|
|
|
|
|
|
| Probing Dynamic Interfacial Evolution in Al(OH)3-Coated CaCO3
Composite Materials via Multispectral Synergy |
| XU Yan1, BAO Wei-jun1*, WEI Fu-guang2, JIANG Zong-chen2 |
1. National Engineering Research Center of Green Recycling for Strategic Metal Resources, Institute of Process Engineering, Chinese Academy of Sciences, Beijing 100190, China
2. Hezhou Inspection and Testing Center, Hezhou 542899, China
|
|
|
|
|
Abstract Using ordinary ground calcium carbonate (D50≈38 μm) as the core phase, a CaCO3/Al(OH)3 core-shell composite material was constructed in a supersaturated sodium aluminate solution via heterogeneous nucleation. By multiple spectroscopic techniques, including X-ray diffraction (XRD), scanning electron microscopy-energy dispersive spectroscopy (SEM-EDS), Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy, and X-ray photoelectron spectroscopy (XPS), the dynamic evolution of phase composition, interfacial chemical states, and bonding structures during the coating process was systematically revealed. The coating pathway was regulated by reaction time gradients (2 h, 12 h, 36 h). Combined with SEM-EDS cross-sectional morphology analysis and XRD phase identification, a three-layer model of the core-shell structure was established: a calcite-type CaCO3 core (≈38 μm), a C3AH6 intermediate layer (300～500 nm), and a dense Al(OH)3outer shell, following a stepwise reaction path of “CaCO3→C3AH6→Al(OH)3”. FTIR and Raman spectra further corroborated the interfacechemical bonding path: FTIR detected the characteristic OH stretching vibration peak of C3AH6 at 3 664 cm-1, while Raman identified additional lattice vibration modes of C3AH6 in the 3 390～3 640 cm-1 range, collectively confirming chemical bonding (via Ca—O—Al bonds) rather than physical mixing between calcium and aluminum. XPS quantitative analysis demonstrated that the surface Ca/Al molar ratio decreased from 1.45 at 2 h (close to the theoretical value of 1.5 for C3AH6) to 0.08 at 36 h. Combined with the Ca(2p) binding energy shift and the Al(2p) chemical state transition (Al—O→Al—OH), this directly revealed the dynamic formation of the C3AH6 intermediate phase and the coverage mechanism of the Al(OH)3 shell. The innovation of the multispectral coupling strategy lies in: achieving phase-morphology collaborative characterization through XRD/SEM-EDS, analyzing bonding structure evolution with FTIR/Raman, and quantitatively tracking surface chemical state migration with XPS. This integrated approach overcomes the limitations of single-technique characterization and systematically elucidates the pivotal role of the C3AH6 intermediate phase in interfacial bonding. The study provides a theoretical foundation for the controllable synthesis of core-shell composites. For instance, optimizing the Al(OH)3 shell thickness (300～500 nm) and uniformity by adjusting the sodium aluminate concentration and reaction time can enhance the material's weathering resistance and interfacial compatibility. Through multidimensional synergy of spectroscopic techniques, this work establishes a critical theoretical basis for the interfacial chemical regulation and industrial applications of CaCO3/Al(OH)3 composites.
|
|
Received: 2025-05-26
Accepted: 2025-09-23
|
|
|
|
Corresponding Authors:
BAO Wei-jun
E-mail: wjbao@ipe.ac.cn
|
|
[1] Song X W, Liu H, Wang J F, et al. CrystEngComm, 2021, 23(24): 4284.
[2] Amanda Gerhardt de Oliveira, Janaina Fernandes Moreno, Ana Maria Furtado de Sousa, et al. Polymer Bulletin, 2020, 77: 2889.
[3] Shen J, Song Z Q, Qian X R, et al. Carbohydrate Polymers, 2010, 81(3): 545.
[4] Hedayatollah Sadeghi Ghari, Azam Jalali-Arani. Applied Clay Science, 2016, 119: 348.
