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Register a new userNanosized precipitates in H13 tool steel low temperature plasma nitriding
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Added by
Luiz Fernando Zagonel
Publication date
2012
fields
Physics
and research's language is
English
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A comprehensive study of pulsed nitriding in AISI H13 tool steel at low temperature (400{deg}C) is reported for several durations. X-ray diffraction results reveal that a nitrogen enriched compound (Epsilon-Fe2-3N, iron nitride) builds up on the surface within the first process hour despite the low process temperature. Beneath the surface, X-ray Wavelength Dispersive Spectroscopy (WDS) in a Scanning Electron Microscope (SEM) indicates relatively higher nitrogen concentrations (up to 12 at.%) within the diffusion layer while microscopic nitrides are not formed and existing carbides are not dissolved. Moreover, in the diffusion layer, nitrogen is found to be dispersed in the matrix and forming nanosized precipitates. The small coherent precipitates are observed by High-Resolution Transmission Electron Microscopy (HR-TEM) while the presence of nitrogen is confirmed by electron energy loss spectroscopy (EELS). Hardness tests show that the material hardness increases linearly with the nitrogen concentration, reaching up to 14.5 GPa in the surface while the Young Modulus remains essentially unaffected. Indeed, the original steel microstructure is well preserved even in the nitrogen diffusion layer. Nitrogen profiles show a case depth of about ~43 microns after nine hours of nitriding process. These results indicate that pulsed plasma nitriding is highly efficient even at such low temperatures and that at this process temperature it is possible to form thick and hard nitrided layers with satisfactory mechanical properties. This process can be particularly interesting to enhance the surface hardness of tool steels without exposing the workpiece to high temperatures and altering its bulk microstructure.
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Due to the mechanical and inertness properties of the Epsilon phase, its formation as a compact monolayer is most wanted in plasma surface treatments of steels. This phase can be obtained by the inclusion of carbon species in the plasma. In this work, we present a systematic study of the carbon influence on the compound layer in an AISI H13 tool steel by pulsed plasma nitrocarburizing process with different gaseous ratios.
The existence of semiconductors exhibiting long-range ferromagnetic ordering at room temperature still is controversial. One particularly important issue is the presence of secondary magnetic phases such as clusters, segregations, etc... These are often tedious to detect, leading to contradictory interpretations. We show that in our cobalt doped ZnO films grown homoepitaxially on single crystalline ZnO substrates the magnetism unambiguously stems from metallic cobalt nano-inclusions. The magnetic behavior was investigated by SQUID magnetometry, x-ray magnetic circular dichroism, and AC susceptibility measurements. The results were correlated to a detailed microstructural analysis based on high resolution x-ray diffraction, transmission electron microscopy, and electron-spectroscopic imaging. No evidence for carrier mediated ferromagnetic exchange between diluted cobalt moments was found. In contrast, the combined data provide clear evidence that the observed room temperature ferromagnetic-like behavior originates from nanometer sized superparamagnetic metallic cobalt precipitates.
The modification of steel (AISI 316L and AISI 4140) surface morphology and underlying inter-crystalline grains strain due to Xe$^+$ ion bombardment are reported to affect nitrogen diffusion after a pulsed plasma nitriding process. The ion bombardment induces regular nanometric patterns and increases the roughness of the material surface. The strain induced by the noble gas bombardment is observed in depths which are orders of magnitude larger than the projectiles stopping distance. The pre-bombarded samples show peculiar microstructures formed in the nitrided layers, modifying the in-depth hardness profile. Unlike the double nitrided layer normally obtained in austenitic stainless steel by pulsed plasma nitriding process, the Xe$^+$ pre-bombardment treatment leads to a single thick compact layer. In nitrided pre-bombarded AISI 4140 steel, the diffusion zone shows long iron nitride needle-shaped precipitates, while in non-pre-bombarded samples finer precipitates are distributed in the material.
In this paper we report the effect of hydrogen on the structural properties of AISI-H13 steel nitrogen-implanted samples in low oxygen partial pressure atmosphere. The samples were implanted in a high vacuum chamber by using a broad ion beam source. The H2+/N2+ ion composition of the beam was varied and the surface composition studied in situ by photoemission electron spectroscopy (XPS). The samples were also ex situ analyzed by X-ray diffraction and scanning electron microscopy (SEM), including energy-dispersive spectroscopy measurements. It was found that hydrogen has the effect of modifying the amount of retained nitrogen at the surfaces. This result shows that hydrogen plays a role beyond the well-established effect of oxygen etching in industrial machines where vacuum is relatively less well controlled. Finally, an optimum concentration of 20 to 40% [H2]/[H2+N2] ion beam composition was determined to obtain maximum nitrogen incorporation on the metal surface.
The nitrocarburization of the AISI-H13 tool steel by ion beam assisted deposition is reported. In this technique, a carbon film is continuously deposited over the sample by the ion beam sputtering of a carbon target while a second ion source is used to bombard the sample with low energy nitrogen ions. The results show that the presence of carbon has an important impact on the crystalline and microstructural properties of the material without modification of the case depth.
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