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CHEMICAL PROBLEMS 2022 no. 1 (20) ISSN 2221-8688
UDC: 546.123.3.644.19.22.23
GLASS FORMATION AND PHASE EQUILIBRIA IN THE Tm-As-S AND Tm-As-Se SYSTEMS AND THEIR PROPERTIES
T.M. Ilyasly, G.G. Gahramanova, R.F. Abbasova, S.M. Veysova, Z.I. Ismailov
Baku State University, Z.Xalilov str., 23, Baku AZ1148, Azerbaijan Republic E-mail: zakir-51@ mail.ru
Received 21.01.2022
Accepted 11.03.2022
Abstract: The nature of the physicochemical interaction in the Tm-As-S and Tm-As-Se systems was studied along various cross sections by methods of Differential Thermal (DTA), X-Ray Diffraction (XRD) and Microstructural (MSA) Analyzes, measuring their micro-hardness and determining their electrophysical properties. The investigation of the alloys of the system started by studying the properties of the initial components in cooling modes of 7-10deg/min. After establishing the boundary of the glass formation region in the systems, the physicochemical properties of glasses and intermediate phases were studied. Analysis showed that all effects on the thermograms were reversible. The compounds of TmAsS3, TmAs4S7, TmAs2S4, Tm3As4S9 compositions were formed in the As2S3-Tm2S3, As2S3-TmS systems. The compounds of TmAs4S7, TmAsS and TmAs2S4 compositions melted congruently, while the compounds of Tm3As4S9 and TmAsS3 melted incongruently. TmAsSe, TmAsSe3, TmAs4Se7, TmAs2Se4 and Tm3As4Se9phases were formed in the Tm-As-Se system while Tm=As4Se9 was formed by the peritectic reaction TmSe + L Tm=As4Se9. Microstructural analysis showed that all alloys of the Tm-As-S, Tm-As-Se cross sections were two-phase, except for the composition of intermediate phases. Proceeding from the results of XRD, the lattice parameters of TmAsS, TmAsS3, TmAs4S7, TmAs2S4, as well as parameters of selenium-containing compound were calculated; it found that it crystallized in the rhombic syngony. Based on the results of physicochemical analysis, it was established that the studied cross sections were quasi-binary sections of the Tm-As-S and Tm-As-Se ternary systems. The phase diagram of cross sections with the participation of sulfur and selenium was plotted using the results of physicochemical analysis; it established that the studied cross sections were quasi-binary sections of the Tm-As-S and Tm-As-Se ternary systems.
Keywords: analysis, cross section, microhardness, alloy, temperature, crystallization DOI: 10.32737/2221-8688-2022-1-68-81
Introduction
Interest in rare earth elements (REE) and their compounds, as well as in arsenic chalcogenide, is related to the use of their compounds in various fields of technology, as well as in obtaining materials with pre-targeted properties. Lanthanide compounds are used as catalysts, HTSC (high-temperature
superconducting) ceramics of conductive materials, additives to various alloys for increasing their mechanical resistance, thermal resistance, for obtaining special types of glass used in nuclear technology, for the manufacture
of luminous compositions and luminescent materials, in radio technology and optoelectronics, as well as in special probes to study the structure of solutions [1-4]. There are sufficient data on the study of the Ln-As-X system [5-7].
There are excerpted data on the interaction of the Tm-containing-systems and its chalcogenides with arsenic chalcogenides and on the intermediate phases [9-10] formed in them.
CHEMICAL PROBLEMS 2022 no. 1 (20)
www.chemprob.org
Purpose of the study
The purpose of this work is to study the nature of the physicochemical interaction in the Tm-As-S(Se) system along various cross sections: Tm-AsS, Tm-As2S3, As2S3-TmS,
As2S3-Tm2S3, Tm-AsSe, As2Se3-Tm, As2Se3-TmSe, As2Se3-Tm2Se3 and the study of the electrophysical properties of compounds in the wide temperature range.
Material and research methods
TmS, AsS, As2S3, AsSe, As2Se3, Tm2Se3 were synthesized from the elements to study abovementioned cross sections; arsenic of grades A-5, Tm-A-1 (99.97), sulfur of the high purity grade for analysis, selenium of grade B-4 were for this synthesis. The synthesis regime was selected on the basis of physicochemical properties of the initial components and the thermogram -the record of alloys synthesis.
