Sintered stainless steels: Fatigue crack propagation resistance under hydrogen charging conditions

Monophasic and multiphasic (two and three phases) sintered stainless steels were prepared both considering premixes of AISI 316LHC and AISI 434LHC stainless steels powders and using a prealloyed duplex stainless steel 25% Cr, 5% Ni, 2% Mo powder. Their fatigue crack propagation resistance was investigated both in air and under hydrogen charging conditions (0.5 M H₂SO₄ + 0.01 M KSCN aqueous solution; applied potential = −700 mV/SCE), considering three different stress ratios (R = 0.1; 0.5; 0.75). Fatigue crack propagation micromechanisms were investigated by means of fracture surface scanning electron microscope (SEM) analysis.For all the investigated sintered stainless, fatigue crack propagation resistance is influenced by hydrogen charging and an increase of crack growth rates dependent on the steel microstructure is obtained. Experimental results also allow to identify the sintered stainless steel obtained from the prealloyed 25% Cr, 5% Ni, 2% Mo powder as the most resistant to fatigue crack propagation in air and under hydrogen charging conditions.     

Synthesis of MoSi2/WSi2 nanocrystalline powder by mechanical-assistant combustion synthesis method

MoSi₂/WSi₂ nanocrystalline powder has been successfully synthesized by the mechanical-assistant combustion synthesis method. This method includes a ball-milling process followed by combustion synthesis. The composition and microstructure of the as-milled powder mixture were detected by X-ray diffraction and scanning electron microscopy analyses. Their results show that the Mo(W) solid solution and Si nanocrystals could be obtained during the ball-milling process. Compared with normal powder mixture (Mo + Si + W), it could be easily ignited and high maximum combustion temperature was achieved. It was also confirmed that MoSi₂/WSi₂ solid solution powder with nanometric structure could be prepared through combustion synthesis method from the mechanical activated powder mixture.     

Microstructure evolution and wear properties of bulk MoSi2 fabricated by field activated sintering

Field activated sintering (FAS) was employed to fabricate dense bulk MoSi₂ from Mo and Si powders. During the FAS process, Si was melted first, and then Mo was dissolved leading to a precipitation of MoSi₂. A eutectic reaction of MoSi₂-Mo₅Si₃ resulted from a combined effect of Mo-Si exothermic reactions and field induced Joule heating. With hyper-stoichiometric amount of Si (Mo/Si = 1:2.06), the FAS MoSi₂ is free of Mo₅Si₃ phase. Subsequently, an un-lubricated sliding wear test of MoSi₂ against carbon steel was conducted. Both normal load and temperature have crucial points related to a transition from mild to severe wear. Sliding speed and relative density have a negative effect on wear rate. In addition, at room temperature the wear is with a protective layer composed of oxide and transferred substance, whereas poor oxidation resistance leads to spalling of the layer and brittle fracture at an elevated temperature up to 500 °C.     

Sintering response of austenitic (316L) and ferritic (434L) stainless steel consolidated in conventional and microwave furnaces

This study compares the effect of heating mode on the densification, microstructure, strength and hardness of austenitic and ferritic stainless steel. The compacts were sintered in a radiatively heated (conventional) and a 2.45 GHz microwave furnace. Both 316L and 434L compacts couple with microwaves and heat up to the sintering temperature rapidly (45 °C/min). The overall processing time was reduced by about 90% through microwave sintering. While the microwave sintered compacts exhibit a finer microstructure, there is no corresponding improvement in densification and mechanical properties. This has been correlated with elongated and irregular pore structure.     

Fabrication of full density near-nanostructured cemented carbides by combination of VC/Cr3C2 addition and consolidation by SPS and HIP technologies

The aim of present work is to study the effect of VC and/or Cr₃C₂ in densification, microstructural development and mechanical behavior of nanocrystalline WC-12wt.%Co powders when they are sintered by spark plasma sintering (SPS) and hot isostatic pressing (HIP). The results were compared to those corresponding to conventional sintering in vacuum. The density, microstructure, X-ray diffraction, hardness and fracture toughness of the sintered materials were evaluated. Materials prepared by SPS exhibits full densification at lower temperature (1100 °C) and a shorter stay time (5 min), allowing the grain growth control. However, the effect of the inhibitors during SPS process is considerably lower than in conventional sintering. Materials prepared by HIP at 1100 °C and 30 min present full densification and a better control of microstructure in the presence of VC. The added amount of VC allows obtaining homogeneous microstructures with an average grain size of 120 nm. The hardness and fracture toughness values obtained were about 2100 HV₃₀ and close to 10 MPa m^1/2, respectively.     

