AD-A 12S121 PREPARATION AND CHARACTERIZATION OF CDRSNN05SE SINGL F /CRYSTALS(U) BROWN UNIV PROVIDENCE RI DEPT OF CHEMISTRY13 KHAZAT ET AL. 03 JAN B3 TR-25 NOCO14-77C-0387
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4. TITLE (and Subtitlie) S. TYPE OP REPORT & PERIOD COVERED
PREPARATION AND CHARACTERIZATION OF.d95Mn 05S SIGERYAL 6. PERFORMING ORO. REPORT NUMOER
_ _ _ _ _ _ _ __ _ _25
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B. Khazai, R. Kershaw, K. Dwight, and A. Wold N01-7C08
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(M Professor Aaron Wold AREA A WORK UNIT NUMUERSBrown University, Department of Chemistry NR-359-653
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19. KEY WORDS fContinue on revorse aide it necessary and Identify by block number) __
1. Manganese-Substituted Cadmium Selenide
* 2. Homogeneous Single Crystals
3. Magnetic Susceptibility and Homoge jty20. AIISTRA9.1j (Continue on rererse side It necessary and Identtify by block nflinteuI Homogeneous crystals of
A ~Cd 9Mn.0 5 Se of high optical quality have b ~pn grown by a modified Bridgmanmethod. Magnetic susceptibility measureme fts verify the uniform distribution 1of 1n(II) obtained after annealing at 6000C Crstals grown in the presence
L of 5 atomic percent excess seleni showed high resistivity; the addit nof (~~I:* __ mg iodine to a 10 g charge sulte n e conductivity and a om temp
L4 ~ ature carrier concentration 1 -3 The Hall mobility these___ crystals was approximately 290 cum2V- sc
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OFFICE OF NAVAL RESEARCH
Contract N00014-77-C-0387
Task No. NR-359-653
TECHNICAL REPORT NO. 25
Preparation and Characterization of
Cd 95Mn 0oSe Single Crystals
by
B. Khazai, R. Kershaw, K. Dwight, and A. Wold
Department of Chemistry
Brown University
Providence, Rhode Island 02912
Prepared for Publication
in the
Materials Research Bulletin
December 17, 1982
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PREPARATION AND CHARACTERIZATION OF Cd. 95Mn. 0 5 S SINGLE CRYSTALS
B. Khazai, R. Kershaw, K. Dwight, and A. WoldDepartment of Chemistry, Brown University
Providence, Rhode Island 02912
ABSTRACT:Homogeneous crystals of Cd.95Mn.05 Se of high optical quality havebeen grown by a modified Bridgman method. Magnetic susceptibilitymeasurements verify the uniform distribution of Mn(II) obtainedafter annealing at 600*C.
Crystals grown in the presence of 5 atomic percent excess seleniumshowed high resistivity; the addition of 1 mg iodine to a 10 gcharge resulted in n-type conductivity and a room-temperaturecarrier concentration of 2.9 x1016 cm-3 . The Hall mobility of thesecrystals was approximately 290 cm2 V-1 sec-1.
Introduction
Recently, cadmium selenide has been the subject of intensiveinvestigation for the characterization of its electro-optical properties(l-S).Joshi et al. (6) have indicated that for cadmium telluride, the characteristicoptical response of the photoconductor can be tuned by the incorporation ofMn(II)(3d5 ). Similar phenomena should be observed for cadmium selenide,with the transition energy gap adjusted by the introduction of controlledquantities of manganese dopant.
Crystallographically, one of the modifications of both MnSe andCdSe is that of the wurtzite structure (7), where the cations are tetrahedral-ly coordinated in a hexagonal plose-packed array in which one half of thetetrahedral sites are occupied by the metal atoms. The structural similaritybetween MnSe and CdSe should therefore allow for the formation of a solidsolution of the type Cdl.xMnxSe. Wiedemeier and Sigai (8) have prepared sucha solid solution containing up to SO atomic percent of manganese andcrystal.izing with the wurtzite structure.
In this study, we are reporting the growth and characterization ofsingle crystal boules of the general composition Cdl.xMnxSe. The materialswere prepared with either high or low resistivities, and the manganese dopingwas kept at S atomic percent in order to minimize manganese-manganese inter-actions.