After vacuum pumping the ampoules, the initial samples (3 g) were placed in the oven which was heated to 650-750K for 6-8 hours, and then the temperature was raised to 1200K. The ampoules were kept at this temperature for 5 hours and the ampoules were slowly cooled to room temperature together with the furnace.
The alloys were subjected to
homogenizing annealing for 650 hours depending on the concentration of components at appropriate temperatures, 50-70 degrees below the solidus.
The nature of the physicochemical interaction in the Tm-As-S and Tm-As-Se systems was studied by the methods of differential thermal (DTA), X-ray phase (XRD) and microstructural (MSA) analyzes, measuring the microhardness and determining the electrophysical properties.
For the study of the high-temperature part, HTSC 987 equipment was used. DTA was carried out by PDS-021 (two-coordinate self-recorder potentiometer). Microscope MIM-7, MIN-8 and microhardness tester PMT-3).
Results of the study and their discussion
The equilibrium state of the alloys was controlled by the MSA and XRD methods. Alloys with a high content of arsenic sulfide were cherry-red and the color of selenide-based alloys was black. Analysis of thermograms
showed that all effects on thermograms are reversible. Mainly, two endothermic effects were obtained on the heating curves, in addition to the compositions corresponding to distectic compounds.
AsS-Tm cr
Alloys of the system were synthesized in rotary tube furnaces; cooling the alloys was carried out at the rate of v=7-10 deg/min (Table 1).
s section
As is seen from Table 1, with a cooling rate of v=7-10 deg/min, the glass formation area reaches to 10 mol%. Some physicochemical properties of glasses are given in Table 1.
Table 1. Some macroscopic properties of alloys (glasses) of the AsS-Tm system (the rate of cooling
v=7-10 deg/min)
№ Composition of the alloys, mol% Thermal effects T,K Density d,g/cM3 Microhardness H, g/mm2 Results of MSA
AsS Tm Tg T T crys Tmelt
1 100 0 430 - 580 3.75 118 Single-turbid phase
2 99 1 436 470 575 3.81 120 Single-turbid phase
3 97 3 450 475 568 3.85 125 Single-turbid phase
4 93 7 465 485 545 3.94 133 Single-turbid phase
5 90 10 468 497 535 3.98 135 Single-turbid phase
6 85 15 475 900 530 4.15 140 Crystalline glass
The equilibrium state of the alloys was provided to establish phase equilibrium in the studied systems.
They were annealed for 500 hours below the solidus by 50-100°C to homogenize the
alloys. After the equilibrium state, the alloys were studied again and, the phase diagram of Tm-AsS was plotted on the basis of the results of the integrated research methods of physicochemical analysis (Fig. 1).
T, K 2075 1875 1675 1475
1275 1075
875
675
475
- L
L+ y (TmAsS)
- Tm+L jCA
_ _ y _
- (TmS) P^iy" V 00 » w \ <
" y (TmAsS) +Tml/|/ » \ i-J 480 \
Vj^/ y(TmAsS)+AsS II Ii
Tm
20
40 60 mol %
80 AsS
Fig. 1. Phase diagram of the Tm-AsS system As is seen from Fig., the TmAsS (y) intermediate phase melting at 1350K was obtained.
AS2S3 -TmS cross section
These alloys were synthesized similarly 13 mol% TmS was obtained in the form of to the alloys of the As2S3-Tm system. After glass. Glassy alloys were investigated synthesis, the alloy was cooled at the rate of physically and chemically. The research results v=7-10 deg/min. After cooling the alloys, about are presented in Table 2.
Table 2. The values of some macroscopic properties of alloys of the As2S3 -TmS system (glasses)
№ Composition of alloys, mol Thermal effects T,K Micro-hardness Density d, g/cm3 Results of MSA
% H g/mm2
As2S3 TmS T T A crys Tmelt
1 100 0 440 470 580 118 3.75 Single-turbid phase
2 97 3 445 478 550 125 3.79 Single-turbid phase
3 95 5 448 480 595 130 3.81 Single-turbid phase
4 93 7 453 485 555 135 3.85 Single-turbid phase
5 88 10 455-465 475-495 525-580 140-145 3.90-3.95 Single-turbid phase
6 87 13 475 495 565 135 4.01 Single-turbid phase
Three thermal effects appeared on thermograms of the alloys (Fig. 2).
