Magnetism research with polarized neutrons at the Centro di Studi Nucleari della Casaccia del C. N. E. N., Roma, Italy

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1 Magnetism research with polarized neutrons at the Centro di Studi Nucleari della Casaccia del C. N. E. N., Roma, Italy B. Antonini, G.P. Felcher, F. Menzinger, A. Paoletti, F.P. Ricci, L. Passari To cite this version: B. Antonini, G.P. Felcher, F. Menzinger, A. Paoletti, F.P. Ricci, et al.. Magnetism research with polarized neutrons at the Centro di Studi Nucleari della Casaccia del C. N. E. N., Roma, Italy. Journal de Physique, 1964, 25 (5), pp < /jphys: >. <jpa > HAL Id: jpa https://hal.archivesouvertes.fr/jpa Submitted on 1 Jan 1964 HAL is a multidisciplinary open access archive for the deposit and dissemination of scientific research documents, whether they are published or not. The documents may come from teaching and research institutions in France or abroad, or from public or private research centers. L archive ouverte pluridisciplinaire HAL, est destinée au dépôt et à la diffusion de documents scientifiques de niveau recherche, publiés ou non, émanant des établissements d enseignement et de recherche français ou étrangers, des laboratoires publics ou privés.

2 Our C. LE JOURNAL DE PHYSIQUE TOME 25, MAI 1964, 604. MAGNETISM RESEARCH WITH POLARIZED NEUTRONS AT THE CENTRO DI STUDI NUCLEARI DELLA CASACCIA DEL C. N. E. N., ROMA, ITALY. By B. ANTONINI, G. P. FELCHER, F. MENZINGER, A. PAOLETTI, N. E. N., Laboratorio di Fisica Nucleare Applicata del Centro di Studi Nucleari della Casaccia, Roma, Italy. F. P. RICCI, Istituto di Fisica dell Universita di Roma, Italy. L. PASSARI, Istituto di Fisica dell Universita di Ferrara, Italy. Résumé Le laboratoire des applications de la Physique Nucléaire du C. N. E. N. utilise, depuis octobre 1961, un réacteur RC 1 (Triga Mark II). Nous avons dû envisager des expériences qui ne seraient pas trop handicapées par le faible flux de neutrons. Aussi nous avons décidé d utiliser la technique des neutrons polarisés pour l étude des substances ferromagnétiques. Nous avons deux spectromètres à neutrons polarisés du type R. F. Dans cet article, nous résumons les travaux d intérêt magnétique réalisés à Casaccia Abstract. group at the " Laboratorio di Fisica Nucleare Applicata " of C. N. E. N. since October 1961 has had in use the RC 1 Reactor (TRIGA Mark II). We had then to face the problem of performing some meaningful experiments which were not too severely handicapped by a low neutron flux. Consequently we decided to use polarized neutrons techniques for investigating ferromagnetic materials. At present two R. F. type polarized neutron spectrometers are in operation. In this review we summarize some work carried out at Casaccia in the field of magnetism. Study of the orderdependent magnetic properties of MnNi3 by means of polarized neutrons. The saturation magnetization of MnNig strongly increases with the order parameter and its temperature dependence appreciably deviates from a Brillouin curve. Such a behaviour is most noticeable for intermediate degrees of order, and several authors have suggested various explanations on the basis of different magnetic structures of the alloy [1]. However, none of these studies was really complete in the sense of measuring both the magnetization and the order parameter. This fact could account for the poor agreement among the results of the different investigations. The magnetic moments of the different sites of the structure were determined only in the case of sets of nearly complete order and two possible magnetic moments for manganese and nickel were given [2]. The polarizedneutron technique provides a powerful investigation tool in the study of such ordered ferromagnetic alloy, since it permits unequivocal location of the magnetic moments at the different sites of the ordered structure. Furthermore, magnetic form factors can be measured with high precision. We have performed both bulk magnetization and polarizedneutron measur ements within the orderparameter range The order parameters were measured by means of neutron diffraction. The neutron measurements have been carried out at the polarized neutron spectrometer of " Centro di Studi Nucleari della Casaccia " by determining for each Bragg reflection the polarization ratio, i. e. the ratio of the intensities for neutrons polarized parallel and antiparallel to the magnetization of the analysing crystal. The polarization ratio, provides