Sintering Behavior and Microstructure of diphasic β-Sialon/Al2O3 Composites

Six compositions with different ratio of β-Sialon/Al₂O₃ were synthesized from Al₂O₃, Si₃N₄ and SiO₂ by sintering with 3%Y₂O₃(mass fraction) as addition under the cover with powders of SiC+C and at nitrogen atmosphere. Theeffects of atmosphere, sintering temperature and composition on the sintering behavior were studied. The results showedthat the composites reached the best sintering behavior with the highest density about 92% at 1 650℃ under the weakreduction atmosphere. Finally the relative density of diphasic β-Sialon and β-Sialon/Al₂O₃ composites were studied andpredicted using ANN (Artificial Neural Networks) method and the results were experimental examined by fore randomsamples.     

Novelty phase synthesis mechanism and morphology in resin-bonded Al-Al2O3-TiO2 composites at high temperatures under flowing N2

An Al-AlN core-shell structure is beneficial to the performance of Al-Al₂O₃ composites. In this paper, the phase evolution and microstructure of Al-Al₂O₃-TiO₂ composites at high temperatures in flowing N₂ were investigated after the Al-AlN core-shell structure was created at 853 K for 8 h. The results show that TiO₂ can convert Al into Al₃Ti (~1685 K), which reduces the content of metal Al and rearranges the structure of the composite. Under N₂ conditions, Al₃Ti is further transformed into a novelty non-oxide phase, TiCN. The transformation process can be expressed as follows:Al₃Ti reacts with C and other carbides (Al₄C₃ and Al₄O₄C) to form TiC_x (x < 1). As the firing temperature increases, Al₃Ti transforms into a liquid phase and produces Ti(g) and TiO(g). Finally, Ti(g) and TiO(g) are nitrided and solid-dissolved into the TiC_x crystals to form a TiCN solid solution.     

In situ reaction mechanism of MgAlON in Al–Al_2O_3–MgO composites at 1700°C under flowing N_2

The Al–Al_2O_3–MgO composites with added aluminum contents of approximately 0wt%, 5wt%, and 10wt%, named as M_1, M_2, and M_3, respectively, were prepared at 1700°C for 5 h under a flowing N_2 atmosphere using the reaction sintering method. After sintering, the Al–Al_2O_3–MgO composites were characterized and analyzed by X-ray diffraction, scanning electron microscopy, and energy-dispersive X-ray spectroscopy. The results show that specimen M_1 was composed of MgO and MgAl_2O_4. Compared with specimen M_1, specimens M_2 and M_3 possessed MgAlON, and its production increased with increasing aluminum addition. Under an N_2 atmosphere, MgO, Al_2O_3, and Al in the matrix of specimens M_2 and M_3 reacted to form MgAlON and AlN-polytypoids, which combined the particles and the matrix together and imparted the Al–Al_2O_3–MgO composites with a dense structure. The mechanism of MgAlON synthesis is described as follows. Under an N_2 atmosphere, the partial pressure of oxygen is quite low; thus, when the Al–Al_2O_3–MgO composites were soaked at 580°C for an extended period, aluminum metal was transformed into AlN. With increasing temperature, Al_2O_3 diffused into AlN crystal lattices and formed AlN-polytypoids; however, MgO reacted with Al_2O_3 to form MgAl_2O_4. When the temperature was greater than(1640 ± 10)°C, AlN diffused into Al_2O_3 and formed spinel-structured AlON. In situ MgAlON was acquired through a solid-solution reaction between AlON and Mg Al_2O_4 at high temperatures because of their similar spinel structures.     

