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Ferromagnetic enhancement and magnetic anisotropy in nonpolar-oriented(Mn, Na)-codoped ZnO thin filmsB. Lu, L. Q. Zhang, Y. H. Lu, Z. Z. Ye, J. G. Lu et al.Citation:Appl. Phys. Lett. 101, 242401 (2012); doi: 10.1063/1.4770290View online: http://dx.doi.org/10.1063/1.4770290View Table of Contents: http://apl.aip.org/resource/1/APPLAB/v101/i24Published by theAIP Publishing LLC.Additional information on Appl. Phys. Lett.Journal Homepage: http://apl.aip.org/Journal Information: http://apl.aip.org/about/about_the_journalTop downloads: http://apl.aip.org/features/most_downloaded

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Ferromagnetic enhancement and magnetic anisotropy in nonpolar-oriented(Mn, Na)-codoped ZnO thin films

B. Lu,a) L. Q. Zhang, Y. H. Lu, Z. Z. Ye,b) J. G. Lu, X. H. Pan, and J. Y. HuangState Key Laboratory of Silicon Materials, Department of Materials Science and Engineering,Zhejiang University, Hangzhou 310027, Peoples Republic of China

(Received 30 October 2012; accepted 21 November 2012; published online 10 December 2012)

High-resistive Zn0.95Mn0.05O and weak p-type nonpolar-oriented Zn0.94Mn0.05Na0.01O thins filmswere grown on quartz by pulsed laser deposition. Both samples exhibit room temperature

ferromagnetism while with Mn-Na codoping, the saturation magnetic moment is greatly enhanced. It

is revealed that the doped Mn impurities are substitutionally incorporated into the ZnO host. Magnetic

anisotropy was also observed in the Zn0.94Mn0.05Na0.01O film, which is the indication for intrinsic

ferromagnetism. The first-principles calculations reveal that codoping of Na in Zn0.94Mn0.05Na0.01O

changes the antiferromagnetic interaction to ferromagnetic due to the hybridization between spin-split

delocalized Mn 3d and shallow acceptor states of Na 2p, thereby enhancing the ferromagnetism.

VC 2012 American Institute of Physics. [http://dx.doi.org/10.1063/1.4770290]

Diluted magnetic semiconductors (DMSs) have attracted

immense interest for potential applications in spin electronics

and magnetic devices.1,2 Among them, the most studied areZnO-based DMSs due to the theoretical predictions of ferro-

magnetic above room temperature for these materials.3

Tremendous efforts have been devoted to the 3d transition-

metal (TM) doped ZnO and in particular, to the Mn-doped

and Co-doped ZnO systems.410 Experimental studies on

Mn-doped ZnO materials reached very conflicting results con-

cerning correlation between ferromagnetism (FM) and con-

duction polarity. FM above room temperature was reported

for both n-type9,11 and p-type7,12 Mn-doped ZnO thin films.

Thus, the circumstance under which Mn-doped ZnO can be

ferromagnetic is still debatable. Meanwhile, several theoreti-

cal approaches have concluded that doping with Mn atoms

does not lead to a FM ground state in ZnO and suggesting the

necessity of codoping, the presence of additional carriers plays

an important role in stabilizing and/or enhancing the magnetic

coupling by the codoping ions in Mn-doped ZnO,6,1316 which

has been experimentally confirmed in recent works. In view

of this, codoping appears to be a potential approach to obtain

intrinsic and enhanced FM in Mn-doped ZnO. In this letter,

we report on our experimental and calculated findings of Mn-

doped and (Mn, Na)-codoped ZnO thin films. The results

show strong evidence for Na codopant effect in tuning the

electrical activity and enhancing the effective magnetic

moments per Mn ion and for the intrinsic nature of ferromag-

netism in (Mn, Na)-codoped ZnO.Polycrystalline Zn1xyMnxNayO thin films were grown

on quartz substrates by pulsed laser deposition (PLD) using a

KrF excimer laser (Compex102, 248 nm, 5 Hz) from corre-

sponding ceramic oxide targets (nominal x0 0.05; y0 0,0.01). The laser repetition rate is 5 Hz and the energy per

pulse is 340 mJ. The base pressure of the deposition chamber

is 1 104 Pa, and films, $800 nm thick, were grown in an

O2 (99.999% purity) atmosphere (PO2 45 Pa) with a depo-sition rate of$0.44 nm/s. Film composition was determined

by inductively coupled-plasma (ICP) emission spectra with xbeing slightly greater than x0 (0.05) while y being slightly

smaller than 0.01 after measuring the magnetic properties.

The crystalline structures of the deposited films were charac-

terized by an x-ray diffractometer (XRD) (Bede D1) with Cu

Ka radiation (k 0.15406 nm). The electrical propertieswere investigated using a four-point probe van der Pauw

configuration (HL5500PC) at room temperature. To deter-

mine the valence state and local geometry of the Mn dopant

in the ZnO lattice, Mn k-edge XANES was employed. Mag-

netization studies were carried out using a superconducting

quantum interference device (SQUID) magnetometer using

an in-plane geometry (magnetic field parallel to the film) on

all samples, unless specified differently. In order to under-

stand the experiment results, first-principles calculations

were utilized to investigate the electronic structures and

magnetic interactions.

