Evolution of Phase Composition and Microstructure upon Synthesis of Zr—Sn Alloy from Zirconium Hydride and Tin Powders

Evolution of Phase Composition and Microstructure upon Synthesis of Zr—Sn Alloy from Zirconium Hydride and Tin Powders

Microstructure and density evolution as well as thermal effects are investigated upon synthesis of Zr—1.5% Sn alloy from powder blends of zirconium-hydride and tin particles. Melting of tin particles at the initial stage of heating results in increased porosity, but does not accelerate chemical homo...

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Date:2015
Main Authors: Savvakin, D.G., Oryshych, D.V.
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Published: Інститут металофізики ім. Г.В. Курдюмова НАН України 2015
Series:Металлофизика и новейшие технологии
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Физика прочности и пластичности
Online Access:http://dspace.nbuv.gov.ua/handle/123456789/111911
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Cite this:Evolution of Phase Composition and Microstructure upon Synthesis of Zr—Sn Alloy from Zirconium Hydride and Tin Powders / D. G. Savvakin, D. V. Oryshych // Металлофизика и новейшие технологии. — 2015. — Т. 37, № 4. — С. 559-569. — Бібліогр.: 12 назв. — англ.

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spelling irk-123456789-1119112017-01-16T03:03:40Z Evolution of Phase Composition and Microstructure upon Synthesis of Zr—Sn Alloy from Zirconium Hydride and Tin Powders Savvakin, D.G. Oryshych, D.V. Физика прочности и пластичности Microstructure and density evolution as well as thermal effects are investigated upon synthesis of Zr—1.5% Sn alloy from powder blends of zirconium-hydride and tin particles. Melting of tin particles at the initial stage of heating results in increased porosity, but does not accelerate chemical homogenization of powder system. Formation of solid intermetallics is accelerated at increased temperatures of 550—800°C due to hydrogen desorption and activation of zirconium matrix. Solid-state homogenization and sintering processes at higher temperatures produce homogeneous tin solution in zirconium. Particle sizes, temperature and time of sintering provide formation of low-porous (with relative density of more than 97%) chemically and microstructurally homogeneous material. Mechanical properties of fabricated alloy are at the level of properties of corresponding material produced with conventional ingot technology. Досліджено еволюцію мікроструктури, густини та термічні ефекти в ході формування стопу Zr—1.5% Sn з порошкових сумішей частинок гідриду Цирконію та цини. Топлення частинок цини на початкових стадіях нагрівання збільшує пористість у порошковій системі, не завдавши помітного розвитку хемічній гомогенізації, але за підвищення температури до 550—800°C прискорюється процес формування твердих інтерметалідних фаз, в тому числі завдяки десорбції Гідроґену з гідриду й активації цирконійової матриці. За високих температур гомогенізація та спікання частинок відбуваються твердофазним шляхом з формуванням однорідного твердого розчину Стануму в цирконії. Використані в роботі розміри порошкових частинок та температурно-часові параметри нагрівання уможливлюють одержати малопоруватий (з відносною густиною більше 97%) хемічно й мікроструктурно однорідний стоп з механічними характеристиками на рівні характеристик даного матеріялу, одержаного методою лиття та гарячого деформування. Исследована эволюция микроструктуры, плотности и термические эффекты в процессе формирования сплава Zr—1.5% Sn из порошковых смесей частиц гидрида циркония и олова. Плавление частиц олова на начальных стадиях нагрева увеличивает пористость в порошковой системе, не приводя к заметному развитию химической гомогенизации, но при повышении температуры до 550—800°C ускоряется процесс формирования твёрдых интерметаллидных фаз, в том числе благодаря десорбции водорода из гидрида и активации циркониевой матрицы. При высоких температурах гомогенизация и спекание частиц происходит твердофазным путём с формированием однородного твёрдого раствора олова в цирконии. Использованные в работе размеры порошковых частиц и температурно-временные параметры нагрева позволяют получить малопористый (с относительной плотностью более 97%) химически и микроструктурно однородный сплав с механическими характеристиками на уровне характеристик данного материала, полученного методом литья и горячей деформации. 2015 Article Evolution of Phase Composition and Microstructure upon Synthesis of Zr—Sn Alloy from Zirconium Hydride and Tin Powders / D. G. Savvakin, D. V. Oryshych // Металлофизика и новейшие технологии. — 2015. — Т. 37, № 4. — С. 559-569. — Бібліогр.: 12 назв. — англ. 1024-1809 PACS: 61.43.Gt, 61.66.Dk, 64.70.dj, 64.70.kd, 81.20.Ev, 81.30.Bx, 81.40.Ef http://dspace.nbuv.gov.ua/handle/123456789/111911 en Металлофизика и новейшие технологии Інститут металофізики ім. Г.В. Курдюмова НАН України
institution Digital Library of Periodicals of National Academy of Sciences of Ukraine
collection DSpace DC
language English
topic Физика прочности и пластичности
Физика прочности и пластичности
spellingShingle Физика прочности и пластичности
Физика прочности и пластичности
Savvakin, D.G.