Effect of partial substitution of Cr for Ni on densification behavior, microstructure evolution and mechanical properties of Ti(C,N)-Ni-based cermets

Four cermets of composition TiC-10TiN-16Mo-6.5WC-0.8C-0.6Cr₃C₂-(32 − x)Ni-xCr (x = 0, 3.2, 6.4 and 9.6 wt%) were prepared, to investigate the effect of the partial substitution of Cr for Ni on densification behavior, microstructure evolution and mechanical properties of Ti(C,N)-Ni-based cermets. The partial substitution of Cr for Ni decreased full densification temperature, and the higher the content of Cr additive was, the lower full densification temperature was. The partial substitution of Cr for Ni had no significant effect of the formation of Mo₂C and Ti(C,N) and the dissolution of WC, and however, it had a significant effect on the dissolution of Mo₂C. Cr in Ni-based binder phase diffused into undissolved Mo₂C to form (Mo,Cr)₂C above 1000 °C at 6.4-9.6 wt% Cr additive, and a small amount of (Mo,Cr)₂C did not dissolve after sintering at 1410 °C for 1 h at 9.6 wt% Cr additive. In the final microstructure, Cr content in Ni-based binder phase increased with increasing the content of Cr additive, and however, regardless of the content of Cr additive, coarse Ti(C,N) grains generally consisted of black core, white inner rim and grey outer rim, and fine Ti(C,N) grains generally consisted of white core and grey rim. The partial substitution of Cr for Ni increased hardness and decreased transverse rupture strength (TRS). Ni-based binder phase became hard with increasing the content of Cr additive, therefore resulting in the increase of hardness and the decrease of TRS. TRS was fairly low at 9.6 wt% Cr additive, which was mainly attributed hardening of Ni-based binder phase and undissolved (Mo,Cr)₂C.     

Effect of silicon addition on the microstructure and corrosion behavior of sintered stainless steel

The influence of silicon addition on the physical properties and the corrosion behavior of sintered austenitic 304L stainless steel was evaluated. The density of the sintered stainless steel changed depending upon the amount of silicon added. A “pseudo-peritectic” reaction developed during the sintering of high silicon content alloys and resulted in an increased sintering rate and enhanced densification. The corrosion resistance of the various sintered stainless steels was evaluated from the results of potentiodynamic polarization curves and corrosion rate measurements and from the appearance of the corroded surfaces. The results indicated that the corrosion resistance was improved with the addition of more than 2 wt.% Si.     

Effect of Sm2O3 content on microstructure and thermal conductivity of Spark Plasma Sintered AlN ceramics

Dense aluminum nitride ceramics were prepared by Spark Plasma Sintering at a lower sintering temperature of 1700 °C with Sm₂O₃ as sintering additives. The effect of Sm₂O₃ content on the density, phase composition, microstructure and thermal conductivity of AlN ceramics was investigated. The results showed that Spark Plasma Sintering could fabricate dense AlN ceramics with superior thermal properties in a very short time. Sm₂O₃ not only facilitated the densification via the liquid-phase sintering mechanism but also improved thermal conductivity by decreasing oxygen impurity. Thermal conductivity decreased with increasing amount of Sm₂O₃ and the highest thermal conductivity was obtained for the AlN ceramics with 2 wt.% Sm₂O₃ content. During Spark Plasma Sintering process, only 2–3 wt.% sintering additives was enough to fabricate dense AlN ceramics, and the microstructures played a key role in controlling the thermal conductivity of AlN ceramics.     

