WAND² | HB-2C | HFIR

Capabilities of the WAND² Instrument

Powder diffraction

Powder diffraction on WAND² can be simulated https://addie.ornl.gov/hfirestimate to inform the user on sample mass and counting time.

Fast acquisition of medium resolution powder diffraction in the Q range 0.2 to 8.2 Å^-1. The left picture shows the silicon standard powder pattern for calibration. The pattern is combined from measurements on 2 detector positions each collected for 20mins.

 On the right side is the same pattern for one position with a collection time of1s. The high flux and highly efficient detector allow WAND² to take refine able data very fast. This allows measurements with changing parameters, for instance for in-situ synthesis of materials.

Single crystal diffraction – superstructures

WAND² can be used to map the reciprocal space searching for superstructure reflections. In this example the magnetic structure of BaSrCo₂Fe₁₁AlO₂₂is revisited. The scattering geometry isHHLplane (left side). The out-of plane coverage of WAND² (±7.5°or +15°) is used to investigate the magnetic Bragg peaks with the propagation vector along c(right side). Measurement time: 30s/sample angle, 180° rotation 0.1° step, m ~ 500mg. (for the original publication see T. Nakajima, Y. Tokunaga, M. Matsuda, S. Dissanayake, J. Fernandez-Baca, K. Kakurai, Y. Taguchi, Y. Tokura, and T. Arima, Phys. Rev. B 94, (2016) 195154).

Single crystal diffraction – diffuse scattering

Reciprocal mapping gives the possibility to investigate short-range correlations for example the reciprocal map of the HK0 plane of Ho₂PdSi₃. The map is the difference plot 10 K – 50 K which leaves only the strong diffuse critical magnetic scattering around the crystallographic Bragg peak positions (T_N= 7K). (20s/sample angle, 180° rotation 0.1° step, m=2.9g; data from the “old” WAND)

Single crystal diffraction – small samples

The low background on WAND² enables also the study of small single crystals. In this example (m = 3.6 mg) we found the magnetic Bragg peaks on the {100} positions. (60s/sample angle, 180° rotation 0.2° step; data from the “old” WAND)

High Pressure Neutron Diffraction

We try to widen the availability of high pressure cells on WAND². Here, we followed the magnetic structure in the multiferroic CuCrO₂using a Ni-Cr-Al pressure cell (photo on the right side, data taken on the “old” WAND). The magnetic Bragg peaks at low pressure are close to (1/3 1/3 L) for integer values of L(left side of the plot). At 2 GPa the peak position remains on (1/3 1/3 L), but Lhas now non-integer value and the reflections broaden considerably along the Ldirection (right side of the plot).

Information for WAND² Users

Shipping Addresses for Samples

Please visit the ORNL User Facilities Sample Handling and Shipping page.

WAND² instrument control

WAND² is controlled through Control System Studio (CSS). Please refer to the manual WAND² control.

For remote user experiments, please visit the User Guide to Remote Experiments webpage.

Access to HB-2C Data

Data is accessed and reduced remotely on the SNS analysis cluster using Mantidworkbench. A good tool to obtain an overview of your measured files is through ONCat.

The data reduction process has changed in 2021. Please refer to the following manuals for data reduction:

• MantidWorkbench – explains how to login to the SNS analysis cluster, start and descibes MantidWorkbenchNightly
• Powder Reduction – manual to reduce powder diffraction data from WAND²
• Event Filtering – describes the script to use Eventfiltering (Time, Temperature …) on a WAND² dataset
• Workflow Single Crystal Reduction – overview on the WAND² single crystal data reduction steps
• Single Crystal Data Reduction – manual for data slicing and peak integration using Mantid-based scripts

Data from the old WAND can be found and downloaded through ONCat too and may be accessed and reduced using the HFIR Graffiti software. 

