Bulk synthesis of nanoporous palladium and platinum powders
View Patent ↗Disclosed is a method for providing nanoporous palladium and platinum powders. These materials were synthesized on milligram to gram scales by chemical reduction of tetrahalo-complexes with ascorbate in a concentrated aqueous surfactant at temperatures between −20° C. and 30° C. The prepared particles have diameters of approximately 50 nm, wherein each particle is perforated by pores having diameters of approximately 3 nm, as determined by electron tomography. These materials are of potential value for hydrogen and electrical charge storage applications.
1. A method for providing a finely divided platinum metal powder, comprising the steps of:
a. forming a first paste, comprising a first aqueous mixture of an ammonium or an alkali metal tetrachloroplatinate, hydrochloric acid and a polyethylene glycol hexadecyl ether surfactant;
b. forming a second paste comprising a second aqueous mixture of ammonium hydroxide and ascorbic acid and a polyethylene glycol hexadecyl ether surfactant;
c. kneading the first and second pastes together on a surface to form a mixed paste;
d. forming a liquid suspension of the mixed paste in a heated polar solvent;
e. separating the liquid suspension into a precipitated solid and a supernatant;
f. recovering the precipitated solid; and
g. drying the precipitated solid in a vacuum or an inert atmosphere thereby providing a finely divided powder of platinum metal.
2. The method of claim 1 , wherein the step of forming the first paste further comprises the steps of:
a. dissolving a first quantity of an ammonium or an alkali metal tetrachloroplatinate into a first volume of water together with more than one equivalent of hydrochloric acid to provide a first aqueous mixture;
b. heating the first aqueous mixture to about 80° C. to form a first solution;
c. melting a first quantity of a polyethylene glycol hexadecyl ether surfactant and adding it to the first solution to provide a second aqueous mixture;
d. agitating the second aqueous mixture to form a first paste;
e. heating the first paste to about 80° C. to form a viscous liquid; and
f. repeating steps d.) and e.) until the viscous liquid is rendered homogeneous.
3. The method of claim 1 , wherein the step of forming the second paste further comprises the steps of:
a. dissolving a first quantity of ammonium hydroxide and ascorbic acid into a second quantity of water to provide a third aqueous mixture;
b. heating the third aqueous mixture to about 80° C.;
c. melting a quantity of a polyethylene glycol hexadecyl ether surfactant and adding it to the third aqueous mixture to form a reductant mixture;
d. agitating the reductant mixture to form a second paste;
e. heating the second paste to about 80° C. to form a viscous reducing liquid; and
f. repeating steps d.) and e.) until the viscous reducing liquid is rendered homogeneous.
4. The method of claim 1 , wherein the steps of forming a liquid suspension of the mixed paste separating the liquid suspension into a precipitated solid and a supernatant and recovering the precipitated powder comprise the steps of:
a. adding a quantity of ethanol to the mixed paste and heating ethanol/mixed paste combination to about 80° C.;
b. mixing and agitating the ethanol/mixed paste combination to dissolve the mixed paste providing thereby a liquid suspension;
c. separating the liquid suspension into a precipitated solid and a supernatant;
d. decanting the supernatant;
e. resuspending the precipitated solid in water to form an aqueous suspension and heating the aqueous suspension to about 80° C.;
f. repeating steps c.) and d.); and
g. repeating steps a.) through d.).
5. The method of claim 1 , wherein the steps of forming a liquid suspension of the mixed paste separating the liquid suspension into a precipitated solid and a supernatant and recovering the precipitated powder comprises the steps of:
a. adding a quantity of a solvent solution comprising ethanol and water to the mixed paste and heating this solvent solution-mixed paste combination to about 80° C.;
b. mixing and agitating the solvent solution-mixed paste combination to dissolve the mixed paste thereby providing a liquid suspension;
c. separating the liquid suspension into a precipitated solid and a supernatant;
d. decanting the supernatant; and
e. repeating steps a.) through d.).
6. The method of claim 5 , wherein the solvent solution comprises 3 parts by volume ethanol to 1 part by volume water.