficult when the Auger line shape depends on composition, when individual peaks overlap or when the composition is changed by preferential sputtering during ion bombardment. As an example, it is shown how these difficulties can be managed in the case of CuNi alloys. Variations of the peak shape in the alloy have been found to be a consequence of a linear superposition of the overlapping peaks of the pure elements. Therefore, the composition can be determined by a peak fitting procedure. The peak‐to‐peak amplitudes, on the other hand, are more complicated functions of the composition. It is shown how a concept including several sensitivity factors for the overlapping peaks can be used in order to determine the composition from the peak‐to‐peak amplitudes. The effects of preferential sputtering which produce an altered layer enriched in Ni can be corrected by an empirical sputtering correction factor. From these results the principal shape of the concentration profile within the altered layer has been estimated.
Simultaneous XRF and XPS analysis
Authors: Castle J. E. , Castle M. D.
Published: December 2004

The concept of utilising the x‐ray fluorescence spectrum, excited by bremsstrahlung radiation, whilst undertaking photoelectron spectroscopy is not new. However, it is only with modern multiprobe instruments and high quality data systems that the simultaneous display of both spectra becomes practicable. This paper explores the effective sampling depth and sensitivities across the energy range 1 to 10 keV. It concludes that the attachment of x‐ray detection equipment to an ESCA instrument is a practical and cost effective solution to the need to probe rather greater depths than XPS itself allows.
Barrier‐type anodic films on aluminium in aqueous borate solutions: 2—Film compositions by Rutherford backscattering spectroscopy and nuclear reaction methods
Authors: Skeldon P. , Shimizu K. , Thompson G. E. , Wood G. C.
Published: December 2004

Compositions and elemental distributions of anodic films formed on aluminium in aqueous borate electrolytes have been investigated by Rutherford backscattering spectroscopy (RBS) and associated nuclear reaction methods, together with controlled crystallization of film sections in the transmission electron microscope (TEM). Films were found to consist principally of Al2O3; the outer regions of the films were contaminated with boron and, for all cases studied, the inner regions were boron‐free. In the absence of film dissolution the contaminated region represented approximately 40% of the film thickness, and this proportion did not vary significantly with changes in current density of film formation. The outer region contained about 1.5 wt% boron, probably as B2O3, and the densities of the inner and outer regions were similar to an accuracy of about 10%.
Applications of a system for real‐time imaging of analyzed areas in surface analysis
Authors: Tomich D. H. , Grazulis L. , Koenig M. F. , Grant J. T.
Published: December 2004

A real‐time imaging system has been used to determine the analyzer acceptance area in electron spectrometers used for surface analysis. This inexpensive system uses an electron beam that is rastered across the specimen to create both specimen images and images of analyzed areas. These two images can then be superimposed on a video monitor or black and white television set for real‐time display at TV rates. The imaging system has been used to examine the properties of a double‐pass cylindrical mirror analyzer (Perkin–Elmer Model PHI‐550) and a hemispherical analyzer (KRATOS ES300). For the double‐pass CMA, the analyzed area was star‐shaped rather than the expected circular shape and in the retarding mode the analyzer pass energy had only a small effect on the size of the analyzed area; also, the minimum analyzed area did not coincide with the focal point of the analyzer as determined by an elastically back‐scattered 2 keV electron beam. For the hemispherical analyzer, the analyzed area was found to depend almost entirely on the size of the entrance slit, was slightly affected by the initial kinetic energy of the imaged electrons and the mode of operation, but was not affected by the analyzer pass energy or the size of the exit slit.
An IETS study of surface reactions applicable to adhesion
Authors: Henriksen P. N. , Gent A. N. , Ramsier R. D. , Alexander J. D.
Published: December 2004

Inelastic electron tunneling spectroscopy (IETS) has been used to study two classes of adhesion promoting compounds adsorbed on alumina: trialkoxysilanes and phosphonic acids. It has been shown that both types of compounds can condense directly with hydroxyl groups on the surface. Condensation is through the alkoxy groups in the case of the silanes and through the hydroxyl groups in the case of the acids. The silanes can further condense to form surface siloxanes. The absence of bands characteristic of the phosphoryl group in the spectra of the acids is indicative of resonance bond formation followed by ionic bonding to the surface.
New approaches to failure analysis using XPS sputter‐depth profiles
Authors: Davis G. D. , Clearfield H. M. , Moshier W. C. , Cote G. O.
Published: December 2004

