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The neutron wavelength resolution, Bragg-edge measurement ability and future prospects regarding the neutron count rate were investigated at AISTANS. The wavelength resolution evaluated by Bragg-edge analysis using an iron powder sample is in reasonably good agreement with calculations at neutron wavelengths of 0.2–0.3 nm. Bragg-edge imaging was also performed on a steel plate sample with distinct regions of BCC and FCC crystallinity, and the different crystal structures were successfully discriminated. In addition, an aluminum sample containing a friction stir spot welding region was also measured and the 200 and 111 Bragg-edges at the two joining areas were observed. However, it was hard to characterize the difference in texture between the two areas. The neutron counting rate for Bragg-edge imaging is expected to increase by approximately a factor 50 in the near future thanks to the planned improvements of the electron beam power and the detection efficiency of the neutron detector.

A new electron accelerator has been designed and is now under construction at AIST, Tsukuba, Japan. The accelerator will be used to produce a pulsed neutron beam for materials analysis. The design maximizes the yield of slow neutrons with high pulse temporal resolution as described in a previous publication [K. Kino et al., Nuclear Inst. and Methods in Physics Research, A 927 (2019) 407–418]. The accelerator is composed of a thermal cathode type electron gun with S-Band buncher/accelerator cavity followed by three, 2.9 m long S-Band acceleration cavities. High power RF is supplied by three klystron units, with klystron No.1 supplying both the electron gun and the 1st cavity, and klystrons No.2 and No.3 connected to the 2nd and 3rd cavities respectively. The design parameters of the accelerator are; pulse rate: 100 Hz, pulse length: 10 μs, electron current: 250 mA, electron energy: 40 MeV. Operating at these parameters a maximum beam power of around 10 kW will be delivered to the water-cooled Ta target for neutron production. In this report we will describe the design and construction of the electron accelerator.

We have designed and been constructing a compact accelerator-driven neutron facility for Bragg edge transmission imaging of structural materials to obtain position dependent crystallographic information. In order to combine a high neutron wavelength resolution, which is especially required for strain measurements, and an intense neutron beam flux at the sample position, which is required for obtaining high quality statistics within practical measurement times, the components of the neutron facility are optimized. To achieve a high wavelength resolution while maintaining an intense neutron beam flux at the sample position, a solid methane decoupled cold moderator at about 20 K coupled with neutron guide tubes is employed. The target–moderator system, especially the moderator thickness was optimized using the Monte-Carlo simulation code PHITS. Neutrons will be produced using a 35-MeV electron accelerator which is currently under construction. The accelerator has a design maximum beam power of 10 kW, a maximum repetition rate of 100 Hz and a maximum pulse width of 10 μ s . The combination of the flight path length of about 8 m and the repetition rate is suitable for efficient Bragg edge measurements. The pulse width of the electron beam is suitable to achieve a high wavelength resolution with the solid methane decoupled moderator. The estimated flux of the neutron beam at the sample position is 1.2 × 104 ∼ 4 . 5 × 104 /cm2/s depending on the usage of super mirror guide tubes. The wavelength resolution at the sample is 0.5 ∼ 0.7% in the wavelength region from 0.3 to 0.4 nm.

We have constructed a compact accelerator-based neutron facility at the National Institute of Advanced Industrial Science and Technology (AIST) in Japan aiming at development of structural materials of transportation vehicles for weight reduction. The facility consists of electron linear accelerator, neutron source, and a neutron beamline with a measurement hutch. Currently we are commissioning the accelerator and expecting a first neutron beam in 2019.

A quantitative nondestructive Bragg-edge imaging technique for power-storage degradation was developed using commercial prismatic-shaped lithium-ion battery cells. The C or Li atoms/ions column density [cm−2] images for five phases of the negative electrode material (graphite, Li0.04C6, Li0.2C6, Li0.5C6, and Li1.0C6) with a 1 mm spatial resolution were obtained by considering the crystalline orientation for both fresh and fatigue cells. In the fresh cell, most of the graphite was uniformly converted to Li1.0C6 by charging, and in the fatigue cell, the graphite changed to various phases (especially, Li1.0C6 and Li0.5C6) by charging, and their spatial distributions were nonuniform.

