▶ Customer Requirements: In-situ SAXS/WAXS Characterization at Ultra-High Temperatures

The BL16B X-ray Small-Angle Scattering Beamline at SSRF is one of the first seven beamlines built at the facility. The beamline is derived from the bending magnet of the storage ring and is equipped with a sagittally focusing water-cooled double-crystal monochromator and a bent cylindrical mirror. The beamline currently serves research in polymer materials, nanomaterials, mesoporous materials, colloids, liquid crystals, metal materials, and other fields for SAXS studies, and has already achieved multi-method coupling including SAXS/WAXS/Raman/IR.

In user experimental scenarios, BL16B faces the following core challenges:

• Ultra-High Temperature Requirements: Studies such as ceramic sintering, metal heat treatment, and high-temperature alloy phase transformation require in-situ SAXS/WAXS experiments in the 1000–1500°C temperature range, enabling real-time tracking of the evolution of microstructures such as nano-scale pores, precipitates, and grain boundaries.

• SAXS/WAXS Optical Path Compatibility: Small-angle scattering experiments measure scattered signals near the main beam, requiring the sample position to maintain high X-ray transmission, low absorption, and low background scattering. At the same time, the sample's positional stability during heating must be extremely high (micron-level) to ensure precise alignment of the scattered signals with the detector.

• Atmosphere Control: Samples are highly susceptible to oxidation at high temperatures, necessitating an inert/reducing protective atmosphere to ensure the authenticity of experimental data.

▶ Solution: GoGo Instruments Synchrotron Radiation Ultra-High-Temperature Heating Stage

GoGo Instruments custom-developed the synchrotron radiation ultra-high-temperature heating stage H1500-SR for the BL16B beamline. This device adopts a resistance-heated furnace-chamber sample stage structure, with the design fully considering the stringent requirements of SAXS experiments for high X-ray transmission and low background scattering. Key specifications are as follows:

Temperature Range:Room Temperature (RT) ~ 1500°C

Maximum Heating Rate:150°C/min

Heating Method:Resistance heating, furnace-chamber sample stage structure

Atmosphere Control:Supports inert/reducing protective gas flow

Compatible Optical Path:Synchrotron SAXS/WAXS transmission geometry

Sample Stage:Standard φ8 mm (O.D.) × 2 mm (slot depth) ceramic grooved sample stage + dedicated powder sample fixture

Beamline Compatibility:Precision-engineered structure ensuring high X-ray transmission, low background scattering, and high sample position stability

Four Technical Highlights:

• Highlight 1: Precise temperature control over a wide range, filling the beamline's ultra-high-temperature gap. The device covers temperatures from room temperature to 1500°C, with a maximum heating rate of 50°C/min, effectively extending the beamline's in-situ variable-temperature capability to 1500°C and providing critical support for high-temperature in-situ SAXS/WAXS studies of ceramics, metals, high-temperature alloys, and other materials.

• Highlight 2: Custom-designed for SAXS transmission geometry, ensuring high X-ray transmission and zero interference. The device features a tailor-made structure addressing the high sensitivity requirements of SAXS experiments for weak scattering signals near the main beam. It comes standard with a φ8 mm (O.D.) × 2 mm (slot depth) ceramic grooved sample stage and a dedicated powder sample fixture, compatible with vertical-incidence transmission geometry. The sample stage is made of high-temperature-resistant ceramic material, offering low X-ray absorption, low background scattering, corrosion resistance, thermal deformation resistance, and non-contaminating properties, ensuring structural stability of the sample holder and data quality at high temperatures.

• Highlight 3: Controlled atmosphere environment to prevent high-temperature oxidation. The atmosphere chamber supports the introduction of inert gases (e.g., Ar, N₂) or reducing protective gases, continuously protecting the sample during high-temperature experiments and ensuring that SAXS/WAXS scattering data truly reflect the intrinsic nanostructural evolution of the material.

• Highlight 4: Deep integration with the beamline's EPICS control system, enabling unified scheduling of temperature control and synchronized data acquisition, allowing users to complete the entire in-situ experimental workflow from the control room.

▶ Delivery On-Site: Installation, Commissioning, and On-Site Training

The technical team of  GoGo Instruments traveled to the Shanghai Synchrotron Radiation Facility to complete on-site installation and commissioning of the equipment. Specialized training was provided on equipment operation, temperature control program settings, and the use of the atmosphere control system, ensuring that beamline researchers and users can quickly get started and independently conduct experiments.

This delivered synchrotron radiation ultra-high-temperature heating stage will be formally integrated into the in-situ experimental equipment system of the BL16B beamline, supporting a full range of in-situ SAXS/WAXS experimental needs, including nanopore evolution during ceramic sintering, precipitation kinetics of precipitates in metal heat treatment, and nanostructural evolution during phase transformations in high-temperature alloys.

GoGo Instruments is consistently dedicated to providing high-performance, high-reliability in-situ testing solutions for scientific researchers. To date, the GoGo Instruments ultra-high-temperature characterization system has undergone deep integration testing at the BL16B beamline of the Shanghai Synchrotron Radiation Facility (SSRF), demonstrating excellent compatibility and stable operation. Whether for standard products or custom requirements, Googol Instrument is committed to advancing every scientific research project with rigorous craftsmanship and professional service.