Thermodynamic analysis and preparation of β-SiC/ZrO2 composites

A predominance area diagram for the Zr-Si-C-O system at 1773 K was plotted according to correlative thermodynamic data. β-SiC/ZrO₂ composites were prepared based on the phase diagram by carbothermal reduction of zircon (ZrSiO₄) in argon atmosphere. Zircon and carbon black were mixed according to the C/ZrSiO₄ mass ratio of 0.2, and with 0, 1wt% and 2wt% extra addition of La₂O₃. Phase evolution of the mixture was investigated at 1723-1803 K by X-ray powder diffraction, and the microstructure of the product prepared at 1803 K for 4 h was examined by scanning electronic microscope. The results show that the decomposition of ZrSiO₄ and the formation of β-SIC can be promoted by increasing the heating temperature and adding La₂O₃. The β-SiC/ZrO₂ composites can be prepared at 1803 K for 4 h in a mixture of zircon, carbon black and La₂O₃, and the contents of β-SIC and m-ZrO₂ in the product sample with 2wt% La₂O₃ reach the highest values of 10.8wt% and 89.2wt%, respectively. The crystal size of the products is about 200 nm.     

Reaction mechanism for in-situ β-SiAlON formation in Fe3Si-Si3N4-Al2O3 composites

In this work, Fe₃Si-Si₃N₄-Al₂O₃ composites were prepared at 1300℃ in an N₂ atmosphere using fused corundum and tabular alumina particles, Al₂O₃ fine powder, and ferrosilicon nitride (Fe₃Si-Si₃N₄) as raw materials and thermosetting phenolic resin as a binder. The effect of ferrosilicon nitride with different concentrations (0wt%, 5wt%, 10wt%, 15wt%, 20wt%, and 25wt%) on the properties of Fe₃Si-Si₃N₄-Al₂O₃ composites was investigated. The results show that the apparent porosity varies between 10.3% and 17.3%, the bulk density varies from 2.94 g/cm3 and 3.30 g/cm3, and the cold crushing strength ranges from 67 MPa to 93 MPa. Under the experimental conditions, ferrosilicon nitride, whose content decreases substantially, is unstable; part of the ferrosilicon nitride is converted into Fe₂C, whereas the remainder is retained, eventually forming the ferrosilicon alloy. Thermodynamic assessment of the Si₅AlON₇ indicated that the ferrosilicon alloy accelerated the reactions between Si₃N₄ and α-Al₂O₃ fine powder and that Si in the ferrosilicon alloy was nitrided directly, forming β-SiAlON simultaneously. In addition, fused corundum did not react directly with Si₃N₄ because of its low reactivity.     

Feasibility of aluminum recovery and MgAl2O4 spinel synthesis from secondary aluminum dross

The feasibility of aluminum recovery from secondary aluminum dross by extraction with NaOH solution and the subsequent synthesis of MgAl₂O₄ spinel by sintering the extracted slag were studied. The extraction percentage of soluble aluminum from the dross reached 80% at a temperature of 353 K, liquid-to-solid ratio of 12 mL·g-1, stirring speed of 300 r·min-1, and an extraction time of 15 min; the hydrolysis percentage of AlN reached 40% with an extraction time of 30 min. The activation energies of the soluble aluminum and AlN extracted from the dross were 7.15 and 8.98 kJ·mol-1, respectively, indicating that their kinetics were controlled by outer diffusion without a product layer. The extracted slag was sintered in the temperature range 1373-1773 K; MgAl₂O₄ spinel with a compressive strength as high as 69.4 MPa was produced in the sample sintered at 1673 K for 3 h. This value exceeds the threshold (40 MPa) prescribed by the National Standard for the Magnesia and Magnesia-alumina Refractory Bricks of China (GB/T 2275-2007). These results establish the effectiveness of aluminum recovery from secondary aluminum dross and subsequent MgAl₂O₄ spinel synthesis.     

