Powder and High-Resolution XRD Facility

Location: LRSM 108
Supervisor/Coordinator: Iryna Golovina
Contact: Iryna Golovina
Phone: 215-573-9482
Email: irynag@upenn.edu
Oversight Committee Chair: Eric A. Stach

The Powder and High-Resolution XRD facility is equipped with two highly versatile multipurpose X-ray diffractometers from Rigaku, SmartLab and SmartLab SE with built-in intelligent guidance. The combined capabilities of the diffractometers provide a comprehensive structural characterization of various types of materials (metals, ceramics, nanoparticles, polymers, geological specimens) in either bulk or thin-film form. The structural materials characterization includes phase identification, qualitative and quantitative composition analysis, differentiation between crystalline and amorphous phases, determination of structure, lattice parameters, orientation and texture, evaluation of crystallite sizes and strains, monitoring of quality control.

photo of the two SmartLab X-ray diffractometers

The SmartLab SE system has recently undergone a major upgrade. The upgrade added a Cross Beam Optics (CBO), Chi-Phi and RxRy attachments, enabling high-resolution XRD (HRXRD) measurements in addition to powder XRD (PXRD) measurements. Specifically, the CBO unit allows easy switching between the direct beam para-focusing (BB) and parallel beam (PB) geometries by simply changing the selection slit, while Chi-Phi and RxRy attachments provide sample tilt and rotation axes to move sample in Chi,  Phi, and Omega axes. The upgrade made available such HRXRD measurements as X-ray reflectivity (XRR), Rocking curves, and Reciprocal space mapping (RSM). The XRD measurement performed by SmartLab SE is controlled by the built-in SmartLab Studio II software. The upgrade added the XRR Plugin and the HRXRD Analysis Plugin to SmartLab Studio II. Thus, in addition to fast phase identification analysis and quantitative analysis of powder samples, the analysis of XRR data and HRXRD data for thin films is now available using SmartLab Studio II. The SmartLab SE system is equipped with a 1D ceramic strip detector D/teX Ultra250 that detects and integrates X-ray intensity efficiently, so that data can be collected as fast as within a few minutes. In addition, the detector has high resolution and therefore can reduce the overall background of the measurement enabling the detection of XRD peaks of minor components easily.

SmartLab is a horizontal sample mount multipurpose X-ray diffractometer that permits measurements and characterization for both powder and thin-film samples. The instrument is equipped with a CBO and 0D detector SC-70. Additionally, features and capabilities include:

  • 3kW long-focus sealed-tube Cu X-ray generator
  • A theta-theta goniometer (omega scans, 2-theta/omega scans, 2-theta scans)
  • A chi axis (tilt adjustment), a Z axis (thickness adjustment), and a phi axis (adjustment of in-plane orientation)
  • The in-plane arm and RxRy attachment
  • Ge(220) 2-bounce and Ge(220) 4-bounce monochromators
  • CBO-f unit for measurements of micro area (μ-XRD) and micro amount of sample
  • Interchangeable double-slit analyzer, parallel-slit analyzer, and 2-bounce analyzer on receiving side

SmartLab SE and SmartLab diffractometers allow PXRD and HRXRD measurements. Compared to PXRD which allows first of all phase identification and structure analysis, the HRXRD methods (XRR, rocking curves, and RSM) allow measurements of film thickness, film density, surface or interface roughness, film quality, complete film orientation, as well as strain state and strain distribution which is important for epitaxial thin films grown on solid substrates.

The Powder and High-Resolution X-Ray Diffraction facility is available to Penn faculty, staff and students, and to outside users on an hourly fee basis. FY2025 Hourly Rates and Fees effective March 1, 2025 through June 30, 2025.

Instrument Non-Penn academic users Industrial users
Rigaku SmartLab SE $12/hour $200/hour or $2000/24-hour day
Rigaku SmartLab $12/hour $200/hour or $2000/24-hour day

There is no charge for initial training.

XRD Measurement Service is available at an additional 39% administrative fee to the total cost of service for outside users who are unable to visit the facility directly.

Facilities users must include the following text in the acknowledgment section of their publications:

“The authors acknowledge the use of the XRD facility supported by the Laboratory for Research on the Structure of Matter and the NSF through the University of Pennsylvania Materials Research Science and Engineering Center (MRSEC) DMR-2309043.”

Oversight Committee:

Thomas Mallouk

Christopher Murray

Eric Stach