Semi-closed Container Research Articles

The Effect of Mn Content on the Structure and Properties of PM Mn Steels

AbstractThe aim of the study was to examine how a reduction of Mn content in PM steels will affect their plastic and strength properties. The results of mechanical, metallographic and fractography tests of sintered (PM) steels containing 1% and 2% Mn are reported and compared with those for 3% Mn PM steel. Höganäs iron powder grade NC 100.24, low-carbon ferromanganese Elkem and graphite powder grade C-UF were used as the starting powders. Powder mixes Fe-(1-2)%Mn-0.8%C were prepared in a Turbula mixer for 30 minutes. Following mixing, “dog bone” compacts were single pressed at 660 MPa, according to PN-EN ISO 2740 standard. Sintering of compacts was carried out in a laboratory tube furnace at 1120°C and 1250°C for 60 minutes in a mixture of 95%N2– 5%H2in a semi-closed container. Three types of heat treatment were then used: sinterhardening (cooling rate – 66°C/min), slow furnace cooling (cooling rate 3.5°C/min) and tempering at 200°C. The studies have shown a beneficial effect of the reduction of manganese on plastic properties (up to 7.96%), while maintaining fracture strengths (UTSs) comparable to those of steel with higher contents of manganese. Currently detailed studies of steel containing 1%Mn are conducted.

The Effects of Post-Sintering Treatments on Microstructure and Mechanical Properties of Mn-Mo Steel

Abstract The effect of heat treatment on density, hardness, microstructure and tensile properties of Fe-0.85Mo-1.3Mn-0.6C sintered steel were investigated. Pre-alloyed Astaloy 85Mo, ferromanganese and UF4 graphite powders were mixed for 60 minutes in a Turbula mixer and then pressed in single-action die at 660MPa to produce green compacts (according to PN EN ISO 2740).The compacts were sintered in a specially designed semi-closed container at 1120 or 1250°C for 60 minutes in N2. The chemical composition of the sintering atmosphere was modified by adding getter and/or activator into the container. Two different types of heat treatment in nitrogen were carried out: sinteraustempering at 525°C for 60 minutes; and sinterhardening with additional tempering at 200°C for 60 minutes. The slightly better combination of strength and plasticity of steel for both sintering temperatures were achieved after sinterhardening+tempering variant. Average values of 0.2% offset yield stress, ultimate tensile strength and elongation after sintering in 1250°C, were 415MPa, 700MPa, and 2.0%, respectively.

Microatmosphere Sintering of Cr–Mn Steel In Furnace Atmospheres of Flowing Hydrogen and Technical Nitrogen

Chromium-containing steels must be sintered in dry atmospheres with low partial pressures of oxygen, such as nitrogen–hydrogen mixtures. The conventional endogas atmospheres have a potential to carburize the main steel and simultaneously oxidize alloying elements, e.g. Cr and Mn, preventing proper sintering. Fe–1.5% Mn–1.5% Cr–0.25% Mo–0.4% C steel is successfully sintered in flowing technical nitrogen by controlling the local microatmosphere, through the use of semiclosed container/getter/activator combinations. Then, the necessary reducing reactions are induced in the dry microatmosphere within and around the specimens. As manganese has a higher affinity for oxygen than chromium, chromium oxide is reduced by relying only on carbon and manganese in the semi-closed container. Mechanical properties of the specimens sintered in technical nitrogen do not significantly differ from those sintered in dry hydrogen.

Mechanical Properties and Microstructure of PM Mn-Cr-Mo Steels With Low Carbon Concentration

The effect of chemical composition of the sintering atmosphere on the microstructure and mechanical properties of PM structural low-carbon steels is presented. The base powders were Astaloy CrL, Astaloy CrM, low carbon ferromanganese and graphite C-UF. From the base powders two mixtures with compositions of Fe-3%Mn-(1.5/3%)Cr-(0.2/0.5)%Mo-0.2%C were prepared. Following pressing in a steel rigid die, compacts were sintered at 1250°C for 60 min in a semi-closed container. 5%H2-95%N2mixture and air were the sintering atmospheres. For sintering in air, lumps of ferromanganese were placed with the compacts in the container. After sintering, half of the samples were tempered at 200°C for 60 minutes in air. Mechanical tests (tensile, bend, toughness, hardness) and microstructural investigations were performed.The microstructures of the steels were inhomogeneous, mainly ferritic-bainic. Tempering of steel based on Astaloy CrM sintered in an atmosphere of 5% H2-95% N2slightly reduced tensile strength and toughness: from 748 to 734 MPa and from 7.15 to 6.83 J/cm2, respectively. Chemical composition had a greater effect; steels based on Astaloy CrL and Astaloy CrM had tensile strengths 526-665 and 672-748 MPa, hardness 280-325 and 388-421 HV, respectively. The best properties were obtained after sintering in air of Fe-3%Mn-3%Cr-0.5%Mo-0.2%C without heat treatment: tensile strength 672 MPa, toughness 6.93 J/cm2, hardness 421.1 HV, 0.2 % offset yield strength 395 MPa.