Fabrication and properties of Al matrix composites strengthened by in situ alumina particulates

New aluminum matrix composites strengthened by Al₂O₃ particulates through stirring cast by adding NH₄Al(SO₄)₂ to the molten aluminum have been fabricated. TEM observation shows that in-situ Al₂O₃ particulates are generally spherical and they are uniformly distributed in the Al matrix. Dry sliding wear test results show that the volume loss of the unreinforced Al matrix is about three times that of the Al₂O₃ reinforced metal matrix composite (MMC) and the volume loss of the MMC fabricated by adding Al₂O₃ is larger than that of the MMC by adding NH₄Al(SO₄)₂. Lubricating sliding wear test results show that the volume loss of the MMCs increases more slowly than that of the matrix with the increasing of the load.     

In-situ fabrication of Al(Zn)-Al2O3 graded composite using the aluminothermic reaction during hot pressing

In this study, the fabrication of multilayer Al(Zn)–Al₂O₃ with different volume fractions of Al₂O₃ was investigated. Al and ZnO powders were milled by a planetary ball mill, after which five-layer functionally graded samples were produced through hot pressing at 580℃ and 90 MPa pressure for 30 min. Formation of reinforcing Al₂O₃ particles occurred in the aluminum matrix via the aluminothermic reaction. Determination of the ignition temperature of the aluminothermic reaction was accomplished using differential thermal and thermogravimetric analyses. Scanning electron microscopy, energy dispersive spectroscopy, and X-ray diffractometery analyses were utilized to characterize the specimens. The thermal analysis results showed that the ignition temperatures for the aluminothermic reaction of layers with the highest and lowest ZnO contents were 667 and 670℃, respectively. Microstructural observation and chemical analysis confirmed the fabrication of Al(Zn)–Al₂O₃ functionally graded materials composites with precipitation of additional Zn in the matrix. Moreover, nearly dense functionally graded samples demonstrated minimum and maximum hardness values of HV 75 and HV 130, respectively.     

Microstructure and electrolysis behavior of self-healing Cu-Ni-Fe composite inert anodes for aluminum electrowinning

The microstructure evolution and electrolysis behavior of (Cu₅₂Ni₃₀Fe₁₈)-xNiFe₂O₄ (x=40wt%, 50wt%, 60wt%, and 70wt%) composite inert anodes for aluminum electrowinning were studied. NiFe₂O₄ was synthesized by solid-state reaction at 950℃. The dense anode blocks were prepared by ball-milling followed by sintering under a N₂ atmosphere. The phase evolution of the anodes after sintering was determined by scanning electron microscopy and energy-dispersive X-ray spectroscopy. The results indicate that a substitution reaction between Fe in the alloy phase and Ni in the oxide phase occurs during the sintering process. The samples were also examined as inert anodes for aluminum electrowinning in the low-temperature KF-NaF-AlF₃ molten electrolyte for 24 h. The cell voltage during electrolysis and the corrosion scale on the anodes were analyzed. The results confirm that the scale has a self-repairing function because of the synergistic reaction between the alloy phase with Fe added and the oxide phase. The estimated wear rate of the (Cu₅₂Ni₃₀Fe₁₈)-50NiFe₂O₄ composite anode is 2.02 cm·a-1.     

Desulfurization ability of refining slag with medium basicity

The desulfurization ability of refining slag with relative lower basicity (B) and Al₂O₃ content (B = 3.5–5.0; 20wt%–25wt% Al₂O₃) was studied. Firstly, the component activities and sulfide capacity (C_S) of the slag were calculated. Then slag-metal equilibrium experiments were carried out to measure the equilibrium sulfur distribution (L_S). Based on the laboratorial experiments, slag composition was optimized for a better desulfurization ability, which was verified by industrial trials in a steel plant. The obtained results indicated that an MgO-saturated CaO-Al₂O₃-SiO₂-MgO system with the basicity of about 3.5–5.0 and the Al₂O₃ content in the range of 20wt%–25wt% has high activity of CaO (a_CaO), with no deterioration of C_S compared with conventional desulfurization slag. The measured L_S between high-strength low-alloyed (HSLA) steel and slag with a basicity of about 3.5 and an Al₂O₃ content of about 20wt% and between HSLA steel and slag with a basicity of about 5.0 and an Al₂O₃ content of about 25wt% is 350 and 275, respectively. The new slag with a basicity of about 3.5–5.0 and an Al₂O₃ content of about 20wt% has strong desulfurization ability. In particular, the key for high-efficiency desulfurization is to keep oxygen potential in the reaction system as low as possible, which was also verified by industrial trials.     

