ferrimagnetic and antiferromagnetic structures of

9
D. E. EASTMAN In both cases Mn'+ is in an octahedral site, with a 4.24-A F=F distance in RbMnFs and a 4. 20-A O' 0' distance in MgO. It is interesting to observe that the ratio Gii/Gss is 4. 6 for Mn'+ in RbMnF, and 4.7 for Mn'+ in MgO. The dependence of 61 and 62 on the normalized sub- lattice magnetization 0. is shown in Fig. 7. It has been assumed that 0. varies with temperature according to a Brillouin function for spin —, '. The temperature de- pendence predicted by the single-ion theory of Callen and Callen'5' is shown by the solid line. According to Refs. 25 and 26, if b1 and b2 are of a single-ion nature, they should vary as Isis(I. '(0)) b(~) = = Is, s(— ~), Ii&s(I. '(0)) where I~+1~~2 is the hyperbolic Bessel function and L, ' is the inverse Langevin function. The above relation ~' K. R. Callen and H. B. Callen, Phys. Rev. 129, 578 (1963). ' E. R. Callen, A. E. Clark, B. DeSavage, and |A'. Coleman, Phys. Rev. 130, 1735 (1963). results from a classical spin average in the molecular field approximation. "" A~2 is nearly equal to a' over most of the range of |T. According to Callen and Callen, " magnetic dipolar ME coupling shouM vary as 0' except at very low temperatures. It is seen from Fig. 7 that the experi- mental b1 and b2 are not described by either the I5~2 or 0-' curves. These data support the above conclusions that both single-ion and magnetic dipolar ME coupling are comparable in magnitude. ACKNOWLEDGMENTS It is a pleasure to acknowledge D. T. Teaney and R. J. Joenk for many valuable discussions; D. T. Teaney also supplied the RbMnFs crystals and R. J. Joenk calculated the magnetic dipolar ME constants. A. M. Toxen was of considerable help in furnishing equipment and assistance for the ultrasonic measure- ment of elastic constants. 2' E. Callen and H. B. Callen, Phys. Rev. 139, 455 (1965). PHYSICAL REVIEW VOLUME 156, NUMBER 2 10 A P R IL 1967 Ferrimagnetic and Antiferromagnetic Structures of QrsSst. B. VAN LAAR Reactor Cerftrles Eederlumd, I'etteri, , The Eetherlelds (Received 14 October 1966) An investigation of the magnetic and the nuclear structures of Cr~S6 at four different temperatures has been carried out by means of neutron dif'fraction. It has been found that in the nuclear structure, deviations from the idealized structure as given by Jellinek are small at all temperatures. The magnetic structure of the antiferromagnetic phase is an antiferromagnetic screw-type spiral with its propagation vector along the c axis. The spin structure in the ferrimagnetic state is collinear and strongly related to the antiferromagnetic structure. Experimental results show that the transition from the antiferromagnetic to the ferrimagnetic state is coupled to the occurrence of a noncollinear component of the moment on the 4f sites. space group: 2 Cr in 2(a): 2 Cr in 2(c): 2 Cr in 2(b): 4 Cr in 4(f): 125 in 12(i): I'31c (Dsg'); 0,0, ~1; 1 2 1. 3&8&4 & 0, 0, 0; 0,0, 2; 8)8) ) 8)8)2 1 2~. 1 2 1 Swlthg=0 7 &)3'pi Wp" X)si 3' *»)si 3'8'k+si g=-„y=0, s= ', . t%'os. sponsored jointly by Reactor Centrum Nederland, The Netherlands and Institutt for Atomenergi, Norway. ' F. Jellinek, Acta Cryst. 10, 620 (1957). INTRODUCTION 'HE crystal structure of Cr5S6 has been deduced by Jellinek. ' It can be considered as a NiAs-type structure in which one of each six Cr atoms has been removed, leading to completely ordered vacancies. The structure as given by Jellinek is At room temperature, the lengths of the unit-cell edges are u=5. 982 A and c=11. 509A, and the cell volume is six times that of the NiAs-type subcell. The magnetic properties of Cr~S6 have been the sub- ject of many studies. The compound is antiferro- magnetic below 168 K, in the sense that there is no net magnetic moment, ferrimagnetic between 168 and 303 Ky and paramagnetic above 303 K. Kamigaichi ' H. Haraldsen and A. Neuber, Z. Anorg. Allgem. Chem. 234, 337 (1937). 'M. Yuzuri, T. Hirone, H. Watanabe, S. Nagasaki, and S. Maeda, J. Phys. Soc. Japan 12, 385 {1957). T. Kamigaichi, J. Sci. Hiroshima Univ. , Ser. A 24, 371 (1960). ' M. Yuzuri, Y. Kang, and Y. Goto, J. Phys. Soc. Japan 17, Suppl. B1, 253 (1962). 6 K. Dwight, R. W. Germann, N. Menyuk, and A. Wo}d, J. Appl. Phys. Suppl, 33, 1341 (1962). ' M. Yuzuri and Y. Xakamura, J. Phys. Soc. Japan 19, 1350 (1964}. 8 C. F. van Bruggen and F. Jellinek, Colloque International sur les derivees semi metalliques du Centre National de la Recherche Scientiique, Orsay, 1965 (to be published).

