Dynamic Mechanical Thermal Analysis and Transmission Electron Microscopy of Elastomer Blends

1986 ◽  
Vol 59 (4) ◽  
pp. 623-633 ◽  
Author(s):  
K. A. Mazich ◽  
M. A. Samus ◽  
P. C. Killgoar ◽  
H. K. Plummer

Abstract Dynamic mechanical thermal analysis and transmission electron microscopy have been used to elucidate the structure of binary and ternary blends of NR, BIIR, and IM. Dynamic measurements at 10 Hz were able to resolve loss-tangent peaks into a major peak due to NR and a broad shoulder associated with BIIR and IM. Interpretation of these data in conjunction with electron micrographs indicate that the butyl polymers (BIIR and IM) form a second phase in a matrix of NR for compositions containing at least 67% NR. Dynamic mechanical properties and TEM micrographs of binary blends of NR with BIIR or IM show that the structure of these binary blends differ; IM forms larger, more distinct domains in the NR matrix. This difference in structure may result from the different molecular weights of the butyl polymers and the ability of BIIR to crosslink with NR. TEM micrographs of both binary blends indicate that carbon black is dispersed in the matrix material and is excluded from the isobutylene-rich domains, The two-phase structure of these blends and the partitioning of carbon black between the phases may enhance the fatigue lives of these composites. Cure temperatures in the range from 130°C to 170°C affected the properties and structure of only one blend studied in this work. This blend, an 80:20:20 mixture of NR, BIIR, and IM, respectively, was able to alter its morphology when the cure temperature was elevated. Material cured at 130°C contained domains with a wide variety of shapes and sizes; material cured at 170°C contained uniform, well-defined inclusions. This ternary blend was the only material that also exhibited a higher fatigue life when the cure temperature was raised. Achieving a well-defined dispersion in a two-phase elastomer blend apparently maximizes the fatigue life of the composite material.

Minerals ◽  
2021 ◽  
Vol 11 (7) ◽  
pp. 727
Author(s):  
Shiyun Jin ◽  
Huifang Xu ◽  
Seungyeol Lee

The enigmatic Bøggild intergrowth in iridescent labradorite crystals was revisited in light of recent work on the incommensurately modulated structures in the intermediated plagioclase. Five igneous samples and one metamorphic labradorite sample with various compositions and lamellar thicknesses were studied in this paper. The lamellar textures were characterized with conventional transmission electron microscopy (TEM) and scanning transmission electron microscopy (STEM). The compositions of individual lamellae were analyzed with high-resolution energy-dispersive X-ray spectroscopy (EDS) mapping and atom probe tomography (APT). The average structure states of the studied samples were also compared with single-crystal X-ray diffraction data (SC-XRD). The Na-rich lamellae have a composition of An44–48, and the Ca-rich lamellae range from An56 to An63. Significant differences between the lamellar compositions of different samples were observed. The compositions of the Bøggild intergrowth do not only depend on the bulk compositions, but also on the thermal history of the host rock. The implications on the subsolidus phase relationships of the plagioclase feldspar solid solution are discussed. The results cannot be explained by a regular symmetrical solvus such as the Bøggild gap, but they support an inclined two-phase region that closes at low temperature.


2006 ◽  
Vol 514-516 ◽  
pp. 353-358 ◽  
Author(s):  
Shinzo Kohjiya

. Generally rubber products are a typical soft material, and a composite of a nano-filler (typically, carbon black or particulate silica) and a rubber (natural rubber and various synthetics are used). The properties of these soft nano-composites have been well known to depend on the dispersion of the nano-filler in the rubbery matrix. The most powerful tool for the elucidation of it has been transmission electron microscopy (TEM). The microscopic techniques are based on the projection of 3-dimensional (3D) body on a plane (x, y plane), thus the structural information along the thickness (z axis) direction of the sample is difficult to obtain. This paper describes our recent results on the dispersion of carbon black (CB) and particulate silica in natural rubber (NR) matrix observed by TEM combined with electron tomography (3D-TEM) technique, which enabled us to obtain images of 3D nano-structure of the sample. Thus, 3D images of CB and silica in NR matrix are visualized and analyzed in this communication. These results are precious ones for the design of soft nano-composites, and the technique will become an indispensable one in nanotechnology.