Neutron imaging is a powerful tool for observing the internal structure of an object without destroying the object. Neutron imaging (neutron radiography) is a prominent application of neutrons but still requires significant improvements, for example, in sensitivity, resolution, radiation hardness, and handling of neutron imaging detectors. This paper presents the development and the first neutron imaging results of a neutron flat-panel detector (nFPD) based on an In-Ga-Zn-O (IGZO) thin-film transistor (TFT)/photodiode array coupled with a LiF/ZnS scintillator sheet. Direct photo-coupling to the scintillator increases the light collection efficiency. Moreover, unlike lens-coupled neutron cameras, the proposed detector is compact and easy to handle. Owing to the high off-state resistance of IGZO TFTs, their leakage current is lower than that of conventional TFTs, enabling the IGZO TFTs to hold an accumulated charge for a longer period of time and allowing longer exposure times for imaging. This would be a powerful feature for imaging at compact neutron sources with limited flux. This paper reports on the first neutron imaging results with an IGZO nFPD, its performance evaluation, and a demonstration of three-dimensional computed tomography with neutrons.

The size of structural vacancies and structural vacancy density of 1/1-Al–Re–Si approximant crystals with different Re compositions were evaluated by positron annihilation lifetime and Doppler broadening measurements. Incident positrons were found to be trapped at the monovacancy-size open space surrounded by Al atoms. From a previous analysis using the maximum entropy method and Rietveld method, such an open space is shown to correspond to the centre of Al icosahedral clusters, which locates at the vertex and body centre. The structural vacancy density of non-metallic Al73Re17Si10 was larger than that of metallic Al73Re15Si12. The observed difference in the structural vacancy density reflects that in bonding nature and may explain that in the physical properties of the two samples.

Native defects and ion-implantation induced defects in GaN were studied by means of positron annihilation. Measurements of Doppler broadening spectra of the annihilation radiation for GaN layers grown on Si substrates showed that optically active vacancy-type defects were formed in the layers. Charge transition of the defects due to electron capture occurred when the layers were irradiated by photons with energy above 2.7 eV. It was found that Ti deposition and subsequent annealing introduced vacancy clusters. We also characterized vacancy-type defects in Mg-implanted GaN. The major defect species of vacancies introduced by Mg-implantation was a complex between Ga-vacancy (VGa) and nitrogen vacancies (VNs). After annealing above 1000C, these defects started to agglomerate, and the major defect species became (VGa)2 coupled with VNs. Through this work, we have demonstrated that positron annihilation spectroscopy is a powerful tool for characterizing vacancy-type defects in GaN for power devices applications.

We constructed a new apparatus, built upon a trap-based slow positron beam, for the production of a collimated, energy-tunable positronium beam under ultra-high vacuum conditions employing the photodetachment of positronium negative ions. A slow positron generator consisting of a 22Na radioisotope (20 mCi) combined with a buffer-gas positron trap is employed to generate high-quality, nano-second positron bursts with a repetition rate of 1 Hz-1 kHz. The positron bursts are focused onto an efficient positron-to-positronium negative ion converter, a Na-coated W thin film in a transmission geometry, using a magnetic lens system. The ions emitted from the opposite surface of the film are electrostatically accelerated to a given energy and photodetached by a pulsed infrared laser to form a mono-energetic positronium beam with kinetic energies of 0.2 keV-3.3 keV. The achieved detection rate of Ps atoms is 23 cps at the energy of 3.3 keV with a signal-to-background ratio as high as 300. The energy spread of the beam was evaluated by comparing the result of the time-of-flight measurements and particle-tracking simulations. With the use of a collimator of 1 mm diameter, a coherent beam with an angular divergence of less than 0.3° is obtained. The obtained Ps beam, having a much higher quality than those reported hitherto, will open up a new field of experimental investigations, such as Ps interacting with a variety of materials and fundamental studies on Ps spectroscopy.

The knowledge of elemental migration associated with angstrom-scale open spaces is a prerequisite for sophisticated material design with respect to nanodispersion as well as a better understanding of molecular migration in a geological environment. Here, we show the methodology for evaluating the diffusion coefficient of guest substances focusing on angstrom-scale open spaces, where the depth-variation of open spaces caused by elemental diffusion in the micrometer-scale surface region is examined by the variable-energy slow positron beam. The present methodology determines a low diffusion coefficient of ∼10-14 cm2 s-1 for potassium at 533 K in SiO2 glass within the framework of Fick's principle providing the evidence that ∼2.5 A open spaces intrinsically present in the glass matrix govern the diffusion process.

