Chapter 3

Literature review

1. The effect of powder metallurgy process parameters on

mechanical properties of micro and nano-iron powder
Abstract
The ever-increasing development of applying the iron pieces made by powder metallurgy in car industries and other usages depends on making pieces with high density and consequently acceptable physical and mechanical properties. Regarding the effect of decrease in the powder bits size on improvement of the mechanical characteristics and on decrease in the temperature of sinter, the experiments on the pure iron powder with the bits size of 5, 45, 63 micron in which 20% of iron nano powder was added to the powder with the bits size of 45 micron, have been studied. Mere iron nano powder also was applied for experiments. Pieces are compacted under 300-850 MPa and lubricants by0.4 and 0.6 percent of the total weight was mixed withthe powders. Various amounts of sintering time and sintering temperature were considered for the sintering of the samples. The survey suggested that applying micro powders resulted in an increase in the linear density and the strength at the relatively high temperatures and high keeping times. Sintering temperature and shrinkage has declined considerably with the decrease in thepowder size and as a result the strength increases. High strength for products made by smaller powders under high pressures and low sintering temperatures using lubricated frame wall are obtained. SEM pictures from the fracture junctions of the samples show the decrease in porosity due to the close impact of the smaller powder size.

1. Introduction
In the powder metallurgy process, the industrial pieces are produced through compacting powder in the frame and sintering within a controlled setting. As a natural character of powder metallurgy process a disadvantage is the production of a work piece with poor mechanical properties due to its porosity. High needed pressure and sintering temperature and long sintering periodhinder the application of this process because of increasing process cost. The powder size, as an important parameter, has the potential to remove aforementioned drawbacks, as typically the temperature of sinter for the smaller powders goes down and also higher strengthened products are achieved using smaller powder sizes (Squire, 1947 and Park et al., 2004 and GibbsThomson,2003 and Fillabi et al., 2008). Sintering temperature, pressure, keeping time, powder density, and bits size are the most important parameters on which the hardness of the produced piece is dependent on. The researches have shown that the effects of the parameters on the hardness are very intricate and their influence may change when the size of the particle decreases. The results suggest that in the sintering operation of the nano powder of the tungsten alloy 90W-Ni-fe, the hardness decreases with the increase in the sintering temperature for small powders (Faridakhtar, 2008 and Meilakh, 2009). Smaller micro and nano powders are increasingly applied in powder metallurgy process due to their special characteristics (Chen et al., 1997 and Wang et al., 2003).Particles with diameter of less than 100 nanometer, in comparison with the bigger particles have higher surface to volume ratio which initiates different characteristics (Chio et al., 2002).These new characteristics such as high surface area result in the intense decrease in sintering temperature, severe viscidity, and unique erosion resistance and

favorable mechanical features (Chio et al.,2002). Powder size is so influential on dimension variation during sintering. For smaller powders more compaction happens in acertain sintering time. Furthermore the speed of compaction for smaller powders is remarkably faster than that for bigger powders(Cheney et al., 1965). Moreover, the effect of particles size, on the time and temperature of the sintering of the composite pieces,AL-AL2O3, is surveyed. The results indicate that when the size of the particle decreases, both product hardness and strength increase. In addition, the highest hardness is achieved in the pieces made with smaller particles and the moderate keeping time and temperatures. An Increase in time and temperature results in a decrease in hardness and strength which could be due to the particles growth (Rahimian, 2009). Researches on nano powder sintering using SPS process show that needed sintering temperature for Nan powder is 200-500 degree less than that for normal size powders (Angerer et al., 2005). With increase in density and increase in compacting pressure and sintering time and temperature, mechanical properties like tensile strength and elongation improves. With increase in sintering time, mostly there is no change in strength and density even though toughness ofthe product increases. When lubricant is added to the raw powder, density decreases linearly (Libsch et al., 1970 and Babakhani etal., 2006). Koch reported that when powder size decreases, flexibility increases and it seems nano powder can increase flexibility of the product (Koch et al., 1999 and Koch, 2003). applying higher pressure number of contacting points increases, thus load carrying capacity of the work piece increases too (Chin et al., 2005). In this paper the effect of process parameters on the productdensity and consequently on product tensile strength is investigated. Powder size, keeping time, pressure and sintering temperatures are considered as the most influential parameters in powder metallurgy.

2. Material properties and research method

In this research, the powder metallurgy operation using the iron powder with 99.7 purity and size of 5, 45 and 63 microns with additional 20% of nano powder to the set with 45 micron iron and also mere iron nano powder are performed. Iron nano powder is produced using the planet miller; Fritsch P-6, in which bullets and container are made of high strength steel. In this research ,bullet/powder weight proportion (BPR) of 10:1, milling time of 27 hours, and the miller rotation speed of 600 rpm are used for milling. Alcohol is used to dilute the process (Suryanarayana,2005). Figure 1 shows scanned electron microscope (SEM) picture of the product cross section. Characteristics of the part produced by powders with the average size of 80 nm are listed in the Table1. Powder of zinc STEARAT with low melting point and approximate density of 1.09 g/cm3 is used as lubricant in the powder mixture. The effect of frame wall lubrication was also investigated.

