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12Condensed Matter and Interphases (Kondensirovannye sredy i mezhfaznye granitsy)
Original articles
DOI: https://doi.org/10.17308/kcmf.2020.22/2835 ISSN 1606-867X
Received 28 January 2020 eISSN 2687-0711
Accepted 15 May 2020 Published online 25 June 2020
The study of the quasi-triple system FeS-Ga2S3-Ag2S by a FeGa2S4-AgGaS2 section
©2020 Sh. H. Mammadov
Institute of Catalysis and Inorganic Chemistry named after Academician M. F. Nagiyev of the National Academy of Sciences of Azerbaijan, 113 G. Javid pr., Baku Az1143, Azerbaijan Abstract
The interest in the study of systems containing sulphides with the formula AIBIIICVI2 is generated in particular by emerging opportunities for their practical use in the production of non-linear optical devices, detectors, solar cells, photodiodes, luminophors, etc. Therefore, taking into account the search for new promising materials based on silver and iron thiogallates, the goal of this work is to study the quasi-binary section FeGa2S4-AgGaS2 of the quaternary system Fe-Ag-Ga-S. The alloys of the AgGaS^FeGa^ system were synthesised from high-purity base metals: iron - 99.995 %, gallium - 99.999 %, silver - 99.99 %, and sulphur - 99.99 %. The alloys were studied using differential thermal analysis, X-ray phase analysis, and microstructural analysis as well as microhardness measurement and density determination.
Using the methods of physicochemical analysis, a T-x phase diagram of the AgGaS2-FeGa2S4 section, which is the internal section of the quasi-triple FeS-Ga2S3-Ag2S system, was studied and constructed for the first time. It was established that this system is of the simple eutectic type. The composition of the eutectic point is 56 mol% FeGa2S4 and T = 1100 K. The solid solution ranges were determined on the basis of the source components. Based on FeGa2S4 and AgGaS2 at the eutectic temperature the solubility stretches to 10 and 16 mol% respectively. With decreasing temperature, the solid solutions narrow and, at room temperature, comprise 4 mol% AgGaS2 based on iron thiogallate (FeGa2S4) and 11 mol% FeGa2S4 based on silver thiogallate (AgGaS2).
Keywords: phase diagram, solid solution, FeGa2S4, AgGaS2, quasi-triple system, eutectic, X-ray analysis, FeS-Ga2S3-Ag2S. For citation: Mamadov Sh. H. The study of the quasi-triple system FeS-Ga2S3-Ag2S by a FeGa2S4-AgGaS2 section. Kondensirovannye sredy i mezhfaznye granitsy = Condensed Matter and Interphases. 2020;22(2): 232-237. DOI: https://doi. org/10.17308/kcmf.2020.22/2835
1. Introduction
The interest in the study of systems containing sulphides with the formula AIBIIICVI2 is generated in particular by emerging opportunities for their practical use in the production of non-linear optical devices, detectors, solar cells, photodiodes, luminophors, etc. [1-17].
The reported data shows that multicomponent sulphide compounds, especially those containing magnetic (FeGa2S4, Fe2Ga2S5, FeIn2S4, etc.) ions, are functional materials and are used in the production of magneto-optical devices, photodetectors, lasers, light modulators, etc. [18-25].
El Sharafat Hajiaga Mammadov, e-mail: azxim@mail.ru
The content is available under Creative Commons
The source components comprising the quaternary system Ag-Fe-Ga-S were thoroughly studied in [26-42]. Compositions AgGaS2, Ag9GaS6 and Ag2Ga20S31 were established during the study of the Ag2S-Ga2S3 binary system [26, 30, 31]. Ag2Ga20S31 is formed from them by a peritectic reaction at 1268 K while AgGaS2 and Ag9GaS6 melt congruently at 1270 and 1063 K respectively. AgGaS2 crystallises within the chalcopyrite-type structure (a = 5.7544, c = 10.299 A space group I42d) [27] and is a p-type semiconductor with a band gap of AE = 2.75 eV [32].
The phase diagram of the section Ga2S3-FeS was studied in [33-42]. The authors established
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that triple compounds FeGa2S4 and Fe2Ga2S5 are formed in the system Ga2S3-FeS [38, 42].
The microhardness of the FeGa2S4 and Fe2Ga2S5 compounds are 4000±5 and 3500±5 MPa respectively [42].