Recently, we have found that the microvoid size in a-Si:H, determined via positron annihilation lifetime spectroscopy (PALS), is systematically correlated with the optical constant, the peak value of e 2 ;e 2 peak, obtained from spectroscopic ellipsometry. This indicates a possibility to establish a novel characterization method that allows the average size and density of microvoid to be estimated readily via spectroscopic ellipsometry. In this presentation, we demonstrate a new finding that the microvoid size and the e 2 peak of a-Si:H films deposited under different conditions, even including the sort of apparatus, are on an identical curve if a-Si:H films are prepared without doping.

Reverse osmosis (RO) has been employed as a key separation process in many industrial applications. In recent years, the use of positron annihilation spectroscopy (PAS) including positron annihilation lifetime spectroscopy (PALS) and Doppler broadening of annihilation radiation to characterise the internal structure of the skin layer of thin film composite membranes has renewed research interest for further development and optimisation of the RO process. In this paper, we highlight the need for better understanding of the skin layer internal structure. We review relevant PAS techniques that could provide an unprecedented level of insight to our understanding of the internal structure of the active skin layer of RO membranes. PALS data reported in previous studies revealed that commercially available RO membranes have a mean free-volume hole-radius of 0.20–0.29 nm in the active skin layer. Data corroborated from the literature show a good correlation between the mean free-volume hole-radius of RO membranes and the rejection of boric acid which can be considered as a model small and neutral solute. The data also highlight the need for a comprehensive inter-laboratory study to standardise free-volume hole-radius measurement using PALS. In addition to free-volume hole-radius, free-volume fraction and thickness of the active skin layer appear to be important membrane properties governing neutral solute rejection. A roadmap is suggested to enhance the understanding of the transport of small and neutral solutes in RO. This includes integrating PAS with other techniques (e.g. molecular dynamics simulation) to describe the internal structure of RO membranes.

A Zero-Boil-Off (ZBO) cryostat is designed to realize a compact, stand-alone cryogenic system for the AIST superconducting accelerator (SCA). Under normal operation there is no evaporative helium loss from the cryomodule and therefore operating costs associated with the supply of liquid helium can be eliminated. The only significant loss of helium from the module occurs during the initial cavity cool-down procedure or when the re-condensing cryostat is replaced. It takes about 3 h to cool down the cryostat head from room temperature (300 K) to 4 K. During this time around 100 L of liquid helium is lost due to evaporation. By pre-cooling the cryostat inside a low heat load vacuum tube before transfer to the cryomodule, this evaporative loss could be essentially eliminated, significantly reducing the volume of liquid helium required for the initial cryomodule cool-down. The pre-cooling system also provides an efficient method to test the cryostat prior to use.

The properties of materials involving polymer–solid interfaces are determined not only by the properties of the constituents but also by the interfacial region of the polymer near the solid, the so-called interphase. Here we report on positron annihilation lifetime spectroscopy (PALS) measurements of the free volume near the interface with a focused positron beam. The measurements were performed at an interface between a Teflon AF 1600 film and a 30 nm thick SiN membrane from the backside of a Si substrate which was locally etched away to expose the ultrathin SiN membrane. We were able to focus the positron beam onto the exposed region and to probe the SiN–Teflon AF 1600 interfacial region with low implantation energies, resulting in very narrow implantation profiles and excellent depth resolution. We found a pronounced decrease in orthopositronium lifetime close the interface. On the basis of modeling, we could estimate the interphase width and the average density increase in the interfacial region as ∼1...

Positron beam facilities are widely used for solid state physics and material science studies. A positron beam facility has been constructed at the Kyoto University Research Reactor (KUR) in order to expand its application range. The KUR is a light-water-moderated tank-type reactor operated at a rated thermal power of 5 MW. A positron beam has been transported successfully from the reactor to the irradiation chamber. The total moderated positron rate was greater than 1.4 × 10 6 /s while the reactor operated at a reduced power of 1 MW. Special attention was paid for the design of the in-pile position source to prevent possible damage of the reactor in case of severe earthquakes.

The effects of heat treatment on membrane fouling resistance and the rejection of small and neutral solutes by reverse osmosis (RO) membranes were elucidated. RO membrane modification by heat treatment reduced fouling and improved boron rejection. However, heat treatment also caused a decrease in the water permeability of RO membranes. Significant improvement on fouling resistance by heat treatment was observed when RO concentrate was used to simulate a feed solution with high fouling propensity. The improved fouling resistance is likely to be due to changes in the hydrophobic interaction between the membrane surface and foulants. Boron rejection by the ESPA2 membrane was enhanced by heat treatment from 26 to 68% (when evaluated at the permeate flux of 20 L/m2 h). Positron annihilation lifetime spectroscopy revealed that heat treatment did not significantly influence the free-volume hole-radius of the membrane active skin layer. The results reported in this study suggested that changes in the other membrane properties such as free-volume fraction and thickness may be the main cause improving boron rejection.