Experimental
Crystal Growth
Single crystals of the system Cdl_xMnxSe were prepared from themelt, using the Bridgman technique. The starting materials were in theirelemental state and were subjected to purification prior to their use.Cadmium (Johnson Matthey 99.999%) was heated to the melting point under adynamic vacuum for a few minutes. Selenium was purified by sublimation ofthe element (Atomergic Chemetals 99.9999%) at 200*C and under a dynamicvacuum. Manganese (Atomergic Chemetals 99.99%) was deoxidized by placingthe metal in a sealed silica tube along with titanium metal in a separatecompartment. The tube was then heated at 1000 0C for 24 hours.
The charge containing approximately 10 g of stoichiometric amountsof the starting materials was placed in a heavy-wall silica tube and sealedunder high vacuum. The tube was then placed in a vertical furnace equippedwith a puller/rotor action motor. The rotor was used to ensure uniformheating across the growth ampoule during crystal formation. The charge wasallowed to prereact overnight in the hot zone of the furnace at 1000*Cbefore increasing the temperature to 12000C. The growth ampoule was subse-quently raised above the hot zone and was allowed to pass through a tempera-ture gradient at a rate of 3.2 cm/day for a period of five days. The bestcrystals were obtained when S atomic percent excess selenium was used. Thecrystal grew approximately along the c axis. The angle between the c axisand the growth direction is %,lS*(±l°)7 The lattice parameters area= 4.268(2)1, c= 6.983(2)X, and the space group is P63mc.
Conducting crystals were prepared by the introduction of smallquantities of iodine into the charge either through an H-tube, for largerquantities, or by prereacting the selenium with iodine at 100*C in a sealedtube for smaller quantities.
The as-grown crystals possessed a relatively high range of inhomo-
geneity with respect to manganese distribution from top to bottom of the
boules. An equilibrium state could, however, be attained by a subsequent
five-day annealing of the growth tube in the constant temperature zone of a
wound-core transport furnace at 6000C or 8000C for high resistivity or
high conductivity samples, respectively. The crystals thus formed were cut
into discs and subjected to various measurements.
X-ray Analysis
Powdered samples were anglyzed on a Philips-Norelco powder dif-
fractometer using CuKal (X = l.S404A) radiation, to ascertain the formationof the cadmium selenide phase.
III II ':4--.-
- u.. • .v W -.
Magnetic Measurements
Magnetic susceptibilities were measured using a Faraday balance (9)at a field strength of 10.4 kOe. The data were then corrected for the corediamagnetism of cadmium selenide.
Electrical Measurements
The electrical measurements were made using the van der Pauw
technique (10). Contacts were made by the ultrasonic soldering of indiumdirectly onto the samples, and their ohmic behaviors were established bymeasuring their current-voltage characteristics. The sign of the majoritycarriers was determined from the qualitative measurement of the Seebeckeffect, as well as from Hall measurements.
Optical Measurements
Optical transmissions were measured using a tungsten iodide lampand a calibrated silicon diode. Spectral transmission data were obtainedusing a monochromator (Oriel Model 7240). No correction was made for thesurface reflectivity of the polished specimen.
Results and Discussion
Crystals of the composition Cd 95Mn osSe were grown from the meltusing the Bridgman technique. High quality, single crystal boules wereobtained when 5 atomic percent excess of selenium was introduced into thegrowth ampoule along with the charge. X-ray diffraction patterns of thesamples indicated the formation of single-phase products which could beindexed on the basis of a hexagonal unit cell (11).
Magnetic measurements on sections cut along the growth axis of thecrystal indicated regions of inhomogeneity with respect to manganese distri-bution, extending from top to bottom of the crystal. Such non-uniformitieswere indicated by differences of as much as 0.6uB/Mn(II) between top andbottom sections of the crystal boule. However, annealing of these crystalsin the growth tube at 600*C resulted in the redistribution of manganesethroughout the boule. The measured effective moments corresponded closelyto the theoretical value of S.9fB, as expected for a localized spin-onlymoment d5 system (Table I).
Figure I indicates the magnetic susceptibility behavior over therange from liquid nitrogen to room terperature. The material shows Curie-
Weiss behavior in this region with a small antiferromagnetism as indicatedby a Weiss constant, 0, of -28K.
The electrical measurements of the as-grown or annealed crystalsindicated resistivities greater than 106Q-cm. Burmeister et al. (3) andHung et al. (12) have shown that the resistivity of cadmium selenide isrelated to cadmium or selenium vapor pressures above the specimen; the resis-tivity increases wl.th .intcreased selenium pcessure and decreases with cadmium
- .--- -. -- ~ - . ... ~ - .' !- • -- . : - ___,-._-.