The FeGa2S4 compound melts congruently at 1418 K [38], although, according to [39], FeGa2S4 is formed by a peritectic reaction at 1343 K and undergoes polymorphous transformation at 1283 K. FeGa2S4 crystallises in a rhombic crystal system of the ZnAl2S4 type with the following parameters: a = 1.289 nm, b = 0.751, c = 0.609 nm [40]. According to [41], this compound has two crystalline modifications: low-temperature trigonal P3ml: a = 0.3654 nm, c = 1.2056 nm; and high-temperature rhombic: a = 1.289, b = 0.751, c = 0.609 nm.
The goal of this work is to study the quasi-binary section FeGa2S4-AgGaS2 of the quaternary system Fe-Ag-Ga-S.
2. Experimental
Synthesis of the alloys of the AgGaS2-FeGa2S4 system were conducted from base metals. The base metals (AgGaS2 and FeGa2S4) were synthesised using high-purity: iron - 99.995 %, gallium -99.999 %, silver - 99.99 %, and sulphur - 99.99 %. Stoichiometric mixtures of the elements were placed in vacuum quartz ampoules (17 cm long and 1.5 cm in diameter) with residual pressure ~0.133 Pa [43]. Then the ampoule was placed in a two-zone furnace. The furnace was slowly heated from room temperature to the fusion temperature of the compound FeGa2S4. Sulphur becomes condensed in the cold region and returns to the interaction zone. The alloys in a liquid state were stirred at regular intervals. The outer part of the ampoule was cooled with water. After 1.52 hours in the cold region, the mass of the sulphur decreased. After that, the whole ampoule was placed in the furnace and held at a temperature of 1450 K for 2.5 hours. The process of synthesis lasted for at least 4 hours. Then the obtained samples were homogenised at a temperature of 800 K for 150 h. The alloys were studied using differential thermal analysis (DTA), X-ray phase analysis (XRD), and microstructural analysis (MSA) as well as microhardness measurement and density determination. XRD was performed on a D2 PHASER using Ni-filtered CuK radiation.
DTA of the alloys of the system was conducted on an HTP-73 device with a heating rate of 10 degrees per minute. Calibrating chromel-alumel thermocouples were used with Al2O3 as a reference standard. An etchant of the composition NH4NO3(3-8 wt%)+ K2Cr207(0.02-0.5 wt%) + conc. H2S04 was used during the study of the microstructure of the alloys with the etching time of 20 sec. The microhardness of the alloys was measured on a microhardness tester PMT-3 at the loads 0.01 and 0.02 N. MSA of the system alloys was performed on a MIM-8 metallographic microscope on preliminarily etched sections polished with the paste.
3. Results and discussion
Based on the results of physicochemical analysis (DTA, XRD, MSA, and density determination), a phase diagram of the system AgGaS2-FeGa2S4 was developed. The DTA results showed that all thermograms of the system alloys (90-10 mol% AgGaS2) have three endoeffects each, except for the alloy containing 56 mol% FeGa2S4 while the alloys containing 90 and 10 mol% AgGaS2 demonstrate two and four endoeffects each respectively (Table 1). The effects at 905 K correspond to the phase transition a-FeGa2S4 ^ p-FeGa2S4.
As Fig. 1 shows, the phase diagram of the system AgGaS2-FeGa2S4 belongs to the eutectic type with limited component solubility in solid state. The solubility at 300 K based on AgGaS2 is
AgGaS; 20 40 GO SO FeGa^ Fig. 1. Phase diagram of the AgGaS2-FeGa2S4 system
Table 1. Composition, results of the DTA of alloys of the AgGaS2-FeGa2S4 system
Table 2. Annealing of the alloys of the AgGaS2-FeGa2S4 system at temperatures of 650 and 800 K
Composition mol% FeGa2S4 Thermal effects, K
100 1420
90 905, 980, 1235, 1405
80 905,1100, 1375
70 905,1100, 1310
60 905,1100, 1175
56 1100 (eutectic)
50 905,1100, 1145
40 905,1100, 1195
30 905,1100, 1230
20 905, 1100, 1250
10 1175, 1260
0.0 1270
11 mol% FeGa2S4 and 4 mol% AgGaS2 based on FeGa2S4. The solubility at the eutectic temperature stretches to 16 and 10 mol% respectively. The eutectic has a composition of 56 mol% FeGa2S4 and crystallises at 1100 K.
