Study of Fe-matrix composites with carbide strengthening, formed by sintering of iron titanides and carbon mechanically activated mixtures

G. Pribytkov, A. Baranovskiy, I. Firsina, Kirill Akimov, Vladimir Krivopalov
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The methods of powder metallurgy combined with preliminary mechanical activation of powder mixtures have become widespread. It is previously established that in mechanically activated powder mixtures of FTi35S5 ferrotitanium, consisting of 82 % of (Fe,Al)2Ti phase, and P-803 carbon black, a reaction occurs with the formation of a composite consisting of a steel binder and titanium carbide. The synthesis reaction of carbides occurs in a solid-phase mode at combustion’s temperatures of 900–950 °C. Therefore, there is no coarsening of the structure due to the growth of carbide particles, which is typical for reactions in the presence of a liquid phase. FTi35S5 alloy contains a plenty of impurities (silicon, aluminum and etc). The purpose of the work is to investigate the phase composition and structure of the products of the interaction of Fe2Ti and FeTi iron titanides with carbon under the conditions of reaction sintering of mechanically activated powder mixtures and to determine the possibility of synthesizing iron-matrix composites strengthened with submicron titanium carbide particles. Research methods. The structure and phase composition of sintered compacts from mechanically activated powders were studied by optical metallography, X-ray diffraction (XRD) and scanning electron microscopy (SEM) using determination of the elemental composition by energy-dispersive X-ray spectroscopy (EDX). Experimental technique. The reaction mixtures were prepared using intermetallic powders obtained by vacuum sintering of compacts from iron and titanium powder mixtures of 2Fe+Ti and Fe+Ti compositions. Carbon black was added to the intermetallic powders to convert all the titanium containing in the intermetallic compounds into carbide. The titanides – carbon black mixtures were processed by an Activator 2S planetary ball mill for 10 min milling time at a rotation speed of 755 rpm (40g). The mechanically activated mixtures were cold compacted into cylindrical samples with a diameter of 20 mm, which were sintered in vacuum at а temperature of 1,200 °C and an isothermal holding time of 60 minutes. Results and discussion. According to the results of X-ray diffraction analysis, almost all titanium contained in iron titanides reacts with carbon to form carbide and reduced iron. The sintering products of compacts of both compositions contain target phases: titanium carbide with a slight shift from the equiatomic ratio and α-iron, which has the lattice parameters close to the reference data, and also a few of other phases. The titanium carbide particles in the iron binder were identified on the back-scattered electron (BSE) images due to the tonal contrast: the heavy iron appears darker against the carbide, which is composed of lighter elements. According to EDX analysis, the relative content of titanium and carbon in the carbide particles indeed corresponds to the composition of non-stoichiometric titanium carbide. Conclusion. The composites including titanium carbide and α-iron binder were obtained by sintering of iron titanides and carbon (carbon black) mechanically activated powder mixtures. The granules of composite powders obtained by crushing of sintered compacts are of interest as feedstocks for wear-resistant coatings and additive technologies, as well as for manufacturing of dense materials by other compaction methods: spark plasma sintering (SPS) or hot pressing (HP).","PeriodicalId":502919,"journal":{"name":"Metal Working and Material Science","volume":" 2","pages":""},"PeriodicalIF":0.0000,"publicationDate":"2024-06-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":null,"platform":"Semanticscholar","paperid":null,"PeriodicalName":"Metal Working and Material Science","FirstCategoryId":"1085","ListUrlMain":"https://doi.org/10.17212/1994-6309-2024-26.2-212-223","RegionNum":0,"RegionCategory":null,"ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"","JCRName":"","Score":null,"Total":0}
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Abstract

