PEARL Diffractometer

PEARL is a medium-resolution, general-purpose neutron diffractometer installed at the 2.3 MW research reactor of Delft University of Technology. PEARL is ideal for conducting diffraction experiments on powdered samples, with varying sample environment capabilities (temperature ranging from 1.7 K to 1500 K). This makes the instrument highly capable and scientifically diverse for studying temperature-dependent structural and/or magnetic transitions. The wide range of applications includes, but is not limited to, energy materials, magnetic materials, high-entropy alloys, magneto-caloric materials etc.

Neutron diffraction is a powerful technique useful to investigate the atomic and/or magnetic structure of materials. This technique leverages the unique properties of neutrons, offering insights that complement those obtained from other diffraction methods such as X-ray diffraction.
In a typical neutron diffraction experiment, a monochromatized beam of neutrons is directed at a sample, and the scattered neutrons are detected and analysed. As the neutrons interact with the atoms in the sample, they are scattered in specific directions, creating a diffraction pattern that can be recorded and studied. This experimentally obtained pattern contains information about the atomic positions within the material, as well as the type and arrangement of the atoms. By analyzing the diffraction pattern, researchers can determine the crystal structure, atomic positions, and even the magnetic properties of the sample.

Key Features / Advantages of Neutrons

Deep Penetration: This property of neutrons allows the study of bulk and internal structure of the material, with complex sample environments.
Sensitivity to Light Elements: Unlike X-rays, neutrons are highly sensitive to light elements such as H, Li, O etc.
Isotope Differentiation: Neutrons can distinguish between different isotopes of the same element (such H and D), providing critical information for various scientific applications.
Magnetic Structure Analysis: Neutrons possess a magnetic moment, enabling them to interact with magnetic moments in materials. This unique feature allows for detailed investigation of magnetic ordering and transitions.

Applications

Scientific studies using PEARL diffractometer cover a broad spectrum of innovative materials and science. These encompass, but are not limited to

Energy storage materials like, battery materials, solid oxide fuel cells, etc.
Hydrogen storage materials
High-entropy alloys
Magnetic materials such as, multiferroics, magnetocaloric materials, charge and orbital ordering transitions etc.
Understanding of materials like, Zeolites, Metal organic frameworks (MOFs).

Few examples

1. Magnetic structure of YNi_4-xCo_xSi alloys

Powder neutron diffraction is a used to resolve the magnetic structure, determine the magnitude and direction of magnetic moments, combined with the precise structure determination of the Ni location in the CaCu₅-type structure.

W. Hanggai, N.H. van Dijk , E. Brück, J. Alloys and Compounds 986 (2024) 174116, https://doi.org/10.1016/j.jallcom.2024.174116

2. Lithium substructure in the Li_6–xPS_5–xBr_1+x series

Neutron diffraction measurements are used to reveal the lithium substructure and the Br site disorder. The lattice parameter, occupancies (Br and S, Wyckoff 4d and 4a), sites (S, Wyckoff 16e), and thermal parameters (S, P, and Br) are obtained by Rietveld refinement of the data.

Ajay Gautam, Hanan Al-Kutubi, Theodosios Famprikis, Swapna Ganapathy, Marnix Wagemaker, Chem. Mater. 2023, 35, 19, 8081–8091
https://doi.org/10.1021/acs.chemmater.3c01525

3. Understanding the Activation of ZSM-5 by Phosphorus

Combined synchrotron XRD and neutron diffraction studies are carried out to study the short range correlations. Structural refinements are performed to demonstrate the localization of phosphate groups inside the pores of P-activated ZSM-5, showing that P atoms migrate into the pores and react with Al atoms in the vicinity of their original positions.

Jaap N. Louwen, Lambert van Eijck, Charlotte Vogt, Eelco T.C. Vogt, Chem. Mater. 2020, 32, 21, 9390–9403
https://doi.org/10.1021/acs.chemmater.0c03411

The PEARL schematic [1]

The PEARL instrument is installed on a reactor beamport (Dia. = 160 mm), with a direct view to the core. As a consequence, shielding of fast and epithermal neutrons has been an important aspect in the design of this instrument. Firstly, by positioning the 10 cm thick sapphire (Al₂O₃) single crystal upstream in the beam port helps reducing the fast neutron background by an order of magnitude. Secondly, the background radiation is further reduced by a compact shielding consisting of paraffin layers, steel, boron rubber, polyethylene and heavy concrete.