Oryshych, D.V.
Evolution of Phase Composition and Microstructure upon Synthesis of Zr—Sn Alloy from Zirconium Hydride and Tin Powders
Металлофизика и новейшие технологии
description Microstructure and density evolution as well as thermal effects are investigated upon synthesis of Zr—1.5% Sn alloy from powder blends of zirconium-hydride and tin particles. Melting of tin particles at the initial stage of heating results in increased porosity, but does not accelerate chemical homogenization of powder system. Formation of solid intermetallics is accelerated at increased temperatures of 550—800°C due to hydrogen desorption and activation of zirconium matrix. Solid-state homogenization and sintering processes at higher temperatures produce homogeneous tin solution in zirconium. Particle sizes, temperature and time of sintering provide formation of low-porous (with relative density of more than 97%) chemically and microstructurally homogeneous material. Mechanical properties of fabricated alloy are at the level of properties of corresponding material produced with conventional ingot technology.
format Article
author Savvakin, D.G.
Oryshych, D.V.
author_facet Savvakin, D.G.
Oryshych, D.V.
author_sort Savvakin, D.G.
title Evolution of Phase Composition and Microstructure upon Synthesis of Zr—Sn Alloy from Zirconium Hydride and Tin Powders
title_short Evolution of Phase Composition and Microstructure upon Synthesis of Zr—Sn Alloy from Zirconium Hydride and Tin Powders
title_full Evolution of Phase Composition and Microstructure upon Synthesis of Zr—Sn Alloy from Zirconium Hydride and Tin Powders
title_fullStr Evolution of Phase Composition and Microstructure upon Synthesis of Zr—Sn Alloy from Zirconium Hydride and Tin Powders
title_full_unstemmed Evolution of Phase Composition and Microstructure upon Synthesis of Zr—Sn Alloy from Zirconium Hydride and Tin Powders
title_sort evolution of phase composition and microstructure upon synthesis of zr—sn alloy from zirconium hydride and tin powders
publisher Інститут металофізики ім. Г.В. Курдюмова НАН України
publishDate 2015
topic_facet Физика прочности и пластичности
url http://dspace.nbuv.gov.ua/handle/123456789/111911
citation_txt Evolution of Phase Composition and Microstructure upon Synthesis of Zr—Sn Alloy from Zirconium Hydride and Tin Powders / D. G. Savvakin, D. V. Oryshych // Металлофизика и новейшие технологии. — 2015. — Т. 37, № 4. — С. 559-569. — Бібліогр.: 12 назв. — англ.