Introduction. The addition of dispersed solid particles of refractory compounds (carbides, borides, silicides) to the structure of alloy is a widely used effective way to increase the wear resistance of steels and alloys. Composites with a matrix of iron-based alloys (steel and cast iron) strengthened by titanium carbide particles are of great practical interest. The main structural characteristics, which define hardness and wear resistance of the composites, are volume fraction, dispersion and morphology of the particles of the strengthening carbide phase. The structure of composites depends on the method of its preparation. The methods of powder metallurgy combined with preliminary mechanical activation of powder mixtures have become widespread. It is previously established that in mechanically activated powder mixtures of FTi35S5 ferrotitanium, consisting of 82 % of (Fe,Al)2Ti phase, and P-803 carbon black, a reaction occurs with the formation of a composite consisting of a steel binder and titanium carbide. The synthesis reaction of carbides occurs in a solid-phase mode at combustion’s temperatures of 900–950 °C. Therefore, there is no coarsening of the structure due to the growth of carbide particles, which is typical for reactions in the presence of a liquid phase. FTi35S5 alloy contains a plenty of impurities (silicon, aluminum and etc). The purpose of the work is to investigate the phase composition and structure of the products of the interaction of Fe2Ti and FeTi iron titanides with carbon under the conditions of reaction sintering of mechanically activated powder mixtures and to determine the possibility of synthesizing iron-matrix composites strengthened with submicron titanium carbide particles. Research methods. The structure and phase composition of sintered compacts from mechanically activated powders were studied by optical metallography, X-ray diffraction (XRD) and scanning electron microscopy (SEM) using determination of the elemental composition by energy-dispersive X-ray spectroscopy (EDX). Experimental technique. The reaction mixtures were prepared using intermetallic powders obtained by vacuum sintering of compacts from iron and titanium powder mixtures of 2Fe+Ti and Fe+Ti compositions. Carbon black was added to the intermetallic powders to convert all the titanium containing in the intermetallic compounds into carbide. The titanides – carbon black mixtures were processed by an Activator 2S planetary ball mill for 10 min milling time at a rotation speed of 755 rpm (40g). The mechanically activated mixtures were cold compacted into cylindrical samples with a diameter of 20 mm, which were sintered in vacuum at а temperature of 1,200 °C and an isothermal holding time of 60 minutes. Results and discussion. According to the results of X-ray diffraction analysis, almost all titanium contained in iron titanides reacts with carbon to form carbide and reduced iron. The sintering products of compacts of both compositions contain target phases: titanium carbide with a slight shift from the equiatomic ratio and α-iron, which has the lattice parameters close to the reference data, and also a few of other phases. The titanium carbide particles in the iron binder were identified on the back-scattered electron (BSE) images due to the tonal contrast: the heavy iron appears darker against the carbide, which is composed of lighter elements. According to EDX analysis, the relative content of titanium and carbon in the carbide particles indeed corresponds to the composition of non-stoichiometric titanium carbide. Conclusion. The composites including titanium carbide and α-iron binder were obtained by sintering of iron titanides and carbon (carbon black) mechanically activated powder mixtures. The granules of composite powders obtained by crushing of sintered compacts are of interest as feedstocks for wear-resistant coatings and additive technologies, as well as for manufacturing of dense materials by other compaction methods: spark plasma sintering (SPS) or hot pressing (HP).
铁钛化物和碳机械活化混合物烧结形成的具有碳化物强化作用的铁基质复合材料研究
导言。在合金结构中加入难熔化合物(碳化物、硼化物、硅化物)的分散固体颗粒是提高钢和合金耐磨性的一种广泛使用的有效方法。用碳化钛颗粒强化铁基合金(钢和铸铁)基体的复合材料具有极大的实用价值。决定复合材料硬度和耐磨性的主要结构特征是强化碳化物颗粒的体积分数、分散性和形态。复合材料的结构取决于其制备方法。结合粉末混合物的初步机械活化的粉末冶金方法已得到广泛应用。之前已经证实,在机械活化的 FTi35S5 钛铁(由 82% 的(Fe,Al)2Ti 相组成)和 P-803 炭黑的粉末混合物中,会发生反应,形成由钢粘合剂和碳化钛组成的复合材料。碳化物的合成反应是在 900-950 °C 的燃烧温度下以固相模式进行的。因此,不会出现因碳化物颗粒生长而导致结构变粗的情况,而这种情况在液相反应中很常见。FTi35S5 合金含有大量杂质(硅、铝等)。这项工作的目的是研究在机械活化粉末混合物反应烧结条件下,Fe2Ti 和 FeTi 铁钛化物与碳相互作用产物的相组成和结构,并确定用亚微米碳化钛颗粒合成强化铁基复合材料的可能性。研究方法。通过光学金相术、X 射线衍射(XRD)和扫描电子显微镜(SEM)研究了机械活化粉末烧结密实物的结构和相组成,并通过能量色散 X 射线光谱(EDX)测定了元素组成。实验技术。制备反应混合物时使用的金属间化合物粉末是通过真空烧结 2Fe+Ti 和 Fe+Ti 成分的铁钛粉末混合物压块获得的。在金属间化合物粉末中加入了炭黑,以便将金属间化合物中含有的钛全部转化为碳化物。钛化物-炭黑混合物用 Activator 2S 行星球磨机以 755 rpm 的转速(40 克)研磨 10 分钟。机械活化后的混合物被冷压成直径为 20 毫米的圆柱形样品,然后在真空中进行烧结,а 温度为 1,200 °C,等温保温时间为 60 分钟。结果与讨论根据 X 射线衍射分析结果,钛化铁中几乎所有的钛都会与碳发生反应,形成碳化物和还原铁。两种成分的压制物的烧结产物都含有目标相:等原子比略有偏移的碳化钛和晶格参数接近参考数据的α-铁,以及少量其他相。铁粘合剂中的碳化钛颗粒是通过反向散射电子(BSE)图像中的色调对比识别出来的:在由浅色元素组成的碳化钛的映衬下,重铁的颜色显得更深。根据 EDX 分析,碳化物颗粒中钛和碳的相对含量确实与非共沸碳化钛的成分相符。结论通过烧结铁钛化物和碳(炭黑)机械活化粉末混合物,获得了包括碳化钛和 α-铁粘合剂在内的复合材料。通过粉碎烧结压实物获得的复合粉末颗粒可用作耐磨涂层和添加剂技术的原料,也可用于通过其他压实方法(火花等离子烧结 (SPS) 或热压 (HP))制造致密材料。
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