COMPOSITE PARTICLES AND METHODS OF MANUFACTURE THEREOF
The present disclosure is generally directed to composite particles which include a matrix material having an innate matrix porosity having matrix pores; and a plurality of additive particles disposed within the matrix material. The present disclosure is further directed to methods of preparing such composite particles.
1 . A method of preparing composite particles comprising a matrix material and a plurality of functional particles disposed within the matrix material, and wherein the composite particles comprise an exterior surface region, the method comprising:
providing a solution of one or more matrix material precursors in a solvent;
suspending functional particles in the solution to form a suspension;
adding a first gelation agent to the solution, initiating formation of an organogel;
combining the suspension with an immiscible liquid to form a mixture;
emulsifying the mixture to provide a plurality of droplets, wherein each droplet in the plurality comprises a plurality of the functional particles;
adding a second gelation agent to the solution, continuing formation of the organogel; and
optionally, drying the organogel particles.
2 . The method of claim 1 , wherein the functional particles are electrochemically active.
3 . The method of claim 2 , wherein the functional particles comprise silicon, germanium, tin, or a combination thereof.
4 . The method of claim 1 , wherein the immiscible liquid is mineral spirits or a silicone oil.
5 . The method of claim 1 , wherein the organogel comprises a polyamic acid, a polyimide, or a combination thereof.
6 . The method of claim 5 , wherein the first gelation agent is acetic anhydride and the second gelation agent is acetic acid.
7 . The method of claim 6 , wherein the composite particles comprise a central region extending from a center of the composite particle outward toward the exterior surface region, wherein the central region comprises more functional particles than the exterior surface region.
8 . The method of claim 6 , wherein the first gelation agent creates a viscosity gradient within the droplets, and wherein the viscosity gradient forces functional particles toward a center of the droplets, such that the exterior surface region of the composite particles has a deficit of functional particles relative to the central region.
9 . The method of claim 1 , further comprising calcining the organogel particles under an inert atmosphere at a temperature of at least about 650° C.
10 . The method of claim 9 , wherein the calcining isomorphically converts substantially all of the organogel to carbon.
11 . The method of claim 1 , wherein the exterior surface region has a thickness in a range from about 0.1% to about 25% of a diameter of the composite particles.
12 . The method of claim 1 , wherein a thickness of the exterior surface region varies along an exterior surface of the composite particle.
13 . The method of claim 1 , wherein the composite particle comprises surface depressions projecting from an outer surface of the particle into the exterior surface region, and wherein said surface depressions comprise one or more functional particles.