Conventional-sized specimens have been well and widely applied in research on hydrogen embrittlement. However, when the limited-size core components (nozzles and valves, etc.) of hydrogen energy equipment are evaluated for service damage, traditional testing with conventional-sized samples is no longer applicable and micro-sample testing methods are required. In this paper, recent progress in the characterization of hydrogen embrittlement achieved via a small-sized sample tensile test, small punch test and nanoindentation test is reviewed. The commonly used geometries and dimensions of various small-sized specimens are first described and the in situ hydrogen-containing environment testing cases equipped with small-sized specimens are presented, proving the advantages of direct observations of hydrogen influences on the mechanical property and microstructure evolution. Then, the quantitative analysis of hydrogen embrittlement sensitivity involving a small punch test is discussed, with a focus on the comparisons of the hydrogen embrittlement index calculated using different definition methods. Finally, the nanoindentation test of investigation on the interaction between hydrogen and dislocation in metals and the effect of indentation strain rate are summarized. Furthermore, the specific research directions and applications of micro-size specimens for further investigation on hydrogen embrittlement are identified.

In this study, a combined experimental and finite element modeling methodology (FEM) for a nanoindentation study is presented to quantitatively investigate the influence of hydrogen on the mechanical properties of ferrite and austenite in 2205 duplex stainless steel. The experimental results showed that, during hydrogen charging, the nano-hardness of ferrite and austenite gradually increased with time, showing a hydrogen-induced hardening phenomenon. After 3 h of hydrogen charging, the nano-hardness of both ferrite and austenite reached a saturation state, and the values of the nano-hardness of ferrite and austenite increased by 17.5% and 46.1%, respectively. FEM is employed by using a dual-phase microstructure-based model to reproduce nanoindentation load–displacement curves. To minimize the indentation size effect, an analytical correction model considering geometrically necessary dislocations (GNDs) was proposed. By considering GNDs, the errors between numerical predictions and experimental data reduced from about 50% to less than 5%.

The utilization of micro-sample testing has demonstrated its effectiveness in conducting quantitative research on mechanical properties, damage evolutions and fracture features. For in-service equipment, millimicron sampling allows for non-destructive testing and analysis of mechanical performance evolution during operation. This paper presents a comparative study of the miniature uniaxial tensile test (MUTT) and small punch test (SPT) by experimental and finite element methods. As a comparison, the standard conventional-size tensile tests were also carried out. Detailed analyses of the elastoplastic behaviors and damage evolutions of MUTT and SPT were presented, followed by an application case illustrating the characterization of hydrogen embrittlement sensitivity based on MUTT and SPT. An inverse finite element modeling method of load–displacement curve reproduction was used to calibrate the variations of damage parameters of hydrogen-charged MUTT and SPT specimens. Hydrogen embrittlement (HE) indexes were determined by using different calculation methods. The results reveal that the HE sensitivity estimated by MUTT is higher than that measured by SPT, which is related to the different deformation processes and strain rates of the two testing methods.