for the reflections investigated the ratio y of the magnetic to the nuclear structure factor [3]. Bulk magnetization measurements were performed with the ballistic method. The experiments have been carried out on a single crystal which at the chemical analysis showed the composition As it is well known, polarization ratio measurements on single crystal can be heavily affected by extinction. Such an effect can be reduced by increasing the mosaic spread of the single crystal and reducing its thickness. We have used a specimen 0.9 mm thick with a mosaic spread parameter YJ 20 min = arc (determined from the rocking curve). According to the Willis treatment [4], the fundamental reflections should be affected by extinction for about 3 % for Article published online by EDP Sciences and available at

3 605 the (111) reflections and less for the other reflections. The superlattice reflections are practically extinction free. of these calcu The validity lations has been checked experimentally by comparing polarization ratio values measured in reflection and transmission. Our sample was equilibrated at the given degrees of order by annealing it at the proper temperature. At the end of each annealing time it was water quenched and the neutron analysis performed along with the bulk magnetization measurement. Then it was reheated to the next lower temperature and the procedure repeated. The temperature steps and the annealing times TABLE I are given in Table I with the measured order parameter. We must point out that we were not interested here in kinetics since our main aim has been the achievement of a homogeneous state of order, consequently we did not care for a very precise determination of the annealing temperatures. However great attention was paid to the control of the homogeneity of the state o~ order through the sample by comparing carefully the half maximum widths of the fundamental and superlattice peaks. On this basis we have checked the total sample homogeneity at every temperature step. The order parameter S was calculated from the ratio of the observed integrated intensities of a superlatti~e reflection to a fundamental one [f. e. (100) and (200)]. The second order wavelength contamination has been measured to be less than 0.5 %. The polarization ratios, corrected for the flipping efficiency and the incomplete neutron polarization, have given for Yhkl the values reported in Table I I. Here the yhkl values for the steps 1, 2, 3, 4 are omitted since the ywci are given by the bulk magnetization for the fundamental reflections and are practically unmeasurable because of the absence of order. Besides room temperature some measurements were also done at other temperatures for reasons which will be made clear in the discussion. Typical results of bulk magnetization measurements for some states of order, are reported in figure 1 as a function of temperature. These measurements were performed at a Oe field which is at least ten times larger than the value at which complete saturation was attained. TABLE II

4 Results Division 606 FIG. 1: of bulk magnetization measurements for some states of order versus temperature. Discussions. From the high and low temperature measurements we see that the y values for the fundamental reflections follow the bulk magnetizationtemperature curve. For superlattice reflections however the y values do not change by going to low temperature while an appreciable decrease is obtained at T = 460 OK. These apparently puzzling facts could be explained if one assumes that the magnetizationtemperature curves for the partially ordered states can be FIG. 2. of the magnetization vs temperature plot in two parts. divided in two parts (fig. 2). This has been suggested first by Marcinkowski and Brown [1] who attributed the portion of the curve with a lower Curie temperature to short range ordered regions and the other portion to long range ordered regions. This of course would imply the coexistence of of order. This regions with different degree assumption is not unusual since there is mounting evidence that many ordering reactions are heterogeneous and similar to the conventional phase transitions [5]. Our measurements would supply a further support to such hypothesis. Namely only the long range ordered regions do reasonably contribute to the superlattice reflections, while both long and short range ordered regions do contribute to the fundamental reflections. Therefore the y values of the superlattice