Synthesis of luminescent 2D layered materials using an amine-met al complex and a slow sulfur-releasing precursor
A method of synthesis of two-dimensional (2D) nanoparticles comprises combining a first nanoparticle precursor and a second nanoparticle precursor in one or more solvents to form a solution, followed by heating the solution to a first temperature for a first time period, then subsequently heating the solution to a second temperature for a second time period, wherein the second temperature is higher than the first temperature, to effect the conversion of the nanoparticle precursors into 2D nanoparticles. In one embodiment, the first nanoparticle precursor is a metal-amine complex and the second nanoparticle precursor is a slow-releasing chalcogen source.
1. A method of preparing MoS 2 nanoparticles comprising:
agitating a mixture of molybdenum hexacarbonyl (Mo(CO) 6 ) and degassed oleylamine in a sealed container to produce a suspension of oleylamine/Mo(CO) 6 ;
transferring the suspension of oleylamine/Mo(CO) 6 into a vessel containing degassed oleylamine to form a reaction mixture;
heating the reaction mixture to about 250° C.;
adding a first portion of 1-dodecane thiol (DDT) to the reaction mixture;
heating the reaction mixture at about 250° C. for about 30 minutes;
adding a second portion of 1-dodecane thiol (DDT) to the reaction mixture;
heating the reaction mixture at about 250° C. for about 30 minutes;
then heating the reaction mixture to about 300° C.;
then adding a third portion of 1-dodecane thiol (DDT) to the reaction mixture; and
heating the reaction mixture at about 300° C. for about 30 minutes.
2. The method recited in claim 1 further comprising:
isolating the nanoparticles; and
dissolving the isolated nanoparticles in a solvent.
3. A method of preparing MoS 2 nanoparticles comprising:
agitating a mixture of molybdenum hexacarbonyl (Mo(CO) 6 ), degassed octadecane, and degassed hexadecylamine in a sealed container to produce a first reaction mixture;
heating the reaction mixture to about 150° C. and then cooling the first reaction mixture to room temperature to form a Mo(CO) 6 amine complex;
heating a volume of degassed octadecane to about 300° C.;
warming the Mo(CO) 6 amine complex to about 40° C. to melt any solids;
adding 1-dodecane thiol (DDT) to the warmed Mo(CO) 6 -amine complex to produce a second reaction mixture;
adding the second reaction mixture to the heated volume of degassed octadecane to form a third reaction mixture; and,
heating the third reaction mixture to about 260° C. for about 8 minutes.
4. A method of preparing MoS 2 nanoparticles comprising:
stirring a mixture of molybdenum hexacarbonyl (Mo(CO) 6 ), degassed hexadecane, and degassed hexadecylamine at about 120° C. to produce a first solution;
heating a mixture of hexadecane and hexadecylamine under vacuum at about 80° C. for about one hour and then heating the mixture of hexadecane and hexadecylamine to about 250° C. under N 2 to form a second solution;
adding portions of the first solution maintained at about 120° C. to the second solution about every 5 minutes for about 1 hour to form a third solution; and
adding 1-dodecane thiol (DDT) to the third solution at about 250° C. over a period of about 1 hour.
5. A method of preparing a luminescent composition of matter, the method comprising:
agitating a mixture of molybdenum hexacarbonyl (Mo(CO) 6 ) and degassed hexadecylamine at 40-50° C. in a sealed container to produce a first reaction mixture;
heating the first reaction mixture to about 150° C. to form a Mo(CO) 6 -amine complex;
heating a volume of degassed hexadecylamine to 300° C.;
adding 1-dodecanethiol (DDT) to the first reaction mixture containing the Mo(CO) 6 -amine complex to produce a second reaction mixture;
adding the second reaction mixture to the volume of degassed hexadecylamine heated to 300° C. to produce a third reaction mixture;
adjusting the temperature of the third reaction mixture to about 260° C.;
maintaining the temperature of the third reaction mixture at about 260° C. for about 40 minutes;
then increasing the temperature of the third reaction mixture sufficiently to reflux the hexadecylamine; and
refluxing the third reaction mixture for about 20 minutes to form a precipitate.