The methodology of failure analysis and the use of XPS sputter‐depth profiles in failure analysis is illustrated in three examples: a titanium adhesive bond, a multilayer optical filter, and an ohmic contact. XPS sputter‐depth profiles supplement those obtained using AES and are essential to the failure analysis of a non‐conducting sample or one that is easily damaged by an electron beam. XPS sputter‐depth profiles also allow chemical state determination and improved quantification, especially for samples in which the Auger signals of different elements overlap.
Surface and thermal desorption investigations of chemically cleaned 316‐L stainless steel tubings
Authors: Simondet F. , di Giulio C. , Noel A. , Olliver E. , de Rugy H.
Published: December 2004

When dealing with high purity gas handling, the nature of metallic surfaces in contact with the gas is a major concern because these surfaces are a possible source of gaseous pollution. Several surface treatments may be applied to stainless steel tubes used in gas handling systems, and these lead to different desorption properties. A comparison of the topographical effects accomplished by roughness and SEM measurements, and chemical effects by XPS determinations was made. Results were correlated to the outgassing behaviour of 316‐L SS surfaces, as determined by thermal desorption mass spectroscopy. It appears that similar treatments of 316‐L SS may not result in similar outgassing properties. Electropolished surfaces are smoother and present the least outgassing, although carefully cold drawn and chempolished stainless steel surfaces also show a comparable outgassing behaviour.
Investigation of surface contamination on silicon wafers with SIMS
Authors: Stingeder G. , Grundner M. , Grasserbauer M.
Published: December 2004

Characterization of the surface of silicon wafers is necessary for control and development of cleaning procedures. An analytical approach for investigation of surface contaminants with SIMS is proposed. The major problem is the presence of the contaminants only in the native oxide (thickness ∼1.5 nm). This means that analysis has to be performed in a surface zone smaller than the implantation depth of the primary ions. Chemical matrix effects and a changing erosion rate are encountered owing to the native oxide and the dynamic process of primary ion implantation and sputtering. Owing to the necessity of analysing extremely thin surface layers very slow sputtering has to be applied (1–10 monolayers per min.). As a consequence the secondary ion intensities are low and hydrocarbon species interfere with the elements to be analysed. For the identification of the secondary ion signals the evaluation of isotopic ratios determined with low mass resolution (M/ΔM ∼ 350) is combined with measurement of high resolution mass spectra.
Development of a numerical simulation of depth profiles of multilayers composed of very thin layers
Authors: Dapor M. , Marchetti F.
Published: December 2004

A numerical approach is presented in order to simulate multilayer depth profiles. In many practical cases the normalized measured intensity may be described well by a superimposition of error functions. Here, calculation of the error function has been performed using an approximation formula that allows it to be obtained via a simple but accurate method.

Particular attention has been paid to the development of a procedure that can be applied to the fitting of experimental data relative to depth profiling of samples composed of many very thin layers.
Combination of ion beam techniques, AES and SIMS for the analysis of samples exposed in the plasma boundary of the JET tokamak
Authors: Coad J. P. , Simpson J. C. B. , Neill G. F.
Published: December 2004

A system combining ion beam and surface‐specific techniques for the analysis of probes exposed in the edge region of the plasma produced by the Joint European Torus (JET) is described. Among examples of the use of the system are the demonstration that 10–40% of the ionic charge flux in the boundary can be due to impurities, erosion and redeposition phenomena can be observed with small probes placed in the plasma boundary, and most of the oxygen observed on collector probes is an artefact resulting from exposure to air.
The application of ion beam bevel sectioning and post‐sputter etch treatment in Auger crater‐edge profiling
Authors: Skinner D. K.
Published: December 2004