reflections should be determined by the portion of the magnetization curve, relative to the higher Curie temperature and the y values of the fundamental reflections should be determined The tempe by the overall magnetization curve. rature dependence of y for both the fundamental and superlattice reflections are in perfect agreement with such an interpretation. However to the long range ordered regions must not be attributed an order parameter S 1 = as supposed by Hahn and Kneller [1]. Such hypothesis would lead to sharp inconsistencies which were already discussed by us [6]. Another problem is the size of the ordered regions. As stated before we have carefully checked by neutron analysis that the thermal equilibrium was attained for each step. With the resolution of our set up we can only say that these ordered regions are definitely greater than 200 A. As far as the magnetic form factor is concerned, useful informations can be deduced mainly from the superlattice reflections, since their magnetic structure factor depends on the difference pmn pni. Now the magnetic scattering amplitude of nickel can be reasonably neglected in first approximation whith respect to the manganese magnetic scattering amplitude [2]. Consequently the ratio of two y values relative to superlattice reflections should be very close to the ratio of the corresponding form factor values for manganese. From the reported experimental results it is easy to verify the excellent agreement with the form factor measured for Mn + + by Corliss et al. [7]. Regarding the calculation of the magnetic moments we notice that from the above y measurements we can calculate the magnetic moments at room temperature for Mn and Ni only if we make some assumptions about the possible dependence of the magnetic moments on the position in the unit cell of Mn and Ni atoms. If we first assume that each atom would

5 Bulk The 607 keep its own magnetic moment independently of the type of nearest neighbours one sees that from the measured y values the ~Ni would turn out to be negative and order dependent, in sharp contrast with the same initial hypothesis. Now two other alternative assumptions are possible : cc) the magnetic moments on Mn and Ni do change their value according to their surroundings ; b) the magnitude of the magnetic moments stay constant and antif erromagnetic couplings are present at intermediate states of order. We think that the first hypothesis can be ruled out on the basis of the experimental results. Namely we notice that for the states of order where the magnetization from the long range ordered regions is very close to the 0 OK value, the y of the superlattice reflections stay constant and equal to the value obtained by Shull and Wilkinson for S = That means that the difference 03BCNi stays constant and it seems then correct that also and P.Ni stay constant individually, i. e. are independent of order. In the limits of validity of this last assumption the magnetic moments of Mn and Ni turn out to be in agreement with the first set of data given by Shull and Wilkinson : On the other side the dependence of the bulk on the order should be then esti a statistical calculation which magnetization mated by using would account for the antiferromagnetic couplings. The statistical weights are given by the exchange interactions between all the possible pairs. 2. Study of the Fe3Si alloy. magnetization measurements of the FeSi system as a function of the concentration have shown [8] [9] [10] [11] that while at low concentrations, aluminum and silicon, act in the alloy as simple diluents, by increasing their content, the average moment per iron atom decreases. It seems then that the presence of non magnetic atoms affects the electronic distribution of iron in such a way that also its spin density varies. In the ordered phase Fe3Si, detailed information about the magnetic moments on the different sites of the unit cell, can be obtained by means of polarized neutrons. The ordered alloy studied first by means of diffraction of polarized neutrons has been Fe3Al [12] [13]. The ordered structure is shown in figure 3 and indicates that there are two types of iron atoms, ~ FIG. 3. structure of Fe3Si and Fe3AI. those occupying the corners, or A sites in the figure, having as nearest neighbours four iron atoms and four aluminum atoms (FeII), and those occupying the body center, or D sites, having as nearest neighbours iron atoms only (Fei). The B sites are totally occupied by aluminum atoms. The magnetic moments, determined with polarized neutrons in Fe3AI were, flfel 2.29 ± 10 = = ± 10 the aluminum moment was found to be zero. The different values of the Fei and Fell moments were correlated to the different atomic population in the immediate surroundings : while Fe, with only iron atoms as nearest neighbours, has the same magnetic moment of metallic iron, Fei, with four iron and four aluminum as nearest neighbours, has a moment definitely lower. TABLE III

