Preparation and Characterization of Bi substituted gadolinium iron garnet
BixGd3-xFe5O12 films with x = 1 to 2.5 by Enhanced Metal Organic
Decomposition method
D. A. Wahid, J. Sato, M. Hosoda, and H. Shimizu
Department of Electronic and Information Engineering, Tokyo University of Agriculture and Technology , 2-24-16 Naka-cho,

Koganei-shi, Tokyo 184-8588, Japan

Bismuth substituted gadolinium iron garnet thin films (Bi xGd3-xFe5O12) were prepared with x = 1, 2, and 2.5 onglass substrates by enhanced metal organic decomposition (EMOD) method. We mixed the solution containing Fe2O3,
Bi2O3 and Gd2O3 carboxylates so that we could obtain desired Bi content x. X-ray diffraction (XRD), opticaltransmittance / reflectivity, and Faraday rotation (FR) were measured for characterizations in order to examine theirdependence on annealing temperatures and different amount of Bismuth substitution ( x). When BixGd3-xFe5O12 thinfilms were directly prepared on glass substrates, Bi 2O3 phase were observed by XRD measurements and withincreasing Bi content x from 1 to 2, the FR increased from 1.2 to 5.8 deg./μm at the wavelength of 530 nm. FR of
Bi2.5Gd0.5Fe5O12 thin films prepared directly on glass substrates were smaller (0.35 deg./μm) than those with x = 2.
When Bi2.5Gd0.5Fe5O12 thin films were prepared with annealing temperature of 620oC with Gd3Fe5O12 buffer layer on
glass substrates, the films showed garnet crystal structure and FR, which is comparable with that of Bi2.5Gd0.5Fe5O12
thin films prepared on (111) (GdCa)3(GaMgZr)5O12 (SGGG) single crystal substrates. These results demonstratethat BixGd3-xFe5O12 thin films can be prepared on glass substrates with controlled Bi content and that FR as high asthat prepared on the SGGG substrate can be obtained by the EMOD method.
Key words: magnetic garnet, enhanced metal organic decomposition method, Faraday effect.

1. Introduction

metal organic decomposition (MOD) method is a

Bismuth substituted rare-earth iron garnets have aconsiderable interest owing to their large magneto optic
effect. Large FR with high transparency in the visible tonear infrared range1) are key properties which made themagnetic

garnetmaterials

suitableforvariousapplications for magneto-optical device elements such as
in magnetoplasmonic structure2), optical isolators3),
circulators4,5), and magnet photonic crystals (MPCs)
used

in

magneto-optic

spatiallight

modulators(MOSLM)6-9).
Bismuthsubstituted

gadolinium

iron

garnet(Bi:GdIG) is a ferrimagnetic material and shows
perpendicular magnetic anisotropy, which is one of themost desirable materials for magneto optical devices
owing to its high optical transmittance and extremely
high magneto optical activity in the visible and nearinfrared regions 10,11) , which enable this material to havehigh frequency application. FR can be controlled by Bi
substitution of Gd. Therefore, it is very important tocontrol the amount of Bi substitution in order to control
and increase the FR. There are several methods toprepare the bismuth substituted rare-earth iron garnet
thin films such as a laser ablation12), a liquid phase
epitaxy13), RF magnetron sputtering14), etc. Among them,promising one to prepare magnetic garnet film, because
it is a simple fabrication method which is composed ofspin coating of the MOD solution and annealing, andguarantees high uniformity in chemical composition andpurity combined with chemical stability. It was reported
that BixGd3-xFe5O12, BixY3-xFe5O12, and BixY3-x(FeGa)5O12
thin films were prepared on gadolinium gallium garnet(GGG) 12-17) and glass substrates 18). We have prepared
Bi:GdIG thin films on GGG substrates by annealing
with and without O2 gas and investigated the crystal
growthprocessandmagnetic

anisotropy19).

Thefabrication of magnetic garnet such as Bi2.5Y0.5Fe5O12
films was reported by using Nd2Bi1Fe4Ga1O12 buffer
layers on glass substrate which was fabricated by the
MOD method, and FR of 13.8 deg./μm at = 520 nm wasreported for the Bi2.5Y0.5Fe5O12 films18). It is important toobtain BixGd3-xFe5O12 thin films having higher Bi
content x and FR.

However, it is reported that

preparation of BixGd3-xFe5O12 with high Bi content on
glass substrates is difficult12-17). Therefore, fabrication of
BixGd3-xFe5O12 thin films with various Bi content x andcharacterization of FR are important. In order toinvestigate the effect of changing the Bi content x on FR
of BixGd3-xFe5O12 thin films by increasing the Bi content

x systematically, we fabricated the BixGd3-xFe5O12 thinfilms on glass substrates by the EMOD method.

samples were pre-annealed at 550°C for 10 min. The

Furthermore, we used the Gd3Fe5O12 buffer layer inthickness by single spin coating step is typically 20 - 30

order to fabricate the BixGd3-xFe5O12 thin films with

nm. The conditions for spin coating, drying, andhigher x of 2.5 showing larger FR by the EMOD method.

pre-annealing were fixed. We changed the mixing ratioof the SYM-BI05 and SYM-GD01 solutions in order to

2. Experimentschange the Bi substitution x in BixGd3-xFe5O12 thin films,

We fabricated BixGd3-xFe5O12 thin films with x = 1, 2

and changed the final-annealing temperature. The

and 2.5 at different annealing temperatures of 620°C,

thickness of the samples slightly changes with the spin

650°C and 700°C on 15 mm x 15 mm glass substrate,coating speed, time and viscosity of the solutions. Spinand BixGd3-xFe5O12 thin film with x = 2.5 on 12 mm x 12

coating, drying and pre-annealing were repeated for 11

mm SGGG (111) single crystal substrate and Gd3Fe5O12

times to obtain an appropriate thickness. Spin coating,buffer layer / glass substrate by the EMOD method. The

drying and pre-annealing, were repeated 6 times for the

EMOD liquids used in this experiment are SYM-FE05

BixGd3-xFe5O12 films on the Gd3Fe5O12 buffer layer / glass

containing Fe2O3 carboxylates, SYM-BI05 containing

substrate.

Bi2O3 carboxylates, and SYM-GD01 containing Gd2O3

SGGG (111) single crystal substrate for a reference

carboxylates by Kojundo Chemical Laboratory so thatsamplewe could obtain BixGd3-xFe5O12 thin films with desired

BixGd3-xFe5O12 films prepared by pre-annealing process

Bi content x. Kojundo Chemical Laboratory Ltd provides

were then annealed at 620, 650 and 700 °C for 2 hours

their own MOD solutions, as well as EMOD solutions

for crystallization (final annealing). The pressure during

developed by Symetrix corporation of the United States

the annealing was atmospheric pressure. Bi:GdIG thin

and Kojundo Chemical Laboratory

Ltd20).

solution contains 2 – 3 kindsof metal oxides

carboxylates

as

and

the

FR.

The

amorphousfilms prepared in this study were characterized by x-ray
diffraction(XRD),

opticaltransmittance,

opticalcarboxylates in acetic ester to prepare BixGd3-xFe5O12

done at room temperature. We measured the XRD fromthin films. In case of preparation of BixGd3-xFe5O12 thin

the central part of the samples. The diameter d of thefilms by the MOD method, Bi content x is fixed. On the

x-ray

other hand, the EMOD solution contains one metal oxide

measurement

carboxylate in xylene and can be mixed with othercrystallinity of the samples over d = 0.4 mm. We

EMOD solutions containing other metal oxide. Therefore

estimated the thickness of the samples from the optical

it is possible to prepare the BixGd3-xFe5O12 thin films inreflectivity spectra, and discussed the relationshipany proportion of Bi content x, which enables greater

between XRD and FR spectra.

andGd2O3,

comparereflectivity, and FR spectra. All the measurement was

freedom

Bi2O3,

toFe2O3

degree ofsuch

The MOD

Also, we prepared a BixGd3-xFe5O12 film on

more precise control ofcomposition in order to prepare BixGd3-xFe5O12 thin films.

beam

is

about

results of

0.4

mm.

Therefore,

the XRD show

theaverage

3. Results and Discussion

When we prepare the BixGd3-xFe5O12 thin films with

Figure 1 shows the optical reflectivity spectra

different Bi content x by the EMOD method, the EMOD

(wavelength  = 250 - 2600 nm) of the BixGd3-xFe5O12

solutions

of

Fe2O3

carboxylate(product

namesamples annealed at 620, 650 and 700 °C, with the Bi

SYM-FE05),

Bi2O3

carboxylate(product

namecontent x = 0, 1, 2 and 2.5 on glass substrates. The

SYM-BI05), and Gd2O3 carboxylate (product nameincident direction of the light was normal to the sample.

SYM-GD05), are mixed and combined for different Bi

In order to estimate the thickness of the BixGd3-xFe5O12

content x, which is advantage compared with the MOD

films, we fitted the measured optical reflectivity spectra

method. The selected components were mixed in theto reproduce the experimental results by the calculated

desired stoichiometric ratio of BixGd3-xFe5O12 withreflectivity spectra.

different value of x = 1, 2 and 2.5 and stirred well. The

spectra by considering the multiple reflection inside thesolution was then filtered by advantec filter paper. The

BixGd3-xFe5O12 films by interfaces between air / film (af)solution was spin-coated in 2 steps process of 500 rpm

and film / glass substrate (fs). We assumed that the film

for 10 s and 2000 rpm for 20 s, followed by drying on a

thickness is uniform and the glass substrate is

hot plate at 120°C for 10 min and the solvent are

non-absorbing and incoherent material. The reflectivity

evaporated. In order to decompose the organic materials

R is calculated by the following formula (1) 21,22).

and obtain the amorphous metal oxide films, theWe calculated the reflectivity

(1)

R

where Rafs, is the reflectivity within the interface
between air (a), film (f), and the interface between film(f) and substrate (s), Rsfa is the reflectivity within theinterface between substrate (s), film (f), and theinterface between film (f) and air (a), and Tafs is thetransmission within the interface between air (a), film (f),and the interface between film (f) and substrate (s). Rafs,

Rsfa and Tafs include the effect of multiple reflections
inside the film and can be expressed by the following
formulas (2), (3) and (4). They are related to the film
thickness d, wavelength , and refractive index n - ik of
the film. Since the refractive index has wavelength
dependence, we divided the optical reflectivity spectra totwo regions ( < 1000 nm and  > 1000 nm), and changed
the refractive index and thickness to reproduce theexperimentally obtained optical transmission spectra23).
In the final stage of the fitting, the films thickness d is
obtained.

(2)

(3)

(4)

The simulated reflectivity spectra showed by thedotted lines in figure 1. The thicknesses were estimatedto 170 - 210 nm for the samples with x = 1, 200 - 260 nm
for the samples with x = 2, and 330 - 360 nm for the
samples with x = 2.5. The viscosity of the solution wasincreased with increasing the Bi content x.

Therefore

the film thickness increased with increasing the Bi
content x.
Figure 2 shows the XRD spectra of the fabricatedsamples on glass substrates.

The XRD spectra ofsamples shows some peaks associated with (420) planeof BixGd3-xFe5O12, (104) plane of Fe2O3, (112) plane of
Gd2O3, (008) plane of -Bi2O3, (200) plane of BiO3, (222)plane of -Fe2O3, and (130) plane of -Fe2O3 phases.

Fig. 1 Optical reflectivity spectra (solid lines) of the
BixGd3-xFe5O12 samples annealed at 620, 650 and
700 °C, with bismuth content x = 0, 1, 2 and 2.5 onglass substrates. The fitted spectra are shown bydashed lines.

b

a

a)

BixGd3-xFe5O12 420

e)

BiO3

b)

Fe2O3 104f)β-Fe2O3 222

c)

Gd2O3 112g)

ε-Fe2O3 130d)ε-Bi2O3 008

u)Unknown phase(Bi:GdIG / glass sub)x = 1, 620°C(Bi:GdIG / glass sub)x = 1,

650°C(Bi:GdIG / glass sub)x = 1,

700°C(Bi:GdIG / glass sub)x = 2,

620°C(Bi:GdIG / glass sub)x = 2,

650°C(Bi:GdIG / glass sub)x = 2,

700°C(Bi:GdIG / glass sub)x = 2.5 , 620°C(Bi:GdIG / glass sub)x = 2.5, 650°C(Bi:GdIG / glass sub)x = 2.5, 700°C

200

ab
b
a

u

c
a
u
c
Intensity (count)

a

b

d
u

a

u

d
u

b

e
a

b

d

a

u

g

e
b

d
u
u
a

a

b

g

f
(GdIG buffer layer / glass sub)

u
a

x= 0,

650°C

f
(Bi:GdIG / GdIG buffer layer/glass sub),x = 2.5, 620°C

10

20

30

40

50

60

70

2θ (deg)
Fig. 2 X-ray diffraction spectra of the BixGd3-xFe5O12 thin films on glass substrates at annealing temperature of620, 650 and 700 °C with Bismuth doped x = 0, 1, 2 and 2.5 on glass substrates and Bi2.5:GdIG on GdIG buffer
layer/glass substrate.

20

30

40

50

BiGdIG 888
SGGG 888

SGGG 666

BiGdIG 444
SGGG 444

SGGG 222

Intensity (count)
10

60
70
2θ (deg)

80

90

100

110

120

Fig. 3 X-ray diffraction spectra of the Bi2.5Gd0.5Fe5O12 thin film on SGGG (111) single crystal substrate at theannealing temperature of 620°C.

Please note that the vertical axis is in logarithmic scale.
When the Bi2O3, Gd2O3 and Fe2O3 carboxylates are
mixed with a ratio of 1 : 2 : 5, and the annealing
temperature of 620 – 700 oC directly prepared on theglass substrates, the diffraction signal from Fe2O3 islarger than that from BixGd3-xFe5O12. When the Bi2O3,
Gd2O3 and Fe2O3 carboxylates are mixed with a ratio of
2 : 1 : 5 and the annealing temperature of 620 – 650 oC
directly prepared on the glass substrates, the diffraction
signal from Gd2O3 is larger than that from BixGd3xFe5O12. When the annealing temperature is 700 oC, thediffraction signal from Bi2O3 is increased. When the
Bi2O3, Gd2O3 and Fe2O3 carboxylates are mixed with aratio of 2.5 : 0.5 : 5 and the annealing temperature of620 – 700 oC directly prepared on glass substrates, thediffraction signals from Bi2O3 and -Bi2O3 are much
more dominant than that from BixGd3-xFe5O12. The
diffraction peak associated with BixGd3-xFe5O12 were theweakest with x = 2.5 among all the samples without the
Gd3Fe5O12 buffer layer. With increasing the final
annealing temperature, the diffraction peak associatedwith ε-Bi2O3 increased. From the XRD spectra of thesamples, it is difficult to fabricate Bi:GdIG thin films
with high Bi content x = 2.5 directly on glass substrate.
In order to solve this problem, we fabricated agadolinium

iron

garnet(GdIG)

thin

film

with

composition of (Gd2O3:Fe2O3 = 3:5) as a buffer layer for
preparation of BixGd3-xFe5O12 thin films with higher Bi
content x of 2.5, with the thickness of 150 nm on theFig. 4 Optical transmittance spectra of the Bi:GdIG
samples annealed at 620, 650 and 700 °C, with thebismuth content of a) x = 2.5 on glass, GdIG buffer
layer / glass and SGGG (111) single crystal
substrates, b) x = 1 and 2 on glass substrates.

glass substrate at final annealing temperature of 650°C
by the EMOD method.

When the Gd2O3 and Fe2O3

carboxylates are mixed with a ratio of 3 : 5, thediffraction signals from Gd3Fe5O12, and -Fe2O3 aredominant.

Fig. 6 Faraday rotation spectra of the Bi2.5Gd0.5Fe5O12
samples annealed at 620°C with the bismuth content

x = 2.5 on gadolinium iron garnet buffer layer / glass
sub and SGGG (111) single crystal substrates.
phases such as ε-Bi2O3, BiO3 and Gd2O3 are suppressed.
The diffraction peak associated with β-Fe2O3 at theright side of the Bi:GdIG diffraction peak is associatedwith the Gd3Fe5O12 buffer layer. From figure 2, it was
confirmed that the Bi2.5Gd0.5-Fe5O12 thin film having
garnet crystal structure was prepared with the buffer
layer on glass substrate by the EMOD method.
Figure 3 shows the XRD spectra of Bi2.5Gd0.5Fe5O12
prepared by the EMOD method on (111) SGGG single
crystal substrate.

444 and 888 diffraction peaks are

Fig. 5 Faraday rotation spectra of the BixGd3-xFe5O12

clearly observed and other peaks associated withsamples with different annealing temperatures andpolycrystalline or impurity phases were not observed.

bismuth content(a) x = 1, (b) x = 2 and (c) x = 2.5.

The lattice constant a was calculated to 1.2587 nm. It
was reported that the lattice constant of Bi 2.5Gd0.5Fe5O12

Then we tried to fabricate a Bi2.5Gd0.5Fe5O12 thin film

samples prepared by liquid phase epitaxy (LPE) wason the GdIG buffer layer / glass substrate. The final

1.259

annealing temperature for Bi2.5Gd0.5Fe5O12 thin film

Bi2.5Gd0.5Fe5O12 thins films on (111) SGGG substrate.

was set at 620°C instead of the annealing temperature

By comparing the lattice constant of two materials andof 650°C shown in figure 2. This is because when thethe results of figure 3, we estimated the composition of

final annealing temperature of the Bi2.5Gd0.5Fe5O12 film

our single crystal film to Bi2.5Gd0.5Fe5O12 by the EMOD

is the same or higher than the final annealing

method.

temperature for the GdIG buffer layer/glass sub., theBi2O3, Gd2O3, Fe2O3, GdIG

part of crystal structure of the GdIG buffer layer can be

polycrystalline samples on the glass substrates weredestroyed25).

confirmed by comparing the lattice spacing d measured

Therefore, we set the final annealingnm24),

andcomparable

to

that

of

Also the diffraction peaks associated withand

BiGdIG oftemperature at 620°C for the Bi2.5Gd0.5Fe5O12 film onby the XRD to the powder diffraction files

the GdIG buffer layer/glass sub.

international

When the Bi2O3, Gd2O3 and Fe2O3 carboxylates are
mixed with a ratio of 2.5 : 0.5 : 5 and the annealing

ourcenterfor

diffraction

data

the

of

(ICDD).

Therefore, we estimated the fabricated crystal structureby the EMOD method to the garnet structure.

temperature of 620 oC with the Gd3Fe5O12 buffer layer

Figure 4 shows the optical transmittance spectra ofon glass substrate, the diffraction signal from BixGd3-

the BixGd3-xFe5O12 thin films on the glass substrates

xFe5O12 is the most dominant and the formation of otherwith / without Gd3Fe5O12 buffer layer and on (111)4. Conclusion

SGGG single crystal substrate. The Bi2.5Gd0.5Fe5O12 on
the Gd3Fe5O12 buffer / glass sub has high transparency

We have prepared BixGd3-xFe5O12 thin films on glassin visible and near infrared region, higher than thesubstrates, with and without Gd3Fe5O12 buffer layer

Bi2.5Gd0.5Fe5O12 film on (111) SGGG substrate.

prepared on glass substrates and (111) SGGG single

Figure 5 shows the FR spectra of the fabricatedcrystalsubstrate

by

the

EMOD

method.