Electrical conductivity optimization of the Na3AlF6-Al2O3-Sm2O3 molten salts system for Al-Sm intermediate binary alloy production

Metal Sm has been widely used in making Al-Sm magnet alloy materials. Conventional distillation technology to produce Sm has the disadvantages of low productivity, high costs, and pollution generation. The objective of this study was to develop a molten salt electrolyte system to produce Al-Sm alloy directly, with focus on the electrical conductivity and optimal operating conditions to minimize the energy consumption. The continuously varying cell constant (CVCC) technique was used to measure the conductivity for the Na₃AlF₆-AlF₃-LiF-MgF₂-Al₂O₃-Sm₂O₃ electrolysis medium in the temperature range from 905 to 1055℃. The temperature (t) and the addition of Al₂O₃ (W(Al₂O₃)), Sm₂O₃ (W(Sm₂O₃)), and a combination of Al₂O₃ and Sm₂O₃ into the basic fluoride system were examined with respect to their effects on the conductivity (κ) and activation energy. The experimental results showed that the molten electrolyte conductivity increases with increasing temperature (t) and decreases with the addition of Al₂O₃ or Sm₂O₃ or both. We concluded that the optimal operation conditions for Al-Sm intermediate alloy production in the Na₃AlF₆-AlF₃-LiF-MgF₂-Al₂O₃-Sm₂O₃ system are W(Al₂O₃) + W(Sm₂O₃)=3wt%, W(Al₂O₃):W(Sm₂O₃)=7:3, and a temperature of 965 to 995℃, which results in satisfactory conductivity, low fluoride evaporation losses, and low energy consumption.     

Effect of interaction of refractories with Ni-based superalloy on inclusions during vacuum induction melting

This study documents laboratory-scale observation of the interactions between the Ni-based superalloy FGH4096 and refractories. Three different crucibles were tested—MgO, Al₂O₃, and MgO–spinel. We studied the variations in the compositions of the inclusions and the alloy–crucible interface with the reaction time using scanning electron microscopy equipped with energy dispersive X-ray spectroscopy and X-ray diffraction. The results showed that the MgO and MgO–spinel crucibles form MgO-containing inclusions (Al–Mg oxides and Al–Mg–Ti oxides), whereas the inclusions formed when using the Al₂O₃ crucible are Al₂O₃ and Al–Ti oxides. We observed a new MgAl₂O₄ phase at the inner wall of the MgO crucible, with the alloy melted in the MgO crucible exhibiting fewer inclusions. No new phase occurred at the inner wall of the Al₂O₃ crucible. We discuss the mechanism of interaction between the refractories and the Ni-based superalloy. Physical erosion was found to predominate in the Al₂O₃ crucible, whereas dissolution and chemical reactions dominated in the MgO crucible. No reaction was observed between three crucibles and the Ti of the melt although the Ti content (3.8wt%) was higher than that of Al (2.1wt%).     

Effect of Al<Subscript>2</Subscript>O<Subscript>3sf</Subscript> addition on the friction and wear properties of (SiC<Subscript>p</Subscript>+Al<Subscript>2</Subscript>O<Subscript>3sf</Subscript>)/Al2024 composites fabricated by pressure infiltration