Sinteraustempering Of Two Mo-(Cu)-(Cr)-(Ni)-(Mn)-C Steels In A Semi-Closed Container In Flowing Nitrogen

Abstract Three types of heat treatment, sinteraustempering in 500°C, 400°C and 350°C; sinterhardening and sintering with cooling at the rate 10K/min) as the final operation, on steels sintered semi-closed container were investigated. Results of mechanical properties, microstructure investigations and fracture and EDX analyses are reported. The study involved two PM steels: DH-1 (Fe-2%Cu-1.5%Mo-0.5%C) and 34HNM (Fe-0.2%Mo-0.8%Mn-1.5%Cr-1.5Ni-0.4%C). Prealloyed Höganäs DH (Direct Hardening) iron powder and graphite powder (grade C-UF) were used to produce DH-1 steel. Prealloyed Astaloy CrL iron powder, low carbon ferromanganese, elemental nickel and graphite grade C-UF powder were the starting powders of 34HNM steel. Pressing was in rigid dies at 660MPa according to PN-EN ISO 2740 standard. After compaction, green compacts were sintered in a specially designed semi-closed container at 1120°C for 60 minutes in a nitrogen atmosphere. The chemical composition of the sintering atmosphere was modified by adding ferromanganese and/or activator into the container. All specimens were tested for tensile strength (UTS), elongation (A), yield offset strength (R0,2), TRS, apparent surface and cross section hardness (HV 30). The best combination of strength and plasticity for both steels was achieved after sinteraustempering at 500°C. The results show that, using the specially designed semi-closed container, sinteraustempering in N2 atmosphere offers the same or even better mechanical properties in comparison with sinteraustempering in vacuum. It means that sinteraustempering in N2 atmosphere is a very interesting process in terms of cost in comparison with vacuum sinteraustempering.

Chemical reactions during sintering of Fe-Cr-Mn-Si-Ni-Mo-C-steels with special reference to processing in semi-closed containers

Sintering of Cr, Mn and Si bearing steels has recently attracted both experimental and theoretical attention and processing in semiclosed containers has been reproposed. This paper brings together relevant thermodynamic data and considers the kinetics of some relevant chemical reactions. These involve iron and carbon, water vapour, carbon monoxide and dioxide, hydrogen and nitrogen of the sintering atmospheres and the alloying elements Cr, Mn, Mo and Si. The paper concludes by presenting mechanical properties data for three steels sintered in local microatmosphere with nitrogen, hydrogen, nitrogen-5% hydrogen and air as the furnace gas.

The use of Weibull Statistics to Quantify Property Variability in Fe-3Mn-0.8C Sinter-Hardened Structurally Inhomogeneous Steels

Abstract Low carbon ferro-manganese and graphite powders were admixed to Hoganas sponge, NC100.24, and water atomised, ABC 100.30 and ASC 100.29, iron powders - to produce three variants of sintered Fe-3Mn-0.8C steel. These were pressed into tensile and bend specimens at 660 MPa, sintered in semi-closed containers for 1 hour in dry nitrogen or hydrogen at 1120 or 1250°C and cooled at 64°C/min. Both tensile strength and transverse rupture strength were examined using Weibull statistics. This paper presents the results of a study to develop and evaluate goodness of fit tests for the two- and three-parameter Weibull distributions. The study was initiated because of discrepancies in published critical values for two-parameter Weibull distribution goodness of fit tests and the lack of general three-parameter Weibull distribution goodness of fit tests for properties of PM steels.

A novel method of sintering hybrid steels in an improved semiclosed container system

Conventional sintering techniques for structural steels have been developed principally for Cu and Ni containing alloys. Applying these to Cr and Mn steels (successful products of traditional metallurgy) encounter the problem of the high affinity for oxygen of these elements. A solution is employing a microatmosphere in a semiclosed container which favours reduction reactions. This has already proved successful on a laboratory scale, especially with nitrogen as the furnace gas. Further modifications to the system, now described, include the use of two sintering boxes, one inside the other. Superior mechanical properties, even using air as the furnace gas, are attainable.