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D. E. EASTMAN

In both cases Mn'+ is in an octahedral site, with a4.24-A F=F distance in RbMnFs and a 4.20-AO'—0' distance in MgO. It is interesting to observethat the ratio Gii/Gss is —4.6 for Mn'+ in RbMnF,and —4.7 for Mn'+ in MgO.

The dependence of 61 and 62 on the normalized sub-lattice magnetization 0. is shown in Fig. 7. It has beenassumed that 0. varies with temperature according to aBrillouin function for spin —,'. The temperature de-pendence predicted by the single-ion theory of Callenand Callen'5' is shown by the solid line. According toRefs. 25 and 26, if b1 and b2 are of a single-ion nature,they should vary as

Isis(I. '(0))b(~) = =Is, s(—~),

Ii&s(I. '(0))

where I~+1~~2 is the hyperbolic Bessel function and L, 'is the inverse Langevin function. The above relation

~' K. R. Callen and H. B. Callen, Phys. Rev. 129, 578 (1963).' E. R. Callen, A. E. Clark, B. DeSavage, and |A'. Coleman,

Phys. Rev. 130, 1735 (1963).

results from a classical spin average in the molecularfield approximation. ""A~2 is nearly equal to a' overmost of the range of |T.

According to Callen and Callen, "magnetic dipolarME coupling shouM vary as 0' except at very lowtemperatures. It is seen from Fig. 7 that the experi-mental b1 and b2 are not described by either the I5~2or 0-' curves. These data support the above conclusionsthat both single-ion and magnetic dipolar ME couplingare comparable in magnitude.

ACKNOWLEDGMENTS

It is a pleasure to acknowledge D. T. Teaney andR. J. Joenk for many valuable discussions; D. T.Teaney also supplied the RbMnFs crystals and R. J.Joenk calculated the magnetic dipolar ME constants.A. M. Toxen was of considerable help in furnishingequipment and assistance for the ultrasonic measure-ment of elastic constants.

2' E. Callen and H. B. Callen, Phys. Rev. 139, 455 (1965).

PHYSICAL REVIEW VOLUME 156, NUMBER 2 10 A P R IL 1967

Ferrimagnetic and Antiferromagnetic Structures of QrsSst.

B. VAN LAAR

Reactor Cerftrles Eederlumd, I'etteri, , The Eetherlelds

(Received 14 October 1966)

An investigation of the magnetic and the nuclear structures of Cr~S6 at four different temperatures hasbeen carried out by means of neutron dif'fraction. It has been found that in the nuclear structure, deviationsfrom the idealized structure as given by Jellinek are small at all temperatures. The magnetic structure ofthe antiferromagnetic phase is an antiferromagnetic screw-type spiral with its propagation vector along thec axis. The spin structure in the ferrimagnetic state is collinear and strongly related to the antiferromagneticstructure. Experimental results show that the transition from the antiferromagnetic to the ferrimagneticstate is coupled to the occurrence of a noncollinear component of the moment on the 4f sites.

space group:2 Cr in 2(a):2 Cr in 2(c):2 Cr in 2(b):4 Cr in 4(f):125 in 12(i):

I'31c (Dsg');

0,0,~1;

1 2 1.3&8&4 &

0,0,0; 0,0,2;

8)8) ) 8)8)21 2~. 1 2 1 Swlthg=0

7

&)3'pi Wp" X)si 3' *»)si 3'8'k+si

g=-„y=0, s= —', .t%'os. sponsored jointly by Reactor Centrum Nederland,

The Netherlands and Institutt for Atomenergi, Norway.' F. Jellinek, Acta Cryst. 10, 620 (1957).

INTRODUCTION

'HE crystal structure of Cr5S6 has been deduced

by Jellinek. ' It can be considered as a NiAs-typestructure in which one of each six Cr atoms has been

removed, leading to completely ordered vacancies. Thestructure as given by Jellinek is

At room temperature, the lengths of the unit-cell edgesare u=5.982 A and c=11.509A, and the cell volumeis six times that of the NiAs-type subcell.

The magnetic properties of Cr~S6 have been the sub-ject of many studies. The compound is antiferro-magnetic below 168 K, in the sense that there is no netmagnetic moment, ferrimagnetic between 168 and303 Ky and paramagnetic above 303 K. Kamigaichi

' H. Haraldsen and A. Neuber, Z. Anorg. Allgem. Chem. 234,337 (1937).

