According to the U.S. Energy Information Administration, solar and wind make up over two-thirds of the 39.7 giga-watts (GW) of new energy capacity added to the grid in 2021. In addition, wind turbine service technicians and solar panel installers are ranked number one and number three respectively on the U.S. Bureau of Labors "Fastest Growing Occupations for 2019-2029". However, currently solar panels require energy-consuming manufacturing processes, are limited to inflexible substrates, and only convert around 20-30% of light into electricity. Many new alternative materials for solar cells emerged with in the past few decades with low-cost solution processing, the ability to print onto flexible substrates, and the potential to convert higher percentages of light into electricity. However, most studies focus on the improvements in performance without studying the impact that changing processing conditions and adding dopants has on the vertical composition and crystalline structure of the material. Here, we study the structural characteristics of different photovoltaic materials to determine the impact of different processing methods and dopants. First, we investigate the vertical composition in solution processed photovoltaic semiconductor materials. While solution-processed solar cells offer a low-cost and less energy consuming manufacturing method, the processing materials and method highly impact the performance of the solar cell. In Chapter 2, we investigate how changes in processing photovoltaic thin-films impacts the film morphology and vertical composition of the film. We use glow discharge optical emission spectroscopy (GDOES) coupled with scanning electron microscopy (SEM) to analyze changes in film morphology. We look at three types of semiconductor materials: polymer/quantum dot blends, kesterite, and chalcopyrite. In polymer/quantum dot blends use GDOES to confirm the depth composition from a three-dimensional reconstruction using discrete algebraic reconstruction technique (DART) from scanning electron microscopy images. We discover that a post-deposition ligand exchange directly from the native quantum dot ligands to shorter, electrically conducting ligands results in damage to film causing cracks and voids. However, using a solution-based exchange to an intermediary ligand before a post-deposition ligand prevents damage to the film and results in better device performance. Next, we use GDOES to show that Ag-doping in kesterite films results in a more homogenous composition throughout the film depth and reduces the voids in the film. Finally, we discover that the selenization copper-rich under higher pressure allows results in films with fewer voids and Na-passivated defects. Overall, we see that processing conditions impact the vertical composition and can change the performance of photovoltaic materials. In addition to changes from processing conditions, changes in material properties can be induced by doping the material. In Chapter 3, we investigate how doping changes the structure of methylammonium lead tribromide (MAPbBr3) single crystals. We observe a shift in the structural phase transition temperature as a result of bismuth incorporation into the crystal structure. Using x-ray diffraction, we discover a contraction in the lattice constant with increase bismuth concentration. We compare the lattice contraction to the effects of applying external pressure to MAPbBr3 and observe a similar shift to lower temperatures for the phase transition. We use density functional theory (DFT) simulations and determine the likely defect species to be BiPb+. In our final chapter, we investigate the impacts of a remote outreach activity on student knowledge and attitudes towards science. We use pre/post-activity surveys to evaluate changes in student understanding of Next Generation Science Standards (NGSS) aligned content about the relationship between energy production and the environment. We also use 5-point Likert-scale surveys to measure student attitudes towards STEM/STEM careers. We use quantitative statistical analysis methods such as Welch’s t-test, Mann-Whitney U test, and Wilcoxon Signed Ranked test to determine the significance of changes between pre/post-activity surveys. We find an increase in the probability of students identifying wind, hydropower, and nuclear energy as renewable resources on the post-survey. Similarly, for non-renewable resources we find an increase in the probability that students identify fossil fuels, gas, and nuclear on the post-activity survey. We observe no changes in student attitudes towards STEM/STEM careers between pre/post survey. However, we determine that teachers over-estimated the changes in student attitudes from the outreach activity. We also observe an interesting result in the post-activity surveys with a higher mean response for “I enjoyed this [outreach] activity” and compared to the mean response for “I enjoy science and engineering activities”. This discrepancy in student attitudes should be further studied, however this provides insight in how we can improve student attitudes towards science and engineering activities.