Preparation and properties of sintered molybdenum doped with La2O3/MoSi2

Sintered Mo with the addition of La₂O₃/MoSi₂ was prepared via the process of solid–solid doping + powder metallurgy. X-ray diffraction experiment, hardness test, three-point bending test and high-temperature tensile test were carried out to characterize the samples. The XRD pattern of a typical sample shows that the sintered Mo was mainly composed of Mo, La₂O₃ and Mo₅Si₃. Mo₅Si₃ was probably formed through the reaction between MoSi₂ and the Mo matrix. Densities and fracture toughnesses of both doped Mo and pure Mo were measured and contrasted. Sintered Mo with the addition of 0.2 wt% La₂O₃/MoSi₂ has the highest toughness, while more addition of La₂O₃/MoSi₂ has smaller effect on improving toughness or even embrittles Mo. The results of three-point bending test and high-temperature tensile test show that the bending strength and high-temperature tensile strength of doped Mo are both higher than those of pure Mo. The formation of Mo₅Si₃ improves the high-temperature strength. The La₂O₃/Mo₅Si₃ dispersed in the Mo matrix refined the grains, and thus strengthened the Mo matrix by dispersion strengthening and grain refinement.     

Thermal and electrical properties of TiB2–MoSi2

The present communication reports the effect of MoSi₂ addition on high temperature thermal conductivity and room temperature (RT) electrical properties of TiB₂. The thermal diffusivity and the thermal conductivity of the hot pressed TiB₂–MoSi₂ samples were measured over a range from room temperature to 1000 °C using the laser-flash technique, while electrical resistivity was measured at RT using a four linear probe method. The reciprocal of thermal diffusivity of TiB₂ samples exhibit linear dependence on temperature and the measured thermal conductivity of TiB₂-2.5% MoSi₂ composites correlate well with the theoretical predictions from Hashin’s model and Hasselman and Johnson’s model. A common observation is that the thermal conductivity of all the samples slightly increases with temperature (up to 200 °C) and then decreases with further increasing temperature. It is interesting to note that both the thermal conductivity and electrical conductivity of TiB₂ samples enhanced with the addition of 2.5 wt.% MoSi₂ sinter additive. Among all the samples, TiB₂-2.5 wt.% MoSi₂ ceramics measured with high thermal conductivity (77 W/mK) and low electrical resistivity (12 μΩ-cm) at room temperature. Such an improvement in properties can be attributed to its high density and low volume fraction of porosity. On the other hand, both the thermal and electrical properties of TiB₂ were adversely affected with further increasing the amount of MoSi₂ (10 wt.%).     

Microstructure of a plasma-sprayed Mo-Si-B alloy

Powders of Mo₅₂Si₃₈B₁₀ were plasma sprayed under inert conditions onto stainless steel substrates to determine if high density free standing forms could be synthesized by this process. Thermal spray conditions were varied to minimize porosity and oxygen impurities while minimizing evaporative metal losses. The assprayed and sintered microstructures were characterized using scanning and transmission electron microscopy and quantitative x-ray diffraction (XRD). The as-sprayed microstructure consisted of elongated splats tens of microns in length and only one to three microns in thickness. The splats contained submicrometer grains of primarily MoB and Mo₅Si₃B _x (T1) and minor amounts of MoSi₂ and a glassy grain boundary phase. The interior of the splats typically consisted of a fine eutectic of MoB and T1. Small pieces were cut out of the cross section of the sample and pressureless sintered for 2, 6, and 10 h at 1800 °C in flowing Ar. After sintering for 2 h at 1800 °C, the samples exhibited a coarser but equiaxed microstructure (1 to 5 μm grain size) containing 78 vol.% T1, 16 vol.% MoB, and 6 vol.% MoSi₂ as determined by XRD. Approximately 8 at.% of the Si formed silica. The high-temperature anneal removed all vestiges of the layered structure observed in the as-sprayed samples.     

Effect of secondary carbides addition on the microstructure and mechanical properties of (Ti, W, Mo, V)(C, N)-based cermets