Additional Software Downloads:

• WinSCP is a free SFTP client. Once you reduced the data on the SNS analysis cluster you can use a SFTP client to transfer the reduced data to your local computer.
• FullProf and GSAS are Rietveld refinement packages for determination of nuclear and magnetic structures.
• SaraH (download file) – contains the user friendly magnetic structure analysis programs SARAh-Representational Analysis and SARAh-Refine. SARAh uses representational analysis to calculate ‘symmetry allowed magnetic structures’ . The front-end SARAh-Refine facilitates analysis of magnetic diffraction data in terms of these results with GSAS and FullProf. When used with GSAS, SARAh allows reverse Monte Carlo/ Simulated Annealing refinement of the moment orientations. When used with FullProf, automatic creation and editing of the magnetic phase can be controlled by the user.
  
  A web version of SaraH can be found here.
   
• Graffiti – For data reduction from the old WAND. This program allows the user to browse through the scans in the experiment. It also allows combining data sets, angle calculations, spurion checks, etc. Data download through Graffiti doesn’t work anymore. Use ONCat.
• DAVE – Singe Crystal data from the old WAND is displayed using MSLICE in the DAVE Software package; make sure to enter the correct WAND Offset angle (2θ) and wavelength (1.488Å).  Spice/Graffiti is used to create a .wand file which can be read with MSLICE.
   

Calibration Standards

Silicon Standard sample files from cycle 514 (WAND²)

• Data (dat)
• Fullprof input file (pcr)
• Fullprof Instrumental resolution file (irf)
• Data (xye)
• GSAS-II input file (gpx)
• GSAS-II instrument parameter file (instprm)
• TOPAS input file (inp)
• TOPAS instrument parameter file (pro)

Silicon Standard sample files from cycle 482 (WAND²)

• Fullprof input file (pcr)
• Data (dat)
• Instrumental resolution file (irf)
• GSAS-II input file (gpx)

Silicon Standard sample files from cycle 468 (old WAND)

• Fullprof input file (pcr)
• Data (dat)
• Instrumental resolution file (irf)
• Vanadium file for MSLICE (cycle 467)

Links Related to Neutron Scattering and Crystallography

• Neutron scattering lengths and cross sections (http://www.ncnr.nist.gov/resources/n-lengths/index.html)
• Calculate absorption, basic activation calculation (http://www.ncnr.nist.gov/resources/activation/)
• Inorganic Crystallographic Structure Database (ICSD) (https://icsd.fiz-karlsruhe.de/search/basic.xhtml)

ORNL Links

• IPTS
• EXPRESS

Lecture Notes and Example Data

Please refer to the Lecture Notes page from the Magnetic Structure Determination from Neutron Diffraction Data Workshop 2016 for example data and relevant articles.

Single crystal neutron diffraction data from WAND² on NdCuGa₃ collected at 300mK. The data has been published in JMMM, 589 (2024) 171515 (https://doi.org/10.1016/j.jmmm.2023.171515).

User Publications

Intent to Publish

As a condition for performing nonproprietary research, the US Department of Energy requires users to publish results from their research. Authorship of publications based on research from these facilities should reflect the normal considerations of recognizing collaborations. It is also important to take into account the considerable efforts of the instrument scientists in their role of designing, constructing, and/or operating the instrument and related facilities. Results are typically published in peer-reviewed journals, proceedings, or presentations at technical conferences. Proprietary users are not required to publish.

Credit Line

The HB-2C Wide-Angle Neutron Diffractometer should be acknowledged with this required statement:

This research [or, A portion of this research] used resources at the High Flux Isotope Reactor [and/or Spallation Neutron Source, as appropriate], a DOE Office of Science User Facility operated by the Oak Ridge National Laboratory. [If applicable: The beam time was allocated to [Instrument] on proposal number IPTS-XXXXX.X.]. 

Reference to the instrument can be found here: Frontzek M., Whitfield R.E., Andrews K.M., Jones A.B., Brobek M., Vodopivec K., Chakoumakos B.C., Fernandez-Baca J.A., “WAND²—A versatile wide angle neutron powder/single crystal diffractometer“, Review of Scientific Instruments, 89, 9, 092801 (2018)

Publication Record

Please submit publications, thesis, patents, etc., to PuSH (Publications of SNS and HFIR) to assist us in recording your contribution. Both the credit statement and links to PuSH are on the Neutron Sciences Publications website.