Two types of commercial cellulose triacetate hollow-fiber membranes with different water fluxes, apposite for a reverse osmosis separation process, were investigated by means of positron annihilation lifetime spectroscopy with a 22Na-radioisotope-based energy-tunable positron beam, in order to elucidate a depth profile of the free-volume hole size in a subnanoscopic viewpoint. The lifetimes of ortho-positronium (o-Ps), the triplet positron-electron pair, for the two membranes were measured as a function of positron incident energy E. The E dependence of the hole size, quantified from the o-Ps lifetime, indicated that the separation-active dense layers with the smallest hole sizes are located at the near-surface region for both the membranes. The ratio of the dense-layer thicknesses for the two membranes was estimated to be more than 50% of the ratio of the respective effective thicknesses calculated from the water flux based on Darcy's law. The result signified that the dense layer with the smallest hole size at the near-surface region considerably contributes to the difference in the water flux.

A new photon-induced positron annihilation lifetime spectroscopy approach has been developed using an S-band compact electron linac at the National Institute of Advanced Industrial Science and Technology (AIST). The high energy ( 42 MeV ), intense (105 photons pulse−1), and ultra-short pulse (3 ps pulse width) photon beam creates positrons throughout an entire sample via pair production. A positron lifetime spectrum can be obtained by measuring the time difference between the accelerator's RF frequency and the detection time of the annihilation gamma rays. The positron lifetimes for lead and yttria-stabilized zirconia samples have been successfully measured.

Open spaces in polyethylene terephthalate (PET) coated with aluminum silicate (Al x Si 1 − x O y ) were probed using monoenergetic positron beams. The energy distributions of the annihilation γ rays and the positron lifetime spectra were measured for 60-nm-thick Al x Si 1 − x O y ( x = 0–1) deposited on PET using electron-beam evaporation. A clear correlation was obtained between the line-shape S parameter of the annihilation γ rays, water vapor, and oxygen transmission rates. The results suggest that open spaces in the Al x Si 1 − x O y layers play an important role in water/oxygen diffusion in Al x Si 1 − x O y /PET, where the concentration/size of such spaces showed its minimum value at x = 0.2–0.3. The free volume fraction below the interface between Al x Si 1 − x O y and PET (region width = 100–400 nm) was decreased by the deposition of the coating layer, and this region was also considered to act as a barrier against penetrations of gasses and molecules.

We investigated the residual defects in low-dose (1013 cm−2) arsenic implanted Si after high-temperature (1100 °C) annealing. The presence of residual damage was successfully revealed after using a rapid thermal process for heat treatment. This damage was identified as vacancy-type defects distributed near the surface, such as tetravacancies or pentavacancies. When O2 gas was introduced to the annealing chamber, vacancy-type defects were transformed into divacancy and carbon–oxygen complex. They were confirmed to be created by a non-equilibrium reaction during the rapid cooling-down step in the annealing sequence.

Pore entrance size of cage-like pores in mesoporous silica films is difficult to be determined by conventional techniques. A simple expedient is proposed by using positron annihilation lifetime spectroscopy (PALS) based on a slow positron beam. Because of the nature of positronium (Ps, the bound state of a positron and an electron) in mesoporous silica, almost no Ps annihilates in the smaller connecting channels of cages. By trimethylsilylation of the silica, an appreciable fraction of Ps can be trapped and annihilate in the channels, which renders the possibility to estimate the pore entrance size from Ps lifetime in it.

Free-volume hole-radii of the active skin layer of one seawater and two low pressure reverse osmosis (RO) membranes – namely SWC5, ESPAB, and ESPA2 respectively – were evaluated using positron annihilation lifetime spectroscopy (PALS) with a slow positron beam. The results were related to the rejection of boric acid and eight N-nitrosamines to provide insights to the transport of these small solutes through RO membranes. At pH 8 (which is the experimental pH in this study), these solutes are uncharged. PALS analysis showed that the SWC5 has the smallest mean free-volume hole-radius (0.259 nm) among the three RO membranes investigated here. Correspondingly, the SWC5 membrane exhibited the highest rejection of boric acid and all N-nitrosamines. Results reported here also showed that the rejection of these chemicals increased in the order of increasing molecular volume. In addition, the difference in their rejection amongst the three RO membranes investigated here was most apparent for those (i.e., boric acid and N-nitrosodimethylamine (NDMA)) with a small molecular volume. The EPSA2 and ESPAB were determined to have mean free-volume hole-radius of 0.289 nm. However, the ESPAB membrane had lower water permeability and showed considerably higher rejection of boric acid and NDMA than the ESPA2 membrane. These results suggest that in addition to the mean free-volume hole-radius, other membrane parameters and properties such as the free-volume hole-radius distribution and thickness of the active skin layer can also play a role in governing the rejection of small and uncharged solutes by RO membranes.