(Ti, W, Mo, V)(C, N)-based cermets were prepared by mixing Mo₂C, WC and TaC with ultrafine (Ti, W, Mo, V)(C, N) powders, and then processed via a conventional P/M technique. The effect of Mo₂C, WC and TaC on the microstructure and mechanical properties of (Ti, W, Mo, V)(C, N)-8 wt.% Ni-7 wt.% Co systems was investigated. The Mo₂C content was varied from 0 to 10 wt.% and additive WC or TaC was added at a level of 5 wt.% with Mo₂C addition. The results show that the densification of (Ti, W, Mo, V)(C, N)-8 wt.% Ni-7 wt.% Co cermets was improved significantly by the addition of Mo₂C. With the increase of Mo₂C content, there is a coarsening tendency in the microstructure of (Ti, 20W, 15Mo, 0.2V)(C, N)-8Ni-7Co system, but the refinement for (Ti, 15W, 5Mo, 0.2V)(C, N)-8Ni-7Co. TaC addition decreases the density of (Ti, 15W, 5Mo, 0.2V)(C, N)-10Mo₂C-8Ni-7Co cermet and thus weakens its bending strength. (Ti, 15W, 5Mo, 0.2V)(C, N)-10Mo₂C-5WC-8Ni-7Co cermet has optimal mechanical properties: bending strength of 1999 MPa, hardness (H_v) of 1677 MPa and toughness of 9.95 MPa m^1/2 respectively by adding WC, which is due to its ultrafine and weak core/rim structure.     

An experimental study on synthesizing submicron MoSi2-based coatings using electrothermal explosion ultra-high speed spraying method

The MoSi₂-based coatings were synthesized on the surface of the low carbon steel substrate using electrothermal explosion ultra-high speed spraying method. Microstructure, phase structure, elements distribution and microhardness of the coatings were characterized by SEM, XRD, EDS and Vickers hardness tester, respectively. It is found that MoSi₂ coating and MoSi₂ + MoB₂ multiphase coating were in-situ formed. The coatings have compact microstructure, submicron-grain and high hardness. The bonding of coating-substrate is metallurgical one. The hardness and microstructure of the MoSi₂ coating were improved by boron alloying. The average and highest hardness of the MoSi₂ coating are 1340 HV_0.2 and 1390 HV_0.2, respectively, and that of MoSi₂ + MoB₂ multiphase coating are 1650 HV_0.2 and 1785 HV_0.2, respectively.     

Determination of critical and optimal powder loadings for 316L fine stainless steel feedstocks for micro-powder injection molding

Adapted from powder injection molding (PIM), the micro-PIM technology satisfies the increasing demands for functionalization and miniaturization of micro-parts. Research works in this area have been carried out through micro injection molding tests issued from mixtures consisting in 316L stainless steel fine powders with D₅₀ = 3.4 μm and different thermoplastic polymeric binders. The well appropriate polymer–powder formulations are composed with different binders. The binders have been adapted to micro-injection and tested to find out an optimum feedstock. The rheological characterization of the elaborated feedstock has been carried out according to the selected stainless steel powders and polymers. The critical powder volume loading has been determinated and fixed in the range of 68–70%, and the optimal powder volume loading has been chosen around 66% for 316L stainless steel feedstock (D₅₀ = 3.4 μm). This choice has been confirmed by processing of the micro-components with the retained feedstock loaded up to 66%.     

Microstructural and mechanical evaluation of Al-TiB2 nanostructured composite fabricated by mechanical alloying

Production of bulk Al-TiB₂ nanocomposite from mechanically alloyed powder was studied. Al-20 wt.% TiB₂ metal matrix nanocomposite powder was obtained by mechanical alloying (MA) of pure Ti, B and Al powder mixture. A double step process was used to prevent the formation of undesirable phases like Al₃Ti intermetallic compound, which has been described in our previous papers. The resultant powder was consolidated by spark plasma sintering (SPS) followed up by hot extrusion. The structural characteristics of powder particles and sintered samples were studied by X-ray diffractometry (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Hardness measurements were conducted on the cross section of powder particles and sintered sample and the tensile behavior of extruded samples was evaluated. The results showed that the prepared Al-20 wt.% TiB₂ nanocomposite has good thermal stability against grain growth and particle coarsening. Extruded Al-20 wt.% TiB₂ showed a hardness value of 180 VHN and yield and tensile strength of 480 and 540 MPa, respectively, which are much higher than those reported for similar composites made by other processes.     

