Process for the synthesis of nanoparticles of transition metal chalcogenides
View Patent ↗A process for the synthesis of transition metal chalcogenides (TMC) having formula (I). More particularly, the present work relates to a one pot single phase process for the synthesis of a TMC system having formula (I) by wet chemistry. Formula (I) is represented as A x -B y .
1. A one pot single phase process for the synthesis of a transition metal chalcogenide nanoparticle system having formula (I) by using wet chemical method, the process comprising:
mixing and stirring both a transition metal precursor and a chalcogen precursor at a temperature in a range of 25° C. to 30 C in the presence of a reducing agent and an accelerating agent under a blanket of an inert gas; followed by raising and maintaining the temperature in the range of 100-150° C. for a time period of 30 min and slowly increasing the temperature to 300° C. by heating at rate of 2°/min or 5° C./min or 10° C./30 min
to obtain the transition metal chalcogenide nanoparticle system having formula (I),
wherein the formula (I) is represented as
A x -B y Formula (I)
wherein,
A is selected from the group consisting of iron, chromium, manganese, cobalt, and nickel;
B is selected from the group consisting of selenium, sulphur, and tellurium; and
A x -B y is selected from the group consisting of AB 2 , A 3 B 4 , A 7 B 8 and AB;
wherein the ratio of x and y is from 1:2 to 1:1,
provided that when A is Fe and B is Se, then the system is not AB;
provided that the chalcogen precursor is Se powder.
2. The process as claimed in claim 1 , wherein said system of formula (I) is selected from the group consisting of FeSe 2 , Fe 3 Se 4 , Fe 7 Se 8 , Co 3 Se 4 , Ni 3 Se 4 and MnSe.
3. The process as claimed in claim 1 , wherein the size of as-synthesized transition metal chalcogenide nanoparticle is in the range of 5 nm to 350 nm.
4. The process as claimed in claim 1 , wherein the shape of as-synthesized transition metal chalcogenide nanoparticle is selected from the group consisting of nano-rod, nano-sphere, nano-sheet, nano-platelet, nano-cube and mixed shape.
5. The process as claimed in claim 1 , wherein the reducing agent is selected from the group consisting of oleylamine, oleic acid, 1-octadecene, octadecylamine, oleyl alcohol, pentylamine, ethylamine and n-octadecane.
6. The process as claimed in claim 1 , wherein the accelerating agent is selected from the group consisting of 1-octadecene, oleic acid, oleylamine, octadecylamine, oleyl alcohol, pentylamine, and ethylamine.
7. The process as claimed in claim 1 , wherein the transition metal precursor is selected from the group consisting of tris(acetylacetonato) iron (III), cobalt (III) acetylacetonate, nickel(II) acetylacetonate, and manganese(III)acetylacetonate.
8. A one pot single phase process for the synthesis of transition metal chalcogenides nanoparticles system wherein said system is Fe—Se system comprising the steps of:
a) mixing Se powder and Fe(acac) 3 at a temperature in the range of 25° C. to 30° C. in the presence of an organic solvent under the blanket of inert gas with constant magnetic stirring;
raising the temperature to 40° C. followed by stirring for 30 min and taking the first sample of only Se powder;
c) further increasing the temperature to 50° C. followed by stirring for 30 min and taking the second sample of only Se powder; and
d) increasing the temperature up to 340° C. with the rate of 10° C./30 min and taking the sample at every 10° C. rise in temperature, as the temperature increases,
wherein FeSe 2 starts forming followed by Fe 3 Se 4 , Fe 7 Se 8 and FeSe.
9. The process as claimed in claim 8 , wherein said organic solvent is selected from the group consisting of oleylamine; oleylamine and 1-octadecene; and oleylamine and pre-dissolved Se powder in 1-octadecene.