A vertically focussed Ge monochromator has a fixed take-off angle of 2q_M = 150° in backscattering geometry. The monochromator comprises 22 crystals, each of which is built up out of stacks of 25 hot-pressed wafers with a rocking curve width of approx. 29’ FWHM. By rotating the monochromator around its vertical axis it is possible to select different wavelengths, l = 1.67 Å, 1.098 Å and 2.51 Å.

PEARL has no collimators, the overall beam collimation is defined by the beam-port dimensions, monochromator size (h = 300 mm, w = 50 mm), sample size (typically Ø = 6, 8 or 9 mm and h = 50 mm) and detector pixel size (h = 200 mm, w = 2.1 mm).

The powder diffraction patterns are collected by a novel 6 LiF– ZnS:Ag scintillator detector, covering the angular range of 10.9° ≤ 2q ≤ 158°. It is based on a concept developed at the ISIS neutron scattering facility. The detection efficiency is 68 % for 1.8 Å neutrons. The scintillation light from neutron absorption is transported to photomultipliers with wavelength-shifting fibers and analyzed by field-programmable gate array (FPGA) electronics that simultaneously decode the fiber encoding. Using fast electronics, it is possible to distinguish neutron- from gamma generated scintillation light and thus discriminate neutrons from gamma rays with a ratio better than 1 p.p.m.

[1] van Eijck, L.; Cussen, L. D.; Sykora, G. J.; Schooneveld, E. M.; Rhodes, N. J.; van Well, A. A.; Pappas, C. Design and Performance of a Novel Neutron Powder Diffractometer: PEARL at TU Delft. J. Appl. Crystallogr. 2016, 49, 1398– 1401, DOI: 10.1107/S160057671601089X

Specs of the instrument in text, table and schematic pictures

Powder Form: Samples should be in a fine and uniformly powdered form, to avoid issues with preferred orientation, to ensure good packing, and avoid density variations, which can influence the diffraction data.
Samples should be of high purity and homogeneity: To minimize the additional diffraction peaks contributed by the presence of impurities and to ensure consistent diffraction patterns.
Sample Quantity: Typically 2 to 5 gms, highly dependent on the density, material’s neutron scattering cross-section
Optimal particle size: 1 – 10 microns

Safety Considerations

Radioactivity: If the sample is radioactive, follow all relevant safety protocols for handling and containment.
Toxicity: For toxic samples, ensure appropriate safety measures, such as using fume hoods or protective equipment.

By adhering to these requirements, researchers can ensure they obtain high-quality neutron powder diffraction data, enabling accurate determination of the sample’s atomic and magnetic structures.

Sample Changer: 6 - 8 samples can be loaded for RT measurements
ILL Orange: Top loading liquid helium cryostat, temperature ranging from 1.7 K – 300 K
Furnace: Temperature ranging from RT – 800 K
Oven: Temperature ranging from RT – 1500 K

Sample cans made up of different materials, 8- and 6-mm dia. V cans, Null alloy can, Al can, TiZr cans (from left to right).

ILL orange cryostat, temperature range of 1.7 K – 300 K

Cu based furnace, temperature range of RT – 800 K

High temperature induction-based oven, temperature range from RT – 1500 K

Please check out the info at the page User Office for Proposal Application, Contact Information and FAQ/QA.

2024

van Hattem, A., Dankelman, R., Colineau, E., Griveau, J.-C., Dardenne, K., Rothe, J., Couweleers, S., Konings, R.J.M., Smith, A.L.
Experimental investigations and thermodynamic modelling of the ternary system Pb-Mo-O
(2024) Journal of Alloys and Compounds, 1003, art. no. 175588, .