'M. Yuzuri, T. Hirone, H. Watanabe, S. Nagasaki, and S.Maeda, J. Phys. Soc. Japan 12, 385 {1957).

T. Kamigaichi, J. Sci. Hiroshima Univ. , Ser. A 24, 371 (1960).' M. Yuzuri, Y. Kang, and Y. Goto, J. Phys. Soc. Japan 17,Suppl. B1, 253 (1962).

6 K. Dwight, R. W. Germann, N. Menyuk, and A. Wo}d, J.Appl. Phys. Suppl, 33, 1341 (1962).' M. Yuzuri and Y. Xakamura, J. Phys. Soc. Japan 19, 1350(1964}.

8 C. F. van Bruggen and F. Jellinek, Colloque International surles derivees semi metalliques du Centre National de la RechercheScientiique, Orsay, 1965 (to be published).

STRUCTURES OF Cr5S6

showed from susceptibility measurements that the spinsshould be in the basal plane in both the ferrimagneticand the antiferromagnetic state, a result which, for theferrimagnetic state, agrees with Jellinek s conclusionsfrom x-ray diffraction patterns of powder samplesoriented in a magnetic field. There are indications' thatthe ferrimagnetism in Cr~S6 disappears when the va-cancies are disordered.

Mechanisms for the transition from ferrimagnetic toantiferromagnetic have been proposed by differentauthors. Yuzuri et al. consider the possibility of somekind of triangular spin arrangement, in which a dis-continuous change of the angles between the spinscould explain the transition. Jellinek gives, as a possiblemechanism, a rearrangement of the spin-order such thatin the ferrimagnetic state the spins are distributed overtwo sublattices in a way different from that in the otherstate.

Finally, Dwight et al. ' consider the two differentchains of Cr ions parallel to the c axis which containthe vacancies, and explain the transition as a shift froma ferromagnetic to an antiferromagnetic interactionbetween these two chains. In the present paper, theresults of a neutron-diffraction study of the two mag-netic phases of Cr5S6 vill be presented, and the spinstructures as deduced from this study will be given.

EXPERIMENTAL

The sample of Cr5S6 used in this investigation hasbeen prepared at the University of Groningen by heatinga mixture of chromium powder (99.99/o) and sulfur(99.9999%%u~) in double-sealed, evacuated quartz tubesfor 48 h at 1000 C. After the heating, it was cooledslowly, powdered, and tempered for some days at300'C. The whole sample consisted of about 25 batchesprepared in this way. Each batch was checked forhomogeneity by x-ray diGraction and by measuring themagnetization-versus-temperature curve before it wasadded to the sample. Only small traces of Cr203 werepresent in the specimen.

Neutron-diffraction patterns were obtained at theFatten high Aux reactor at temperatures of 4.2, 78, 208,and 370'K from a sample contained in a cylindricalsample holder with a diameter of 20 mm.

The neutron wavelength employed was 2.57 A, ob-tained from the (111)planes of a copper monochromat-ing crystal. 'The Soller slits which were placed betweenthe reactor and the monochromator had a horizontalangular divergence of 30'. The angular divergence ofthe slits in front of the BF3 counter was 10' for the dia-grams taken at He and N2 temperatures and 30' forthe other diagrams.

As a second-order 6lter, a block of pyrolytic graphitewith a thickness of 7.5 cm was employed, as describedby Loopstra. ' In addition, in order to study the tran-

9 S.0.Loopstra, Nucl. Instr. Methods 44, 181 (1966).

TAsl.z I. Final structural parameters of Cr5S6 at T=370'K.

zLCr in 4(f)gxLS in 12(z)jyfS in 12(i)jzPS in 12(z)g

B isotropic (Cr)B isotropic (S)2 factor

0.993+0.001

0.337+0.0050.998+0.0030.377+0.002

1.2~0.2 A1.5a0.2 i.2

3 5%

sition from the antiferromagnetic state to the ferri-magnetic state, two sections of the diagram werescanned repeatedly while the sample was allowed towarm up slowly from liquid-nitrogen temperature. Theheating rate was about 10 per hour and the temperaturedifference between the lower and the upper part of thesample, which was contained in an aluminum sampleholder with a wall thickness of 2 mm, was about 3 .

Q, w;(Q, I.b,—Q„I„i,) '

by a full-matrix refinement technique. Here, p; is thesum over all peaks which can be separated in thediagram, w, is the weight of one peak, and P„ is thesum over the overlapping reflections in such a peak.

The results are given in Table I. It was found thatthe deviations from the idealized structure are signi6-cant only for the s parameter of the Cr in 4(f).

