層狀複金屬氫氧化合物(LDHs)具層狀結構、層間陰離子可交換與金屬組成可調等特性，廣泛應用於碳捕集、電催化與磁性材料。本研究以Ni–Fe LDHs為核心，建立「增量製備→TEPA官能化CO₂吸附→泡沫鎳披覆產氫→高溫轉相NiFe₂O₄磁性材料」之整合驗證流程，並比較Ni:Fe＝2:1、2.5:1、3:1。製備方面以鐵氟龍瓶水熱取代高壓釜，經SEM/XRD證實片狀形貌與結晶相一致，單批產量由4 g提升至40 g。CO₂吸附方面以TEPA改質，TGA顯示TEPA含量達到20 wt%表現最佳，其中2:1吸附量達0.389 g CO₂/g LDH。產氫方面將LDHs披覆於泡沫鎳，定電流10 mA長時測試顯示披覆可提升產氫並延緩劣化；2:1於9 h產氫約30 mL(較裸泡沫鎳提升約 11%)，並可穩定至15 h以上達50 mL。GC檢測證實產氣峰與氫氣標準一致且無明顯雜質；EIS檢測顯示披覆後界面電荷轉移阻抗降低，2:1於反應前後皆呈最小半圓，對應最佳產氫與耐久性。磁性應用方面，LDHs於1000°C並持溫燒結5分鐘後會轉相變為尖晶石NiFe₂O₄，並雷射披覆於不鏽鋼；XRD檢測則顯示保有NiFe₂O₄特徵峰，SQUID檢測顯示2:1比例的LDHs磁性最強，披覆後試片飽和磁矩提升至約0.34 emu。綜合結果證實Ni:Fe＝2:1時在CO₂吸附、產氫與磁化效果具最佳整體表現，提供後續碳捕集、鹼性水電解與磁性功能塗層工程化開發基礎。

Layered double hydroxides (LDHs) possess a layered structure, interlayer anion exchangeability, and tunable metal compositions, enabling broad applications in carbon capture, electrocatalysis, and magnetic materials. In this study, Ni–Fe LDHs were used as the core material to establish an integrated validation workflow of “scale-up synthesis → TEPA functionalization for CO₂ adsorption → hydrogen evolution via coating on nickel foam → high-temperature phase transformation to NiFe₂O₄ magnetic material,” and the performance of Ni:Fe = 2:1, 2.5:1, and 3:1 was compared. For synthesis, a Teflon-bottle hydrothermal method was adopted to replace conventional autoclaves; SEM/XRD confirmed consistent platelet-like morphology and crystalline phases, and the batch yield increased from 4 g to 40 g. For CO₂ capture, TEPA modification was applied, and TGA indicated that 20 wt% TEPA provided the best performance; the 2:1 sample achieved a CO₂ uptake of 0.389 g CO₂/g LDH. For hydrogen production, coating LDHs on nickel foam under a constant current of 10 mA enhanced hydrogen evolution and mitigated degradation during long-term operation. The 2:1 sample produced approximately 30 mL H₂ at 9 h (about 11% higher than bare nickel foam) and remained stable beyond 15 h, reaching 50 mL. GC confirmed that the gas peak matched the hydrogen standard with no significant impurities, while EIS showed reduced interfacial charge-transfer resistance after coating; the 2:1 sample exhibited the smallest semicircle both before and after reaction, consistent with the best hydrogen evolution and durability. For magnetic applications, LDHs were transformed into spinel NiFe₂O₄ by sintering at 1000°C for 5 min and then laser-coated onto stainless steel. XRD retained characteristic NiFe₂O₄ peaks, and SQUID measurements showed that the 2:1 ratio exhibited the strongest magnetism, with the coated specimen reaching a saturation magnetization of ~0.34 emu. Overall, Ni:Fe = 2:1 delivered the best combined performance in CO₂ adsorption, hydrogen evolution, and magnetization, providing a basis for further engineering development in carbon capture, alkaline water electrolysis, and magnetic functional coatings.

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