series Металлофизика и новейшие технологии
work_keys_str_mv AT savvakindg evolutionofphasecompositionandmicrostructureuponsynthesisofzrsnalloyfromzirconiumhydrideandtinpowders
AT oryshychdv evolutionofphasecompositionandmicrostructureuponsynthesisofzrsnalloyfromzirconiumhydrideandtinpowders
first_indexed 2025-07-08T02:53:09Z
last_indexed 2025-07-08T02:53:09Z
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fulltext 559 PHYSICS OF STRENGTH AND PLASTICITY PACS numbers:61.43.Gt, 61.66.Dk,64.70.dj,64.70.kd,81.20.Ev,81.30.Bx, 81.40.Ef Evolution of Phase Composition and Microstructure upon Synthesis of Zr—Sn Alloy from Zirconium Hydride and Tin Powders D. G. Savvakin and D. V. Oryshych* G. V. Kurdyumov Institute for Metal Physics, N.A.S. of Ukraine, 36 Academician Vernadsky Blvd., UA-03680 Kyiv, Ukraine *Taras Shevchenko National University of Kyiv, 64 Volodymyrska Str., UA-03022 Kyiv, Ukraine Microstructure and density evolution as well as thermal effects are investi- gated upon synthesis of Zr—1.5% Sn alloy from powder blends of zirconium- hydride and tin particles. Melting of tin particles at the initial stage of heat- ing results in increased porosity, but does not accelerate chemical homogeni- zation of powder system. Formation of solid intermetallics is accelerated at increased temperatures of 550—800С due to hydrogen desorption and activa- tion of zirconium matrix. Solid-state homogenization and sintering processes at higher temperatures produce homogeneous tin solution in zirconium. Par- ticle sizes, temperature and time of sintering provide formation of low- porous (with relative density of more than 97%) chemically and microstruc- turally homogeneous material. Mechanical properties of fabricated alloy are at the level of properties of corresponding material produced with conven- tional ingot technology. Досліджено еволюцію мікроструктури, густини та термічні ефекти в ході формування стопу Zr—1.5% Sn з порошкових сумішей частинок гідриду Цирконію та цини. Топлення частинок цини на початкових стадіях на- грівання збільшує пористість у порошковій системі, не завдавши поміт- ного розвитку хемічній гомогенізації, але за підвищення температури до 550—800С прискорюється процес формування твердих інтерметалідних фаз, в тому числі завдяки десорбції Гідроґену з гідриду й активації цир- конійової матриці. За високих температур гомогенізація та спікання час- тинок відбуваються твердофазним шляхом з формуванням однорідного твердого розчину Стануму в цирконії. Використані в роботі розміри по- рошкових частинок та температурно-часові параметри нагрівання умож- ливлюють одержати малопоруватий (з відносною густиною більше 97%) Металлофиз. новейшие технол. / Metallofiz. Noveishie Tekhnol. 2015, т. 37, № 4, сс. 559—569 Оттиски доступны непосредственно от издателя Фотокопирование разрешено только в соответствии с лицензией 2015 ИМФ (Институт металлофизики им. Г. В. Курдюмова НАН Украины) Напечатано в Украине. 560 D. G. SAVVAKIN and D. V. ORYSHYCH хемічно й мікроструктурно однорідний стоп з механічними характерис- тиками на рівні характеристик даного матеріялу, одержаного методою лиття та гарячого деформування. Исследована эволюция микроструктуры, плотности и термические эф- фекты в процессе формирования сплава Zr—1.5% Sn из порошковых сме- сей частиц гидрида циркония и олова. Плавление частиц олова на начальных стадиях нагрева увеличивает пористость в порошковой систе- ме, не приводя к заметному развитию химической гомогенизации, но при повышении температуры до 550—800С ускоряется процесс формирова- ния твёрдых интерметаллидных фаз, в том числе благодаря десорбции водорода из гидрида и активации циркониевой матрицы. При высоких температурах гомогенизация и спекание частиц происходит твердофаз- ным путём с формированием однородного твёрдого раствора олова в цир- конии. Использованные в работе размеры порошковых частиц и темпера- турно-временные параметры нагрева позволяют получить малопористый (с относительной плотностью более 97%) химически и микроструктурно однородный сплав с механическими характеристиками на уровне харак- теристик данного материала, полученного методом литья и горячей де- формации. Key words: microstructure, mechanical properties, chemical homogeniza- tion, zirconium hydride, tin. (Received January 28, 2015) 1. INTRODUCTION Due to corrosion resistance and small cross-section of thermal-neutron capture, zirconium is extensively used in the nuclear reactor struc- tures. Particularly, fuel element cans of thermal neutron reactor cores [1] are fabricated of zirconium—tin alloys (with tin content about 1.2— 1.7 wt.