6 Magnetic The 608 A good check of these results could be possibly obtained with the study of the Fe3Si system which is in many respects similar to the Fe3Al, but from the other side shows some difterences probably due to the replacement of aluminum by silicon. The experimental results are given in Table III. The polarized neutron investigation accomplished on fundamental and superlattice reflections along with bulk magnetization measurements performed with the ballistic method gave for the magnetic moments in the Fe3Si unit cell the following values : The experimental results indicate an appreciable difference between the moments on the different sites of the unit cell of Fe,Si, compared to the values measured by Nathans et al. [12] [13] on Fe,Al. We notice first that within the experimental errors the magnetic moment on Fei is the same in the two alloys and of the same order of magnitude as in pure iron. This can be expected on the basis of the consideration that for Fei the nearest neighbours are all iron atoms, like in the pure metal. On the contrary the moments on Fen turn out to be different in Fe,Al and Fe,Si, outside the experimental errors 1.50 ~ 0.10 and 1.20 ~ This is in agreement with the bulk magnetization measurement on the FeAl and FeSi system as a function of the concentration of the non magnetic component (fag. 4). L FIG. 4. moment per iron atom in FeAl and FeSi system. We recall that Feii atoms have 4 silicon and 4 iron as nearest neighbours. The low value for the Feii moment in Fe,Si can then be related to the larger number of outer electrons (s and p) in Si than in Al. According to Goodenough [14], in Fe,Al and Fe,S1, both the s and p electrons of Al and Si are active in bonding, producing a shift of the band of iron (which is the sp bonding band of iron). This shift is much larger in Fei, with Al or Si atoms nearest neighbours than in FeT with Fe and Al atoms as nextnearest neighbours and would be responsible for the reduction of the magnetic moment on Feii. It seems then reasonable on this ground to suppose that the shift of the tzu band produced by Si with an outer electrons configuration 3s2 3p 2 is larger than for Al with a 3s2 3p configuration. It is also interesting to compare our experimental results with the measurements of the magnetic field at the nuclei of Fei and Fen with the M6ssbauer technique. Fe3Si has been investigated by several authors [15] [16] [17] and two diff erent values of He on Fei and Feii have been found. Particularly interesting are the results of Johnson et al. [17], who have investigated also Fe3AI. The He values in Fe3Si are 318 koe and 199 koe for Fei and Feii, while it is found 295 koe and 212 koe respectively for Fe3AI. We can then see that in Fe3S the ratio He(Fei) /He(FeiI) is definitely larger than in Fe3AI supporting therefore our results. Finally we want to point out that as far as the unpaired spin density is concerned, we can just say, compairing the y values of (115) and (333) reflections, that it is not spherically symmetric. A spin density map of Fe3Si would be extremely helpful providing useful information on the relative occupation of the eg and t2g subbands and would permit to put on a more firm basis the interpretation of the magnetic moment values which have been found. 3. Measurements of the high temperature coherent magnetic scattering of thermal neutrons by f. c. c. cobalt. purpose of our investigation was to determine whether the variation with temperature of the ratio y of the magnetic scattering amplitude to the nuclear one was exactly following the temperature dependence of the magnetization intensity. One can expect a difference in the change with temperature of y in respect to the magnetization if the magnetic form factor does change with the temperature and/or if the mean square amplitude of vibrations of the unpaired electrons is different from that of the nuclei giving rise to different and the DebyeWaller factors for the magnetic nuclear amplitude of scattering.

