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IR-35 radioactive laboratory: This laboratory has been designed to complete the activities of IR-30 with the aim of covering the current requirements and future needs of new research trends as unique laboratories in Spain that provide this type of service and scientific support to public institutions, nuclear power plants and industries. It is close to completing its construction, equipment and licensing to allow the complete nuclearization of the different characterization laboratories of the URRAA. 
The relevance of this new facility is centered on activity limits for handling radioactive materials that are higher than those of the IR-30, and the adaptation of the equipment that currently allows working with "exempt" quantities of radionuclides. In this laboratory, most of the surface characterization techniques will be implemented, which are currently carried out with the corresponding restriction, in non-radioactive facilities in this line of research (Microdurometer, Rheometer, XRD, BET, Raman spectroscopy, SEM-EDX, diffraction laser, etc).
Supervisors of the IR30/IR35 Radioactive Facilities:
Optical & SEM-EDX
In the IR-35 (Ed.12. S1. V10) facility of CIEMAT (Madrid, Spain) we have a Scanning Electron Microscopy (SEM) unit with an additional probe for measuring Ray Scattering X (EDX). Using this technique, images of the surfaces of the different samples with which the unit works can be acquired, reaching a micron scale to observe the morphology of the particles that make them up. Using the EDX probe, it is possible to quantify the chemical elements present in the sample, through the measurement of the X-rays scattered when the laser falls on the surface of the material.
The main application of SEM is based on morphological analysis. In this way, it makes it possible to characterize the shape of the uranium particles, for example, an important fact as a step prior to the sintering of fuel pellets. Also with powdery material, it makes it possible to qualitatively identify the degree of oxidation of UO2-type materials, by analyzing the cracks produced in the material by the effect of oxygen, or by the different morphologies of the oxidized phases of UO2, in particular U3O8. Finally, its application in the characterization of nuclear fuel pellets is also possible. Especially interesting is its application in the measurement of the mean grain size of the sintered materials, a crucial parameter in the manufacture of new nuclear fuels, since it will determine the safety margins that they provide against the increase in the degree of burn-up in the reactor.
Technicians:
Raman
There is a wide variety of Raman spectroscopy equipment depending on the needs that you want to cover, but they all have a series of essential components that are common to this type of equipment. This common instrumental part is made up of a laser radiation source, a filter, a monochromator with a diffraction grating, and a detector. At the HLWU- we have several Raman spectroscopy equipment: a HORIBA LabRam HR Evolution confocal Micro-Raman spectrometer from Jobin Yvon Technology and a new portable Raman spectroscopy equipment, an i-Raman from B&W Tek.
The performance of both temporary and definitive repositories of nuclear fuel requires knowledge of the stability of the fuel under different storage conditions. For this, some of the studies focus on the stability of spent nuclear fuel in dry conditions, focusing mainly on the oxidation of the UO2 matrix of the spent fuel. In case of shielding failure, the oxidation of UO2 occurs due to its contact with atmospheric oxygen and the high temperatures present. The in situ monitoring of this reaction under different conditions is one of the most important applications of Raman spectroscopy in solids. Some representative spectra of these phases are shown below.
In order to perform Raman spectroscopy measurements of liquids, closed cuvettes were designed that allow measurements of small volumes of samples (less than 100 μL) under safe conditions. It also allows the refrigeration of the cuvette for exothermic tests or those that require slowing down the kinetics. But clearly the best advantage of this proprietary design is the possibility of encapsulating the sample and therefore they can be measured in conventional laboratories (because they are free and encapsulated samples). In addition, the parts of the capsule are recyclable and easy to disassemble and clean. As example, with this chamber, the entire analysis methodology in aqueous medium of acetohydroxamic acid (AHA) and its hydrolytic degradation compounds has been developed.
Technicians:
X Ray Diffraction (XRD)
In the IR-35 facility (Building 12 S1.D10) of the CIEMAT (Madrid, Spain) we have the D8 Advance Eco diffractometer from the Bruker firm. This equipment allows access to conventional powder diffraction, microdiffraction, grazing incidence (GIXRD) techniques and the study of phase transformations using the controlled atmosphere and temperature chamber platform. The X-ray generator has a power limited to 1 Kw and a closed cooling circuit for the tube.
Powder diffraction allows the identification of phases present in the sample by comparing the values of diffracted angle, intensity and profile of the spacings with those contained in the reference database for pure phases. Each phase has a characteristic pattern or “fingerprint” that allows identification. The Rietveld method allows quantitative analysis from phase models containing crystallographic information.
The controlled temperature and atmosphere chamber allows the study of the stability of crystalline compounds as a function of temperature, as well as crystallographic transitions or the evolution of phases in reactions with reactive atmospheres. The controlled atmosphere and temperature platform enables monitoring of the stability of nuclear fuel under dry conditions. The in situ study of the oxidation reaction of nuclear fuel under different conditions is one of the most interesting applications of diffraction with a temperature and atmosphere chamber.