The observed and calculated intensities are listed inTable II. The anal E factor, defined as

was 3.5/q.The value for the coherent nuclear scattering ampli-

tude of sulfur used in the refinement was 0.28)&10—"cm, as given by Menyuk, Dwight, and %old. ' Use ofthe value of 0.31)&10 "cm, listed in the InternationalTables for X-Ray Crystallography, Vol. III, leads toan abnormally high value for the individual isotropictemperature factor of the sulfur atoms. For the chro-mium scattering amplitude, the value of 0.352)(10—"cm was used.

"N. Menynk, K. Dv~ight, and A. Wold, J. Appl, Phys. $li, 1088(1965).

CRYSTALLOGRAPHIC STRUCTURE IN THEPARAMAGNETIC STATE

The structure of CrsSs given by Jellinek is an ideal-ized one, and an attempt was therefore made to de-termine more accurately the s parameter of the Cratoms in 4(f) and the x, y, and s parameters of thesulfur atoms from the neutron intensities obtained at370'K

The above-mentioned structural parameters weredetermined by means of a least-squares program whichminimizes the quantity

656

TABLE II. Calculated and observed intensities of CrqSs in theparamagnetic state (T=370'K).

0 0 20 1 00 1 10 1. 20 1 31 1 00 0 4

1 21 2

0 2 00 20 1 40 2 20 2 30 1 5

1 41 1 4

2 01211 2 10 2 40 0 6122

2 20 1 6123

2 30 3 00 2 50 30 3 21 2 41 2 41 1 61 1 60 3 30 1 70 2 62 2 0

2 52

0 3 4

26

12121262666

121212121266

12121212

2121.21212126

121212121266

1212126

121212

I.sic

27596

594150441

12833

37201467

611579358

24948

53664803

5093

1162110771433

161188

676043

01713033

5701783

025231

481433018

Q„I„),27596

594150

12833

5248

25058

249

1021750

240

9133

7151171

2416

25231

p. Iob'

263 ( 62)146 ( 61)54s ( 70)

74 ( 66)4O8 ( 61)

1312 ( aS)64 ( 57)

5269 (120)

231 ( 56)0( 60)0( 6Q)

io229 (125}0( 60)

121 ( 63)

0( 60)0( 60)

7131 (125)0( 60)

2429 ( 93)

263 ( 76)0( 60)

599 ( 93)

a Numbers in parentheses are estimated standard deviations.

MA65'ETIC STRUCTURES

A'Otiferromagnetic State

In the diagrams obtained at 4.2 and 78 K, manyextra peaks of magnetic origin were found. ThesecouM not be indexed satisfactorily on the basis of aunit cell which was a simple multiple of the nuclear

cell, considering an up to twenty-fivefold increase ofits vohune. This means that there is no simple relationbetween the periodicities of the magnetic and thenuclear structure.

In general, the spin-vector on the uth atom in the ethunit cell in a periodic spin structure can be written asa Fourier sum":

S„„=P,Q„(z) expi~ R .,

where R„„is the position vector of the atom and g thepropagation vector of the Fourier component. Neutron

"D. H. Lyons, F. A. Kaplan, K. Dwight, and N. Menyuk. ,Phys. Rev. 126, 540 (1962).

TABLE DI. Schematic representation of magnitude and rela-tive phase angle of magnetic moments in the magnetic phasesof CrgS6.

Atom Position x Moment Phase angle

23456789

10

14,123

31

1

2+83

p

Ij,b

Pap$pgPfPojllf

PfpcJtlf

pO

180'po

180'+rt

PO

+400

scattering from such a spin structure occurs in direc-tions associated with reciprocal-lattice vectors e = H —~;the structure factor will be

F(H, ~) =P„Q„(~)expiH r„,

where 8 is a reciprocal-lattice vector associated with thenuclear structure and r„ is the position vector in thenuclear unit cell of the vth atom. Because of this, themagnetic scattering manifests itself in a number ofsatellites around each nuclear reciprocal-lattice point.There can be as many satellites around each point asthe number of nonzero components in the Fourierexpression for the spin structure. In the diagrams ofCr~S6 in the antiferromagnetic state, no magneticscattering has been observed in directions associatedwith nuclear reciprocal-lattice points, which means thatthere is no component in the spin structure with thesame periodicity as the nuclear structure.

All directions in which magnetic scattering occurscorrespond to lattice spacings d, given by

I/ds= (I s+h~+V) ]a') s+(I ] c*~~ (.[)s.

This shows that only two Fourier components are non-zero, one with propagation vector +~ and one with

propagation vector —~, parallel with the c~ axis.The existence of only two Fourier components im-

mediately rules out the possibility of an antiphase-domain-type structure. Kamigaichi's observation4 thatthe spins should be in the basal plane leaves a screw-typespiral structure as the remaining possibility. In such anarrangement, the manner in which the spin componentvaries from one unit cell to the next is given by thepropagation vector c. In each crystallographic unit cell,a phase angle p„can be assigned to each magnetic atom.

