Two new zinc-terephthalate MOFs, (H 2 NEt 2)[Zn 3 (BDC) 3 (HCO 2)]Á1.5DEF (1) and Zn 4 (BDC) 3 (HCO 2) 2 (DEF) 4 (2), based on trinuclear zinc secondary building units have been solvothermally synthesized from the well-studied MOF-5 system Zn-H 2 BDC-DEF (H 2 BDC = 1,4-benzenedicarboxylic acid or terephthalic acid; DEF = N,N-diethylformamide). It is shown that adding small amounts of formic acid to this system has a great influence on the formation of 3D networks based upon trimetallic zinc building units Zn 3 (O 2 CR) 6. The structures of 1 and 2 comprise stacked 3 6 tessellated 2D zinc-terephthalate layers which are linked into 3D frameworks either by bridging formate monoanions (1) or by in situ generated neutral bridging units Zn(HCO 2) 2 (DEF) 4 (2). Flowing supercritical-CO 2 activation of 1 led to a partially ($80%) desolvated and probably collapsed structure (1-SC) with a measured BET (Brunauer-Emmett-Teller) surface area of 38 m 2 g À1 .
porous binder-free monoliths of few-walled carbon nanotubes by spark plasma sintering. Journal of Materials Science, Springer Verlag, 2018Verlag, , vol. 53 (n°5), pp. 3225-3238. 10.1007Verlag, /s10853-017-1784 Open Archive TOULOUSE Archive Ouverte (OATAO) OATAO is an open access repository that collects the work of Toulouse researchers and makes it freely available over the web where possible.
ABSTRACTCarbon nanotubes with few walls (FWCNTs) are prepared by catalytic chemical vapor deposition. Transmission electron microscopy investigations for each sample show the average number of walls (3, 4 and 8) as well as the internal and external diameter distributions. Binder-free FWCNT monoliths are prepared by spark plasma sintering (SPS) at temperatures in the range 1000-1600 °C. A combination of techniques including Raman spectroscopy, scanning-and transmission electron microscopy, electron microdiffraction is used to characterize the samples. Compared to the FWCNT powders, the high temperatures used for SPS favor the elimination of surface defects in CNT walls but also some limited amorphization, without dramatic damage to the CNTs. Increasing the SPS temperatures produces an increase in densification. N 2 adsorption-desorption cycles revealed that the powders and monoliths show microporosity and, mostly, mesoporosity. Some monoliths show a specific surface area equal to about 500 m 2 /g. The 4WCNTs when consolidated into monoliths by SPS at 1000 or 1100 °C are able to retain a high amount of mesoporosity that contributes to a high porous volume of the order of 0.8 cm 3 /g.
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