Technicians:
PSD Measurement of Particle Size and Distribution Medida de Tamaño y Distribución de Partícula
At the IR-35 facility (Ed.12 S1. D35) of the CIEMAT (Madrid, Spain) we have a MALVERN MASTERSIZER 3000 particle size and distribution measurement device, designed for rapid and high-precision measurement of the size distribution of particles of samples in liquid and dry dispersion.
The team uses the technique LD for Laser Diffraction or LS for Laser Scattering, which is based on the theory of low angle laser light scattering. It has two light sources: a red Helium-Neon laser of 633nm in length and blue LED light of 470nm in wavelength, which interact with the particles of the solid in suspension, dispersing at certain angles depending on the size of the particles, allowing a range of measurements from 0.01 to 3500 microns in a single analysis without the need to change the optics of the equipment.
This equipment has different measurement cells, which allow simultaneous measurements in both dry and wet methods by means of large volume HYDRO EV liquid dispersion units for aqueous and solvent bases and automatic dry dispersion unit with stainless steel venturi system. AERO S.
Within the projects in which HLWU is involved (EURAD, DISCO and OCATS), we commit ourselves to the manufacture of samples (pellets with different compositions of metal oxides) that will later be subjected to different tests (dissolution, oxidation, etc. ). In any of the manufacturing lines used (ceramic processing and conforming by Slip Casting), it is necessary to start from the initial characterization of the particle size of the metal oxides, either to determine the compatibility/reaction surface between the various oxides, as once the dissolution, oxidation, etc. tests have been carried out. to verify its evolution and how the variability of this parameter will affect, for example, final storage in humid (AGP) or dry (ATC) conditions, by presenting a greater or lesser surface area exposed to external elements.
Technicians:
BET
At the IR-35 facility (Building 12 S1. D35) of CIEMAT (Madrid, Spain) we have a Micromeritics ASAP 2020 unit for analysis of surface area and pore volume.
The specific surface area is defined as the surface of solid particles divided by its mass, its determination is of the utmost importance due to its direct relationship with fundamental physical properties such as particle size, surface energy, light scattering, the sintering properties, moisture retention and the porosity of the material to be studied, properties that influence the processing of powders. There are few techniques that allow obtaining a quantitative and systematic value of the area due to the roughness of the solid particles, it is also a determining property in the control of the kinetics of chemical interaction between solids and gases or liquids, due to the fact that the external surface It is the part that interacts with the matter that surrounds it.
Due to the activities in which the CIEMAT HLWU is involved (nuclear fuel stability evaluation studies), the main objective of the specific surface studies are related to porosity and particularly are aimed at determining its involvement in the dissolution rates of the fuel during its Centralized Temporary Storage (ATC) or its final location in a Deep Geological Storage (AGP).
However, it is not only a property whose study is applicable to water-fuel systems, but it would also give an idea of the physical-chemical changes that occur in the fuel pellet, as a consequence of its irradiation, or during processes of oxidation in which the porosity and/or the particle size change.
Technicians:
Nuclear Fuel Analog Manufacturing Line
In the manufacturing line of nuclear fuel analogues that will be used in R&D tests related to the management of high activity waste and on the behavior of spent fuel under temporary storage conditions and AGP carried out by the Waste Unit High Activity different equipment is used:
Dispositivo de prensado de la marca POWER TEAM: el dispositivo de prensado está ubicado sobre poyata y dentro de una caja de guantes estanca sellada con
POWER TEAM brand pressing device: the pressing device is located on a bench and inside a watertight glove box sealed with specific silicone for this type of system and with chlorosulfonated polyethylene gloves. Inside it is located the press driven by a hydraulic pump with a maximum capacity of 25 T of pressure, both of the POWER TEAM brand, and a PARKER brand portable meter.
Termolab TH1700 oven: for firing and sintering the samples. It reaches a maximum temperature of 1700ºC and allows the control of the working atmosphere by means of a rotameter. It has a programmer that allows the programming of the oven creating a heating ramp, target temperature and residence time.
Homogenizing mill: Retsch MM 400 is designed as a laboratory device suitable for grinding and homogenizing soft, fibrous, hard and brittle materials in a dry and wet state of 2 samples at the same time. It has screw-on grinding vessels, to guarantee the complete recovery of the samples, with a capacity of 35 ml coated with zirconium oxide. The frequency can be selected between 3 and 30 Hz.
Retsch ReMetaServ™ 250 polisher: with semi-automatic head that allows polishing of four samples at the same time. Rotation head with speed of 50-500rpm and assortment of sandpapers and polishing cloths up to a 3 µm diamond dust suspension.
Technicians: