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Chapter 4 Results and discussion for films

4.3 Magnetostrictions data

4.3.1 Young’s modulus (E f

Fig. 4.7 shows that for the Fe81-yNiyGa19/glass films, as y increases, Ef is almost constant, 120 GPa, except when y = 17, the Ef is up to 133 GPa, and for the Fe81-xNixGa19/Si(100) films, as x increases from 0 to 17, Ef first increases from 170 to 182 GPa, then decreases from 182 to 154 GPa, and finally when x > 17, Ef increases again. Different film-growth mechanisms, due to uses of different substrates, cause the former being less denser than the latter.

Thus, even under the same film composition condition (i.e., x = y), Ef of the x-film is stiffer than that of the y-film.

Fig. 4.7 This is Young′s modulus of the two series of Fe81-xNixGa19/Si(100) and Fe81-yNiyGa19/glass films, respectively.

78

According to Ref. 22, the D019 phase and L12 phase are detrimental to saturation magnetostriction. In this study, we found the addition of Ni into Fe81Ga19 alloy films oppresses the formation of D019 and L12 phases. Even when y = 22 at.%Ni, there is only one single A2 phase. So we get magnetostriction constants in the FeNiGa ternary alloys higher than those of the Fe81Ga19

The t

binary alloys. In addition, notice that the saturation field of these films is very low, about 15 Oe. Hence, their magnetostriction sensitivity can be quite high, about 1.9 – 2.7 ppm/Oe, which is suitable for the low field and high frequency application.

f dependence of λS of Fe59Ni22Ga19/Si(100) and Fe59Ni22Ga19/glass films is shown in Fig. 4.9. The trend for Fe59Ni22Ga19/Si(100) films is that as tf increases from 65 to 195 nm, λS increases from 25 to 30 ppm and, and as 195

< tf ≤ 260 nm, λS remains constant. The trend for Fe59Ni22Ga19/glass films is similar. These results can be explained by the surface oxidation and/or the film/substrate interface effects [42].

79

0 5 10 15 20 25 30 5

10 15 20 25 30

35 Fe

81-x Ni x Ga 19 /Si(100) Fe 81-y Ni y Ga 19 /Glass

x, y (at. %Ni) λ s ( ppm )

Fig. 4.8 Saturation magnetostriction (λS) reaches maximum, when x or y = 22 at.%Ni.

Fig. 4.9 The tf dependence of λS of the Fe59Ni22Ga19/Si(100) and Fe59Ni22Ga19/glass films.

80

5. Results and discussion for ribbons

5.1 XRD data

According to the x-ray diffraction patterns (Table 5.1) of the melt-spun Fe81-zNizGa19 and the JCPD information[43], we can identify the A2(110), A2(200), and A2(211) diffraction peaks. From these findings, lattice constant (a0) of melt-spun Fe81-zNizGa19 can be calculated respectively[44]. For

example, Fig. 5.1 shows the information of θ angle and the corresponded lattice of the melt-spun Fe81Ga19 x-ray diffraction pattern peaks of A2(110), A2(200), and A2(211). From these three points, the value of a0 can be found by plotting ahkl (lattice) against (cos2θ/sinθ+cos2θ/θ), which approaches zero as θ

approaches 90o; a fitting line runs through three points and crosses the a-axis[45].

That can make sure the lattice constant of the melt-spun Fe81Ga19 ribbon.

Each melt-spun Fe81-zNizGa19 ribbon samples are shown in Fig. 5.2. The lattice constant first increases from 2.925 Å to 2.931 Å, then decreases to 2.900 Å finally thenstabilizes around 2.900 Å, as z of the FeNiGa ribbons increases.

The radii of atomic Fe, Ni are about 1.23Å, 1.23Å, and the radii of ion Fe2+, Ni2+

are about 0.74Å, 0.69Å,respectively[46]. Thus, the lattice constants of these ribbons showed dependence on z. Furtherance exhibited the similar trends in z-dependence, as the lattice constant and electrical resistivity, shown in section 5.3. However, for z=24 at.% Ni, the diffraction peaks are not all identified, indicating these might exist some other phases at in these ribbon. We will come back on this in chapter 7.

81

Table 5.1 Structural properties, the x-ray diffraction peaks, of the Fe81-zNizGa19 ribbons. I/Imax is the peak intensity ratio. a0

z

82

Fig. 5.1 The lattices constant of melt-spun Fe81Ga19 be calculated by the red line cross y-axis. The lattice constant of this ribbon is 2.925 Å.