Aluminum (Al) 2024 matrix composites reinforced with alumina short fibers (Al₂O_3sf) and silicon carbide particles (SiC_p) as wear-resistant materials were prepared by pressure infiltration in this study. Further, the effect of Al₂O_3sf on the friction and wear properties of the as-synthesized composites was systematically investigated, and the relationship between volume fraction and wear mechanism was discussed. The results showed that the addition of Al₂O_3sf, characterized by the ratio of Al₂O_3sf to SiC_p, significantly affected the properties of the composites and resulted in changes in wear mechanisms. When the volume ratio of Al₂O_3sf to SiC_p was increased from 0 to 1, the rate of wear mass loss (K_m) and coefficients of friction (COFs) of the composites decreased, and the wear mechanisms were abrasive wear and furrow wear. When the volume ratio was increased from 1 to 3, the COF decreased continuously; however, the K_m increased rapidly and the wear mechanism became adhesive wear.     

Graphene-reinforced aluminum matrix composites prepared by spark plasma sintering

Graphene-reinforced 7055 aluminum alloy composites with different contents of graphene were prepared by spark plasma sintering (SPS). The structure and mechanical properties of the composites were investigated. Testing results show that the hardness, compressive strength, and yield strength of the composites are improved with the addition of 1wt% graphene. A clean, strong interface is formed between the metal matrix and graphene via metallurgical bonding on atomic scale. Harmful aluminum carbide (Al₄C₃) is not formed during SPS processing. Further addition of graphene (above 1wt%) results in the deterioration in mechanical properties of the composites. The agglomeration of graphene plates is exacerbated with increasing graphene content, which is the main reason for this deterioration.     

Activity coefficient of NiO in SiO2-saturated MnO–SiO2slag and Al2O3-saturated MnO–SiO2–Al2O3slag at 1623 K

As a part of the fundamental study related to the reduction smelting of spent lithium-ion batteries and ocean polymetallic nodules based on MnO–SiO₂slags,this work investigated the activity coefficient of NiO in SiO₂-saturated Mn O–Si O₂slag and Al₂O₃-saturated Mn O–SiO₂–Al₂O₃slag at 1623 K with controlled oxygen partial pressure levels of 10^-7,10^-6,and 10^-5Pa.Results showed that the solubility of nickel oxide in the slags increased with increasing oxygen partial pressure.The nickel in the Mn O–Si O₂slag and Mn O–Si O₂–Al₂O₃slag existed as Ni O under experimental conditions.The addition of Al₂O₃in the Mn O–Si O₂slag decreased the dissolution of nickel in the slag and increased the activity coefficient of Ni O.Furthermore,the activity coefficient of Ni O(γN_(i O)),which is solid Ni O,in the Si O₂saturated Mn O–Si O₂slag and Al₂O₃saturated Mn O–Si O₂–Al₂O₃slag at 1623 K can be respectively calculated asγN_(i O)=8.58w(Ni O)+3.18 andγN_(i O)=11.06w(Ni O)+4.07,respectively,where w(Ni O)is the Ni O mass fraction in the slag.     

Development of inclusions in 3104 alloy melt during heating and holding treatments

Developments in the contents of different typical inclusions in 3104 alloy melt were described during heating and holding processing. The settling process of inclusion particles was investigated by measuring the contents of inclusions in the surface, center, and bottom layers of the molten metal. In the results, main inclusions observed and determined by Prefil and PoDFA methods are MgO, Al₂O₃, spinel (MgAl₂O₄), and TiB₂ particles or thin films. It is found that some small particles of Al₂O₃ and MgO are transformed into spinel particles, and the formation rate increases as the temperature and the holding period of melt increase. The content of inclusions increases from 3.37 mm2·kg-1 to 7.54 mm2·kg-1 and then decreases to 3.08 mm2·kg-1 after holding for 90 min. This is attributed to a settling phenomenon and a significant increase in settling velocity after holding for 60 min. The content of inclusion particles decreases by means of settlement and flotation in liquid aluminum with an increase in holding time. The theoretical analysis and experiment results are in essential agreement with those from industrial production.     