The Formation of an Epitaxial-Graphene Cap Layer for Post-Implantation High Temperature Annealing of SiC and its <i>In Situ</i> Removal by Si-Vapor Etching

As a new graphene functionality applicable to post-implantation high temperature annealing of SiC, a method of in situ formation and removal of large area epitaxial few-layer graphene on 4H-SiC(0001) Si-face is proposed. It is demonstrated that the homogeneous graphene layer formed by Si sublimation can be preserved without the decomposition of the underlying SiC substrate even in the excess of 2000 oC in ultrahigh vacuum. It is due to the existence of the stable (6√3×6√3) buffer layer at the interface. To ensure this cap function, the homogeneity of the interface must be guaranteed. In order to do that, precise control of the initial SiC surface flatness is required. Si-vapor etching is a simple and versatile SiC surface pre/post- treatment method, where thermally decomposed SiC surface is compensated by a Si-vapor flux from Si solid source in the same semi-closed TaC container. While this Si-vapor etching allows precise control of SiC etch depth and surface step-terrace structures, it also provides a “decap” function to remove of the graphene layer. The surface properties after the each process were characterized by AFM and Raman spectroscopy.

Ethylene insensitivity does not increase leaf area or relative growth rate in Arabidopsis, Nicotiana tabacum, and Petunia x hybrida.

The plant hormone ethylene plays a role in various growth related processes. In this detailed study of the vegetative growth of Arabidopsis, Nicotiana tabacum, and Petunia x hybrida plants, we show that ethylene insensitivity does not result in an increased total leaf area or relative growth rate (RGR) under optimal growth conditions. When grown in semiclosed containers, leaf area of ethylene-insensitive plants was larger compared to the wild type. This effect was caused by a buildup of ethylene inside these containers, which inhibited the growth of wild-type plants. Ethylene-insensitive Arabidopsis and N. tabacum plants had a lower biomass, which was mainly the result of a smaller seed mass. RGR of vegetative plants was not affected by ethylene insensitivity, but the underlying components of RGR differed; specific leaf area (leaf area per unit leaf mass) was higher, and unit leaf rate (growth rate per unit leaf area) was lower. The latter was a result of a slower rate of photosynthesis per unit leaf area in the ethylene-insensitive plants.

Industrial processing, microstructures and mechanical properties of Fe–(2–4)Mn (–0.85Mo)–(0.3–0.7)C sintered steels

The potential of PM Mn steels has been established in laboratory experiments. This paper deals with sintering of Fe–(2–4)Mn–(0.3/0.7)C, also with 0˙85%Mo addition, in an industrial pusher furnace at 1180°C in an atmosphere of 25% hydrogen plus 75% nitrogen, obtained from a cryogenic liquid, giving an inlet dew-point of −55 °C. Tensile, bend (including fatigue) and miniature Charpy specimens were sintered in flowing gases and in semiclosed containers with a getter of ferromanganese, carbon and alumina. The quenched and tem- pered state was investigated, as was sinter hardening (cooling rate of 55 K min −1), simulated for comparison with slow cooling at 10 K min −1. As there was no forma tion of oxide networks at the combination of sintering temperature and dewpoint, in accordance with the Ellingham–Richardson diagram for Mn oxidation/reduction, the use of semiclosed containers was superfluous. The quenched and tempered specimens were brittle. Sinter hardening lead to an improvement in mechanical properties. The reproducibility of tensile and TRS data was high for the sintered materials, characterised by Weibull moduli m of 12–41. All the alloy microstructures were complex and heterogeneous, consisting of, depending on the local manganese and carbon contents, the diffusive and non-diffusive transformation products (pearlite, bainite, martensite) and additionally ferrite and retained austenite. The highest mechanical properties in the entire range of compositions investigated in the furnace cooled state: yield, tensile and bend strengths of 499, 637 and 1280 MPa, respectively, with impact energy of 18 J, and tensile and bend strains of 1˙17 and 1.57%, were achieved for the Fe–2Mn–0.85Mo–0.5C alloy, marginally superior to Fe–2Mn–0.7C. For the sinter hardened Fe–4Mn–0.3C alloy yield, tensile and bend strengths were 570, 664 and 1263 MPa, respectively, at an acceptable impact energy of 14 J, with tensile and bend strains of 0.52% and 1.8%. Many of the results compare favourably with the requirements of MPIF standard 35. Mn is a more effective strengthening agent than either Ni or Cu, or their combination, though generally at reduced plasticity.