Commercial composite membranes for water purification were studied by means of the variable-energy positron annihilation γ-ray technique. The positron incident energy E dependence of R parameter (3γ/2γ ratio) analyzed from positron annihilation γ-ray spectra revealed the layer structure consisting of a dense top layer and a porous substrate for the membranes. Thickness of the dense layer for each membrane was evaluated from the R(E) based on a positron implantation stopping profile.

We describe the recent installation of a new slow positron beamline at AIST and our plans to develop a dedicated superconducting accelerator for positron production. The new positron beamline is already installed and should be operational by the end of this fiscal year (March 2012). Initially positrons will be generated using a 70 MeV electron beam from the existing accelerator directed onto a newly installed converter and moderator assembly. The beamline has two experimental ports both dedicated to positron lifetime spectroscopy, one port with a focused beam (diameter ~ 30 microm) and the other unfocussed (~ 10 mm). A superconducting accelerator for positron production is currently under development. When completed, it will deliver a high frequency (~ MHz), high current (~ mA), short pulse length (< 100 ps) beam to the positron production target. We investigate the possibility of transporting the positron pulses thus produced directly onto samples for lifetime measurement. Such a scheme would remove the necessity for pulse stretching and chopping which is required with the existing LINAC and should allow for greatly increased slow positron transport efficiency.

Positron annihilation lifetime spectroscopy (PALS) is an experimental technique whereby the lifetime spectrum of positrons injected into a material is measured. Analysis of this spectrum can be used to characterize defects in the material. While radioisotope positron sources are often used for PALS, there are several advantages of using mono-energetic, slow positron beams. In order to measure lifetime spectra with such beams it is necessary to produce a pulsed beam with an extremely short pulse length (~ 200 ps). In this article we discuss the advantages of using pulsed, slow-positron beams, the various methods of beam production and pulsing methods. We focus in particular on intense beams generated by electron accelerators and describe the current status and future plans for the accelerator based facility at AIST.

Hydrogen behavior and hydrogen-enhanced lattice defect formation under elastic stress of tempered martensitic steel were clarified with respect to dislocations and vacancies by thermal desorption analysis (TDA) using hydrogen as a probe of defects and a positron probe microanalyzer (PPMA). The relationship between hydrogen embrittlement and lattice defects associated with hydrogen was also investigated. The amount of lattice defects increased gradually with increasing the time of applied stress during hydrogen charging. The specimen fractured under elastic stress in the presence of hydrogen macroscopically showed brittle fracture without necking. Whereas fracture surface was attributed to localized plastic deformation, since the morphology of the microscopic fracture surface was mostly quasi-cleavage fracture. The increased lattice defects in the near-fracture area were subsequently removed by annealing at 200°C. The mean positron annihilation lifetime measured with the PPMA for a fractured specimen was longer in the near-fracture area than in other areas. Thus, the most probable reason for the increase in the amount of lattice defects can be ascribed to an increase in the amount of vacancies or vacancy clusters. Regarding hydrogen embrittlement involving microscopic plastic deformation, the localized enhanced vacancies due to interactions between dislocations and hydrogen under elastic stress directly caused ductility loss, because ductility loss occurred even though hydrogen was completely removed by degassing before the tensile test. Besides hydrogen content and applied stress, the time of formation and accumulation of vacancies are also concluded to be important factors causing hydrogen embrittlement.

Nanometer-sized voids formed in Si after H implantation to a dose of 3¥10 16 cm -2 and annealing at 600 or 800 iC were characterized by slow-positron and ion-beam analyses. Depth profiles of defects were calculated from the S parameter curves of Doppler broadening and from Rutherford backscattering/channeling spectra. Concentrations of gettering sites were also calculated from the Rutherford backscattering spectra of the samples after Au gettering. Defect profiles by Doppler broadening measurements were found to be shallower than the projected range of implanted H, while profiles of defects and gettering sites detected by the backscattering measurements were close to the projected range. The peak concentrations of defects and gettering-sites were dependent on annealing temperature and analytical techniques. The observed annealing behaviors can be explained by the evolution of vacancy clusters and the interaction of H with defects.