[5] Fırat Karaka瘙塂, Behzad Vaziri Hassas, Mehmet S Çelik. Progress in Organic Coatings, 2015, 83: 64.
[6] Hanna Koivula, Martti Toivakka, Patrick Gane. Journal of Colloid and Interface Science, 2012, 369(1): 426.
[7] Zhang S C, Li X G. Powder Technology, 2004, 141(1-2): 75.
[8] YUE Lin-hai, CAI Ju-xiang, HUA Yi-miao(岳林海, 蔡菊香, 华益苗). Journal of Zhejiang University (Science Edition)[浙江大学学报(理学版)], 2002，(1): 67.
[9] Tao H, He Y Y, Zhao X. Powder Technology, 2015, 283: 308.
[10] GAO Hong-xia, XU Yang，FU Mao-gang, et al(高洪霞, 徐 洋, 付茂刚, 等). China Pulp & Paper (中国造纸), 2016, 35(9): 21.
[11] Ota Y, Iwashita T, Kasuga T, et al. Journal of the Ceramic Society of Japan, 1997, 105(5): 374.
[12] DING Xiao-chu, YUE Lin-hai, JIN Da-lai(丁孝初, 岳林海, 金达莱). Chinese Journal of Inorganic Chemistry(无机化学学报), 2005, 21(6): 879.
[13] ZHANG Hui-zhu, JIN Da-lai, YUE Lin-hai(张惠珠, 金达莱, 岳林海). Journal of Zhejiang University (Science Edition)[浙江大学学报(理学版)], 2008，(4): 422.
[14] LI Xiao-bin, ZHENG Jie, QI Tian-gui, et al(李小斌, 郑 洁, 齐天贵, 等). Journal of Central South University (Science and Technology)[中南大学学报(自然科学版)], 2013, 44(7): 2663.
[15] Andrey V Porsin, Vladimir N Rogoznikov, Alexander V Kulikov, et al. Crystal Growth and Design，2017, 17(9): 4730.
[16] LI Yuan-yuan, RONG Jian-xin, ZHANG Qing-xin(李媛媛, 戎建鑫, 张庆新). Chinese Journal of Colloid & Polymer(胶体与聚合物), 2020, 38(4): 165.
[17] ZHANG Bin, XIAO Xiao, HAN Yun-jiao, et al(张 彬, 肖 霄, 韩芸娇, 等). Inorganic Chemicals Industry(无机盐工业)，2021, 53(1): 97.
[18] JIN Da-lai, YUE Lin-hai, XU Zhu-de(金达莱, 岳林海, 徐铸德). Chinese Journal of Inorganic Chemistry(无机化学学报), 2004, 20(6): 715.
[19] Hidalgo A, García J L, Alonso M C, et al. Journal of Thermal Analysis and Calorimetry, 2009, 96(2): 335.
[20] Gevers B R, Labuschagné F J W J. Crystals, 2020, 10(8): 672.
[21] YU Hai-yan, LI Wen-cheng, BI Shi-wen, et al(于海燕, 李文成, 毕诗文, 等). Journal of Northeastern University (Natural Science)[东北大学学报(自然科学版)], 2010，(7): 995.
[22] Zhang Wenshuang, Li Xinyong, Qu Zhenping, et al. Materials Letters, 2010, 64(1): 71.
[23] Baer D R, Marmorstein A M, Williford R E, et al. Surface Science Spectra, 1992, 1(1): 80. |
| [1] |
PENG Jian-wen1, XIAO Chong1, SONG Qiang1, PENG Zhong-chao1, HUANG Ruo-sen1, YANG Ya-dong3, TANG Gang1, 2, 3*. Flame Retardant Mechanism Investigation of Thermoplastic Polyurethane Composite/Ammonium Polyphosphate/Aluminum Hydroxide Composites Based on Spectroscopy Analysis[J]. SPECTROSCOPY AND SPECTRAL ANALYSIS, 2021, 41(12): 3901-3908. |
|
|
|
|
