Advanced carbon materials used for energy-related applications often contain nitrogen as a heteroatom, which can substantially influence their physical, chemical, and electronic properties. However, conventional analytical techniques for nitrogen environments provide limited compositional and structural information in high sensitivity, which significantly restricts rationalized materials design. Herein, we present the advanced temperature-programmed desorption (TPD) technique up to 2,100°C as a comprehensive analytical tool for chemical speciation in bulk nitrogen-doped carbon materials with record-high sensitivity. Employing complementary X-ray photoelectron spectroscopy, elemental analysis, and computational modeling, we discovered that the gas emission patterns can provide both compositional and structural information regarding nitrogen environments. Importantly, TPD enables the bulk quantification of nitrogen species at 10 ppm levels, which is two orders of magnitude more sensitive than conventional methods. Such an advanced characterization method provides a foundation for next-generation research, focusing on the structural design at the ppm level, and offers significant potential for industrial applications.

用于能源相关应用的先进碳材料通常含有氮作为杂原子，这会极大地影响其物理、化学和电子性能。然而，传统的氮环境分析技术在高灵敏度下提供的成分和结构信息有限，这极大地限制了合理的材料设计。在此，我们提出了高达 2,100°C 的先进程序升温解吸 (TPD) 技术，作为一种综合分析工具，用于分析块状氮掺杂碳材料中的化学形态，具有创纪录的高灵敏度。采用互补的 X 射线光电子能谱、元素分析和计算模型，我们发现气体排放模式可以提供有关氮环境的成分和结构信息。重要的是，TPD 能够对 10 ppm 水平的氮物质进行批量定量，这比传统方法灵敏两个数量级。这种先进的表征方法为下一代研究奠定了基础，重点关注 ppm 级的结构设计，并为工业应用提供了巨大的潜力。