A slow-positron beam system for in-situ positron lifetime measurements during ion beam irradiation is currently under development in order to obtain fundamental information on radiation-induced defects. The system uses a high-intensity positron beam generated through pair-creation by a 70 MeV electron beam from a linear accelerator. The system has typical pulsing electrodes for chopping and bunching positrons. The incident directions of positrons and ions are 0° and 45° to the surface normal of samples, respectively. H, He and inert-gas ions up to 150 keV can be introduced to a target chamber with the irradiation temperature variable from room temperature to 600 °C. In a preliminary examination of the beamlines, 150 keV Ar+, electrons from a photocathode and positrons from a radioisotope were successfully transported to the target chamber from their respective sources. In addition, in-situ lifetime measurements using the existing positron beamline were demonstrated.

Positron annihilation lifetime spectroscopy (PALS) using a low-energy positron microbeam extracted into air was applied to elucidating molecular-level pore structures formed in silicon-oxide-backboned microporous thin films under controlled humidity conditions; as a result, a direct observation of the interstitial spaces in the micropores filled with water molecules was achieved. It was demonstrated that PALS using a microbeam extracted into air in combination with water vapor adsorption is a powerful tool for the in-situ elucidation of both open and closed subnanoscaled pores of functional thin materials under practical conditions.

To improve the spatial resolution of positron annihilation spectroscopy (PAS), a system to produce an intense positron microbeam was developed in AIST. A slow positron beam, which was produced by an electron linear accelerator, was focused by a lens onto a remoderator to enhance its brightness. The brightness-enhanced beam with an intensity of ≈1 × 106 e+/s was extracted from the remoderator and focused onto the sample by a lens. The beam size at the sample was 25 μm, which is more than two and half orders of magnitude smaller than that in the magnetic transport system (≈10 mm). Hence, the spatial resolution of PAS with an AIST positron microbeam can be drastically improved relative to PAS using conventional methods.

Positronium annihilation lifetime (PAL) spectroscopy and Doppler broadening energy spectra (DBES) have been used to search for selectivity and sensitivity for cancerous skin samples with and without cancer. This study is to further explore the melanoma cancerous system and other different types of skin samples. We found that the S parameter in melanoma skin samples cut at 0.39 mm depth from the same patient's skin is smaller than near the skin surface. However in 10 melanoma samples from different patients, the S parameters vary significantly. Similarly, among 10 normal skin samples without cancer, the S parameters also vary largely among different patients. To understand the sensitivity of PAS as a tool to detect cancer formation at the early stage, we propose a controlled and systematic study of in vivo experiments using UV-induced cancer skin from living animals.

Mesoporous silica films were synthesized via a sol–gel process under an acidic condition. Various amounts of triblock copolymer F38 were loaded to precursor sols as the pore generator. The evolution of the pores generated by porogen decomposition was investigated as a function of F38 loading by positron annihilation gamma-ray energy spectroscopy and positron annihilation lifetime spectroscopy based on slow positron beams. The threshold of pore percolation is found to be around 10 wt% of F38 loading by positron annihilation gamma-ray energy spectroscopy. Positron annihilation lifetime spectroscopy in the films show that the pore size increases from 1 nm to 3 nm with increasing F38 loading from 5 wt% to 30 wt%.

The free-volume depth profile of asymmetric polymeric membrane systems prepared by interfacial polymerization is studied using positron annihilation spectroscopy coupled with a variable monoenergy slow positron beam. Significant variations of S, W, and R parameters from the Doppler broadened energy spectra vs positron incident energy up to 30 keV and orthopositronium lifetime and intensity are observed at different doping times of triethylenetetraamine (TETA) reacting with trimesoyl chloride (TMC) in an interfacial polymerization on modified porous polyacrylonitrile (PAN) asymmetric membrane. The positron annihilation data are analyzed in terms of free-volume parameters as a function of depth from the surface to nano- and micrometer regions of asymmetric membranes. A multilayer structure is obtained in polymerized polyamide (PA) on modified PAN membranes (m-PAN): a nanometer scale skin polyamide layer, a nanometer to micrometer scale transition layer from dense to porous m-PAN, and the porous m-PAN suppo...