T,K
> ^
Fig. 2. Thermograms of the alloys of [As2S3]0,90[TmS]0;1 composition Tg - vitrification temperature, Tcrys - temperature of crystallization, Tmelt - melting temperature
T,K
1473
1273
1073
873
673 " a+L
AS2S;
2S3 20
40 60
mol%
80 TmS
Fig. 3. Phase diagram of the As2S3 -TmS system
X
The phase diagram of the As2S3 -TmS cross section was plotted after providing an equilibrium state for the alloys (Fig. 3).
Three intermediate phases Tm3As4S9, TmAs2S4 and TmAs4S7 were formed along the studied cross section. TmAs2S4 and TmAs4S7
compounds melted congruently at the temperatures of 915K and 1175K, respectively, while compounds of Tm3As4S9 composition were formed by the following subsequent peritectic reaction:
1173
L + TmS <==> Tm3As4S9
The results of XRD showed that new diffraction patterns appear on the diffractograms of the alloys. XRD analysis data are given in Table 3. The Table shows the relationship between inter-planar distances and intensities of diffraction lines.
The XRD results showed that new diffraction lines appear on the diffraction patterns of the alloys in addition to the line of the initial As2S3 and TmS. The data of XRD are given in Table 3.
Table 3.Results of XRD analysis for intermediate phase obtained in the As2S3 -TmS system
Formula of compounds 0 lexp. 1% da
TmAs4S7 13.21 10 48.48 3.374
16.56 16 69.57 3.712
16.85 18 78.26 2.661
17.44 24 100 2.621
19.55 23 98 2.220
20.73 16 78.13 2.710
TmAs2S4 12.31 18 37.14 3.622
15.62 13 37.16 2.871
16.12 15 42.36 2.780
16.62 33 94.29 2.713
16.18 35 100 2.504
22.34 11 31.43 2.102
25.76 5 14.29 1.775
Tm3As4S9 10.71 15 22.41 4.152
12.27 18 26.89 8.634
15.7 19 28.42 2.851
16.5 32 47.81 2.801
16.57 46 68.72 2.710
19.1 67 100 2.403
19.6 29 43.3 2.310
22.11 16 23.88 2.051
25.83 9 13.43 1.813
Parameters of crystalline lattice, singonies and based on the calculated data (table 4). volume of elemental cells were determined
Table 4. Crystallographic and physicochemical properties of thulium ternary compounds
(intermediate phases)
Compound Space group Singony Type of structure Parameters of lattice, nm Density, g/cm3 Micro-hardness MPa
Pbnm Rhomb. Sb2S3 a b c z p Pcalc. P A pc.
TmAs4S7 1.189 1,449 0.403 4 4.19 4.17 1925
TmAs2S4 1.155 1.350 0.356 4 4.43 4.41 2215
Tm3As4Se9 2.681 2.438 0.402 4 4.65 4.62 2025
TmAsSe3 1.115 1.194 0.403 5.09 5.06 1865
As2S3 -Tm2S3 cross section
Synthesis and cooling of alloys were were obtained in a glassy form. The values of carried out similar to the above systems. In this some macroscopic properties of glasses are case, alloys containing up to 15 mol% Tm2S3 presented in Table 5.
Table 5. Some physicochemical properties of the glasses of the system (rate of cooling v=7-10
deg/min.)