WAND² Mail in program

HB-2C WAND² is now accepting mail-in proposals to measure powder samples. This program aims to utilize WAND²’s fast data acquisition capabilities (potentially less than 5 minutes per diffractogram and/or event mode data collection). If your project falls outside the specific scope of the mail-in program or requires additional support from instrument scientists, please submit a General User Program proposal.  Powder diffraction on WAND² can be simulated https://addie.ornl.gov/hfirestimate to inform the user on sample mass and counting time.

Mail-In Program Overview

The WAND² Mail-In Program allows researchers to submit proposals year-round, independent of the semi-annual general user proposal calls. Results of the mail-in WAND² measurements should facilitate to imminent submission of a publication. The following outlines the key details and guidelines:

1. Measurement Specifications: Data collection uses a 1.486 Å constant wavelength with a default two-theta range of 5°–125°. If a different range is required, please specify it in your proposal.
2. Samples: Samples must be prepared before submitting your proposal. Once your proposal is approved, vanadium sample cans will be shipped to your home institution to load and return to HFIR within two weeks. Sample Loading Sheet must be filled in the IPTS system before shipping mail-in or remote samples to HFIR. Samples will be disposed after measurement unless return is specifically requested. Please inform the instrument team if you wish to have your samples returned.
3. Beam Time and Temperature Range:
   1. A maximum of 6 hours effective measurement time can be requested in a six month period. 
   2. The allowed temperature range is 2K–100K and/or at room temperature (RT), supporting samples with discrete temperature steps OR samples for time-dependent (temperature ramp) event mode data collection.
   3. For discrete temperatures measurements, one proposal can ask for up to 6 measurements (6 samples, or 6 temperatures between 2-100 K, or any combination, up to 6 total). For time-dependent (temperature ramp) event mode measurements, only one sample is allowed at temperature range 2-100K. 
   4.  Room-temperature measurements can be requested but will usually be performed without a cryostat at a different time.
4. Proposals are reviewed for feasibility and conflict of interest with GU proposals. While we strive to accommodate as many proposals as possible, some mail-in proposal may not be accepted, though detailed feedback may not always be provided.
5. Experiments are conducted on a first-come, first-served basis. You will be notified when data collection is complete. If the number of samples exceeds the number of available slots on a given day, priority is given to new users.
6. An experimental status report or a publication reference is required before a 2^nd mail-in proposal will be approved from the same research group.  
7. Contact the instrument scientists if you have any questions.

Mail-In Proposal Process

1. Make sure your samples are ready.
2. Use the provided proposal template to prepare your proposal. Contact the instrument scientists if you have any questions or need clarification.
3. Submit your proposal through IPTS, ensuring you select Mail-In as the proposal type.
4. If your proposal is accepted, you will receive an email with additional information, Empty sample cans will be shipped to the address provided in your proposal.
5. Follow the provided sample loading instructions to load your samples into the vanadium cans and complete the sample loading spreadsheet in IPTS. Incomplete sample information will automatically reject the sample for beam time.
6. Samples should be returned to HFIR within two weeks of receiving the empty cans. Ship the loaded samples back to the address listed on the Shipping Guidance page.
7. Your samples will be measured at the earliest available opportunity on a first-come, first-served basis.
8. After data collection, you will receive an email with instructions. Visit the WAND² User Guidance page for details on how to download and analyze your data.
9. All publications resulting from WAND² data must include the required HFIR instrument acknowledgment and be submitted to the PuSH publication tracking system.
10. Samples will be disposed by default after the experiments. Please contact instrument team if you want your samples returned. 