7 609 As it has been already reported [18], in the first part of our investigation we studied six reflections of an alloy of cobalt with 9 % of iron (which stabilizes the cobalt f. c. c. phase at room temperature). The reflections studied were those for which more precise measurements could be performed with the polarized neutron technique, i. e. those with a y value between 0.7 and 0.1 [19]. The ratio of the y values at high temperature (600 C) and room temperature were found to be measurably different from the ratio of the magnetizations at the same temperatures ; furthermore it was found that the ratio of the y values increased regularly with the increase of Bragg angle of the reflections. The results could be interpreted either as evidence of a variation of the form factor with temperature, or under the hypothesis that only the DebyeWaller factors were different, assuming that the unpaired electrons vibrated with only 1/3 of the mean square amplitude of thermal vibrations of the nuclei. Also a contribution of both effects could not be ruled out. With the purpose of distinguishing between the two possible interpretations of the previous results of the high temperature coherent magnetic scattering by f. c. c. cobalt, other reflections namely (440), (333), (511), (442) and (600) have been investigated. If the difference between the high temperature and the room temperature value of the ratio y of the magnetic to the nuclear amplitude of scattering was due only to the difference between the magnetic and the nuclear DebyeWaller factors, one would expect a regular increase of this diff e rence with the Bragg angle. What has been observed for the new reflections studied is that the deviation of the high temperature values from the room temperature ones, does not follow the regular behaviour to be expected assuming a difference between the mean square amplitude of thermal vibrations of the unpaired electrons and the nuclei. Therefore it seems that a reasonable interpretation of the results can be given by assuming a variation of the magnetic form factor with temperature. According to the first six reflections one should say that the form factor is more expanded at high temperature than at room temperature, i. e. that the radial charge density of the unpaired electrons is more contracted at high temperature. The further reflections now examined suggest that there should also be a redistribution of the electrons in the orbitals T2g and.~$ which result from the splitting, caused by the cubic crystalline field, of the fivefold degenerate 3d level of the free atom. It has been observed, in fact, that the difference in y values of the couple of reflections (511) and (333), which have the same sin 0 / x value, is reduced at high temperature., REFERENCES [1] KOUVEL and GRAHAM, J. Phys. Chem. Solids, 1959, 11, 220. HAHN and KNELLER, Z. Metall., 1958, 49, 426. VOLKENSTEIN and TURCHINFKAYA, J. E. T. P., 1960, 11, 195. MARCINKOWSKI and BROWN, J. Appl. Physics, 1961, 32, 375. [2] SHULL and (C. G.) WILKINSON, (M. K.) Phys. Rev., 1955, , [3] NATHANS (R.), PIGOTT (M. T.) and SHULL (C. G.), J. Phys. Chem. Solids, 1958, 6, 38. [4] WILLIS (B. T. M.), Pile Neutron Research in Physics, 1962, p [5] SMOLUCHOWSKI (R.), J. Physique Rad., 1951, 12, 389. [6] PAOLETTI (A.) and RICCI (F. P.), J. Appl. Physics, 1963, 34, [7] CORLISS (L. M.), ELLIOT (N.) and HASTINGS (J. M.), Phys. Rev., 1956, 104, 924. [8] FALLOT (M.), Ann. Physique, 1936, 6, 305. [9] SUCKSMITH (W.), Proc. Royal Soc., 1939, 171 A, 525. [10] SATO (H.) and ARROT (A.), Phys. Rev., 1959, 114, [11] PARSONS (D.), SUCKSMITH (W.) and THOMPSON (J. E.), Phil. Mag., 1958, 34, [12] NATHANS (R.), SHULL (C. G.), SHIRANE (G.) and ANDRESEN (A.), J. Phys. Chem. Solids, 1959, 10, 138. [13] PICKART (S. J.) and NATHANS (R.), Phys. Rev., 1961, 123, [14] GOODENOUGH (J. B.), Phys. Rev., 1960, 120, 67. [15] NAKAMURA (Y.), Private communication. [16] STEARNS (M. B.), Phys. Rev., 1963, 129, [17] JOHNSON (C. E.), RIDOUT (M. S.) and CRANSHAW (T. E.), Private communication. [18] MENZINGER (F.) and PAOLETTI (A.), Phys. Rev. Letters, 1963, vol. 10, 7, 290. [19] PAOLETTI (A.) and RICCI (F. P.), To be published in Nucl. Instr. and Methods.

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