Composition of Thermal effects Micro- Density d, g/cm3
№ alloys T,K hardness H g/mm2 Results of MSA
As2S3 Tm2S3 T T i crys Tmelt
1 100 0 440 475 580 120 3.75 Single-turbid phase
2 97 3 448 480 565 125 3.83 Single-turbid phase
3 95 5 455 485 510 128 3.85 Single-turbid phase
4 93 7 460 490 485 135 3.94 Single-turbid phase
5 90 10 465 510 470 143 4.01 Single-turbid phase
6 85 15 480 515 485 140 4.25 Single-turbid phase
7 80 20 485 520 505 145 4.30 Crystalline glass
Fig. 4. X-ray diffraction patterns of the alloys of the As2S3 -Tm2S3 system (before annealing) 1-5
mol%, 2-10 mol%, 3-20 mol% Tm2S3
The XRD results showed that there were Single-turbid phase appeared from the
no intense X-ray diffraction lines on the microstructural analysis; micrographs of the
diffraction patterns of alloys from the glass alloys are shown in Fig. 5. formation area (Fig. 4).
a) b)
Fig. 5. Microstructures of the alloys of the As2S3 -Tm2S3 systems a) 5 mol% As2S3 b) 15 mol% Tm2S3
Results of integrated methods of composition was formed in the system at the physicochemical analysis showed that one temperature of 1123K according to the incongruently melting compound of TmAsS3 following reaction:
1123
L+y-Tm2S3 TmAsS3
Fig. 6. Phase diagram of the As2S3 -Tm2S3 system
AsSe -Tm
The alloys were synthesized by the direct ampoule method; the synthesis mode was stepwise. The systems based on AsSe were annealed at the temperature of 475K for 500 hours, and as a result of that alloys were obtained. The phase diagram of AsSe - Tm cross section was plotted on the basis of the
oss section
results obtained from the integrated methods of PCA. As is seen from Fig.7, one congruently melting compound of TmAsSe composition was formed in the system at 1125K. The solubility range of up to 2 mol Tm % was found on the basis of AsSe.
mol %
Fig. 7. Phase diagram of the AsSe -Tm system
Fig. 8. Thermogram of alloys of [As2Se3]090[TmSe]01 composition
As2Se3 -TmSe Alloys of this system were synthesized similarly to the above systems and cooled with the rate of v=7-10 deg/min.
Alloys of up to 30-40 mol% TmSe were obtained in the form of a black powder; while alloys of 12 mol% TmSe in the form of conchoidal fracture. The obtained alloys were investigated by the integrated methods of physical-chemical analysis. The study showed
cross section
that these alloys were glasses. Thermograms of the alloys containing 10 mol% TmSe are shown in Fig.8.
Results of XRD analysis are shown in
Fig.9.
As is seen from the diffraction pattern of alloys of the As2Se3-TmSe system, there are no intense diffraction lines special to crystalline substances (Fig. 9)
Fig. 9. Diffractograms of alloys of 1) [As2Se3]o.9o[TmSe]0.i 2) [As2Se3]o.85[TmSe]o.i5 systems
Table 6. Some physicochemical properties of the alloys of As2Se3-TmSe system
(Rate of cooling v=7-10 deg/min)
№ Composition of alloys Thermal effects T,K Microhardness g/mm Density d, g/cm3 Results of MSA
As2Se3 TmSe Tg T T crys Tmelt
1 100 0 450 - 650 130 4.58 Glass
2 99 1 456 520 645 130 4.61 Glass
3 97 3 465 515 640 135 4.70 Glass
4 95 5 476 500 635 140 4.75 Glass
5 90 10 480 510 630 148 4.83 Glass
6 85 15 485 518 615 155 4.85 Glass
7 80 10 493 500 610 160 4.95 Crystalline glass
After providing the equilibrium state for the alloys, they were studied again by means of
the physicochemical analysis, the phase diagram of the As2Se3-TmSe system was plotted (Fig. 10).
Fig. 10. Phase diagram of the As2Se3 -TmSe system
Three intermediate phases Tm3As4Se9, system. TmAs4Se7 melts congruently, while TmAs2Se4 and TmAs4Se7 are formed in the TmAs2Se4 and Tm3As4Se9 melt incongruently.
As2Se3 -Tm2S
Synthesis of the alloys of this system was carried out similarly to the alloys of the As2Se3 -TmSe system. The synthesis process was stepwise: firstly, the temperature of the furnace was raised to 750K, then up to 900-1000K; the alloys were kept at this temperature for 2 hours, and then they were cooled together with the furnace. After synthesis, the alloys were obtained in the compact form up to 70% Tm2Se3, and then they turned into the spec form and had porous. The alloys were annealed at the temperature of 750K for 300 hours to provide the equilibrium state.
i cross section
The phase diagram of the As2Se3 -Tm2Se3 cross section was plotted using the results of physical and chemical analysis (Fig. 11).