Lin, J., Schaller, M., Indris, S., Baran, V., Gautam, A., Janek, J., Kondrakov, A., Brezesinski, T., Strauss, F.
Tuning Ion Mobility in Lithium Argyrodite Solid Electrolytes via Entropy Engineering
(2024) Angewandte Chemie - International Edition, 63 (30), art. no. e202404874, .

Yartys, V.A., Akselrud, L.G., Denys, R.V., Vajeeston, P., Ouladdiaf, B., Dankelman, R., Plomp, J., Koldemir, A., Schumacher, L., Kremer, R.K., Pöttgen, R., Wragg, D.S., Eggert, B.G.F., Berezovets, V.
Crystal, Magnetic Structures, and Bonding Interactions in the TiNiSi-Type Hydride CeMgSnH: Experimental and Computational Studies
(2024) Chemistry of Materials, 36 (12), pp. 6257-6268.

Hanggai, W., van Dijk, N.H., Brück, E.
Structural and magnetic properties of YNi4-xCoxSi alloys
(2024) Journal of Alloys and Compounds, 986, art. no. 174116, .

Ojiyed, H., van den Berg, M., Batashev, I., Shen, Q., van Dijk, N., Brück, E.
Magnetocaloric properties of Mn5(Si,P)B2 compounds for energy harvesting applications
(2024) Journal of Alloys and Compounds, 978, art. no. 173485, .

Yartys, V.A., Denys, R.V., Akselrud, L.G., Vajeeston, P., Dankelman, R., Plomp, J., Block, T., Pöttgen, R., Wragg, D., Eggert, B.G.F., Berezovets, V.
Structure and bonding in TiNiSi type LaMgSnH intermetallic hydride
(2024) Journal of Alloys and Compounds, 976, art. no. 173198, .

Alders, D.C., Vlieland, J., Thijs, M., Konings, R.J.M., Smith, A.L.
Experimental investigation and thermodynamic assessment of the BaCl2–CeCl3 system
(2024) Journal of Molecular Liquids, 396, art. no. 123997, .

Mercadier, B., Legein, C., Body, M., Famprikis, T., Morcrette, M., Suard, E., Masquelier, C., Dambournet, D.
Insights into the Micro-Structure-Transport Relationships of the Fluoride-Ion Conductor t-BaSnF4 Synthesized by Spark Plasma Sintering
(2024) Chemistry of Materials, .

Dronskowski, R., Brückel, T., Kohlmann, H., Avdeev, M., Houben, A., Meven, M., Hofmann, M., Kamiyama, T., Zobel, M., Schweika, W., Hermann, R.P., Sano-Furukawa, A.
Neutron diffraction: A primer
(2024) Zeitschrift fur Kristallographie - Crystalline Materials, .

2023

Gautam, A., Al-Kutubi, H., Famprikis, T., Ganapathy, S., Wagemaker, M.
Exploring the Relationship Between Halide Substitution, Structural Disorder, and Lithium Distribution in Lithium Argyrodites (Li6-xPS5-xBr1+x)
(2023) Chemistry of Materials, 35 (19), pp. 8081-8091.

Shen, Q., Batashev, I., Zhang, F., Ojiyed, H., Dugulan, I., van Dijk, N., Brück, E.
Exploring the negative thermal expansion and magnetocaloric effect in Fe2(Hf,Ti) Laves phase materials
(2023) Acta Materialia, 257, art. no. 119149, .

Wissel, K., Riegger, L.M., Schneider, C., Waidha, A.I., Famprikis, T., Ikeda, Y., Grabowski, B., Dinnebier, R.E., Lotsch, B.V., Janek, J., Ensinger, W., Clemens, O.
Dissolution and Recrystallization Behavior of Li3PS4 in Different Organic Solvents with a Focus on N-Methylformamide
(2023) ACS Applied Energy Materials, 6 (15), pp. 7790-7802.

Shen, Q., Zhang, F., Dugulan, I., van Dijk, N., Brück, E.
Magnetoelastic transition and negative thermal expansion of Fe2Hf0.83Ta0.17 ribbons
(2023) Scripta Materialia, 232, art. no. 115482, .