%). Conventional fabrication of these alloys includes very com- plex ingot technologies and hot working of ingots, while their subse- quent machining results to appreciable percentage of material loss as the scraps. The obtaining of alloys from powder materials serves as an alternative and a relatively technologically simple method. This allows us not only to avoid a number of problems associated with melting of alloys, viz. uncontrolled grain growth, appearance of the segregation of alloying elements, but also to reduce significantly metal loss in ob- taining of products several times reducing their cost. Production of zirconium alloys with necessary physical-mechanical characteristics via the synthesis of heterogeneous systems of powder particles of zir- conium and alloying elements is interesting from material science and practical point of view. It was recently shown that this method of syn- thesis of titanium and zirconium alloys [2, 3] results to their desired characteristics due to replacement of the powders of appropriate met- PHASE COMPOSITION AND MICROSTRUCTURE UPON SYNTHESIS OF Zr—Sn 561 als by the powders of their hydrides. Hydrogen in a specified method is a temporary alloying element activating sintering of particles and chemical homogenization of powder systems when they are heated, which improves characteristics of synthesized alloys. Synthesis of zirconium alloys occurs at a temperature above the 1000С in a single-phase -region [3]. According to the state diagram [4] (see Fig. 1), during the formation of Zr—Sn alloys from the powders of these elements, a liquid Sn phase appears at the initial stages of heating and chemical homogenization of powder system, while the complete synthesis of these alloys with a relatively small tin content occurs in a solid-phase way. It is well known that the appearance of liq- uid phases during sintering of different powder systems can lead to both significant pore formation (e.g., in Ti—Al [5] and Ti—Fe [6] sys- tems) and, vice versa, accelerated sintering (e.g., in W—Cu, W—Ni, and Cu—Sn systems [7]) with a reduced volume fraction of pores. The goal of this work is to study synthesis of Zr—1.5% Sn alloy from the heterogeneous powder blends of zirconium hydride and tin, to as- certain peculiarities of microstructure evolution of such systems when liquid phase appears, and to determine the potential of forming chemi- cally- and microstructurally homogeneous alloy with low volume frac- Fig. 1. State diagram of Zr—Sn system [4]. Heavy dashed line (at 1250С) de- notes the synthesis temperature of alloy at issue. 562 D. G. SAVVAKIN and D. V. ORYSHYCH tion of pores and appropriate mechanical characteristics. 2. EXPERIMENTAL METHODS The Zr—1.5 wt.% Sn alloy was prepared of the mixture with appropri- ate proportion of powder particles of zirconium hydride ZrН2 and tin. In this work, we used the sieved fraction of hydride zirconium parti- cles smaller than 100 m while their average size was 56 m, and tin particles smaller than 200 m while their average size was 138 m. The powder blend was pressed at a room temperature and pressure of 640 МPа in the cylindrical (with 10 mm of both diameter and height) and rectangular (651010 mm3) samples, which then were heated up to 1250C in a vacuum furnace ( 10 3 Pa) with 10С/min heating rate with further isothermal annealing during four hours for simultaneous dehydrogenation and formation of a bulky homogeneous alloy. For a step-by-step study of the phase and structural transformations during the hydrogen desorption and transformation of the powder blend into alloy, except of ZrН2  1.5% Sn composition, in some cases we also used a model blend of the powders with higher tin content, ZrН2   10% Sn. The heating up to 320, 550, 800, and 1250C at a rate of 10С/min was followed by cooling in the furnace without isothermal annealing. Phase composition of the material was determined by the X- ray diffraction analysis using the CuK radiation. The differential scanning calorimetry method was used to establish general course of the phase transformations and thermal effects during the synthesis of alloy, for which we heated the powder blend ZrН2  10% Sn and hy- dride zirconium powder in an inert gas with the rate of 10оС/min up to 1250С. The structure of material was investigated by the optic and scanning electron microscopy methods. The change in density of Zr— 1.5% Sn samples at different heating stages was determined by the hydrostatic method. Mechanical characteristics of the synthesized Zr— 1.5% Sn alloy were determined via tensile testing and measuring Vick- ers hardness. Oxygen content in the synthesized alloy was determined using the gas analyser ELTRA OH900. 