The intensities of the satellite rejections in a screw-

type spiral structure are given by

I(H, —~) =JL(q')F'(H —~)exp( —8/2d') for e= H+g

I(H, +~)=jL(q')F'(H +~)exp( —8/2d') for e=H —q

where

F(H, &~)=0.2695 P„f„(H, +~)p„expi(H r„~g„).

In these expressions, f„(e) is the form factor of the

657

TABLE IV.. Final structural anura an'

parameters fan magneticne lc states.

0

S~RUCq UR FS OF

It should belar

be mentioned that in1 tio factors a e

n, rat er

PPrameters. As a result the

e i erent

the diffett dfi d th an the se ar

en

and str

'erent position Is. n Table IV

parate moment fs 0

as ructural param tmeters are l

, the 6nal maa neticd

Ant'nh erromagnet'

T =4.2oK T =77'K

(5.962 +0.003)(11 509+0 011) g (11.506 +0.005) g

A (53.25 &0.32) A

Ferrimagnetic

T =208'Z

(S.974 a0.012) A(11.509 &0.028) g

Spiralperiodicity

z PCr in 4(f)js LS in 12(i)gy LS in 12(i)&z LSin 12(i)$

papbpopf

0.993+0.0010.331&0.0030.998+0.0020.376 +0.001

(2.98 +0.25)ps(2.VV +0.12)pg(2.78 +0.10(2 57~0,)PB

(2.73 +0.04)pg

(129.1 +2.7) '0 A~

0.995 +0.0010.328 +0.0030.998+0.0020.378 &0.001

(2.87 +0.84(2,66&0 5( .56+0.19)pg

o I 6)pg

(2.34 &0.32)pgg

(2.ss +0.06)p~

(131 2~9 2) o

(0.3 +0.1) A&

4 7'Fo8 over-a11R factor

) C3

I

gp, a

~'D E Cox %'

eman for Cr'+.

. Cox, W. J.Takei, and G. Sh', . ys. hCox, W. . ', . lrane, J.Phys. Chys. hem. Solids

an . J. Freeman, Acta Crc a ryst. 14, 27 (1961).

p, b

b

Fxo. 1.vacan

' ntderromagn tth lattice a

elc s inlce are represented be y open squares.

0.992 +0.004

nd calculaisted whil

t t i h0.991+0,007

---F 1

0.379 +0.004

(1.70 +0.34)paFerrimagnetic State

paver age

(1.69 +0.20)p~ n t ediagram og, obtained at 208'Kthb' fhth d'

.-., l

ase, it was deduc d te antiferro-

P'

f'

g'

h

man ' 'ngnetic ion v and

Fn, n p„is its ma nThe

P fo s

um is taken ov

p' struc u e w

uc ure.

ni ce".

spins in the basuc a

e basal plane is

ver all equivalent reflec-„ f„(H)p„K„expiH.~ s v Pz fy

2 —1g =

g 1+cos 7/) i

av a equivalent

n anced by its h'

vector in the d' 'e

, which is st

f thbl h th

hlsho

e same meaninng as before. It

tio b do re ative an

can be

n e educed from owdn e om powder data.

a icaly considering all os' ' ' '

t b de eterminede magnetic

ii

o rin

n addition, one orP e ers should also

~ ~

io rmined.e re6nement of both ma ne

're ot magnetic and str t

carrie out a a'ructura

p g'

by ull-magram. This resulted in

fo th d tI'A band 78 K

p

l L

o ained form

atson and Fre

jIL

C

B. vAN LAA R

Ter.z V. Calculated and observed intensities of Cr5S6 in the antiferromagnetic state. The column s indicateswhether the intensity is nuclear (s=o), or magnetic (s=+1).

00001

11111

1110

1

00111

1222

2121222212

21

1022222222022210222122122

+1—1+0+1+0

+1—1+0+1—1+0+1—1+0—1+0—1+1+1+0+1—1+0+0—1+1+0—1+1—1+0+0+1+1+0+1—1—1+0

+0+1+0+0+1+1—1—1+0—1+1—1+0+0+0+0+1+1—1

+1+0+0+1+0—1—1+1+0+0

2222666

12121212121212122666

1222

1266

1212666

121212121212121212

1212121266

12122

12121212241212122

24

2412

2121224122412121212

616373

722

42400

2781696

1084620231

4291514745971337

473756

1717

22670

23115594517

101

8600

38456197

15368

3188182

2695957

5

5913454

17089158791389

083

13400

2728839017845

11003

23442118

398

1682052ii2770

1302551677

426278

16961084620231

4291514745971337

47

315 (130)190 (120)

