The remarkable size and shape dependence of physical, optical, and electronic properties of metal and semiconductor nanocrystals make them compelling components of modern materials chemistry. [1][2][3] When spherical metal particles are transformed into nanoscale rods or triangular prisms, the surface plasmon resonances are strongly affected, typically red-shifting and even splitting into distinctive dipole and quadrupole plasmon modes. 4 Colloid chemists have recently made much progress in preparing monodispersed spherical nanocrystals via ambient temperature wet-chemical routes or organometallic methods. 2 Although the synthesis of spherical nanocrystals is well developed for many materials, systematic manipulation of the shapes of nanocrystals is a significant challenge. Recent work devoted to making nonspherical nanocrystals via anisotropic inorganic nanocrystal growth in liquid media (including electrochemical growth) has yielded Au rods, 5 BaCrO 4 rods, 6 TiO 2 rods, 7 Ag rods, 8 Pt cubes and pyramids, 9 and rod-, arrow-, teardrop-, and tetrapod-shaped CdSe nanocrystals. 10,11 Fabrication of these materials is useful not only for understanding fundamental phenomena such as quantum confinement but also for obtaining "building blocks" featuring optical and electronic properties that are desirable for advanced applications in photovoltaic solar cells, light-emitting diodes, and biological diagnostics. 4,12,13 In contrast to nanorods, nanodisks and nanoprisms such as triangles are less well-known. Although a few strategies do exist for synthesizing Co disks, 14 Ag disks, 15 and Ag triangle nanoprisms, 4,16 there is great interest in developing new methods for making nanoparticles with control over shape and size. Herein, we report a new synthesis of disk-shaped Ag nanoparticles using polystyrene spheres as templates.An aqueous colloidal suspension of carboxylate-functionalized polystyrene (PS) spheres was purchased from Interfacial Dynamics Corporation. Fresh Ag solution containing 10 wt % AgNO 3 and 6% ammonium hydroxide was prepared. Briefly, 160 µL of 110-nm diameter PS spheres and 75 µL of Ag solution were added to 60 mL of somewhat aged N,N-dimethylformamide (DMF). Then, the solution was heated with stirring on a hotplate. Within 8-12 min, the solution color changed from yellow through red to purple, after which the temperature was quickly reduced via a cold-water bath. The product was purified by gradient centrifugation and then kept at 4°C.A rich variety of recipes are now available for making Ag nanoparticles in solution. DMF is one of the standard organic compounds used both as solvent and reducing agent. The reduction of Ag + ions in DMF can take place at room temperature, but the reaction rate is markedly increased at higher temperatures. It is also known that DMF slightly decomposes to a more easily oxidized amine upon aging or upon catalytic decomposition with solid base. The availability of the amine evidently accelerates the reduction of silver ions. (We found that dialkylamines are ineffective ...