We

BixGd3-xFe5O12 thin films crystallized at 620, 650, andcharacterized the XRD, FR and optical transmittance

700 °C with x = 1, 2 and 2.5 on glass substrates. The

spectra of the samples.

magnetic field of 1 T was applied perpendicular to theannealing temperature of 650 °C is the optimum

samples in order to fully magnetize the samples.

condition for crystallization of BixGd3-xFe5O12 on the

The samples with the annealing temperature ofglass

substrate.

The FR shows that the

From

the

XRD

spectra,the650°C show larger FR (negative) than the other samples

Bi2.5Gd0.5Fe5O12 samples on the Gd3Fe5O12 buffer layer

with x = 1, 2, and 2.5 annealed at 620 and 700 °C.

shows that the Bi:GdIG thin films were successfully

Therefore the annealing temperature of 650°C is the

fabricated on the glass substrates without forming Bi2O3

optimum condition for crystallization of the BiGdIG thin

and Gd2O3 phases, which are observed in samples

films on the glass substrate by the EMOD method. The

without Gd3Fe5O12 buffer layer.

FR of Bi:GdIG increased with increasing x to 2, andFaraday rotation (27.9 deg./μm at  = 533 nm) was

decreased in the sample with high Bi content of x = 2.5.

obtained on the sample with the Gd3Fe5O12 buffer layer

Figure 6 shows the FR spectra of the Bi2.5Gd0.5Fe5O12than that without Gd3Fe5O12 buffer layer, and thethin films on the GdIG buffer layer / glass substrate andFaraday rotation is comparable with that prepared on

SGGG (111) single crystal substrate. Bi2.5Gd0.5Fe5O12

SGGG (111) single crystal substrate.

thin film on the GdIG buffer layer / glass substratesuppress the formation of the Bi2O3 and Gd2O3 phases byshowed 27.5 deg./μm at the wavelength of 533 nm, which

the Gd3Fe5O12 buffer layer in order to prepareis 8 times larger than that without the GdIG buffer layer.

BixGd3-xFe5O12 thin films having higher Bi content x andThis is because the sample with the GdIG buffer layer

FR, from the XRD spectra and measurement of theshowedFaraday rotation.

thelargestdiffraction

signalfrom

the

Furthermore, larger

It is important to

These findings are important to

BixGd3-xFe5O12 and garnet structure, and the samples

realize BixGd3-xFe5O12 thin films having large Faraday

without garnet structure including other phases such as

rotation for future applications to MOSLMs and optical

Bi2O3 and Gd2O3 showing little FR,as shown in figure 2.

isolators on the glass substrates.

Maximum FR (negative) angle of the Bi2.5Gd0.5Fe5O12
thin films on SGGG substrate is 32.5 deg./μm at the
wavelength of 533 nm. The maximum FR of theBi2.5Gd0.5Fe5O12 thin films on the GdIG buffer layer /glass substrate is comparable with that on (111) SGGG
single crystal substrate. The FR of Bi2.5Gd0.5Fe5O12 thinfilms on the Gd3Fe5O12 buffer layer / on glass substrate(27.5 deg./m at  = 533 nm) is 3 time larger than that of
the reported Bi1.4Gd1.6Fe5O12

sample (9.3 deg./m at

= 520 nm.), which was fabricated by sintering, hotpress and annealing method26). Also it was reported that
Bi2.5Gd0.5Fe5O12 films on Nd2Bi1Fe4Ga1O12 buffer layers
on a glass substrate which was fabricated by the MOD
method had FR of 13.8 deg./m at  = 520 nm, which ishalf of the FR of our Bi2.5Gd0.5Fe5O12 thin films on the
Gd3Fe5O12 buffer layer / on glass substrate 18). Therefore,
our samples fabricated by the EMOD method showed 2 3 times larger FR compared with that of previously
reported BixGd3-xFe5O12 samples.

Acknowledgements

This

work

was

partially

supported by JSPS KAKENHI (Grant Number 24656010
and 15K13942) and Support Center for Advanced
Telecommunications
Foundation.

(SCAT)

Technology

Research,

The authors would like to thank Prof. T.

Sameshima for the guidance of the optical reflectivity
measurement.

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Received Jan. 27, 2016; Accepted May. 12, 2016