IPERION CHIntegrated Platform for the European Research Infrastructure ON Cultural Heritage

FIXLAB

The goal of FIXLAB is to provide access for the Cultural Heritage (CH) community to largescale facilities that develop and maintain sophisticated stateoftheart instrumentation for advanced diagnostics and archeometry. Access is offered to researchers in Heritage Science to help address the major questions posed by the materiality of CH artefacts in terms of their genesis, manufacturing processes, alterations, conservation and preservation.

The unique FIXLAB services offered to the CH community embrace:

  • advanced stateoftheart instrumentation
  • dedicated facilities with teams of experts in the field of microanalysis of CH artefacts
  • novel developments resulting from IPERION CH joint research activities to progressively improve access
  • development of both new samplepositioning devices at a microscale and software tools for the integration of imaging data

 

Contacts
Name: Michel Menu
Email: michel.menu@culture.gouv.fr

PIGE ( Particle Induced Gamma ray Emission )
Providers:

AGLAE-C2RMF (FR)

PIXE ( Particle Induced X-ray Emission )
Overview

Proton induced X-ray emission (PIXE) provides simultaneous elemental analysis from sodium to uranium in conventional vacuum and from aluminum to uranium external-beam in air arrangement. The sample is bombarded by protons of 1-4 MeV energy, inner shell ionization occurs followed by a prompt electron re-arrangement processes which is associated by emission of characteristic X-ray photons. The energies of the X-ray photons are determined by the atomic number of the emitting element, while the relative intensities are related to its concentration. Because of the intensive energy loss of the penetrating protons and absorption of the emitted X-rays in the sample itself the PIXE inherently sensitive to the near surface region up to some tens of micrometer depth. The elemental sensitivity of the PIXE analysis is determined by several factors, in favorable conditions it is in the ppm range. The external-beam PIXE technique is expansively applied for the non-invasive analysis of matrix and trace elements in unique archaeological artifacts and fine art creations.

Technical details

The external milli-beam PIXE setup at the 5 MV Van de Graaff accelerator of Wigner Research Centre for Physics is dedicated to cultural heritage applications. The properly collimated proton beam of 2–3.5 MeV energy is extracted from the evacuated beam pipe to air through a 7.5 micrometer thick Kapton foil. The target-window distance is 10 mm, at which distance the beam diameter was is about 0.8 mm. The extracted proton beam current can be set within the 1–10 nA range. The objects for analyses are fixed on a three-dimensional positioning stage. Manual positioning available for large objects up to 50 kg, and a computer controlled fine positioning for the smaller ones up to 5 kg The characteristic x-rays are detected and analyzed by an AMPTEK X-123 detector system. The SDD detector is positioned at 135° backward angle with variable absorbers to reduce the low energy x-ray counts and to stop the backscattered protons.

Further readings
  1. M. Mödlinger, P. Picardo et al. Archaeometallurgical characterization of the earliest European metal helmets, Materials Characterization 79:22-36,·February 2013
  2. B. Constantinescu, Daniela Cristea-Stan at al. Provenance studies of Central European Neolithic obsidians using external beam milli-PIXE spectroscopy, Nuclear Instruments and Methods in Physics Research Section B Beam Interactions with Materials and Atoms 318:145-148, January 2014
Providers

AGLAE-C2RMF (FR)

BNC-WIGNER (HU)

MTA-Atomki (HU)

 

PESA ( Proton Elastic Scattering Analysis )
Providers:

MTA-Atomki (HU)

 

NRA ( Nuclear Reaction analysis )
RBS ( Rutherford Backscattering Spectrometry )
ERDA ( Elastic Recoil Detection Analysis )
Providers:

MTA-Atomki (HU)

 

 

STIM ( Scanning Transmission Ion Microscopy )
Providers:

MTA-Atomki (HU)

 

 

XRF ( X-ray fluorescence )
FTIR ( Fourier transform infrared spectroscopy )
XAS ( X-ray Absorption Spectroscopy )
Raman
XRD ( X-ray Diffraction )
PGAA ( Neutron‐induced Prompt Gamma Activation Analysis )