Properties of a reaction-bonded β-SiAlON ceramic doped with an FeMo alloy for application to molten aluminum environments

An FeMo-alloy-doped β-SiAlON (FeMo/β-SiAlON) composite was fabricated via a reaction-bonding method using raw materials of Si, Al₂O₃, AlN, FeMo, and Sm₂O₃. The effects of FeMo on the microstructure and mechanical properties of the composite were investigated. Some properties of the composite, including its bending strength at 700℃ and after oxidization at 700℃ for 24 h in air, thermal shock resistance and corrosion resistance to molten aluminum, were also evaluated. The results show that the density, toughness, bending strength, and thermal shock resistance of the composite are obviously improved with the addition of an FeMo alloy. In addition, other properties of the composite such as its high-temperature strength and oxidized strength are also improved by the addition of FeMo alloy, and its corrosion resistance to molten aluminum is maintained. These findings indicate that the developed FeMo/β-SiAlON composite exhibits strong potential for application to molten aluminum environments.     

Fabrication of Fe–TiC–Al2O3 composites on the surface of steel using a TiO2–Al–C–Fe combustion reaction induced by gas tungsten arc cladding

The aim of the present study was to fabricate Fe–TiC–Al₂O₃ composites on the surface of medium carbon steel. For this purpose, TiO₂–3C and 3TiO₂–4Al–3C–xFe (0 ≤ x ≤ 4.6 by mole) mixtures were pre-placed on the surface of a medium carbon steel plate. The mixtures and substrate were then melted using a gas tungsten arc cladding process. The results show that the martensite forms in the layer produced by the TiO₂–3C mixture. However, ferrite–Fe₃C–TiC phases are the main phases in the microstructure of the clad layer produced by the 3TiO₂–4Al–3C mixture. The addition of Fe to the TiO₂–4Al–3C reactants with the content from 0 to 20wt% increases the volume fraction of particles, and a composite containing approximately 9vol% TiC and Al₂O₃ particles forms. This composite substantially improves the substrate hardness. The mechanism by which Fe particles enhance the TiC + Al₂O₃ volume fraction in the composite is determined.     

AISI 321不锈钢钢钢包精炼过程中钙含量对夹杂物的影响

The effect of three heat processes with different calcium contents on the evolution of inclusions during the ladle furnace refining process of AISI 321 stainless steel was investigated. The size, morphology, and composition of the inclusions were analyzed by scanning electron microscopy and energy-dispersive X-ray spectroscopy. After the addition of aluminum and titanium, the primary oxide in the AISI 321 stainless steel was an Al₂O₃–MgO–TiO_x complex oxide, in which the mass ratio of Al₂O₃/MgO was highly consistent with spinel (MgO·Al₂O₃). After calcium treatment, the calcium content in the oxide increased significantly. Thermodynamic calculations show that when the Ti content was 0.2wt%, the Al and Ca contents were less than 0.10wt% and 0.0005wt%, respectively, which was beneficial for the formation of liquid inclusions in molten steel. Moreover, the modification mechanism of calcium on TiN-wrapped oxides in combination with temperature changes was discussed.     

Microstructure characterization of a pressureless infiltrating oxidized SiCp preform by Al-8Mg

The microstructure of a pressureless infiltrating 55vol% oxidized SiC preform by Al-8Mg alloy was characterized by transmission electron microscopy (TEM), high resolution TEM (HRTEM), field emission scanning electron microscopy (FE-SEM), and X-ray diffraction. The TEM image of the interface between Al and SiC shows that the surface of SiC is covered by a rough nanocrystal layer of MgAl₂O₄, Al₂O₃, and Si, produced by the interfacial reaction of Al, Mg, and SiO₂ on the surface of SiC. The Al-SiC interface is also examined by HRTEM to be better understood how MgAl₂O₄ and Al₂O₃ are produced. Dendritic Al₂O₃ crystals are embedded in the pores of the composite generated from the mutual bonding of SiO₂ on the surface of SiC. Columnar AlN crystals of about 250 nm in length are bunched vertically on the SiC particle surface.