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<p>Archaeological bone is a heterogeneous biocomposite that undergoes severe physicochemical degradation after burial, leading to mineral loss, increased porosity, and reduced mechanical strength. Consolidation strategies must therefore restore structural integrity while maintaining chemical compatibility with the native bone mineral and accounting for inherent limitations in reversibility. In this study, four phosphate-based consolidation systems were evaluated on archaeological human bone from the early Islamic–Seljuk period. Treatments included diammonium hydrogen phosphate (DAP) alone and sequential combinations of DAP with calcium hydroxide Ca(OH)₂ and/or magnesium hydroxide Mg(OH)₂ nanoparticles applied via immersion. The treated samples were characterized using field-emission scanning electron microscopy (FESEM), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), porosity analysis, and Vickers microhardness testing. All treatments promoted in situ hydroxyapatite (HAp) formation within the degraded bone matrix, resulting in improved mineral organization and mechanical properties relative to untreated samples. DAP treatment reduced porosity from 80.6% to 48.6% and increased hardness from 34 to 109 HV. Ca(OH)₂ pre-treatment further enhanced mineral precipitation, yielding higher hardness (134 HV) and reduced porosity. Mg(OH)₂ treatment resulted in magnesium-modified hydroxyapatite with comparable porosity reduction but slightly lower hardness (104 HV). The Ca(OH)₂ + Mg(OH)₂ + DAP system showed the highest performance, reducing porosity to 33.6% and increasing hardness to 183.5 HV, accompanied by improved microstructural homogeneity and crystallographic ordering. The results suggest that dual-cation phosphate-based consolidation provides an effective and chemically compatible approach for archaeological bone stabilization. However, in situ hydroxyapatite formation is inherently irreversible, and the absence of long-term aging data and statistical inference should be considered when evaluating the applicability of the method.</p>

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In situ phosphate-based consolidation of archaeological bone: mechanical strengthening using diammonium phosphate and Ca/Mg hydroxides

  • 期刊论文

  • 发表日期：

    2026年6月29日

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  • Danial Harandi,
  • Monireh Moradienayat

摘要

Archaeological bone is a heterogeneous biocomposite that undergoes severe physicochemical degradation after burial, leading to mineral loss, increased porosity, and reduced mechanical strength. Consolidation strategies must therefore restore structural integrity while maintaining chemical compatibility with the native bone mineral and accounting for inherent limitations in reversibility. In this study, four phosphate-based consolidation systems were evaluated on archaeological human bone from the early Islamic–Seljuk period. Treatments included diammonium hydrogen phosphate (DAP) alone and sequential combinations of DAP with calcium hydroxide Ca(OH)₂ and/or magnesium hydroxide Mg(OH)₂ nanoparticles applied via immersion. The treated samples were characterized using field-emission scanning electron microscopy (FESEM), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), porosity analysis, and Vickers microhardness testing. All treatments promoted in situ hydroxyapatite (HAp) formation within the degraded bone matrix, resulting in improved mineral organization and mechanical properties relative to untreated samples. DAP treatment reduced porosity from 80.6% to 48.6% and increased hardness from 34 to 109 HV. Ca(OH)₂ pre-treatment further enhanced mineral precipitation, yielding higher hardness (134 HV) and reduced porosity. Mg(OH)₂ treatment resulted in magnesium-modified hydroxyapatite with comparable porosity reduction but slightly lower hardness (104 HV). The Ca(OH)₂ + Mg(OH)₂ + DAP system showed the highest performance, reducing porosity to 33.6% and increasing hardness to 183.5 HV, accompanied by improved microstructural homogeneity and crystallographic ordering. The results suggest that dual-cation phosphate-based consolidation provides an effective and chemically compatible approach for archaeological bone stabilization. However, in situ hydroxyapatite formation is inherently irreversible, and the absence of long-term aging data and statistical inference should be considered when evaluating the applicability of the method.