Characterization of Nanoreinforcement Dispersion in Inorganic Nanocomposites: A Review
Abstract
:1. Introduction
2. Qualitative Characterization
2.1. Characterization Techniques
2.2. Metal Matrix Nanocomposites
Characterization technique | Mode of analysis | Sample form | Extent of distribution |
---|---|---|---|
Scanning Electron Microscopy (SEM) | direct | powder and bulk | localized (2D) |
Transmission Electron Microscopy (TEM) | direct | powder and bulk | localized (2D) |
Atomic Force Microscopy (AFM) | direct | bulk | localized (3D) |
X-ray Microcomputed Tomography | direct | bulk | localized (3D) |
X-ray mapping | direct | powder and bulk | localized and bulk |
Zeta Potential Measurements | indirect | powder | localized and bulk |
Raman Confocal Microscopy | direct | bulk | localized and bulk (3D) |
Ultra-Small Angle X-ray Scattering (USAXS) | indirect | powder and bulk | – |
Nanocomposite | Fabrication process | Characterization technique | Composite form | Dispersion quality | Reference |
---|---|---|---|---|---|
SiC/Al | high energy ball milling; plasma activated sintering | SEM and TEM | bulk | well-dispersed | [35 ] |
CNT/Cu | molecular level mixing and vacuum sintering | TEM | bulk | well-dispersed | [34 ] |
Al2O3/Fe | high frequency induction heated sintering | SEM and X-ray mapping | bulk | well-dispersed | [70 ] |
WC-10% Co/Cu | direct metal laser sintering | AFM | bulk | aggregated for 40 wt%; well-dispersed for 30 wt% | [5 ] |
ZrO2/Ni | electrochemical plating process | zeta potential measurements | powder | well-dispersed for pH value = 2; aggregated for pH value = 3.5 | [6 ] |
Al2O3/Al | stir casting | Holotomography and phase contrast tomography | bulk | well-dispersed | [66 ] |
Fly ash/Al | wet blending, cold compaction and sintering | SEM and AFM | bulk | well-dispersed | [75 ] |
SiC/Al | pressure-die casting | AFM, SEM and X-ray mapping | bulk | not reported | [76 ] |
Ni/Al alloy | blending, cold-pressing and extrusion | SEM and phase contrast tomography | bulk | particles oriented in the extrusion direction | [77] |
Si-Zr/Al | blending, hot-pressing and extrusion | phase contrast tomography | bulk | homogeneous | [78] |
SiC/Al alloy | rheocasting and extrusion | phase contrast tomography and SEM | bulk | well-dispersed | [79] |
SiC/Al and Ta/Al | melt-stirring | SEM and X-ray mapping | bulk | well-dispersed | [80] |
Al2O3/Al | high-energy ball milling | SEM and X-ray mapping | powder | well-dispersed | [13] |
Al2O3/Al alloy | squeeze casting | SEM and TEM | bulk | well-dispersed and intentionally agglomerated | [81] |
Al2O3/Fe-Cr | high-energy ball milling and pulsed current activated sintering | SEM and X-ray mapping | bulk | well-dispersed | [82] |
CNT/Cu | molecular level mixing and spark plasma sintering | SEM and TEM | bulk | well-dispersed | [83] |
Cu-Ni | reduction of mixed metal oxides | SEM | powder | mix of agglomerates and dispersed particles | [12] |
CNT/W-Cu | wet ball-milling and hot-pressing | SEM | bulk | well-dispersed | [84] |
W/Cu | wet ball-milling of oxide powder and reduction | SEM and TEM | powder | well-dispersed | [85] |
AlN/Al alloy | cryomilling and hot-pressing | TEM | bulk | well-dispersed | [86] |
Al2O3/Cu | wet chemical processing, cold pressing, and pressureless sintering | TEM, STEM, X-ray mapping | bulk | well-dispersed | [14] |
CNT/Al | ultrasonication, wet ball-milling, cold compaction and sintering | SEM, TEM and X-ray mapping | bulk | well-dispersed | [87] |
2.3. Ceramic Matrix Nanocomposites
Nanocomposite | Fabrication process | Characterization technique | Composite form | Dispersion quality | Reference |
---|---|---|---|---|---|
SiO/Graphene | In situ chemical synthesis | SEM; TEM | bulk | uniform | [91] |
MWCNT/Al2O3 | SPS | TEM; zeta potential | bulk | uniform | [9] |
Si3N4/Graphene | SPS | SEM | bulk | uniform | [92] |
CNT/YSZ | In situ growth of CNTs on zirconia SPS | FESEM; TEM | bulk | uniform | [89] |
Si-C-N/MWCNT | ball milling pyrolysis | SEM; confocal raman mapping | bulk | uniform for 10% CNTs not uniform for 5% CNTs | [7] |