Fig. 5.2. The lattice constant first decreases from 2.925 Å to 2.900 Å and then stabilizes around 2.900 Å for the FeNiGa ribbons.

83

5.2 VSM results

In general, addition Ni replace Fe at.% in alloys to be caused refined magnetic in rich-Fe alloys. Especially in the magnetic anisotropy energy and saturation magnetization, there would be shown later. The VSM results of the Fe81Ga19

ribbon are shown in Fig. 5.3. When θ=0o, the in-plane external field HE is parallel (//) to EA, and when θ=90o, HE is perpendicular (┴) to EA. We can obtain MS, SQR, HC, and Hs from these two plots. In addition, upon the addition of Ni in the series of Fe81-zNizGa19 ribbon, the magnetic anisotropy energy disappeared completely. Namely, the magnetic anisotropy energy because isotropic for the series Fe81-zNizGa19 ribbons, except when z is 0.

In soft ferromagnetic alloy devices, the basic requirements are that low coercivity (HC), and high saturation magnetization (MS). Fig. 5.4(a) shows MS

plotted as a function of z. As z increases from 0 to 24 in Fe81-zNizGa19, MS

decreases from 170 emu/g to 116 emu/g. Fig. 5.4(b) indicates that HC

increases from 4.8 Oe not a lot, as z increases except z=24. As will be discussed later in Chap. 7, this implies that there are other phases in the Fe57Ni24Ga19 alloy ribbon. At last, Fig. 5.4(c) shows that Hs does not change too much with increasing z.

84

-1000 -500 0 500 1000

-200 -150 -100 -50 0 50 100 150

200 M s =170.7 (emu/g) H c =4.84 (Oe)

SQR=4.7 (%) H s =634 (Oe)

θ=0 o

Fe

81

Ga

19

M ( em u/ g)

H (Oe)

Fig. 5.3 The easy-axis (θ=0o) hysteresis loops of the melt-spun Fe81Ga19.

85

0 5 10 15 20 25

110 120 130 140 150 160 170

(a) 180 Fe

81-z Ni z Ga 19

z (at. %) M s (em u/ g )

0 5 10 15 20 25 4

6 8 10

(b) 12 Fe 81-z Ni z Ga 19

z (at. %)

H c ( Oe )

86

0 5 10 15 20 25

500 550 600 650 700 750

(c) 800 Fe

81-z Ni z Ga 19

z (at. %) H s ( Oe )

Fig. 5.4 shows Saturation magnetization (Ms), coercivity (Hc), and saturation field (Hs) hysteresis of the melt-spun Fe81-zNizGa19.

87

5.3 Electrical resistivity

Fig. 5.5 illustrates the ρ vs. x plot, as z increases from 0 to 13, ρ of the melt-spun Fe81-zNizGa19 decreases little from 111 µΩcm to 95 µΩcm, as z increases from 0 to 13, ρ of the melt-spun Fe81-zNizGa19 increases little from 95 µΩcm to 108 µΩcm. The resistivity and lattice constants reaches minimum simultaneously for the melt-spun Fe68Ni13Ga19, indicating that substituting larger Fe2+ with smalls Ni2+ may introduced more carriers. The rapid increase of ρ of the Fe57Ni24Ga19, however, might be due to the existence of other phases arising from the excessive doping of Ni.

0 5 10 15 20 25

90 100 110

Fe 81-z Ni z Ga 19

z (at. %)

ρ (µΩ cm )

Fig. 5.5 Electrical resistivity (ρ) of the melt-spun Fe81-zNizGa19.

88

5.4 Young’s modulus of the ribbon

The magnetostriction is a dependence of Young’s modulus E of a magnetic material on its state of magnetization. When an originally demagnetized specimen is saturated, its modulus increases by an amount ∆E. The value of

∆E/E0

Fig. 5.6 shows the normal σ vs. ∆ε plot, which plot is called normal, because it is concave up, as shown in Refs. 2, 3, and 38. That is, the slope of the dotted fitting line (slope I) is smaller than that of the solid fitting line (slopeII). At the intersection of the slopes I and II lines, we can define the critical internal stress (σ

depends greatly on the way in which it is measured, as will be explained below[2].

ic) of the ribbon[3,38]. The physical meaning of σic can be considered as the critical transition point for the ribbon sample from the demagnetized state to the saturation state through the magneto-elastic mechanism; e.g., Fig. 8.26 of Ref.