Conclusion and result

In this paper tensile strength of samples with different iron Micro-powder size of 63_m, 45_m, 5_m, 45_m and addition of 20% of the nano powder and also iron nano powder with average size of 80nm was investigated experimentally. the effect of process parameters such as sintering temperature, keeping time and compaction pressure on tensile strength was studied and followings results are obtained: Decrease in powder size in order to achieve a high raw density needs a very high pressure. As density goes up with compression, temperature and keeping time, mechanical characteristics and particularly tensile strength improves. in smaller powders, regarding high sensitivity of surface diffusion mechanisms to the bit size and increase in sintering activation energy, higher density is established at lower temperatures and medium keeping times;

 With decrease in necessary sintering temperature need of sinter-assisted materials can be neglected and the sintering costs are decreased. The strength of samples made by smaller powders is higher because they need higher compaction pressure which decreases samples porosity. The powder size has intense effect on the dimensional changes in sintering. For a specified sintering time, more bits in smaller powders are accumulated and consequently accumulation speed for smaller powders is considerably faster. With increase in the percentage of the lubricant in the powder mixture, the samples raw density decrease

2. CHARACTERIZATION OF THE PASSIVE FILM ON MILD STEEL IN CO2 ENVIRONMENTS. Jiabin Han, Passivation of the steel beneath a primary iron carbonate layer was elucidated to
play a key role in the localized CO2 corrosion of mild steel. Identification of the phases which constitute the film furthers the understanding of the localized corrosion mechanism. Scanning electron microscopy and X-ray diffraction indicated that FeCO3 was initially formed under the test conditions, but it failed to passivate the surface. After most of the steel surface was covered with the FeCO3 layer, passivation was observed during the spontaneous passivation tests. Surface analysis by grazing incidence X-ray diffraction indicated that an additional trace Fe3O4 phase, magnetite, was identified after the passivation of the coupon was complete, compared with the non-passive coupon with an exclusively FeCO3 layer. The dominant phase that constituted the passive film was FeCO3 (99.6%) while the Fe3O4 phase (0.4%) plays a key role in the passivation process. These results were confirmed using Rutherford Backscattering analysis.

Conclusion: Crystalline iron carbonate formed in the first phase of the CO2 corrosion
experiments on mild steel and formed a macroscopic product layer. The secondary formed passive film was preliminarily identified to be Fe3O4 under the test conditions. GIXRD (grazing

incidence XRD) analysis shows only a trace amount of it (i.e. very thin passive film) which is critical to the process of passivation.

3.Steel.O.S.I Fayomi In the area of Zinc coating research is unending because of its unique
property and low cost. In this paper, the mechanical (wear and hardness) and corrosion behaviors of Zn Coated Mild Steel in 3.65% NaCl is described. A thin film of Zn on steel substrates was prepared by electro deposition technique using Zn particles to form a bath plating solution. Scanning electron microscope and Atomic force microscope were used to study the surface morphology, the topography and the surface adherent properties of the coatings. The crystal particles present were observed by X-ray diffraction pattern (XRD) and energy dispersive X-ray diffraction spectrometer (EDS). The hardness of deposited plate, the electrochemical behavior and the corrosion properties of the deposits were investigated by means of Vickers hardness tester and polarization measurements.

Conclusion:
The average increase in hardness of the mild steel substrate was 55 HVN to deposited sample Zn 3 was 108 HVN, about twice the hardness value of the mild steel was achieved. The corrosion resistance of mild steel was improved after zinc deposition

4 . An Investigation of the Properties of Zn Coated Mild Steel

Researches in the area of zinc coatings on steel are rather unending because of the unique properties and the very low cost that it offers. In this paper, the mechanical (wear and hardness) and corrosion behaviours of Zn Coated Mild Steel in 3.65% NaCl are described. A thin film of Zn on steel substrates was prepared by electrodeposition technique using Zn particles to form a bath plating solution. Scanning electron microscope and Atomic force microscope were used to study the surface morphology, the topography and the surface adherent properties of the coatings. The crystal particles present were observed by X-ray diffraction pattern (XRD) and energy dispersive X-ray diffraction spectrometer (EDS). The microhardness of deposited plate, the electrochemical behavior and the corrosion properties of the deposits were investigated by means of Vickers microhardness and polarization measurements. The uniform deposits of Zn showed fine grains and good protection against corrosion as appreciated 75% hardness value was achieved.

