Developing a new set of temperature calibration materials for high-temperature thermal analyses

Area of Science:

• Materials Science
• Analytical Chemistry
• Physical Chemistry

Background:

• Accurate temperature calibration is crucial for high-temperature thermal analysis techniques like DSC and DTA.
• Existing calibration standards, such as Nickel, present limitations due to oxidation and eutectic reactions, leading to uncertainties.
• A need exists for reliable calibration materials in the intermediate temperature range between gold and nickel.

Purpose of the Study:

• To develop and validate a new set of Research Grade Test Materials (RGTMs) for high-temperature thermal analysis calibration.
• To provide accurate temperature calibration standards for differential scanning calorimetry (DSC) and differential thermal analysis (DTA) instruments.
• To address the limitations of current calibration methods, particularly those involving Nickel.

Main Methods:

• Synthesis and characterization of candidate eutectic binary alloys.
• Determination of melting points using high-temperature thermal analysis techniques.
• Evaluation of the performance of new RGTMs for temperature calibration in DSC/DTA.

Main Results:

• A new set of RGTMs including Ni-41Nb (1181°C), Co-13Nb (1240°C), Fe-10Nb (1372°C), Rh-23.5Si (1421°C), and Ru-28Si (1535°C) was developed.
• These alloys cover the temperature range between the melting points of gold and nickel.
• Calibration using RGTMs instead of Nickel significantly improved accuracy, reducing variance from 9.16 to 0.65 °C.

Conclusions:

• The developed RGTMs provide accurate and reliable temperature calibration for high-temperature DSC and DTA.
• These new materials overcome the limitations associated with Nickel-based calibration, enhancing measurement precision.
• The availability of these RGTMs enables more accurate intermediate temperature calibration for thermal analysis instruments.