A method of Auger crater‐edge profiling is described that uses electronic contouring of the ion beam from a focused ion source for the sputter formation of bevelled cross‐sections. Vanishingly shallow angles can be produced by this method, allowing high lateral magnification of layered structures with in‐depth resolution equal to the best obtainable by conventional Auger profiling. The many advantages of this approach are discussed, together with details of a new approach for improving in‐depth resolution. This entails post‐treatment of the sputter‐formed bevel using low‐energy sputtering and chemically assisted reactive ion beam etching. The methods are demonstrated using samples of buried SiO2 in Si and InP/GaInAs superlattice structures.
Growth and characterization of GaAs on sapphire (0001) by molecular beam epitaxy
Authors: Diebold Alain C. , Steinhauser S. W. , Mariella R. P. , Marti Jordi , Reidinger F. , Antrim R. F.
Published: December 2004

Crystal epilayers of (111)‐oriented GaAs have been grown successfully on sapphire (0001) substrates by molecular beam epitaxy. Although the epilayers were found to have a very high twin density, large areas (cm2) with no grain boundaries were observed. Both substrate surface preparation and temperature controlled the crystallinity. Reflection high‐energy electron diffraction (RHEED) was used to characterize the sapphire surface after ozone cleaning. RHEED patterns taken at several azimuths were consistent with an outermost layer of oxygen atoms. Powder x‐ray diffraction and rotation x‐ray photographs were used to determine growth conditions that resulted in an improvement in the crystalline order. Cross‐sectional transmission electron microscopy confirmed the crystalline nature of the GaAs epilayers. The quality of the GaAs was also characterized by photoluminescence. Finally, crystalline quality was assessed using double‐crystal x‐ray diffraction rocking curves.
The influence of chemical environment upon the mercury 5d electronic structure
Authors: Dowben P. A. , Kime Y. J. , Lagraffe D. , Onellion M.
Published: December 2004

We have investigated one and two monolayers of Hg adsorbed on Cu(100) by angle‐resolved photoemission. The electronic structure of one monolayer of Hg on Cu(100) is very similar to that of the free atom. Two monolayers of Hg on Cu(100) has an electronic structure that closely resembles that of bulk Hg. These results are compared to those obtained for Hg overlayers on Ag(100). We have also observed that the shallow 5d core levels of the first monolayer of Hg shift by 0.38 ± 0.05 eV to greater binding energy following the adsorption of the second monolayer of Hg.
XPS analysis of the interphase between an anaerobic adhesive and metal substrates
Authors: Hudak S. J. , Boerio F. J. , Clark P. J. , Okamoto Y.
Published: December 2004

X‐ray photoelectron spectroscopy (XPS) has been used to study the interphase between a model anaerobic adhesive system composed of triethylene glycol dimethacrylate monomer (TRIEGMA) and a curing system consisting of cumene hydroperoxide (CHP), acetylphenyl hydrazine (APH) and saccharin (BS), and the substrates copper, iron, zinc and aluminum. Miniature cantilever beam specimens were prepared by curing beams of the adhesive against beams of the metal substrates. The specimens were then immersed in liquid nitrogen, causing the adhesive to delaminate from the substrate. XPS spectra obtained from the adhesive failure surfaces were very similar to spectra obtained from the bulk adhesive, containing peaks corresponding to carbon, oxygen and trace amounts of sulfur and nitrogen. However, the spectra also contained peaks due to trace amounts of metal or metal ions from the substrate. Spectra obtained from the substrate failure surfaces were very different from those of the corresponding adhesive failure surfaces and contained peaks due to higher concentrations of metal or metal ions and higher concentrations of nitrogen and sulfur, indicating that failure was near the interface and that both BS and APH segregated to the interface. C 1s multiplex spectra obtained from thin films of BS spin‐coated from dilute solutions onto iron, copper and zinc contained a weak component shifted from the main hydrocarbon peak to higher binding energy by ∼3.1 eV. This was more similar to the shift observed from the hydrated sodium salt of BS (Δ2.9 eV) than neat BS (δ3.7 eV), indicating that BS readily forms a complex with these substrates. When a copper foil was placed in a solution of BS and analyzed periodically in XPS, peaks due to Cu(I) were initially observed in the Cu 2p spectra, but peaks due to Cu(II) appeared after ∼110 h. The Cu(II) BS complex was also observed when a blue powder, which precipitated when a copper foil was placed in a solution of BS in methanol, was analyzed. Spectra obtained from aluminum (which does not catalyze the polymerization of the anaerobic adhesive as well as copper or iron) did not show the formation of a BS‐metal complex in any of the samples studied.