Helpful Documents

WAND² Mail in Proposal Template

Sample Loading Instructions 

Instrument parameters for Rietveld refinement, determined using Silicon standard data collected during Cycle 514 on WAND²:

• Data (dat)
• Fullprof input file (pcr)
• Fullprof Instrumental resolution file (irf)
• Data (xye)
• GSAS-II input file (gpx)
• GSAS-II instrument parameter file (instprm)
• TOPAS input file (inp)
• TOPAS instrument parameter file (pro)

WAND² Sample Environment

A list of equipment available at HB-2C can be found in the Sample Environment Equipment Database. The database contains detailed equipment specifications and images, drawings and other documents when available.

How to configure the Lakeshore Model 336 Temperature Controller and Heater: Lakeshore Model 336 Temperature Controller Sensor and Heater Quick Start Guide.pdf

Belt-driven Automated Sample Changer
Our belt-driven automated sample changer, capable of measuring 23 powder samples from 2K-300K, are available for Mail-in and GU proposals starting from the 2025-B cycle.

Room Temperature Spinning Automated Sample Changer
Our spinning automated sample changer can accommodate up to 7 powder/bulk samples at RT. During data collection, each samples can spin to reduce the preferred orientation. 

In Operando Battery Cycling Cell
A Swagelok-type cell made from the null-scattering material TiZr is available in two cylindrical sizes, 12 mm and 20 mm in diameter, optimized for use on constant-wavelength beamlines. This cell is suitable for both conventional secondary-ion batteries and solid-state batteries. It is designed so that the neutron beam exclusively illuminates the electrode located at the end of the cell. WAND² also offer users stainless steel cells, enabling users to perform preliminary tests at their home institutions before using the TiZr cell at the beamline. See publication: https://doi.org/10.1002/cmtd.202200046.

Humidity Chamber
Temperature and relative humidity controlled sample environment designed especially for HB-2C WAND² beamline. See publication: https://doi.org/10.1107/S1600576718001243

Closed Cycle Refrigerators—Bottom Loader
Typically used for single crystal experiments, the bottom loading CCR has an operating temperature range of 5 K – 300 K (base temperature dependent on particular CCR used).  The standard sample is mounted in a single crystal sample can that has been vacuum sealed with an indium gasket in an inert atmosphere—for high temperature experiments, the indium gasket is omitted.  The distance between the sample mount to beam center is a 2.375” (60 mm).  Cooling to base takes approximately 2 hrs.  High temperature bottom loading CCRs can reach temperatures up to 700 K and have a ¼-28 female interface and a 2.375” (60.3 mm) distance from the sample mount to beam center.  Both standard and high temperature bottom loading CCRs can be tilted to +/- 20 degrees when mounted on the sample goniometer with a translation limit of +/-0.4” (10 mm).  High capacity CCRs are available for use with specialized high-pressure cells and have a tilt limit of +/-5 degrees.  Contact the WAND instrument team for more information.

Closed Cycle Refrigerators—Janis Top Loaders
Used for both powder and single crystal experiments, the Janis top loading CCR has an operating temperature range of 4 K – 400 K.  The standard single crystal sample is mounted on an aluminum plate or rod and attached to the stick insert.  The powder samples are loaded into aluminum or vanadium sample cans that have been vacuum sealed with an indium gasket in an inert atmosphere (see below for information on powder sample cans), which is then mounted on the insert.  The sample mount is a ¼-28 female thread on the stick insert with a 2.375” (60 mm) distance from the sample mount to beam center.  Cooling to base takes approximately 2 hrs.  The Janis CCR has a high temperature insert available for operations up to 800 K.  Specialized high temperature powder sample cans are required for operation above room temperature.  The Janis has a tilt limit of +/-5 degrees with a +/-0.4” (10 mm) translation limit.  