14. Moreover, from slope II, we can determine the Young’s modulus (ES) in the saturated state. Also, from slope II and the intercept of the solid fitting line, we can find the elastic strain ∆εel and magneto-elastic strain ∆εme

𝐸0 = σ

∆𝜀𝑒𝑙 + ∆𝜀𝑚𝑒 (5.1)

[14, 22]. As a result of these two kinds of strain, the modulus in the demagnetized state is[2]

and the modulus in the saturated state is

89

𝐸𝑠 = σ

∆𝜀𝑒𝑙 (5.2)

These two relations lead to

∆𝐸

𝐸0 = 𝐸𝑠 − 𝐸0

𝐸0 =∆𝜀𝑚𝑒

∆𝜀𝑒𝑙 (5.3)

For sample of the Fe81Ga19 ribbon, we fixed σ = 25 Mpa to calculate ES and

∆E/E0 by Eq. 5.2 and Eq. 5.3. In Fig. 5.7, we find ES of the Fe81-zNizGa19

ribbons is in the range 115 to 52 GPa. In Fig. 5.8, we find ∆E/E0 is in the range 14% to 115%. In Fig. 5.9, σic not change a lot between Fe81Ga19 and Fe78Ni3Ga19, as z increases from 3 to 19 in Fe81-zNizGa19, σic increases, and σic

decreases at z = 24. There are two points to be noted here. Firstly, the

Fe57Ni24Ga19 has phases other than A2 phase existing in the ribbon, which may account for the deviation of the general trend in this series of ribbon. (As can be seen in Fig. 5.7- 5.9 and Fig. 5.12 in the next section.) Secondly, we were unable to obtain reliable data from Fe68Ni13Ga19 ribbon. The reason is not clear at present, and further investigations are need.

90

Fig. 5.6 The stress (σ) vs. strain (∆ε) curves of the as-spun Fe81Ga19

0 5 10 15 20 25

40 50 60 70 80 90 100 110 120

Fe

81-z

Ni

z

Ga

19

z (at. %) E s (Gp a )

ribbon.

Fig. 5.7 The Young’s modulus in the saturated state (Es) plotted as a function of z.

91

92

5.5 Magnetostriction data

The magnetostriction (λ) hysteresis curve of the Fe81Ni3Ga19 ribbon, under an external weight w = 208.6 g, which means the external stress σ= 25.7 MPa, is shown in Fig. 5.10. By applying a horizontal field HE, up to + 6 kOe, we tried to turn 𝑀��⃑𝑠 toward the transverse (or + x) directions, by 90o. Due to the reason of stress anisotropy, we could not support enough external field to saturate λ.

As expected, the λ vs. HE plot in Fig. 5.10 is symmetric, and ∆λ decreases from zero to -95 ppm for the as-spun Fe81Ni3Ga19

In Fig. 5.11, we still summarize all the values under the varied external weight and the same external field (6000 Oe) for the series of the melt-spun Fe

ribbon.

81-zNizGa19 ribbons. According to Ref. 13, they found that for the rapidly quenched Fe78Ni7Ga15 ribbon, its λ < 200 ppm under 6 kOe external field, which is roughly in agreement with our finding. In this study, that is the largest magnetostriction in the Fe74Ni7Ga19

Although we could not provide enough external field to saturate the sample, λ

ribbon.

s could be calculated from the ∆E effect. This effect since the applied stress causes a deformation through the change in domain magnetization in addition to the elastic deformation. In general, the deformation (∆εme) is caused by rotation magnetization or a displacement of 90o walls, but no deformation can be induced by 180o wall displacement. The relation of the

∆εme and λs in polycrystalline can be written as[2, 3]

93

∆ε𝑚𝑒 =3𝜆𝑠2

5𝐾𝑢 ∆ε𝑒𝑙. (5.4)

Since this gives the additional elongation,

3𝜆𝑠2 shows the sample of the ∆λ which is not saturated by external field, while Fig.

5.12 shows the sample of the λ

can be calculated. The results are shown in Fig. 5.12.

s which was calculated from the ∆E effect. In this study, we found that the values of ∣∆λ∣ in Fig. 5.11 are larger than the values of λs in Fig. 5.12. Since the Ni addition in Fe81Ga19 let the ribbons become more isotropic in magnetic anisotropy. When Ku≒0, ∆E effect would diverge. This reason makes the ∆E effect not be ideally used to calculate λs. But the ∆E effect model still shows that reducing Ku is good for the magnetic material.

