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We present a direct electrospinning fabrication technique for the manufacture of PEDOT:PSS/PEO polymer fibers containing embedded cubic lanthanum hexaboride (LaB6) particles. We focus on the impact of relative humidity on the formation of uniform polymer fibers and show that a relative humidity of 5% is optimal, resulting in an average fiber thickness of 266 ± 88 nm. As the relative humidity is increased, the fibers contain beads as a consequence of Rayleigh instabilities. The addition of lanthanum hexaboride cubic particles to the polymer solution before electrospinning results in the encapsulation of the LaB6 particles inside the fibers. We investigate the effect of LaB6 particle size on morphology and observe that particles of ~500 nm yield a fiber-cube-fiber morphology, while 2 μm particles result in fewer embedded cubes along the length of the polymer fibers. This phenomenon likely arises from electrodynamic interactions between the LaB6 particles in the polymer solution and the electric field lines generated during electrospinning between the spinneret and the collector. Our results display the versatility of the electrospinning technique in the fabrication of unique polymer/hexaboride composite fibers.