Kiecana, A., Schaefers, W., Thijs, M., Dankelman, R., Ojiyed, H., Batashev, I., Zhang, F., van Dijk, N.H., Brück, E.
Competing magnetic interactions, structure and magnetocaloric effect in Mn3Sn1-xZnxC antiperovskite carbides
(2023) Journal of Magnetism and Magnetic Materials, 577, art. no. 170782, .

van Hattem, A., Vlieland, J., Dankelman, R., Thijs, M.A., Wallez, G., Dardenne, K., Rothe, J., Konings, R.J., Smith, A.L.
Structural Studies and Thermal Analysis in the Cs2MoO4-PbMoO4 System with Elucidation of β-Cs2Pb(MoO4)2
(2023) Inorganic Chemistry, 62 (18), pp. 6981-6992.

Zhang, F., Batashev, I., van Dijk, N., Brück, E.
Effect of off-stoichiometry and Ta doping on Fe-rich (Mn,Fe)2(P,Si) based giant magnetocaloric materials
(2023) Scripta Materialia, 226, art. no. 115253, .

van der Maas, E., Famprikis, T., Pieters, S., Dijkstra, J.P., Li, Z., Parnell, S.R., Smith, R.I., van Eck, E.R.H., Ganapathy, S., Wagemaker, M.
Re-investigating the structure-property relationship of the solid electrolytes Li 3−xIn1−xZrxCl6 and the impact of In-Zr(iv) substitution
(2023) Journal of Materials Chemistry A, 11 (9), pp. 4559-4571.

van der Maas, E., Zhao, W., Cheng, Z., Famprikis, T., Thijs, M., Parnell, S.R., Ganapathy, S., Wagemaker, M.
Investigation of Structure, Ionic Conductivity, and Electrochemical Stability of Halogen Substitution in Solid-State Ion Conductor Li3YBrxCl6-x
(2023) Journal of Physical Chemistry C, 127 (1), pp. 125-132.

2022

van der Stok-Nienhuis, J., Beentjes, T., Ngan-Tillard, D., van Eijck, L., Joosten, I., van Bommel, M.R.
Unravelling the construction of silver filigree spheres from a seventeenth century shipwreck using non-invasive imaging
(2022) Heritage Science, 10 (1), art. no. 98, .

Zhang, F., Taake, C., Huang, B., You, X., Ojiyed, H., Shen, Q., Dugulan, I., Caron, L., van Dijk, N., Brück, E.
Magnetocaloric effect in the (Mn,Fe)2(P,Si) system: From bulk to nano
(2022) Acta Materialia, 224, art. no. 117532, .

2021

Ioannidou, C., Navarro-López, A., Dalgliesh, R.M., Rijkenberg, A., Zhang, X., Kooi, B., Geerlofs, N., Pappas, C., Sietsma, J., van Well, A.A., Offerman, S.E.
Phase-transformation and precipitation kinetics in vanadium micro-alloyed steels by in-situ, simultaneous neutron diffraction and SANS
(2021) Acta Materialia, 220, art. no. 117317, .

Weninger, B.M.H., Thijs, M.A., Nijman, J.A.C., Van Eijck, L., Mulder, F.M.
Neutron Diffraction Study of a Sintered Iron Electrode in Operando
(2021) Journal of Physical Chemistry C, 125 (30), pp. 16391-16402.

Shen, Q., Batashev, I., Zhang, F., Ojiyed, H., van Dijk, N., Brück, E.
The antiferromagnetic to ferrimagnetic phase transition in Mn2Sb1-xBix compounds
(2021) Journal of Alloys and Compounds, 866, art. no. 158963, .

2020

Dixit, V., van Eijck, L., Huot, J.
Investigation of dehydrogenation of Ti–V–Cr alloy by using in-situ neutron diffraction
(2020) Journal of Alloys and Compounds, 844, art. no. 156130, .

