Introduction of Synthesis and Characterization of (CH_3 )_2 NPF_4 “Phosphorene”

Phosphorene is more advance material than graphene, because it possess novel properties including mechanical, chemical and physical properties. The potential application of Phosphorene are in electronic devices. There are two strategies for the preparation of phosphorene including bottom up and top bottom method 1. The first fabrication was done during 2014, by the exfoliation process. The number of publications increased tremendously for the puckered layer structures. The fundamental studies increased due to applications spanning on optoelectronic, electronic, storage devices, and thermoelectric for the energy conversion 2. In literature, focus of studies are associated with the synthesis, layer number determination, applications, tuning of band gap, and anisotropic properties 3.

The present report the comprehensive report is provided for the synthesis, modification method, device applications, structure and properties of phosphorene. The present report deals with inorganic synthesis by the reagents that are  and in the vacuum system. The precise amount of reagents was added to the heavy walled ampule that was sealed with a particular torch.

Experimental of Synthesis and Characterization of (CH_3 )_2  NPF_4 “Phosphorene”

Phosphorene was produced by inorganic synthesis and the reaction was on the smaller scale. The reagents were first purchased and then added to the ampule with the Teflon stopcock instead of an ampule while the particular condition was constriction for the sealed process with the torch 4. The measured amount of 10 m mol of was added to reaction by syringe.

Figure 1: Multilayer phosphorene

Source: https://pubs.acs.org/doi/ipdf/10.1021/acsnano.5b02599 

The reagents used in the experiment are and . The NMR spectroscopic data was added to tabular form for  and the measured properties by the NMR spectroscopic data were chemical shifts () and the coupling constant J.

The NMR spectra was recorded by the SGI/Bruker DRX-400 spectrometer and the solvents used for the analysis were . The chemical shift in the NMR spectra was positive for while the downfield shift in NMR spectra was for . The external references for the spectra are . The elemental analysis and the IR spectra was obtained while the analysis was done by Nicolet 560 IR spectormenter and Carlo Erba Strumentazione CHN elemental analyzer 1106.

In the vacuum system  gas was added with precise pressure as according to the vacuum system. The gas law was used for the calculation of vacuum system. The measured amount of product volume was determined by two consecutive and individual trails. The vacuum system was adjusted on 40/50 joint as muck trap and liquid nitrogen was added to Dewar.

The open manifold for the vacuum pump was measured by McLeod Gauge and the reaction ampule was considered for the vacline. Liquid nitrogen was used to cool the ampule at . And the ampule was opened to the vac system. In order to avoid the condensing of Hg the stopcock and Mcleod guage was attached to the manometer. The last step is trapping process that was done under precise temperature of  and distillation was done by ice-acetone.     

Figure 2: Experimental setup

Results and discussion of Synthesis and Characterization of (CH_3 )_2  NPF_4 “Phosphorene”

The 2D materials are mainly composed of singly polyhedral thick layer or some sort of single atom thick material. The products produced in the middle trap was reweighted in the flask by doing some vacuum transfer. The amount yield by the process and the reaction was 0.95 gram, as detected by C13 spectrum of the produced compound. The Bruker DRX-400 spectrometer was given preference on the JEOL.

The selected frequency of the spectrometer was 100.617 MHz and the scale for the amount measured was ppm 4. The next process was 2 bond determination by the J-PC coupling and the 3 bond J – FC coupling as measured in Hz. The strategical analysis suggests it like a doublet of pentets. The NMR spectra of the produced phosphorene is mentioned below in the appendix as figure 3.    

The reagents used in the production process are of two phases was used in the form of liquid as added in the system by syringe while on the other hand was added in the gaseous form. The quantity of gas was measured and volume of final product was measured by the gas law that is where P represents pressure of gas, V represents volume of the gas, n is the number of moles, R is the universal gas constant and T is the temperature of system in the experiment.