CONCLUSION

Proper electrodeposition of mild steel using zinc particle was carried out. The microhardness and corrosion behaviour of the resultant deposition were investigated with the following deductions: rdness of the mild steel substrate was 55 HVN to deposited sample Zn 3 was 108 HVN, about twice the microhardness value of the mild steel was achieved. produced with the highest applied voltage displayed the best microhardness value, and had the highest corrosion resistance. This was featured by a decrease in corrosion current density and corrosion current, increase corrosion potential and the polarization resistance. , meaning that only few hydrated ion(s) in the electrolyte migrated toward the cathode under the influence of the applied voltage. s sample 3>2>1. 5. EXPERIMENTAL RESEARCH ON CREATING FUNCTIONAL MODELS BY POWDER METALLURGY IN THE AUSTENITIC STAINLESS STEEL ALUMINA SYSTEM ABSTRACT: This paper sets out to present experimental research done on a mixture of powders of austenitic stainless steel AISI316 L and alumina, out of which bush type pieces (valve seats for automobiles) were created by powder aggregation. The dimensions were: exterior diameter: 34mm, interior diameter: 21mm and height: 11mm. In the specially designed cast for this experiment, 2 sets of 9 samples each were created from mixtures of stainless steel, 10, 20 and 30% Al2O3 and 0.5% Zinc stearate.Two values were chosen for pressing forces: 400 kN and 200 kN. After pressing, the mass variation of the samples sintered at 1200C for 1 h was analyzed, and the micro structural aspect. It was noted that the samples containing 20% Al2O3 had the least mass variation and present the most uniform structure, both by particle size and by homogeneity. KEY WORDS: powder metallurgy, stainless steel, alumina, sintered, experimental 5. CONCLUSIONS Functional models, created in 2 sets of 9 samples each, are bush type parts and present a uniform pressing degree and have a relatively homogenous structure for both values of the pressing force used: 400 kN and 200 kN. The dosage of the powder mixture was donegravimetrically, but we recommend volumetric dosage for mass production. The dimensions and mass variations of the samples have low values, specific to the process of manufacturing by pressing the powder mixture intomolds. The design of a new mold was necessary, toinsure guidance on two columns and to provide modular elements in order to be able to manufacturea variety of types and dimensions of parts manufactured by powder metallurgy. Experimental research was continued with themetallographic study of the samples, determination of hardness (HB and HV 0.1), corrosion tests in acid solution environments and abrasive wear.

6.RESEARCH ON COPPER ALUMINA COMPOSITE MATERIALSOBTAINED BY POWDERS METALLURGY

ABSTRACT: The paper presents the experimental research related to the obtaining of copperalumina composite. The copper-alumina composite material was obtained by procedures specific to powder metallurgy. The structure was analyzed by electron microscopy (SEM). The mechanical and electrical properties and the behavior during welding have been studied. KEY WORDS: powders metallurgy, copper powder, alumina RESULTS AND DISCUSSIONS The green density of the compressed samples depends on the compaction pressure, between 8.10 to 8.40 g/cm3. The density of sintering samples is between 8.01 to 8.32 g/cm3. The distribution of the alumina particles is shown in figure 4. We can notice relatively uniform distribution of aluminum oxide particles in the matrix.

Figure1: SEM image of the Cu-1%Al2O3 material, 200x zoom The hardness was determined by theBrinell method. The average values of thehardness have values between 35 40 HB.The electrical conductibility values wereinfluenced both the pressure and sintering parameters and the content of Al2O3. Electrical conductivity of the obtained Cu-Al2O3 material ranges around the value of 50-60% IACS.I made a simulation of the extrusion process withthe help of the software to determine the dimensions of to extruding toolsas the work parameter. Figure 2 is illustrated theextruding process and value mean stress in workpiece.Due to the low

hardness electrodes, the samples have been maintained for one hour at 950 degrees in inert atmosphere and aftercoolness, the cylindrical samples were coldextruded by an extrusion die, reducing thesample diameter from 20 to 14 mm. Thepressure value applied to extrusion was of 750 MPa.After the extrusion the samples hardening has increased at 110 HB and therefore it was drawn the conclusion that the material Cu-1% Al2O3 may be strengthened by cold deformation.

Figure 2: Value mean stress in work piece The analyzing micro structure after recrystallization process and plastic deformation shows the active part of the alumina particles upon the structure.In the initial microstructure the alumina particles were distributed in the boundary crystalline grains, and after recrystallization it is being observed inside the crystalline grains and at theboundary crystalline grain.he average values of micro hardness HV0.1 after extrusion have values between 110-125 HV, andthe figure 6 is shown a picture of hardness impression. CONCLUSIONS We obtained satisfactory distribution of alumina oxide particles in the copper matrixmass.The materials conductivity, after particle reinforcement, should be maintained in the50 -60% range IACS, in order to have acceptable current efficiency. Current density in thematerials changes, since the reinforcing particles have lower conductivity than the matrix.The hardness of the material copperalumina significantly improved after cold extrudedby an extrusion die.The alumina particles incorporated in the matrix of copper contribute to the hardening ofthe metallic matrix