Page 51 - Annual Report_21-22
P. 51

Chemically coupled Hematite-rGO electrocatalyst for nitrogen reduction to ammonia

            The  chemically  coupled  hematite  with  rGO  was
            successfully  synthesized,  as  confirmed  by  the  XRD  and
            Raman analysis. The FTIR analysis was further confirmed,
            by the presence peak at 568 cm corresponding to the Fe-
                                      -1
            O-C  bond.  The  chemically  coupled  hematite/rGO shows
            enhanced  activity  for  the  nitrogen  reduction  reaction
            (NRR)  than  that  of  bare  α-Fe O   and  GO,  attributed  to
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            the improved e- transport across the interface and higher
            degree of N  activation for NRR catalysis, Figure 3. These
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            findings serve as an example to design an inexpensive but
            efficient catalyst by chemically coupling for the NRR.



                                                                      Fig. NH3 yield rate of hematite/rGO
                Ultrafast synthesis of Ti3SiC2 MAX phase by reactive Flash sintering for production of  2-D
                                                material Ti3C2TX MXene


            MXenes, a new class of two-dimensional transition metal   conventionally synthesized Ti SiC  MAX phase. The novelty
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            carbides,  nitrides  and  carbonitrides  (MXenes)  have  out-  of our research is its ability to synthesize different MAX
            performed other 2D nanomaterials and rapidly position-  phases with the desired composition in any atmosphere
            ing in numerous promising applications due to their ex-  (Vacuum, inert or air) in bulk using the ultrafast Flash sin-
            tra-ordinary properties. MXenes, provide very attractive   tering technique. The use of the flash sintering technique
            building blocks for a very large variety of applications, such   presented here for the synthesis of the MAX phase is an
            as energy storage, including super capacitors, lithium-ion   innovative  and  scalable  approach  capable  of  producing
            batteries, oxygen evolution reaction, heavy metal adsorp-  MAX phases in large quantities in a short time. Thus, it
            tion, water purification, electrocatalysis for H  generation,   could be a breakthrough for the rapid synthesis of a wide
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            medicine, and transparent coatings etc. Production of MX-  range of MAX phases on an industrial scale
            ene is still at a very early stage. One of the limiting factors
            for large-scale and low-cost manufacturing of MXenes is
            the cost and limited availability of MAX phases. Howev-
            er, making good-quality MXene requires not just “a MAX”,
            but a MAX phase with appropriate properties optimized
            for MXene synthesis. The existing conventional methods
            for the synthesis of MAX phases are expensive, complex,
            time and power consuming. Here, we have developed an
            ultrafast  route  with  a  cost-effective,  consolidated  flash
            sintering technology for the synthesis of the Ti SiC  MAX
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            phase which is feasible in the air as well as in a vacuum.
            Here, a relatively low voltage (35-42 V/cm) was applied
            using a DC power source across a compact Ti/Si/C mix-
            ture sandwiched between two graphite electrodes, prior
            to ignition at a constant external heating temperature of
            300  C. Strong light emission was observed confirming the   Figure:    Field  emission  scanning  electron  microscope
                o
            flashing event for just 10-15 seconds with a quick rise in   (FESEM) image of (a) flash synthesized Ti SiC MAX phase
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            current flow and temperature with a heating rate of about   showing  typical  compact  layered  structure,  (b)  clearly
                                                              open layered structure of Ti C T  MXene after etching in
            450  C/sec  within  the  sample.  Two-dimensional  Ti C T    HF/H O ,  (c)  well-defined  accordion  like  morphology  of
                o
                                                                                     3 2 X
                                                       3 2 X
            MXene  nanosheets  were  successfully  synthesized  from   multi-layered Ti C T  MXene stack at higher magnification,
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                                                                           3 2 X
            the flash synthesized Ti SiC  MAX phase by oxidant-assist-  (d)  more  expanded  and  well  separated  Ti C T
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                                                                                                         3 2 X
            ed HF etching. The MXene thus obtained exhibited com-  MXene  nanosheets  after  de-lamination  using  TBAOH.
            parable properties to that previously reported from the
            ANNUAL REPORT 2021-22                                                                               49
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