As is seen from the Fig. 11, the cross section is a quasi-binary section of the Tm-AsSe ternary system.
After the separation of the intermediate phases, their temperature dependence of the electrical conductivity was determined individually (Fig. 12,13). It has been established that they are p-type semiconductors.
Fig. 11. Phase diagram of the As2Se3 - Tm2Se3 system
Fig. 12. Temperature dependence of the electrical conductivity of sulfide compounds
Fig. 13. Temperature dependence of the electrical conductivity of selenide compounds.
Conclusions
1. When studying the cross sections of the Tm-As-S and Tm-As-Se ternary systems, glass formation areas were revealed in them and their boundary of existence was outlined.
2. When studying Tm-AsS, Tm2S3-As2S3, TmS-As2S3 Tm-AsSe, TmSe-As2Se3, Tm2Se3-As2Se3 cross sections, intermediate phases TmAsS, TmAsS3, TmAs4S7, TmAs2S4, Tm3As4S9, TmAsSe, TmAs4Se7, TmAs2Se4, Tm3As4Se9 and TmAsSe3 also appeared in these cross sections; their
formation and melting nature was determined. It was established that the cross sections were quasi-binary sections of the Tm-As-S and Tm-As-Se ternary systems.
3. Parameters of the crystal lattice and intermediate phases have been calculated. It is established that they crystallize in a rhombic syngony.
4. Study into the electrical conductivity of the glasses and intermediates revealed that they are semiconductors of p-type conductivity.
References
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in amorphous As-S-Se films. Optoelectronics and Advanced Materials. 2011, vol.13, no. 11-12, p.1531.
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10.5923/j.ijmc.20130302.03
3. Seema Kandpal, Kushuana R.P. S.Photoacoustic spectroscopy of thin films 6. of As2S3, As2Se3 and GeSe2. Indian Academy of Sciences PRAM ANA journal of physics. 2007, vol. 69, no. 3, pp. 481-484.
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Ilyasly T.M., Sadigov F.M., Bayramova U.P., Mamedova L.M, Gahramanova G.G. As2S3-TmS and As2S3-Tm2S3 quasi-binary cross sections of the Tm-As-S ternary
systems. International Journal of app. and gen. Researches. 2017, vol. 1, no. 8, pp. 40-44.
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Journal, (Warsaw, Poland) 3(31), 2018 part 2. pp. 60-65 [email protected]
9. Teymur Ilyasly, Gunel Gahramanova, Rana Abbasova, Sitara Veysova, Zakir Ismailov. Investigation of the electrical properties of glasses of Tm-As-S and Tm-As-Se systems. New Materials, Compounds and Applications. 2021, vol. 5, no. 3, pp. 227234.
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Tm-As-S Vd Tm-As-Se SiSTEMLERiNDd §Ü§dLd§Md, FAZA TARAZLIGI Vd ARALIQ
FAZALARIN XASSdLdRI
T.M. ilyasli, G.H. Q9hr9manova, R.F. Abbasova, S.M. Veysova, Z.i. ismayilov
Baki Dövldt Universiteti, AZ1148 Baki, Z.Xdlilov kûç.,23; e-mail: [email protected]