Overview

Prompt Gamma Activation Analysis (PGAA) is a non-destructive bulk analytical tool for determination of elemental composition, based on the detection of prompt-gamma radiation induced by neutron capture into the atomic nucleus. The method is suitable to quantify the most major components and a few trace elements (e.g. B, Cl, Co, Cd, Hg, Sm and Gd) in rocks, minerals, ceramics, glass, metals and many inorganic materials. Compared to other analytical techniques, the PGAA has lower sensitivity for many geochemically important trace elements, thus application of complementary techniques are recommended.

Technical details

The PGAA instrument is located near the end position of the neutron guide No. 1. The upgraded 2Qc supermirror neutron guide improved the thermal-equivalent neutron flux at the PGAA sample positions to 9.6Å~107 cm–2 s–1. The beam can be collimated to a maximum cross-section of 2Å~2 cm2. Other cross-sections of 14Å~14 mm2, 10Å~10 mm2, 42 mm2, 23 mm2, 5 mm2 can be adjusted. Furthermore, a 1/30 attenuator can be applied to reduce the beam intensity, if necessary. A pneumatically actuated instrument shutter is used to control the entry of the neutron beam into the cabin while two computer-controlled secondary shutters are in place to allow independent operation of the PGAA and NIPS/NORMA facilities. The targets are mounted on thin Al frames by Teflon strings. The detector system of the PGAA facility consists of an n-type high-purity germanium (Canberra HPGe 2720/S) main detector with closed-end coaxial geometry, and a BGO Compton-suppressor surrounded by a 10 cm thick lead shielding.

Further readings
  1. Szentmiklósi, L., Belgya, T., Révay, Zs., Kis, Z., 2010. Upgrade of the prompt gamma activation analysis and the neutron-induced prompt gamma spectroscopy facilities at the Budapest Research Reactor. J. Radioanal. Nucl. Chem. 286, 501-505.
Providers

BNC-WIGNER (HU)

 

RAD ( Neutron X‐ray and gamma‐ray imaging )
Overview

RAD instrument utilizes transmission of neutrons or X-rays to obtain visual information on the structure and/or inner processes of a given object. Neutrons are able to pierce through several cm thick materials, so the inner structure of even a bulky object can be characterized in a non-destructive way. The interactions between the neutrons and the matter, however, result in the attenuation of the transmitted neutron beam so giving contrast on a sensitive screen. The image detection of the RAD station comprises digital imaging equipments being able to carry out 2D and 3D imaging using suitable scintillation screens. The dynamic radiography is performed by means of a low-light-level TV camera with a fast imaging cycle, making possible real-time imaging.

Technical details

The RAD neutron imaging facility is served by an in-pile, Cd-covered pin-hole-type collimator for neutron radiation. The measurement positions can be used for dynamic (DNR) and for static (SNR) imaging with a max. beam diameter of ~200 mm. The thermal-equivalent flux at target positions is around 4Å~107 cm-2s-1. The measured L/D ratio is ~250. The scintillation screens for neutron radiography have spatial resolutions between 70-250 μm; while the intensifying screens for X-ray radiography are with a spatial resolution of 100-200 μm. For better flexibility, there is a possibility to apply larger or smaller fields of views (FOV). There is a possibility to use beam filters made of boron-containing rubber and lead bricks, giving a fast/thermal neutron flux ratio of 77 instead of 0.6. Moreover, a sapphire-crystal filter is available to suppress fast neutrons, giving a fast/thermal neutron flux ratio of 0.029. The RAD facility is also equipped with an optional X-ray tube with a max. voltage of 300 kV, allowing dual-modality imaging. Two motorized sample stages, one for small and one for large samples (with a maximum load up to 250 kg) are available to support the investigated objects.