氧化物/不锈钢梯度复合材料初步设计与评价

采用粉末层叠和整体热压烧结的方法,制备了Y₂Ti₂O₇/316L不锈钢功能梯度复合材料。经金相显微镜、X射线衍射仪和电子探针分析确定,该材料在金属和氧化物界面处实现了成分和微观组织的梯度过渡。对不同梯度含量复合材料的力学性能测试表明,界面处的力学性能存在相应的梯度变化,即随各层金属相含量的逐渐增加,过渡区材料的致密度、抗弯强度不断提升,而硬度则不断下降。     

Densification and mechanical properties of fine-grained Al2O3-ZrO2 composites consolidated by spark plasma sintering

Alumina matrix composites containing 5 and 10 wt% of ZrO₂ were sintered under 100 MPa pressure by spark plasma sintering process. Alumina powder with an average particle size of 600 nm and yttria-stabilized zirconia with 16 at% of Y₂O₃ and with a particle size of 40 nm were used as starting materials. The influence of ZrO₂ content and sintering temperature on microstructures and mechanical properties of the composites were investigated. All samples could be fully densified at a temperature lower than 1400 °C. The microstructure analysis indicated that the alumina grains had no significant growth (alumina size controlled in submicron level 0.66-0.79 μm), indicating that the zirconia particles provided a hindering effect on the grain growth of alumina. Vickers hardness and fracture toughness of composites increased with increasing ZrO₂ content, and the samples containing 10 wt% of ZrO₂ had the highest Vickers hardness of 18 GPa (5 kg load) and fracture toughness of 5.1 MPa m^1/2.     

Effect of MgO particle size on the microstructure, mechanical properties and wear performance of ZTA-MgO ceramic cutting inserts

The mechanical properties, microstructure and wear performance of zirconia-toughened alumina (ZTA) cutting inserts with Magnesia (MgO) in different particle sizes as additives was investigated. The MgO particle sizes were varied from 80 nm to 7000 nm. The alumina (Al₂O₃), yittria stabilized zirconia (YSZ) and MgO powders were mixed, compacted and sintered at 1600 °C using the solid-state sintering method. The mechanical and physical properties of the samples such as wear resistance, Vickers hardness, fracture toughness, microstructure and density were analyzed. Commercially available stainless steel (316L) was used as the workpiece for the wear resistance study. It was observed that smaller MgO particle sizes induce better wear performance and mechanical properties for the cutting inserts. Wear resistance analysis showed that the cutting insert with nano-sized MgO (particle size 80 nm) had the lowest wear area of 0.019 mm². The same cutting insert also possessed the highest Vickers hardness value of 1740 Hv compared to the other samples. Furthermore, microstructural observations show that the Al₂O₃ grain size depends on the particle size of MgO, and is directly related to its hardness property.     

Bulk WC-Al2O3 composites prepared by spark plasma sintering

WC and WC-Al₂O₃ materials without metallic binder addition were densified by spark plasma sintering in the range of 1800-1900 °C. The densification behavior, phase constitution, microstructure and mechanical properties of pure WC and WC-Al₂O₃ composite were investigated. The addition of Al₂O₃ facilitates sintering and increases the fracture toughness of the composites to a certain extent. An interesting phenomenon is found that a proper content of Al₂O₃ additive helps to limit the formation of W₂C phase in sintered WC materials. The pure WC specimen possesses a hardness (HV₁₀) of 25.71 GPa, fracture toughness of 4.54 MPa·m^1/2, and transverse fracture strength of 862 MPa, while those of WC-6.8 vol.% Al₂O₃ composites are 24.48 GPa, 6.01 MPa·m^1/2, and 1245 MPa respectively. The higher fracture toughness and transverse fracture strength of WC-6.8 vol.% Al₂O₃ are thought to result from the reduction of W₂C phase, the crack-bridging by Al₂O₃ particles and the local change in fracture mode from intergranular to transgranular.     

Synthesis of Ti3SiC2 by infiltration of molten Si

High-purity Ti₃SiC₂ compounds have been fabricated by infiltration of molten Si into a precursor, a partially sintered TiC_x (x = 0.67) preform. The Si source and the TiC_x preform were placed side by side on carbon cloth, and the system was heated to 1550 °C. Molten Si infiltrated the preform through the carbon cloth, and a direct reaction between TiC_x and molten Si immediately occurred at the reaction temperature to yield pure Ti₃SiC₂. We could observe phase formation and the microstructure of the bulk products with time, which were investigated by X-ray diffraction (XRD) and scanning electron microscopy (SEM) equipped with energy-dispersive spectroscopy (EDS). Pure Ti₃SiC₂ compounds were formed on the exterior of the TiC_x preform at 1550 °C when the sintered TiC_x:Si ingot molar ratio was 3:1.4. At 1550 °C, no other minor phases were detected for any of the sintering time ranges.