1659 (120)10530 (160)20791 (250)

359 (100)14783 (170)4972 (135)1384 (110)

40 (100)

3790226

7

23

1607610

186

038

3196182

2695957

5834

5913454

3833 (120)327 ( 90)

0( 70)0( 70)

45 ( 80)

15999 (170)0( 70)0( 70)

45 ( /0)

0( 70)30 ( 70)

510 ( 90)ruSS ( 95)

3140 (115)107 ( 85)

2634 (110)1001 (100)

0( 70)800 (110)30 ( 60)

380 (100)30 ( 60)

1500 (200)138 ( 80)

0 ( 70)

100 ( 70)20 ( 70)

2000 1936 (120)

4447 {160)0( 60)

300 (100)1836 (130)

70 ( 50}

7=4.2'K

6163 6165 (400)73 250 (150)

722 614 (135)

Ioa,1o

435

27300

107862

43949140

20871501955574

191820

1275

1

54322235

21900

14240

65613

140590

1214382

34422

10116

85527150495

0520

153189131

7398

0876766

1414776959

2491

471

T= 77'Kg, I„),

275107862

43949140

20871501955574

19

140790

1214

15702495

0

250

Er Job:

0( 60)490 ( 68)

136 ( 60)0( 60)

774 ( 66)4465 (100)9119 (410)

189 ( 52)7164 (112)1916 ( 68)593 ( 59)

0( 60)

1768 { /0)95 ( 70)0( 60)0( 60)0( 60)

0 ( 60)0( 60)

182 47)574 47)

1395 ( 64)0( 60)

1133 ( 60)

493 ( 61)

388 ( 57)

139 ( 44)

16131 (470)484 ( 60)

0( 60)0( 60)0( 60)

0 ( 60)

785 ( 80)

1893 ( 90)931 ( 75)

0{60}

156 STRUCTURES OF Cr5S6 659

TAsx.E V. (coltcliied).

0 3 00 3 00 3 00 2 5

2 30 30 2 50 3 2

1 60 3 21 2 40 3 2

2 41 2 41 1 61 1 60 1 71 2 40 2 61 1 60 3 30 1 70 2 60 1 7

2 50 2 60 3 42 2 02 2 02 2 0

2 51 2 50 0 80 3 41 2 50 3 42 2 22222 2 20 0 82 2 21 3 01 3 01 3 01 3 11 3 10 1 8

+0

+1+0+1+0+1—1—1+0—1+1+0+0+0+0—1+1—1+1+0+0+0+1+1—1+1—1+1+0+0—1+0+1+1—1+0+0+0+1+0—1+1+1+0—1

Jl

666

122412121212122412121266

1224121212121212241212666

1212

212241212662

12121212122

12

I~lo

2370122

139460

5813

22554

20

135133

22776424355

31031

100

96110339

2729

141672

11

15293

720

T=4.2'KQ„I ),

23845460

5813

57520

93253

1031

97110339

2

26627

20

Zr Iobs'

23755 (200)40 ( 60)o( 7o)

7Oo (13O)20 ( 60)

600 (130)o( 7o)0 ( 70)

9412 (140)o( 7o)

1206 (150)

847 (12s)ioo ( 6o)30 ( 60)o( 7o)

2480 (2oo)o( 7o)

63 ( 85)

lcale

1102911

92100

15902

31600

7766

9023182

1020

26920

34947

1178

3773

00

9570

114

13000

119529173634

0134

001

320

T= 77'KQ„I„l,

111340

15902

31600

10888 (130)0( 60)

125 40)0 60)o( 6o)0( 60)0( 60)0( 60)

43280

4154 (110)0( 60)

62047

71

1783

442 ( 7s)o ( 60)0( 60)0( 60)

40 ( 60)50 ( 60)

94014

1300

8oo (iio)o( 6o)0( 60)0( 60)

0( 60)

7880 8073 (150)

' Numbers in parentheses are estimated standard deviations.

The model in Table III gives the best fit to the intensi-ties also in this case. While in the antiferromagneticstate, the quantity P has a value different from 180',the data for the ferrimagnetic phase 6tted perfectly amodel in which this phase angle was 6xed at 180'.

Figure 2 shows the ferrimagnetic spin structure. Aleast-squares refinement of structural and magneticparameters resulted in an R factor of 3.9/o. The ob-tained form factor in this refinement was very close tothe Cr'+ form factor of Watson and Freeman. "Thiswould suggest that the moments are somewhat lessspread out than in the antiferromagnetic state, but it isvery doubtful whether such a quantitative interpre-tation is justihed.