Tensile properties of Fe-3Mn-0·6/0·7C steels sinteredin semiclosed containers in dry hydrogen, nitrogen and mixtures thereof

Tensile properties of powder metallurgy 3% manganese-0·8% carbon (content of green compact) steels were determined following laboratory sintering in (nearly) full, semiclosed containers with no getter powders in dry, 0-100% hydrogen-nitrogen atmospheres. Manganese was mixed with the NC 100·24 sponge iron powder as low carbon ferromanganese and carbon as a graphite addition. Dogbone compacts were pressed at 660 MPa, the sintering temperatures were 1120 and 1250°C and cooling rates ~65 K min- 1. In specimens sintered in nitrogen containing atmospheres at 1120°C, final carbon content was ~0·7% and for those processed at 1250°C ~0·6%. Sintering in dry hydrogen resulted in lower carbon and oxygen contents. Independent of the H2/N2 ratio in the furnace atmosphere, however, all the specimens were ductile and exhibited similar strengths. Yield strengths R0·2 were in the range: 426-464 MPa, tensile strengths Rm were 724-780 MPa and strains to failure were 1·6-2·0% after sintering at 1250°C. The 1120°C sintering temperature resulted in 10-15% lower strength values. The microstructures, significantly devoid of oxide networks, comprised mainly mixtures of bainite and fine (divorced) pearlite, with very little martensite and retained austenite. Reproducibly successful sintering of manganese containing compacts requires that reduction conditions exist at the sintering temperature. Ellingham Richardson diagrams dictate that the dewpoints of hydrogen required are-55 and-40°C at 1120 and 1250°C, respectively. A semiclosed container, how ever, ensures a different microclimate. It is suggested that then the initial relevant reactions there are: Mn[vapour]+H2O=MnO+H2, 3Fe2O3 +H2= 2Fe3O4+H2O, Fe3O4+H2=3FeO+H2O, FeO+H2= Fe+H2O and C+O2=CO2, which provide hydrogen andwater vapour,also within the pores. The manganese vapour further acts as a 'shield' by generating further hydrogen from the water vapour. The following reactions involving carbon monoxide are postulated above 927°C, when CO is a more effective reducing agent than hydrogen: C+H2O=H2+CO, 3Fe2O3+ CO=2Fe3O4+CO2, Fe3O4+CO=3FeO+CO2, FeO+CO=Fe+CO2 and C+CO2=2CO. Accordingly, irrespective of whether it is hydrogen or nitrogen in the semiclosed container, if there is a supply of carbon, reducing conditions prevail at the sintering temperature,embrittling oxidenetworks arenot formed and ductile manganese steels are processed.

Wet-Fixation Process for Improved Durable-Press Cotton1

This paper is concerned with a new research development for imparting durable press to cotton in which finishing resins are deposited inside the wet, swollen cotton fiber. This is accomplished by padding an N-methylol resin-mineral acid solution on the fabric, heating the fabric in a closed or semi-closed container for 15 min at 180° F, neutralizing in sodium carbonate solution, washing, and drying. The heating results in deposition of the resin in the fiber in such a manner that it is not removed by washing and so sustains the fibers in a somewhat swollen condition. Subsequent application of cross-linking catalyst followed by a high-temperature dry cure results in only modest loss of fabric strength compared with conventional pad-dry-cure processing. The key to arriving at good strength properties of the finished fabric and high levels of fabric performance, both in resistance to wrinkling and good crease retention, lies in the use of two resin components. One of these, called a polymer builder, acts to swell the fibers and keep them in a swollen state (melamines are particularly effective in this regard) ; the second component is primarily a cross-linking agent for cotton, contributing only moderately to the swelling of the fiber but enhancing wet wrinkle recovery and, once catalyzed and dried, imparting high dry wrinkle recovery to the fabric (dihydroxy dimethylolethylene urea and methylol carbamates are good examples of this class). A total dry resin add-on of 8% to 15% is required to achieve the enhancement of fabric properties. Resin combinations for use on colored goods and white fabrics have been developed. A twill fabric treated by this process in the laboratory gave breaking strength retention values of 60% (filling), dry wrinkle recovery values of 300 degrees, and wash- wear ratings of 5. This fabric, converted to simulated trouser cuffs, showed less wear in laundering than cuffs conventionally finished by pad-dry-cure at comparable perform ance levels. In 20 laundering and tumble-drying cycles, most of the wet-fixed samples were not worn, whereas the pad-dry-cure controls all failed, on the average, at the sixth cycle. Similar results have been obtained in other abrasion tests.