Further readings
  1. Kis Z, Szentmiklósi L, Belgya T, Balaskó M, Horváth LZ, Maróti B. (2015) Neutron based imaging and element-mapping at the Budapest Neutron Centre, Physics Procedia. 69 (2015) 40 – 47.
Providers

BNC-WIGNER (HU)

FSANS (Time of Flight Small Angle Neutron Scattering)
Overview

The FSANS instrument is a recently built instrument at the Budapest Neutron Centre site, used for non-destructive study of the nano-structural features of various materials, among them archaeological objects. The studied size range is between 10 nm and 500 nm. Because of its technical characteristics, it is complementary to the Yellow Submarine SANS Instrument.

Technical details

The FSANS diffractometer covers a Q-range from 0.0003 to 0.03 Å-1 and complementary to the Yellow Submarine SANS instrument allows to probe structures at larger length scales than the pinhole type SANS instrument. The instrument is installed on the bottom section of the curved neutron guide No.3, made of m = 2 supermirrors. The beam time structure is provided by 4 choppers: a counter-rotating pair of pulse definition choppers, one wavelength limiting and one frame overlap chopper. The available wavelength range is 2–16 Å. The width of the wavelength uncertainty can be set by choosing the pulse definition chopper window to 0.3 A° with 8° opening (better resolution mode) or 0.75 A° with 20° opening (higher intensity mode) respectively. The collimation distance is 3.7 m, the sample to detector distance is maximum 4.3 m. Samples from several millimetres to several tens of centimetres in diameter can be placed at the sample position, the beam size can be varied from 4mm (pinhole collimation mode) to 40 mm (focusing mode) in diameter. The scattered neutrons are detected by a 256 Å~ 256 pixels (0.7 mm Å~ 0.7 mm pixel size) two dimensional position sensitive detector filled with 3He gas. Data acquisition is performed in event recording mode.

Further readings
  1. http://www.bnc.hu/?q=node/18
Providers

BNC-WIGNER (HU)

NAA (Instrumental Neutron Activation Analysis)
Overview

Neutron activation analysis (NAA) is a method for quantitative composition analysis of chemical elements based on the conversion of stable nuclei in the sample to radioactive nuclei by nuclear reactions, followed by the quantitation of the reaction products via their gamma radiations. The k0-standardized neutron activation analysis (k0-NAA), combined with high-resolution and highthroughput gamma-ray spectrometry, offers mostly non-destructive, multi-elemental analysis for many branches of science and technology. NAA has inherently favorable characteristics, negligible matrix effect, excellent selectivity and high sensitivity. Even small amount (few tens of milligrams) of samples (mostly solid) can be measured, in which about 35–75 elements in less than 0.01 μg quantities can be determined.

Technical details

Samples for NAA are irradiated with thermal neutrons. Short and long time irradiations are possible in two designated vertical channels of the reactor. Short irradiations are done by means of a pneumatic rabbit system, whereas samples for long irradiations are loaded into the rotating channel of Budapest Research Reactor. The gamma-rays emitted from the sample are counted in low-level gamma-spectroscopic counting chamber to reduce the external background. In our NAA laboratory there are three low-level gamma-spectroscopic chambers, which are built from pre-World War II steel (free of any manmade radioactivity), have 10 cm thick wall covered with 2 mm thick Cu-layer inside to attenuate the X-rays. Two high-purity Ge detectors and two digital gamma spectrometers are used to detect the gamma-rays and to collect the spectra. The spectra are evaluated with the gamma spectroscopy package Hyperlab 2013.1. This includes automatic peak search, energy calibration the nonlinearity option, and net peak area computation, efficiency correction. For quantitative evaluation, the KayZero for Windows 3 program is used, based on the k0 standardization.