94

Fig. 5.10 Magnetostriction of the Fe81Ni3Ga19 ribbon plotted as a function of a horizontal in-plane field under an external weight w = 208.6 g.

100 150 200 250 300 350 400 450 -160

Fig. 5.11 Under the 6 kOe external field, plotted the ∆λ VS. w for the series of the melt-spun Fe81-zNizGa19 ribbons.

95

0 5 10 15 20 25

0 20 40 60 80 100

120 Fe 81-z Ni z Ga 19

z (at. %) λ s (ppm )

Fig. 5.12 The melt-spun Fe81-zNizGa19 saturation magnetostriction (λs) is calculated by ∆E/E0, Es and σic.

96

6 Conclusions

6.1 For Films

We have made series of Fe81-xNixGa19/Si(100) and Fe81-yNiyGa19/glass films, with 0 x or y 26 at.%Ni, at room temperature by the magnetron sputtering method. Magnetic hysteresis loop, magnetostriction, and FMR measurements were performed on these films. Line width mechanisms of ∆H have been studied by many investigators. The most comprehensive channel of the dissipation of the energy from the precessing spin system is that through the eddy-currents induced by the precessing magnetization. Besides the effect of eddy currents, the hopping motion of electrons causes another route of energy dissipation, as first pointed out by Verwey[47]. Yager, Galt, and Merritt find the anisotropy forces the magnetization to rotate parallel to the direction of easy magnetization, and, for the same reason, rotation of magnetization may cause a change in the arrangement of two kinds of ions such as to rotate the easy direction toward the direction of magnetization[2, 48]. Thus the precession motion the magnetization is expected to cause a hopping of electrons, which is accompanied by loss of energy. In this study, we find the addition of Ni into Fe81Ga19 films that causes refined the magnetic anisotropy energy which let the HK decreases, 13.8 – 6.3 Oe, as at% Ni increases. On the other hand, we observed that (∆H)exp of each film is in general asymmetric. Hence, (∆H)exp is composed of two parts: (∆H)exp = (∆H)S + (∆H)A, where (∆H)A and (∆H)A are the symmetric and asymmetric parts. The explanation for this asymmetry is

97

believed to be related to the degrees of the structural and/or magnetic inhomogeneities in each film.

From Ref. 22, λs is 132 ppm for A2, -7 ppm for D019, and -32 ppm for L12, such that the D019 phase and L12 phase are detrimental to saturation magnetostriction. In this study, when y = 22 at.%Ni, there is only one single A2 phase, and when y =0, 4, 11, and 17 at.%Ni, there are mixed phases with A2 (major) and D019 and/or L12 phases (minor), λs

As x or y increases, we found that [I] 4πM

reaches a maximum at x or y = 22 at.%Ni

s just decreases a little, 16.6 – 15.0 KG, [II] HC is small, 34.4 – 13.8 Oe, [III] λs first increases and reaches a maximum at x or y = 22 at.%Ni, [IV] fFMR decreases, 1.6 – 0.8 GHz, [V] µR

increases, 1212 – 3993, and [VI] α decreases, 0.076 – 0.018. Thus, from this study we conclude that the Fe59Ni22Ga19/glass film should be most suitable for the magneto-electric microwave device application.

98

6.2 For Ribbons

We have made a series of Fe81-zNizGa19 ribbons by the rapidly quenching method. From XRD, these ribbons change the lattices constants which depend on number of z. From VSM studies, we found that the magnetic anisotropy Ku

decreases, as at%. Ni added in. As z increases from 0 to 24 in Fe81-zNizGa19, Ms decreases in general from 170 emu/g to 125 emu/g, and Hc inceases from 4.8 Oe to 11.7 Oe. We also discovered that as z increases from 0 to 19, ∆E/E0

In Ref. 4 and 22, there were added B in FeGa allays, one of the purposes is reduced K

increases. The most important, λ increases at z = 7 at.%Ni.

u. This way also reduces a lot the magnetization. The Ni addition in in FeGa allays not reduced too much magnetization, but reduced Ku

Thus, from this study we conclude that the Fe

.

74Ni7Ga19 ribbon should be most suitable for the magneto-electric device application.

99

7. Appendix

7.1 XRD discussion

In this study, we were unable to identity all diffraction peaks. Fig. 7.1 shows the XRD pattern of the Fe81Ga19 alloy film on Si(100) substrate. There are too many phases in the sample; however, it appears that film samples on the glass substrate are better than these deposited on the Si substrate. As result, our discussions were focused on film samples deposited on the glass substrate. Fig.