3. RESULTS AND DISCUSSION Applying the differential scanning calorimetry method, we deter- mined the main temperature effects of the phase transformations oc- curring during the heating of ZrН2  10% Sn model blend (curve 1 in Fig. 2). Comparing this curve with the curve of heating for similar conditions of zirconium hydride powder (curve 2 in Fig. 2), we reveal that the first endothermic effect at 231С is associated with melting of tin particles, and the following effects within the range of 390—800С PHASE COMPOSITION AND MICROSTRUCTURE UPON SYNTHESIS OF Zr—Sn 563 are resulted of hydrogen desorption from zirconium hydride and for- mation of zirconium dehydrated particles. Generally, calorimetric curve of the studied powder blend in the 300—1200С temperature range practically coincides with the curve of heating of zirconium hy- dride powder (curve 2 in Fig. 2) without any appreciable effects deal- ing with the presence of tin and its possible reaction with zirconium matrix. The presence of tin results to the appearance of relatively weak exothermic peak only at 1209С. The microstructure evolution at a heating of the gathered powder blends is shown in Fig. 3. Tin particles located in hydride matrix are irregular in shape. Cleavage of powder compacts occurs mainly over the brittle hydride particles, which have low strength, therefore a rela- tively small number of tin particles is observed on the fractured sur- face (Fig. 3, a). Microstructure evolution appears already at a melting temperature of the tin. In the samples, cooled from 320С, tin particles change their shape into spherical one (Fig. 3, b). Such shape of the par- ticles indicates that at a heating temperature tin was in a melt state with spherical shape due to the surface tension, but appearance of liq- uid phase does not lead to the instantaneous reaction of tin with hy- dride particles. The gradual chemical homogenization of the system begins with the formation of tin liquid phase and occurs, however, ra- ther slowly: X-ray microspectrum analysis data show that crystallized spherical tin droplet contains 4% of zirconium (Fig. 3, b), while hy- dride particles around it contain 1% of tin. Fig. 2. Calorimetric curves of the heating of zirconium hydride and 10% of Sn powder (1), and zirconium hydride powder (2). 564 These partly ex zirconium sult to th the press in our stu tin to ex cant hete ume. At fur Fig. 3. Mi particles ing from local tin c D results agr xist at 300 m. Accordi he weak ten sed samples udy, a relat ist as the d erogeneity rther temp icrostructur (with compo the room te content. . G. SAVVAK ree with da C during 4 ing to Ref. ndency for s s under the tively rapid droplets, di in the distr erature inc re evolution osition corre mperature ( KIN and D. V ata of Ref. 48 hours wh . [8], such small Sn dr e action of g d heating a id not resul ribution of creasing, tw a b c n of the syst esponding to (a) to 320С V. ORYSHYCH [8], where hile it is he temperatur roplets to m gravitation and, therefo lt to the ap f droplets o wo process tem of zirco o Zr—1.5% S С (b) and 800 H liquid tin p ated in con re—time reg move to lowe nal forces. H ore, limited ppearance o ver the sam ses occur si nium hydrid Sn alloy) du 0С (c). Arro phase can ntact with gimes re- er part of However, d time for of signifi- mples vol- imultane- de and tin uring heat- ows denote PHASE COMPOSITION AND MICROSTRUCTURE UPON SYNTHESIS OF Zr—Sn 565 ously: desorption of hydrogen from hydride matrix (above the temper- ature of  390С), which leads to ZrH2  Zr transformation, and redis- tribution of tin in the matrix with contribution of the liquid phase. Tin droplets gradually react with zirconium matrix. We did not ob- serve the crystallized spherical Sn droplets in the microstructure of the samples cooled from 550С and 800С (Fig. 3, c); instead of them voids with Sn-enriched surfaces were seen (e.g., 13% in Fig. 3, c). The X-ray analysis also confirmed the absence of pure tin after heating to 550С (Fig. 4, a), while ZrSn2 phase appeared, which coexists with hy- dride (-phase) and small amount of -zirconium formed due to desorp- tion of hydrogen from hydride. During heating to 800С, the most ac- tive stage of hydrogen desorption occurs, and hydride is totally trans- formed into the -phase of zirconium (Fig. 4, b). At the same time, the amount of Sn-enriched ZrSn2-phase significantly decreases, which can be caused by further tin spreading into the zirconium matrix and the formation of regions with lower local concentration of Sn. Thus, the transition of Sn into the liquid state during heating pro- vides its gradual reaction with zirconium matrix already at the rela- tively low temperatures (up to 550С) with the formation of solid phas- es. As follows from Ref. [8], ZrSn2 is the first phase forming at a con- tact of liquid tin and zirconium that occurs in a wide temperature range from 300 to 700С and, in contrast to our data, requires long- term exposures. For instance, an isothermal exposure at 500С during 1 hour is not sufficient for disappearance of pure tin [8]. In our case, the effect of accelerated disappearance of tin with the formation of ZrSn2-phase can be explained by the high defectiveness of dehydrogen- ated zirconium matrix [9] that contributes to the development of in- terdiffusion. Hydrogen desorption, being completed at 800—850С, a b Fig. 4. The X-ray diffraction peaks for Zr—10% Sn sample after heating up to 550C (a) and 800С (b). 