How to change between high and low temperature operation with the Janis Cryofurnace high temperature insert: Janis Cold_Hot Setup.pdf  

Liquid Helium Cryostats—ILL Orange Cryofurnace and Oxford Variox
The top loading liquid helium cryostats have a base temperature of 1.5 K and can be used with ultra-low temperature inserts described below.  Cooling to base takes approximately 1.5 hrs.  The same sample cans as used for the Janis CCR are used for the liquid helium cryostats.  Tilt limits for both cryostats are +/-5 degrees with +/-10 mm translation limit.  The sample mounts on the same ¼-28 female interface.  The distance from the mounting interface to beam center varies from 1.75” (44.5 mm) to 2.44” (62 mm).  The standard bore diameter is 1.9” (50 mm), however 2.75” (70 mm) and 3.937” (100 mm) diameter bores are available on the Orange cryostat for use with ultra-low temperature inserts.  For concerns regarding sample mounting, contact the WAND instrument team.

How to change a sample in an ILL Orange Cryostat: SampleChangeforOrangeCryostat.pdf

ILL Niobium Foil Vacuum Furnace
The ILL vacuum furnace has an operating temperature range of 30 C to 1500 C (303 K – 1773 K).  Special high temperature plates are used to mount single crystal and high temperature cans for powder samples, described below.  The mounting interface is an M8x1.25 male thread with 1.25” (31.7 mm) distance from the mounting interface to beam center.  The bore is 1” (H) x 1.9” (D)  (25 mm (H) x 50 mm (D)).  The ILL vacuum furnace has a tilt limit of +/-5 degrees with +/-0.4” (10 mm) translation limit.

Controlled Atmosphere Furnace (CAF)
The CAF has an operating temperature from 30 C to 1000 C (303 K – 1273 K).  Samples are typically inserted into 1 m long 0.375” (9.5 mm) ID quartz tubes.

Cryomagnets
WAND² uses a 6T cryomagnet. The magnets available are called MAG-I and MAG-J and are identical. They have a standard operating temperature range of 1.5 K – 300 K and can be tilted to +/-2.5 degrees with a +/0.4” (10 mm) translation limit.  The magnet has a 50mm bore and can accommodate ULT-inserts for temperatures down to 50mK. The mount interface on the standard stick is a 5/16-18 Female.

Ultra-Low Temperature Inserts—Dilution Refrigerator and 3He
Two types of ultra-low temperature inserts are available for use with the Orange and Variox liquid helium cryostats as well as the cryomagnets. The Oxford Dilution insert reaches a base temperature of 0.05 K and the 3He insert of 0.3 K.  For powder samples, copper lids on either copper cans (dilution) or aluminum cans (3He) are used for ultra-low temperature experiments. Equipment to pressurize these cans with 10bar He is available. Tilt limits are reduced to +/-3 degrees with use of these inserts. 

Ultra-Low Temperature 3He-CCR
The ACV/³He CCR/Heliox-7 from OXFORD is a sample environment for neutron scattering covering the temperature range from 300mK to 300K. The system uses cryogenic liquids in a closed circuit and operates as “push-button” with the “Set temperature (T_set)” the only parameter. It is a robust system capable of cooling larger samples. Disadvantage is a slow initial cooling time, which requires off-line preparation.

Pressure Cells
A 6 kbar Al-helium gas pressure cell is available for use in an Orange cryostat for in situ pressure changes.  Various BeCu clamp pressure cells (up to 2 GPa) are available for higher pressure experiments.  The pressure capabilities and currently expanding.  Contact the WAND² instrument team for more information.

Uniaxial Pressure Stick
A uniaxial pressure stick for in situ single-crystal measurement. The pressure stick can be used in a cryostat or cryomagnet, supporting a maximum load of 300 Ib (~1kN). Sample size is up to 10mm(H)*10mm(W)*5mm(L). Sample require careful polishing to provide parallel loading surfaces.

Additional Sample Environments
Additional custom specialized sample environments may be accommodated at the WAND²—e.g. gas flow, liquid flow, electric field, etc.  Users are strongly encouraged to discuss experimental needs with the WAND² instrument team before requesting custom sample environments for their proposals.

Sample Holders
Various sample holders are available for single crystal sample mounting with custom mounts provided as needed.  Detailed information about the various powder sample cans mentioned above, dimensions and photos, is in the following document from the HB-2A instrument team.