TABLE I
Electrical and Magnetic Data on Cd.9RoSe
Crystal Section I2(mg) 0 cm) X1O-6 a_____ _____ 2(ng) 300Kfc) (10 emu/g) P'ef f
top 0 >10 6 3.46 S.79Ibottom 0 >106 3.46 5.79
top 1 1.94 3.58 5.88II
bottom 1 0.83 3.46 5.79
a Corrected for core diamagnetism of CdSe = 0.31x 10- 6emu/g.
vapor. This is consistent with the high resistivities observed for themanganese-doped samples grown in the presence of excess selenium. However,annealing under cadmium pressure at 4000C resulted in the formation ofnon-homogeneous, surface-conducting materials.
Optical transmission data for this system is indicated in Figure 2.Very high transparency is observed in the longer wavelengths as the energy ofthe incident photons becomes small compared to the optical transition gapwhich is 1.74 eV for cadmium selenide.
FIG. 1
A Temperatu re ,e:enderte of the 3nverse magnetic susceptibility of Cd.9gn. 0 $Se.
II, -p-
FIG. 2
Variation of optical transmission with wavelength for Cd.Q 5 14n * 0 5 5e slices
with both high and low resistivity and thicknesses of 0.81 and 0.74 -,respectively.
FIG. 3
Temperature dependence of the resistivity of conducting Cd.9 Shi05 Se.
FIG. 4Variation of Hall carrier concentration with temperature for conductingCd Mn 0Se.
FIG.S5
-Variati~on of Hall mobility with temperature for conducting Cd.9 s Mn OSo.
S-.-.-w.-~~ - U,-
The crystals prepared from charges containing 1 mg iodine for a10 g charge showed n-type conductivity, with room temperature resistivitiesless than 2.0 0-cm. Figure 3 indicates the variation of resistivity withtemperatures; the resistivity decreases up to about 2000K where it stabilizesand remains essentially constant to room temperature. This behavior may beexplained by the exhaustion of the majority charge carriers in the donorlevel, as well as by losses in mobility due to increased lattice scattering.Analysis of Hall measurement data (Figure 4) indicates that this donor stateis very shallow, located 0.03 eV below the conduction band with a carrierconcentration of 2.9x 1016 cm "3 . The Hall mobility of the electrons at room
temperature is approximately 290 cm2V-lsec-1 and shows some temperature de-pendence (Figure 5). This value is approximately half that reported for
cadmium selenide crystals grown in the presence of excess cadmium vapor (3)or with an argon atmosphere (13).
The optical transmission data for conducting crystals are included
in Figure 2. The behavior is similar to that observed for high resistivitysamples; slightly lower transparency was observed at wavelengths approaching
the optical energy gap of cadmium selenide. This behavior can be attributedto the presence of low energy transitions to shallow donor levels.
Acknowledlements
The authors would like to thank the Office of Naval Research,
Arlington, Virginia, for the support of Bijan Khazai and Kirby Dwight.
Acknowledgement is also made to Brown University for the use of its MaterialsResearch Laboratory.
References
1. M. Grynberg; Phys. Stat. Sol. 27, 255 (1968).
2. R. laubinas, A. Sakalas, A. Smilga, and J. Viscakas; Phys. Stat. Sol. 24,
K91 (1967).
3. R.A. Burmeister, Jr. and D.A. Stevenson; Phys. Stat. Sol. 24, 683 (1967).
4. S. Bergwall, A.S. Nigavekar, and P. Ohlin; Ark. for Fys. Band 40, 275
(1969).S. H. Nimura, K. Koyama, S. Kamada, and T. Nakau; Jap. J. Appl. Phys. 17,
No. 3, 581 (1978).
6. N.V. Joshi, J. Martin, and P. Quintero; Appl. Phys. Lett. 39, 1, 79 (1981).
7. R.W.G. Vyckof; "Crystal Structures" Vol. 1, Interscience Publishers, Inc.
New York, 1948.
8. H. Weidemeier and G. Sigai; 3. Solid State Chem. 2, 404 (1970).
9. B. Morris and A. Mold; Rev. Sci. Inst. 39, 1937 (1968).
10. L.J. van der Pauw; Philips Res. Rep. 13, 1 (1968).
11. Powder Diffraction File compiled by the JCPDS International Centre for
Diffraction Data, Card No. 8-459.
12. M. Hung, N. Ohashi, .and K. IgabL; Jap. 3. Appl. Phys. 8, No. 6, 6S2 (1969).
13. K. Navita, H. Watant and' dada; Jap. J. Appl. Phys. 9, 1275 (1970).
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