566 D. G. SAVVAKIN and D. V. ORYSHYCH forms activated zirconium matrix that significantly accelerates sinter- ing of zirconium particles and diffusion of tin into them with devel- opment of homogenization of the system. According to the state diagram [4], intermetallic ZrSn2-phase exists up to 1142С. Next stage of chemical homogenization of the system consists in the dissolution of ZrSn2 and formation of intermetallic Zr5Sn3-phase [8], and this process can be a solid-phase one during the long-term exposures below the specified temperature. In our experi- ments on the X-ray analysis for Zr—10% Sn samples heated to 800С, the clear presence of Zr5Sn3-phase was not revealed along with diffrac- tion peaks of -zirconium and ZrSn2, which is caused by the short time of high temperatures subjected to the material. At a continuous heat- ing in our case, the remains of the untransformed ZrSn2-phase have to be melting above the 1142С. Therefore, one can explain an appearance of exothermal peak at 1209С (curve 1 in Fig. 2) by the accelerated chemical homogenization and formation of phases with lower tin con- tent due to two reasons: first, activation of solid-phase diffusion at the increased temperatures, and, second, melting of the remains of ZrSn2- phase. The relatively weak endothermic melting effect in this case is suppressed by the exothermic effect of the formation of new phases, therefore it is not observed on calorimetric curves. According to the thermodynamic calculations [10] of energy effect of formation of in- termetallic phases in Zr—Sn system, the strongest exothermic effect takes place for the formation of Zr5Sn3 phase. This effect exceeds the effects of the formation of Zr4Sn and ZrSn2 phase approximately by 3 and 3.5 times, respectively. Therefore, exothermic effect at 1209С can be associated with the formation of Zr5Sn3 phase, first, and, proba- bly, Zr4Sn one. Increase in temperature up to 1250С leads to rapid tin spreading over all matrix and disappearance of the regions with high concentra- tion gradient of this element, although some heterogeneity in a distri- bution remains. The concentration of tin in the sample cooled after the heating to 1250С is 1—2%. The total chemical homogeneity of the ma- terial can be reached relatively fast at the isothermal exposure at 1250С. The density increase of the samples at a heating is represented in Fig. 5. Note that, against the background of a general increase in den- sity of the samples with increasing temperature, the density decreases at 800C. During the heating in the range of 300—550С, a certain de- crease in density is typical for compressed powder systems based on the zirconium hydride particles [3]. For a relatively weak traction between zirconium hydride particles, the elastic energy accumulated in them relaxes, and hydride particles demonstrate microcracks being generat- ed in the samples. This slightly increases volume of the compressed system, decreasing the density. In addition, the voids, being generated PHASE COMPOSITION AND MICROSTRUCTURE UPON SYNTHESIS OF Zr—Sn 567 on the same places occupied by the tin particles, also contribute to den- sity decreasing for the samples heated to 800С (Fig. 3, c). The hydro- gen desorption is the most intensive within the 600—800С. During this process, the particles decrease their volume, while sintering, be- ing in progress at high temperature, leads to disappearance of voids between the particles, therefore the density rapidly increases. After 4- hour isothermal exposure at 1250С, volume fraction of the pores sig- nificantly decreases, while massive chemically and microstructurally homogeneous Zr—1.5% Sn alloy is generated (Fig. 6). However, some rather large pores remain in the synthesized alloy and substitute voids appearing on the places of tin particles during the temperature in- creasing. The sizes of the largest pores are comparable with the sizes of initial tin particles (Fig. 6). Additional experiments confirmed that using of small tin particles allows decreasing of the volume and sizes of residual pores hereby approximating experimental density of the syn- thesized alloy to theoretical value, which is necessary condition to reach high mechanical characteristics. The sizes of tin particles used in the present work (daver  138 m) gave density of the synthesized alloy: 6.37 g/cm3–97.3% of theoretical value. X-ray phase analysis indicates that alloy synthesized at 1250С dur- ing four hours is a single-phase (h.c.p.) solid solution of tin in zirco- nium. Such state practically corresponds to composition of Zr—1.5% Sn on the state diagram, while intermetallic Zr4Sn-phase is not ob- served on the X-ray pattern. Fig. 5. Density evolution for samples during continuous heating up to 1250С and four-hour isothermal exposure at this temperature. 