In Table IU, the 6nal parameters are shown, and thecalculated and observed intensities are given in TableVI. Here again, rather large correlation factors were

computed between the magnetic parameters, particu-larly between p, ~ and pj, where this factor was close to—1. As a result, the sum of these moments is welldefined [(3.13+0.38)yiij, while the separate momentshave large standard deviations. Also, the net momentper unit cell is very ill defined [(0.2+10.7)ic~f. Thevalue found by means of magnetization measurementsin a field of 8530 Oe, carried out at the University ofGroningen, ' is 0.98 p~.

TRANSITION FROM THE ANTIFERROMAGNETICSTATE TO THE FERMMAGNETIC STATE

Apart from the magnitude of the moments, there areonly two differences between the spin structures of thetwo magnetic phases. Firstly, in the antiferromagnetic

'4 C. F. van Bruggen (to be published).

Too . IR ion

156

. o obtain the variationIR ion ersus ten1peraturc. en was e satellites

expenment, the tern

sate, arate intensitiesn ese

a t es were obtained.e o owing quantities wc l lculated.

660

TABLE pl . Calculated and observed'

o served intensitiesr o

l~& p) ill

8 ~ &AN

g etic state (E=20

h k J Ie calo I@a calc

0 0 2 2 307

c ts calc Itot calc

130 45 17455 587 1242

403 163 567

1 1 2 6 1506 0 15060 3599

33 7 4096 188

0 2 2 12 5757 1132 1189

0 1 5 12 2222 131 1534562 0 4562

0 5578 102931 5 50

163 34 19739 34 7248 6 54

2 2 32612212 ' '2

12 39 403 44112 39 883

0 3 0 6 69616961 0 6962

0 30311200 0 7517

1 2 3936 2 39

I 1 6 6 569 069 0 569 26040 0 0 0

026 12 8 2' "' "922O 6 478 0 478

5 18 230341280 8 602

Z. Itot "1. tot obs

239 ( 55)174 222 ( 55)

1248 ( 7o)6043 6056 (100)

567 611 ( 50)123O 1237 ( 65)

42 ( 5O)

5105 4970 (100)0 ( 60)

I'C Ca

(~&»r &/0 2695&&f)'== (~.—2~i »n4)',

(F&Ou+)/0 2695.X

198 ( 55

f) glp+2pr slug)

1255 ( 65)) I'om th.c int cnsltlcs below thc tI'

43o ( 6o)

w c tI'RQsltlon point, Rnd2791189

(Fou/0. 2695Xf)2= p,—PC

10474 (125) from the inten" '

83 ( 4O tin ensities above the tr

t esc quantities aree transition point, . In

is gure, it can bI sus tcInpcI'Rtuic. Fl

graduall t e to the

733 ( 70)As both quantitiesuantities, ~posing~ and . a

s o say that the beha'

p . This will be discussed

For the lnterpretatio

ough it is therefore i

one magnetic state to the other is of r i imental re y avor such a

a N Q1T1N'iimbers in parentheses are een eses are estimated stand d d' ' s.ar eviations.

phase a helical orderin, r eI'in alue of the spiralha r erlng with a unite valc ln the fcl I

periodicity ls I 6 0' g b'»ls zero in the ferrimagnetic stat -h'

ln t~c Rntifcrromastudy experiment ll

e transition point.e ers ln the vicinity of

The variation of the m'

hVCCtOI C

o e magnitude of thr c as a function of tern ep

inuously the (012u ic by

peaks while warmrming up slowlsR e ltc

between these tw

and (012+) sat 11'

wo peaks provides ay. Thc angular dl tis ance

c . The temperatuure resolution er1 CS R 11CCt 1Tleasure f1C Oi

per run was about 3 .e separation of these p kpea s at

In Fig. 4, the resultincs ting curve of versus tempera-gures ows that ~ d

y to zero when thCCI'CRSCS Con-

transition point.pcrature approaches

C

Qp, a

FIG. 2. Ferrimagnetic s inspin arrangement ln i gSG.

STRUCTU RES OF Cr5S6 661

1000l

109o K 159o K

E500

th

o0'I—

UJx0

M

Ul

I/

~ ~ ~ ~~ ~ Q

I I

~ Not ~ t tl ~I~ 1~

I I I

I

~o~ Oyo ~ gt4 ~

~01~

I I I I

166o K

r~ lyO~ Ops

I I I I'

I

~' 1700 K

1000—

500

/|l/ .

r'l

sV ~ ~

~ yyyyO ~1~ ~ ~ 00 ~ ~ 00000

I I I I I I

38 40 4236

I~ 001yy ~OOgs

I I I

36 38

I~ ~

~ ~'i ~ Itelo 01~

40- 42

COUNTER ANGLE (2e )

Fro. 3. Typical examples of the angular separation of the (012 )and (Oj.2+) peaks at four different temperatures in Cr~S6.