The liquidus of the system AgGaS2-FeGa2S4 consists of the primary crystallisation branches a and b solid solutions crossing at 56 mol% FeGa2S4 and T = 1100 K. The temperature of the phase transition P(FeGa2S4)^P'(FeGa2S4) is reduced to 905 K under the influence of the second component. MSA of the annealed alloys showed that the alloys of the system AgGaS2-FeGa2S4 are single-phase except for the alloys containing 1196 mol% FeGa2S4
Below solidus, a and b solid solutions co-crystallise. The solubility regions based on source components are narrow: 11 mol% FeGa2S4 based on AgGaS2 and 4 mol% AgGaS2 based on the second component. Solubility limits were determined using the XRD and MSA of the alloys annealed and quenched at the temperature 700 K.
To determine the limits of the regions of solid solutions of the source components (AgGaS2 and FeGa2S4), 98, 96, 95, 93, 91, 90, 89, 88 mol% were additionally synthesised from both sides. These alloys were annealed at 650 and 800 K with the annealing duration of 1 month (Table 2).
After the annealing, a microstructural analysis of the alloys was conducted that showed that there are limited solubility regions near AgGaS2 and FeGa2S4. Solid solutions based on AgGaS2 belong to the Ag2GeS3 structural type and
Composition mol% 650 K phase count 800 K, phase count
AgGaS2 FeGa2S4
0.0 100 a a
2.0 98 a a
4.0 96 a+p a
5.0 95 a+p a+p
7.0 93 a+p a+p
9.0 91 a+p a+p
10 90 a+p a+p
11 89 a+p a+p
12 88 a+p a+p
100 0.0 p p
98 2.0 p p
96 4.0 p p
95 5.0 p p
93 7.0 p p
91 9.0 p p
90 10 a+p p
89 11 a+p p
88 12 a+p a+p
crystallise in the monoclinic syngony. Within the solubility limits, the parameters of the crystal lattice increase: a = 0.627+0.748, b = 0.580+0.664, c = 1.318^1.386 nm, p = 93.27+93o61.
The results of the X-ray phase analysis are in good agreement with the data of the microstructural analysis and confirm the formation of solid solutions based on the source components in the system AgGaS2-FeGa2S4.
The data of the X-ray powder patterns of the alloys of the system AgGaS2-FeGa2S4 showed that the samples of the compositions 0-11 and 95-100 mol% FeGa2S4 are single-phase. Their diffraction lines are identical to the diffraction patterns of the source components (silver thiogallate and iron thiogallate). The diffraction pattern of the alloys containing 11-96 mol% FeGa2S4 is two-phase (Fig. 2).
4. Conclusions
1. Using the methods of physicochemical analysis (XRD, DTA, MSA), a phase diagram of the system AgGaS2-FeGa2S4 was studied and constructed for the first time. It was established that the system is a quasi-binary cross-section of the FeS-Ga2S3-Ag2S quasi-triple system and belongs to the simple eutectic type.
a . I 1 !.. . 1
ill 2
1 .Kl L I 1 1 1 1 .
[ Jl I . 1 1 1 J ll. . . 4
1 1 ■A J .1 i il. .. . 5
2-Theta - Scale
Fig. 2. Diffraction pattern of the alloys of the AgGaS2-FeGa2S4 system: 1 - AgGaS2; 2
40 mol% FeGa2S4; 4 ■
96 mol% FeGa2S4; 5 ■
FeGaA
11 mol% FeGa2S4; 3 ■
2. The formation of solid solutions based on their source components was found in the AgGaS2-FeGa2S4 system. The solubility based on iron thiogallate at room temperature is 4 mol% AgGaS2 and the solubility based on silver thiogallate is 11 mol% FeGa2S4.
Conflict of interests
The author declares that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper.
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Information about the authors
Sharafat H. Mammadov, PhD in Chemistry, Associate Professor, Senior Researcher, Institute of Catalysis and Inorganic Chemistry n.a. Academician M. F. Nagiyev of the Azerbaijan National Academy of Sciences, Baku, Azerbaijan; e-mail: azxim@mail.ru. ORCID iD: https://orcid.org/0000-0002-1624-7345.
Author have read and approved the final manuscript.
Translated by Marina Strepetova
Edited and proofread by Simon Cox
