TY - JOUR
T1 - Quantification of surface grinding during the sample preparation of cementitious materials by optical profilometry
AU - Holthuizen, Patrick
AU - Çopuroğlu, Oğuzhan
PY - 2024
Y1 - 2024
N2 - Sample preparation is of utmost importance for any microscopy and microstructural analysis. Correct preparation will allow accurate interpretation of microstructural features. A well-polished section is essential when scanning electron microscopy (SEM) is used in backscattering electron (BSE) mode and characteristic X-rays are to be quantified using an energy-dispersive spectroscopy (EDS) detector. However, obtaining a well-polished section, especially for cementitious materials containing aggregates, is considered to be challenging and requires experience. A sample preparation procedure consists of cutting, grinding and polishing. Undercutting of soft and brittle paste between harder aggregates can be overcome by vacuum epoxy impregnation offering mechanical support in the matrix. Furthermore, most of the attention during the sample preparation is given to the polishing of the sample. There is a wide range of suggestions on polishing steps, ranging from grain sizes, time and applied force; however, the final assessment of a polish surface is often subjective and qualitative. Therefore, a quantitative, reproducible guidance on the grinding steps, effect of experimental parameters and the influence of different grinding steps on the surface quality are required. In this paper, the influence of grinding was quantitatively evaluated by a digital microscope equipped with optical profilometry tools, through a step-wise procedure, including sample orientation, grinding time and the difference between cement paste and concrete. Throughout the grinding procedure, the surface profiles were determined after each grinding step. This showed the step-wise change in surface roughness and quality during the grinding procedure. Finally, the surface qualities were evaluated using optical and electron microscopy, which show the importance of the grinding/prepolishing steps during sample preparation.
AB - Sample preparation is of utmost importance for any microscopy and microstructural analysis. Correct preparation will allow accurate interpretation of microstructural features. A well-polished section is essential when scanning electron microscopy (SEM) is used in backscattering electron (BSE) mode and characteristic X-rays are to be quantified using an energy-dispersive spectroscopy (EDS) detector. However, obtaining a well-polished section, especially for cementitious materials containing aggregates, is considered to be challenging and requires experience. A sample preparation procedure consists of cutting, grinding and polishing. Undercutting of soft and brittle paste between harder aggregates can be overcome by vacuum epoxy impregnation offering mechanical support in the matrix. Furthermore, most of the attention during the sample preparation is given to the polishing of the sample. There is a wide range of suggestions on polishing steps, ranging from grain sizes, time and applied force; however, the final assessment of a polish surface is often subjective and qualitative. Therefore, a quantitative, reproducible guidance on the grinding steps, effect of experimental parameters and the influence of different grinding steps on the surface quality are required. In this paper, the influence of grinding was quantitatively evaluated by a digital microscope equipped with optical profilometry tools, through a step-wise procedure, including sample orientation, grinding time and the difference between cement paste and concrete. Throughout the grinding procedure, the surface profiles were determined after each grinding step. This showed the step-wise change in surface roughness and quality during the grinding procedure. Finally, the surface qualities were evaluated using optical and electron microscopy, which show the importance of the grinding/prepolishing steps during sample preparation.
KW - grinding
KW - optical profilometry
KW - sample preparation
KW - surface roughness
UR - http://www.scopus.com/inward/record.url?scp=85180890476&partnerID=8YFLogxK
U2 - 10.1111/jmi.13256
DO - 10.1111/jmi.13256
M3 - Article
C2 - 38108514
AN - SCOPUS:85180890476
SN - 0022-2720
VL - 294
SP - 128
EP - 136
JO - Journal of Microscopy
JF - Journal of Microscopy
IS - 2
M1 - jmi.13256
ER -