CNT/Al2O3 | SPS of individually alumina decorated CNTs | SEM; TEM; Zeta Potential | bulk | uniform for 2.6%–15% CNTs | [11,88] |
CNT/Al2O3 | sol-gel process | SEM | bulk | uniform | [93] |
Fe/MgO | spray pyrolysis | SEM | powder | uniform | [10] |
ZrO2/WC | SPS | SEM; X-ray mapping | bulk | uniform | [39] |
NdAlO3/AL2O3 | CVD | AFM; TEM | bulk | uniform | [44] |
Pt/Al2O3 | Co-sputtering | SAXS | thin film | uniform | [90] |
3. Quantitative Analysis
3.1. Local Area Fraction Method
3.2. Nearest-Neighbor Distance and Near-Neighbor Distance Methods
3.3. Mean Intercept Length Method
3.4. Quadrat Method
3.5. Radial Distribution Function
3.6. Second Order Intensity Function
4. Future Directions
5. Conclusions
- -
- The SEM and TEM remain the most widely used techniques although both of them cannot be regarded as self-sufficient techniques for a reliable characterization owing to the size limitation of the selected cross-sectional area of the bulk sample which leads to sampling bias in the results.
- -
- Techniques, which provide a broader view of the distribution in the bulk volume, can lead to much more reliable prediction of the properties of nanocomposites. Some of these characterization techniques, which can yield a relatively large-scale distribution analysis in nanocomposites, directly result in a pictorial image of the distribution (for example Confocal Raman Microscopy and Atomic Force Microscopy). Other techniques rely on an indirect analysis for distribution characterization in the bulk volume (like Small-angle X-ray Scattering and Zeta-Potential measurement).
- -
- The X-ray microcomputed tomography is currently only applicable for micro- and macro-composites analysis. However, X-ray nanocomputed tomography may result in a very efficient and reliable three-dimensional pictorial image of the nanoreinforcement distribution within bulk volume of nanocomposite.
- -
- Zeta potential measurement technique offers a two-fold advantage of not only analyzing the distribution of nanoreinforcement in the overall bulk volume of nanocomposite before its consolidation but also yielding a highly reliable measurement of interfacial bond strength between the matrix and the reinforcement phase.
- -
- Qualitative characterization techniques suffer from a common drawback of inability to quantify the distribution of the reinforcement phase within the host matrix—a necessary prerequisite needed for practically feasible evaluation of bulk mechanical properties of nanocomposites.
- -
- Quantitative characterization techniques used for conventional composites involve analyses of microstructure images from which various quantitative measures, either deterministic or probabilistic, are calculated. Deterministic measures include quantities such as mean-intercept lengths in Dirichlet tessellations or local area fractions, while probabilistic measures include probability density functions or frequency distributions in techniques, such as the quadrat method or the nearest neighbor distances.
- -
- There is a potential to modify and upgrade quantitative characterization techniques used for conventional composites to extend their use for nanocomposites.
Acknowledgments
Author Contributions
Conflicts of Interest
References
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Saheb, N.; Qadir, N.U.; Siddiqui, M.U.; Arif, A.F.M.; Akhtar, S.S.; Al-Aqeeli, N. Characterization of Nanoreinforcement Dispersion in Inorganic Nanocomposites: A Review. Materials 2014, 7, 4148-4181. https://doi.org/10.3390/ma7064148
Saheb N, Qadir NU, Siddiqui MU, Arif AFM, Akhtar SS, Al-Aqeeli N. Characterization of Nanoreinforcement Dispersion in Inorganic Nanocomposites: A Review. Materials. 2014; 7(6):4148-4181. https://doi.org/10.3390/ma7064148
Chicago/Turabian StyleSaheb, Nouari, Najam Ul Qadir, Muhammad Usama Siddiqui, Abul Fazl Muhammad Arif, Syed Sohail Akhtar, and Nasser Al-Aqeeli. 2014. "Characterization of Nanoreinforcement Dispersion in Inorganic Nanocomposites: A Review" Materials 7, no. 6: 4148-4181. https://doi.org/10.3390/ma7064148