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Determination of borides in Fe-Mo-B sintered powders using diffraction methods

Karwan-Baczewska J., Perek-Nowak M., Majchrowska M., Garbacz-Klempka A.

Archives of Materials Science and Engineering

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2024

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Vol. 127, nr 1

5--11

EN

Purpose: Modification of sintered iron with the addition of molybdenum and boron leads to the formation of boride phases that significantly impact the properties of the sintered materials. The paper aims to determine Fe-Mo-B phases that might be formed during the sintering of base powders. With EDS microanalysis, determining those phases in the microstructure is difficult since the B-Kα peak is extremely close to Mo-Mζ (only a 9.3 eV difference). Thus, diffraction techniques must be implemented to unambiguously define the phases occurring in the sintered samples (WDS and EBSD). Design/methodology/approach: The sintered samples were obtained from initial powders of Fe, Mo, and B that were mixed and compressed. The reducing hydrogen atmosphere was used to sinter green samples at 1200°C for 60 minutes. The obtained sinters were subjected to microstructural observations by scanning electron microscope, and some analyses (EDS/WDS and EBSD) were conducted, which led to the determination of phases present in the material. Findings: Based on the investigations conducted, iron, molybdenum, and molybdenum-iron borides have been reported. It is confirmed with the EBSD method that Fe2B, MoB and FeMo2B2 phases are formed in particles’ connection regions. Besides, the interparticle region, formed due to a liquid phase during sintering, is based on Fe-Fe2B eutectic. The microstructural observations prove that the amount of the liquid phase, and thus the size of the interparticle region, diminishes with increasing molybdenum content. It was also noted that the iron matrix (interior of former iron particles) is free from contributing elements coming from boron or molybdenum powders. Research limitations/implications: The application of the EDS method is limited in the case of measuring boron in Mo-containing alloys and phases. The EDS method does not have a sufficient energetic resolution to separate the B-Kα line from Mo-Mζ one. Thus, it must be complemented with WDS and EBSD in order to unambiguously determine the presence and localization of iron and molybdenum borides. Practical implications: It can be stated that WDS has sufficient energy resolution to separate B-Kα from Mo-Mζ emission lines. Therefore, WDS analysis is suitable for boride observation in sintered iron powders by constructing distribution maps of interparticle connection regions and precipitates. Besides, measurements by the EBSD method can be used to confirm the presence of Fe2B, MoB and FeMo2B2 phases. Originality/value: Determination of boron-containing phases in Fe-Mo-B sinters by means of diffraction methods.

2

Effect of Particle Size of a Powder upon the Properties and Microstructure of Boron-modified Fe-Ni-Mo-Cu Sinters

Karwan-Baczewska Joanna, Perek-Nowak Małgorzata, Majchrowska Magdalena, Rosso Mario

Journal of Casting & Materials Engineering

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2023

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Vol. 7, no. 1

1--8

EN

The article discusses the effect of different particle fractions of prealloyed iron powder on the microstructure, density and hardness of sintered material. Each particle fraction (apart from 160–200 µm, which is a trace fraction) was modified with boron, its contents being, respectively, 0.2 wt.%, 0.4 wt.% and 0.6 wt.%. Next, the powder mixtures were pressed under a pressure of 600 MPa, and the final compacts were subject to sintering at 1200°C for 60 min in a hydrogen atmosphere. It was observed that the higher values of density and hardness were found in samples made from finer fractions of powder. A higher homogeneity of the microstructure and the highest degree of compactness was obtained in sinters from powder of 40–56 µm particle size, with 0.4 wt.% boron. Due to the use of small particle fractions of prealloyed powder, a higher degree of compactness in sinters was obtained with lower boron content. Also indicated was which particle fraction of Fe-Ni-Mo-Cu powder should be applied to obtain density in sinters with boron addition equal to almost 100% of the relative density of the analyzed alloy. The presented studies have both scientific and technological aspects.

3

The influence of chromium compounds on boron carbide sintering

Rutkowski P., Stobierski L., Bućko M.

Composites Theory and Practice

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2013

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R. 13, nr 4

245--249

EN

The paper concerns the activated sintering of boron carbide based materials. The work shows the influence of introduced Cr3C2, CrSi2, Cr3Si modifiers on the sintering of commercial boron carbide. A high-temperature graphite dilatometer was used in order to investigate boron carbide sintering with various additives. The shift of the onset and endset sintering temperature of different sample compositions was determined. The influence of chromium compounds on sintering was explained by XRD phase analysis. The phase changes in the sinters vs. increasing volume fraction of the additives were made. The same analyses were made on samples heat-treated close to the onset sintering temperature.