7.2 shows the XRD pattern of the Fe57Ni24Ga19 ribbon. Peak I is the peak with

Another disbelieving proof is the Curie temperature which was obtained from magnetic thermal gravimetric (MTG) scan up to 900

ribbon maybe consists of two phases, A2 and γ structure. The tree peaks look like the tree γ peaks respective.

Peak II correspondence γ(111), Peak III correspondence γ(200), and Peak II correspondence γ(220). diffraction peaks, and needs further investigation.

100

Fig. 7.1 XRD pattern of the FeGa alloy film on Si(100) substrate.

30 45 60 75 90

0 500 1000 1500 2000 2500

P e a k II I ( 2 θ= 50. 51

o

) Pe a k IV ( 2 θ= 74. 00

o

)

P eak I (2 θ= 29. 19

o

)

In st e n si ty

2 θ

deg.

P eak I I ( 2 θ= 43. 41

o

) (110) A 2 (200) A 2 (211) A 2

Fe

57

Ni

24

Ga

19

Ribbon

Fig. 7.2 XRD pattern of the Fe57Ni24Ga19 ribbon with the quenching rate (rotating copper wheel speed) was about 15m/s.

101

Fig. 7.3 MTG scans of the Fe57Ni24Ga19 ribbon.

102

7.2 TEM photo for the Fe

70

Ni

11

Ga

19

/Si(100) film

The cross-section transmission electron microscopy photo of the Fe70Ni11Ga19/Si(100) film is shown in Fig. 7.4. In Fig. 7.4(a), we find that the Fe70Ni11Ga19 alloys deposited on Si(100) substrate similar pillars, and the width of a pillar is quite large, about 25 nm. Fig. 7.4(b) shows the Fe70Ni11Ga19 film with some nano-crystals. Fig. 7.4(c) shows the Fourier transform pattern, which means crystal and amorphous in this film.

103

Fig. 7.4 The cross-section transmission electron microscopy photo of the Fe70Ni11Ga19/Si(100) film. (a) The Fe70Ni11Ga19 alloys deposited on Si(100) substrate similar pillars. (b) This shows the polycrystal substrate. (c) Shows the Fourier transform pattern.

104

7.3 σ vs. ∆ε of the Fe

68

Ni

13

Ga

19

ribbon

We could not obtain reasonable Es, ∆E and σic in the Fig. 7.5. The strain (∆ε) are to small too let the Es

unreasonable larger than 900 MPa.

0 60 120

0 30 60 90

Slop III Slop II

Slop I

Fe 68 Ni 13 Ga 19 Ribbon

σ (MP a )

∆ε (ppm)

Fig. 7.5 The stress (σ) vs. strain (∆ε) curves of the as-spun Fe68Ni13Ga19 ribbon.

105

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109

Biographical Notes

Chi-Ching Liu (劉奇青)

Sex : Male

Date of Birth : September 23, 1982

E-mail:

Education:

ccliu@phys.sinica.edu.tw

Research interests:

Magnetostriction and application; Magnetic domains and domain walls;

Ferromagnetic resonance

Selected Publications:

1. Magnetic properties of Fe-rich Fe-V alloy films ( Journal of Applied Physics 106, (2009 ) 013901)

2. Effects of Substrate Temperature on Magnetostriction of Fe

62

Co

19

Ga

19

3. Ferromagnetic resonance properties of Fe

/Si(100) Films (ICCE-20 Conference)

81-x

Ni

x

Ga

19

/Si(100) and Fe

81-y

Ni

y

Ga

19

4. Magneto-elastic and mechanical properties of Fe81-xNixGa

/glass films (Journal of Alloys and Compounds 562, 111 (2013))

19

/Si(100) and Fe

81-y

Ni

y

Ga

19

5. Magnetic domain studies of La

/glass films (MEMSM 2013 Conference)

0.7

Sr

0.3

MnO3 film deposited on SrLaAlO

3

(001) substrate (J. Phys. D: Appl. Phys., 46, (May 2013), 255001)

2001- 2005: B. Sc., Physics, Fu Jen Catholic University

2005- 2008: M. Sc., Institute of Optoelectronic Sciences, National Taiwan Ocean University

2010-2013: Ph. D., Dept. of Electrophysics, National Chiao Tung Univ.

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