DISCUSSION

If the assumption that Cr5S6 is purely ionic is valid,it can be expected that there are six Cr'+ ions and fourCr'+ ions in the crystallographic unit cell, with spin-only values for the magnetic moments of 4' and 3',respectively, which results in an average moment of 3.6p~ per Cr ion. In the present work, the observed averagemoment at 4.2'K is (2.73&0.04)p~, and no moment ashigh as 4@~ has been found. This probably means that

the purely ionic model is not correct, and that metallicCr-Cr bonds are present, as pointed out by Jellinek. '

This is supported by the fact that metallic conductionhas been observed by Kamigaichi' in specimens ofCrS with 1.13&x&1.20.

To illustrate the behavior of the two quan. titiesr ~r

andr pf sing

rwhen the temperature is varied, and in

order to of'fer a possible explanation for the existence oftwo magnetic phases, we will consider the Heisenbergenergy of the system. . The interactions which will betaken into account can be divided into three groups:(a,) interactions between nearest neighbors in (00l)planes; (b) interactions between nearest neighbors alongthe L00l] direction; (c) interactions between momentsat distances (+-sr, &s, -„') Lapart from the small devia-tion from zero of the z-parameter of Cr in 4(f)]. Theanion-anion-cation angles for these three types of inter-actions in the idealized structure are, respectively,89', 72, and 132 . In the actual structure, these anglesdeviate slightly from these values.ls As it is dificult to say which one of these interactionsis of predominant importance, we will take them allinto consideration. The Heisenberg energies resultingfrom these three groups of interactions are

L~', = —2Csy cosp —Crf cos2&+C«,

Eg=+2C~ cossn —2Ccf cos(n+Q) )

L~', = —2Cs, c osn+2 Cy cos(n+P)+2C,r' cos(n —Q) —2C,f cos(n —P) .

The energy for the whole system is

&a.a.i= ~.+~b+~'In these formulas, C;;=J,;p;p;, where J;;is the exchangeintegral for the interaction between the moments p,; andp; at the crystallographic positions i and j.

0.2 5

Fn. 4. Variation of the wavevector r with temperature inCr~S6. The left-hand ordinate ivesthe wave vector in units of c~r,the right-hand ordinate the spiralperiodicity in units of rcr. Theopen and 6lled circles representtwo different warming runs.

0.20

0.1 5

0.10

0.05

0 --i75 100

I

125 150 175

TEMPERATURE ( DEGREES K)

O—5

D—6

i——7 (J

oC3

—9—10

-15—20

V)

—30-50

200

B. vAN LAAR 156

40

ijt sin ('f 1

e 30m

"lA

CV

~ 20X

LAChCDP4

CD

h. EO

P4

Fxo. S. Variation of F' ofthe (011-) and (011+) re-Qections helot the tran-sition point and of the(011) re6ection above thispoint. The 611ed circle indi-cates the value of p,2 asobtained from the diagramat T=78'K.

I

100

~011: ( )jc- 2 yt s in ('f )

0 O O

1 I I

f50 175 200

TEMPERATURE ( OEGREES K )

C,r stands for interactions over a dists, nce (st, ~„—' —s),C,r' for interactions over (—'„—rs, rs+s), C.f for inter-actions over (s, ~» sr+s), and C,f' for interactions over

(0, 0, sr —s). a, the turn angle of the spiral between. twoadjacent Cr layers, isde6ned asn=(~~~/(c*~)X2s-, and

P has the same meaning as in Table III.We will assume the interactions of group (c) to be

positive and the interactions of the two other groups tobe negative. It can be shorn that, if the absolute valuesof the quantities C,f and Cf~ are not too large, the energyis minimized for n=0' and &=180o, as is the case forthe ferrimagnetic structure. When, for some reason, theabove-mentioned quantities become relatively more im-

portant, the minilnum energy is no longer obtained forn=0 and &=180', and P will deviate from 180'. Theturn angle 0. is then given by

(C f—C,y'+C.r—C,r')singkgo,'=—

(C.r+C.x C r —C r')cos4' —Cs.+C.s

From this, it is seen that a goes to zero when~ pr sing~

approaches zero. This 6ts the observed behavior with

varying temperature of these t%o quantities.The fact that ~yr sing~ is zero. above the transition

point means that &=180' in the ferrirnagnetic state.Although, in this state, the observed moment p~ does

not differ signi6cantly from zero, the observed valuefor the sum of the moments pr and ps of (3.13+0.38)psis too large to be attributed. to pg only.

ACKNDWLEDGME5TS

The author wishes to thank Professor F. Jellinekfor the suggestion of the problem and for his interestin the work, Dr. C. F. van Bruggen for providing themagnetization data and for the elaborate checking ofthe sample, and A. Bruiniag for the preparation of thespecimen. The valuable assistance of J. F. Strang with

the experiment. al work is gratefully acknowledged,