Further reading
  1. László Szentmiklósi, Dénes Párkányi, Ibolya Sziklai-László, Upgrade of the Budapest neutron activation analysis laboratory, J. Radioanal. Nucl. Chem. (2016) 309 91–99 DOI: 10.1007/s10967- 016-4776-7
Providers

BNC-WIGNER (HU)

TOF-ND (Time of Flight Neutron Diffractometer)
Overview

The TOF-ND instrument is a general purpose high resolution time-of-flight powder diffractometer. It covers a d-spacing range from 0.5 to 2.5Å (2.5 to 12.5 Å-1 in Q-range) at variable band-with and resolution (d=0.0015–0.15Å). It is applicable for structure determination and refinement, peak profile analyses, phase and texture analyses of solid state materials and for liquid diffraction as well. TOF provides information of the fine phase changes inside the materials, without producing any type of destruction in the sample.

Technical details

The instrument is installed at a radial thermal neutron beam. The monochromator system consists of a fast double and two single choppers and a straight neutron guide with 2.5Å~10 cm2 cross section at the exit. The double chopper is designed for a maximum speed of 12000 rpm. While in high resolution mode the very short – 10μs – neutron pulse and the 25 m total flight path allows to obtain a diffractogram with an accuracy of 1.5Å~10-3Å (at back scattering mode) in a single measurement on polycrystalline materials, in low resolution mode liquid diffraction can be performed at good neutron intensity up to 12.5 Å-1 scattering vector value. The beam is filtered by a silicon single crystal against fast neutrons. The double disk chopper (Ch1 and Ch2) has two windows: a 1.5° opening for short pulses (10 μs) and a 15° window for long variable pulses (20–200 μs), that can operate in parallel and in counter rotating mode. The latter option is used to produce very short pulses at high speed. To minimize the opening time, the neutron beam is reduced from 25 to 10 mm width at the position of the pulse choppers using a 4.5 m compressor neutron guide section before and a same decompressor after them. Ch3 defines the bandwidth and Ch4 prevents frame overlap. The instrument is recently equipped with a large surface back-scattering detector bank consisting of 88 pieces of squashed 3He tubes. It covers 20° scattering angle (2=145°–165°). The data are collected in the so called event recording mode: all events on the detector, the chopper signals and optionally changes in the sample environment are registered versus time. If this mode is used, many uncertainties can be filtered out during the data treatment, allow to perform time-dependent in-situ experiments in a single measurement.

Further readings
  1. http://www.bnc.hu/?q=node/10
Providers

BNC-WIGNER (HU)

PSD (Powder Diffractometer with a Position Sensitive Detector System)
Overview

The PSD neutron diffractometer is suitable for atomic structure investigations of amorphous and crystalline materials, as well as liquids where the resolution requirements are not high. The measured diffraction pattern is related to the positions of the atoms relative to each other in the material. PSD is a two-axis diffractometer equipped with a linear position sensitive detector system. The detector assembly is mounted on the diffractometer arm and it spans a scattering angle range of 25° at a given detector position. The entire diffraction spectrum is measured in five steps.

Technical details

The detector of the PSD is a system from Studsvik NFL (Sweden). It is based on three 3He filled linear position sensitive Reuter-Stokes tubes (610 mm in length, 25 mm diameter). The three detectors are placed parallel to the scattering plane, above each other. Data transfer and instrument control has been done by PC-AT (Master PC) with Eagle I/O card. The instrument software package has been developed by the local instrument staff. Recently the sample environment has been renewed. An in-situ high temperature cell has been designed and built, with temperature range from room temperature to 900°C.

Further readings
  1. http://www.bnc.hu/?q=node/18
  2. M. Fábián: PSD Neutron Diffractometer, Research Instruments of the Budapest Neutron Centre, Handbook of the CETS, Published by Budapest Neutron Centre, ISBN 978-963-12-8757-8, pp.59-71 (2017)
Providers

BNC-WIGNER (HU)

SANS (Small Angle Neutron Scattering - Yellow Submarine)
Overview

The Yellow Submarine instrument is used for non-destructive studies of nano-structural features (from 1 nm to 15 0nm) of a large range of materials. It gives information about the orientation, size, size-distribution, agglomeration, quantity of the nano-domains inside the sample, which can be correlated to several macroscopic characteristics of the material, such as firing temperature of clays and bricks, oriented strain or stress that affected the raw material or the fabrication procedure, deterioration degree of textiles, etc.