Clay Minerals ◽  
2004 ◽  
Vol 39 (4) ◽  
pp. 391-404 ◽  
Author(s):  
J. E. F. C. Gardolinski ◽  
G. Lagaly ◽  
M. Czank

AbstractKaolinite and synthetic γ-Al(OH)3 (gibbsite or hydrargillite) were reacted with phenylphosphonic, phenylphosphinic and 2-nitrophenol-4-arsonic acids. The products were studied by powder X-ray diffraction, transmission electron microscopy/selected area electron diffraction/ energy dispersive X-ray/Fourier transform infrared and simultaneous thermogravimetric/differential thermal analysis. The acids were not intercalated but, instead, easily destroyed the structure of the minerals. Lamellar Al phenylphosphonate and aluminium phenylphosphinate and phenylarsonate with polymeric linear-chain structures were formed from kaolinite. The reaction between gibbsite and the same acids yielded almost identical products. No evidence of formation of grafted kaolinite derivatives after the reaction with phenylphosphonic acid was found.


1994 ◽  
Vol 67 (2) ◽  
pp. 280-287 ◽  
Author(s):  
Tyler C. Gruber ◽  
T. W. Zerda ◽  
Michel Gerspacher

Abstract A three-dimensional modeling technique is used to characterize the structure of carbon-black aggregates. The relative positions of individual particles in aggregates are determined using transmission electron microscopy (TEM). Data are acquired from two-dimensional projections taken with the aggregates at two different orientations with respect to the electron beam. Computerized aggregate models are generated using data from TEM projections in our reconstruction algorithm. Inspection of these models shows that their projections very closely replicate the TEM micrographs. Quantitative analysis of the aggregate models reveals that aggregates generally exhibit anisotropy, in the form of a reduction of aggregate breadth, or “flatness,” in one direction. The flat sides tend to align preferentially, along the plane of the TEM sample grid. The dimensions for each aggregate with respect to its best-fitting plane of flatness are determined, and are related through a “flatness index.”


1994 ◽  
Vol 9 (1) ◽  
pp. 236-245 ◽  
Author(s):  
S.D. Walck ◽  
M.S. Donley ◽  
J.S. Zabinski ◽  
V.J. Dyhouse

Films of PbO/MoS2, grown by pulsed laser deposition, exhibit a significant improvement in tribological performance compared to MoS2 films grown by the same process. The microstructure and crystallography of PbO/MoS2 composite films were investigated using transmission electron microscopy (TEM) to identify the features responsible for this tribological improvement. Self-supporting samples were prepared from pulsed laser deposited, PbO/MoS2 thin films grown on single crystal sodium chloride substrates. Films deposited at room temperature exhibited a two-phase microstructure with one of the phases being amorphous. X-ray microanalysis results showed that the crystalline phase had significantly higher concentration ratios of Mo/Pb, Mo/S, and Pb/S than did the amorphous phase. Films grown at 300 °C were polycrystalline, with a grain size of about 20 nm, and had a NaCl type structure which was isomorphous to PbS. The grains had rectangular shape, and exhibited preferred orientation with the sodium chloride substrate. The concentration of S for these films was approximately 80% of the S concentration for films grown at room temperature. Both the high temperature and room temperature films had S concentrations which were higher than expected from the MoS2 in the target; this was attributed to gettering of the S in the vacuum chamber by Pb. The electron diffraction results, together with previously published results, suggest that the crystal structure of the phases in these films is not responsible for the improvement in tribological properties. However, the microstructural components formed during film growth do determine the wear-induced chemical reaction pathways.


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