Louwen, J.N., van Eijck, L., Vogt, C., Vogt, E.T.
Understanding the Activation of ZSM-5 by Phosphorus: Localizing Phosphate Groups in the Pores of Phosphate-Stabilized ZSM-5
(2020) Chemistry of Materials, 32 (21), pp. 9390-9403.

Yu, C., Li, Y., Adair, K.R., Li, W., Goubitz, K., Zhao, Y., Willans, M.J., Thijs, M.A., Wang, C., Zhao, F., Sun, Q., Deng, S., Liang, J., Li, X., Li, R., Sham, T.-K., Huang, H., Lu, S., Zhao, S., Zhang, L., van Eijck, L., Huang, Y., Sun, X.
Tuning ionic conductivity and electrode compatibility of Li3YBr6 for high-performance all solid-state Li batteries
(2020) Nano Energy, 77, art. no. 105097, .

Smith, A.L., De Zoete, N., Rutten, M., Van Eijck, L., Griveau, J.-C., Colineau, E.
Report of the Double-Molybdate Phase Cs2Ba(MoO4)2with a Palmierite Structure and Its Thermodynamic Characterization
(2020) Inorganic Chemistry, 59 (18), pp. 13162-13173.

Epifano, E., Volfi, A., Abbink, M., Nieuwland, H., Van Eijck, L., Wallez, G., Banerjee, D., Martin, P.M., Smith, A.L.
Investigation of the Cs2(Mo,Te)O4Solid Solution and Implications on the Joint Oxyde-Gaine System in Fast Neutron Reactors
(2020) Inorganic Chemistry, 59 (14), pp. 10172-10184.

Kauric, G., Epifano, E., Martin, P.M., Van Eijck, L., Bouëxière, D., Clavier, N., Guéneau, C., Smith, A.L.
Structural and Thermodynamic Investigation of the Perovskite Ba2NaMoO5.5
(2020) Inorganic Chemistry, 59 (9), pp. 6120-6130.

Lai, J., You, X., Dugulan, I., Huang, B., Liu, J., Maschek, M., van Eijck, L., van Dijk, N., Brück, E.
Tuning the magneto-elastic transition of (Mn,Fe,V)2(P,Si) alloys to low magnetic field applications
(2020) Journal of Alloys and Compounds, 821, art. no. 153451, .

2019

Lai, J., Huang, B., Miao, X., Van Thang, N., You, X., Maschek, M., van Eijck, L., Zeng, D., van Dijk, N., Brück, E.
Combined effect of annealing temperature and vanadium substitution for mangetocaloric Mn1.2-xVxFe0.75P0.5Si0.5 alloys
(2019) Journal of Alloys and Compounds, 803, pp. 671-677.

Wang, H., Yu, C., Ganapathy, S., van Eck, E.R.H., van Eijck, L., Wagemaker, M.
A lithium argyrodite Li6PS5Cl0.5Br0.5 electrolyte with improved bulk and interfacial conductivity
(2019) Journal of Power Sources, 412, pp. 29-36.

Smith, A.L., Verleg, M.N., Vlieland, J., de Haas, D., Ocadiz-Flores, J.A., Martin, P., Rothe, J., Dardenne, K., Salanne, M., Gheribi, A.E., Capelli, E., van Eijck, L., Konings, R.J.M.
In situ high-temperature EXAFS measurements on radioactive and air-sensitive molten salt materials
(2019) Journal of Synchrotron Radiation, 26 (1), pp. 124-136.

Smith, A.L., Kauric, G., van Eijck, L., Goubitz, K., Clavier, N., Wallez, G., Konings, R.J.M.
Structural and thermodynamic study of Cs3Na(MoO4)2: Margin to the safe operation of sodium cooled fast reactors
(2019) Journal of Solid State Chemistry, 269, pp. 1-8.

2018

Almomani, S., Seong, B.-S.
Conceptual design of a new high-resolution powder diffractometer at Jordan Research and Training Reactor
(2018) Physica B: Condensed Matter, 551, pp. 390-394.