Technical details

Yellow Submarine is a pin-hole type SANS instrument covering a Q-range from 0.003 to 0.7Å-1. The instrument is installed on the curved neutron guide No.2, with 4×4 cm2 cross-section, made of (1.5 c) supermirrors. The beam is monochromatized by a multidisc type velocity selector. The width / of the transmitted wavelength distribution can be varied between 12% and 30% by changing the tilt angle between the selector axis and the direction of the neutron beam. The collimation distance is 4.7 m. In most of the experiments an automatic sample changer with 6 positions is used. It can be thermostated from an external bath between 10°C and 90°C. An 11 position sample changer can be used for ambient temperature experiments. Electromagnets can also be mounted on the sample table (field 1.6T in the gap 25 mm), with a vertical automatic sample holder with 9 sample positions. The minimum sample size is of several millimetre in diameter, the maximum is about half a meter, limited by thickness (because of occurrence of multiple scattering for the case of thick samples). The scattered neutrons are detected by a 64 Å~ 64 pixels (1 cm Å~ 1 cm pixel size) two dimensional position sensitive LETI (Grenoble, France) detector filled with BF3 gas. The control and data acquisition electronics has been made by Laboratoire Léon Brillouin, Saclay, France, and ANTE Ltd., Budapest, Hungary, the data acquisition software was designed in BNC.

Further readings
  1. http://www.bnc.hu/?q=node/18
  2. A. Len: Small Angle Neutron Scattering, Research Instruments of the Budapest Neutron Centre, Handbook of the CETS, Published by Budapest Neutron Centre, ISBN 978-963-12-8757-8, pp.84-100 (2017)
Providers

BNC-WIGNER (HU)

NIPS-NORMA (Neutron-Induced Prompt Gamma-ray Spectroscopy & Neutron Optics and Radiography for Material Analysis)
Overview

The NIPS-NORMA instrument, similarly to the PGAA, is suitable for the non-destructive determination of bulk elemental composition of various samples, based on the detection of the characteristic prompt-gamma radiation induced by neutron capture into the atomic nucleus. The most of the major components and a few trace elements (e.g. B, Cl, Co, Cd, Hg, Sm and Gd) in rocks, minerals, ceramics, glass, metals and many inorganic materials can be determined. In addition, NIPSNORMA station allows performing a position-sensitive elemental analysis of well-defined spots on larger objects (sculptures, vessels, etc. with up to the size of ca. 15 cm). Furthermore, it is possible to combine the 2D or 3D neutron imaging with local elemental analysis. At the moment, this technique is exclusively available at the BNC. The NIPS-NORMA and the PGAA instruments share the same cold neutron guided beam.

Technical details

The thermal-equivalent neutron flux at the NIPS sample positions is 2.7Å~107 cm–2 s–1. The beam could be collimated to any rectangular shape with a max. cross-section of 4Å~4 cm2. A sample chamber with dimensions of 20Å~20Å~20 cm3 is available for large-sample analysis and positionsensitive applications. Objects up to 5 kg (such as swords, vases, stones, etc.) can be positioned and analyzed in the beam using a XYZ motorized sample stage with a travel distance of 150 mm. An n-type coaxial HPGe detector (Canberra GR 2318/S) equipped with a Scionix BGO Compton suppressor is used for the routine prompt-gamma measurements. Variable lead gamma collimators with slits of 30 mm diameter, 2Å~20 mm2 or 5Å~5 mm2 are available for PGAI measurements. A digital signal processor combined with an Ethernet-based multichannel analyzer module (Canberra AIM 556B) collects the counts. A user-friendly facility control program is used for manual, semiautomatic, and unattended automatic batch measurements.

Further reading
  1. Kis Z, Szentmiklósi L, Belgya T (2015) NIPS–NORMA station—a combined facility for neutronbased non-destructive element analysis and imaging at the Budapest Neutron Centre. Nucl Instr Meth A 779:116-123.
Providers

BNC-WIGNER (HU)