Xulasd: Tm-As-S vd Tm-As-Se sistemldrindd fiziki-kimysvi qarçiliqli tdsirin xarakteri müxtdlif en kdsiyldr boyunca Diferensial Termiki (DTA), X-§üalarinin difraksiyasi (XRD) vd Mikroquruluç (MQA) analizldri ild öyrdnilmi§, onlarin mikrosdrtlikldri vd elektrofiziki xassdldri müdyydn edilmiçdir. Sistemin drintildrinin tddqiqind 7-10ddr/ddq soyutma rejimldrindd, ilkin komponentldrin xassdldrinin öyrdnilmdsi ild ba§lanmi§dir. Sistemldrdd §ü§d dmdldgdlmd sahdsinin sdrhddi müdyydn edildikddn sonra §ü§dldrin vd araliq fazalarin fiziki-kimydvi xassdldri tddqiq edilmiçdir. TmAsS3, TmAs4S7 , TmAs2S4, Tm3As4S9 birldçmdldri As2S3-Tm2S3, As2S3-TmS sistemldrindd dmdld gdlir. TmAs4S7, TmAsS vd TmAs2S4 kompozisiyalarinin birldçmdldri konqruent olaraq driyir, Tm3As4S9 vd TmAsS3 birldçmdldri isd inkonqruent driyir. Tm-As-Se sistemindd TmAsSe, TmAsSe3, TmAs4Se7, TmAs2Se4 vd Tm3As4Se9 fazalari dmdld gdlir. Tm3As4Se9 peritektik reaksiya ild TmSe + L ^ Tm3As4Se9 dmdld gdlir. Mikroquruluç tdhlili göstdrdi ki, araliq fazalarin tdrkibi istisna olmaqla, Tm-As-S, Tm-As-Se kdsikldrinin bütün drintildri ikifazalidir. XRD-nin ndticdldrind dsasdn TmAsS, TmAsS3, TmAs4S7, TmAs2S4-ün qdfds parametrldri, hdmçinin selen tdrkibli birldçmdnin parametrldri hesablanmiçdir. Müdyydn edilmiçdir ki, birldçmdldr rombik sinqoniyada kristallaçirlar. Tddqiqat ndticdldrind dsasdn müdyydn edilmiçdir ki, tddqiq olunan kdsikldr Tm-As-S vd Tm-As-Se ^lü sistemldrinin kvazibinar kdsikldridir. Fiziki-kimydvi analizin ndticdldrinddn istifadd etmdkld kükürd vd selenin içtiraki ild kdsikldrin faza diaqrami qurulmuçdur; müdyydn edilmiçdir ki, tddqiq olunan kdsikldr Tm-As-S vd Tm-As-Se ^lü sistemldrinin kvazibinar kdsikldridir. Açar sözlar: analiz, kdsik, mikrobdrklik, drinti, temperatur, kristallaçma
СТЕКЛООБРАЗОВАНИЕ И ФАЗОВЫЕ РАВНОВЕСИЯ В СИСТЕМАХ Tm-As-S И Tm-As-Зе И ИХ СВОЙСТВА
Т.М. Ильяслы, Г.Г. Гахраманова, Р.Ф. Аббасова, С.М. Вейсова, З.И.Исмаилов
Бакинский государственный университет AZ 1148 Баку, ул. З.Халилова, 23; e-mail [email protected]
Аннотация: Методами дифференциально-термического (ДТА), рентгенофазового (РФА) и микроструктурного (МСА) анализов, измерением микротвердости и электрофизических свойств изучен характер физико-химического взаимодействия в системах Tm-As-S и TmAsS по различным разрезам. Исследование сплавов системы было начато изучением свойств исходных компонентов в режимах охлаждения со скоростью 7-10 град/мин. После установления в системах границы области стеклообразования изучали физико-химические свойства стекол и промежуточных фаз. Анализ термограмм показал, что все эффекты на термограммах обратимые. В системах As2S3-Tm2S3, As2S3-TmS образуются соединения состава TmAsS3, TmAs4S7, TmAs2S4, Tm3As4S9. Соединения TmAs4S7, TmAsS, TmAs2S4 плавятся конгруэнтно, а соединения Tm3As4S9 и TmAsS3 - инконгруэнтно. В системе Tm-AsS выявлено образование фаз TmAsSe, TmAsSe3, TmAs4Sey, TmAs2Se4 и Tm3As4Seg. Tm3As4Seg образуется no перитектической реакции TmSe Ж Tm3As4Seg.
Микроструктурный анализ показал, что все сплавы разрезов Tm-As-S, Tm-AsS двухфазные кроме состава промежуточные фаз. По результатам РФА рассчитаны параметры решетки соединений TmAsS, TmAsS3, TmAs4S7, TmAs2S4 а также соединений с участием селена и установлено, что они кристаллизуется в ромбическом сингонии. По результатам физико-химического анализа построена диаграмма состояния разрезов с участием серы и селена и установлено, что исследованные разрезы являются квазибинарными сечениями тройных систем Tm-As-S и Tm-AsS.
Ключевые слова: анализ, разрез, микротвердость, сплав, температура, кристаллизация