Figure 1 shows the XRD spectra for Zn0.95Mn0.05O (des-

ignated as ZMO) and Zn0.94Mn0.05Na0.01O (designated as

ZMNO) thin films. Both samples are of the wurtzite structure

of ZnO with no distinct evidence of secondary phases. In the

FIG. 1. XRD spectra of Zn0.95Mn0.05O and Zn0.94Mn0.05Na0.01O thin films

deposited on quartz substrates under identical growth conditions.

a)Author to whom correspondence should be addressed. Electronic mail:

[email protected] .b)

Electronic mail: [email protected].

0003-6951/2012/101(24)/242401/4/$30.00 VC 2012 American Institute of Physics101, 242401-1

APPLIED PHYSICS LETTERS 101, 242401 (2012)

http://dx.doi.org/10.1063/1.4770290http://dx.doi.org/10.1063/1.4770290http://dx.doi.org/10.1063/1.4770290http://dx.doi.org/10.1063/1.4770290mailto:[email protected]:[email protected]://crossmark.crossref.org/dialog/?doi=10.1063/1.4770290&domain=pdf&date_stamp=2012-12-10mailto:[email protected]:[email protected]://dx.doi.org/10.1063/1.4770290http://dx.doi.org/10.1063/1.4770290http://dx.doi.org/10.1063/1.4770290

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ZMO film, the non-polar related phases are minority as com-

pared to the polar one. While for the ZMNO film, the c-axis-

related peak is completely suppressed and the preferential

nonpolar 1010 plane predominant over other nonpolarplanes such as 1120 and 2020 planes is seen. The resultsindicate that Mn-Na codoping facilitates the formation of

nonpolar-oriented ZnO film on quartz substrates.

The Mn k-edge XANES spectrum of Zn0.94Mn0.05

Na0.01O is presented in Fig. 2 along with the reference mate-rials of Mn metal, crystalline MnO, and MnO2. The exis-

tence of these reference materials can be easily excluded

due to significant difference in XANES spectral shapes

and edge positions between that from them and from the

ZMNO. Additionally, the pre-edge feature at h$ 6534 eV(marked A) allows a definitive assignment to be made, as was

demonstrated for Mn-doped GaN.17 This small peak arises if

Mn substitutes Zn in tetrahedral coordination and exhibits

a 2 formal charge state. However, if the Mn is formally 3,there will be a pre-edge doublet.18 Moreover, other accompa-

nied near edge characteristics peaks of B (6547 eV), and C

(6556 eV) observed in ZMNO can be reproduced by simula-

tion19 and calculation20 when Mn dopants occupy Zn sites in

ZnO, indicating that Mn is effectively substituted into the

ZnO lattice and has been experimentally confirmed.21

Figure 3 shows the magnetization as a function of the

applied field at 300 K for the Zn0.95Mn0.05O and Zn0.94Mn0.05Na0.01O thin films. The diamagnetic contribution from the

quartz substrate has been subtracted from the raw data. Both

samples demonstrate ferromagnetic hysteresis. However, the

saturation magnetic moment (Ms) of the ZMNO film is

1.52lB/Mn, greater than that ($0.15lB/Mn) of ZMO film. Aswe know, neither Mn metal nor any oxide of Mn is RT ferro-

magnetic, the possibility of ferromagnetism in our ZMO and

ZMNO films originating from the secondary phases such asMn or Mn related oxides can be excluded, which is consistent

with the above structural analyses.

Figure 4 shows the out-of-plane (magnetic field perpen-

dicular to the film) and in-plane (magnetic field parallel to

the film) magnetic field dependences for a ZMNO thin film.

The magnetic anisotropy is a further proof of the intrinsic na-

ture of the ferromagnetism in ZnO DMS materials,5,22 since

cluster-related ferromagnetism is generally isotropic. The

easy axis of the magnetization is perpendicular to the surface

while the hard axis of magnetization is in the plane but with

larger coercivity (see inset). Similar anisotropic results werealso observed previously5,9 and the anisotropy is conjectured

somehow arose from an orbital moment.5

Based on the above results, the RTFM observed should

be intrinsic. In the ZMO sample, the Mn2 substitution of the

Zn2 does not introduce any carriers. Indeed, the as-grown

ZMO films in the present study are found to be highly insulat-

ing with q> 105 X cm. However, the weak p-type ZMNO

samples were reproducibly produced with hole concentration

of 9.51 1015-1.86 1017 cm3, being electrically stable overseveral months. The realization of p-type conversion in

Na-doped ZnO films verifies the suggestion that NaZn may be

a shallow acceptor.23,24 Moreover, the p-type conduction in

the Zn0.94Mn0.05Na0.01O with enhanced FM supports the pre-diction that the ferromagnetic Mn2:ZnO state should be

more stable in p-type samples.3 In order to provide more

insights into this issue, we employed first-principles calcula-

tions on the electronic structures and magnetic interactions

FIG. 2. Experimental Mn k-edge XANES spectra of Zn0.94Mn0.05Na0.01O,

Mn metal, MnO, and MnO2.