568 D. G. SAVVAKIN and D. V. ORYSHYCH Hardness of synthesized alloy is HV  (181.3  13.7) kg/mm2. Me- chanical properties of the alloy after the tensile test are presented in Table, where the data are also compared with literature ones [11, 12] on the properties of this material obtained by a traditional method of casting and hot working. Generally, the data presented in the litera- ture differ widely due to different content of impurities, structure, and methods of the treatment of this alloy. At the same time, we can assert that characteristics of the strength and plasticity of alloy at is- sue are up to the corresponding characteristics that can be achieved by a traditional production method. Thus, the alloy synthesized from powders is a prospective for a practical use. 4. CONCLUSIONS (i) The Zr—1.5% Sn alloy was synthesized from a two-component zirco- nium hydride and tin powder blend. We used the size parameters of powder particles and temperature-time conditions of the synthesis al- lowing obtaining homogeneous alloy with density close to theoretical value. (ii) There are two simultaneous processes during the heating: hydrogen Fig. 6. Microstructure of Zr—1.5% Sn alloy synthesized at 1250С during four hours. TABLE. Characteristics of Zr—1.5% Sn alloy obtained in this work as com- pared with material obtained by a tradition method. Method of obtaining Density, g/сm3 0.2, MPa B, МПа , % Traditional technology [11, 12] 6.55 353 430 541 520 23.5 — Synthesized from ZrH2 powder 6.37 (97.3%) 475 561 12—13 PHASE COMPOSITION AND MICROSTRUCTURE UPON SYNTHESIS OF Zr—Sn 569 desorption from the hydrogenated zirconium matrix and its reaction with melted tin. Sn totally reacts at the stage of heating to 550С form- ing ZrSn2-phase. (iii) The melting of tin particles at early heating stages results in for- mation of pores that substitute tin droplets in hydride matrix. De- crease in size of tin particles enables decreasing sizes and total volume of residual pores in the synthesized alloy and makes closer its experi- mental density to theoretical value. (iv) The Zr—1.5% Sn alloy synthesized by the presented method demonstrates the complex of tensile properties comparable with those a traditionally obtained material possesses. This confirms practical importance of the method applied in the paper. REFERENCES 1. S. Yu. Zavodchikov, L. V. Zuev, and V. A. Kotrekhov, Metallovedcheskie Voprosy Proizvodstva Izdeliy iz Splavov Tsirkoniya (Metal Science Problems of the Products from Zirconium Alloys) (Мoscow: Nauka: 2012) (in Russian). 2. О. М. Ivasishin, D. G. Savvakin, and M. М. Gumenyak, Metallofiz. Noveishie Tekhnol., 33, No. 7: 899 (2011) (in Russian). 3. D. G. Savvakin and M. M. Gumenyak, Metallofiz. Noveishie Tekhnol., 35, No. 3: 349 (2013) (in Russian). 4. J. P. Abriata, J. C. Bolcich, and D. Arias, Bulletin of Alloy Phase Diagrams, 4, No. 2: 147 (1983). 5. M. Dahms, G. Leitner, W. Poessnecker, S. Schultrich, and F. Schmelzer, Z. Metallkd., 84, No. 5: 351 (1993). 6. V. V. Skorokhod, Yu. М. Solonin, and I. V. Uvarova, Khimicheskie, Diffuzionnye i Reologicheskie Protsessy v Tekhnologii Poroshkovykh Materialov (Chemical, Diffusion and Rheological Processes in Powder Materials Technology) (Kiev: Naukova Dumka: 1990) (in Russian). 7. А. G. Kostornov, Materialovedenie Dispersnykh i Poristykh Metallov i Splavov (Material Science of Disperse and Porous Metals and Alloys). Vol. 1 (Kiev: Naukova Dumka: 2002) (in Russian). 8. T. Studnitzky and R. Schmid-Fetser, Z. Metallkd., 93, No. 9: 894 (2002). 9. V. A. Goltsov, N. I. Тimofeev, and I. Yu. Machikina, Dokl. AN USSR, 235, No. 5: 1060 (1977) (in Russian). 10. N. Subasic, Calphad, 22, No. 2: 157 (1998). 11. L. M. Howe and W. R. Thomas, J. Nuclear Materials, 2, No. 3: 248 (1960). 12. O. H. Kwon, K. B. Eom, J. I. Kim, J. M. Suh, and K. L. Jeon, Nucl. Eng. 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<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> /ENU (Use these settings to create Adobe PDF documents best suited for high-quality prepress printing. 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