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Intumescent fire-retardants (IFR) are widely applied in fire protection coatings of steel and wooden structures. The addition of inorganic fillers, such as layered ionic clays, can improve the fireproof performance of IFR coatings. However, a fundamental insight of how these filler materials synergistically interact with the IFR materials remains elusive. In this study, we address this fundamental knowledge gap by systematically investigating the synergy between the IFR fire protection coatings and the CaAlCO 3 -layer double hydroxide (LDH) or montmorillonite (MMT) fillers, which render substantially longer fire resistance (>20 min), reduced specific extinction area (by 54.7 and 44.1 m2 kg−2, respectively), and reduced heat release (by 0.9 and 0.7 MJ m−2, respectively). Combining experimental results and density functional theory calculations, we show for the first time that the superior fireproof performance of the MMT-IFR fire coating originates from the chemical modifications of the char layer by Si-doping. The chemical stabilisation of the silicon- and nitrogen-doped graphene (Si–N-G) structures improves the oxidation resistance of the char layer. Additionally, the formation of the Si–N-G structures with limited lattice deformation stabilised the porous morphology of the char layer, thereby promoting its heat-shielding performance. [Display omitted] [ABSTRACT FROM AUTHOR]

[Display omitted] • An IFR containing acid, carbon, and gas sources was prepared by in-situ calcination. • HRR, EHC, THR, and TOC of fabric with IFR were less than those without IFR. • Carbonization process and fireproof mechanism of IFR on fabric were studied. A novel macromolecular carbon-nitrogen-phosphorous (C-N-P) intumescent flame retardant (IFR) containing acid, carbon, and gas sources was prepared by calcining polyphosphate (APP), pentaerythritol (PER), and melamine (MEL) through the direct heating method. The carbonization and expansion behaviors of IFR were investigated by testing the products of IFR, using nuclear magnetic resonance, X-ray photoelectron spectroscopy, transmission electron microscope, and scanning electron microscopy, at 360 °C, 450 °C, and 600 °C. Conjugated double bonds polymerized the nitrogenous polyaromatic structures as polyphosphate decomposed into phosphoric acid and diphosphate. Noncombustible gases released by MEL increased the internal pressure of the viscoelastic materials to make it expand. At temperatures below 450 °C, MEL promotes the formation of nitrogenous polyaromatic structures in the material, thereby optimizing the IFR char layer structure. The heat release rate, effective heat combustion, total heat release, and total oxygen consume of the IFR coated fabric were less than those of an uncoated fabric by 18%, 5%, 16%, and 13%, respectively, reducing the risk of fire hazard. The foam char formed during the burning of an IFR coated fabric controls the fabric's oxidation process and prevents its shrinking. [ABSTRACT FROM AUTHOR]

• The addition of MgAlCO 3 -LDHs to the IFR coating effectively reduced the TSP and SPR from the cone calorimetry. • Thermal decomposition of MgAlCO3-LDHs could promote and catalyze esterification between APP and PER. • The C-N-P-MgAl coating could improve the thermal insulation performance of the char layer. MgAlCO 3 -layered double hydroxides (MgAlCO 3 -LDHs) were introduced in a waterborne intumescent fire retardant (IFR) with nano-coating containing ammonium polyphosphate (APP), pentaerythritol (PER), and melamine (MEL). The effects of MgAlCO 3 -LDHs were evaluated based on thermogravimetry (TG), differential thermal analysis (DTA), Fourier transform infrared spectroscopic analyses (FT-IR), X-ray power spectroscopy (XPS), scanning electron microscopy (SEM), fire performance test, and cone calorimetry. The 1.8 wt% of MgAlCO 3 -LDHs added to the IFR coating promoted the expansion of the char layer to improve its thermal insulation performance during the fire performance test. The results characterized by TG, DTA, XPS, and FT-IR revealed that MgAlCO 3 -LDHs enhanced the residual weight, the thermal stability and the oxidation resistance of the IFR coating. There was statistical evidence that the heat-shielding performance was reinforced by adding an appropriate amount of MgAlCO 3 -LDHs to the IFR coating to form uniform and compact foams in the char layer by using the digital image to process SEM images. The cone calorimetry revealed that a 46% reduction in total smoke production (or total smoke release) and a 25% decrease in the smoke production ratio were achieved in the coating with added MgAlCO 3 -LDHs compared with that without. It can be concluded that the addition of MgAlCO 3 -LDHs to IFR coating actively interacts with APP, PER, and MEL, thus improving the fire retardant properties of the coating. [ABSTRACT FROM AUTHOR]

• Addition of MgAlCO 3 -LDHs and CaAlCO 3 -LDHs improved thermal insulation of IFR coating. • Metal ions from LDHs were chelated with carbon materials to form 3D reticular char. • LDHs can delay oxidation and improve degradation performance of char layers. MgAlCO 3 -layered double hydroxides (LDHs) and CaAlCO 3 -LDHs were respectively added as a synergistic agent to intumescent fire retardant (IFR) coatings. The 2.4 wt% of MgAlCO 3 -LDHs and the 6.7 wt% of CaAlCO 3 -LDHs were found to possess the best thermal insulation according to the fire performance tests. Further characterization by a cone calorimeter shows that the MgAlCO 3 -LDHs are superior to decreasing the specific extinction area of IFR coating, and the CaAlCO 3 -LDHs are advantageous in some other properties such as heat release rate, effective heat combustion and total heat release. Moreover, the X-ray diffraction (XRD) results infer that the flame retardant of char layer is primarily dependent on the amorphous structure formed after exposure to fire, the X-ray photoelectron spectroscopy (XPS) measurements of O 1s , C 1s , P 2p and N 1s reveal that the LDHs fillers suppress the oxidation of the IFR coating, and the Fourier transform infrared spectroscopy (FTIR) tests demonstrate that the LDHs protect the bridge frame structures. It is concluded that the LDHs can prevent the degradation and improve the thermal insulation of IFR coatings. [ABSTRACT FROM AUTHOR]

• An analysis method for SEM images of intumescent fire retardant char layers is proposed. • Foams in an intumescent fire retardant char layer are characterized quantificationally. • Appropriate addition of CaAlCO 3 -LDHs makes the char layer compact and uniform. • Unsatisfactory result image after color transformation is returned to object segmentation. A new characterization method is proposed to investigate the microscopic morphology of intumescent fire retardant (IFR) char layer observed under a scanning electron microscope (SEM). The method consists of object segmentation extracting the object, color transformation improving the recognition of subtle details, and statistical analysis obtaining the features (area, average, and standard deviation) of the object in the SEM images. There is a descending trend in the standard deviation of the foams with the increase of CaAlCO 3 -LDHs (layered double hydroxides) added to the coatings. Specifically, the number of the foams in the IFR coating with 5 wt% of CaAlCO 3 -LDHs addition is increased from 102 (that of the char layer without CaAlCO 3 -LDHs) to 123. Meanwhile, the standard deviation of the foams in the char layer is decreased from 6383.6 to 4304.5, demonstrating that an appropriate addition of CaAlCO 3 -LDHs can improve the foam quality of the IFR coating by making it more compact and uniform, and enhance the thermal insulation of the char layer covered on the substrate surface. [ABSTRACT FROM AUTHOR]