FIG. 3. Magnetization hysteresis loops of Zn0.95Mn0.05O and Zn0.94Mn0.05Na0.01O thin films at 300 K.

FIG. 4. Anisotropic magnetism for a (Mn, Na)-codoped ZnO thin film

(Zn0.94Mn0.05Na0.01O). The in-plane magnetization shows a smaller satu-

rated moment than out-of-plane magnetization. The inset is a magnified plot

near zero field showing larger coercivity for in-plane magnetization.

242401-2 Lu et al. Appl. Phys. Lett. 101, 242401 (2012)


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between the Mn ions in the Mn doped and (Mn, Na)-codoped

ZnO. Since it is previously suggested that in the Mn-doped

ZnO, the Mn distribution is slightly weighted in favor of

nearest-neighbor pairs as dimmers via an intervening O atom

(rather than stochastic distributed),

8,15,25

thus in the presentcalculations, the Mn-Mn positions were arranged in a close

configuration, in which the Mn ions in the same unit cell were

separated by a single O ion. Likewise, the Na codopant is

unlikely to distribute stochastically in the film due to the lim-

ited concentration. Our calculations show that it is energeti-

cally favored when Na is accommodated near the Mn-O-Mn

dimmer. Thus, we consider the geometry in which the Na ion

substituted the nearest neighboring Zn in the same chain of

Mn dimer as MnOMnONabonds.

The densities of states (DOSs) for the ZMO and the

ZMNO are illustrated in Fig. 5. For the Mn-doped ZnO, it is

noticing that, despite the hybridization between the Mn 3d

and O 2p states (Fig. 5(a)), Mn 3d states are rarely intro-duced at the Fermi level and no free carriers to mediate the

long range FM interaction. Therefore, the superexchange

interaction between the neighboring Mn2 ions is antiferro-

magnetic (AFM) in character (AFM state is 0.05 eV lower in

energy than FM state). The origin of the observed small

moment (0.15lB/Mn) in the insulated Zn0.95Mn0.05O film

should arise from other mechanism such as bound magnetic

polaron, as suggested previously in a nonequilibrium pro-

cess.25 Turning to the codoped sample, as Na atoms replace

some of the Zn sites in the Mn-doped ZnO, FM ground state

is about 0.3 eV lower in energy than AFM. The total energy

calculations revealed that a Na dopant derived shallow

acceptor-type impurity state (spin-split) in close proximity to

the valance band edge with binding energy around 320 meV

appeared (see Fig. 5(b)), which accounts for the p-type

conductivity in the film. Meanwhile, the Mn 3dpartial DOSs

are strongly hybridized with the Na 2p gap state. This inter-

action (p-d hybridization) leads to a ferromagnetic coupling

between the two Mn ions mediated by holes (introduced by

Na codoping). That is, the codoping of Mn and Na in ZMNO

changes the Mn-Mn antiferromagnetic interactions to ferro-

magnetic coupling and thereby enhances the magneticmoment in the Zn0.94Mn0.05Na0.01O. Our results are in agree-

ment with previous theoretical works that ferromagnetism

favors in p-type Mn2:ZnO3,8,26,27 and are an extension of

the spin-split donor impurity band model (Ref. 5) considered

exclusively ferromagnetism in n-type materials.

In summary, Zn0.95Mn0.05O and Zn0.94Mn0.05Na0.01O thin

films with RTFM were grown on amorphous quartz substrate

using PLD. The XRD and XANES analyses as well as electri-

cal measurements show that Mn-Na codoping leads to p-type

fully non-polar Zn(Mn, Na)O thin film with Mn incorporated

substitutionally into the ZnO lattice at Zn sites. Compared to

the Mn monodoped ZnO, the saturation magnetic moment is

greatly enhanced by almost a factor of ten for the Mn-Na

codoped sample. The observation of magnetic anisotropy

in p-type ZMNO film indicates that the ferromagnetism is

intrinsic. First-principles calculations reveal that intrinsic

Mn-doped ZnO favors AFM ordering and codoping of Mn

and Na in Zn0.94Mn0.05Na0.01O changes the antiferromagnetic

interaction to ferromagnetic due to the hybridization between

Mn 3d and Na 2p at band gap. The hole-mediated FM

obtained in p-type Zn0.94Mn0.05Na0.01O is consistent with that

there is requirement of a hole-rich environment for FM pre-

dicted by theory.

This work was supported by the National Natural

Science Foundation of China (Grant Nos. 51002134 and

11004171) and Qianjiang Talent Project of Zhejiang Prov-

ince (Grant No. 2011R10044).

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