PL

Artykuł dotyczy aktywowanego spiekania materiałów na osnowie węglika boru. W pracy przedstawiono wpływ dodatku wprowadzonych modyfikatorów w postaci Cr3C2, CrSi2orazCr3Si na spiekanie komercyjnego węglika boru. Do badań użyto wysokotemperaturowego grafitowego dylatometru w celu prześledzenia przebiegu procesu spiekania węglika boru ze zmienną zwartością różnych dodatków. W ramach badań dylatometrycznych określono przesunięcie temperatury początku i końca spiekania dla różnych przygotowanych składów materiałowych. Wpływ dodatków związków na bazie chromu na spiekanie badanych tworzyw wyjaśniono przy użyciu analizy XRD. Przeprowadzono analizę zmian fazowych spieków w funkcji wzrastającego udziału objętościowego dodatków. Te same badania wykonano również dla wybranych składów wygrzewanych w temperaturach bliskich temperaturze początku spiekania. Przeprowadzono obserwacje mikrostrukturalne SEM.

4

The properties of Fe-Ni-Mo-Cu-B materials produced via liquid phase sintering

Karwan-Baczewska J.

Archives of Metallurgy and Materials

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2011

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Vol. 56, iss. 3

789-796

EN

Sintered materials base on pre-alloyed powders (Fe-Ni-Mo-Cu) are expansively applied in the automotive industry. However, their applications are limited by the particular porosity values of those materials. To reduce the porosity and, simultaneously, to increase the consolidation of sintered alloys, miscellaneous methods within powder metallurgy technologies are utilised, as well as an activated sintering process; for example some boron is added. The boron and iron built a system that is not soluble in any of the three allotropic forms of iron. While sintering at a temperature higher than 1433 K, a permanent liquid phase was generated as a result of a eutectic reaction between iron and Fe2B. Owing to the limited boron solubility in iron, a liquid phase was continuously present during the sintering process, influence changes in the morphology of the porosity and the increase in density, also mechanical properties. In addition, boron showed a strong chemical affinity to oxygen; in sintering process it reacted with a chemically bound oxygen on the surface of powder particles and it simultaneously activated the sintering process. The paper presents the production of sintered materials based on Höganäs Distaloy SA (Fe-1.75% Ni-0.5% Mo-1.5% Cu) powder modified by boron powder in amounts of 0%, 0.2%, 0.4% and 0.6%. Alloys were manufactured using powder metallurgy technology through mixing of powders, compacting at 600 MPa pressure and sintering at 1473 K, during 30 minutes in hydrogen atmosphere. One of the phenomenon, which exists on the surface of sinters made from boron modified pre-alloyed powders (Fe-Ni-Mo-Cu) type Distaloy SA is creating a thickened layer. The similar thickened layer was observed also on the surface of another samples base on pre-alloyed powders with boron addition. As well as the properties: density, hardness, tensile strength were examined and microstructure investigations were performed. Experimental results showed that if boron was added, while sintering, the shrinkage phenomena increased and properties were improved.

PL

Materiały spiekane na osnowie stopowanego proszku Fe-Ni-Mo-Cu znajdują szerokie zastosowanie w przemyśle motoryzacyjnym. Jednakże ze względu na pewien stopień porowatości tych materiałów ich wykorzystanie jest ograniczone. Ażeby obniżyć porowatość i równocześnie podwyższyć zagęszczenie stopów spiekanych stosuje się różne warianty technologii metalurgii proszków oraz procesy aktywowanego spiekania, na przykład poprzez wprowadzenie dodatku boru. Bor tworzy z żelazem układ o prawie całkowitym braku rozpuszczalności w obu odmianach alotropowych Przy spiekaniu powyżej 1143 K w wyniku reakcji eutektycznej pomiędzy żelazem a Fe2B tworzy się faza ciekła. Wskutek ograniczonej rozpuszczalności boru w żelazie proces spiekania przebiega przy ciągłej obecności fazy ciekłej, co w konsekwencji wpływa na zmiany w morfologii porowatości, wzrost zagęszczenia i podwyższenie właściwości mechanicznych. Ponadto bor posiada bardzo silne powinowactwo chemiczne do tlenu i podczas procesu spiekania reaguje z chemicznie związanym tlenem na powierzchni cząstek proszku i równocześnie aktywizuje proces spiekania. W artykule omówiono proces wytworzenia stopów na osnowie proszku Distaloy SA (Fe-1.75% Ni-0.5% Mo-1.5% Cu) produkcji firmy Höganäs, modyfikowanego borem w ilości 0%, 0.2%, 0.4% i 0.6%. Powyższe stopy były otrzymywane metodą metalurgii proszków w wyniku mieszania proszków, prasowania pod ciśnieniem 600 MPa i spiekania przy temperaturze 1473 K, podczas 30 minut, w atmosferze wodoru. Jednym z ciekawych zjawisk występujących podczas spiekania proszków Fe-Ni-Mo-Cu z gatunku Distaloy z dodatkiem boru jest występowanie zagęszczonej bezporowatej strefy, której grubość zmniejsza się wraz ze wzrostem zawartości boru. Podobne warstwy tworzą się na powierzchni spiekanych stopów na osnowie innych stopowanych proszków modyfikowanych borem. W toku eksperymentów oznaczono gęstość, twardość i wytrzymałość analizowanych próbek oraz przeprowadzono badania strukturalne. Wykazano, że dodatek boru do proszków stopowanych podczas procesu spiekania odpowiada za zjawisko skurczu oraz wpływa na podwyższenie właściwości analizowanych próbek.