Yu, C., Ganapathy, S., Hageman, J., Van Eijck, L., Van Eck, E.R.H., Zhang, L., Schwietert, T., Basak, S., Kelder, E.M., Wagemaker, M.
Facile Synthesis toward the Optimal Structure-Conductivity Characteristics of the Argyrodite Li6PS5Cl Solid-State Electrolyte
(2018) ACS Applied Materials and Interfaces, 10 (39), pp. 33296-33306.

Juhás, P., Louwen, J.N., van Eijck, L., Vogt, E.T.C., Billinge, S.J.L.
PDFgetN3: Atomic pair distribution functions from neutron powder diffraction data using ad hoc corrections
(2018) Journal of Applied Crystallography, 51 (5), pp. 1492-1497.

Zhou, Z., Plomp, J., van Eijck, L., Vontobel, P., Harti, R.P., Lehmann, E., Pappas, C.
FISH: A thermal neutron imaging station at HOR Delft
(2018) Journal of Archaeological Science: Reports, 20, pp. 369-373.

Cugini, F., Righi, L., van Eijck, L., Brück, E., Solzi, M.
Cold working consequence on the magnetocaloric effect of Ni50Mn34In16 Heusler alloy
(2018) Journal of Alloys and Compounds, 749, pp. 211-216.

Smith, A.L., Pignié, M.-C., van Eijck, L., Griveau, J.-C., Colineau, E., Konings, R.J.M.
Thermodynamic study of Cs3Na(MoO4)2: Determination of the standard enthalpy of formation and standard entropy at 298.15 K
(2018) Journal of Chemical Thermodynamics, 120, pp. 205-216.

Zhang, J., Xia, Y., Wang, Y., Xie, C., Sun, G., Liu, L., Pang, B., Li, J., Huang, C., Liu, Y., Gong, J.
High resolution neutron diffractometer HRND at research reactor CMRR
(2018) Journal of Instrumentation, 13 (1), art. no. T01009, .

2017

Kumar, A., Vermeulen, P.A., Kooi, B.J., Rao, J., Van Eijck, L., Schwarzmüller, S., Oeckler, O., Blake, G.R.
Phase Transitions of Thermoelectric TAGS-85
(2017) Inorganic Chemistry, 56 (24), pp. 15091-15100.

Smith, A.L., Kauric, G., van Eijck, L., Goubitz, K., Wallez, G., Griveau, J.-C., Colineau, E., Clavier, N., Konings, R.J.M.
Structural and thermodynamic study of dicesium molybdate Cs2Mo2O7: Implications for fast neutron reactors
(2017) Journal of Solid State Chemistry, 253, pp. 89-102.

Thang, N.V., Yibole, H., Miao, X.F., Goubitz, K., van Eijck, L., van Dijk, N.H., Brück, E.
Effect of Carbon Doping on the Structure and Magnetic Phase Transition in (Mn,Fe2(P,Si))
(2017) JOM, 69 (8), pp. 1432-1438.

Boeije, M.F.J., van Eijck, L., van Dijk, N.H., Brück, E.
Structural and magnetic properties of hexagonal (Mn,Fe)3-δGa
(2017) Journal of Magnetism and Magnetic Materials, 433, pp. 297-302.

Yu, C., Ganapathy, S., Van Eck, E.R.H., Van Eijck, L., Basak, S., Liu, Y., Zhang, L., Zandbergen, H.W., Wagemaker, M.
Revealing the relation between the structure, Li-ion conductivity and solid-state battery performance of the argyrodite Li6PS5Br solid electrolyte
(2017) Journal of Materials Chemistry A, 5 (40), pp. 21178-21188.

2016

Yu, C., van Eijck, L., Ganapathy, S., Wagemaker, M.
Synthesis, structure and electrochemical performance of the argyrodite Li6PS5Cl solid electrolyte for Li-ion solid state batteries
(2016) Electrochimica Acta, 215, pp. 93-99.

Van Eijck, L., Cussen, L.D., Sykora, G.J., Schooneveld, E.M., Rhodes, N.J., Van Well, A.A., Pappas, C.
Design and performance of a novel neutron powder diffractometer: PEARL at TU Delft
(2016) Journal of Applied Crystallography, 49 (5), pp. 1398-1401.